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QUALITY

ASSURANCE

PROGRAM PLAN

B C LABORATORIES, INC.

4100 ATLAS COURT

BAKERSFIELD, CA 93308

(661) 327-4911

FAX (661) 327-1918

www.bclabs.com

Carolyn Jackson Sara Guron

CEO/President Quality Assurance Officer

(661) 327-4911 Ext. 213 (661) 327-4911 Ext. 288

Effective Date: January 08, 2016

UnControlled Copy:

Issued to:

Printed Date:

Location:

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QUALITY ASSURANCE PROGRAM PLAN OF


Approved by

Signed by

Date

CEO/President:

Technical Director:

Quality Assurance

Officer:

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BC LABORATORIES, INC.

QUALITY ASSURANCE PROGRAM PLAN

TABLE OF CONTENTS

TABLE OF CONTENTS

PAGE i

SECTION

CONTENTS

# of PAGES

REVISION

DATE

PAGE #

I.

Introduction

2

13

03/17/16

1-1 thru 1-2

II.

Organization, Responsibilities,

Communication and Redundancy

14

29

03/17/16

2-1 thru 2-14

III.

Quality Assurance Objectives

1

10

01/08/16*

3-1

IV.

Sampling Procedures

8

20

01/08/16

4-1 thru 4-8

V.

Sample Custody

6

18

01/08/16

5-1 thru 5-6

VI.

Facilities

4

20

01/08/16

6-1 thru 6-4

VII.

Personnel / Training

4

16

01/08/16*

7-1 thru 7-4

VIII.

Records / Documents

11

13

03/17/16

8-1 thru 8-11

IX.

Instrumentation

19

31

01/08/16

9-1 thru 9-19

X.

Calibration Procedures and Frequency

20

26

01/08/16*

10-1 thru 10-20

XI.

Analytical Procedures

9

22

01/08/16*

11-1 thru 11-9

XII.

Data Reduction, Validation and

Reporting

14

21

01/08/16*

12-1 thru 12-14

XIII.

Analytical Quality Control

5

16

01/08/16*

13-1 thru 13-5

XIV.

Performance and Systems Audit

7

21

01/08/16

14-1 thru 14-7

XV.

Data Assessment Procedures

6

18

03/17/16

15-1 thru 15-6

XVI.

Preventive Maintenance

6

13

01/08/16*

16-1 thru 16-6

XVII.

Corrective Action/Quality

Improvement

8

14

01/08/16

17-1 thru 17-8

XVIII.

QA Reports to Management

1

8

01/08/16*

18-1

XIX.

Suppliers / Subcontractors

3

9

01/08/16*

19-1 thru 19-3

XX

Security

3

7

01/08/16*

20-1 thru 20-3

XXI

Code of Ethics

3

8

01/08/16*

21-1 thru 21-3

Appendix

A. SOP Listing

B. Established MDL/PQL's

C. Employee Evaluation

D. QC Logic Flow Diagrams

E. Process Flow Diagrams

F. Ethics Agreement

G. Flag Index

H. Employee SOP Acknowledgement and Agreement Form

A-1 thru A-5

B-1 thru B-21**

C-1 thru C-3*

D-1 thru D-17 *

E-1 thru E-16*

F-1*

G-1 thru G-5*

H-1 thru H-5

Figures

1. Personal Signatures and Initials Identification

2. Laboratory Organizational Chart

3. Bottle Order Form

2-13

2-14

4-5

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QUALITY ASSURANCE PROGRAM PLAN TABLE OF CONTENTS

TABLE OF CONTENTS

PAGE ii

4. Example of Chain-of-Custody Form 5. Cooler Receipt Form 6. Laboratory Floor Plan 7. Internal Assessment Schedule 8. Preventative Maintenance Schedule Example 9. System Improvement Report Form

5-5 5-6 6-4

14-3 thru 14-5 16-6 17-7

Tables

1. Analysis Reference Chart 2 500 Series Semi-Volatile Organics 3. 8000 Series Semi-Volatile Organics 4. 8000 Series Volatile Organics 5. Metal Methodologies 6. Organic Methodologies 7. Inorganic Methodologies 8. Level of QC Effort

4-5 thru 4-7 10-15 thru 10-1610-17 thru 10-1810-19 thru 10-20

11-7 11-8 11-9 13-5

Note: * = The following QAPP Sections have been Reviewed on 01/08/2016 (No Changes were needed) * * = MDL’S listed in the Appendix B of the QAPP may not be the current MDL’S. Please contact BC Labs to confirm sensitivity.

*** = The sections in red were updated in March of 2016



ACRONYMS

ACRONYMS

PAGE iii

AA Atomic Absorption

AAI Auto-analyzer

BCL BC Laboratories, Inc.

CERLA Comprehensive Environmental Response,

Compensation, and Liability Act.

BFB Bromofluorobenzene

CCB Continuing Calibration Blank

CCC Calibration Check Compound

CCV Continuing Calibration Verification

CLP Contract Laboratory Program

COC Chain of custody

CRDL Contract Required Detection Limit

CV Cold Vapor

DOD Department of defense

DOE Department of energy

DFTPP Decafluorotriphenylphosphine

DQO Data Quality Objective

Dup Duplicate

EB Equipment Blank

ELAP Environmental Laboratory Accreditation

Program

GC Gas Chromatography/Chromatograph

GC/MS Gas Chromatography/Mass Spectrometry

GFAA Graphite Furnace Atomic Absorption

GHAA Gaseous Hydride Atomic Absorption

IC Ion Chromatography/Chromatograph

ICP Inductively Coupled Plasma

ICP/MS Inductively Coupled Plasma/Mass

Spectrometry

ICS Interference Check Sample

ICV Initial Calibration Verification

IDC Initial Demonstration of Competency

IS Internal Standard

LCL Lower Control Limit

LCS Laboratory Control Sample

LOD Limit of Detection

LOQ Limit of Quantitation

MB Method Blank

MCL Maximum Contaminant Level

MDL Method Detection Limit

MS Matrix Spike

MSD Matrix Spike Duplicate

PB Preparation Blank

PQL Practical Quantitation Limit

QAPP Quality Assurance Program Plan

QA/QC Quality Assurance/Quality Control

RCRA Resource Conservation Recovery Act

RFP Request for Proposal

RFQ Request for Quotation

RL Reporting Limit

RLS Reporting Limit Standard

RPD Relative Percent Difference

RSD Relative Standard Deviation

RSO Radiological Safety Officer

SAP Sampling Analysis Program

SIF System Improvement Form

SM Standard Methods

SMC System Monitoring Compound

SOP Standard Operating Procedure

SOW Statement of Work

SPCC System Performance Check Compound

SRM Standard Reference Material

STLC Soluble Threshold Limit Concentration

TB Trip/Travel Blank

TCLP Toxicity Characteristic Leaching

Procedure

TOX Total Organic Halides

TQM Total Quality Management

TRPH Total Recoverable Petroleum

Hydrocarbons

TTLC Total Threshold Limit Concentration

UCL Upper Control Limit

WET Waste Extraction Test

WPS Word Processing Specialist

ZHE Zero Headspace Extraction

UCMR Unregulated Contaminated Monitoring

Regulation

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INTRODUCTION

SECTION I

REVISION NO. 13

EFFECTIVE DATE: 03/22/16

Page 1-1

1.0 OBJECTIVES

The primary objectives of the BC Laboratories, Inc. (BCL) Quality Assurance Program Plan (QAPP) are to provide

QA/QC guidelines to 1) assure the data produced is of known quality, 2) ensure our organization is capable of

providing results which are of value to our customers, 3) ensure the system can consistently perform under adverse

conditions, and to 4) comply with quality goals and objectives as set forth in government and industry standards.

1.1 POLICY STATEMENT

B C Laboratories Inc. is an organization committed to providing legally defensible data that is technically valid

and in accordance with professional standards, project goals, and government regulations. The management

and staff at B C Laboratories, Inc. are committed to use all available resources to supply accurate, precise,

timely and fully documented results. BCL=s goal is to provide analytical results and services which are of value

to our customers.

1.2 COMPONENTS OF THE QUALITY PROGRAM

Our overall program can be broken down into five essential parts: 1) Preclusion, 2) Assessment, 3) Validation,

4) Corrective Action, and 5) Improvement.

PRECLUSION: This is comprised of an orderly program of positive actions taken before and during analyses

to ensure that analytical systems are functioning properly. Components include quality control planning,

training, documented and approved methodologies, calibration of instrumentation, instrument maintenance,

comprehensive standardization, control charting, internal and external monitoring.

ASSESSMENT: This includes all components of determining analytical performance. Components include

matrix duplicates, matrix spikes, matrix spike duplicates, post spikes, blank spikes, blank spike duplicates,

laboratory control samples, calibration checks, calibration blanks, method blanks and surrogate additions.

Inclusion of all or some of these components and their frequencies are method dependent. B C Laboratories'

standard operating procedures (SOP's) contain all pertinent information concerning respective QC criteria

needed for assessment and approval of data. The adequacy of the QC program is measured through internal and

external auditing and client feedback on customer surveys.

VALIDATION: This consists of all the steps taken to ensure that generated analytical data is complete and

correct. Steps include maintenance of sample tracking and data processing systems, technical review of raw

data and final results review and approval by management staff.

CORRECTIVE ACTION: The actions rendered to determine the causes of quality defects and restore proper

function of the analytical system. This includes troubleshooting techniques, re-evaluations of analyses and/or

methodologies, dilution, calculation checks and continued training of analysts.

IMPROVEMENT: Actions taken to improve standard quality baselines. Steps include assessing windows of

improved performance, total quality management training of personnel, and research / development.

1.3 OTHER SOURCES FOR QUALITY GUIDELINES

Since BCL=s scope of work is very diversified, pertinent Standard Operating Procedures (SOP's) are used at the

bench level to provide guidance and direction. Specific project plans are developed to narrow the scope of

work, and thus provide QA/QC protocols on a limited scale and provide for possible modifications to standard

practice.

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INTRODUCTION

SECTION I

REVISION NO. 13


Page 1-2

1.4 REVISION PRACTICES

The QA Officer is responsible for the maintenance of the QAPP. Review of this plan should take place by each

department supervisor and President before the end of each calendar year. All revisions and additions are

submitted to the word processing specialist for entry, and then each revision is reviewed by pertinent personnel.

Once final approval is granted, the revision number is sequentially increased by one and the date of approval is

recorded. All revised sections are distributed to persons who have controlled copies of the QAPP.

1.5 SUMMARY

BC Laboratories, Inc. is an organization committed to providing useful, legally defensible and technically valid

results to all of our clients. Incorporating a commitment from upper management, TQM training, process

control and improvement, and a system of constant monitoring of the work process assures us of satisfying our

goals. Our QAPP provides the guidelines to achieve our goals.

1.6 BC Laboratories, Inc. Certifications

BCL Certifications

Expiration

Date

Oregon NELAP - Accreditation Certification # 4032-002 04/22/2016

DoD-ELAP - United States Department of Defense Environmental Laboratory Accreditation

Program Certificate # L14-199-R1. ISO/IEC 17025:2005 DOD QSM version 5.0. July 2013

07/10/2016

CA ELAP (SWRCB) - State of California, Department of Health Services, Environmental

Laboratory Accreditation Program (ELAP) Certificate No 1186

05/31/2016

Alaska – The State of Alaska, Department of Environmental Conservation Certificate # UST-101 04/04/2016

Nevada - State of Nevada, Department of Conservation + Natural Resources; Division of

Environmental Protection. Certification # CA000142012-1 07/31/2016

DOE - Department of Energy, Consolidated Audit Program (CAP)

County Sanitation Districts of Los Angeles County Laboratory ID No 10199

Vendor Approval list - Shell Global Solutions, Benzene Waste NESHAP Audit

1.7 REFERENCE DOCUMENTS

BC Laboratories, Inc. in its continuing effort to maintain a quality laboratory environment references Good

Laboratory Practices and DOE 414.1.

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ORGANIZATION, RESPONSIBILITIES, COMMUNICATION AND REDUNDANCY

SECTION II

REVISION NO. 29


PAGE 2-1

2.0 RESPONSIBILITIES

Job responsibilities must be properly designated in order to efficiently conduct work, manage processes and plan for improvement and

change. General job responsibilities and job requirements are addressed in the BC Laboratories, Inc. Job Description Manual.

Responsibilities outlined here in this document, cover those duties which may not be covered in detail in the Job Description Manual.

(See section 2.3 for Specific Responsibilities)

2.0.1 Approval Verifications

The responsibility of approval of final work lies with middle and upper management (Please refer to pg.2-13). Page

(2-13) illustrates examples of signatures and initials of persons with the authority of final approval.

2.1 ORGANIZATION

The structural organization of the laboratory is illustrated in Figure 2. The laboratory has five analytical operation

groups; Inorganics, Metals, Organics (Volatiles, Semi-Volatiles) and Petroleum. These groups are supported by six

departments which include Sales and Marketing, Laboratory Information Management System, Client Services,

Safety, QA/QC, and Human and Resources.

2.2 COMMUNICATIONS

The effectiveness of any organization can, in large part, be measured by the efficiency of the communications

systems. Communication paths and flow are constantly evolving by increased use of technology and heightened

focus on customer satisfaction.

2.2.1 Communication Systems

2.2.1.1 Board Meetings and Biweekly Executive Committee Meetings

Discussions on lab direction, major business and labor decisions and policy.

2.2.1.2 Biweekly Technical Department Manager Meeting:

Held as a forum to 1) discuss decisions from board meetings, 2) review analytical department

capacities and late work, 3) review potential new projects, 4) discuss any quality improvement

ideas, and 5) to initiate project/process planning.

2.2.1.3 Minutes from Executive Committee Meeting:

Posted to communicate topics covered to employees.

2.2.1.4 Department Meetings:

Held on a regular schedule or on as needed basis. Used to convey pertinent information within

respective departments.

2.2.1.5 Project Planning Meetings:

Scheduled meeting with the purpose of planning and organizing projects.

2.2.1.6 Laboratory Memos:

Posted records that inform employees of information of interest or reiteration of policy.

2.2.1.7 Training Modules:

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SECTION II

REVISION NO. 29


PAGE 2-2

Structured sessions, which are designed to increase quality through basic skill and knowledge.

2.2.1.8 Laboratory literature

2.2.1.8.1 Employee Policy Manual - Outlines the employee benefit package and the laboratory

rules of conduct.

2.2.1.8.2 QAPP - Contains the protocols, parameters and policies of BCL=s quality system.

2.2.1.8.3 SOP=s - Approved, controlled documents, which describe the operative for given

procedures.

2.2.1.8.4 Chemical Hygiene Plan - The safety compliance guide, which outlines all laboratory

safety policies and safety engineering plans.

2.2.1.8.5 Injury and Illness Prevention Plan - Protocols on the prevention and handling of

workplace injuries.

2.2.1.8.6 Customer surveys - Forms which provide for customer feedback regarding quality, price,

and service.

2.2.1.8.7 System Improvement Forms - Vehicle by which quality improvement and corrective

action can be communicated and addressed by all employees.

2.2.1.8.8 Quality Assurance Protocols Manual (QAPM) - Acts as a bench working manual.

2.2.1.8.9 Employee Safety Manual. Manual that outlines safety rules and policies.

.

2.2.1.8.10 Affirmative Action Plan for minorities and women - the principles of equal employment

opportunity

2.2.1.8.11 Substance Abuse Policy Manual - protocol to provide a drug-free environment.

2.2.1.9 Comments section of client=s LIMS files and laboratory bench sheets - Information regarding

non-standard client-specific practices or requirements.

2.2.1.10 Internal E-mail:

Mechanisms used to communicate information on an informal level.

2.2.1.11 External E-mail:

Mechanisms used to communicate and transfer client information.

2.2.1.12 Sales correspondence:

Informal transfer of pertinent information obtained during sales calls.

2.2.1.13 Client Service correspondence:

Information obtained by project coordinators and managers during the course of verbal and electronic

correspondence.

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SECTION II

REVISION NO. 29


PAGE 2-3

2.2.1.14 Client training seminars:

Training sessions conducted by the labs that provide clients with valuable information regarding

internal processes or other important information.

2.2.1.15 Complaint Forms:

Forms that are used to document incidences of client initiated quality failures.

2.2.1.16 External Seminars:

Informational gatherings, which would hopefully provide information regarding industry trends

and changes, or provide value through advanced training.

2.2.1.17 BCLABNET

Program used as a client service tool. Website used to expand our market and to act as a

mechanism for services such as result status, historical data archiving and correspondence.

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SECTION II

REVISION NO. 29


PAGE 2-4

2.3 SPECIFIC RESPONSIBILITIES

I CEO/President

(Allocate and secure capital to support laboratory activities and staff.)

Appointed Deputy (Vice President)

1. Procurement

2. Insurance Policy Maintenance

3. Business direction and development.

4. Director of the Business Plan.

5. Supervisor of all Department Supervisors, Accounts Payable/Receivable,

Maintenance Technicians, QA/QC and Human Resources /Health & Safety Coordinator

6. Capital Management

A Accounts Payable / Receivable/Billing Clerks

1. Client account maintenance.

2. Collections.

3. Financial Records.

4. Invoicing.

5. Distributing / mailing of invoices.

B Maintenance Technicians

1. Laboratory maintenance chores.

2. Installation of laboratory hoods.

3. Maintenance of laboratory supplies.

4. Maintenance of the waste disposal site.

C. HR/Health & Safety Coordinator/Radiological Safety Officer

1. Maintenance of the Safety Program.

2. Oversees the Waste Disposal Program.

3. Injury response.

4. Spill response.

5. Fire response.

6. Employees and upper management liaison, new hires coordinator

7. Radiological Safety Officer (RSO)

D. Quality Control

E. Laboratory Coordinator

II Vice President

Appointed Deputy (President)

1. Development of sampling program plans.

2. Field Service Purchasing.

3. Marketing strategies, analysis and sales efforts.

4. Supervision of all Business Development Specialist

8. RFQ and quote completions using the LIMS Quote Program.

9. Quality Improvement of Processes.

10. Monitoring capacities.

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SECTION II REVISION NO. 29


PAGE 2-5

11. Maintenance of Marketing Materials.

A. Business Development Specialist

1. Sales

2. Initial Client Contact

3. Set prospect meetings, presentations and close sales

B. Marketing and Sales Coordinator

1. Quote completions using the LIMS Quote Program.

2. To provide the laboratory information for use in benchmarking.

2. Review Sales Contract

III. Technical Director/Radiological Safety Officer

Appointed Deputy (Director of Human Resources)

1. Oversees day-to-day activities of the laboratory

2. Provides leadership, by example, establishing and maintaining quality standards and in conjunction with the

Director of Human Resources, hire, counsel, discipline, provide training and monitor performance of those

reporting to the Technical Director

3. Responsible for all analytical and technical activities of the laboratory

4. Responsible for the accuracy and quality of all data reported by the laboratory

5. Final Report approval

6. Delegates Quality Improvement of Processes

7. Works in conjunction with managers of laboratory to attain company goals for growth


9. Compliance with DoD QSM and ISO 17025:2005

IV. Laboratory Coordinator

Appointed Deputy (Technical Director)

1. Program management and operations director.

2. RFP and bid approval - Sales

3. Final Report Approval.

4. Delegates Quality Improvement of Processes.

5. Resource person for laboratory personnel

6. Handle issues relating to analytical reports and quality control and dealing with analytical testing questions

7. Assist client service teams with reporting results in nonstandard formats and electronic deliverables.

8. Work with Technical Director, Supervisors, and Team Leaders to direct activities in the analytical portion of

the lab.

9. Provide input and perspective to President from the analytical and LIMS areas of the laboratory

10. Train in the use of the LIMS.

11. Assist LIMS Manager in development of new features or refines existing features of the LIMS

12. Define Quality Control processing tests in the LIMS.

13. Maintain MDL, PQL, and validation parameters in the LIMS

V. LIMS Manager

Appointed Deputy (Laboratory Coordinator)

1. LIMS development, modification, and maintenance

2. LIMS training

3. Data reporting formatting

4. Electronic Data archiving and securement

5. Electronic Data Deliverables

6. LIMS equipment and supply approval

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PAGE 2-6

7. Supervision of LIMS Assistant

8. Delegate Quality Improvement of Processes

A. LIMS Programmer

1. LIMS Training

2. Electronic Data Deliverables formatting

3. LIMS Maintenance

4. Data Processing

5. Programming

6. Writing SOPs

7. Website Maintenance

B LIMS Specialist

1. Repair and troubleshoot computers and printers

2. Routine maintenance of computers and printers

3. Purchasing supplies.

4. Creating and editing report definitions.

5. Maintain documentation of all repairs, troubleshooting and maintenance of computers and printers

VI. Semi-Volatile Organics Manager


1. Supervision and management of all organics testing analysts and preparation technicians

2. Sample throughput and scheduling (prioritization)

3. Turnaround / holding time monitoring

4. Method and chemistry consultation

5. Data review, approval, and interpretation

6. Method development

7. Adherence of work to project specific goals

8. SOP Development and review

9. Instrument / supply procurement

10. Training

11. Quality Improvement of Processes

A. Semi-Volatiles Organics Preparation Technicians

1. Sample preparation and extraction in accordance to QC protocols

2. Documentation of tasks.

a. Preparation Logs

b. Bench worksheets

c. Reagent Logs

d. Maintenance Log

3. Documentation review

4. SOP development

5. Training

B. Organic Method Analysts

1. Sample analysis in accordance to QC protocols.

2. Reporting of sample results onto bench worksheets.

3. Analysis and instrument documentation.

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PAGE 2-7

a. Instrument maintenance

b. Ordering instrument supplies

c. Analysis records

(1) Run / Analysis Log

(2) Standard Logs

(3) Reagent Logs

(4) Maintenance Logs

4. Temporary data storage



7. SOP development

8. Training

VII Volatile Organics Manager


1. Supervision and management of all organics testing analysts and preparation technicians

2. Sample throughput and scheduling (prioritization).

3. Turnaround / holding time monitoring.

4. Method and chemistry consultation. Data review, approval, and interpretation.

5. Method development.

6. Adherence of work to project specific goals.

7. SOP Development and review.

8. Instrument / supply procurement.

9. Training.


A. Organic Method Analysts

1. Sample analysis in accordance to QC protocols.

2. Reporting of sample results onto bench worksheets.

3. Analysis and instrument documentation.

a. Instrument maintenance.

b. Ordering instrument supplies.

c. Analysis records.

(1) Run / Analysis Log.

(2) Standard Logs.

(3) Reagent Logs. Maintenance Logs



6. SOP development

7. Training

VIII. Petroleum Department Manager

Appointed Deputy (Project Manager)

1. Supervision and management of all Petroleum testing

2. Development of sampling program plans

3. Sample throughput and scheduling (prioritization).

4. Turnaround / holding time monitoring.

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PAGE 2-8

5. Method and chemistry consultation. Data review, approval, and interpretation.

6. Method development.

7. Adherence of work to project specific goals.

8. SOP Development and review.

9. Instrument / supply procurement.

10. Training.

11. Work in conjunction with laboratory director to company’s growth and goals


IX. Inorganic Department Manager

Appointed Deputy (Lab Coordinator)

1. Supervision and management of all Inorganic Preparation/Sample receiving// Microbiology, metals/wet

chemistry and miscellaneous testing analysts

2. Sample throughout and scheduling (prioritization)

3. Turnaround / holding time monitoring

4. Method and chemistry consultation

5. Data review, approval, and interpretation


7. Adherence of work to project specific goals

8. SOP Development and review

9. Instrument procurement

10. Training


A. Inorganics Team Leaders

1. Sample analysis in accordance to QC protocols

2. Reporting of sample results onto bench worksheets

3. Analysis and instrument documentation



c. Analysis records


(2) Standard Logs

(3) Reagent Logs



5. Technical data review


7. SOP development

8. Training

B. Metals and Wet Chemistry Methods Analysts


2. Calculation and reporting of sample results onto bench worksheets




c. Analysis records

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PAGE 2-9


(2) Standard Logs

(3) Reagent Logs


d. Temporary data storage

e. Technical data review

f. Method development

g. SOP development

h. Training

4. Data Processing

C. Preparation and/or Misc. Analytical Technicians

1. Sample preparation, digestion, and extraction in accordance to QC protocols

2. Documentation of tasks

a. Preparation Logs

b. Bench worksheets

c. Reagent Logs

d. Maintenance Logs

3. Documentation review

4. SOP development

5. Training

6. Various Wet Chemistry testing

7. Data Processing

D. Microbiology Methods Analysts


2. Reporting of sample results onto bench worksheets




c. Analysis records


(2) Standard Logs

(3) Reagent Logs



5. Technical data review


7. SOP development

8. Training

E. Sample Control Specialists

1. Sample numbering

2. Entering samples into designated holding areas

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PAGE 2-10

3. Distribute copies of COC=s

4. Liaison between sample receiving and client services

F. Sample Custodian

1. Receiving samples (signing and reviewing Chain of Custody)

2. Assigning Submission numbers

3. Distribution of samples with short holding times

4. Distribution of samples with rush status

5. Completion of cooler receipt forms

6. Secondary sample tracking

X. Director of Human Resources/Health and Safety Coordinator/Radiological Safety Officer


1. Provide leadership, by example, establishing and maintaining quality standards. In conjunction with the

Technical Director and Department Managers, hire, counsel, discipline, provide training and monitor

performance of those reporting to the Department Manager

2. Review all performance evaluation forms for all employees

3. Maintain a current list of all personnel with their names, status, titles, hire dates, and educational level.

4. Maintain payroll information on all employees

5. Originate new employee personnel files and maintain all employee personnel files and forms according to

company policy, federal and state regulations

6. Employee timecard and eligibility records

7. Manage an effective operation to insure the attainment of the Company’s goals and objectives to provide

quality service to both internal and external clients.

8. Employee Health Benefits Director.

9. 401K Plan Administrator.

10. Responsible for all aspects of BC Laboratories, Inc. Safety Program including Chemical Hygiene Plan,

Injury and Illness Prevention Program, Fire Prevention Plan, Waste Disposal Practices, Respiratory

Protection Plan, Substance Abuse Testing Program, and Employee Safety Manual.

11. Laboratory Training Coordinator.


XI. Quality Assurance Officer


1. Development and maintenance of QAP.

2. Management of internal audit programs

3. SOP development and maintenance

4. Correspondence with clients concerning audit results

5. Data validation

6. Project Plan Development

7. TQM Training

8. QC Reporting

9. QA Monitoring

10. Final report approval

11. Qualifying subcontractors


13. Qualifying instruments and apparatus

14. System capability

15. Supervision of QA Specialist & Word Processor

16. Compliance with DoD QSM and ISO 17025:2005

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PAGE 2-11

A. QA/QC Specialist

1. QC Reporting.

2. QA Monitoring.

3. Data Processing.

4. Control Chart Maintenance.

5. Final report formatting.

6. Data storage

B. Word Processor

1. Processing correspondence

2. Processing, creating, and distributing Bids / Intro Package

7. Processing, creating, and distributing Logbooks

4. Bacteriological Reporting

5. Overflow reporting

6. Processing controlled documents

XII Customer Services Manager

Appointed Deputy (Project Manager)

1. Supervise day-to-day activities of the Receptionist

2. Liaison between the client and the laboratory staff

3. Project organization and maintenance

4. Supervision of Receptionist, Project Coordinators, Head Field Service Technician, Field Service Technicians,

Courier, Bottle Prep Technician and Log-In Specialist (Sample Receiving)

5. Data / Report review

6. Data Deliverables Packaging

7. Method Consultant

8. Supervision of Field Services Personnel


10. Bottle orders

11. Project checklist completions

12. Field Service Job and task organization, and scheduling.

13. Liaison between the project manager and field service personnel

14. Field service duties.

A. Project Manager

1. Liaison between the client and the laboratory staff.

2. Project organization and maintenance.

3. Data / Report review.

4. Data Deliverables Packaging.

5. Bottle orders.

6. Project checklist completion.

7. Field Service scheduling.

B. Receptionist

1. Answer and direct phone calls.

2. Maintenance of visitor tracking log.

3. Bacteriological reporting.

4. Data tracking.

5. Some invoice tracking.

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PAGE 2-12

6. Clerical Supply Procurement

C. Field Service Technicians

1. Courier duties.

2. Soil and water sampling.

3. Maintenance of instrumentation, safety equipment, sampling equipment and vehicles.

D. Courier

E. Sample Receiving

1. Review of Submission (COC and paperwork).

2. Work with client service for specific project info.

3. Phone Back-up

4. Subcontract COC's and Samples

5. Receive sample from walk-in Clients, Fed-Ex & UPS

F. Data Entry Specialists

1. Generate reports (Bacteriological)

2. Filing COC's - Subcontract COC's.

3. Phone back-up.

G. Bottle / Container Preparation Specialist

1. Preparing preservatives.

2. Washing containers.

3. Preparing bottle orders.

4. Shipping containers.

5. Monitoring TB water.

In cases of key personnel absences, the noted appointed deputy or contingency person will assume the absent key person's

responsibilities limited to workload scheduling and other duties necessary to continue operations.

2.4 In the absent of technical Director (manager) for a period of time exceeding fifteen (15) consecutive calendar days, the

laboratory will designate another full-time staff member meeting the qualifications of the technical director (manager) to

temporarily perform the function.

In the absence of technical director (manager) for a period of time exceeding thirty-five (35) consecutive calendar days, the

primary accreditation body will be notified in writing

2.5 WORK CESSATION

The QA officer is vested with the authority to independently stop work in response to quality problems. If the QA officer is not

available, his/her backup can assume this responsibility.

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PAGE 2-13

FIGURE 1

PERSONNEL SIGNATURES/INITIALS IDENTIFICATION

NAME

TYPED

INITIALS

SIGNATURE

SIGNED

INITIALS

EMPLOYME

NT DATE

Carolyn Jackson

CEJ

05/25/62

Keith Vogel

KEV

10/01/86

Richard Penner

RLP

09/30/91

Marna Atencio

MSA

07/01/72

Stuart Buttram

SGB

06/01/87

Sara Guron

SKG

06/13/00

Tina Green

TG

05/23/93

Steve Bennett

SPB

09/07/90

Jatinder Riar

JKR

05/05/95

Teresa Shaw

TMS

04/20/89

Shelly Maritt

SLM

06/16/99

Robert Cortez

RDC

02/08/12

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PAGE 2-14

Laboratory Organizational ChartCompany Structure

Business Development

Specialist

President / CEO

Production Departments

CustomerService Manager

LIMS Manager Inorganics

Manager

Quality Assurance

Officer

Project Manager

Field Services Technician

Courier

LIMS Programmer

Quality Assurance Specialist

Metals Supervisor

HR Director / Health & Safety Coordinator

Non - Production Departments

Volatiles

Manager

Semi - VolatilesOrganic Manager

Analyst II

Analyst I

Lab Technician II

Lab Technician I

Sample Custodian

Analyst II

Analyst I

Analyst II

Analyst I

Lab Technician II

Lab Technician I

Safety Assistants

MaintenanceLaboratory

Coordinator

Technical Director

ServiceTechnician

&Billing Clerk

Receptionist

Sample Receiving

Bottle Prep

WordProcessor

LIMS Specialist

Board of Directors

Semi Volatiles Extraction Supervisor

WetChem

Supervisor

Marketing & Sales

Coordinator Accounts Payable/Receivalble

Vice-President

Specialist

Organic

Specialist

Rev. 2015

PetroleumManager

And Radiological Safety Officer

And Radiological Safety Officer

Sample Control

Specialist

Data EntrySpecialist

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QUALITY OBJECTIVES

SECTION III

REVISION NO. 10


PAGE 3-1

3.0 QUALITY OBJECTIVES

Quality assurance (QA): objectives are set to provide external parameters that chemist and their instruments must meet to insure the

integrity of data, confidence of regulatory agencies, and its’ clients. Parameters include PE’s, audits and meeting EPA mythology

requirement.

Quality Control (QC): objectives of internal systems are to insure that the laboratory, it’s chemist and their instruments meet the parameters

defined in the QA program on a daily basis. QC parameters include preparation blank, surrogate, spikes, duplicates, laboratory control

samples, travel blanks, temperature checks, preservation confirmation, and accurate record keeping insuring policies are followed:

Specific Parameters:

Accuracy - Defined as the degree to which the analytical measurement reflects the true value present. Surrogate, ICV, CCV, RLS, LCS

and matrix spike recoveries will be used to measure accuracy. See section 13.4 for the algorithm used to measure accuracy.

Precision - Defined as the measure of mutual agreement among individual measurements of the same pollutant in a sample, secured under

the same analytical protocols. Laboratory precision will be expressed as relative percent difference (RPD). The goals for precision are

related to the proximity of the sample to the detection limit. At or less than five (5) times the PQL, the precision goal will be expressed in

absolute concentration (quantitation limit) terms. See section 13.4 for the algorithm used to compute the relative percent difference.

Representativeness - Dependent upon the sampling plan. Assessment of site and collection representativeness is done by subcontracted

or laboratory field service personnel. Procedures to ensure representativeness will be determined prior to the initiation of individual projects.

Comparability - Defined as the extent to which samples can be verified or duplicated by another independent laboratory or compared

against results previously found. Comparability will be assessed through parallel studies, round robin programs and internal and external

audit results. Acceptable levels of comparability will be addressed in specific project plans.

Completeness - Defined as the percentage of valid data obtained, as judged by objectives, compared to the total amount of data collected.

QC parameters that shall be assessed for quantitative determinations of completeness shall include initial calibrations, continuing

calibrations, surrogate percent recovery, RPD's of duplicates, percent recovery and RPD for matrix spike recoveries, percent recovery for

laboratory control samples, and holding times. The requirement for the quantitative assessment of completeness is 90%.

Sensitivity - Established practical quantitation limits (PQL's) and method detection limits based on procedures outlined in Appendix B of

40 CFR Part 136, have been documented for analytes of interest. (See Appendix B) Please note that these detection limits are established

under ideal conditions, i.e., matrices used for detection limit studies are "clean" soils and deionized laboratory water. MDL studies must be

performed annually for each matrix type - water and soil. MDL=s and PQL=s must meet standards set in SW-846, EPA 500 series methods,

EPA 600 series methods and standard methods 18th

edition. Special provisions may be necessary in cases of project specific goals, which

exceed the aforementioned standards. MDL/PQL derivation procedures are addressed in the QA Protocols Manual.

Note: = The following QAPP Sections have been Reviewed on 01/08/2016 (No Changes were made)

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SAMPLING PROCEDURES

SECTION IV REVISION NO. 20


PAGE 4- 1

4.0 SAMPLING PROCEDURES

Proper collection, preservation and storage of samples is needed to ensure sample integrity and representativeness. Samples are

collected by trained, experienced field personnel according to guidelines established by Standard Methods for the Examination of

Water and Wastewater, Test Methods for Evaluating Solid Waste (SW-846), and 40 CFR Part 136. The Field Services Standard

Operating Procedures (SOP) Appendix A, displays the scope of capabilities of our Field Services Department. All protocols for proper

sample collection and handling are addressed in respective Field Service SOP's.

4.1 DOCUMENTATION

Proper documentation, including use of Sampling Logs, Field Logs and Chain-of-Custody forms are maintained throughout

sampling procedures. Field measurements are recorded in ink in bound Field Logs with entries signed by respective field service

personnel. Field sample information is entered directly into the LIMS upon receipt by a representative of the Sample Control

Department. A chain of custody form must be properly completed to track samples in from the field.

4.2 SAMPLE CONTAINERS

All samples collected have proper containers and preservatives with which they are associated. All containers used are typically

made of plastic or glass. All BCL glass containers are ordered pre-certified. Only polyethylene containers are received uncertified

and prepared in-house. All in-house prepared containers are monitored for artifacts on a quarterly basis or whenever new lot #

containers are used.

Table 1 displays information on proper containers, preservatives and holding times.

4.2.1 SAMPLE BOTTLE / CONTAINER PROCESSING

Preservatives are routinely analyzed before usage. Documentation exists to trace the preservative used for each

sample submitted in a laboratory supplied containers.

1. Containers are prepared.

2. Preservatives are made as needed

A. Reagent - grade chemicals are used.

B. Once the preservative is made, it is given a batch ID.

C. The preservative is tested before use by testing an aliquot brought up to volume in a proper sample

container.

D. The preservative test is logged into the LIMS.

E. The preservative is analyzed for constituents of concern.

F. If all constituents of concern are not detected, the preservative can be used. If detections are found, the

process must be reinitiated.

3. A reagent log is kept on file to record chemicals used.

4. Records are filed with all regular sample submissions

4.2.2 TRIP BLANKS

Trip blanks are used to identify the presence of volatile compound contamination attributable to transfer across a

sample container septum during shipping and storage of samples. A trip blank is a sample of Analyte-free matrix

that is transported from the laboratory to the field with sample containers, then stored during sampling and finally

transported back to the laboratory with the samples. The trip blank is then treated as an environmental sample in the

laboratory with the following exceptions:

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SAMPLING PROCEDURES



PAGE 4- 2

1. Analyze trip blanks only when detections are found in associated samples.

2. Analyze according to specific project protocols.

4.2.1.1 Trip blank Preparation

Trip blank matrix is prepared in the laboratory by purifying deionized water. k Deionization of laboratory water can

be broken into two major steps, macro and micro polishing. Tap water is passed through large resin beds then

polished by being passed through a second set of micro resin beds and a carbon cartridge. After purification, the

water is collected into a large glass bottle, which is fitted with a carbon filter. A sample, labeled with the batch

number and date, is then taken in a 40 ml VOA and analyzed for volatiles by GC/MS. If any Analyte concentrations

are found above 1 g/L, the process is re-initiated.

4.2.1.2 Monitoring

Every week the stored trip blank water must be analyzed to assure integrity. A sample is taken and labeled with the

date and the batch number followed with a letter from the alphabet, which corresponds to the number of samplings

after the initial sampling.

Example: Batch 215 initialized and sampled on 05/23/97.

The following weeks= sample is labeled - Batch 215A 05/30/97.

If any target analytes are quantified above 2.0 g/L, a new trip blank batch should be processed.

4.2.3 EQUIPMENT BLANK

A sample of deionized water, which is poured over or through field sampling equipment. This water is processed as

an environmental sample in the laboratory for the use of verifying whether or not the decontamination of field

equipment was adequate.

4.3 HOLDING TIMES

Samples should be analyzed as soon as possible after collection. The times listed in Table 1 are the maximum time limits that

the samples may be held before requested analyses are initiated. Analyses conducted beyond proper sample holding times are

to be considered minimum values. Samples may be held for longer periods if the permittee, or monitoring laboratory has data

on file to show that the specific types of samples under study are stable for a longer time, and has received a variance from the

person in authority. A permittee, or monitoring laboratory is obligated to hold samples for shorter times if knowledge exists

showing necessity of maintenance of sample stability. Our goal is to meet every holding time.

4.4 SAMPLE / CONTAINER ORDERING

Completing a bottle order is the responsibility of Client Service personnel. An order is completed by entering all pertinent

information from the client into the LIMS. The bottle order form is generated and submitted to the bottle preparation

technician. The bottle preparation technician completes the tasks listed on the bottle preparation form and acknowledges

completion with the ordering party. Sample containers are now available for client pick up, shipping or courier submittal. A

copy of the bottle order form is included for each respective bottle order and should be submitted back to the laboratory after

field activities. An example of a Bottle Order Form is given in Figure 3. The bottle ordering process flow chart is located in

Appendix E.

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SAMPLING PROCEDURES



PAGE 4- 3

Sampling

Location

Location

ID

Number

Matrix

Depth

(units)

Analytical

Parameter

# Samples

(include

field

duplicates)

Sampling

SOP #

Sample

Volume

Container

s #, size,

type

Preservation

(chemical,

temperature,

light

protected)

Maximum

Holding

Time:

Preparation/

analysis

Water

Quality

Inorganic Water Surface Nitrate as N

One per site BCGEN048 8 oz Plastic None 48 hours

Water

Quality

Inorganic Water Surface Ortho-

Phosphate as P

One per site BCGEN051 8 oz Plastic None 48 hours

Water

Quality

Inorganic Water Surface Turbidity One per site BCGEN014 8 oz. Plastic

bottle

None 48 hours at 4

°C, dark

Water

Quality

Inorganic Water Surface Ammonia as N One per site BCGEN061 8 oz Plastic H2SO4 28 days

Water

Quality

Inorganic Water Surface Metals (200.8) One per site BCMET037 Quarts Plastic None 28 days

Water

Quality

Inorganic Water Surface TDS One per site BCGEN013 Quarts Plastic None 7 days

Water

Quality

Inorganic Water Surface TSS One per site BCGEN022 Quarts Plastic None 7 days

Water

Quality

Inorganic Water Surface Residual

Chloride

One per site BCGEN010 8 oz Plastic None Immediately

Water

Quality

Semi-

Volatile

Water Surface 1664 Oil &

Grease

One per site BCORG026 1 L Amber HCl 28 days

Water

quality

Inorganic Water Surface Nitrates as N One per site BCGEN048 8 oz Plastic None 48 hours at 4

°C, dark

Water

quality

Inorganic Water Surface Ortho-

phosphate as P

One per site BCGEN051 8 oz Plastic None 48 hours at 4

°C, dark

Water

quality

Inorganic Water Surface Total nitrogen One per site BCGEN055 8 oz Jar None 48 hours at 4

°C, dark

Water

quality

Inorganic Water Surface Organic

nitrogen

One per site Calculation 8 oz Jar None 48 hours at 4

°C, dark

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SAMPLING PROCEDURES



PAGE 4- 4

Sampling

Location

Location

ID

Number

Matrix

Depth

(units)

Analytical

Parameter

# Samples

(include

field

duplicates)

Sampling

SOP #

Sample

Volume

Container

s #, size,

type

Preservation

(chemical,

temperature,

light

protected)

Maximum

Holding

Time:

Preparation/

analysis

Water

quality

Inorganic Water Surface Ammonia as N One per site BCGEN061 8 oz Plastic H2SO4 28 days

Water

quality

Inorganic Water Surface Nitrite as NO2 One per site BCGEN055 8 oz Jar None 48 hours at 4

°C, dark

Water

quality

Inorganic Water Surface Total Kjeldahl

nitrogen

One per site BCGEN059 8 oz Plastic H2SO4 28 days

Water

quality

Inorganic Water Surface Total

phosphorous

One per site BCGEN060 8 oz Plastic H2SO4 28 days

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SAMPLING PROCEDURES



PAGE 4- 5

Bottle Order Form

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SAMPLE PROCEDURES

SECTION IV

REVISION NO. 20


PAGE 4-6

Table 1 MAXIMUM HOLDING TIME AND CONTAINER CHART

GENERAL / INORGANIC CHEMISTRY

ANALYSIS WATER (< 6°C) SOIL

(< 6°C)

Max HT1 in Days

(unless noted) Min Sample Quantity2

Container Type Preservative Container Water Soil Water (ml) Soil (gm)

Alkalinity Pint P -- 8 oz. jar 14 -- 100 10

Ammonia (NH3) Pint P H2SO4; pH<2 8 oz. jar 28 28 100 5

BOD Quart (H) P -- 8 oz. jar 48 Hrs. 48 Hrs. 1000 150

Bromide Pint P -- 8 oz. jar 28 28 50 30

Chloride Pint P -- 8 oz. jar 28 28 50 30

Chlorine (Residual) Pint (H) P -- -- 15 Min. -- 500 --

COD Pint P H2SO4 pH<2 8 oz. jar 28 28 50 25

Color Pint AG/P -- -- 48 Hrs. -- 100 --

Cyanide (Total) Pint P NaOH; pH>12 8 oz. jar 14 14 200 20

Cyanide (Reactive) Pint P -- 8 oz. jar ASAP ASAP 50 50

Dissolved Oxygen Quart (H) P -- -- 15 Min. -- 500 --

Dissolved Organic Carbon 4 oz. AG -- -- 28 -- 100 --

Electrical Conductivity (EC) Pint P -- 8 oz. jar 28 28 200 --

Flashpoint Pint AG -- 8 oz. jar -- -- 500 100

Fluoride Pint P -- 8 oz. jar 28 28 50 30

Gross Alpha Quart P HNO3 <2 or Upres 8 oz. jar 6 Mo. 6 Mo. 1000 250

Gross Beta Quart P HNO3 <2 or Upres 8 oz. jar 6 Mo. 6 Mo. 1000 250

Hardness Pint P -- -- 28 -- 200 --

Hexavalent Chromium (Cr+6) 2 oz. P Borate/HCO3/CO3 -- 5 30 Days till Ext. 50 --

Pint P -- 8 oz. jar 24 Hrs. 7 Days to run 50 20

Iodide Pint P -- 8 oz. jar ASAP 28 Days 50 30

Nitrate/Nitrite (NO3/NO2) 2oz p H2SO4; pH <2 8 oz. jar 28 28 Days After Ext. 50 30

Nitrite (NO2) Pint P -- 8 oz. jar 48 Hrs. 48 Hrs. After Ext. 50 30

Nitrate as NO3 Pint P -- 8 oz. jar 48 Hrs. 48 Hrs. After Ext. 50 30

Odor Pint AG -- -- -- -- 500 --

ORP Pint (H) P -- -- ASAP -- 100 --

Perchlorate Pint P -- 8 oz. jar 28 28 50 30

pH Pint P -- 8 oz. jar 15 Min. -- 100 50

Phenols 4 oz. A H2SO4; pH <2 8 oz. jar 28 28 200 10

Total Phosphorous Pint P H2SO4; pH <2 8 oz. jar 28 28 100 10

Ortho- Phosphorous Pint P -- 8 oz. jar 48 Hrs. 48 Hrs. After Ext. 50 30

TDS Quart P -- -- 7 -- 500 --

TSS Quart P -- -- 7 -- 1000 --

Settleable Solids Quart P -- -- 48 Hrs. -- 1000 --

Total Solids Quart P -- 8 oz. jar 7 7 500 50

Specific Gravity Pint P -- 8 oz. jar 28 28 500 10

Sulfate Pint P -- 8 oz. jar 28 28 50 30

Sulfide (Total) Pint P Zn Acetate 8 oz. jar 7 -- 200 --

Sulfide (Reactive) Pint P -- 8 oz. jar ASAP ASAP 50 50

Surfactants (MBAS) Quart P -- -- 48 Hrs. -- 500 --

Coliforms 8 oz. GN Na2S2O3 -- 6, 30 Hr. -- 125 --

Total Kjeldahl Nitrogen (TKN) Pint P H2SO4; pH <2 8 oz. jar 28 28 100 10

Total Organic Carbon (TOC) 4 oz. A H2SO4; pH <2 8 oz. jar 28 28 100 25

Total Organic Halide (TOX) Pint A H2SO4; pH <2 8 oz. jar 7 Not specified 500 50

Turbidity Pint AG, P -- -- 48 Hrs. -- 50 --

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SAMPLE PROCEDURES

SECTION IV

REVISION NO. 20


PAGE 4-7

TABLE 1 (CONTINUED) MAXIMUM HOLDING TIME AND CONTAINER CHART

METALS

ANALYSIS Container Type Preservative Max HT (1) Min. Sample Vol.

(mls)(2)

WATER

Total Metals Pint P HNO3 6 Months ( 28 Days -Hg/Si) 100

Dissolved Filtered in Field Pint P HNO3 6 Months ( 28 Days -Hg/Si) 100

Dissolved not filtered Quart P 6 Months ( 28 Days -Hg/Si) 250

Organic Lead Quart AG Chill to <°6 C 14 Days 1000

200.8 Copper and Lead5 Quart P HNO3 in lab pH<2 6 Months 1000

ANALYSIS Container Type Preservative Max HT1 Min Quantity (gms)2

SOIL

Total Metals 8 oz. Jar G Chill to <°6 C 6 Months ( 28 Days -Hg) 50

WET/STLC As needed G Chill to <°6 C 6 Months ( 28 Days -Hg) 50

TCLP As needed G Chill to <°6 C 6 Months ( 28 Days -Hg) 150

SPLP As needed G Chill to <°6 C 6 Months ( 28 Days -Hg) 150

Hexavalent Chromium 8 oz. Jar G Chill to <°6 C 30 Days / 7 Days from Ext. 50

Organic Lead 8 oz. Jar G Chill to <°6 C 14 Days 50

ORGANIC CHEMISTRY

ANALYSIS

WATER (< 6°C)

SOIL (<

6°C)

Max HT(1) in Days

(unless noted)

Water Soil

Min Sample

Quantity(2)

Container Type Preservative Container Extract Analysis Extract Analysis Water Soil (gms)

504 2x VOA G Na2S2O3 (3) 8 oz. Jar 14 1 14 14 1 VOA 10

508 Liter AG Na2S2O3 (3) 8 oz. Jar 7 14

1 L 50

524.2/ TCP/THMS 2x VOA (H) G Ascorbic/HCl in field -- -- 14 -- -- 1 VOA --

525.2/507 Liter AG Na2SO3/HCl in field -- 14(4) 30 -- -- 1 L --

548 2 x 250ml AG Na2S2O3 (3) -- 7 21 -- -- 200 mls --

549 Liter AP Na2S2O3 (3) -- 7 21 -- -- 200 mls --

552.3 125 ml AG NH4Cl -- 14 28 -- -- 1 VOA --

556 2 x VOA A NH4Cl/CuSO4 -- 7 40 -- -- 1 VOA --

632 Liter AG (3) 8 oz. Jar 7 40 14 40 1 L 50

8015B Gasoline Range 2x VOA (H) G HCl(3) 8 oz. Jar 14 14 -- 14 1 VOA 10

8015B Diesel Range Liter AG -- 8 oz. Jar 14 40 14 40 1 L 50

8015 Ethanol/Methanol

2x VOA (H) G -- 8 oz. Jar -- 14 -- 14 1 VOA 10

8021 BTEX/MTBE 2x VOA (H) G HCl(3) 8 oz. Jar -- 14 -- 14 1 VOA 10

8081/8082/608 Liter AG Na2S2O3 (3) 8 oz. Jar 7 40 14 40 1 L 50

8141 Liter AG (3) 8 oz. Jar 7 40 14 40 1 L 50

8151/615/515.1 Liter AG Na2S2O3 (3) 8 oz. Jar 7 40 14 40 1 L 50

8260/8240/624 2x VOA (H) G Ascorbic (6)/HCl in field 8 oz. Jar -- 14 -- 14 1 VOA 10

8270/625 2 x Liter AG (3) 8 oz. Jar 7 40 14 40 1 L 50

8310/610 Liter AG -- 8 oz. Jar 7 40 14 40 1 L 50

8330 Liter AG -- 8 oz. Jar 7 40 14 40 1 L 50

1664 Oil and Grease Liter AG HCl 8 oz. jar 28 -- 28 -- 1 L 50

1664 TPH Liter AG HCl 8 oz. jar 28 -- 28 -- 1 L 50

TCLP Volatiles 8 oz. G -- 8 oz. Jar 14 7 14 7 1 L 50

TCLP Semi Volatiles Liter (Each test) AG -- 8 oz. Jar 7 40 14 Days until TCLP Leaching

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SAMPLE PROCEDURES

SECTION IV

REVISION NO. 20


PAGE 4-8

A= Amber

AG= Amber Glass with Teflon lined Cap

AP= Amber Plastic

G= Glass

GN= Sterilized Glass or Nalgene

H= Headspace Free

HT= Holding Time

P= Plastic

VOA= 40 ml Glass Vials with Teflon lined Cap


AIR / VAPOR ANALYSIS

Container

Keep from Light Max HT1 Min Mass (L)

ASTM D-1946 Fixed Gases Tedlar Bag 3 1

Summa Canister 30 5

25C Landfill Gases TGNMO Tedlar Bag 3 1

Summa Canister 30 5

TO-3 TPH Gas Tedlar Bag0. 3 1

Summa Canister 30 5

TO-14A/TO-15 VOCs Tedlar Bag 3 1

Summa Canister 30 5

NOTES:

(1) = Calculated from time the sample is collected.

(2) = Amount needed to achieve normal method detection limits or regulatory requirements.

(3) = Samples containing residual chlorine must be dechlorinated at the time of sampling.

(4)= 7 Days if Diazonin is requested.

(5)= First Draw sample after 6 - 12 Hour idle period.

(6)= Ascorbic only if from chlorinated source

Fill all containers as much as possible.

TCLP and STLC extractions cannot be conducted on acid-treated containers.

Keep all Air/Vapor samples out of light.

8 oz. Jars all have Teflon lined Caps

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SAMPLE CUSTODY

SECTION V REVISION NO. 18

EFFECTIVE DATE: 01/08/16 PAGE 5- 1

5.0 SAMPLE CUSTODY

All samples must remain under custody from the time of sample collection to the time of sample disposal. A sample is considered

under custody if:

1) It is in one's or a team=s possession verified by some form of documentation, or

2) It was in one's possession and he/she locked it or placed it in a sealed container to prevent tampering, or

3) It is within the laboratory grounds.

5.1 CHAIN-OF-CUSTODY PROCEDURES

5.1.1 Samples will be collected, transported, and received under Chain-Of-Custody (COC) protocols consistent with

procedures established by the EPA for litigation-related practices. The Chain-of-Custody record will validate the

transfer of samples among client personnel, BCL Field Personnel, and/or BCL Sample Control Personnel.

5.1.2 Upon receipt at the laboratory, the Sample Custodian is the primary person who will assume sample custody. If the

Sample Custodian is not available, any person from the Sample Control Department will be able to handle initial or

secondary custody procedures.

5.1.3 The COC record is the documentation supporting the integrity of a sample from data collection to data reporting. COC

procedures must be followed for all samples from which analytical results may be obtained and introduced as evidence

in litigation.

5.2 COOLER RECEIPT FORM

5.2.1 Cooler Receipt Forms will be used to document the condition and availability of samples on arrival at the laboratory.

The temperature of the air inside sample coolers and/or the temperature of samples is recorded on the Cooler Receipt

Form. Sample shipping, type numbers, condition, and containment is also recorded on this form.

5.3 SAMPLE LABELS AND CUSTODY SEALS

5.3.1 If sample containers originated from the laboratory, the sample labels will include fields for the following information:

5.3.1.1 Laboratory Name (defaulted)

5.3.1.2 Sample ID

5.3.1.3 Sampler ID

5.3.1.4 Date and Time of sampling

5.3.1.5 Method (defaulted)

5.3.1.6 Preservative if applicable (defaulted)

5.3.1.7 Preservative batch number if applicable (entered by lab personnel prior to shipping to client)

5.3.2 Some sample labels are color coded to indicate preservative types:

5.3.2.1 Yellow - Sulfuric acid

5.3.2.2 Red - Nitric acid

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SAMPLE CUSTODY

SECTION V REVISION NO. 18 EFFECTIVE DATE: 01/08/16 PAGE 5- 2

5.3.2.3 Green - Sodium Hydroxide

5.3.2.4 Blue - HCl

5.3.2.5 Brown - Zinc Acetate

5.3.6 Custom Labels

Custom labels are provided for according to specific project plans or under an additional service agreement.

5.3.4 Custody Seals

Custody seals will be used to assure tampering of samples has not taken place before submission to the laboratory.

Information on the custody seal includes the date when the container/cooler was sealed and the signature of the sampler

or relinquisher. Custody seals should be placed at the proper point of opening on coolers or containers such that the

sample contained within the cooler or receptacle cannot be tampered with without tearing the custody seal. The seals

have adhesive backing and should be partially covered with packaging tape to prevent accidental tearing during normal

container handling. Broken custody seals will be noted in the comments section of the COC record and the Cooler

Receipt Form.

5.4 CUSTODY RECORD

5.4.1 All sample shipments must be accompanied by a COC record (see Figure 4 an example of a COC form with information

on how to complete entries). Information on the COC record includes:

5.4.1.1 Package contents

5.4.1.2 Sample identification numbers

5.4.1.3 Sampling Location

5.4.1.4 Date and time of sample collection

5.4.1.5 Requested analyses

5.4.1.6 Project or task information

5.4.1.7 Billing Information

5.4.1.8 Sample tracking

5.4.1.9 Sample Type

5.4.2 The COC record should be completed by the client unless project specific protocols dictate otherwise. Information on

the COC should be consistent with wording written on the sample labels and seals.

5.4.3 The original COC is submitted back to the client as part of the data deliverables package.

5.5 CUSTODY TRANSFER

5.5.1 When transferring custody, the relinquisher must record the time and date of transfer, then acknowledge by placing

his/her signature in the "relinquished by" field. The receiver must then assume custody by signing the "received by"

field, then record the date and time of sample receipt.

5.5.2 The original COC record will accompany the shipment, and a copy will be retained by the client (if the client or a client

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SAMPLE CUSTODY

SECTION V REVISION NO. 18 EFFECTIVE DATE: 01/08/16 PAGE 5- 3

representative is available). The signed original COC record must be obtained by the Sample Custodian after the

samples have been received and their condition checked.

5.6 INTERNAL CUSTODY

5.6.1 The sample receiving custodian will accept custody of the shipped samples and verify that the information on sample

labels match the descriptions as noted on the COC. Pertinent information concerning sample condition, shipment,

pickup, and couriers will also be checked. The Cooler Receipt Form (See Figure 5) will be completed by the Sample

Receiving Custodian, prior to transferring samples and paperwork to Sample Log-In Custodian. If problems are

encountered at this stage, the Sample Receiving Specialists will 1) inform the concerned Project Manager or client

service representative, 2) hold logging proceedings, and 3) wait for guidance.

5.6.2 Possible Problems

5.6.2.1 COC descriptions do not match sample labels.

5.6.2.2 Samples were received at temperatures outside the 0 - 6C interval.

5.6.2.3 Sample condition problems

5.6.2.3.1 VOA vials have not been properly filled.

5.6.2.3.2 Sample container is inappropriate.

5.6.2.3.3 Sample container received broken.

5.6.2.3.4 Inappropriate preservatives used.

5.6.2.3.5 Insufficient sample volume or mass submitted.

5.6.2.4 Samples were received past holding times.

5.6.2.5 Number of samples does not match the COC.

5.6.2.6 Sample descriptions are not legible

5.6.3 If problems are not encountered, the samples are logged into a ledger and given a unique laboratory number. The

custodian will then transfer the sample(s) to the appropriate secured refrigerators. Samples are logged into refrigerators

by bar-coding system. Information on the bar code scanner include sample ID's, date and time of logging, relinquisher

initials, sample removal date and time, and receiver initials. All environmental samples are maintained in refrigerators

during the entire analytical process, unless project specific goals warrant otherwise.

5.6.4 In cases where sample splitting, compositing, and/or other processing is necessary, the sample splitter will assume

custody by scanning the appropriate refrigerator number. When sample splitting/processing is complete, the sample

splitter will check the original samples back into the proper refrigerator(s) and place split portions into designated split

sample refrigerators.

5.6.5 Laboratory personnel are responsible for the care and custody of samples from the time of submittal till the time of

transfer of custody for final disposal. Laboratory sample disposal is tracked with the use of the Sample Tracking

Scanner. Samples are kept for at least thirty (30) days after analyses have been completed. If samples are required to be

retained for longer periods of time, they are stored in refrigerators until all holding time restrictions have been exceeded

(six months, then they are transferred to on site sea trains). Approval of sample disposal must be granted by the client

before disposal of archived samples can be initiated.

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SAMPLE CUSTODY



PAGE 5-4

5.7 DIGEST/EXTRACT CUSTODY

Transfer of custody of sample digests and extracts from the preparation team and the analyst team is documented on respective

preparation logs. A member of the preparation team and a member of the analyst team must record their initials to authorize the

transfer of custody. The date of the transfer is also recorded. If custody transfer of prepared samples cannot immediately take

place, the preparation technician must place the digests or extracts in a designated holding area. The preparation technician

should then initial and date the preparation log to acknowledge the relinquishing of prepared samples to the holding area. The

analyst can then assume custody at their convenience by initialing and dating the preparation log. Once analysis is complete, it is

the responsibility of the analyst, except for hazardous waste metals testing, to ensure that prepared sample extracts and digests are

given to the disposal persons for proper waste streaming. See the QA Protocols Manual for additional details.

5.8 WASTE DISPOSAL

Waste disposal procedures were based on the requirements set in the state Hazardous Waste Control Law in the Health and

Safety Code 25100 through 25250 and Title 22 regulations. Most tests utilized generate some type of hazardous waste which

must be collected and properly disposed. Other possible forms of waste in the laboratory are samples, reagents, standards, other

substances used in various capacities. Waste, designated into waste streams, must be collected in suitable properly labeled

containers. These containers are then submitted to the maintenance department for discharge into drums. Drums, secured with

secondary containment, are housed in the waste facility until either the storage time restriction is due or the storage drum is full.

Consult the Waste Disposal SOP for details

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SAMPLE CUSTODY



PAGE 5-5

FIGURE 4

Laboratories, Inc.

Sample

#

Description Date

SampledTime

Sampled

Analysis Requested

Attn:

Street Address:

City, State, Zip:

Phone: Fax:

Email Address:

Project

Description:

Project Code:

Sampler(s):

Tur

naro

und

# of

wor

k da

ys*

Soil

Was

tew

ater

Gro

undw

ater

Dri

nkin

g W

ater

Slud

ge

Sample Matrix

NotesOther

Client:

Report To:

Chain of Custody Form

BC Laboratories, Inc. - 4100 Atlas Ct. - Bakersfield, CA 93308 - 661.327.4911 - Fax: 661.327.1918 - www.bclabs.com

Page ___ of ___

1. Relinquished By

2. Relinquished By

3. Relinquished By 3. Received By

1. Received By

2. Received By

Date

Date Date

Date

Date Date

Time

Time

Time

Time

Time

Time

Cost Center:______________________________________

Submission #:

Are there any tests with holding times

less than or equal to 48 hours?

BC

Client:

Address:

City: State Zip

Billing

*Standard Turnaround = 10 work days

Attn:

San Joaquin

Yes No

EDD Format Options

MBU Site

CVX RCRA

Geotracker 5 File

(CA Default)

Geotracker 2 File

Other (Specify)

Comments:

EMC

Global ID:___________________________________________

Check the appropriate sample

Use this field to

convey any special

information such as

sample hazards and/or

non-standard

turnarounds

Must be completed by

the submitting party

Please complete to

assure proper invoicing

Enter sample description. Please

verify that sample descriptions and

dates match the like information

on respective sample containers

The report will be sent

to this address under

this person's attention

Enter project

information

Enter sample dates

and times

Check for standard

turnaround

Please refer to page 2 for

Analysis Legend.

Use the legend on

Page 2 to reference

analytical methods

Check the appropriate

EDD Format.

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SAMPLE CUSTODY

FIGURE 5



PAGE 5-6

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QUALITY ASSURANCE PROGRAM PLAN FACILITIES

SECTION VI

REVISION NO. 20


PAGE 6-1

6.0 FACILITY

The facility was specially designed to alleviate those undesirable factors, which would affect quality in a

detrimental way. Emphasis was placed on 1) minimizing cross contamination potentials, 2) providing extensive

bench space and considerable refrigerated sample storage areas to ensure effective sample handling processes, 3)

maximizing sample and data flow processes, and 4) ensuring a safe working environment.

Laboratory features:

1) (2) Walk-In and (4) large wall reach-in refrigerators

2) (6) Fire proof data storage rooms

3) Chemical storage rooms

4) Two-story storage area

5) Hazardous Waste drum storage facility

6) 8/9 eye - safety showers

7) (3) hood rooms (24 hoods)

8) Conference room with reference library

9) Bottle preparation room

10) Automated sample submission doors

11) Sample split room

12) (3) Compressed Gas storage rooms

13) Kern Securities fire and security systems

14) On site maintenance department

15) Separate volatiles rooms: GC, GC/MS

16) (1) Warehouse Data Storage with 2 Accounting Offices

The laboratory was built on a large lot which is company owned to accommodate expansion. Figure 6

displays the laboratory floor plan.

6.1 ORGANICS LABORATORY

6.1.1 Separate semi-volatiles and volatiles laboratories.

6.1.2 Semi- Volatiles

6.1.2.1 Separate HPLC, and GC/MS Laboratories

6.1.2.2 Gases piped in from gas storage room.

6.1.2.3 1,600 sq. ft. of working area.

6.1.3 Volatiles

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REVISION NO. 20


PAGE 6-2

6.1.3.1 Located in the NW corner of the facility (Extractions located in the SE corner).

6.1.3.2 Two separate laboratories, GC-GC/MS.

6.1.3.3 Maintained under positive pressure.

6.1.3.4 Special carbon filters are integrated into the ventilation systems.

6.1.3.5 2,500 sq. ft. of working space.

6.1.3.6 One (1) Laboratory hood

6.1.4 Extractions

6.1.4.1 Laboratory equipped with 10 ventilated hoods.

6.1.4.2 400 cubic ft. refrigerator.

6.1.4.3 750 sq. ft. of working space.

6.2 WET CHEMISTRY LABORATORY

6.2.1 3,200 sq. ft. of laboratory space.

6.2.2 560 cubic ft. of refrigerator space.

6.2.3 Preparation area segregated from analytical laboratory.

6.2.4 Six (6) laboratory hoods.

6.3 METALS LABORATORY

6.3.1 Separate preparation areas (soil / water).

6.3.2 Two analytical laboratories (ICP,ICP-MS / GFAA-AA, CV)

6.3.3 Gases piped in from gas storage room.

6.3.4 2,200 sq. ft. of working space.

6.3.5 500 cubic ft. refrigerator.

6.3.6 Seven (7) laboratory hoods.

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SECTION VI

REVISION NO. 20


PAGE 6-3

6.4 LOG-IN DEPARTMENT

6.4.1 1,000 sq. ft. of working space.

6.4.2 100 cubic ft. of refrigerator space.

6.4.3 One (1) laboratory hood.

6.5 RECORD KEEPING

6.5.1 Nine (9) Sea - Trains for data and equipment storage and warehouse for Data Storage

6.5.2 Fireproofed data storage room for temporary storage of data

6.6 WASTE DISPOSAL AREA

6.6.1 Built from the ground up to be a waste disposal storage unit.

6.6.2 Secondary containment for individual waste containers.

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SECTION VI

REVISION NO. 20


PAGE 6-4

4100 Atlas CourtBakersfield, CA 93308

BCL FLOOR PLAN

1

2 3

45

6 7 8

91011

12 13 14

15

1620 23 26

17

19

21

18

29

30 32

33

31A

22

24

25

27

28

A A

A

A35 36

38

34

37N

S

EW

39 4041

Seatrains (ST)

MR

WR

OSR

MR WR

W

42

43

Field Service LIMS

13456 279 BC LABORATORIES INC.

WF

WF

W

Field Service

47a

(A/R) Office

44(A/P) Office

45 46A/P & A/R Storage

Warehouse Storage

47

4116 Atlas Ct.

Bakersfield CA 93308

H EA

OS

TEL

GW

Crash

PCB

Area

AWPhenolic HgNaOH

WW

OIS

SA

AW

AW

HCS

CS

CS

WW

8

0

KEY

Administrative Office

ST #1 QC Raw DataST #2 Client Service Raw DataST #3 Field ServiceST #4 Gen-Chem (Sample Storage)ST #5 LimsST #6 Gen-Chem Sample StorageST #7 Gen-Chem Sample StorageST #8 Acct Receivables/PayablesST #9 CLP Raw Data

Air TestingGC/MS Volatiles/GCSample SplittingGC/MS VolatilesCompressed Air DryerMaintenance OfficeGas StorageGas StorageGas StorageICP LabGC/MS VolatilesMetals Digestion (Solid)Walking/RefrigeratorElectrical Room Atomic Absorption LabBottle Prep

BacteriologyWet Chemistry DepartmentGC/MS Volatile Lab Inorganic Dept.Inorganic Dept.

Metals Digestion (Water/Solid)

GC/MS Semi-Volatiles LabTPH LabPesticides/PCB’s LabGC LabHPLC LabOrganic ExtractionQA/QC/Word Processing Dept.Sample Receiving DeptClient Services/Log-In Dept.ReceptionLobbyComputer RoomBreak RoomConference RoomHR/Safety DirectorPresident’s OfficeAcct Office (A/R)

Misc Receiving AreaSample Storage

ST Seatrains

123456789

101112

151413

1617181920212223242526272829303132333435363738394041

43

Acct Office (A/P)Field Service Trailer

42

AHazardous Waste StorageHWalk-in RefrigeratorMen RestroomsWomen RestroomsWater FountainOffice Supply Storage Room

WFOSR

WMRWR

Acct Office (A/P)44A/P_A/R Storage Room45

Warehouse Storage47QC Storage Room47a

Acct Office (A/R)46

Storage

File Name: S:\WPDoc\Word Docs\LABDOCS\Vision\BCL Floor Map

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PERSONNEL / TRAINING

SECTION VII

REVISION NO. 16


PAGE 7-1

7.0 PERSONNEL

BC Laboratories, Inc. is staffed by qualified, experienced and well-educated personnel. Brief résumés on key

personnel are located in our Statement of Qualifications manual. Job descriptions are in process to be finalized

for all laboratory positions. Each position requires specific qualifications to be met. The training program is

structured to ensure that curricula addresses specific needs of employees and the organization.

7.1 QUALIFICATIONS

Technical positions require minimum educational standards and experience to be met. Each analyst

must perform an initial demonstration of competency (IDC) before analyses solely generated by the

concerned analyst can be reported to clients. These IDCs will follow guidance as listed in SW-846,

Method for the Determination of Metals in Environmental Samples, Methods for the Determination of

Organic Compounds in Drinking Water, and Standard Methods, 19th

edition.

Training is conducted by persons with a solid background in respective subject matter. Module training

is presented by individuals who are technically competent and qualified in instructional techniques.

7.2 INTERNAL TRAINING PROGRAM

Basic skills and training knowledge are conducted through in-house programs and/or subcontract

programs. The in-house program includes an initial orientation, on the job training and a training

module program, which covers various aspects of laboratory operations.

In House Training Modules (offered as needed and/or biennial). See the QAPM. (Ethics training is

annual)

MODULE

TOPICS

JOB TITLES

(attendance is

required)

TRAINER

A-1

Initial Orientation

LIMS

Ethics

Sexual Harassment

Orientation

For New Hires

Steven Bennett

Basic Laboratory Operations

Introduction to Quality Control

Introduction to Laboratory Analyses

Glassware

Types

Volumetric Measurements

Using Burettes and Pipettes

Calibration

Safety, Cleaning, and Storage


Analysis Terms

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SECTION VII

REVISION NO. 16


PAGE 7-2

MODULE

TOPICS

JOB TITLES

(attendance is

required)

TRAINER

Procedures and Methods Instrument

ation

Data Generation

Linear Measurement

Temperature Measurements

B Laboratory Math I

Weighing and Measuring

Units of Measurement

Mass Measurements

Significant Figures and Rounding

Percents

Exponential Numbers

Analyst/Prep Technician

Richard Penner

C-1

Quality Assurance, Quality Control

Concepts

Parameters

Basic Tasks

Measurement and Assessment

Documentation and Audits

Corrective Logic

All

Sara Guron

C-2

Data Management

Recordkeeping Procedures

Responsibilities

Storage

All

Sara Guron

C-3

System Improvement-Corrective Action

Continuous Improvement

When to Initiate Corrective Procedures

Procedures

Identifying the Error

Implementing Corrective Action

Demonstrating Corrective Action

Closure

Documentation

All

Sara Guron

D

Ethics

Industry Standards

Case Studies

Code of Ethics Policy

All

Sara Guron

E

Sexual Harassment

All

Steven Bennett

F LIMS I

Logging on through Passwords

Security

Features

Policy

All

Keith Vogel

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SECTION VII

REVISION NO. 16


PAGE 7-3

Training module attendance is job dependent. Each job description has associated minimum training

requirements; Trainees may need to pass training examinations before acknowledgment of successful

completion of pertinent training modules, which are determined according to job description.

Module training will be appropriately scheduled to accommodate both working shifts. Effort will be

put forth to provide a flexible and workable schedule to prevent any significant disruption of work

flow.

Individual module presentations should be posted on the memo board and near time clock at least one

week prior to each training session. Employees are required to sign the attendance ledger on the

posted schedules.

JOB TITLES

1. President

2. Technical Director

3. Director of Human Resources

4. Health + Safety Officer/Radiological

Safety Officer

5. Service Technician

6. Client/Field Services Manager

7. Project Manager

8. Client Services Representative

9. Field Services Representative

10. Courier

11. Lab Technician I (Non Production Data)

12. Sample Custodian

13. Billing Clerk

14. Receptionist

15. Accounts Payable Clerk

16. Accounts Receivables Clerk

17. Inorganics Manager

18. Supervisor (Production Inorganics)

19. Lab Technician I (Inorganics)

20. Lab Technician I (Organics)

21. Lab Technician II (Inorganics)

22. Lab Technician II (Organics)

23. Analyst I (Inorganics)

24. Analyst I (Organics)

25. Analyst II (Inorganics)

26. Analyst II (Organics)

27. LIMS Manager

29. LIMS Programmer

30. LIMS Specialist

31. Volatile Organic Manager

32. Quality Assurance Officer

33 Quality Assurance Specialist

34. Sales & Marketing Director

35. Salesperson

36. Laboratory Coordinator

37. Semi-Volatile Organic Supervisor

38. Semi-Volatile Extraction Supervisor

39. Word Processor Specialist

7.3 ON THE JOB TRAINING

After the orientation is completed, the trainee will be directed to his/her respective department

supervisor. The department supervisor will initiate on the job training procedures. (See the

Training Procedures in the QAPM).

7.4 INITIAL DEMONSTRATION OF COMPETENCY

Each analyst must perform an initial demonstration of competency (IDC) before analyses solely

generated by the concerned analyst can be reported to clients. These IDC's will follow

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SECTION VII

REVISION NO. 16


PAGE 7-4

guidance as listed in SW-846, Methods for the Determination of Metals in Environment

Samples, Methods for the Determination of Organic Compounds in Drinking Water, and

Standard Methods, 19th edition. Each analyst must undergo an annual demonstration of

capability. This can be accomplished by passing a yearly audit sample. If a given analyst does

not run an annual audit sample then all analysts can perform 4 ICV=s or LCSW=s to satisfy an

annual demonstration of capability requirement.

7.5 EXTERNAL TRAINING PROGRAM

External training is conducted through manufacturer=s instrument training programs, various

independent seminars, California State University at Bakersfield (CSUB), and Bakersfield

College. External training is addressed under the Educational Assistance section of the

Employee Policy Manual.

Each supervisor is encouraged to attend at least one outside services seminar or training

session, which would enhance his/her job performance or knowledge. In order to attend,

supervisors must be granted an approval by the President.

7.6 SAFETY

Safety training begins with the new employee orientation. Quarterly safety meetings are held

to provide for continuing training regarding safety- related updates and to ensure safe working

conditions by providing reiterated safety practice and policy information. All employees,

unless absence is approved by the Health and Safety Coordinator, are required to attend

quarterly meetings. Meeting schedules can be found posted in the memo board. Additional

information is listed in the Safety Module Training SOP.

7.7 PERFORMANCE EVALUATIONS

To monitor employee progress and efficiency, department supervisors evaluate each specialist

annually. These annual screenings are conducted on a one-on-one basis with supervisors rating

employee performance on various job-related subjects. During these interviews, goals are set

to provide for deficiencies, or to help employees further their training and skills. Evaluation

forms used are exclusive for each laboratory department. (See Appendix C to see an example

of an evaluation form.)

7.8 EMPLOYMENT

BC Laboratories, Inc. offers a comprehensive benefit package for each employee to ensure a

productive and efficient work force. All agreements and particulars are addressed in the BC

Laboratories, Inc. Employee Policy Manual.

Note: This section was reviewed on 1/08/16 (No changes were needed)

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RECORDS / DOCUMENTS

SECTION VIII

REVISION NO. 13


PAGE 8-1

8.0 RECORDS

Documentation is the heart of every viable QA/QC Program. Without adequate documentation

the ability to defend generated data is impossible. The purpose of documentation for viable

QA/QC programs is to provide the ability to defend and recreate steps taken associated with

each sample from sampling to final submittal and disposal. Documentation falls into two

categories: 1) documents providing assurance of data quality objectives, and 2) documents

providing information pertaining to contingent processes to support activities concerning sample

and sample data handling. Necessary documentation includes:

8.1 SAMPLE CONTROL RECORDS

8.1.1 Chain of Custody - A record verifying the custody of samples and requested and

associated analyses. The COC will be generated by the person(s) in the field.

Completion of this record is addressed in the LOG-IN SOP BCSAM002.

8.1.2 Laboratory Sample Tracking

8.1.2.1 The COC records identify all individuals who physically handled individual

sample.

8.1.2.2 COC received by the laboratory, the laboratory personnel are responsible for care

and custody of the sample

8.1.2.3 Cooler Receipt Form - Record of samples submitted and their disposition,

condition, and number.

8.1.2.4 Internal Chain of Custody Ledger - Record of initial sample tracking record.

8.1.2.5 Sample Split Log - Record of sample preparation of solid matrices prior to

analytical manipulations.

8.1.2.6 Water Tracking Log - Used to track internal sample custody in the Metals

Department.

8.1.2.7 Sample Disposal Log - Tracks sample route from temporary storage to disposal.

8.1.2.8 Archive Refrigerator Log - Record of internal sample tracking for archived

samples.

8.1.3 Refrigerator Logs - Logs which track internal sample custody used in the Organics’, Wet

Chemistry, and Metals Departments.

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RECORDS / DOCUMENTS

SECTION VIII

REVISION NO. 13


PAGE 8-2

8.1.4 Sample Control Approval Form - Provides a review of the log-in process on a

submission basis, also used to verify sample condition.

8.1.5 Preservative Reagent Log - Record of preservative preparation.

8.2 SUPPORT DOCUMENTATION RECORDS

8.2.1 Phone Records - Record of phone correspondence between laboratory personnel and

clients.

8.2.2 Sample Tracking Logs - Record of sample tracking via project coordinators.

8.2.3 Archived Files Request Log - Used to document requests for archived files.

8.2.4 Subcontract COC Log - Record of sample tracking of submissions to a subcontractor.

8.2.5 Shipping Logs (Federal Express / UPS / DHL) - Used to track shipping of samples

and/or data supplies.

8.2.6 Requisition Form - Procurement record.

8.2.7 Maintenance Request Form - Record of scheduled maintenance.

8.3 TECHNICAL RECORDS

8.3.1 Records of original observations, data calibration records, staff records (including

training, IDC, and Performance evaluation)

8.3.2 Maintenance and Disposal of Data records.

8.3.3 Log of names, Initials and signatures for all individuals who are responsible for signing

or initialing any laboratory record are maintained by a laboratory.

8.4 CONTROLLED DOCUMENTS

There is a necessity in maintaining certain documents under a controlled status. Documents

under control will assure 1) proper use of procedures 2) use of the latest version of the

document 3) document review before use and 4) persons requiring the document will receive

and use an approved copy.

8.4.1 Controlled Documents

8.4.1.1 The Quality Assurance Program Plan

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RECORDS / DOCUMENTS

SECTION VIII

REVISION NO. 13


PAGE 8-3

8.4.1.2 Quality Assurance Protocols Manual

8.4.1.3 SOPs (refer to Appendix A for a list of SOPs)

8.4.1.4 LIMS SOP

8.4.1.5 Chemical Hygiene Plan (CHP)

8.4.1.6 Illness and Injury Prevention Plan (IIPP)

8.4.1.7 Safety Manual

8.4.1.8 Employee Policy Manual

8.4.1.8 Substance Abuse Policy

8.4.1.10Laboratory Logbooks (maintenance, standards/reagents)

8.4.2 EXTERNAL SOURCES

8.4.2.1 STANDARDS AND (PJLA) POLICIES/PROCEDURES

8.4.2.1.1 PL-1 Policy on Proficiency Testing Requirements-(Revision 1.13 Revised 7/2015)

8.4.2.1.2 PL-2 Measurement Traceability Policy-(Revision 1.8 Revised 6/2013)

8.4.2.1.3 PL-3 Policy on Measurement Uncertainty-(Revision 1.8 Revised 7/2015)

8.4.2.1.4 PL-4 Calibration Scopes of Accreditation-(Revision 1.4 Revised 6/2013)

8.4.2.1.5 SOP-3- Accreditation Symbol Procedure-(Revision 1.6 Revised 11/2015)

8.4.2.1.6 SOP-9- Complaint Procedure-(Revision 1.4 Revised 3/2013)

8.4.2.1.7 SOP-11- Suspension, Withdrawal or Reduction of Accreditation-

(Revision 1.6 Revised 5/2014)

8.4.3 Process - Document control will be handled through the QA/QC Department and the

Word Processor Specialist (WPS). The Word Processor Specialist will handle all test

processing and record keeping. Approvals will be granted by the QA Officer and/or

pertinent department supervisors.

8.4.3.1 Text Entry - When a document has been produced and approved by pertinent

supervisors outside the LIMS or laboratory document parent directory (WP

Version 8.0 or MS Word 2007), it must be entered and maintained in:

8.4.3.1.1 [S:\WPDOCS\WordDocs\LAB_DOCS\QAPP]

8.4.3.1.2 [S:\WPDOCS \WordDocs\LAB_DOCS\SOPS]

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RECORDS / DOCUMENTS

SECTION VIII

REVISION NO. 13


PAGE 8-4

8.4.3.1.3 [S:\WPDOCS \WordDocs\LAB_DOCS\SOPS\LIMSOP]

8.4.3.1.4 [S:\WPDOCS \WordPerfect\LAB_DOCS\LOGBOOKS]

8.4.3.1.5 [S:\WPDOCS \WordDocs\LAB_DOCS\QAPM]

8.4.3.1.6 [S:\WPDOCS \WordDocs\LAB_DOCS\Safety Manuals

8.4.3.1.7 [S:\WPDOCS \WordDocs\LAB_DOCS\Employee Policy Manual]

8.4.3.1.7 [S:\WPDOCS \WordDocs\LAB_DOCS\Illness and Injury Prevention

Plan (IIPP)]

8.4.3.1.8 [S:\WPDOCS \WordDocs\LAB_DOCS\Substance Abuse Testing

Policy (SATP)]

8.4.3.1.9 [S:\WPDOCS \WordDocs\LAB_DOCS\Chemical Hygiene Plan

(CHP)]

The (draft) document will be processed by the WPS and approved by pertinent

personnel.

8.4.3.2 Approvals - Approvals are documented on Approval Log sheets and document

title pages. Document title page approvals are handled by the WPS.

Parameters checked by the WPS are:

8.4.3.2.1 Complete Document

8.4.3.2.2 Correct Document

8.4.3.2.3 Document print quality

Once approved, the document is submitted to the receiving party. An approval log

sheet is initialed and/or signed by the receiving party and information on this

transaction is documented in an Access Database, LIMS record or a suitable word

processing/spreadsheet program. Approvals of SOPs are documented on Approval

Log sheets. All procedures are reviewed and approved by the QA Officer and

pertinent department supervisors.

8.4.3.3 Maintenance of control documents

8.4.3.3.1 SOP=s, Logbooks, QAPM, and the QAPP. Maintenance

information is located in the QA Protocols Manual.

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SECTION VIII

REVISION NO. 13


PAGE 8-5

8.4.3.3.2 Employee Company policy, revisions are handled through the

Director of Human Resources.

8.4.3.3.3 LIMS SOPs are handled by the LIMS Supervisor.

8.4.3.3.4 Administrative Records

8.4.3.3.4.1 Personal qualifications, training records

8.4.3.3.4.2 Records of demonstration of capability

8.4.3.3.4.3 Log of names, Initial and signatures for all

individuals responsible for signing and

initialing laboratory records

8.5 PROTOCOL

Proper procedures for completing forms and records can be found in specific method SOP's.

8.5.1 General Practices

8.5.1.1 Use only indelible ink.

8.5.1.2 Complete each record. Do not leave empty fields. Line through fields not used or “Z”

out non-filled space.

8.5.1.3 Use proper correction techniques; lined through error then date and initial.

8.6 ANALYTICAL / INSTRUMENT RECORDS

8.6.1 Bench Worksheets (Analytical Data Forms) - Used to record analytical results and

support information.

8.6.2 Extraction Log - Record of sample extraction.

8.6.3 Digestion Log - Record of sample digestion.

8.6.4 Filtration Log - Used to document sample filtration.

8.6.5 Analysis Logs (Run Log) - Record of the sample analytical sequence on respective

instrumentation and can include other QC information.

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8.6.6 Maintenance Log - Used to document routine maintenance and subcontract repair of

instrumentation.

8.6.7 Standards Log - Record of standards preparation.

8.6.8 Reagent Log - Record of reagent preparation and use.

8.6.9 Raw data - Printouts, charts, and chromatograms produced by instrumentation also will

include handwritten records for instrumentation without printing capabilities.

8.6.10 ELEMENT Print out- Records of instrument processing and laboratory corrective

activities.

8.6.11 QC Sheets - Used to document QC and batching capability.

8.7 RAW DATA RECORDS

All raw data records are maintained by the QA/QC Department. The QA/QC Department

obtains records in the following manner:

8.7.1 Organics Department

8.7.1.1 Instrument data is kept by respective analysts until one(1) data file box

(approximately 30 analytical runs) is full. Custody of the file box of instrument

runs should be released within one month to the QA/QC Department. This is

the temporary storage phase. Data custody is documented on a ledger. The file

box is maintained in the QC Dept hallway. This is the secondary storage phase.

After secondary storage, file boxes are also stored and maintained at 4116 Atlas

Ct in Bakersfield.

8. 7.1.2 Approval by the President for record destruction must be made and

documented before any data destruction is to commence.

8. 7.1.3 Records including maintenance, extraction, analytical, reagent, and

standards logs are released to the QA/QC department approximately one (1)

month after the final entry is made into pertinent logs. The QA/QC

Department assumes custody by recording pertinent information into a

ledger, then stores records and documents in designated boxes which are

maintained in the QC Dept hallway. When boxes are full, they are

transferred to on site sea-trains or final storage location is 4116 Atlas Ct in

Bakersfield.

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8. 7.1.4 Tapes and disks are stored temporarily near respective instruments then

indefinitely in the Data Storage Room. Custody is maintained by the

QA/QC Department.

8. 7.2 Inorganics Department

8. 7.2.1 Record maintenance for ICP and ICP-MS follows the same

practices as Organic's records. AA, Hg by CV, and GFAA records

are stored in files by month in file storage cabinets and data boxes

in the Metal's area. Records in these cabinets are removed on a

yearly basis by Metal's Department personnel and released to the

QA/QC Department. Records, in file boxes, are stored in the QC

Dept hallway then eventually to on site sea-trains or QC warehouse

4116 Atlas Ct, in Bakersfield CA.

8. 7.2.2 Logs are maintained in the same manner as Organic's logs.

8. 7.2.3 Disks are stored near respective instruments temporarily then

indefinitely in the Data Storage Room. Custody is maintained by

the QA/QC Department.

8. 7.2.4 Record maintenance is similar to storage procedures for the metals

department.

8. 7.2.5 Logs are maintained in the same manner as Organic's logs.

8. 7.2.6 Tapes are stored temporarily near respective instruments then

indefinitely in the Data Storage Room. Custody is maintained by

the QA/QC Department.

8. 7.3 Sample Control Department, Field Services Department, Client Services

Department

8. 7.3.1 All records are released to the QA/QC Department on an as

needed basis. Records are stored temporarily in the Lab’s Hallway by

the QC Department then transferred to their designated location.

Final storage locations are either on site sea-trains or the storage

building on 4116 Atlas Ct in Bakersfield.

8. 7.4 Data Control Department

8. 7.4.1 Submission files which include case narratives, check sheets, bench

worksheets, chain of custody records, QA/QC reports, and possibly

copies of spreadsheets, extraction log sheets, instrument printouts,

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and other records, are filed in the Data Office. The data filing

specialist assumes and maintains custody of submission files.

8. 7.5 LIMS Department

8. 7.5.1 Records from the LIMS which include data processing records,

programs, and data modification records are maintained by the

LIMS Department until lack of storage space necessitates

transferred of records to the QA/QC Department. These records are

stored in on site sea-trains and onsite warehouse then moved to

4116 Atlas Ct in Bakersfield.

8. 7.5.2 Program projects and LIMS modifications are put into individual

folders numbered with a unique project number. Folders are stored

in boxes in sequential order. Boxes are kept in LIMS manager’s

office for one year then transferred to the LIMS department sea-

train (the final Aresting place=). Microsoft Outlook is used to track

projects and keep brief summaries of work performed.

8. 7.5.3 System back-up tapes are maintained by the LIMS Department

Supervisor on and off site. On site storage is the Computer Room

and an in on-site safe; offsite storage is a climate controlled book

storage unit.

8.8 QA/QC RECORDS

8.8.1 Technical Review Sheets – Analysis sequence which guide reviewers to parameters

of interest. This is a record of technical review.

8. 8.2 Organic secondary data review is documented by analysis sequence sheet.

8. 8.3 Balance Monitoring Log - Use to document analytical and top-loading balance

calibration on a daily basis and weekends only designated balances(See SOP

BCQC008 for balance monitoring)

8. 8.4 Refrigerator and Freezer Monitoring Log - Use to document refrigerator and Freezers

temperatures on a daily basis.

8. 8.5 Oven Monitoring Log - Use to monitor oven temperatures on a work basis.

8. 8.6 Thermometer Calibration Check Log - Record of thermometer external checks

against a NIST reference thermometer.

8. 8.7 Waterbath Logs - Record of waterbath temperature during analysis.

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8. 8.8 Auto-diluter Calibration Record - Gravimetric checks of auto-diluter volume

deliveries.

8. 8.9 Data Custody Log - Record of custody of data.

8. 8.10 Spreadsheets and Access Databases- Use to track controlled documents

8. 8.10.1 Audits

8. 8. 10.2 IDC - Initial Demonstration of Competency Forms

8. 8. 10.3 Instruments Tracking

8. 8. 10.4 Raw Data Custody

8. 8. 10.5 SIF=s

8. 8.10.6 Sample Custody

8. 8. 10.7 Logbooks

8.9 RECORD / DOCUMENT STORAGE

8.9.1 Data Storage Log - Record of custody of instrument data.

8. 9.2 Archived In/Out Raw Data Log - Used to document custody of In/Out Archived Raw

Data.

8. 9.3 Electronic records are maintained to document 1) all LIMS activities, and 2) analytical

activities on IC's, GC's, GC/MS's, ICP's and the ICP-MS's. Electronic records are in the

form of tapes and disks.

8. 9.4 All records are backed up in dual process: one is data (hardcopy) file box and the other

is raw data CDs. Sample control records, Analytical/Instrument records, QA/QC

records and support documentation records received in a QA/QC.

Department are documented in a raw data management storage log with date affective,

instrument #, date relinquished/received custody of records with analyst initial. Each

data file box/data CD is assigned a number in a sequential order per year (e.g. 09-000 or

09CD000) numbers are entered into raw data Microsoft Access Database. However,

Internal audits, management reviews, corrective and preventive actions (SIFs) are kept

in an on-site fireproof record storage for seven (7) years.

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8. 9.5 Data is transferred to a CD on a monthly basis for each instrument and all CDs are

stored in fire proof storage in a sequential order per year. In case, substitution of lost

and /or replacement of damaged records can be retrieved from the back-up CDs.

8.9.6 MAINTENANCE OF RECORDS:

Data file records are stored and retained in such a way that they are readily retrievable

in a facility and off-facility storage, 4116 Atlas Ct in Bakersfield, which provides a

suitable environment to prevent damage and or loss of records.

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8.10 STORAGE RECORDS

After creation, records are stored in the onsite sea-trains or QC warehouse at 4116 Atlas Ct in

Bakersfield which is used for final storage of records. Records are kept for at least seven (7)

years, unless particular project specific protocols mandate otherwise. All destructive records

are moved to inactive file.

8.10.1 Closure of BC Laboratory

8.10.1.1 In case of permanent laboratory closure all records associated with analytical

data will stored off-site archived record storage until time limit has been

exceeded.

8.11 DATA ARCHIVAL

Final data are in the following forms:

Hardcopy

Submission files

Raw data

Support data

Diskette

Data disks

Tapes

All records, except submission files, are submitted to and archived by QA/QC Department

personnel. Submission file archival procedures are conducted by the filing specialist.

8.11.1 Hardcopy Archival

All hardcopy files are collected into boxes which are sequentially numbered by the filing

specialist or QA/QC personnel. Box ID's are then entered into a spreadsheet with the

following corresponding data:

Box number

Box contents

Instrument number

Analysis code

Custody date

All boxes are temporarily stored on site, until storage space is exhausted, then

transferred to the 4116 Atlas Ct in Bakersfield.

8. 11.2 Diskette

Diskettes are stored in the onsite raw data storage room. Each diskette is labeled and

stored in a box which is also labeled. All information is kept in spreadsheet form.

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8. 11.3 Data disks

Imaged data is maintained on hard drive type disks. Back up disks are labeled and kept

in an on-site safe. The LIMS Department is responsible for storage of these disks.

8. 11.4 Tapes

Tapes are used to archive both instrument data and LIMS files. All instrument tapes are

labeled by respective analysts then submitted to the QA/QC Department for storage.

Instrument tapes are stored in labeled boxes in the raw data storage room.

LIMS backup tapes are maintained by LIMS Department personnel. One of the six sets

of tapes is kept off site to provide additional security in case of catastrophic events.

8.12 CONTROLLED ACCESS OF RECORD

All secondary data storage areas are maintained under lock and key. Warehouse storage is

electronically secured thus persons requiring retrieval of data must adhere to protocol in order

to obtain access.

8.12.1 Procedure

Contact the respective person(s) responsible for particular archived items. Have the

responsible person document custody procedures, and then assume custody. The person

who assumes custody is now responsible for all items in hand until documentation of

return of items is complete.

Submission files

Contact: Data filing specialist

Custody documentation: Internal COC out cards & Altered Completed Files Form

Raw data hardcopies

Contact: QA/QC Department personnel

Custody documentation: Internal COC logbook

Diskette



Data Disks

Contact: LIMS Department personnel


Tapes



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8.12.2 Limitation of Access

The person(s) responsible for maintenance of archived data has the right of refusal of

access, thus President and/or Supervisor approval may be needed in order to access

data.

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9.0 INSTRUMENTATION

9.1 Wet Chemistry

9.1.1 Ion Chromatographs

Instrument ID Analysis Year in

Service

Method

Dionex Model DX500

LC20 CE (CE01 Chromatography Enclosure)

CD20 (CD03/CD04 Conductivity Detector)

IP25 (IP01/IP02 Peak Net Software )

AS 40 (AS52/AS46 Automated sampler)

EG01/EG02 Eluent

IC1 /IC2

Chloride, Nitrate, Sulfate

Bromide, Fluoride

2000 EPA-300.0

IC-04

Dionex Ion Chromatograph (AD-02)

AS 40 (AS47 Autosampler)

IP 25 (IP03 Isocratic Pump)

LC 20 (CE03 Chromatography Enclosure)

PC 10 (PC01 Pneumatic Controller)

Dionex VWD (AD02 Absorbance Detector)

EG04 (Eluent)

IC4 Hexavalent Chromium

2005 EPA-218.6/

SW-7199

IC5

AS40 (AS58 Automated Sampler)

LC20 (CE04 Chromatography Enclosure)

IC25 (IP05 Ion Chromatography)

EG09 (Eluent)

IC5 Chloride, Nitrate, Sulfate

Bromide, Fluoride

2009 EPA-300.0

IC-06

Dionex Model ICS 2100

AS 64 Automated Sampler

EG10 Eluent Generator

IC6

Perchlorate

Iodide/Thiosulfate

2012

EPA-314.0

IC-07

Dionex Model IC 25


EG40 Eluent Generator 1(EG-03A, EG-03B)

LC25 Chromatography oven (CE-02)

IC7

Volatile Fatty Acid

2013

EPA-300.0

IC-08

Dionex Model IC 25


EG40 Eluent Generator 1(EG-11)

LC25 Chromatography oven (CE-05)

CD06 Conductivity Detector

IP06 Isocratic Pump

PC02 Pneumatic Controller

IC8

2014

EPA-300.0

9.1.2 Auto Analyzer Systems


Service

Method

Konelab 20

Thermo clinical labsystems

Kone-1 Nitrite, Ortho - phosphate,

Hexavalent Chromium,

Cyanide, Phenols,

Ferrous Iron

2003 EPA-353.2

SW-7196A

EPA-365.1

EPA-335.2

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EPA-420.4

Smart Chem

(Westco Scientific Inst)

SC-1 NH3-N, TKN, NO3/ NO2,

Total.Phosphate

2007 350.1, 351.2,

353.2, 365.4

9.1.3 Other Instruments Instrument

ID

Analysis

Year in

Service

Method

Spectronic 20 Genesys

Spec 06

COD

MBAS

Sulfide

2014

EPA-410.4

EPA-425.1

SM-4500SD Orion Research Analog pH meter 301

Beckman 360 pH/Temp/mv Meter(2)

360

pH in water samples

2000

EPA-150.1,9045,

9040

YSI Model 3100-115V Conductivity Meter

CND-4

Electrical Conductivity

2013

EPA-120.1

Hach DBR 200 COD Reactor

COD03

COD

2008

EPA-410.4

Hach Model DRB200

COD04

COD

2011

EPA-410.4

Hach Model 2100N Turbidimeter

Turb-01

Turbidity

2003

EPA-180.1

Hach Model 2100N Turbidimeter

Turb-04

Turbidity

2013

EPA-180.1

YSI Model 57 Oxygen Meter

IMHOFF Cone

Thermolyne (Auto Mixer)

YSI-57

BOD, C-BOD, Dissolved O2

Seattleable Solids

TKN, Total. P

1990

SM-5210B

EPA-360.1

EPA-160.5

Brinkman Digital Buret

BDB

Alkalinity (HCO3, CO3, OH)

1995

EPA-310.1

Aurora Model 1030

Auto Sampler 1088

TOC-2

TOC Analysis

2006

EPA-415.1

Metrohm

PEA 1R

pH, EC, OH, CO3,HCO,

2008

EPA-150.1,

9040, 120.1,

9050, 310.1, SM

2320 B Metrohm

PEA 1C

pH, EC, OH, CO3,HCO

2008

EPA-150.1,

9040, 120.1,

9050, 310.1, SM

2320 B

9.2 Metals

9.2.1 Inductively Coupled Argon Plasma / Mass Spectrometer


Service

Method

Perkin Elmer

Elemental Scientific ICP-MS(SC2DXS)

PE-EL2 Metals 2011 EPA 200.8

SW 6020B

Perkin Elmer Elan 9000

ICPMS (P2160412)

PE-EL 3 16 Routine metals;Additional metals

available upon request

2014 EPA-200.8/6020

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9.2.2 Inductively Coupled Argon Plasma

Instrument ID Analysis

Year in

Service

Method

Perkin Elmer Optima 4300DV PE-OP2 Metals 2004 EPA 200.7

SW 6010B

Perkin Elmer Optima 8300DV PE-OP3 Metals 2014 EPA 200.7

SW 6010B

9.2.3 Graphite Furnace Atomic Absorption Spectrophotometers

Instrument ID Analysis

Year in

Service

Method

Perkin Elmer SIMAA 6000

Auto sampler 72

Zeeman Background

AA Winlab Software

Perkin Elmer

Furnace Cooling

System FCSO1

PE-1 Chromium

2000 EPA-200.9

9.2.4 Mercury Analyzers

Instrument

ID

Analysis

Year in

Service

Method

Quick Trace Mercury Analyzer M-6100

CETAC1

Mercury

2004

SW-7470A/245.1 &

SW-7471A

9.2.5 Flash Point Instrument

ID

Analysis

Year in

Service

Method

Koehler, K16200 Flash Point Unit FP#1 Pensky Martin

Closed Cup

Manual Flash Test

2012

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9.3 ORGANICS

9.3.1 GC/MS - Semi Volatiles Instrument

ID

Analysis

Year in

Service

Method

HP 5972 Series GC System

HP 5890 Series Autosampler

HP Tray ASTR08

HP7976 AS71

HP Chemstation with Enviroquant

MS-B1

Semi-Volatiles

1994

EPA-625

EPA-8270C


HP 59822B IAG02

HP GC System injector

HP 5890 Series Autosampler

HP Tray ASTR06


MS-B2

Semi-Volatiles

1994

EPA-625

EPA-8270C

Varian 4000 GC / MS

Varian CP-8400

Autosampler

MS-B3

Synthetic Organic

Compounds

2007

EPA-548


GC System injector 7673

HP 5973 Mass Selective Detector

MS-B4

8270 NDMA, 8270 SIM,

PNA, 1,4-Dioxane

2003

EPA 8270C

HP 6890 Series GC, 7673 Injector

MS-B6

525, 507, 548(TBD)

2012

EPA-525

EPA-507 HP 6890 Series GC System

HP 5973 Mass Spectrometer 7673 Injector

HP GC System injector 7673

MS-B7

LUFT GC-MS, Diluent,

Motor Oil, Crude, Diesel,

8270 SIM, PNA

2013

Luft GC-MS

EPA 8270C

9.3.2 GC/MS - Volatiles

Instrument

ID

Analysis

Year in

Service

Method

HP 5890 II Series GC System

HP 5972 Series (MSD)

Tekmar 3100 Concentrator

Tekmar Dohrmann Solatek 72


MS-V2

Volatiles

2009

EPA-8240B

Soil**

EPA-8260B

Soil**




Tekmar Dohrmann Solatek 72


MS-V3

Volatiles

1993

EPA-8240B Soil

EPA-8260B Soil

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Tekmar Dhormann Aqua Tek 70


MS-V5 Volatiles 1999 EPA-8240B

EPA-8260B**

521.2



Tekmar Aqua Tek 70



MS-V6

Volatiles

2000

EPA-524.2(SIM

1,2,3-TCP)






MS-V7

Volatiles

2001

EPA-601/602**

EPA-624**



OI Analytical eclipse Model 4660 Concentrator

OI Analytical 4551-A Sampler


MS-V10

Volatiles

2001

EPA-8260B

Short List



OI Analytical eclipse Model 4660 Concentrator

OI Analytical 4551-A Sampler


MS-V12

Volatiles

2003

EPA-8260B

Short List

Agilen Technologies 6890N Network GC System

Agilen Technologies 5973 (MSD)




MS-V13

Volatiles

2003

EPA-8240B

EPA-8260B






MS-V14

Volatiles

2013

EPA-524.2

EPA-8260B

EPA-8240B

EPA-8260B SIM

** DOD Project Specific

9.3.3 Air Room Testing Instrument

ID

Analysis

Year in

Service

Method

MS-A1 HP 6890 Series GC System

MSD-19 HP Agilent 5973

PCT-1 Preconcentrator 7100AR

AS-62 Autosampler 7405

CCI-A1 Canister Cleaner 3100A

MS-A1

a TO-14V Full

a TO-15V Full

2009

TO-14A

TO-15

MS-A2 Agilent 6890 N

MSD-18 Agilent 5973N

MS-A2

a TO-3V Full

2009

TO-3

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AS-60 Autosample and Pre. Concentrator model

7032AB-L MS-A3 Agilent 6890

MSD-20 Agilent 5973 Mass Selective Detector

AS-63 Autosampler model 7032AQ-L

MS-A3

a TO-3V Full

2009

TO-3

GC-A1 Agilent 6890 N (TCD/FID)

AS-59 Autosampler 7032 AB-L

DD-10 Dynamic Dilutor(4600A)

GC-A1

a 3CV fixed gasses

a A-D 1946 fixed gasses

2009

3C Fixed

Gases

9.3.4 Gas Chromatography

Instrument

ID

Analysis

Year in

Service

Method

HP 5890 Series II Dual FID

HP 7673 Dual Tower Autosampler

HP Chemstation with GC-Enviroquant

GC-2

Diesel

Fuel Fingerprint

Carbon Ranges

1991

8015M

HP 5890 Series II Dual ECD

HP 6890 Injector

HP Chemstation with GE-Enviroquant

GC-3

Haloacetic Acids

Formaldehyde

2008

2009

EPA-552.3

EPA-556.1

Varian 3300 Dual ECD

Varian 8200 Autosampler


GC-4

DBCP and EDB

1989

EPA-504.1

HP 5890 Series II Split/Splitless Injector

HP 7673 Autosampler


GC-5

Diesel

1989

8015 M

HP 5890 Series II

HP GC System


HP 7673 injector

HP Controller

GC-8

Chlorinated herbicides

1990

EPA-515.1

EPA-8150

EPA-8151A

615




HP 7673 injector

GC-12

Methanol, Ethanol

1992

8015 DI




HP Controller

GC-13

Diesel

1992

8015M

HP 6890 Series

HP 6890 Autosampler


GC-14

pesticides

2011

EPA-508

EPA-608

EPA-8082

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HP Controller HP 6890 Series II

HP 6890 Autosampler


GC-15

pesticides

2012

EPA-508

EPA-608

EPA-8082 HP 6890 Series II

HP 6890 Autosampler


GC-17

pesticides

2013

EPA-508

EPA-608

EPA-8080

EPA-8081A

EPA 8082 HP 6890 Series II

HP 6890 Autosampler


GC-18

Organophosphorus pesticides

2015

EPA-8140

EPA-8141A

9.3.5 Gas Chromatography - Volatiles

Instrument

ID

Analysis

Year in

Service

Method

Varian 3400 GC-V1 RSK-175

RSK-175 FULL

1991 Methane, Ethene,

Ethane

Mehane,Ethene,

Ethane, Propane HP 5890 Series II with PID and FID


Tekmar Precept II Autosampler


GC-V8

BTEX, MTBE, TPH (gas)

1998

EPA-8020,

8021B

8015M

5035 HP 5890 Series II with PID and FID

Tekmar 3100 Sample Concentrator

Aqua Tek 70 Auto Sampler


GC-V9

BTEX, MTBE, TPH (gas)

2013

EPA-8020,

8021B

8015M

9.3.6 PETROLEUM Instrument

ID

Analysis

Year in

Service

Method

Grabner, Minivap VPXpert PE#1 Vapor Pressure 2012 Petroleum

Agilent 6890, FPD PE#2 Sulfur Compounds 2012 Petroleum

Agilent/Wesson 6890, Dual TCD, FID PE#4 Fixed Gases, C1-C6+

Hydrocarbons

2012 Petroleum

Thermo Scientific, 2839

High Temp Water Bath

PE#5 Various 2012 Petroleum

IEC, HN Centrifuge PE#6 Centrifuse Procedures Unknown Petroleum

TOX-100 AM743931

PE#7 Organic Chlorides

Total Sulfur

2013 Petroleum

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PAC OptiDIst 04071 PE#8 Distillations 2013 Petroleum

Density Meter-DMA4500M

PE#9 API Gravity, Density and

Specific Gravity

2013 Petroleum

Viscometer-SVM3000 PE#10 Viscosity 2013 Petroleum

9.3.7 HPLCs Instrument

ID

Analysis

Year in

Service

Method

HP 1050 Model 79856A

Quarternary Eluent Pump

HP 1100 Series

Autosampler

Multiwavelength UV Detector


LC-14

Polynuclear Aromatic

Hydrocarbons

Carbamate and Urea-containing

Pesticides

Nitroaromatic and Nitramines

1994

EPA-610

EPA-8310

EPA-632

EPA 8330

EPA 549

9.3.8 Instrument


Service

Method

SPE - DEX (main)

(Controller Extractor)

Horizon Technology

model - SPE - 100

Serial - 06 - 0489

SPE - DEX 525 Extraction 2007 525 Extraction

Extractor SPE 03

model - SPE - 4790


Extractor SPE 04

model - 06 - 0799


Extractor SPE 05

model - 06 - 0797


Extractor SPE 06

model - 06 - 0802


Extractor SPE 07

model - 06 - 0798


Extractor SPE 08

model - 06 - 0800


Extractor SPE 09

model - 06 - 0801


Extractor SPE 10

model - 06 - 0796


9.3.9 Other Instruments

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Service

Method

OA-SYS (Heating System Blue M)

Precision Scientific (Coliform Incubator

Bath)

1992

3510

3550

3580

9.3.10

Instrument ID

Analysis

Year in

Service

Method

Liquid-Liquid Extractor 2 LLE-2 3520

Continuous Liquid-

Liquid Extraction

2008 3520

Continuous Liquid-

Liquid Extraction


Continuous Liquid-

Liquid Extraction

2008 3520

Continuous Liquid-

Liquid Extraction


Continuous Liquid-

Liquid Extraction

2008 3520

Continuous Liquid-

Liquid Extraction


Continuous Liquid-

Liquid Extraction

2008 3520

Continuous Liquid-

Liquid Extraction


Continuous Liquid-

Liquid Extraction

2008 3520

Continuous Liquid-

Liquid Extraction


Continuous Liquid-

Liquid Extraction

2008 3520

Continuous Liquid-

Liquid Extraction


Continuous Liquid-

Liquid Extraction

2008 3520

Continuous Liquid-

Liquid Extraction


Continuous Liquid-

Liquid Extraction

2008 3520

Continuous Liquid-

Liquid Extraction


Continuous Liquid-

Liquid Extraction

2008 3520

Continuous Liquid-

Liquid Extraction


Continuous Liquid-

Liquid Extraction

2008 3520

Continuous Liquid-

Liquid Extraction


Continuous Liquid-

Liquid Extraction

2008 3520

Continuous Liquid-

Liquid Extraction


Continuous Liquid-Liquid

Extraction

2008 3520

Continuous Liquid-

Liquid Extraction


Continuous Liquid-

Liquid Extraction

2008 3520

Continuous Liquid-

Liquid Extraction


Continuous Liquid-

Liquid Extraction

2008 3520

Continuous Liquid-

Liquid Extraction

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Continuous Liquid-

Liquid Extraction

2008 3520

Continuous Liquid-

Liquid Extraction


Chiller Recirculation

2008 Chiller

Recirculation


Chiller Recirculation

2008 Chiller

Recirculation


Liquid Extraction

2008 Liquid

Extraction

9.4 Microbiology Instrument

ID

Model

Analysis

Year in Service

Incubator - VWR Model(1)

102

1565

5.5.5 or 10 Tube

1989

Incubator - VWR Model (2)

102

1565

1989

Incubator - ASP Model (3)

American Scientific

103

IS-81

5.5.5 or 10 Tube

1989

Autoclave (1)

Marketforge Sterilmatic (2)

AMS001

STM-E

STM-EL

1600 Tubes of media (3200)

1990

WaterBath

Thermo Scientific (Precision)

W13

2862

10/20 Tube Samples

2008

Quebec Colony Counter

Capacity/100

Potential Capacity/200

QCC001

3330

Colony Counter

1980

IDEX Spectroline

IDEXX

IDXS001

CM-10

Total Coliform E. Coli Colliert

presence/Absence

1996

IDEXX

Quanti Tray Sealer Model 2X

IDXT001

2X

Total Coliform E. Coli Colliert

presence/Absence

2003

9.4.1 BACTERIOLOGICAL EQUIPMENT Equipment

Manufacture

Model

Date Last

Maintenance

pH Meter Orion Research 301 Per Use

Balance Mettler Toledo JB3002-L-G/A 7/16/2013

Conductivity Meter YSI 3100 Per Use Incubator

VWR 1565

Monthly VWR 1565

American Scientific IS-81

WaterBath

Thermo Scientific (Precision) 2862 Quarterly

Refrigerator North Star - As Needed Autoclave

Marketforge Sterilmatic STM-E Weekly/Monthly

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STM-EL

Hot Air Over VWR 1370FM Per Use/Monthly

Colony Counter Darkfield Quebec 3330 Per Use Ultraviolet Light 254 nm

IDEX Spectroline

IDEXX

EA-160 Per Use

9.5 ORGANICS

9.6 Field Service-Sampling Equipment

1. 2'= Grunfos Pump with hydralic Reel and Control Box

for pumping water out of monitor wells.

2. ProAir Air compressor, 20 gal, 5 HP model # PRFB5020VP

3. Genetac megaforce 6500 generator model No. 1006-0

4. Quik-E-bailer model 300DC For taking water out of monitor wells

5. Dissolved oxygen meter model 51B, serial # 13633 for Field Do=s *

6. Turbidity meter model 2008 serial # 1914-3593 *

7. H2S monitor model HS-82A serial # HS7568

8. H2S Continuos Monitor TXL01

9. Oakton pH/conductivity and temperature meter serial # 35858 – PH11

10. Oakton pH/conductivity and temperature meter serial # 510764– PH15

11. Oyster pH/conductivity and temperature meter serial # 976858– PH16

12. Sensidyne gastec pumpkit model # 800 *

For testing H2S in the field.

13. Airchek sampler model 224-PCXR7 serial # 523231 *

Sampling air in the field.

14. 2'= Grunfos Pump with Hand Reel and Control Box

for dumping water out of monitor wells.

15. Scott 2.2 self contained breathing apparatus serial # 39700110 *

16. 3-extra oxygne tanks for Scott 2.2 SCBA=s *

17. ISCO 3210 ultrasonic flow meter serial # 09748-025

Measuring the amount of water that has flowed during a certain amount

of time

18. Scott 2.2 self contained breathing apparatus serial # 39800176 *

19. Scott 2.2 self contained breathing apparaturs serial # 39700096 *

20. ISCO 3700 24 hr water sampler serial # 09421-074

21. ISCO 2700 24 hr water sampler serial # 06112-097

22. CLT01

23. 2-chlorine test kits model CN-70

24. 3-Hand soil Auyers and extentions

25. Sigma 24 hr auto sampler model # 1350 serial # F07937875 *

26. Gas meter and air sampling canister serial # 27515 *

27. Gas meter and air sampling canister serial # 1197501 *

28. Gas meter and Air sampling canister serial #1197500 *

29. 5 cooling coils and hoses for sampling Hot samples to cool them

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down before sampling *

30. O2,lel,H2S monitor model 6x82 serial # 13545 *

31. 4 ISCO batteries and 2 chargers

32. Clam shell sampler for sludge

33. Half-face respirator Scott 66M

34. Half-face respirator North 770030 Series M *

35. Full Face respirator Scott P/N 802451-01 *

36. Half-face respirator Scott 66M

37. Vacuum pump serial # 1190 model # 2Z866

38. Gas Powered soil Auger and extensions *

Note: * = These equipments are available for use.

9.7 Support Equipment & Supplies

9.7.1 Laboratory Information Management System (LIMS)

1. Hardware

1. Compaq Proliant ML530

1. Intel Pentium XEON 1 Ghz Processor

2. 1 Gb SDRAM

3. Hot Plug Drive Cage - Ultra 2

4. Integrated Ultra 2 SCSI Controller

5. Compaq Smart Array 431 Controller

6. RAID 5 with Online Spare Setting

7. 1.44 Mb Floppy Disk Drive

8. Five 18.2 Wide Ultra 3 SCSI Hot pluggable drive

9. 32x CD-ROM

10. Compaq 10/100 TX UTP NIC

11. Compaq 40/80 Gb DLT Drive-Internal

12. Automatic Server recovery

13. Compaq Insight Server Manager

14. 3 year Limited Warranty


3. ML530 Hot Pluggable Redundant Power Supply

4. Device ID: 11001

5. Serial Number; D043FPW1K126

2. Installed Software

1. Novell Netware 5.1 with Service Pack 2.0A

1. 105 user license

2. Serial Number = 300792721

Activation Key = 2D27C68EFE2CB72F

3. Serial Number = 400439667

Activation Key = 4B5669AA6C9E1D16

2. Arev NLM 5.0

3. Backup Exec for Netware Version 8.5 Revision 3012 Multi-Server Mode (by

Veritas)

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4. Inoculate - IT Version 4.5 100 User (Not used)

3. Volumes

Volume Name Drive

Size, MB

Major Contents

SYS

G:

3000

System Files, Email In-Box

APPS

F:

20000

LIMS Database, Raw Data

DOCS

H:

8002

Client EDDs, Word Document, Control Charts

QUE

Q:

2000

Print Job Queues

WEB_APPS

W:

18000

Web Pages, User Home Directories, Quotes, Time Clock, Quotes, Misc

Printers

1. Laser Jet Printers 84

2. Ink Jet Printer 7

3. Dot Matrix Printers 2

4. Label Printers 10

5. PC – Pentium 2 1



8. PC – Pentium Dual Core 48

9. PC – Pentium Quad Core 3

10. PC – Lap tops 13

4. Scanners 2

I.

Servers - Novell File Server

LIMS SOP 0521

Purpose

This file server is used for user authentification, print

services, file services, and hosts the Legacy Arev LIMS

database.

II. Configuration

A. Information

1. Server Name SRV_BCLABS

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2. Device ID 11001

3. Serial Number D043FPW1K126

B. Hardware


a. Intel Pentium XEON 1Ghz Processor

b. 1 Gb SDRAM

c. Hot Plug Drive Cage - Ultra 2

d. Integrated Ultra 2 SCSI Controller

e. Compaq Smart Array 431 Controller

f. RAID 5 with Online Spare Setting

g. 1.44 Mb Floppy Disk Drive

h. Five 18.2 Wide Ultra 3 SCSI Hot Pluggable Drives

i. 32x CD-ROM

j. Compaq 10/100 TX UTP NIC

k. Compaq 40/80 Gb DLT Drive - Internal

l. Automatic Server Recovery

m. Compaq Insight Server Manager

n. 3 year Limited Warranty


3. ML530 Hot Pluggable Redundant Power Supply

C. Installed Software

1. Novell Netware 5.1 with Service Pack 2.0A

a. 105 user license

b. Serial Number = 300792721Activation Key =

2D27C68EFE2CB72F

c. Serial Number = 400439667Activation Key =

4B5669AA6C9E1D16

2. Arev NLM 5.0

3. Backup Exec for Netware Version 8.5 Revision 3012

Multi-Server Mode (by Veritas)

4. Inoculate-IT Version 4.5 100 User (Not used)

D. Volumes

Volume Name Drive Size, MB Major Contents

SYS G: 3000 System Files, Email In-Box

APPS F: 20000 LIMS Database, Raw Data

DOCS H: 8002 Client EDDs, Word Documents, Control Charts QUE Q: 2000 Print Job Queues

WEB_APPS W: 18000

Web Pages, User Home Directories, Quotes, Time Clock,

Quotes, Misc

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Servers – Windows SQL Server (Test)

LIMS SOP 0522a

I. Purpose

This file server is used exclusively as a Test SQL database server.

II. Configuration

A. Information

1. Server Name: BCL_LIMS_Pinos

2. Device ID: 11002

3. Serial Number: 6J32LOG55C002

4. IP Address 192.168.168.008

B. Hardware

1. Compaq Proliant ML570 G2

Intel Xeon 2.00 GHz processor

4 GB RAM (2x1024, 2x512, 4x256)

Two 6x1” Drive cages (holds up to 12 1” hard drives)

Integrated Dual Wide-Ultra 3 Controller

Smart Array 5304/256MB Four Channel Controller (RAID)

RAID 5 with online spare

Four 36.4GB pluggable Ultra3 SCSI hard drives

AIT 100 GB tape drive, hot pluggable

NC3163 Fast Ethernet 10/100 WOL PCI

NC7131 Gigabit Server Adapter, 64-bit/66MHz, PCI, 10/100/1000-T

Two redundant 600W hot pluggable power supplies

Redundant hot pluggable fan

1.44MB floppy disk drive

48X CD-ROM drive

Compaq Insight Server Manager

3-year limited warranty


1. Windows 2000 Server plus 5 CALs

2. Microsoft SQL Server 2000 Enterprise (1 processor)

Servers - Windows SQL Server (Test)

LIMS SOP 522b

I. Purpose

This file server is used exclusively as a Test SQL database server

II. Configuration

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A. Information

1. Server Name Bcl_Lims_Slate

2. Device ID: 11003

3. Serial Number: 6J35LG52R00H

4. IP Address 192.168.168.007

B. Hardware


a. Intel Pentium 4 2.53 GHz processor

b. 1 GB RAM (4x256, PC2100 ECC DDR SDRAM)

c. Integrated Single Channel Ultra3 SCSI Adapter

d. Smart Array 642 Controller (RAID) (RAID 1 setting)

e. 36.4GB Ultra3 SCSI 10,000 rpm Hard Drive

f. 1.44MB Floppy Disk Drive

g. High speed IDE CD-ROM Drive

h. Compaq NC7760 PCI Gigabit Server Adapter (Integrated/Imbedded)

i. SmartStart and Insight Manager

j. 1-year Limited Warranty

2. Drive Cage

a. ML3xx Two Bay Hot Plug SCSI Drive Cage

b. 3 146.8 GB 10K Pluggable Universal Hard Drives


1. Windows Server 2003 Standard Edition plus 5 CALs

2. Microsoft SQL Server 2000 Standard Edition

Servers - Windows SQL Server (Production)

LIMS SOP 522e

I. Purpose

This file server is used exclusively as a Production SQL database server

II. Configuration

A. Information

1. Server Name Bcl_Lims_Shasta

2. Device ID: 11005

3. Serial Number: USE907N25C

4. IP Address: 192.168.168.10

B. Hardware

1. HP Proliant ML370 G5 Tower Server

a. Intel Quad core Xeon E5440 2.83 GHz processor

b. 32 GB RAM (8x4GB, PC2-5300, DDR2, 667 MHz)

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c. Smart Array P400-Series 512MB (RAID 6 setting)

d. Eight 72GB SAS SFF Single Port 15K rpm Pluggable Hard Drive

e. 1.44MB Floppy Disk Drive

f. High speed IDE DVD/CD-ROM Drive

g. HP Gigabit Server Adapter (Integrated/Imbedded)

h. HP Redundant Hot Plug Power Supply

i. HP Redundant Hot Plug Fan

j. 3-year On-Site 24x7 6-hour call-to-repair warranty


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9.8 Laboratory Water System

Instrument Year in Service

Ionics Deionized Water System 1990

Ionics Nanopure Water System 1990

9.9 Glassware


Class A for Reagent and Standard Preparation 1990

Various Calibrated Units 1990

9.10 Diluters


Hamilton Microlab 500 Series (Diluters #’s 4) 2000





9.6.5 Refrigerators


Northstar Walk-In 1987

Rancho Reach-In (2) 1990

Traulsen Reach-In (1) 1987

Nor lake (1) 1987

Refrigerator: Monitowoc(1), Zero Zone(1), VWR Scientific(2), Reach In (1), GE(4),

Magic chef(1), Sears Cold Spot(1), McCall(1), Ardco (1), FRIGIDAIRE (GM)

Freezer: Box Freezer(1), Cold Spot(1), Whirlpool(1), GE(3), Montgomery Ward(1)

9.11 Ovens


Fisher Scientific (3)(#’s 17, 20, 10) 1987

VWR (2)(#’s 19& 22) VWR Scientific (1) (#’s 16) 1987

Precision Scientific (2)(#’s 13) 1987

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Thermo Precision Scientific(2)(#’s 19&21) 2008

Thermo Precision Scientific(2)(#’s 23) 2009

9.12 Misc Equipment Instrument

Year in Service

Balance- Mettler Toledo

Top Loading

ML3001E/03(#29)

2012

Balance- Sartorius

Sartorius ED124S (#28)

2011

Balance- Sartorius

ED224S (#27)

2009

Balance-Mettler Toledo

Analytical

AB 204-S (#25)

1987

Balance-Ohaus Precision Standard

Top-Loading

Scout Pro SP202(2) (#24 & 23), TS4KD (#16)

1988


Top-Loading

PE3600, PL300 (#10 & 12)

1988


Top-Loading

PB3002-S, BD202, PB1502-S (#19, 13 & 21)

2000

Balance-Denver Instrument

Analytical

Denver Model A160 (#8)

2000


JB3002-L-G/A(#26)

2008

Mettler Toledo

Analytical

PB303 (#8)

2000


Top-Loading

TS400 (#16 & 11)

2008


Top-Loading

TS400 (#30)

2014

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9.13 Safety

Instrument Qty

Laboratory Hoods 24

Fire Extinguishers

Halon

Combined Class ABC

36

Eye/Safety Showers 8/9

Chemical Spill kit 3

First Aid Kits 6

Fire Blanket 1

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CALIBRATION PROCEDURES AND FREQUENCY

SECTION X

REVISION NO. 26 EFFECTIVE DATE: 01/08/16

PAGE 1

10.0 INTRODUCTION

Outlined in this section are procedures, criteria, and frequency for the calibration of instrumentation

and protocols regarding standards, reagents and QC materials. Calibration processes are described in

further detail in respective method SOP's: Calibration procedures and criteria in specific SOP=s

supersede information listed in this document.

10.1 MATERIALS

Pre-qualification of standard stocks, reagents and support equipment or parts are addressed in

section XIX.

10.1.1 Standards

Accurate standards, stock purity and subsequent diluted aliquots, are required for

sound, accurate results. Standards are used as references by which all results are

derived or as accuracy verification checks (i.e. gravimetric based testing or flashpoint).

Protocols for standards are addressed in the QA Protocols manual.

10.1.2 Reagents

Use of properly prepared and bias-controlled reagents is essential in obtaining high

integrity results. Stock reagents must meet method specific purity requirements and as

well as concentration requirements. Information regarding reagent protocols are

addressed in the QA Protocols manual.

10.2 INITIAL CALIBRATION OF INSTRUMENTS

10.2.1 A minimum of five calibration standards for organics and a minimum of 3 calibration

standards for Inorganics should be prepared for each parameter of interest. One of the

calibration standards should be at a concentration near, but above, the MDL. Other

standards should correspond to the range of concentrations found in real samples but

should not exceed the linear range. Each standard should contain each Analyte for

detection be method.

10.2.2 Initial calibration points used shall be a subset of the original set. It should be noted

that only high point of the curve may be deleted. The low point is at the PQL and the

Mid-point of the initial calibration cannot be deleted. In addition, the minimum

linearity of the curve shall be determined either be a linear regression correlation

coefficient greater than or equal to 0.995 or by relative standard deviation (%RSD) of

20% for each Analyte. The calibration points cannot be re-analyzed more than once.

If the criteria is not met corrective action must be taken to correct the problem and a

new 6-point calibration curve MUST be generated. The curve, once generated, must

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have its accuracy verified by the second source standard (ICV) from different vendors.

10.3 CALIBRATION OF INSTRUMENTS

10.3.1 Inductively Coupled Plasma (ICP)

The ICP units are calibrated at the beginning of each day. Three standards, comprised

of various concentrations of metals, and a calibration blank are used in the calibration

process. The instruments are profiled before each run to maximize efficiency of

instrument performance.

Immediately after calibration, a check standard prepared from an external source is

analyzed to verify standardization process. Values must fall within acceptable limits

or recalibration must commence. After an acceptable check standard is run, an

instrument blank is analyzed of which all elemental results must be below the practical

quantitation level, or reevaluation of instrument parameters must take place, and/or

corrective action procedures must be employed.

An Interference check is run at the beginning and end of all sample runs to monitor

spectral interference associated with Ca, Mg, Fe and Al. All instrument readings of the

interference check must fall below the absolute value of each respective practical

quantitation limit. Continuing calibration verifications (check standards) and

continuing calibration blanks are run after every ten samples and the end of each run.

QC purposes: for ICP 6010B, a group of twenty samples are batched together. All

standards are prepared from NIST traceable sources.

METHOD

ICV

CRITERIA

CCV

FREQUENCY

CCB

FREQUENCY

LINEAR

RANGE STUDY

6010B

90-110%

Recovery

10%

10%

Annual

200.7

95-105%

Recovery

5%

5%

Annual

10.3.2 Inductively Coupled Plasma - Mass Spectrometer (ICP - MS)

The instrument is optimized each day before use, following manufacturer’s

specifications and criteria. After all optimization criteria are met the instrument is

calibrated with a blank and three standards, linearity criteria is set at r 0.995. An

ICV followed by an ICB is run and if these values are outside established limits the

instrument should be recalibrated before samples are run. Continuing calibration

verification and calibration blanks are run after every ten samples and at the end of

each run. All standards used are prepared from NIST traceable sources.

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REVISION NO. 26


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METHOD 200.8:

ICV CRITERIA

CCV

CRITERIA

CCV

FREQUENCY

CCB

FREQUENCY

Linear Range

Study

90-110% Recovery

85-115%*

Recovery

10%

10%

Annual

*For analysis of additional samples to continue, CCV's must be from 90-110% of their

expected values.

RF = AxCis

AisCx

10.3.3 Gas Chromatograph - Mass Spectrometer (GC/MS)

Each GC/MS system must be hardware tuned to meet the criteria listed in each

respective method. Analyses should not begin until all these criteria are met.

Background subtraction should be straightforward and designed only to eliminate

column bleed or instrument background ions. GC/MS tuning standard should also be

used to assess GC column performance and injection port inertness. For semi-volatiles

degradation of DDT to DDE and DDD should be less than 20%. Benzedrine and

Pentachlorophenol should be present at their normal responses and no peak tailing

should be visible. Peak tailing for 625's involve checking Benzedrine and

pentachlorophenol's peak tailing. Benzedrine must be <3 and pentachlorophenol must

be <5. If degradation is excessive and/or poor chromatography is noted, retention time

of 0.80-1.20 relative to one of the internal standards. Use the base peak ion from the

specific internal standard as the primary ion for quantitation. The injection port may

require cleaning. It may also be necessary to cut off the first 6-12" of the guard

column.

The internal standards should permit most of the components of interest in a

chromatogram to have for semi-volatiles analyze 1 l of each calibration standard

(Containing internal standards) and tabulate the area of the primary characteristic ion

against concentration for each compound. Calculate response factors for each

compound as follows:

Where: Ax = Area of the characteristic ion for the compound being measured.

Ais = Area of the characteristic ion for the specific internal standard.

Cx = Concentration of the compound being measured (g/ml).

Cis = Concentration of the specific internal standard (g/ml).

The Average RF should be calculated for each compound. The percent relative

standard deviation (%RSD = 100[SD/aveRF]) should also be calculated for each

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compound. The %RSD for each individual Calibration Check Compound (CCC) must

be less than 30%. The relative retention times of each compound in each calibration

run should agree with 0.06 relative retention time units (RRT). Construct calibration

curves of area versus concentration using first or higher order regression fit of the five

calibration points. The validity of the calibration is verified by the calculation of

percent drift of CCCs. The percent drift of all CCCs must be < 20%.

A system performance check must be performed to ensure that minimum average RF's

are met before the calibration curve is used. SPCC's typically have very low RFs (0.1-

0.2) and do tend to decrease in response as the chromatographic system begins to

deteriorate or the standard goes bad. They are usually the first to show poor

performance. Therefore, they must meet the minimum requirement when the system is

calibrated.

Daily GC/MS Calibration

Prior to analysis of samples, the GC/MS tuning standard must be analyzed. The meeting of tuning

criteria must be demonstrated prior to each 12-hour shift.

A calibration standard at the mid-level concentration containing all analytes, including all required

surrogates, must be performed prior to every 12-hr shift. If duplicate calibration standards are

analyzed, both must be evaluated and reported.

System Performance Check Compounds: A system performance check must be made prior to every

12-hr shift. If the SPCC criteria are met, a comparison of response factors is made for all

compounds. This is the same check that is made during the initial calibration step. If the minimum

response factors are not met, the system must be evaluated, and corrective action must be taken

before sample analysis begins. Some possible problem areas are standard degradation, inlet port

contamination, head of column contamination, or active sites in the chromatographic system. This

check must be met before analysis begins.

Calibration Check Compounds: After the system performance check is met, CCC's are used to

check the validity of the initial calibration. The percent difference in RF's is calculated for each

CCC. If the %D for each CCC is less than 20%, the initial calibration is assumed to be valid. If the

criteria is not met for any CCC (>20% difference), corrective action must be taken. If no source of

the problem can be determined after corrective action has been taken, a new six-point curve must be

generated. This criterion MUST be met before sample analysis begins.

The internal standard response and retention times in the calibration check standard must be

evaluated immediately after or during data acquisition. If the retention time for any internal

standard changes by more than 30 sec. from the last calibration check (12 hr), the chromatographic

system must be inspected and adjustments made as necessary. If the area for any internal standard

base ion has changed by more than a factor of two (-50% to +100%) from the last daily calibration

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standard check, the mass spectrometer must be inspected for malfunctions and corrections must be

made, as appropriate.

10.3.4 Gas Chromatographs (GC)

For each Analyte of interest, prepare calibration standards at a minimum of five

concentrations by adding volumes of one or more stock standards of a volumetric flask

and diluting to volume with an appropriate solvent. One of the external standards should

be at a concentration near, but above, the method detection limit. The other

concentrations should correspond to the expected range of concentrations found in real

samples or should define the working range of the detector. (See Tables 2-4)

Inject each calibration standard using the technique that will be used to introduce the actual samples

into the gas chromatograph (e.g. 2-5 L injections, purge-and-trap, etc.). Tabulate peak height or

area responses against the mass injected. The results can be used to prepare a calibration curve for

each analyte. Alternatively, for samples that are introduced into the gas chromatograph using a

syringe, the ratio of the response to the amount injected, defined as the calibration factor (CF), can

be calculated for each analyte at each standard concentration. If the percent relative standard

deviation (%RSD) of the calibration factor is less than 20% over the working range, linearity

through the origin can be assumed, and the average calibration factor can be used in place of a

calibration curve.

*For multi response pesticides/PCB's, use the total area of all peaks used for quantitation.

The working calibration curve or calibration factor must be verified on each working day by the

injection of one or more calibration standards. If duplicate calibration standards are analyzed, both

must be evaluated and reported. The frequency of verification is dependent on the detector.

Detectors, such as the electron capture detector, that operate in the sub-nanogram range are more

susceptible to changes in detector response caused by GC column and sample effects. Therefore,

more frequent verification of calibration is necessary. The flame ionization detector is much less

sensitive and requires less frequent verification. If the response for any Analyte varies from the

predicted response by more than 15%, a new calibration curve must be prepared for that Analyte,

if quantitation takes place.

Percent Difference = R1-R

2

R1

X 100

Where: R1 = Calibration Factor from the initial curve.

R2 = Calibration Factor from succeeding analyses of the CCV.

Calibration Factor Total Area of Peak

concentration of the standard

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Retention Time Windows

Before establishing windows, make sure the GC system is within optimum operating conditions.

Make three injections of all single component standard mixtures and multi-response products (i.e.

PCB's) throughout the course of a 72 hour period. Serial injections over less than a 72 hour period

result in retention time windows that are too tight.

Calculate the standard deviation of the three retention times (use any function of retention time;

including absolute retention time, or relative retention time) for each single component standard.

For multi-response products, choose one major peak from the envelope and calculate the standard

deviation of the three retention times for that peak. The peak chosen should be fairly immune to

losses due to degradation and weathering in samples.

Plus or minus three times the standard deviation of the retention times for each standard will be

used to define the retention time window; however, the experience of the analyst should weigh

heavily in the interpretation of the chromatograms. For multi-response analytes (i.e. PCB's), the

analyst should use the retention time window, but should primarily rely on pattern recognition.

In those cases where the standard deviation for a particular standard is zero, substitute the standard

deviation of a close eluting, similar compound to develop a valid retention time window.

10.3.5 Graphite Furnace Atomic Absorption (GFAA) Gaseous Hydride Atomic Absorption

(GHAA) and Atomic Absorption (AA)

Instruments are calibrated before each sample run using a calibration blank and at least

three standards. Calibration standards are prepared from NIST traceable sources.

Calibration standards for trace level analyses must be prepared daily.

TECHNIQUE

CCV CRITERIA

CCV

FREQUENCY

ICV CRITERIA

LINEARITY

WATER

SOIL

WATER

SOIL

GHA*/AA/GFAA

90-110

80-120

10%

90-110

(95-105)

for GFAA

90-110

r 0.995

10.3.6 Continuous Flow Instruments

A minimum of three (3) standards and a blank must be used for initial calibration. A set

of initial calibration standards must be analyzed for each analytical run. Linearity

criteria is set at r 0.995. An external calibration standard must be analyzed to verify

the accuracy of the working stock standard and the calibration curve. The CCV and ICV

% recovery criteria is set at 90-110%. Frequency of calibration verification is 10%.

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PAGE 10-7

10.3.7 SPECTROPHOTOMETERS

A minimum of three (3) standards and a blank must be used for initial calibration. A set

of initial calibration standards must be analyzed for each analytical run. Linearity

criteria is set at r 0.995 and/or %RSD 20%. An external calibration standard must

be analyzed to verify the accuracy of the working stock standard and the calibration

curve. This external calibration standard, the ICV, must be within 10% of the known

value. If this criteria is met, sample analysis can commence. CCV's must be analyzed at

a 10% frequency and must meet the same accuracy criteria as the ICV. Wavelength

checks are done on a semi-annual basis.

10.3.8 pH Meters

All pH meters are calibrated before each use using two buffer solutions. If acidic

samples are to be measured, buffer solutions pH-4 and pH-7 are used while buffer

solutions pH-7 and pH-10 are used to calibrate for basic samples. Buffers are to be

discarded after use. Accuracy requirement is set at known value 0.05 pH units.

10.3.9 Specific Ion Meter

The specific ion meter is calibrated before each use using appropriate traceable EPA

standards. Two calibration standards are used to establish calibration range.

Recalibration must be done if sample concentrations fall outside the calibration range.

Accuracy and frequency criteria are set at 90-110% and 10% respectively.

10.3.10 Ion Chromatograph

A minimum of three (3) standards and a blank must be used for initial calibration.

Linearity criteria is set at r 0.995. An external calibration standard must be analyzed

to verify the accuracy of the working stock standard and a calibration curve. This

external calibration standard, the ICV, must be within 10% of the known value. If this

criterion is met, sample analysis can commence. CCV's are analyzed at the beginning of

each workday and at a 10% frequency. When the CCV criterion of 10% recovery of

the known value is exceeded, corrective action procedures must be initiated.

10.3.11 Mercury by Cold Vapor

A minimum of a blank and five standards must be used to generate an initial calibration

curve. Linearity criteria is set at r 0.995. A calibration curve should be prepared for

every hour of continuous sample analysis.

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PAGE 10-8

METHOD

ICV CRITERIA

CCV CRITERIA

CCV

FREQUENCY

7470

95-105% Recovery

90-110% Recovery

10%

7471

90-110% Recovery

80-120% Recovery

10%

10.3.12 Balances

Two (2) S-1 class weights are used for daily calibration of each top-loading and

analytical balance. The S-1 class weights are calibrated every two years. Acceptable

ranges are noted on each respective Balance Logbook. The Balances Annual calibration

service is conducted by Watson Brothers.

10.3.13 Thermometers

Thermometers are calibrated against a reference thermometer on an annual or quarterly

basis. Thermometers are compared at the temperature of working thermometer use. See

the thermometer calibration SOP for details. The reference thermometer calibration is

verified annually.

10.3.14 Micro-Pipettes

Each micro-pipette is calibrated for each day of use. The calibration process involves a

gravimetric check of water delivered at specified volumes. See the QA Protocols

Manual for details.

10.3.15 Auto-Diluters

Quarterly calibration is conducted on each auto-diluter by QA personnel. Calibration

involves weighing water delivered at specific speeds and volumes on an analytical

balance. Data is processed to verify the best case scenario for each dilution scheme and

verify diluter performance.

10.4.1 Measurement quality objectives for laboratory measurements

Group Parameter Accuracy Precision Recovery Target

Reporting

Limits

Completeness

Water quality and

stormwater quality –

First Flush, Urban

Watch

Nitrates as N 80 – 120% + 10% 90 – 110% 0.1 mg/L 90%

Water quality and


Ortho-

phosphate as P

90 – 110% +10% 90 – 110% 0.02 mg/L 90%

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PAGE 10-9

Group Parameter Accuracy Precision Recovery Target

Reporting

Limits

Completeness

First Flush, Urban

Watch

Water quality and


First Flush, Urban

Watch

Turbidity NA NA NA 0.1 NTU 90%

Water quality and


First Flush, Urban

Watch

Ammonia as N 90 – 110% + 10% 90 – 110% 0.05 mg/L 90%

Water quality and


First Flush, Urban

Watch

Metals (200.8)

Cu

Ni

Pb

Zn

70 – 130% + 20% 85 – 115% Various 85%

Water quality and


First Flush, Urban

Watch

TDS NA + 10% 90 – 110% 10 mg/L 90%

Water quality and


First Flush, Urban

Watch

TSS NA + 10% NA 0.5 mg/L 90%

Water quality and


First Flush, Urban

Watch

Residual

Chloride

NA + 10% NA 0.1 mg/L 90%

Water quality and


First Flush, Urban

Watch

1664 Oil &

Grease

78 – 114% + 18% 78 – 114% 5 mg/L 80%

Water quality Nitrates as N 80 – 120% + 10% 90 – 110% 0.1 mg/L 90%

Water quality Ortho-

phosphate as P

90 – 110% +10% 90 – 110% 0.02 mg/L 90%

Water quality Total nitrogen NA NA NA NA Calculation

Water quality Organic

nitrogen

NA NA NA NA Calculation

Water quality Ammonia-

nitrogen

90 – 110% + 10% 90 – 110% 0.05 mg/L 90%

Water quality Total Kjeldahl

nitrogen

80-120% + 20% 80-120% 0.2 mg/L 80%

Water quality Nitrite as NO2 90 – 110% + 10% 90 – 110% 0.17 mg/L 90%

Water quality Total

phosphorous

80-120% + 20% 80-120% 0.05 mg/L 80%

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PAGE 10-10

10.4.2 Laboratory Analytical Methods

Analyte/

Instrumentation

Laboratory /

Organization

Project Action

Limit (units,

wet or dry

weight)

Project

Quantitation

Limit (units,

wet or dry

weight)

Analytical Method Achievable Laboratory Limits

Analytical

Method/ SOP

Modified

for Method

yes/no

MDLs (1)

Method (1)

Nitrate as N

(Dionex DX-100

IC) for First Flush,

Water Quality and

Urban Watch

BC Labs

Inc.

Based on

concentration

level

0.1 mg/L EPA Method

300.0

No 0.014 mg/L 0.1 mg/L

Orthophosphates as

P(Kone 1) for First

Flush, Water

Quality and Urban

Watch

BC Labs Inc Based on

concentration

level

0.02 mg/L SM 4500-P E No 0.0041 mg/L 0.02 mg/L

Turbidity for Water

Quality


concentration

level

0.1 NTU SM 2130B No 0.1 NTU 0.1 NTU

Ammonia as N

(Smart-Chem)

BC Labs

Inc.

Based on

concentration

level

0.05 mg/L SM-4500-D No 0.025 mg/L 0.05 mg/L

Dissolved Metals:

Metals (200.8)

ICP_MS

Cu, Ni, Pb, Zn

BC Labs Inc NA NA EPA-200.8 No Cu – 0.35 µg/L

Ni – 0.14 µg/L

Pb – 0.16 µg/L

Zn – 1.6 µg/L

Cu – 2.0 µg/L

Ni – 2.0 µg/L

Pb – 1.0 µg/L

Zn – 5.0 µg/L

TDS BC Labs Inc Based on

concentration

level

10 mg/L SM2540C No 10 mg/L 10 mg/L

TSS BC Labs

Inc.

Based on

concentration

level

0.5 mg/L SM2540D No 0.5 mg/L 0.5 mg/L

Residual Chloride BC Labs Inc Based on

concentration

level

0.1 mg/L SM4500-C/G No 0.1 mg/L 0.1 mg/L

1664 Oil & Grease BC Labs Inc Based on

concentration

level

5 mg/L EPA1664 No 1.4 mg/L 5 mg/L

Total Kjeldahl

nitrogen


concentration

level

0.2 mg/L EPA 351.2 No 0.056 mg/L 0.2 mg/L

Total nitrogen BC Labs Inc NA NA NA NA Calculation Calculation

Organic nitrogen BC Labs Inc NA NA NA NA Calculation Calculation

Nitrite as NO2 BC Labs Inc Based on

concentration

level

0.17 mg/L EPA 353.2 No 0.0048 mg/L 0.17mg/L

Total phosphorous BC Labs Inc Based on

concentration

level

0.05 mg/L EPA 365.4 No 0.016 mg/L 0.05mg/L

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PAGE 10-11

10.4.3 Analytical QC for water quality, stormwater and Urban Watch monitoring

Matrix: Water

Sampling SOP: BCGEN048,BCGEN051, BCGEN014,

BCGEN061, BCMET037, BCGEN013, BCGEN022,

BCGEN010, BCORG026, BCGEN059, BCGEN060,

BCGEN058

Analytical Parameter(s): Nitrates as N, orthophosphates as

P, TDS, TSS, oil & grease, dissolved metals, turbidity,

residual chlorine, ammonia-nitrogen, TKN, Nitrite as N,

Total Phosphorus

Analytical Method/SOP Reference: Nitrate (EPA 300.0),

Orthophosphates (SM 4500-P E), TDS (SM2540C), TSS

(SM-4500-D), Oil & Grease (EPA1664), Dissolved Metal

(EPA 200.8). Turbidity (SM 2130B), Residual

Chloride(SM4500-C/G), Ammonia Nitrogen(SM4500-

NH3D), TKN (EPA 351.2), Total Phosphorous (EPA

365.4), Nitrite as N (EPA 353.2).

# Sample locations: Various

Laboratory QC Frequency/Number Acceptance Limits

Method Blank One per batch < TRL

Reagent Blank One per new lot < TRL

Storage Blank NA

Instrument Blank: Dissolved

metals

One per day of analysis < TRL

Lab. Duplicate

One per batch or one per 10

samples

Orthophosphates: RPD ≤ 10%

Nitrates: RPD < 10%

Turbidity: < 10%

TDS: RPD ≤ 10%

TSS: RPD < 10%

Metals (200.8): < 20%

Residual Chlorine: RPD ≤ 10%

1664 Oil & Grease: RPD < 18%

Ammonia as N: < 10%

Lab. Matrix Spike One per batch or one per 10

samples

Orthophosphates: recovery 90-110%

Nitrates: recovery 80-120%

Turbidity: NA

TDS: NA

TSS: NA

Metals (200.8): recovery 70-130% RPD

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PAGE 10-12

Residual Chlorine: NA

1664 Oil & Grease recovery 78-114%: RPD

Ammonia as N Recovery 90-110%: RPD ≤ 10%

Matrix Spike Duplicate One per batch or one per 10

samples

Orthophosphates: 90-110%, RPD ≤ 10%

Nitrates: 80-120%, ≤ 10%

Turbidity: NA

TDS: NA

TSS: NA

Metals (200.8): recovery 70-130% RPD ≤ 20%


1664 Oil & Grease recovery 78-114%: RPD < 18%

Ammonia as N Recovery 90-110%: RPD ≤ 10%

Lab. Control sample One per batch or one per 10

sample

Orthophosphates: 90-110%

Nitrates: 90-110%

Turbidity: NA

TDS: 90-110%

TSS: NA

Metals (200.8): 85-115%


1664 Oil & Grease recovery 78-114%

Ammonia as N: 90-110%

Surrogate NA NA

Internal Standards NA NA

Others: NA NA

10.4.4 Testing, inspection, maintenance of analytical laboratory

Equipment /

Instrument

SOP reference Calibration Description and Criteria Frequency of

Calibration

Responsible

Person

BC Labs: Nutrient

analysis

BC Labs SOP External calibration with 6 standards covering the

range of sample concentrations prior to sample

analysis. At low end, the lowest standard at or near

the MDL. Linear regression > 0.995. Calibration

verification every 10 samples after initial

calibration. Standard source different than that used

for initial calibration. Recovery 90 – 110%.

Nitrate as N

Daily

Ortho-phosphate:

Once per batch

LDI

TDC

BC Labs: Turbidity BC Labs SOP NA NA

Ammonia as N BC Labs SOP External calibration with 6 standards covering the


analysis. At low end, the lowest standard at or

near the MDL. Linear regression > 0.995.

Calibration verification every 10 samples after

initial calibration. Standard source different than

that used for initial calibration. Recovery 90 –

110%.

Daily CDR

Metals (200.8) BC Labs SOP External calibration with 3 standards covering the


Daily PPS

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SECTION X


PAGE 10-13

Equipment /

Instrument


Calibration

Responsible

Person


near the MDL. Linear regression > 0.995.




110%.

TDS BC Labs SOP Sample Duplicate and Laboratory Control

analyzed every 10 samples to confirm system is in

control.

90-110% RML

TSS BC Labs SOP Sample Duplicate and Laboratory Control

analyzed every 10 samples to confirm system is in

control.

10% RML

Residual Chlorine BC Labs SOP NA NA MSA

1664 Oil & Grease BC Labs SOP Sample QC (MS\MSD, LCS & MB) analyzed

every 20 samples to confirm instrument is in

control.

1 per 20 samples JAK

BC Labs: Ammonia

as N




near the MDL. Linear regression r2> 0.995.




110%.

Daily SDU

BC Labs: Total

nitrogen








110%.

Daily SDU

BC Labs: Organic

nitrogen








110%.

Daily SDU

BC Labs: Nitrite as

NO2








110%.

Daily SDU

BC Labs: Total

Kjeldahl nitrogen



Daily SDU

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PAGE 10-14

Equipment /

Instrument


Calibration

Responsible

Person






110%.

BC Labs: Total

phosphorous








110%.

Daily SDU

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SECTION X

REVISION NO. 26


PAGE 10- 15

Table 2 Cont. 500 Series Semi-Volatile Organics

Revision Date: 04/15/11 SGB

Method Parameters

Method

HT

days

ICC/IC

V <%

Rsd

CCV

<%

Diff

Solvent

used

Exch.

sol.

Conc.

vol

(mls)

Conc.

Type

Detector

Type

Inst

ID

# Smps

per QC

LPC

y/n

CCV TIme

RUN

HT

Comments

504.1

14

20/30

30

Hex

None

2

none

ECD

GC-4

10

y

12Hrs/10Smp

1

LPC is an MDL check

standard

508 7 20/20 20 MeCl MTBE 10 Turbo ECD GC-1 10 y 8Hrs/10Smp 14

515.1

14

20/20

20

MeCl

10

Turbo

ECD

GC-8

10

y

8Hrs/10Smp

28

507/525.2

14**

30/30

30

MeCl

MTBE

1

Turbo

GC-MS

MS-B3

20

Tune

12Hrs

30

SPE

547

14

10/15

20

None

None

DInj

.

None

FLUOR

10

y

8Hrs/10Smp

-

548

7

30/20

20

SPE

None

1

N-

Evap

GC-MS

10

n

8Hrs

14

549.1 7 20/20

20 SPE None

None

10

None

UV

10

Tune

n

8Hrs/10Smp

21

Int. Std >70% last CCV

& >50% of ICC

** If Diazinon is an analyte HT is 7 days.

Laboratory Performance Check

Sensitivity

Column Performance

Column Resolution

Breakdown

508

515.1

Chlorpyrifos

0.002ppm

Dinoseb 0.004ppm

DCPA 0.05 ppm

0.8 < PGF < 1.15

4-Nitrophenol 1.6 ppm

0.7 < PGF < 1.05

Chlorothalonil & D-BHC

R > 0.5

4-Nitrophenol & 3,5-Dichlorobenzoic acid

R > 0.4

Endrin < 20%

pp=-DDT < 20%

None

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REVISION NO. 26


PAGE 10- 16

Legend

DInj = Direct Injection

ECD = Electron Capture Detector

SPE = Solid Phase Extraction

Turbo = Turbovap

NEvap = Nitrogen Evaporation

Fluor = Fluorescence Detector

UV = UltraViolet Detector

Tune = Tuned to DFTPP Method Criteria

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SECTION X

REVISION NO. 26


PAGE 10- 17

Table 3 Cont. 8000 Series Semi-Volatile Organics

Revision Date: 7/12/04 SGBSW-846 Update 4

Method Parameters

Method

Semi-Volatile

Compounds

HT

days

W/S

ICC/ICV

<% Rsd

CCV

<%

Diff

Solven

used

Exchange

solvent

Conc.

vol(mls)

Conc.

Type

Detector

Type

Inst ID

CCV

Freq.

LPC

y/n

#

Smps

QC

RUN

HT

Comments

8015M

8080A/8081

A/8082

8140/8141A

8150B/8151A

8310

8270C

Diesel Range

Organochloride

pesticides

Organophosphorus

pesticides

Chlorinated acid

herbicides

PAH=s

BNA

14/14

7/14

7/14

7/14

7/14

7/14

20/15

20/15

20/15

20/15

20/15

15/20

15

15

15

15

15

20

MeCl

MeCl

MeCl

MeCl

MeCl

MeCl

None

Hex

Hex

Hex

1:1ACN/OFW

None

5

10

5

10

4

1

Turbo

Turbo

Turbo

Turbo

K-D

K-D

FID

ECD

TSD

ECD

Fluor/UV

GC/MS

GC-2, 5,12,13

GC-1,14,15

GC-7

GC-8

HPLC-14

MS-B1,B2,B4,B5

10smp

10smp

10smp

10smp

10smp

12Hrs

n

y

n

n

n

Tune

20

20

20

20

20

20

40

40

40

40

40

40

DDT/Endrin

Breakdown

<15%

ICC: If %

RSD >15, use

best fit

regression

Semi-Volatile Mass Spectrometry Tune/CCV Requirements

Method: 8270C

Tuning Compound: Decafluorotriphenylphosphine (DFTPP) LPC Requirements:

Tune Frequency: Every 12 Hr Shift DDT Breakdown: <20%

CCV Frequency: Every 12 Hr Shift Pentachlorophenol: Normal response

Internal Standard Requirements: Benzidine: Normal response

EICP area: (-50% to +100%) of last daily CCV Peak tailing:

Retention time: <30 sec. from last daily CCV (within 12 Hrs) Pentachlorophenol PGF <5.0

CCC Requirements: %RSD of ICC: <30% Benzidine PGF <3.0

% D of CCV: <20%

Compounds: Acenaphthene Fluoranthene 2-Nitrophenol Di-n-Octylphthalate

1,4-Dichlorobenzene Benzo(a)pyrene Phenol

Hexachlorobutadiene 4-Chloro-3-methylphenol Pentachlorophenol

N-Nitrosodiphenylmine 2,4-Dichlorophenol 2,4,6-Trichlorophenol

SPCC Requirements: N-Nitroso-di-n-propylamine RF>0.050

Hexachlorocyclopentadiene RF>0.050 Surrogate Requirements: See established limits

2,4-Dinitrophenol RF>0.050

4-Nitorphenol RF>0.050

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SECTION X

REVISION NO. 26


PAGE 10- 18

8000 Series Organics Legend

Tune = Tuned to DFTPP (8270B) and BFB (8240B & 8260A) Method Criteria

ECD = Electron Capture Detector

FID = Flame Ionization Detector

TSD = Thermionic Specific Detector

Fluor = Fluorescence Detector

UV = Ultraviolet Detector

ELCD = Electrolytic Conductivity Detector

PID = Photo Ionization Detector

EICP = Extracted Ion Current Profile

Turbo = Concentrated by Turbovap

K-D = Concentrated by Kuderna-Danish apparatus

BNA = Base neutral acid extractables

PAH=s = Polynuclear Aromatic Hydrocarbons

ICC = Initial Calibration Curve

ICV = Initial Calibration Verification

CCV = Continuing Calibration Verification

CCC = Calibration Check Compound

SPCC = System Performance Check Compound

PGF = Peak Gaussian Factor

LPC = Laboratory Performance Check

RF = Response Factor

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SECTION X

REVISION NO. 26


PAGE 10- 19

Table 4 Cont. 8000 Series Volatile Organics

Revision Date: 04/08/11 SGBSW-846 Update 4

Method Parameters

Method

Volatile

Compounds

HT

days

W/S

ICC/ICV

<% Rsd

CCV

<%

Diff

Detector

Type

Inst ID

#

Smps

per

QC

CCV

Freque

ncy

Tune

Comments

8020A/8021B

8015M

8260B

Aromatic

Gasoline

Range

Various

7/14

7/14

7/14

20/15

20/15

15/30

15

15

20

PID

FID

GC-MS

GC-V4 - V8

GC-V4 - V8

MS-V2-MS-

V7, MS-V10,

V12, V13

20

20

20

10 Smp

10 Smp

12Hrs

N

Tune

ICC: If % RSD>15, use best fit regression

ICC: If % RSD>15, use best fit regression

Volatile Mass Spectrometry Tune/CCV Requirements

Method: 8240B Method: 8260B

Tuning Compound: 4-Bromofluorobenzene Tuning Compound: 4 -Bromofluorobenzene

Tune Frequency: Every 12 Hr Shift Tune Frequency: Every 12 Hr Shift

CCV Frequency: Every 12 Hr Shift CC V Frequency: Every 12 Hr Shift

Internal Standard Requirements: Internal Standard Requirements:

EICP area: (-50% to +100%) of last daily CCV EICP area: (-50% to +100%) of last daily CCV

Retention time: <30 sec. from last daily CCV (within 12 Hrs) Retention time: <30 sec. from last daily CCV (within 12 Hrs)

CCC Requirements: %RSD of ICC: <30% CCC Requirements: %RSD of ICC: <30%

% D of CCV: <20% % D of CCV: <20%

Compounds: 1,1-Dichloroethene Toluene Compounds: 1,1-Dichloroethene Toluene

Chloroform Ethylbenzene Chloroform Ethylbenzene

1,2-Dichloropropane Vinyl Chloride 1,2-Dichloropropane Vinyl Chloride

SPCC Requirements: Chloromethane RF>0.300 SPCC Requirements: Chloromethane RF>0.100

1,1-Dichloroethane RF>0.300 1,1-Dichloroethane RF>0.100

Bromoform RF>0.100 Bromoform RF>0.100

1,1,2,2-Tetrachloroethane RF>0.300 1,1,2,2-Tetrachloroethane RF>0.300

Chlorobenzene RF>0.300 Chlorobenzene RF>0.300

Surrogate Requirements: See established limits Surrogate Requirements: See established limits

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SECTION X

REVISION NO. 26


PAGE 10- 20

8000 Series Organics Legend

Tune = Tuned to BFB Method Criteria

ELCD = Electrolytic Conductivity Detector

FID = Flame Ionization Detector

PID = Photo Ionization Detector

ICC = Initial Calibration Curve

ICV = Initial Calibration Verification

CCV = Continuing Calibration Verification

CCC = Calibration Check Compound

SPCC = System Performance Check Compound

EICP = Extracted Ion Current Profile

LPC = Laboratory Performance Check

RF = Response Factor

Note: This section has been Reviewed on 01/08/2016 (No Changes were made)

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ANALYTICAL PROCEDURES

SECTION XI

REVISION NO. 22


PAGE 11-1

11.0 ANALYTICAL PROCEDURES

BC Laboratories, Inc. conducts approved methodologies which have been promulgated by Federal and State legislators,

and ASTM and in-house methods for non-regulated analyses.

References

Drinking Waters - 40 CFR Parts 131, 143 Methods for the Determination of Metals in Environmental

Samples(EPA/600/R-94/111, May 1994, Methods for the Determination of Inorganic Substances in Environmental

Samples (EPA/600/R-93/August 1993), Methods for the Determination of Organic Compounds in Drinking Water

(EPA/600/4-88/039, EPA/600/4-90/020), Methods for the Chemical Analyses of Water and Wastewater (EPA-600 4-79-

020), and Standard Methods for the Examination of Water and Wastewater, 18th Edition (1992), Standard Methods for

the Examination of Water and Wastewater, 19th Edition.

Waste waters - 40 CFR Part 136, Standard Methods for the Examination of Water and Wastewater, Methods for the

Chemical Analyses of Water and Wastewater, Methods for the Determination of Metals in Environmental Samples

(EPA/600/R-94/111, May 1994), Methods for the Organic Chemical Analysis of Municipal and Industrial Wastewater.

Soils, sludges, wastewater, hazardous waste, and solids - SW-846 Federal Register Test Methods for Evaluating Solid

Waste Physical/Chemical Methods, Third Edition, Update I, II, & III.

Fuels - LUFT Manual, State Water Resources Control Board and the SB 1764 (1994) Advisory Committee.20

Each method has been outlined in respective laboratory standard operating procedures (SOP's). Information such as

procedural steps for conducting analysis, standard and reagent preparation, documentation, safety, and quality control are

included in each analytical SOP. Refer to Appendix A for listing of SOP=s. Table 5-7 list methods conducted on-site.

11.1 SOP CREATION

Department Supervisor's, the Technical Director, and/or the QA Officer will determine the person(s) responsible

for SOP creation, and then delegate the task. The template below will be used as guidance for analytical SOP's:

SOP TEMPLATE

1.0 SCOPE AND APPLICATION

2.0 SUMMARY OF METHOD

3.0 INTERFERENCE AND THEIR CORRECTIVE ACTION

4.0 APPARATUS AND MATERIALS

4.1 APPARATUS

4.2 INSTRUMENT PARAMETERS

5.0 REAGENTS AND STANDARD SOLUTIONS

5.1 REAGENTS - NAME AND SOURCE

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5.2 SOLUTIONS - DILUTION SCHEMES

5.3 WORKING STANDARDS

5.4 SPIKES

6.0 SAMPLE COLLECTION, PRESERVATION AND HANDLING

7.0 PROCEDURE

8.0 QUALITY CONTROL

8.1 DETERMINATION OF IDL, MDL, AND PQL

8.2 METHOD BLANKS

8.3 QC SETS - DUPLICATES & SPIKES

8.4 CONTROL CHARTS

8.5 LOG BOOKS

9.0 CALCULATIONS

10.0 FORMS

10.1 QC SHEET

10.2 OTHER FORMS

11.0 METHOD PERFORMANCE

12.0 GENERAL MAINTENANCE

13.0 WASTE MANAGEMENT

14.0 POLLUTION PREVENTION

15.0 SAFETY

16.0 REFERENCES

Non-analytical SOP=s do not follow a standard format, however these documents should contain sufficient detail to

ensure processes can be carried out completely and competently. Non-analytical SOP=s should contain but are not

limited to the following selections: Scope and Application, Summary of Method, Materials, Procedure, Forms and

References. When completed by the responsible party, the SOP is entered into the LIMS via the word processor.

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SOP identification will be by method number, technique, and a laboratory/department sequential numbering

identification (i.e., BCGEN001, BCGEN002 ...etc.). The word processing specialist will return the SOP to the

author for corrections. When corrections are completed, the SOP will be reviewed by the Department Supervisor.

When the supervisor review and correction phase is complete, the QA Officer will conduct a final review and

approval.

11.2 CONTROL OF SOP'S AND LOGBOOKS

In order to receive a copy of an SOP, a request must be made to the QA officer, Department Supervisor, or

Technical Director. One of these persons will inform the word processor specialist to generate the requested SOP.

Records pertaining to SOP retrieval will be kept by the word processor.

Record: SOP ID.

File Name

Issued To

Received by

Revision Number

Controlled Copy Number

Date Issued

SOP Location

Relinquished by

The SOP will be generated with an approval by the word processing specialist. Logbooks requests are honored by

the Word Processing Specialist. Logbook request sheets are located at the word processing station. Once a

logbook is created, the Word Processing Specialists records the following information:

QC Tracking Number

WPS Tracking Code

Logbook Name

Logbook Number

Issued To

Date of generation

Relinquished by

Accepted by

The Word Processing Specialist will then review the logbook and acknowledge final approval by initialing and

dating the logbook cover.

11.3 DEPARTURE FROM SOP

In cases where it is necessary to depart from standard practice, approval must be granted by the department

supervisor and the Quality Assurance Officer. Departures for standard procedures must be documented on all

affecting final reports.

11.3.1 Documentation - Document nonstandard practice on affecting worksheet(s). Client notification must be

made and documented before departure can be granted. Affected final reports must have a comment

which alludes to the modification of method.

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11.3.2 Approvals from the client must be verified in order to close the deviation of standard practice.

11.4 ASSESSMENT AND HANDLING OF NEW/ADDITIONAL WORK

11.4.1 Summary

Project information must be legible and obtained in a timely fashion to allow necessary modifications to be

made prior to projects initiation. Information is obtained from QAPPs, SAPs, CDAPs, or subsets of the

aforementioned formats, or from projects initiation forms completed by laboratory interviewers. The

information is translated into the appropriate language then discussed through supervisor meetings.

Discussion topics:

* Confirmation of amount of new/additional work

* Baseline capacities

* Potential capacities

* Labor

* Instrumentation

* Certification/Methods

* Materials

* Implementation

* Monitoring

* Responsibilities

* Deliverables

Once discussed, accommodations addressing pertinent concerns are made in each department. The Project

Manager verifies that all project specific work requirements are secured; especially all non-routine tasks. Project

Initiation Forms are then completed and distributed to affecting department supervisors, and if possible, to

pertinent clients before initiation of sampling. Performance monitoring will be conducted by the QA/QC

Department to measure compliance with project specifications and customer satisfaction.

The LIMS will act as the tool used to confirm analytical capabilities.

11.4.2 Responsibilities

Sales and Marketing

1. Obtain project deliverables information

2. Confirm the amount of work and compare to the capability/capacity of the laboratory

3. Confirm type of work (DOD, DOE, RCRA, CERLA, etc)

4. Monitor project quotes

5. Establish probabilities of project awards

6. Identify project initiation date

7. Obtain project method specifications

8. Obtain quality goals

9. Act as liaison between laboratory and client until award is granted

10. Submit all pertinent information to Client Services Department

Project Coordinator

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1. Obtain project information from Sales and Marketing or client.

2. Translate project information.

3. Assign projects to project managers.

4. Provide guidance in project handling.

5. Provide guidance on completing Project Checklist Form.

Project Manager

1. Gather project information into a Project Initiation Form.

2. Distribute project initiation forms.

3. Modify project initiation forms as needed.

President

1. Facilitate brainstorm sessions.

2. Allocate resources.

3. Approve laboratory system modifications.

4. Approve instrumentation purchases.

5. Approve labor allowances.

6. Secure and allocate resources.

7. Approve purchases of materials and instruments.

Department Manager

1. Assess department capacities.

2. Review and approve prospective work.

3. Coordinate with project coordinator.

4. Initiate IDCs or IDPs for new analysts and/or methods.

QA Officer

1. Monitor performance.

2. Provide method guidance.

LIMS Manager

1. Write programs to handle project specific requirements.

2. Update, increase, and modify LIMS capabilities.

11.4.3 Procedure

Sales and Marketing representative produces bid packages then rates the probability of an award by

obtaining information through contracts and/or correspondence with bid proprietors. When awards are

confirmed, a request for project information is made, if not already available in RFPs or RFQs, by a

representative of Sales and Marketing or the Project Coordinator. The Project Coordinator gathers all project

information then translates this information into BC Laboratories' language. Translation will be discussed

during supervisor meetings and on a one-to-one basis. A project Quotation Form, which is completed

through the LIMS or by hand, is created then distributed to all pertinent personnel.

11.5 CAPACITY

Capacities are functions based by method, # of instruments, # of analysts, # of work shifts, potential # of

samples analyzed per 8 hour shifts, sample matrix, and baseline levels of continuous work.

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Daily capacity is figured by finding the number of samples which can be analyzed (excluding CCV's,

Curve Stds, blanks, LCS's and MS's) on one instrument by one analyst during an eight hour work shift.

Actual capacity will vary based on time of year, workload, analyst vacations, and instrument configuration

for multiple Analyte analysis, instrument performance, and analyst performance. To adjust this daily

capacity, take the average amount of samples analyzed per year and divide by the number of work days in a

year, then subtract this number from the daily capacity. This will give us available capacity.

Quarterly capacity will be assessed more accurately detailing available capacity during high workload periods.

This can be found by finding the average daily workload during quarterly monitoring periods.

Projected workload is based on number of analyses and turnaround time.

Projected workload = Number of analyses

Turnaround Time (days)

In order to verify if additional workload can be handled, find the daily capacity and/or the quarterly capacity,

projected workload (analyses per day) and place in the following algorithm:

Available capacity - projected workload

If this number is positive, the additional workload can be approved. If negative, available capacity must be

increased through more instrumentation, more labor, and/or modified system changes.

11.6 METHOD QUALIFICATION

Each new method must be pre-qualified prior to use. Prequalification entails meeting reporting and performance

criteria outlined in the ELAP manual AData Package Guidelines@. Further details can be found in the QA Protocols

Manual.

11.7 USE OF NON-STANDARD METHODS

In order to utilize methods which are non-referenceable or deviate significantly from referenced methods, we are

required to obtain client and/or regulatory agency approval. If regulatory approval is needed, the QA Officer will

initiate the process of obtaining method exceptions. Approvals by our clients must be documented in writing on a

record which is recognized by our system. All data associated with non-standard methods should be flagged on

affected final reports.

11.8 USE OF DIFFERENT METHOD VERSIONS

In cases of combined analytical methods, the most stringent requirements for each of the various calibration and

quality control steps must be incorporated in the merged procedure. All instruments are set up to accommodate the

most stringent QC requirements for like methods so reporting can be a function of sample matrix or project method

reporting protocol. Sample results reported under particular methods must be referenced correctly on final reports

either in the heading or in a comments section.

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TABLE 5 METAL METHODOLOGIES

SECTION XI

REVISION NO. 22


PAGE 11-7

METALS

ICP

METHODOLOGY

AA/GHA/CV

METHODOLOGY

GFAA

METHODOLOGY

ICP/MS

METHODOLO

GY Aluminum

EPA 200.7, 6010B,

Antimony

EPA 200.7, 6010B

EPA 200.8/6020

Arsenic

EPA 200.7, 6010B

EPA 200.8/6020

Barium

EPA 200.7, 6010B

EPA 200.8/6020

Beryllium

EPA 200.7, 6010B

EPA 200.8/6020

Boron

EPA 200.7, 6010B

Cadmium

EPA 200.7, 6010B

EPA 200.8/6020

Calcium

EPA 200.7, 6010B

Cobalt

EPA 200.7, 6010B

EPA 200.8/6020

Copper

EPA 200.7, 6010B

EPA 200.8/6020

Chromium

EPA 200.7, 6010B

EPA 200.9

EPA 200.8/6020

Iron

EPA 200.7, 6010B

Lead

EPA 200.7, 6010B

EPA 200.8/6020

Lithium

EPA 200.7, 6010B

EPA 200.8/6020

Magnesium

EPA 200.7, 6010B

Manganese

EPA 200.7, 6010B

EPA 200.8/6020

Mercury

EPA 245.1, SW7471A,

SW7470A

Molybdenum

EPA 200.7,6010B

EPA 200.8/6020

Nickel

EPA 200.7,6010B

EPA 200.8/6020

Potassium

EPA 200.7,6010B

Selenium

EPA 200.7,6010B

EPA 200.8/6020

Silica

EPA 200.7,6010B

Silver

EPA 200.7,6010B

EPA 200.8/6020

Sodium

EPA 200.7,6010B

Strontium

EPA 200.7,6010B

Tin

EPA 200.7,6010B

EPA 200.8/6020

Titanium

EPA 200.7,6010B

Thallium

EPA 200.7,6010B

EPA 200.8/6020

Vanadium

EPA 200.7,6010B

EPA 200.8/6020

Zinc

EPA 200.7,6010B

EPA 200.8/6020

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TABLE 6 ORGANIC METHODOLOGIES

SECTION XI REVISION NO. 22


PAGE 11-8

ANALYSIS

WATER METHODOLOGY

SOIL, OIL, SLUDGE

METHODOLOGY Purgeables (GC)

EPA 8021B, EPA 8015B

EPA 8021B, EPA 8015B

Purgeables (GC / MS)

EPA 524.2, EPA 624, EPA 8240B,

EPA 8260B, EPA 601/602 by GC/MS

EPA 8260B

EDB / DBCP

EPA 504.1

EPA 504M

Pesticides, Herbicides (GC)

EPA 608,EPA 515, EPA 508

EPA 8080A, EPA 8081A, EPA

8082,

EPA 8141A, EPA 8140, EPA 525.2,

EPA 8150B, EPA 8151A Gasoline Residue

LUFT Manual 8015M

LUFT Manual 8015M

Diesel Residue

LUFT Manual 8015M

LUFT Manual 8015M

PCB's

EPA 608, EPA 625

EPA 8082

Phenols

EPA 525.2

EPA 8270C

Title 22

State Method

Priority Pollutants (GC/MS)

EPA 625, EPA 525.2

EPA 8270C

Oil and Grease

EPA 1664

EPA 1664

TPH

EPA 1664

EPA 1664

Pesticides, Herbicides (HPLC),

Carbamates

EPA 632

EPA 632

PAH's

EPA610

EPA 8310

Explosives

EPA8330

EPA8330

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TABLE 7 INORGANIC METHODOLOGIES

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PAGE 11-9

ANALYSIS

WATER METHODOLOGY

SOIL, OIL, SLUDGE

METHODOLOGY Alkalinity

EPA 310.1, SM2320B

Chloride

EPA 300.0

EPA 300.0

Chromium VI

SW 7196A, SM 3500Cr D, 218.6

SW7196A, SW7199

Corrosivity

EPA 150.1

SW9040

Conductivity

EPA 120.1, SM2510B

SW9050

Cyanide

EPA335.1,EPA 335.3, EPA 335.2,

EPA 335.4

SW9012A, SW9010,SECTION 7.3,SW846

Fluoride

EPA 300.0

EPA 300.0

Nitrogen Forms

EPA 350.1, EPA 353.2,SM4500-NH3H

EPA 300.0, EPA 351.2,SM4500-NO3F

EPA 350.1, EPA 353.2,

EPA 300.0, EPA 351.2 Bacteriologicals

SM9215B,SM 9221A,B,C, 9221C,E, 9223

SM 9221B, 9221C,E, SM9215B

D.O.

EPA 360.1, SM4500-OG

N/A

Bromide

EPA 300.0

EPA 300.0

Chlorine Residue

SM 4500CLB F, EPA 330.4

Color

EPA 110.2

N/A

pH

EPA 150.1, SW9040, SW9045,

SM4500H+B, EPA 305.1, SM2310B

SW9045C, SW9040B

Phenols

EPA 420.4

SW9066

Phosphorous

EPA 365.1, EPA 365.4, SM4500PF

Sulfur Forms

EPA 376.1, EPA 376.2, SM4500-S,D,E

SW9030, SW 7.3.4.2

Sulfate

EPA 300.0

EPA 300.0

BOD

EPA 405.1, SM5210B

COD

EPA 410.4, SM5220D

TOC

SM5310C

SW 9060

Residue

EPA 160.1 - SM2540B-SM2540F

MBAS

EPA 425.1, SM5540C

Odor

EPA 140.1

Turbidity

EPA 180.1, SM2130B

Perchlorate

EPA 314.0

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DATA REDUCTION, VALIDATION, AND REPORTING

SECTION XII

REVISION NO. 20

EFFECTIVE DATE: 01/0

PAGE 12-1

12.0 SUMMARY

It is the responsibility of the analyst to conduct initial data reduction procedures by using calculations referenced in State

and Federally recognized methodologies and within respective SOP=s. The tools used to reduce data include Excel

spreadsheets, Dionex AI-450 software, HP Chemstation software, calculators, Enable database software, LIMS

processing programs and instrument programs.

Validation and verification processes include analyst reviews, technical reviews, supervisor reviews, project management

reviews, QA department reviews, data processing checks, and final approvals. See the appropriate flowcharts in

Appendix D.

Results are entered onto laboratory bench worksheets, then introduced into the LIMs via a data processing system . (BC

participates in CLP like projects, which requires raw data from COC to injection log with analytical report. At least 10%

of data packages are reviewed thoroughly by QA/QC officer to ensure integrity of the data. Raw data is verified through

element analytical reports and validated with LIMS statistical data calculations.

12.1 REDUCTION

12.1.1 Organics Department

12.1.1.1 GC/HPLC

Data is processed via HP Chem software reduced by hand if necessary and recorded onto

worksheets. When dual column confirmation is used, it is BC Laboratories policy to report values

from the primary column. However, clients may specify in writing that the higher of the two

confirmed results be reported. The reduced data is electronically transferred to the LIMS. The

LIMS performs statistical calculations (% recoveries % RPD, % found, etc) and sample

calculations.

12.1.1.2. GC/MS

All data is processed and reduced on manufacturer's software. Sample analyses are processed via

data systems enviroquant and Varian's enviropro. Results are then recorded onto worksheets. The

reduced data is electronically transferred to the LIMS. The LIMS performs statistical calculations

(% recoveries % RPD, % found, etc) and sample calculations in test solutions sample weights,

extract volume and sample dilution.

12.1.1.3 TRPH

Data is recorded onto QC bench sheets, reduced by hand, then recorded onto worksheets.

Calibration factors are used in the linear regression model which is used to reduce data. The

reduced data is electronically transferred to the LIMS. The LIMS performs statistical calculations

(% recoveries % RPD, % found, etc) and sample calculations in test solutions sample weights,


12.1.2 Metals Department

12.1.2.1 ICP, ICP/MS, GFAA, AA

Instrument data is reduced on manufacturer's software. All dilutions are accounted for on

laboratory worksheets. The reduced data is electronically transferred to the LIMS. The LIMS

performs statistical calculations (% recoveries % RPD, % found, etc) and sample calculations in

test solutions sample weights, extract volume and sample dilution.

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12.1.2.2 Hg by cold vapor

The method of least squares, using chart line versus concentration, is used as the linear regression

model. Results are reduced onto a QC bench sheet then entered onto worksheet. The reduced

data is electronically transferred to the LIMS. The LIMS performs statistical calculations (%

recoveries % RPD, % found, etc) and sample calculations in test solutions sample weights, extract

volume and sample dilution.

12.1.3 General Chemistries

12.1.3.1 IC

Data is reduced via the use of manufacturer's software. Values are recorded onto a QC

bench sheet then transferred to worksheets. The reduced data is electronically transferred

to the LIMS. The LIMS performs statistical calculations (% recoveries % RPD, % found,

etc) and sample calculations in test solutions sample weights, extract volume and sample

dilution.

12.1.3.2 Meters, titrimetric and gravimetric tests.

Data is recorded onto QC bench sheets then transferred to worksheet. The reduced data is

electronically transferred to the LIMS. The LIMS performs statistical calculations (%

recoveries % RPD, % found, etc) and sample calculations in test solutions sample weights,


12.1.3.3 Optical Analyses

The method of least squares, using chart line versus concentration, is used as the linear

regression model. Results are reduced on QC log sheets then transferred onto worksheets.

The reduced data is electronically transferred to the LIMS. The LIMS performs statistical

calculations (% recoveries % RPD, % found, etc) and sample calculations in test solutions

sample weights, extract volume and sample dilution.

12.1.4 Data acquisition by the LIMS

Methods which have been linked to the LIMS are processed in the following manner:

1) Instrument readings are either hand entered or electronically transferred into the LIMS

2) Review of data entry

3) Data is processed and posted

4) Review of processing

5) A result file is created

The reduced data is electronically transferred to the LIMS. The LIMS performs statistical

calculations (% recoveries % RPD, % found, etc) and sample calculations (final results driven from

Analyte concentration in test solutions sample weights, extract volume and sample dilution.)

Electronic transfer of data is currently used as QC tool by providing parallel reporting. Data from

worksheets supersede electronically processed data unless worksheet data is proven discrepant.

12.1.5 Calculations

12.1.5.1 % Relative Abundance

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Abundance of X

Abundance of Y x 100%

12.1.5.2 Relative Response Factor

RRF = Ax

Ais x

Cis

Cx

Mean Relative Response Factor

RRF =

5

ji=1

RRFi

5

Where: RRFi="i"th Relative Response factor

A = Area of the characteristic ion

C = Concentration

is = Internal standard

x = Analyte of interest

12.1.5.3 Standard Deviation

S =

n

ji=1

(xi x )2

n-1

Where: S = Standard deviation of RRF's

X = Mean of RRF's

X = Sample reading

n = number of samples

12.1.5.4 % Relative Standard Deviation

% RSDSD

RFx

x

100%

Where: RSD = Relative Standard Deviation

RFX = Mean of 5 initial RRF=s for a compound.

SD = Standard Deviation of RRF=s.

12.1.5.5 Percent Difference

%D =

RRFi

- RRFc

RRFi

x 100

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Where: RRFi = average RRF from initial calibration

RRFc = RRF from continuing calibration standard

12.1.5.6 Percent Drift

%( )

DiftC C

Cx

C

1

1

100

Where: C1 = Calibration check compound standard concentration

Cc = Measured concentration using selected quantitation method.

12.1.5.7 Percent Recovery (Surrogates)

%Recovery = Concentrationªamount found

Concentrationªamount spiked x 100

12.1.5.8 Percent Recovery (matrix spikes)

% Recovery = SSR -SR

SA X 100

Where: SSR = Spiked Sample Result

SR = Sample Result

SA = Spike Added

12.1.5.9 Calculations for matrix spike recoveries for non-prepared samples are as

follows:

MSR x y sample result sample result

spike levelx

/

100

Where: MSR = matrix spike result

X = mls of spike

y = total mls (spike + sample)

or,

MSR sample result x y

spike levelx

* /1

100


x = mls of spike


12.1.5.10 Relative percent difference (matrix spikes)

RPD = |MSR -MSDR |

1ª2(MSR +MSDR ) X 100%

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Where: RPD = Relative Percent Difference

MSR = Matrix Spike Recovery

MSDR = Matrix Spike Duplicate Recovery

12.1.5.11 Concentration (waters) volatile. GC/MS

Fgªl = Ax x Is x Df

Ais x RRF x Vo

Concentration (low level soils) volatiles

Fgªkg = Ax x Is

Ais x RRF x Ws x D

Concentration (med level soils) volatiles (dry weight basis)

Fgªkg = Ax x Is x Vt x 1000 x Df

Ais x RRF x Va x Ws x D

Where: Ax = Area of characteristic ion for compound

Ais = Area of characteristic ion for internal standard

Is = Amount of internal standard added (ng)

RRF = Daily relative response factor for compound

Vo = Volume of water purged (mL)

Ws = Weight of sample (g)

D = (100%- Moisture) / 100% - conversion to dry weight (optional)

Vt = Volume of methanol (mL)

Vi = Volume of extract added (l) for purging

Df = Dilution factor

Va = Volume of the aliquot of the methanol extract (l) added to reagent water for

purging.

12.1.5.12 PQL Adjustment

Adjusted PQL = Non-adjusted PQL x sample Df

FgªL = Ax x Is x Vt x Df

Ais x RRF x Vo x D

12.1.5.13 Concentration semi-volatiles (water) GC/MS

FgªL = A

x x I

s x V

t x Df

Ais x RRF x V

o x D

Concentration (soils)

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ICS %R = FoundSolutionAB

TrueSolutionAB x 100

LCS %R = LCS Found

LCS True x 100

Fgªkg = Ax x Is x Vt x Df

Ais x RRF x Vi x Ws x D

Where: Ax = Area of characteristic ion for compound

Ais = Area of characteristic ion for internal standard

Is = Amount of internal standard added (ng)

RRF= Daily relative response factor for compound

Vo = Volume of water purged (mL)

Vi = Volume of extract injected (l)

Vt = Volume of concentrated extract (l)

Df = Dilution factor

D = (100-% Moisture) / 100% - conversion to dry weight (optional)

Ws = Weight of Sample (g)

12.1.5.14 ICV / CCV Recoveries

%R = Found

True x 100

Where: Found = Concentration of Analyte measured in the analysis

True = Concentration of Analyte in ICV or CCV source.

12.1.5.15 ICP Interference Check Sample (ICS)

Where: Found Solution AB = Concentration of Analyte measured in the analysis of solution AB

True Solution AB = Concentration of each Analyte in solution AB

12.1.5.16 Laboratory Control Sample

Where: LCS Found = Concentration (in g/l for aqueous; mg/kg for solid) of each Analyte

measured in the analysis of LCS solution.

LCS True = Concentration (in g/l for aqueous; mg/kg for solid) of each Analyte in the

LCS source.

12.1.6 Manual Integration Policy

1. All lone> 90% baseline peaks are to be integrated valley to valley.

2. All peaks with adjacent peaks < 90% resolved will be integrated baseline to baseline, dropping a

perpendicular at the minimum.

3. All peaks with shoulders will be integrated in the best manner possible. Analyst’s judgment.

(Tangential skim or dropping a perpendicular.)

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4. In a busy Chromatogram, the analyst=s judgment as to the best integration technique will supersede

above.

5. All manual re-integrations are printed and reviewed during the raw data review process.

Acknowledgement of review is either on instrument printouts or technical review sheets.

6. No peak shaving is to be observed or practiced.

7. Manual integrations are documented by the software being use. HP chemstation places an Am@ by

each peak that is manually integrated. The Dionex software states that the run was reprocessed and

the date upon which the reprocess occurred.

8. For DoD projects, peaks that require manual integration will be printed before and after adjustment.

The date, the reason for the manual integration and the signature/initials of the person performing

the manual operation will be noted on the chromatograph. The following flags must be noted on the

manual integration are (B) Baseline Adjustment – moving peak start to end. (P) Peak correction –

misidentification correction and (R) Rider Removal – splitting of secondary peaks or tails. Please

see DoD QSM version4.2, June 2003 for detail.

12.2 VALIDATION

QC parameters to be checked to validate results:

12.2.1 Volatiles (GC, GC/MS)

Holding Times

GC/MS Instrument performance check

Initial Calibration

Continuing Calibration

Blanks

Batching

Surrogate spikes

Matrix spikes/matrix spike duplicate

Laboratory control sample

Internal standards (if applicable)

Compound Identification and Chromatography

Compound Quantitation and reporting limits

Tentatively identified compounds (if applicable)

System performance

Retention Times

Overall assessment of data

12.2.2 Semi-volatiles (GC, GC/MS)

(Same list as volatiles)

12.2.3 TRPH

Holding times

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Initial calibration

Continuing calibration

Blanks

Batching



Quantitation and reporting limits

System performance


12.2.4 Gravimetric Testing

Holding times

Blanks

Batching

Duplicates



System performance


12.2.5 Metals (ICP, GFAA, GHA, AA)

Holding times

Initial calibration


Blanks

Batching

ICP Interference check sample


Duplicate sample

Matrix spike/ matrix spike duplicate

Post spikes (if applicable)


System performance


12.2.6 Metals (Hg)

Holding times

Initial calibration


Blanks

Batching


Duplicate sample


Post spike (if applicable)

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PAGE 12-9


System performance


12.2.7 Metals (ICP-MS)

Holding times

Short-term stability check

Initial calibration


Blanks

Batching

Surrogate spikes

Duplicate



Post spike (if applicable)

Internal standards

Compound Quantitation and reporting limits

System performance


12.2.8 Titrimetric Testing

Holding times

Blanks

Batching

Duplicates

Matrix spikes/matrix spike duplicate (if applicable)



System performance

Overall assessment of data.

12.2.9 Colorimetric Testing

Holding times

Initial calibration


Blanks

Batching

Duplicates




System performance


12.2.10 Ion Chromatography

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SECTION XII

REVISION NO. 20


PAGE 12-10

Holding times

Initial calibration


Blanks

Batching

Duplicates



Compound identification and chromatography

Compound quantitation and reporting limits

Retention Times

System performance


12.2.11 Meter

Holding times

Calibration

Blanks

Batching




System performance


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SECTION XII

REVISION NO. 20


PAGE 12-11

12.3 REPORTING

All reports generated by BC Laboratories include information necessary for proper sample, client identification

and complete result reporting. Report packages include: Cover sheets that contain information pertaining to

sampling procedures and analysis requested; report sheets displaying analytical results, methods used, PQL's,

concentration units and report approval signatures; Chain-of-Custody documents and QC report if requested.

All reports released are:

Complete

Neatly typewritten and presented

Associated with a unique project or lab number

BC Laboratories, Inc. will make all necessary corrections if the above criteria are not met.

Specialized reporting formats are available upon request for specific project requirements.

12.3.1 Reporting Procedures for Qualified Data

12.3.1.1 Holding time exceeded. If holding times are exceeded, qualify results as estimated. Add a

comment to the final report and/or other pertinent deliverables which explains the qualifier.

12.3.1.2 GC/MS Initial Calibration Incompliance - If %RSD is greater than 20.0% and initial

calibration RRF's greater than or equal to 0.05, qualify positive results as estimated, and

non-detected target compounds using professional judgment. If any initial calibration RRF

is less than 0.05, qualify positive results that have acceptable mass spectral identification as

estimated and non-detected analytes as unusable.

12.3.1.3 GC/MS Continuing Calibration Incompliance - If the %D is outside 20.0% criterion and

the continuing calibration RRF is greater than or equal to 0.05, qualify positive results as

estimated. If the %D is outside 20.0% criterion and the continuing calibration RRF is

greater than or equal to 0.05:

Qualify non-detect target compounds as estimated if -20%.

Do not qualify non-detect target compounds if +20%.

12.3.1.4 Blanks Incompliance - If a compound is detected in the sample and in the blank, the sample

result is qualified if the sample concentration is less than ten (10) times the associated PQL.

Report method blank bias for associated sample concentrations >10 times the respective

PQL=s. Results must not be corrected by subtracting any blank value, unless method

references state otherwise.

12.3.1.5 Surrogate Incompliance - If a surrogate has a recovery greater than the upper acceptance

limit, detected target compounds are qualified while results for non-detected target

compounds should not be qualified.

If a surrogate has a recovery greater than or equal to 10% but less than the lower acceptance

limit, detected target compounds are qualified while non-detected compounds quantitation

limits are qualified as approximated.

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REVISION NO. 20


PAGE 12-12

If surrogate recovery is less than 10% and less than the lower acceptance limit, detected

compounds are qualified and non-detected target compounds may be qualified as unusable.

12.3.1.6 Matrix Spike/Matrix Spike Duplicate Incompliance - No action is taken on MS/MSD data

alone unless informed professional judgement is used in conjunction with other QC criteria.

In matrix evaluation, QC acceptance criteria should be used to compare MS/MSD

recoveries to DoD LCS limits. If MS results are outside the LCS limits, data should be

evaluated to determine the source of error and to determine if there is any matirix

interference or analytical error.

12.3.1.7 Laboratory Control Samples Incompliance - Action on the LCS recovery should be based

on both the number of compounds that are outside of the recovery and the magnitude of the

exceedance of the criteria. If the LCS recovery criteria are not met, then the LCS results

should be used to qualify samples data for the specific compounds that are in the LCS

solution. If the LCS recovery is greater than the UCL, then positive results for the

particular compounds should be qualified. If LCS compounds are below associated LCL's,

then affected results should be rated unusable. If more than half the compounds in the LCS

are not within the required recovery criteria, then all of the associated detected target

compounds should be qualified and all associated non-detected target compounds should be

qualified unusable. Please note that the proximity of recoveries to 100% should be

considered in assessment. All of the methods analytes laboratory=s in-house limits are

calculated from the laboratory=s historical data. Laboratory=s in-house limits are established

as part of their quality control system to evaluate trends and monitor laboratory

performance. When laboratory=s in-house limits are outside the DoD limits, laboratory in-

house limits must be reported, even if the LCS of the preparatory batch fall within the DoD

specified limits.

12.3.1.8 Internal Standard Incompliance - If an IS area count is outside -50% or +100% of the area

for associated standard; positive results for compounds quantitated using that IS should be

qualified, non-detected compounds quantitated using an IS area count greater than 100%

should not be qualified, non-detected compounds quantitated using an IS area count less

than 50% are reported with an approximated quantitation limit.

12.3.1.9 Initial Calibration Incompliance (GC) - If %RSD is greater than 20%, qualify all positive

results as estimated and use professional judgment in assessing non-detect target analytes.

12.3.1.10 Continuing Calibration Incompliance - If % diff is greater than 15%, qualify positive

results as estimated. If % diff is less than -15%, qualify positive results as estimated and

approximate the non-detect target analytes quantitation limits. For DOE/DOD work, if

the CCV standard or surrogate analyzed acceptance criteria are high only samples that

are non-detected may be reported. All positive samples affected by unacceptable CCV

will be reanalyzed after a new calibration curve has been established. If the CCVs

surrogate acceptance criteria are low, samples may be reported if they exceed Maximum

Regulatory Limit (MRL). Otherwise, all samples affected by unacceptable CCV will be

reanalyzed after a new calibration curve has been established and accepted. The

surrogate recoveries in the method blank and the instrument blank must be within

criteria for the analytical sequence to be valid.

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REVISION NO. 20


PAGE 12-13

12.3.1.11 Initial Calibration Incompliance (Inorganics) - If the minimum number of standards

were not used for initial calibration, or if the instrument was not calibrated daily and

each time the instrument was set up, qualify the data as unusable. Please note that Ion

Chromatography procedures mandate that an initial curve is validated by continuing

calibration checks. If the correlation coefficient is <0.995, qualify results as estimated.

12.3.1.12 Continuing Calibration Incompliance (Inorganics) - If the CCV or ICV %R falls outside

the acceptance windows, use professional judgement to qualify all associated data.

12.3.1.13 Interference Check Sample - For samples with concentrations of Al, Fe, Ca, and Mg

which are comparable to or greater than their respective levels in the Interference Check

Sample:

1) If the ICS recovery for an element is >120%, qualify detected results.

2) If the ICS recovery for an element falls between 50 and 79%, qualify detected and

non-detected results.

3) If ICS recovery results are <50%, qualify data as unusable.

12.3.1.14 Duplicate Incompliance - If duplicate analysis results for a particular analyte fall outside

the appropriate control windows, qualify the results for that analyte in all associated

samples of the same matrix as estimated.

12.3.1.15 Post Spike Incompliance - If sample absorbance is <50% of the post digestion spike

absorbance then:

1) If the post spike recovery is not within 85-115%, qualify results as estimated.

2) If method of standard additions is required but has not been done, qualify the

sample results as estimated.

3) If MSA spike levels are not appropriate, qualify data, and

4) If MSA correlation coefficient is <0.995, qualify data as estimated.

12.3.2 Use of flags

In cases where data must be qualified, data qualifiers (flags) must be used. Please see Appendix G

for index of flags.

12.4 ROUNDING RULES FOR REPORTING DATA

12.4.1 Significant figure and rounding rules for inorganic=s analyses.

Significant figures are method specific and response specific.

Rounding off numbers is the process of dropping digits that are not significant. In order to round off

a number to a particular place holder (for example, to the nearest 10) one looks at the next smallest

place holder (the 1's place). If the next smallest place holder is a 6, 7, 8 or 9, then increase the

preceding digit by one and drop the digits to the right (if to the right of the decimal) or replace them

with zeros (if to the left of the decimal). If the next smallest place holder is a 1, 2, 3 or 4, then do not

change the preceding digit and drop the digits to the right or replace with zeros. If the next smallest

place holder is a 5 and any number to the right of the 5 is not zero, then treat it as 6, 7, 8 or 9 as

above. If the next smallest place holder is a 5 and all digits to the right of this digit are zero, then

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SECTION XII

REVISION NO. 20


PAGE 12-14

round the preceding digit to the nearest even number (0, 2, 4, 6, 8) and drop the digits to the right or

replace with zeros. Thus, 2.250001 becomes 2.3 and 2.250000 becomes 2.2, and 6.750 becomes

6.8.

When rounding values, do not round off values that have been previously rounded. In other words,

do not round off during a preliminary calculation. Carry as many digits as possible until the final

value has been calculated and then round off as needed.

12.4.2 Significant figure and rounding rules for organic=s analyses.

Two significant figures are used as a rule for organics. Rounding rules are the same as for Inorganics

testing.

Note: This section has been reviewed on 01/08/2016 (No Changes were made)

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ANALYTICAL QUALITY CONTROL REQUIREMENTS

SECTION XIII

REVISION NO. 16


PAGE 13-1

13.0 QC PARAMETERS

Required QC parameters will vary according to method, specific project requirements, and/or sample matrices

encountered.

Table 8 illustrates generalized criteria. QC parameter requirements in specific SOP=s supersede those listed in Table 8.

QC Parameters for Wet Chemistry testing

Sample/Sample Duplicate

Matrix Spike/Matrix Spike Duplicate

Laboratory Control Sample-Water or Solid

Method Blank

Exceptions:

pH, EC, TDS


Laboratory Control Sample

TSS, Settleable Solids


QC Parameters for Metals testing



Laboratory Control Sample-Water or Solid

Method Blank

Post Spike

QC Parameters for Organics testing



Method Blank

Surrogate

Exceptions:

Oil and Grease, Total Recoverable Petroleum Hydrocarbons




Method Blank

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SECTION XIII

REVISION NO. 16


PAGE 13-2

13.1 BATCHING

A group of samples of similar matrix that behave similarly with respect to the procedures being employed.

The number of samples in a batch may never exceed 20, (consult SOP to verify maximum batch size). All

samples in a batch must be processed as a unit with the same method sequence and the same lots of reagents

and standards. The manipulations common to each sample in a batch must be performed simultaneously or in

a continuous sequence without significant interruption. If an analytical sequence contains more than one

distinct step, such as a preparation procedure, quality control samples required by the method for the batch

must be assigned and prepared in the initial step. This group of samples is called a preparation batch, and

must contain all quality control samples required by the method, including (PB/MB, Dup, MS, MSD, LCS,

other). A preparation batch must not contain more than twenty field samples. Laboratory QC samples

processed in the preparation batch are not counted in the maximum batch size of 20. If the instrumental

analysis of the samples in one preparation batch is not performed in a continuous sequence, the method blank

from the preparation batch must be analyzed with each set of samples from the same preparation batch. If re-

analyses are required (e.g. to perform dilutions) it is not necessary to include the method blank in the

reanalysis.

13.2 LABELING CONVENTIONS

Unique batch identifiers are needed to properly coordinate referencing of QC parameters to associated

work order. Preparation sets which are processed into the LIMS are labeled by batch #, date and set

number. All prepared samples within the batch are associated automatically by the LIMS. If preparation

tasks are not processed into the LIMS, preparation batches are labeled on individual preparation logs. QC

parameters are labeled by a combination of 1) QC parameters type, 2) batch #, 3) Sample number, 4) date

and 5) file #.

13.3 QC PARAMETER CONTROL LIMITS

Control limits are calculated from recoveries of laboratory control samples and/or matrix spikes. A minimum

of twenty observations should be used to calculate control limits. 500 and 600 series methods mandate

calculation of control limits with the statistical use of the word "control" in mind.

Control Limits = Mean Recovery 3 s

s is the standard deviation of the recoveries

The SW-846 series calculation for control limits are as follows:

Control Limits (Matrix Spikes) = Mean Recovery 3 s


Control Limit (for surrogates) = Mean Recovery 3 s


In order to monitor trends in the analytical process, the latest thirty to forty observations are used to calculate

laboratory control sample control limits. New control limits are compared to previously calculated limits to

track possible trends. Comparisons are made on the means, UCL, LCL and numbers of outliers.

When calculating control limits for matrix spikes, the database will be continually added to until major

modifications occur to a method.

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REVISION NO. 16


PAGE 13-3

% RECOVERY = X - B

T 100

There exist many variables that would cause new control limits to be initiated.

Variables: 1. New Analyst

2. New Preparation Tech

3. Method Modification

4. Instrument Modification

5. Reagent and/or standard vendor change

Control limits are subject to change without notification.

Control limits are calculated by analysts using QA Admin in Element then select Control Chart.

13.3.1 CLP projects: SW-846 control limits or CLP projects specific limits are reported. If any of the

compound CLP control limits are not available then in-house calculated control limits are used.

RPD calculation of MS/MSD Analysis

100)( 21

xX

XXRPD

Where: X = Amount of Analyte found in Matrix Spike

X = Amount of Analyte found in Matrix Spike Duplicate

X = Mean Value of Analyte found in X1 and X2.

13.4 CALCULATIONS

Precision

Precision is defined as the measure of mutual agreement among individual measurements of the same

pollutant in a sample secured under the same analytical protocols. Field and lab precision will be expressed as

relative percent difference where:

*RDP calculation of MS/MSD, RPD is calculated using MS/MSD final concentration of spiked sample.

RPD = *x1 - x2*

X H 100

RPD = Relative percent difference between MS/MSD final concentrations

||= Absolute value of the difference between MS/MSD X1 and X2

X = Mean value of MS/MSD results, X1 and X2

The goals for precision are related to the proximity of the sample value to the detection limit. At or less than

five times the practical quantitation limit, the precision goal will be expressed in absolute concentration

(quantitation limit terms).

Accuracy

Accuracy is defined as the degree to which the analytical measurement reflects the true value present.

Overall accuracy will be estimated by recovery performance of spiking events, internal standards and control

samples. Accuracy will be measured as percent recovery where:

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SECTION XIII

REVISION NO. 16


PAGE 13-4

X = measured concentration in sample after spiking

B = background concentration in sample

T = concentration of spike added to sample

If the sample concentration is below the MDL, zero (0) will be used in the calculation. In all other cases, the

sample concentration must be used to calculate percent recovery. When the sample concentration is greater

than four (4) times the spike level, the percent recovery result will be expressed as "High Mean". Percent

recovery for selected inorganic method soil matrix samples may use the average of the sample and sample

duplicate in the percent recovery equation.

13.5 COMPLETENESS

Completeness shall be evaluated qualitatively and quantitatively if necessary to meet specific project

requirements. The qualitative evaluation of completeness shall be determined as a function of all events

contributing to the sampling event including items such as correct handling of chain of custody forms, etc.

The quantitative description of completeness shall be defined as the percentage of Contract controlled QC

parameters that are acceptable.

QC parameters that shall be assessed for quantitative determinations of completeness shall include initial

calibrations, continuing calibrations, surrogate percent recovery for organics analyses, analysis of laboratory

duplicates for Relative Percent Difference (RPD), analysis of Matrix Spike/Matrix Spike Duplicate analyses

for percent recovery and RPD, and analysis of Laboratory Control Samples for percent recovery, and holding

times. The requirement for the quantitative assessment of completeness shall be 90%. The 90% standard

shall be applied to the entire list of parameters described above such that a minimum of 90% of the data for

each analytical method is associated with acceptable quality control criteria as described above and in other

sections of this document. The quantitative assessment of completeness shall be calculated for each

analytical method as the ratio of acceptable sample results to all sample results. For multi-Analyte methods

(organics analyses) each analysis of the aggregate of analytes shall be considered a single sample result. The

requirement for holding times shall be 100%. If any sample exceeds the holding time specified by EPA SW

846 (or other guidance documents for other analyses), that sample should be re-sampled and reanalyzed,

unless redirected by the client.

13.6 CORRECTIVE ACTION

Corrective Action will be initiated for instances of QC parameter in compliance. The extent and steps of

corrective action procedures will vary according to project requirements or individual client protocols.

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SECTION XIII

REVISION NO. 16


PAGE 13-5

TABLE 8 LEVEL OF QC EFFORT

QC TERM

MATRIX

FREQUENCY

CRITERIA

CHEMISTRY

Duplicate

Water

10% or 1 per batch, whichever is greater

<10% RPD above 5 times PQL, if <5

times PQL, PQL.

Inorganic

Soil/

Wastewater

5% for solid and wastewater matrices

<20% RPD above 5 times PQL, If <5

times PQL, 2 x PQL. Matrix

Spike, Matrix

Spike Dupl.

Water


Within defaulted Control Limits

Inorganic except TSS, TDS, Color, Odor,

Turbidity, pH, Conductivity

Soil/other 5% or 1 per batch, whichever is greater

Within defaulted Control Limits

Solid Matrix Metals, Solid Matrix Inorganics


Within Control Limits

Organic

LCS

NA

1 per batch

90 - 110% Recovery or Within Control

Limits

Wet Chemistry

1 per batch

85 - 115% Recovery or Within Control

Limits

Metals, Wet Chemistry (Prepared Samples)

1 per batch Within Control Limits Organic

ICV / CCV

NA

10%

90 - 110% Recovery, for CCV

95 - 105% Recovery, for ICV (See SOPs)

Inorganic, except Hg on solids

200.7, 7470, GFAA for waters Every 12 hours

See SOP

GC/MS

10% 15% diff 8000 Series except for GC/MS and 500/600 series

CCB NA Run after ICV and each CCV <PQL Inorganic, Organic Preparation/Met

hod Blank

NA

1 per batch or 20 (whichever more frequent)

<PQL or

<2 PQL for DoD ELAP (Navy) work.

Please refer to DoD QSM version 2 June

2002.

Inorganic, Organic

Initial

Calibration

NA

Before each sample run and/or when CCV unacceptable >0.995 Corr. Coeff. Inorganic When CCV unacceptable, when target compounds out

<20% RSD or regression model Organic except GC/MS

<15% RSD/If >15% RSD-use linear

regression

GC/MS

Note: This section has been reviewed on 01/08/2016 (No Changes were made)

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PERFORMANCE AND SYSTEMS AUDIT

SECTION XIV


PAGE 14-1

14.0 PERFORMANCE AUDITS (Proficiency Testing)

In order to validate BC Laboratories, Inc. method performance accuracy and comparability to standards of the

environmental laboratory industry, a program of external and internal performance evaluations must be

incorporated into the Quality Program. Comparability studies are through external PE sample analyses, while

internal assessments are conducted to validate and maintain control of the analytical system.

14.1 EXTERNAL PERFORMANCE EVALUATION SAMPLES

BC Laboratories, Inc. is involved in 1)the Absolute Standards Water Supply and Water Pollution

performance evaluation studies, 2)the NPDES DMR PE studies, 3) a program of PE samples for soil

matrices through Absolute Standards, 4) an internal PE sample assessment through purchased standards

from Absolute Standards, 5) ERA Microbiology Evaluation Study and 6) Mixed Analyte Performance

Evaluation Program. PT studies are performed every six month interval. WS and WP are done in January

and July along with AK PT Studies. RCRA (Soil) are performed in April and October.

Air Testing Analysis PT provider is Sigma-Aldrich. These are schedule in April and October.

All performance sample studies are completed (i.e., we participate in every WS, WP and DMR QA PE/PT

Study). This is not a necessity since one compliant Analyte result per PE study will validate that parameter

for one year. Each PE sample is analyzed to validate continuous control of the analytical system.

14.1.1 Scope of Analytical Parameters

14.1.1.1 Water Supply - Corrosively, MBAS, Silica, Perchlorate, DOC, Vanadium, GAD, PCB,

Tert-Butyl Alcohol, Metals, Mercury, pH, Inorganics, Alkalinity & Sodium, Turbidity,

Residual Chlorine, Nitrite, Nutrients, Cyanide, TOC, Bromide, Hardness, Standard Plate

Count, MicrobE, Regulated Volatiles, Halomethanes, Unregulated Volatiles, Regulated

Pesticides, Toxaphene, Chlordane, EDB/DBCP, Regulated Semivolatiles, Regulated

Herbicides.

14.1.1.2 Water Pollution - PAHs, Boron, Surfactants, Acidity, Bromide, Nitrite, Settable Solids,

Volatile Solids, Silica, Sulfide, Turbidity, Carbamates, pH, Hardness, Demand, Simple &

Complex Nutrients, Cyanide, Phenolics, Grease & Oil, TRC, Trace Metals, Mercury,

Minerals, Tin and Titanium, Hexavalent Chromium, MicrobE, Volatiles, PCBs, Pesticides,

Chlordane, Toxaphene, Herbicides, Base Neutrals and Acids.

14.1.1.3 (DMR – QA Study) - pH, Hardness, Demand Group, Simple & Complex Nutrients,

Cyanide, Phenolics,Oil & Grease, Total Residual Chlorine (TRC), Trace Metals, and

Mercury.

14.1.1.4 Soil Series-Gasoline in Soil & Water, Diesel in Soil & Water, TPH in Soil & Water, BTEX

in Soil & Water, Trace Metals, Cyanide, Hexavalent Chromium, Base/Neutrals & Acids,

Pesticides, Chlordane, Toxaphene, Volatiles, Herbicides, PCBs, Organophosphorous

Pesticides, Ready to Use Volatiles, PAHs, Nitroaromatics & Nitramines, Corrosivity, and

Anions

14.1.1.5 MAPEP-Semi-Volatile Organics

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PERFORMANCE AND SYSTEMS AUDIT

SECTION XIV

REVISION NO. 21


PAGE 14-2

14.1.1.6 As stated on SOP BCSAM005 BC Laboratories will not accept any sample that

may contain “Radioactive Material” above background levels.

14.2 SYSTEMS AUDIT

14.2.1 Internal

Systems audits will be conducted on a annual basis and will cover 1) parameters outlined on the

Internal Assessment Schedule (Figure 7), 2) LIMS, 3) invoicing, 4) conformance to methodology

of Inorganic/Organic and SOP procedural outline, and 5) other tasks with performance objectives.

A completed Systems Audit Report will be submitted to the General Manager annually. Topics of

concern which arise during the year will be addressed at the quarterly Supervisor's Meetings.

14.2.2 External

External based audits are conducted by representatives of the state of California, and other private or

government entities.

14.3 ACTION

The QA Officer is responsible for completing annual systems audits and initiating subsequent corrective

actions as needed. If corrective action is required, the QA Officer has the authority to delegate

responsibilities and to initiate progressive discipline if tasks are not completed sufficiently to restore

acceptable performance of the analytical system. Corrective action documentation will illustrate tasks,

responsibilities, time frames, and will validate restoration of the process to a controlled status. Corrective

action documentation and System Improvement Forms are stored in the QA/QC Department and in

pertinent files.

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INTERNAL ASSESSMENT SCHEDULE

FIGURE 7

SECTION XIV

REVISION 21


ASSESSMENTS

TASK

DOCUMENTATION

TASK COMPLETION

TIME WINDOW Balance Calibration

Secure service from Watson Bros.

Calibration Sheets,

Balance Stickers

June - July

Balance Calibration

Daily Monitoring - Two range

Balance Logbooks

Each Workday

Class S-1 Weight

Calibration

Secure service from Watson Bros.

Calibration Sheets,

Weights Sticker

March-April, every two

years Working

Thermometer Checks

Check working thermometers against a

NIST traceable thermometer

Thermometer

Calibration Log

Mercury in glass - Dial-

type-annual –

March-April Reference

Thermometer

Calibration

Secure service from Tektronix

Calibration Sheets,

Thermometer Sticker

Nov.-Dec.

Working

Thermometer

Monitoring

Daily Monitoring of refrigerators,

waterbaths, incubators, auto claves, and

ovens

Respective Logbooks

Each Workday, Each

Monday for 24 hr dial-

type thermometers for

TCLP and Walk-In

refrigerators Auto-diluter

Calibration

Gravimetric check of volume deliveries for

auto diluters

Diluter Calibration

Worksheets

March, June, Sept, Dec.

Micro-pipette

Calibration

Gravimetric check of volume deliveries of

micro-pipettes

Preparation

Logbooks/Run Logs

Each Workday

Non-Class-A

Glassware calibration

Gravimetric check of volume delivery

Weight written on the

glassware

Before use after purchase-

semi-annual if in use. Corrective Action

Audit

Secure PE samples from ERA + Absolute

Standards

PE Summary Reports

When needed

LIMS

Check for any anomalies in reporting of

results, methods, formats, etc.

Evaluate data processing, resources, and

EDD's.

Annual Internal Audit

Report

Jan-Dec

Field Services

Check for: correctness of preserved

container submittals, safety compliance,

maintenance schedules of vehicles and

other equipment. Conduct client

interviews and review SOP's and Field

documentation.


Report

Jan-Dec

Sales and Marketing

Review submitted bids.

Conduct client interviews.


Report

Jan.-Dec.

Client Services

Review the following: Project Initiation

Forms, Non-Conformance Reports and

SOPs. Conduct client interviews


Report

Jan.-Dec.

Non-Conformances

Review SIFs

Annual Internal

Jan.-Dec.

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FIGURE 7

SECTION XIV

REVISION 21


ASSESSMENTS

TASK

DOCUMENTATION

TASK COMPLETION

TIME WINDOW

SIFs Report/Database Instruments Support

Equipment

Verify fitness for use

Spreadsheet

Jan.-Dec.

Login Department

Review sample receipt forms, non

conformance reports, and SOP's.

Evaluate chain of custody procedures and

sample "cradle to grave" system.

Audit the bottle preparation area.


Report

Jan.-Dec.

Preparation

Department

Review SOP's for conformance to method

and practice. Check and evaluate

documentation for: control charting,

preparation logs, run logs, maintenance

logs, standard and reagent logs. Evaluate

new processes.

Review System Improvement Forms.


Report

Jan.-Dec.

Inorganics

Department






new processes.



Report

Jan.-Dec.

Organics Department






new processes.



Report

Jan.-Dec.

Data Control

Department

Review the process and pertinent SOP's

Audit the retrieval of data


Report

Jan.-Dec.

Record Keeping

Review the system and pertinent SOP's.

Inspect data storage areas.


Report

Jan - Dec

Training

Review orientation documentation.

Obtain information of training done from

external sources.

Review attendance of internal QA/QC

Training. Check for IDC's for pertinent

personnel


Report,

QA/QC Outline and

Training Sheets.

Database

Attendance

External Training

Documentation

Jan.-Dec.

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FIGURE 7

SECTION XIV

REVISION 21


ASSESSMENTS

TASK

DOCUMENTATION

TASK COMPLETION

TIME WINDOW Annual Internal Audit

Report

Complete into final form


Report

Nov - Dec

Supervisor or

authorized personnel

Review of standards, reagents and

maintenance log will be performed at least

in a monthly basis. Review of logbooks

for completeness, legibility purposes. All

Wet Chemistry analysis for all manual

tests review is performed in the Element as

a supervisor review. All non-manual tests

(e.g. metals) logbooks review performed

as stated above.


Report

Monday -- Friday

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FIGURE 7

SECTION XIV

REVISION 21


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DATA ASSESSMENT PROCEDURES

SECTION XV


PAGE 15-1

15.0 SCOPE

This section identifies the required concentration range and data on sensitivity (detection limits), precision, and

accuracy. Analytical data quality requirements for accuracy and precision established for each measurement

parameter will be based on (1) prior knowledge of the specific measurement system used and (2) method

validation studies employing replicate analyses, spikes, standards, recoveries, and project-specific requirements.

15.1 ACCURACY - ORGANICS AND GENERAL CHEMISTRY

Accuracy will be evaluated through the collection and analysis of matrix spike and matrix spike duplicate

(MS/MSD) samples, laboratory control samples (LCS), and by spiked samples with surrogate compounds,

where applicable. QC criteria for GC/MS analyses (surrogate recoveries, LCS recoveries, MS/MSD

recoveries and RPD) must conform to the Contract Specifications, SW-846, and CLP standards. Accuracy

is a quantitative parameter of the bias in a measurement system. Sources of error include the sampling

process, field contamination, preservation, handling, sample matrix, sample preparation, and analysis

techniques. Accuracy is calculated as follows:

! For measurements where matrix spikes are used:

%R = 100% x

S-U

Csa

%R = percent recovery

S = measured concentration in spiked aliquot

U = measured concentration in unspiked aliquot

Csa = actual concentration of spike added

MSR x y sample result sample result

spike levelx

/

100


x = mls of spike


or MSR sample result * 1 x / y

spike levelx 100


x = mls of spike

y = mls of spike + mls of sample

! For situations where a surrogate or standard reference material (SRM) is used instead of or in addition

to matrix spikes:

%R =

C

M

Ca

x 100%

%R = percent recovery

Cm = measured concentration of SRM

Ca = actual concentration of SRM

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For GC and GC/MS each sample, spike, and blank will contain surrogate compounds to validate individual

sample preparation and analysis. If surrogate recoveries are not within the control limits, the following

procedure will apply. Calculations, surrogate solutions, and internal standards will be checked for errors. If

no errors are found, instrument performance will be checked. If an instrument performance problem is

identified, the problem will be corrected and the sample reanalyzed. If no instrument problem is found, the

sample will be reanalyzed if sufficient sample and time are left on holding time. If, upon reanalysis, the

recovery is again not within the designated control limits, the data will be flagged appropriately.

A matrix spike/ matrix spike duplicate pair will be prepared and analyzed along with each preparation batch

(not to exceed 20 samples per batch). The matrix spike and matrix spike duplicate samples will be spiked

with a mid-range concentration of a series of method target compounds, while a third aliquot of the sample

will be analyzed unspiked. Routine general chemistry listing will include a duplicate of the unspiked sample

(see SOP=s) Accuracy will be measured in terms of percent recovery of each MS/MSD. Analyses not

meeting the laboratory quality control criteria will be re-extracted/reanalyzed once unless it can be

documented that the failure (such as a calculation error) was not associated with the samples, or that matrix

effects were the cause and LCSs were acceptable.

Analysis of a benign matrix (ASTM Type II water, baked sand), spiked with the same solution used for

matrix spikes, is used to validate the accuracy of the analytical system under ideal matrix conditions. This

QC parameter, known as the Laboratory Control sample is a required QC sample, which is prepared and

analyzed with each batch at a frequency set per method. LCS validity is assessed through percent recoveries

compared against statistically based control limits unless general criteria has been defaulted. If any LCS

analytes are outside acceptable limits, associated sample data should be considered estimated, thus the entire

batch should be considered estimated, thus the entire batch should be reprepared and reanalyzed unless it can

be proven that effects can solely be attributed to the LCS and no other QC indicators show possible quality

compromise. If reanalysis is not feasible, data will be flagged accordingly.

15.2 ACCURACY - INORGANICS

Accuracy for Inorganics analyses will be evaluated through the collection and analysis of matrix spike

samples and laboratory control samples. QC criteria for metals analyses, will conform to standards specified

by the contract specifications, SW-846, and CLP. Matrix spikes will be prepared and analyzed along with

each preparation batch (not to exceed 20 samples per batch). The matrix spike samples will be spiked with a

mid-range concentration of the method target compounds, while an aliquot of the sample will be analyzed

unspiked. The matrix spike for Inorganics analyses will be an analytical spike - a spike of the solution being

prepared prior to the preparation procedure. Accuracy will be measured in terms of percent recovery of each

of the spiked components (as indicated in the formula for matrix spikes). MS analyses not meeting the

laboratory quality control criteria will be re-prepared/reanalyzed unless it can be discerned that the failure

was not associated with the samples (such as a calculation error) or that matrix effects were the cause and

LCSs were acceptable.

Analysis of a benign matrix (ASTM Type II water, baked sand), spiked with the same solution used for

matrix spikes, is used to validate the accuracy of the analytical system under ideal matrix conditions. This

QC parameter, known as the Laboratory Control sample is a required QC sample, which is prepared and

analyzed with each batch at a frequency set per method. LCS validity is assessed through percent recoveries

compared against statistically based control limits unless general criteria has been defaulted. If any LCS

analytes are outside acceptable limits, associated sample data should be considered estimated, thus the entire

batch should be considered estimated, thus the entire batch should be reprepared and reanalyzed unless it can

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PAGE 15-3

RPD - (C

1-C

2) x 100%

(C1 + C

2)2

be proven that effects can solely be attributed to the LCS and no other QC indicators show possible quality

compromise. If reanalysis is not feasible, data will be flagged accordingly.

Post-digestion spikes are prepared by adding a known amount of analyte to an aliquot of sample. If the

analyte concentration is below the detection limit for all samples in the batch, the sample is spiked at a

concentration equivalent to approximately 10 to 20 times the PQL. Acceptance limits for percent recovery

for the post-digestion spike are 85 to 115 percent. Failure to meet the acceptance criteria requires corrective

action, which may include dilution and respiking of the sample or reanalysis of all samples in the batch by

the method of standard addition (MSA). If dilution is performed to further reduce physical interferences, an

acceptable post-digestion spike must be performed on the diluted sample.

15.3 SENSITIVITY

Method detection limit studies will be performed annually as described in 40 CFR 136 Appendix B.

Practical quantitation limits will be determined as a concentration approximately three to five times the

standard deviation of the low level spikes used for the method detection limit study, or set at levels of

confidence as determined by our specialists. PQL levels must not exceed those levels set in respective

method references listed in section XI.

15.4 PRECISION

Precision will be evaluated through the collection and analysis of field and laboratory duplicate samples and

matrix spike duplicates. Laboratory duplicate samples not meeting quality control criteria will be re-

extracted/reanalyzed once, unless it is determined that the RPD of the reanalysis will not significantly differ

from the primary analysis. For organics analyses, failure of different matrix spike compounds to meet QC

criteria on successive runs will constitute failure and satisfy the requirement for reanalysis.

Precision is a quantitative parameter of the variability of a group of measurements compared to their average

value. Sampling precision is evaluated from field duplicate samples and analytical precision is evaluated

from matrix spike duplicate samples and split samples. Precision is calculated in terms of the relative

percent difference as follows:

Where: RPD = relative percent difference

C1 = larger of the two observed values

C2 = smaller of the two observed values

In cases where duplicate concentrations are in close proximity to detection or quantitation limits, precision

will be assessed in concentration terms. This assessment will be used in cases where the sample or the

sample duplicate concentration is less than or equal to five (5) times the PQL for the Analyte of concern.

Refer to the Method Blank assessment flowchart in Appendix D for further details.

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PAGE 15-4

Example:

PQL = 0.2 mg/L

Sample value = 0.4 mg/L

Duplicate value = 0.5 mg/L

Precision control = 0.2 (PQL)

Both 0.4 and 0.5 are less than five (5) times 0.2.

0.5 - 0.4 = 0.1 mg/L

0.1 is less than 0.2 (precision control), therefore precision requirement was met.

Laboratory duplicates will be performed for all inorganic analyses at a rate of 1 in 20 (1 for each batch up to

a maximum of 20) for soils/waters under SW-846 methodologies and 1 in 10 for waters under other

references. Precision for organics analyses may be determined by the analysis of matrix spike/matrix spike

duplicate samples at a rate of 1 in 20 (1 for each batch to a maximum of 20). RPD is based on the difference

between sample value and sample duplicate value which is a source of uncertainty measurements. In this

situation uncertainty measurement is 0.1 mg/L. The Laboratory analytical measurement uncertainty is

represented by the LCS Control Limits

15.5 There are many aspects of the sampling and analysis process which can contribute to analytical uncertainty.

The representativeness of the sample and aliquots taken from the submitted sample, the accuracy of

calibration stock solutions and dilutions made from them, the stability of the analyte within the sample

matrix and other factors which are difficult if not impossible to measure may all contribute to uncertainty of

analytical results in samples. However, within the somewhat controlled environment of the laboratory we

can use a statistical analysis of the Laboratory Control Sample (LCS) to make an estimate of the uncertainty

of a given analysis. The LCS is a clean matrix with an established Analyte concentration which is carried

through the entire preparation and testing procedure with each analytical batch of samples. Over time the

routine analysis of the LCS provides us with data with which we can estimate the uncertainty of that analysis.

After approximately 30 analyses of the LCS, the standard deviation is calculated and assuming a normal

distribution of those values, 95% of them should fall within 2 standard deviations of the mean. The

Laboratory will use a band of 2 sample standard deviations as the estimate of analytical uncertainty for any

given analysis.

The following chart of analytes and their uncertainties will be updated on an annual basis. The sample

standard deviation is calculated by taking the square root of the sum of squared deviations from the mean

divided by one less than the number of measurements. The estimate of uncertainty does not take into

account the possibility of higher or lower uncertainty based on different Analyte concentrations and many

other factors that will affect real world samples.

Analyte Method Average σn-1 Uncertainty

Benzene EPA 8260 98 3.73 7.46

1,4-Dichlorobenzene EPA 8270 81.4 7.05 14.1

1,1,1Trichloroethane EPA 624 102 4.91 9.82

1,2-Dibromoethane EPA 8260 99.2 5.15 10.3

Acetone EPA 8260 91.7 5.73 11.5

1,2-Dibromoethane TO-15 89 9.8 20

Vynyl Chloride EPA 624 95.6 5.82 11.6

1,3-Butadiene TO-15 94 7.94 16

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Dis Mercury EPA 7470A 102 5.04 10.0

Total Recoverable EPA 200.7 98.7 4.02 8.04

Total Iron EPA 6010 109 4.15 8.30

Total Recoverable Chromium EPA 6020 105 3.69 7.38

Dissolved Calcium EPA 200.7 101 1.93 3.86

Bromide EPA 300.0 101 4.02 8.0

Chloride EPA 300.0 103 3.03 6.0

Sulfate EAP 300.0 102 2.98 6.0

Nitrite as N EAP 353.2 102 2.82 5.6

Ortho-Phosphate EPA 365.1 102 3.47 6.94

COD EPA 410.4 100 3.3 6.6

TOC SM5310C 102 1.66 3.32

Ammonia as N EPA 350.1 104 3.83 7.66

Hexavalent Chromium EPA 7199 101 3.52 7.04

TPH-Diesel EPA-8015B 77.5 6.85 13.7

Bolstar EPA 8141A 87.9 20.3 40.6

2,3-DB EPA 8151A 81.7 16 32

15.6 LABORATORY CONTROL SAMPLE (LCS)

Acceptability of batch runs will depend heavily on the analyte recovery(s) of the LCS. (See Section 12.0 for

acceptance protocol and Appendix D for corrective logic.) Laboratory Control Sample can be matrix dependant,

but in lieu of appropriate matrix, accuracy can be validated through the recovery of the Laboratory Control Sample

Water (LCSW). The Laboratory Control Sample is a sterile sample which has been spiked and brought through the

entire analytical process.

15.7 MONITORING OF LCSW

The Laboratory Control Sample Water is the QC spiked parameter of choice to be monitored through control

charting.

15.7.1 Charting of Multi-Analyte Methods - In cases where charting organic multi-Analyte methods is not

feasible, a select subset of analytes should be identified and charted. Those analytes chosen should

represent the entire retention time range and must represent normal analytical activity or performance

(i.e. do not chart abnormally stable or unstable analytes).

15.7.2 Development of Control Charts

A minimum of 30 data points is required in order to administer statistical manipulations to a

particular QC parameter. Once at least twenty values are obtained, the standard deviation and mean

of the data set can be calculated. The mean plus or minus two sigma will define warning limits while

the mean plus or minus three sigma will represent control limits or the extremes of the acceptable

range. Please contact the QA Officer for guidance or for additional charting options.

15.7.4 Maintenance of Control Charts

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PAGE 15-6

15.7.4.1 Electronic Charting

Instrument data which is processed via Element, control limits are calculated by analyst using

QA admin in Element then select control charts. Recalculations of control limits shall be

monitored on an on-going basis (at least quarterly) for shifts in mean recovery, changes in

standard deviation, and development of trends. The recalculated limits should be submitted to

the QA/QC Department for LIMS updating.

15.7.4.2 Calculation Controls

It is important that control limits are properly calculated to correctly assessed control of the

system and to validate presence of interferences and bias.

General Rules

1 Include all recoveries unless outliers are validated.

2 If significant changes are made, reestablish control limits by initiating a new data set.

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PREVENTATIVE MAINTENANCE

SECTION XVI

REVISION NO. 13


PAGE 16-1

16.0 SCOPE

Preventive maintenance is an orderly program of positive actions (equipment cleaning, lubricating, reconditioning,

adjustment and/or testing) done to prevent the failure of measurement systems or support equipment. The goal is

to ensure the analytical system is in control and to prevent any nonconformance from occurring before tasks are

initialed. Use of preventive maintenance schedules for each analytical measurement system and support equipment

type aids in the foretelling of possible problems. Documentation of preventive procedures is through Preventive

Maintenance Logs.

Preventive Maintenance Logs are maintained for all instrumentation and equipment. These logs are stored near

respective instrumentation and are maintained by responsible analysts or technicians. Figure 8 displays an example

of a preventive maintenance schedule.

16.1 GENERAL PROCEDURES

Preventive maintenance will be performed by qualified personnel. Records of repairs, adjustments, and

calibrations will be maintained and available for inspection. The records will document and state the return

to control of instruments after repair or maintenance. Periodic checks of Preventive Maintenance Logs and

schedules will be performed by department supervisors. Documentation of these checks will consist of

approval initials on pertinent logs.

If an instrument is not working properly and cannot be restored by laboratory personnel, a service call to the

manufacturer will be made. Approval of a service call must be made by the concerned department

supervisor before initiation. Documentation of each service call will be maintained in respective Preventive

Maintenance Logs.

16.2 TAGGING OUT

In cases when instrumentation or equipment is not operational, they must be labeled out of service, do not

use. A sign with the aforementioned label will be affixed to non-operational instruments or equipment by

department supervisors or the QA Officer. All out - of - calibration equipments tagged or segregated will not

be used, until they have been re-calibrated. Equipment found out - of - calibration will be repaired or

replaced. Responsibility of the removal of warning signs is designated to either department supervisors or

the QA Officer.

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SECTION XVI

REVISION NO. 13


PAGE 16-2

16.3 GENERAL PREVENTIVE MAINTENANCE CHECKS

EQUIPMENT MONITORING

Equipment

Check Acceptance

Criteria

Frequency

Top-loading

balances

Verify accuracy with weights calibrated against

certified class-S weights

0.02 g

Daily or with each use

Analytical balances

Verify accuracy with weights calibrated against

certified class-S weights

0.0005g


Thermometers

Verify accuracy against NIST-certified thermometer,

or if purchased with certificate of traceability, check

for mercury separation daily.

+1.0C

Annually

Temporary storage

refrigerators

Verify temperature within range.

0C-6C

Daily

Long-term storage

refrigerators


0C-6C

Daily

Freezers


≤ -10C

Daily

Water baths


60-80C

80-90C


Ovens


105C2C


Fume hoods

Check fan condition and velocity.

Monthly Safety showers

Inspect for working order.

N/A

Monthly

Fire extinguishers

Pull pin in place.

Gauge reads

full.

Monthly

Eyewash stations

Inspect for working order.

N/A

Monthly

PREVENTATIVE MAINTENANCE CHECKS AND SERVICES: GAS CHROMATOGRAPH

Items to be Inspected

Probable Problem

Service Interval

Procedure (Internal)* Line fuses (GC)

Inactive GC, blown fuse

As required

Replace fuse

Splitless injector for capillary

columns heater or sensor

Failure to heat

As required

Replace heater or sensor

Injector septum in the GC

Leaks, septum bleed

Weekly, as needed

Replace as required

Injector liner

Poor chromatography, active sites

As required

Clean, inspect, or replace

as required Carrier gas connections and

couplings

Leakage

As required

Tighten or replace fittings

Carrier gas filter in GC

Poor baseline

As required

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SECTION XVI

REVISION NO. 13


PAGE 16-3

PREVENTATIVE MAINTENANCE CHECKS AND SERVICES: GAS CHROMATOGRAPH


Probable Problem

Service Interval

Procedure (Internal)*

Filter flow controller Dirty filter Every 3 months Replace filter Capillary column

Poor chromatography

As required

Inspect or replace as

needed Detector heater/sensor

GC not ready

As required

Replace heater or sensor

Autosampler Syringe

Poor reproducibility / leaking

Daily

Inspect or replace

* Applicable procedures are presented in the Varian or Hewlett Packard operator manual.

ROUTINE PREVENTATIVE MAINTENANCE: GC LABORATORY INSTRUMENTATION

Instrument

Routine Maintenance Performed

Frequency GC/ECD

Replace septum, check syringe

Replace injection port liner

Swab injector port with a series of 4 solvents

Every 72 hours or as needed

Every 72 hours

Every 72 hours HPLC

Column flushed with methanol

Daily

Spectrophotometer

Replace lamps

Wavelength check

6 mos

6 mos

PREVENTATIVE MAINTENANCE CHECKS AND SERVICES: MASS SPECTROMETER


Probable Problem

Service Interval

Procedure (Internal) Glass jet separator

Obstruction or glass breakage

As required

Clean or replace

Glass jet separator ferrules

Leaks

As required

Replace

Vacuum Manifold

Gross leaks, persistent pressure due

to degassing of trapped gases in the

vacuum system, faulty CAL gas

pressure, faulty switch

As required

Inspect

Quadrapole mass analyzer

Failure to pass tune; dirty

As required

Inspect, replace or clean

Electron multiplier

Low sensitivity

As required

Replace

Vacuum pumps

Locks up

Every 3 months

Purge weekly and replace

oil Turbo pump

Dirty oil

Bimonthly

Purge weekly and replace

oil Vacuum system filter

Excessive use, dirty filter

As required

Clean and inspect

Ion source

Lack of sensitivity, irregular peak

shape, no autotune

3-6 months

Clean and inspect

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SECTION XVI

REVISION NO. 13


PAGE 16-4

PREVENTATIVE MAINTENANCE CHECKS AND SERVICES: GC/MS INTERFACE OVEN


Probable Problem

Service Interval

Procedure (Internal) Capillary interface tubing

Plugged

As required


Separator divert fitting

Leakage

Every 3 months

Tighten or replace

Vacuum divert valve

Clogged

Every 3 months


PREVENTATIVE MAINTENANCE CHECKS AND SERVICES: COMPUTERS


Problem

Service Interval

Procedure (Internal) Fan

Faulty fan rotation

As required

Inspect or replace

Output signal

Failure to boot

As required

Check and verify

Adjustable DC

Low voltage

As required

Check and verify

Disk drive

Crash

As required

Inspect or replace; check

software

ROUTINE PREVENTATIVE MAINTENANCE: GC/MS LABORATORY INSTRUMENTATION

Instrument


Frequency Volatile GC/MSs

Change septum, column maintenance, clean

injection port liner, backflush purge and trap

device, change trap.

As needed; checked each shift

Semivolatiles GC/MSs

Change septum, clean or replace injection port

liner, clean injection port, perform column

maintenance.

Every 12 hours, as needed

ROUTINE PREVENTATIVE MAINTENANCE: Inorganics Laboratory Instrumentation

Instrument


Frequency AA

Check and clean air filter.

Check cuvettes.

Check drain lines.

Daily

Daily

Daily ICP

Clean torch.

Check and clean filters.

Clean nebulizer chamber area.

Replace pump tubing.

As required, minimum weekly



As required, minimum weekly ICP-MS

Replace worn reagent tubing lines

As needed; checked daily

Autoanalyzers

Check and replace work pump tubing.

Clean platens

Wash manifolds

Clean pump roller cage

As needed

Daily

Weekly

3 months

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SECTION XVI

REVISION NO. 13


PAGE 16-5

Clean pump fan

Lubricate pump gears

Replace redundant tubing lines

Replace lamps

Replace photomultiplier tubes

3 months

3 months

6 months

6 months

Annually Leeman

Change pump tubings

Change redundant tubing

Change sample probe

Replace optical cell

Weekly

Every 2-3 months

As needed

Monthly IC's

Conductivity

System pressure

Leak check

Regenerate level

Guard column

Sep. column

Bed support

Daily

Daily

Daily

Daily

As needed

As needed

As needed Spectrophotometer

Wavelength Checks

Every 6 months

ROUTINE PREVENTATIVE MAINTENANCE: Organic=s Laboratory

Instrument


Frequency Total organic carbon

analyzer

Change septum

Change permeater

Change pump tubing.

Check gas flow rate.

Change glass, wool and sodium hydroxide in

scrubber.

Clean dust out of electronics cabinet.

Clean sample cell on IR detector.

Empty water trap.

Monthly

Every 3 months

Daily

Daily

Monthly

Every 3 months

Semiannually

Daily IR

System check

Noise check

Clean cell windows

Daily

Daily

Monthly

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SECTION XVI

REVISION NO. 13


PAGE 16-6

Table 8.0 Maintenance Log

DAY

1

2

3

4

5

6

7

8

9

10

11

12

13

14

15

16

17

18

19

20

21

22

23

24

25

26

27

28

29

30

31

INITIALS

DAILY

Clean Platens

Empty Waste Containers

Wipe Spills

Dispose of Sample Cups

WEEKLY

Wipe Pump Rollers

Clean Manifolds - KemWash

MONTHLY

Clean Wash Reservoir

160-200 HRS

Change Pump Tubing

400 HRS

Clean Pump Roller Cage

Clean Pump Fan

Lubricate Pump Gears

6 MONTHS

Replace Wash Res. Tubing

Replace Cart. Drain Tubing

Replace Transmission Tubing

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CORRECTIVE ACTION/QUALITY IMPROVEMENT

SECTION XVII

REVISION NO. 14


PAGE 17- 1

17.0 DEFINITIONS

17.0.1 Corrective Action (CA)

A process by which a critical error is corrected in such a way as to prevent future errors of the same

nature or type.

Some examples of when to initiate corrective action:

S Calculation errors.

S Client Request.

S Out of control trend

S Significant QA/QC anomalies

S Unacceptable PE results.

S Poor curve linearity.

S Dilution error (if sample is diluted).

S Equipment malfunction.

S Improper methodology for sample matrix.

S Contamination.

S Incorrect report formatting.

S Clerical discrepancies.

S Invoicing problems.

S Field service problems.

S Inherent or chronic problems with methodology.

17.0.2 System Improvement Form (SIF)

A term used to describe a preemptive positive action or process modification, which increases the level

of quality and customer satisfaction.

17.1 Corrective Action Process

(Corrective and preventive action steps for reporting and correcting problems for non conformance

measurement or instruments)

1. Identify the problem: A problem must be identified in a clear and concise term.

2. Evaluation (Root Cause): A root cause of the problem must be determined to see whether the problem

is local or systematic.

3. Extent of Problem: Extent of the problem must be specific to the area of the problem; so that it can be

addressed appropriately.

4. Develop Action: Develop a through action plan to address the problem in question

5. Implementation of Corrective Action: A plan needs to be designed that reflect how this plan was

implemented that demonstrates the outcome of implementation.

6. Expected Completion Date: A problem expected completion date ought to be assigned

7. Evaluate of Effectiveness of Corrective Action: Develop a plan (test) to evaluate the effectiveness of

the corrective action

8. Criteria for Verification: A criteria needs to be set up in order to verify whether your action was

effective

9. Documentation: All Corrective Action must be documented for future reference

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REVISION NO. 14


PAGE 17- 2

PROCESS

Implement

Corrective

Action(s)

Demonstrate

correction of

the problem

Close the

corrective action

process

(documentation)

END

Identify what

went wrong

Identify the

root cause

Extent of

problem

Develop Action

Expected

Completion Date

Evaluate the

effectiveness of

Corrective Action

Please refer to Appendix D for background on initiation of analytically based corrective action.

17.1.1 Determining the Root Cause

Quality problems can be the result of complex causes. Once a problem has been identified in a

process, the potential causes need to be determined before any corrective actions are taken.

The cause and effect diagram is one of the tools that can be used to identify all of the potential causes.

The cause and effect diagram is also used to describe the relationship between the various causes of

variation. This half of the diagram is the cause side. The right side of the diagram lists the problem or

quality characteristic to be improved. This half is the effect side. The major purpose of the cause and

effect diagram is to identify the relationships that exist between each of the various causes and to

determine their overall effect on the problem.

All things vary. That is, each result or item differs to some degree from the others produced by the

process. These differences are the result of various causes in the process. Causes of variation can be

categorized as common or assignable.

Common causes of variation result from normal events operating within the process. Common causes

cannot be eliminated entirely, but their effect on the quality of items can be controlled. Assignable

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REVISION NO. 14


PAGE 17- 3

causes, on the other hand, are the result of abnormal or unnatural events in the process. Assignable

causes can be detected, corrected, and eliminated.

Common causes of variation are usually group into five major categories; people, machinery, methods,

materials, and environment.

People: Since every person is unique, individual performance and perceptions vary from one person to

the next. Even when established procedures are used to perform a specific task, no two people

perform tasks in the exact same manner. Given this, variation occurs as a result of the people involved

in the process.

Machinery (instrumentation): The performance of instrumentation and equipment used in processes

changes daily. These changes are due to mechanical functions, wear, calibration, and so on. Variation

naturally occurs as a result of equipment, instrumentation and so on.

Methods: On the surface, method of operation appears to be fairly consistent, yet differences exist.

These differences may occur between shifts, supervisors, pressures, location, and so on. The methods

used in a process are based on interpretation. Various interpretations of methods affect the variation of

the process.

Materials: The basic composition and measurements of raw materials vary. In addition the materials

delivered by various suppliers also vary. Therefore, the materials used in any process vary to some

degree.

Environment: The events that naturally make up the environment, such as organizational culture,

management, humidity, temperature, pollution, and so on, all affect the variation in the process.

When these factors are combined in a process, a certain level of variation will occur in the process.

These causes of variation are referred to as common cause variation, which cannot be entirely

eliminated.

In addition to common cause variation in the process, assignable causes may also be present.

Assignable causes of variation are the result of abnormal or unnatural events. Any factor outside the

realm of a common cause can be defined as an assignable cause.

Examples of assignable causes:

Environmental factors such as air conditioner breakdowns, power outages, or abnormally high levels

of pollution.

Measurement devices or gauge malfunctions.

Equipment malfunctions.

Whenever an attempt is made to condense or reduce the amount of time normally required doing a job

or performing a given task, variation in the process increases.

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REVISION NO. 14


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For the most part, both common and assignable causes of variation are present in all processes. These

combined levels of variation directly affect the quality of the items produced by the process. The

higher the level of variation, the poorer the quality. To improve quality, the variation should be

eliminated and common cause variation can be reduced by improving the process continuously.

The cause and effect diagram can be used to identify the causes of variation in the process. This information

allows you to identify the major causes of variation that can be controlled or eliminated. The net effect of

these efforts will enable you to reduce variation in the process and improve quality.

Constructing a Basic Cause-and-Effect Diagram

Step 1: Identify a problem or quality characteristic.

Once a specific problem has been identified, draw a box on the right side of the paper and write the

problem in the box.

Step 2: Draw on a line pointing to the problem identified.

After one problem has been identified, draw a perpendicular horizontal line pointing to the problem.

Step 3: Determine the major causes of the problem.

Identify the major causes of the problem that have been identified and list each major cause in a box

around the main line. Then draw an arrow pointing toward the main line.

Step 4: Determine the minor causes of the problem.

Minor causes are the causes associated with each major cause. Isolate each major cause and determine

all the factors that contribute to each major cause. Then list each minor cause around the main line.

Then draw an arrow pointing to the major cause.

Step 5: Identify the sub-causes for each minor cause.

The primary purpose of the cause and effect diagram is to illustrate the interactions among various

causes of variation in a given process. Therefore, it is necessary to break each cause down, in a step-by-

step fashion, from the most major to the most minor aspects of each cause. For example, if equipment

is listed as the major cause, a piece of equipment could be listed a minor cause; the condition of the

equipment could be a sub cause; and the measurements or characteristics or calibration could be another

sub cause. List all of the sub causes around the minor cause and draw an arrow from the sub cause to

the minor cause to illustrate their relationship.

Step 6: Review the cause-and-effect diagram.

When you review the diagram, be sure that all of the items contributing to the problem have been

identified.

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SECTION XVII

REVISION NO. 14


PAGE 17- 5

17.3 DOCUMENTATION

Documentation of corrective action and quality improvement will be in the form of System Improvement

Forms (SIF) (See Figure 9), Complaint Forms and Corrective Action/Quality Improvement Reports.

17.3.1 Any person can initiate a Corrective Action and Quality Improvement measure. System Improvement

Forms are available through each department supervisor and the QA Officer. Each field on the SIF

must be completed or addressed.

Field Information

SIF # {SIF}-{Date}-{Extension}: Enter SIF-date (MM-DD-YY) - extension = 01, 02, 03.

Initiated by: Anyone can initiate.

Date: Date of initiation of the form.

Responsible party for restoring the system: Either a person or group of persons.

Non-Conformance type: Circle the category, which best describes the problem.

Work stoppage Required? Yes/No Client Notification Required? Yes/No Authorized by Date

Description/Observation of Non-Conformance/Non-Performance: Identify the problem.

Underlying Cause: Describe the root cause.

Corrective Action/Quality Improvement: Document corrective procedures or quality improvement

suggestions.

Client Notification: Company Name, Contact Name, Date Contacted

Client Code: Information can be found in the LIMS.

Project Code/Name: Information in Project checklists and Project Quotes. See Client Services

Description of how client=s work was impacted

Verification of corrective procedures: Proof that system is in control.

Comments:

Date system returned to a controlled status: Date after evidence proves system is in control.

Initials of person closing corrective action: Either the person(s) responsible for corrective action or

pertinent department supervisor.

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SECTION XVII

REVISION NO. 14


PAGE 17- 6

SIF Processing

1. Notifying department supervisor and QA Officer. (Quality Improvement suggestions will be

discussed during supervisor meetings)

2. Close the CA/QI task (complete the SIF)

3. Submit the original SIF to the QA officer (Keep a copy)

4. SIF information is entered into a database.

17.4 CORRECTIVE ACTION/SYSTEM IMPROVEMENT FORM

A corrective action process is being implemented in a QAPP/QAPM to address issues identified in a system

and prevent the reoccurrence of similar issues. BC Laboratories, Inc. (BCL) system issues are being tracked

through corrective action/system improvement form (SIF). All corrective action issues occurred should be

handled through SIFs (customer complaint, internal audits) nonconformance of external assessments. SIFs are

tracked into SIF spreadsheet and hard copy to be filed in a binder. SIF/corrective action completion varies by

extent of the problem and main focus will be to resolve corrective action in a timely manner.

17.5 FOLLOW UP

In cases where data of questionable quality has been submitted, the client must be advised by written

notification. Research must be done to verify the scope of the problem in order to notify affected clients. The

Client Service Representative or QA Officer will be responsible for the correspondence and closure of each

matter.

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SECTION XVII

REVISION NO. 14


PAGE 17- 7

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SECTION XVII

REVISION NO. 14


PAGE 17-8

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SECTION XVII

REVISION NO. 14


PAGE 17-9

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QA REPORTS TO MANAGEMENT

SECTION XVIII

REVISION NO. 8


PAGE 18-1

18.0 QUALITY ASSURANCE REPORTS

Quality Assurance reports, prepared by the Quality Assurance Officer, are issued on a quarterly basis. The

purpose of these quarterly updates is to give an indication of overall laboratory performance and quality of work.

These reports contain information pertaining to the overall performance of the laboratory. Annual internal audit

reports are also completed to measure laboratory performance during the previous three month spans.

Information is gathered from internal and external audit results, control charts, monitoring programs and

supervisor/analyst interviews. Situations such as equipment malfunctions, new or updated QC techniques, revised

analytical procedures, corrective action activities, and any significant QC or performance evaluations will also be

addressed in the report. Copies of these reports are available upon request.

The QA Officer maintains a direct line of communication with upper management to relay quality related

information, therefore eliminating conflict of interest influence from concerned parties.

Note: This section was reviewed on 01/08/16 (No changes were made)

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SUPPLIERS / SUBCONTRACTORS

SECTION XIX

REVISION NO. 9


PAGE 19-1

19.0 SUPPLIERS

All supplies, devices and instrumentation purchased by BC Laboratories must meet requirements, set by BC

Laboratories and suppliers, as to their intended use. Methods for acceptance include:

1) Review of manufacturing process control data.

2) Source verification.

3) Receipt inspection.

4) Pre-installation and post installation testing.

5) Review of certificates and conformance.

6) Pilot runs.

Before a purchased item can be used; procurement specification, inspection and test requirements are to be

satisfied.

19.1 QUALIFICATIONS

Products of suppliers must conform to known performance standards or compare against recognized

referenceable specifications.

Standards

NIST traceable.

Certificates of Constituency.

Lot numbers.

Expiration dates.

Reagents

NIST traceable.

Certificate of Analysis (Impurity tolerances).

Lot number.

Expiration date.

Containers

Certificates of Analysis (if applicable)

Volume checks (if applicable)

Bias (acceptable for intended use)

Integrity (breakage, leaks, etc.)

Devices

Meets acceptable tolerances (manufacturer, BC Laboratories)

Secondary supply acceptable (pipette ends, tubing, etc.)

Acceptable for intended use.

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SECTION XIX

REVISION NO. 9


PAGE 19-2

Instrumentation

Method requirements.

Manufacturer requirements.

Acceptable for intended use.

Secondary supply acceptable.

Clerical

BC Laboratories requirements for intended use.

19.2 PROCESS

Purchases are initiated by persons completing requisition forms, which can be obtained from department

supervisors. The department supervisor will review the prospective purchase and if acceptable, will

approve the purchase. When purchases are received, the department supervisor or QA/QC department will

inspect the item(s) and conduct qualification procedures. The receiving of the purchased item(s) are

confirmed by Accounts Receivable.

19.2.1 Reagent Qualification - When reagents are received, the Fitness for Use Program will initiate testing

as appropriate for the intended use of the material that may affect the quality of environmental test

for cleanliness. All testing must be verified and approved before materials can be used, unless

documentation can be produced by the manufacturer which will validate purity. For DoD ELAP

(Navy) projects no target analytes are detected above 2 the PQL.

19.2.2 Standard Qualification

Standards which have been purchased from a particular vendor for the first time will be cross

checked against the standard in use to validate its accuracy and to verify purity. The responsible

analyst will contact the Department Supervisor or the QA Officer after completion of the

comparability study. All testing must be verified and approved before standard can be used, unless

documentation can be produced by the manufacturer, which will validate purity.

19.2.3 Support Equipment Qualification

Support equipment will be checked for fitness of use through performance checks conducted by

pertinent analysts and/or the QA Officer. Conformance to manufacturer's specifications and tolerances

will be used to access fitness.

19.2.4 Instrumentation Qualification

Instrument performance will be accessed through performance evaluation sample analyses and an

MDL studies. Department supervisor with one or two analysts are trained on instrument operations

by a manufacturer's representative. Verification of fitness will be validated through an initial

demonstration of competency.

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SECTION XIX

REVISION NO. 9


PAGE 19-3

19.3 SUBCONTRACTORS

Subcontractors must meet or pass the following requirements:

1) Certification for the analytes or tests of interest.

2) PE Sample or Parallel Samples (Submitted by BC Laboratories).(if available)

3) Acceptable QAPP, SOQ and/or pertinent SOP.

4) Acceptable staff. (Experience / academics)

5) WP/WS PE sample results.

Approvals from clients must be verified before the use of a subcontract laboratory. Our clients may have

policy or project specific requirements regarding subcontractors. The DoD ELAP (Navy) policy requires

that samples be subcontracted only to other DoD ELAP (Navy) approved laboratories. The DoD ELAP

(Navy) must be advised in writing of any plans to subcontract sample. Please refer to DoD QSM version

4.2, June 2003.

All BC Laboratories certified analytical reports reference subcontract work if applicable, by flagging

subcontracted work appropriately. The original report from the subcontract lab is included in the data

deliverables package.

Subcontractors will be assessed on an annual basis by our obtaining of annual PE results conducted through

the state or reputable auditing firms, subcontractor status will be defined and maintained by the QA Officer.

Status Types: Prepared - All information acceptable, All PE samples acceptable, No associated

complaints.

Acceptable - All information acceptable, All PE samples acceptable, complaint on file.

Pending - Incomplete information and/or incomplete performance rating.

Not acceptable - Incomplete information, PE=s not acceptable.

Note: This section has been reviewed on 1/08/16 (No changes were needed

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SECURITY

SECTION XX

REVISION NO. 8


PAGE 20-1

20.0 SECURITY

20.1 Facility

Facility security is assured through controlled limited access and a subcontracted security monitoring system. All

doors except the front door are locked during normal daylight working hours. Facility access after the first shift via

the front entrance is controlled by LOGIN personnel or the swing shift team leader. This door is locked at 1800

hours. Entrance door in the back of the lab is equipped with a combination type lock to prevent access by

subcontractors and any undesirable. All entrances have signs posted which say "Authorized Personnel Only",

"Protected Area, No Trespassing" or "Employees Only".

A security alarm system, which is equipped with motion sensors, smoke detectors and forced entry sensors, is

maintained by Kern Securities, Inc. Initial entry and final exit of the facility is acknowledged by access code

and password. Kern Securities representatives will call the lab in cases of unusual activity.

20.2 The Perimeter

A chain link fence surrounds the back parking lot of the laboratory grounds. Both gates of the fence are

locked at 1800 hours by swing shift personnel.

20.3 Visitors

All visitors are required to sign the visitor=s log which is kept by the receptionist. Information on this log

includes the visitor's name, the time of entrance and exit from the lab, and the organization which the visitor is

affiliated. Visitors must have proper personnel protective equipment before being escorted into the operations

area.

20.4 Sample Storage

Samples are stored in refrigerators throughout the lab. Access is granted to all pertinent lab personnel.

Custody documentation is in the form of refrigerator logs which must be completely filled out prior to

receiving samples. The archive refrigerator can be used for high security sample storage. In order to access

high security samples, each employee must contact the LOGIN Supervisor or the lead sample custodian. The

employee will then be escorted to the archive refrigerator where custody procedures can take place.

Procedures are outlined in the LOGIN SOP. Custody of extracts and digests remain under preparation

technicians until these prepared items are submitted to analysts. Analysts who assume possession of extracts

and/or digests will take responsibility for the care and security of the aforementioned items. Once analyses

are completed, the analyst will initiate digest and extract storage and/or disposal procedures.

20.5 Confidential Information

20.5.1 Submission files

Maintenance of submission files is the responsibility of the Data Filing Clerk. In order to access a

submission file, an employee of the laboratory must complete custody procedures by signing an out

card. Submission files should be returned as soon as possible.

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SECURITY

SECTION XX

REVISION NO. 8


PAGE 20-2

20.5.2 Raw Data

Maintenance of archived raw data is the responsibility of the QA Department. In order to access raw

data, an employee of the laboratory must complete custody procedures by completing an out card.

QA personnel will retrieve the data as requested. Data should be returned as soon as possible. Raw

data remains under secured conditions in on-site sea trains and in the raw data storage room at 4116

Atlas Ct in Bakersfield.

20.6 Access and Modification of Data

Change of data must be accompanied by some form of documentation to provide an audit trail.

20.6.1 Data prior to client submittal

20.6.1.1 Bench level

Data modifications are acknowledged by following proper correction techniques:

1) Line through the data being modified

2) Record the modified information

3) Record the date of modification and initial accordingly

4) Use indelible ink

Following through the reporting process to find any potential impacts associated with the

modification(s).

20.6.1.2 Clerical Level

Follow the same correction procedures as listed under 20.6.1.1 whenever applicable.

Changes made to certified analytical reports (CARs) are tracked by the LIMS, thus when

submitting CARs to data entry for corrections, it is not necessary to acknowledge by dating

and initialing modified results. Since modified CARs must be approved by a supervisor,

the original report must accompany the modified report to illustrate change of information

prior to approval signature.

20.6.2 Submitted Data

Changes made to reported data is tracked electronically by the LIMS and clerically by the completion

of AAltered Completed Files Forms.@

20.6.2.1 Bench Level

Procedures outlined in Section 20.6.1.1 are followed. A System Improvement Form may

be initiated to document necessary corrective procedures.

20.6.2.2 Clerical Level

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SECURITY

SECTION XX

REVISION NO. 8


PAGE 20-3

Modified reports are acknowledged by labeling each report as "revised" near the laboratory

sample ID. Revisions are sequentially numbered as necessary. Refer to the Data Control

SOP for more detailed procedures.

20.7 LIMS Audit Trail

All modifications to reports and processed data is tracked by the LIMS. Each morning all data changes are

printed by the LIMS Department. These records are organized and maintained by the LIMS department until

submittal to the QA department for final storage.

Note: This section has been Reviewed on 01/08/2016 (No Changes were made)

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BC LABORATORIES


CODE OF ETHICS POLICY

SECTION XXI

REVISION NO. 8


PAGE 21-1

21.0 CODE OF ETHICS

21.1 It is imperative that all staff members of BC Laboratories agree to abide to the following code of ethics.

To cooperate in elevating and maintaining the professional status of our laboratory.

To deal honestly and openly with our clients, the public and fellow employees.(Appendix B F)

To abide with all components of the Ethics and Integrity Agreement (Appendix B F) at all times.

Under no circumstances will dishonest action be tolerated at BC Laboratories, Inc. Irreparable damage can

result from dishonest acts, thus immediate termination may result for anyone falsifying data, concealing poor

data, concealing mistakes, and/or providing misleading or inaccurate information. Some examples of

falsifying data include:

Knowingly reporting inaccurate preparation and/or analysis date/times

Altering data to pass quality control requirements

Reporting data that was never properly produced

Purposefully not following known BC Laboratories, Inc. procedures

All staff members must tell the truth at all times regarding analytical and informational data. We can deal

with mistakes and isolated incidents of late and/or rejected data, but we cannot cope with acts of dishonesty

that would put the laboratory in peril.

We encourage that all staff members contact the QA Officer if any questions arise on whether or not

questionable actions are appropriate or not. Resolution may come at this level or may be handled at the

President level.

Remember that a single dishonest act can cast suspicion on the lab and everyone who works here. One lie can

lead to another which then increases exposure, thus leading to more dishonest acts. No amount of corrective

action or quality control can erase doubts of clients or potential clients after an act of deception. In our

industry, honesty and integrity are of utmost importance and our clients depend on us to produce defensible

data.

All staff members (BCL Personnel) are required to attend an Ethics training (Module D) conducted by BC

Laboratories, Inc. on an annual basis.

Additionally, all staff members must comply with the following sections involving client confidentiality and

corporate issues.

21.2 Confidential Information

Employees may become privy to confidential information (that is , information not available to the public)

concerning the affairs and business transactions of BC Laboratories, Inc. , its present and prospective

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BC LABORATORIES


CODE OF ETHICS POLICY

SECTION XXI

REVISION NO. 8


PAGE 21-2

customers, its suppliers, its shareholders and other employees. Safeguarding confidential information is

essential to the conduct of the company=s business. Therefore, caution and discretion are required in the use

of such information. It should be shared only with those who have a legitimate or legal need to know.

Information concerning a customer may be released, with the consent of the customer involved; to third

parties, organizations, or governmental bodies that seek it. All other requests for information concerning a

customer ( other than routine credit inquiries, including requests pursuant to legal process (such as subpoenas

or court orders), must be promptly referred to the President. No information may be released, nor should the

customer involved be contacted until so authorized by the President. Failure to follow these procedures can

result in civil penalties against BC Laboratories, Inc.

21.2.1 Client Data Confidentially

During the course of daily work employees may have access to analytical results. In order to maintain

complete client confidentially; employees agree not to copy, reproduce, or communicate in any

manner these results to anyone but the party indicated on the COC unless proper approval has been

granted. Additionally any work approved to leave the laboratory or information gathered outside of

the laboratory regarding clients shall not be copied and shall be brought back to the Lab in its entirety.

Any notes, pages, or reports no longer required are to be shredded on site.

21.3 Competition

In its many business activities, the company engages in vigorous, but fair and ethical, competition.

Discussions and agreements, oral or written, with competitors concerning pricing or other competitive

practices are not permitted. Care should be taken to ensure that, in meetings of trade associations and other

industry groups, competitive practices are not discussed without prior legal clearance.

21.4 Contributions and Donations

The company=s policy regarding contributions and donations provides that disbursements of corporate funds

will be made in full compliance with all applicable laws, and that no disbursements of corporate funds will be

made, either directly or indirectly to any organization which fosters or encourages racial, religious, class or

other prejudices.

21.5 Reporting of Irregularities

Employees who become aware of known or suspected irregularities should report them promptly and

confidentially to their supervisor who is responsible for reporting for further handling by the following

organizations:

21.5.1 Internal Auditing

Is responsible for those investigations requiring account and/or auditing techniques into such matters

as embezzlement, misappropriation of company property involving the alteration of company records,

improprieties by employees and persons in contractual relations with BC Laboratories contractors,

consignees, agents, etc.....

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SECTION XXI

REVISION NO. 8


PAGE 21-3

21.5.2 Board of Directors

Is responsible for those investigations requiring skills in the techniques of detection, interrogation and

surveillance concerning such matters as bribes, burglaries, conflicts of interest, misappropriation of

company property not involving the alteration of company records, unlawful use of confidential

information, commingling of products, sales of competitors= products under the BC Laboratories

label, threats or acts of violence/terrorism, and vandalism.

Note: This section has been reviewed on 1/08/16 (No changes were needed)

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APPENDICES

Appendix A SOP Listing

Appendix B Established MDL/PQL’s

Appendix C Employee Evaluation

Appendix D QC Logic Flow Diagrams

Appendix E Process Flow Diagrams

Appendix F Ethics and Data Integrity Agreement

Appendix G Comments (flags)

Appendix H Employee SOP Acknowledgement and Agreement

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APPENDIX A

APPENDIX A

S:\WP DOCS\WORD Doc\LAB_DOCS\QAPP\QAPPA010816

REVISED 01/22/16

PAGE A-1

SOP #

SAVED AS

TITLE

REV.

REVIEWED DATE

BCDOC002

COCR4

Chain of Custody

4

03/30/15

BCDOC004

XLOGR6

Extraction Log

6

07/27/15

BCDOC007

VOL_GCRLR6

Volatiles GC Run Log

6 01/19/16

BCDOC008

VOL_STANR5

Volatiles Standard Log

5

01/19/16

BCDOC010 DETERTCPR1 1, 2, 3 – TCP DRINKING WATER BY P & TRAP

GC/MS

1 09/25/15

BCDOC011 XREAGLOGR2 Extractions Reagent Log 2 07/27/15

BCDOD001 DODR2 Department of Defense (DOD) Compliance 2 09/15/15

BCDOE004

REAGPFR4

REAGENT PURITY/FITNESS FOR USE

4

07/27/15

BCFS001

FSGCMSR3

EPA 8020/8240/8270

3

03/23/15

BCFS002

FSSITESPR2

Site Specific Plan for Field Service

2

03/23/15

BCFS004

FSOPEXR2

SOIL SAMPLING IN OPEN EXCAVATION

2

03/23/15

BCFS006

FSMSGR3

FIELD MEASUREMENTS ON SURFACE AND

GROUNDWATER

3

03/23/15

BCFS007

FSPMWBR3

SAMPLING MONITOR WELLS WITH A BAILER

3

03/23/15

BCFS008

FSMPDWR3

SAMPLING DOMESTIC WELLS

3 03/23/15

BCFS009

FSMPLVORCR3

SAMPLING FOR VOLATILE ORGANIC

COMPOUNDS

3

03/23/15

BCFS012

FSWATLMR1

WATER LEVEL MEASUREMENT

1

03/23/15

BCFS013

FSGENIFPR2

GENERAL INSTRUCTIONS FOR FIELD

PERSONNEL

2

03/23/15

BCFS014

FSMPLCDR2

SAMPLE CONTROL AND DOCUMENTATION

2

03/23/15

BCFS015

FSMPLCPR2

SAMPLE CONTAINERS AND PRESERVATION

2

03/23/15

BCFS016

FSGHNDPSR1

GUIDE TO SAMPLING HANDLING, PACKAGING,

AND SHIPPING OF SAMPLES

1

03/23/15

BCFS017

FSGEQUIPDR1

GENERAL EQUIPMENT DECONTAMINATION

1

03/23/15

BCFS018

FSCALIFR2

CALIBRATION & MAINTENANCE OF FIELD

INSTRUMENTS USED IN MEASURING

PARAMETERS OF SURFACE AND GROUND

WATER AND SOILS

2

03/23/15

BCGEN004

ALKALSOPR7

Carbonate, Bicarbonate, Alkalinity, 310.1/SM 2320B

7

12/03/15

BCGEN005

COLOR5

Color/ 110.2/SM 2120B

5

11/30/15

BCGEN007

DSOXYGENR5

Dissolved Oxygen/360.1 SM4500-06

5

11/30/15

BCGEN009

SETTEABLR7

Settleable Solids/160.5/SM 2540

7

* 11/30/15

BCGEN010

CHLORINER6

Residual Chlorine/330.4/SM 4500-CLF

6

12/09/15

BCGEN011

ECR6

Specific Conductance (EC)9050 120.1 SM 2510B

6

11/30/15

BCGEN013

TDSR8

Total Dissolved Solids Filterable Residue 160.1/SM

2540C

8

12/09/15

BCGEN014

TURBIDITR5

Turbidity/180.1/SM 2130B

5 01/20/16

BCGEN016

WCBACTERREV13

Bacteriology

13 12/09/15

BCGEN017

BODR8

Analyte: Biochemical Oxygen 405.1 SM5210B

8

01/20/16

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APPENDIX A

APPENDIX A


REVISED 01/22/16

PAGE A-2

SOP #

SAVED AS

TITLE

REV.

REVIEWED DATE

BCGEN020

SULF376_1R7

Sulfide/376.1

7 11/30/15

BCGEN021

MBASR8

MBAS/EPA 425.1/ SM 5540C

8

12/18/15

BCGEN022

TSSR6

Total Suspended Solids/EPA 160.2/SM 2540 D

6 12/18/15

BCGEN024

ODOR6

Odor/EPA 140.1/SM 2150

6

12/09/15

BCGEN026

COD410_4R8

Chemical Oxygen Demand Colormetric,

Manual/410.4/SM 5220D

8

12/18/15

BCGEN033

PHREV8

PH/EPA 150.1/9040

8

12/09/15

BCGEN035

REACTSULREV7

Reactive Sulfide\\EPA Method 7.3.4.1

7

12/18/15

BCGEN039

WCTOCR15

Total Organic Carbon (TOC)/ SW 5310C/EPA 415.1

15

12/09/15

BCGEN040

SULF376_2R7

Sulfide Method 376.2

7

12/18/15

BCGEN043

160.4R5

Fixed and Volatile Solids, 160.4/SM 2540E

5

12/09/15

BCGEN044

GLASSWR6

General Glassware Washing

6

12/18/15

BCGEN046

TOTRESR4

Total Residue 160.3 SW 2540B

4

12/18/15

BCGEN048

EPA300R10

Determination of Anion in water and solid by Dionex IC

DX500/EPA 300.0

10 11/30/15

BCGEN049

EPA314R9

Perchlorate / 314.0

9

12/18/15

BCGEN050

DEWAPR2

Deionized Water Production

2

11/30/15

BCGEN051

KLORTH_365.1R5

ORTHOPHOSPHATE EPA 365.1 5 11/30/15

BCGEN052

KLHEXACROMR6

HEXAVALENT CHROME

6

11/30/15

BCGEN053

PhSOLIDR4

EPA METHOD 9040B, 9045C

4

12/09/15

BCGEN055

KLNOR5

KONELAB NITRITE NITROGEN EPA 353.2

5

01/08/16

BCGEN056

HEXCR_218_6R7

HEXAVALENT CHROMIUM EPA 218.6/7199

7

02/18/15

BCGEN057 KLNCYR7 KONELAB CYANIDE EPA 335.2/335.4/9012A 7 11/30/15

BCGEN058 SC_NO3-NR4 SMARTCHEM,NITRATE-NITRITE/EPA 353.2 4 11/30/15

BCGEN059 SC_TKN-NR5 SMARTCHEM TOTAL KJELDAHL NITROGEN 5 12/18/15

BCGEN060 SC_TOT_PR4 SMARTCHEM TOTAL PHOSHPHOROUS EPA

365.4/SM 4500-P

4 11/30/15

BCGEN061 SC_NH3-NR4 SMARTCHEM AMONIA-NITROGEN/EPA 350.1 4 01/08/16

BCGEN062 KLPHENOLR5 KONELAB TOT. Rec. PHENOLICS EPA 420.4 5 11/30/15

BCGEN063 REACTCYANR1 REACTIVE CYANIDE\\EPA METHOD 7.3.3.2 1 11/30/15

BCGEN065 METROHMR2 ELECTICAL CONDUCTIVITY, pH, ALKALINITY //

EPA 9050/120.1/SM 2510B, EPA 9040/150.1/SM

4500HB, EPA 310.1 / SM 2320B

2 11/30/15

BCGEN066 CO2_R1 Free Carbon Dioxide in Water 1 01/20/16

BCGEN067 ORP_R1 Oxidation-Reduction Potential in Water//ASTM D1498 1 01/20/16

BCGEN069 FLASHPOINTR0 Flash Point by Pensky-Martens Closed Tester/ASTM D-

93, EPA Method 1010

0 01/20/16

BCGEN070 IGNIT_EPA1030R0 IGNITABILITY OF SOLIDS-EPA Method 1030 0 04/01/15

BCGEN071 EPA300M-FATTYAR0 DETERMINATION OF ORGANIC ACIDS IN

WATER BY DIONEX IC/EPA 300.0M

0 04/20/15

BCGEN072 pHSM4500-HBR0 DETERMINATION OF ORGANIC ACIDS IN 0 12/09/15

UNCONTROLLED COPY



APPENDIX A

APPENDIX A


REVISED 01/22/16

PAGE A-3

SOP #

SAVED AS

TITLE

REV.

REVIEWED DATE

WATER BY DIONEX IC/EPA 300.0M

BCHRC001

HUMRSR4

HUMAN RESOURCE COORDINATOR

4

11/16/15

BCLIMS001 BASR1 BATCHES AND SEQUENCE 0911 - 0913 1 06/01/15

BCLIMS002 DESR1 DATA ENTRY 0921 - 0923 1 06/01/15

BCLIMS003 BCELMCALCR3 BCELM CALCULATORS 0931 - 0932 3 06/01/15

BCLIMS004 DTSR3 DATA TOOL 0941 3 06/01/15

BCLIMS005 DRSR3 DATA REVIEW 0951 - 0955 3 06/01/15

BCLIMS006 SCSR2 SAMPLE CONTROL 1030 - 1035 2 06/01/15

BCLIMS007 BARCODER1 BAR CODE 1 06/01/15

BCLIMS008 RDSR0 Data Processing-0960-0964 0 06/01/15

BCLIMS009 EDSCLPR0 CLP REPORTING 1060-1064 0 06/01/15

BCLIMSOP LIMSOPR10 LIMS MANUAL 10 04/20/15

BCMDL001 MDL_SSR1 Lab-Wide MDL Spreadsheet use 1 12/10/15

BCMET010

HG_747015

MERCURY (Hg) // EPA 7470A/EPA 245.1

15

12/09/15

BCMET011

HG_7471R19

MERCURY (Hg) // EPA 7471 / 245.5

19

12/09/15

BCMET013

6010METALR19

Determination of Metals and Trace Elements in Water

and Waste Waters by ICP-AES 200.7/6010

19

02/18/15

BCMET025

MOISTURER3

% Moisture/ % Solids

3

04/01/15

BCMET037

6100ELANR13

EPA METHOD 200.8 USING ELAN 6100 ICP-MS 13

12/09/15

BCMET038

EPA6020R12

EPA6020

12 05/19/15

BCMGT001

MGTRO

Management Review

0

01/19/16

BCMGT002

DATAINTRO Data Integrity Policy

0

01/19/16

BCMIC001

WORKLOADR3

Assessment and Handling of new additional work

3

03/30/15

BCMIS002

WASTEDR12

Waste Disposal

12

04/02/15

BCMIS007

XROUMAINR4

Extractions Routine Maintenance

4

07/27/15

BCMIS009

SHIPPINGR9

Shipping

9

03/30/15

BCORG001

549.2R7

EPA 549.2 Diquat and Paraquat

7

01/21/16

BCORG002

515815R13

EPA 515.1, 615, 8150B, 8151

13

09/18/15

BCORG003

TPHGASB21

TPH(GA) BTEX/8015M,8020, and 8021B

21

08/20/15

BCORG004

8140R10

EPA METHOD 8140/8141/614

10

01/20/16

BCORG005

TPHFELR14

TPH(FUELS)/ EPA 8015M

14

01/19/16

BCORG006 548R6 Determination of Endothal in drinking water 6 01/19/16

BCORG008

525_2R5

Determination of Organic Compounds in Drinking

Water by Liquid-Solid Extraction and Capillary Column,

Gas Chromatography/Mass Spectrometry.

5

09/18/15

BCORG009

504R12

EPA 504.1

12 01/21/16

BCORG011

8310REV14

Polynuclear Aromatic Hydrocarbons by HPLC/EPA

8310/610

14 01/21/16

BCORG014

508R15

Organchlorine Pesticides and PCB=s by Gas

Chromatography EPA 508/608/8080/8081

15

01/20/16

UNCONTROLLED COPY



APPENDIX A

APPENDIX A


REVISED 01/22/16

PAGE A-4

SOP #

SAVED AS

TITLE

REV.

REVIEWED DATE

BCORG016 ZHEREV7 Zero Head Space Extraction for Volatiles/EPA 1311 7 09/25/15

BCORG018

632R5

High Performance Liquid Chromatography for

Carbamate and Urea Pesticides in Wastewater/EPA 632

5

09/18/15

BCORG019

8082R14

Gas Chromatography for Polychlorinated Biphenyls

EPA 8082

14 01/21/16

BCORG020 625827R16

GC/MS for Semi-Volatiles/EPA 625/8270

16

4/14/15

BCORG025

5035R6 Closed System Purge & Trap (5035) 6

01/19/16

BCORG026

EPA1664R9

Method 1664

9

01/08/16

BCORG029

8330R10

Nitroaromatics & Nitroamines by High Perfomance

Liquid Chromatography Method 8330

10

09/18/15

BCORG040

ORGCR3

ORGANIC GLASSWARE CLEANING

3

09/25/15

BCORG042

525_2SPER3

SOLID PHASE EXTRACTION/EPA METHOD 525.2

3

04/13/15

BCORG045

8260TPHR6

EPA METHOD 8260 TPPH

6

01/06/16

BCORG047

ExprescreeningR1

Extract Pre-screening

1

09/25/15

BCORG049

624R14

EPA METHOD 624

14

07/15/15

BCORG051

8240_8260R11

EPA METHOD 8240/8260

11

08/20/15

BCORG053

8270SIMR5

EPA 8270 SIM PNA

5 09/18/15

BCORG054

524R8

EPA 524.2

8

12/07/15

BCORG055

GCMSLUFTR4

GC/MS FOR SEMI-VOLATILES//LUFT TPH

4

09/18/15

BCORG056

ORGVAPR2

MERCURY AND ORGANIC VAPOR MONITOR

ANALYSIS

2

11/16/15

BCORG057 SCREENXPLR0 SCREENING FOR EXPLOSIVES IN SOIL 0 01/21/16

BCORG058 DETERHAA5R4 DETERMINATION OF HAA5 IN WATER BY

LIQUID, LIQUID MICROEXTRACTION

4 10/16/15

BCORG059 METHETHR3 EPA 8015B Methanol-Ethanol 3 09/18/15

BCORG060 556R3 EPA METHOD 556 3 9/18/15

BCORG061 AIRTO14_15R3 AIR TESTING METHOD TO-14A AND TO-15 3 10/16/15

BCORG062 CANISTER2 CANISTER CLEANING 2 9/25/15

BCORG063 DYNAMICR0 DYNAMIC DILUTION 0 09/25/15

BCORG064 FIXGASR4 FIXED GAS ANALYSIS 4 08/20/15

BCORG065 SYRINGER1 Glass Syringe Accuracy Determination 1 9/25/15

BCORG066 SULF307.91MR1 307.91M SULFUR COMPOUNDS METHOD 1 10/16/15

BCORG067 RSK175M_R3 RSK-175 -Dissolved Gas Analysis in Water for

Methane/Ethane/Ethene

3 01/06/16

BCORG068 TO3-R1 AIR TESTING METHOD TO-3 1 08/20/15

BCORG069 AK101R1 AK 101: Determination of Gasoline Organics 1 01/19/16

BCORG070 AK102_103R2 AK102: Determination of Diesel Range Organics 2 01/19/16

BCPREP001

EX3510R15

Extractions-Waters by EPA 3510 & All Methods

15

07/27/15

UNCONTROLLED COPY



APPENDIX A

APPENDIX A


REVISED 01/22/16

PAGE A-5

SOP #

SAVED AS

TITLE

REV.

REVIEWED DATE

BCPREP002

OR3550R13

Organics Extractions - EPA 3550/Ultrasonic Extractions

All Methods

13

07/27/15

BCPREP004

3580RV10

Organics Extractions/EPA 3580//Dilution Extraction/All

Methods

10

01/21/16

BCPREP006

3010R10

Acid Digestion of Aqueous Samples and Extracts for

Total Metals for Analysis by ICP Spectroscopy/Method

3010A

10

12/09/15

BCPREP008

TCLP_EXTR2

TCLP Extraction

2

12/18/15

BCPREP009 SPLP_EXTR0 Synthetic Precipitation Leaching Procedure EPA 1312 0 11/30/15

BCPREP011 WET_EXTR2 Wet Extraction 2 01/04/16

BCPREP013

EPA9095R3

Paint Filter Liquids Test / EPA Method 9095B

3 03/16/15

BCPREP014

SPLITR6

Splitting and Refrigerating Samples

6 05/19/15

BCPREP015

3050R17

ACID DIGESTION OF SEDIMENTS, SLUDGES AND

SOILS FOR ANALYSIS OF TOTAL METALS BY ICP,

AND ICP-MS SPECTROSCOPY / METHOD 3050B

17

11/24/15

BCPREP016

SILICA-3630cR5

Silica Gel Cleanup for PAH=s\EPA 3630C

5

07/27/15

BCPREP017

2002BLOKR6

Hot Block Digestion of Water Total Recoverable Metal

Method 2002.2

6

12/18/15

BCPREP018

FREELIQDETR2

Free Liquid Determination

2

01/04/16

BCPREP019 3060AR1 EPA METHOD 3060A 1 01/04/16

BCPREP020

SILICA-3630MR1

Silica Gel Cleanup for EPA 3630 Modified

1

09/25/15

BCPREP021

EPA1320R0

METHOD 1320 MULTIPLE EXTRACTION

PROCEDURE

0

12/02/15

BCPROC001 PROCPR7 PROCUREMENT PROCESS 7 01/15/16

BCQC002

QCTHRMR19

QC - Thermometer Monitoring

19

09/15/15

BCQC005

QCFRDGR16

QC - Refrigerator Monitoring

16

09/15/15

BCQC007

QCOVENR13

QC - Oven Monitoring

13

09/15/15

BCQC008

QCBLNCR17

QC - Balance Monitoring

17

09/15/15

BCQC009

QCINTAUR8

INTERNAL AUDITS

8

09/15/15

BCQC010

QCSUVEASAR8

Supply Vendor and Analytical Subcontractor Approval

8 09/15/15

BCQC011

QCDILMONR5

QC-DILUTER MONITORING

5

09/15/15

BCQC012 QCCLPR3 CONTRACT LABORATORY PROTOCOL 3 09/15/15

BCQC013 QCEPPENDORFR0 QC - EPPENDORF PIPETTE CALIBRATION 0 01/05/16

BCREC001

RECEPTR6

RECEPTIONIST

6

03/30/15

BCSAF001

EMERGRESR9

Emergency Response and Evacuation Plan

9

03/12/15

BCSAF002

FIRPREVR2

Fire Prevention Plan

2

04/01/15

BCSAF003

RESPREVR6

Respiratory Prevention Plan

6

01/19/16

BCSAF004

LABCRAGTRCKR5

Laboratory Sample/Laboratory Waste Cradle to Grave

Tracking

5

04/01/15

BCSAF005

LABSMPCTCKR4

Laboratory Sample Cradle to Grave Tracking

4

04/01/15

UNCONTROLLED COPY



APPENDIX A

APPENDIX A


REVISED 01/22/16

PAGE A-6

SOP #

SAVED AS

TITLE

REV.

REVIEWED DATE

BCSAF006 FORKLIFTR2 FORKLIFT OPERATION & TRAINING 2 11/16/15

BCSAF007

SAFETRAINR2

SAFETY MODULE TRAINING 2 04/01/15

BCSAF008

QLFITESTR1

Qualitative Respiratory Fit Testing (QLFT)

1

11/16/15

BCSAF009

BENZAWARER0 BENZENE AWARENESS PROGRAM

0

01/19/16

BCSAF010

BLOODBPECPR0

Blood Borne Pathogen Exposure Control Plan

0

01/19/16

BCSAF011

LADDERSAFR0

Portable ladder safety 0 04/01/15

BCSAF012

H2SPROGR0

Hydrogen Sulfide (H2S) Safety Program

0

01/19/16

BCSAF013

HEATIPROGR0

HEAT AND ILLNESS PREVENTION PROGRAM

0

07/07/15

BCSAL001

SALESR2

ACCOUNTS RECEIVABLE

2

04/01/15

BCSAL002

Sales&MrkngR0

SALES AND MARKETING

0

01/21/16

BCSAM002

LOGISLR15

Sample Log-in Prep

15

03/30/15

BCSAM005

LOGISRV20

Sample Receiving

21 01/11/16

BCSAM009 EMPLTRNGR14 Employee Training 14 11/16/15

BCSER001

BOTPRER14

Bottle Prep 14

12/7/15

BCSER002

CUSTCOMMR5 Customer Communications

5

03/30/15

BCSER003

CONFIDENR4

Customer Confidentiality

4

03/30/15

BCSER004

COURIER4

Courier Service

4

03/30/15

BCSER006

COCTRACKR3

COC & Tracking

3

03/30/15

BCSER007

DATAPAKR5

Data Packing

5

03/30/15

BCSER012

BAY&NCAR2

Courier Service

2

03/30/15

BCSER013

BENCHCMR3

Customer/Project Specific Information Communications

to the Bench/Analysts Level

4

03/30/15

BCSER014

LLNLEDDR1

LLNL EDD TRANSFER

1 03/30/15

BCWOR001

WORDPROCR14

Word Processing Department

14

04/01/15

D= DRAFT * = In the process of being Review

UNCONTROLLED COPY



PREFERRED DRINKING WATER METHODS FOR METALS

APPENDIX B

Revision 8

EFFECTIVE DATE 01/08/16

PAGE B-1

Please note that MDL=s change on an annual basis. Appropriate analyses are updated in Element that is affected by New

MDL study results. Please contact the QA Officer to confirm sensitivity.

SYMBOL

ANALYT

METHOD

TECHNIQUE

PQL (g/L)

MDL (g/L)

Sb

Antimony

200.8

ICP-MS

2

0.087

As

Arsenic

200.8

ICP-MS

2

0.61

Be

Beryllium

200.8

ICP-MS

1

0.14

Cd

Cadmium

200.8

ICP-MS

1

0.02

Cu

Copper

200.8

ICP-MS

2

0.35

Pb

Lead

200.8

ICP-MS

1

0.16

Hg

Mercury

200.8

ICP-MS

0.2

0.058

Hg

Mercury

245.1

CV

0.2

0.04

Ni

Nickel

200.8

ICP-MS

2

0.14

Se

Selenium

200.8

ICP-MS

2

0.23

Sn

Tin

200.8

ICP-MS

1

0.099

Tl

Thallium

200.8

ICP-MS

1

0.046

UNCONTROLLED COPY



PREFERRED DRINKING WATER METHODS FOR METALS

APPENDIX B

Revision 8


PAGE B-2

SYMBOL

ANALYTE

METHOD

TECHNIQUE

PQL (g/L)

MDL (g/L)

AS

Arsenic

200.7

.2

ICP

50

20

Be

Beryllium

200.7

ICP

10

0.37

Cu

Copper

200.7

ICP

10

1.8

Cr

Chromium

200.8

ICP-MS

3

0.85

Mo

Molybdenum

200.8

ICP-MS

1

0.19

Se

Selenium

200.7

ICP

100

9.9

Ag

Silver

200.8

ICP-MS

1

0.042

Tl

Thallium

200.7

ICP

100

24

V

Vanadium

200.8

ICP-MS

3

0.92

Mn

Manganese

200.8

ICP-MS

1

0.27

Co

Cobalt

200.8

ICP-MS

1

0.23

Zn

Zinc

200.8

ICP-MS

5

1.6

Ba

Barium

200.8

ICP-MS

1

0.33

Cr

Chromium

200.9

GFA

1

0.23

Cd

Cadmium

200.7

ICP

10

4

Ni

Nickel

200.7

ICP

10

1.8

UNCONTROLLED COPY



PREFERRED GROUNDWATER/WASTEWATER METHODS FOR METALS

APPENDIX B

Revision 8


PAGE B-3

SYMBOL

ANALYTE

METHOD

TECHNIQUE

PQL (g/L)

MDL (g/L)

Al

Aluminum

200.7

ICP

50

15

Sb

Antimony

200.7

ICP

100

14

Ba

Barium

200.7

ICP

10

1.4

Be

Beryllium

200.7

ICP

10

0.37

B

Boron

200.7

ICP

100

16

Cd

Cadmium

200.7

ICP

10

4

Ca

Calcium

200.7

ICP

50

5.9

Co

Cobalt

200.7

ICP

50

3.2

Cu

Copper

200.7

ICP

10

1.8

Cr

Chromium (3+6)

200.7

ICP

10

1.2

Cr+6

Hexavalent Chromium

7196A

Colorimetric

2

1

Fe

Iron

200.7

ICP

50

28

Mg

Magnesium

200.7

ICP

50

19

Mn

Manganese

200.7

ICP

10

3.7

Hg

Mercury

245.1

CV

0.2

.022

Mo

Molybdenum

200.7

ICP

50

5.8

Ni

Nickel

200.7

ICP

10

1.8

K

Potassium

200.7

ICP

1000

110

Ag

Silver

200.7

ICP

10

1.9

Na

Sodium

200.7

ICP

500

120

Sr

Strontium

200.7

ICP

10

0.44

Ti

Titanium

200.7

ICP

10

0.73

V

Vanadium

200.7

ICP

10

2.3

Zn

Zinc

200.7

ICP

10

6.1

UNCONTROLLED COPY



ALTERNATIVE GROUNDWATER/WASTEWATER METHODS FOR METALS

APPENDIX B

Revision 8


PAGE B-4

SYMBOL

ANALYTE

METHOD

TECHNIQUE

PQL (g/L)

MDL (g/L)

Sb

Antimony

200.8

ICP-MS

2

0.085

As

Arsenic

200.7

ICP

50

20

Be

Beryllium

200.8

ICP-MS

1

0.22

Cu

Copper

200.8

ICP-MS

2

0.48

Mo

Molybdenum

200.8

ICP-MS

1

0.087

Se

Selenium

200.7

ICP

100

9.9

Ag

Silver

200.8

ICP-MS

1

0.075

Ba

Barium

200.8

ICP-MS

1

0.084

Cd

Cadmium

200.8

ICP-MS

1

0.09

Li

Lithium

200.8

ICP-MS

1

0.11

Cr

Chromium

200.8

ICP-MS

3

0.82

Co

Cobalt

200.8

ICP-MS

1

0.073

Mn

Manganese

200.8

ICP-MS

1 0.81

Ni

Nickel

200.8

ICP-MS

2

0.49

V

Vanadium

200.8

ICP-MS

3

0.97

Pb

Lead

200.7

ICP

50

4.1

Sn

Tin

200.7

ICP

50

4.9

Cr

Chromium

200.9

GFA

1

0.13

UNCONTROLLED COPY



PREFERRED SLUDGES/WOODS/SOIL METHODS FOR METALS

APPENDIX B

Revision 8


PAGE B-5

SYMBOL

ANALYTE

METHOD

TECHNIQUE

PQL (mg/kg)

MDL (mg/kg)

Al

Aluminum

6010B

ICP

5.0

1.3

Sb

Antimony

6010B

ICP

5.0

0.5

As

Arsenic

6010B

ICP

1

0.38

Ba

Barium

6010B

ICP

0.5

0.077

Be

Beryllium

6010B

ICP

0.5

0.05

B

Boron

6010B

ICP

5

0.5

Cd

Cadmium

6010B

ICP

0.5

0.5

Ca

Calcium

6010B

ICP

25

2.5

Co

Cobalt

6010B

ICP

2.5

0.25

Cu

Copper

6010B

ICP

1

0.12

Cr

Chromium (3+6)

6010B

ICP

0.5

0.06

Fe

Iron

6010B

ICP

5

3.7

Pb

Lead

6010B

ICP

2.5

0.25

Mg

Magnesium

6010B

ICP

2.5

0.77

Mn

Manganese

6010B

ICP

0.5

.05

Hg

Mercury

7471A

CV

.16

0.012

Mo

Molybdenum

6010B

ICP

2.5

0.25

Ni

Nickel

6010B

ICP

.5

0.058

K

Potassium

6010B

ICP

50

5

Se

Selenium

6010B

ICP

1

0.51

Ag

Silver

6010B

ICP

.5

0.05

Na

Sodium

6010B

ICP

25

2.5

Sr

Strontium

6010B

ICP

0.5

0.05

Ti

Titanium

6010B

ICP

0.5

0.16

Tl

Thallium

6010B

ICP

5

0.73

V

Vanadium

6010B

ICP

0.5

0.05

Zn

Zinc

6010B

ICP

2.5

0.25

UNCONTROLLED COPY



ALTERNATIVE SOIL METHODS FOR METALS

APPENDIX B

Revision 8

EFFECTIVE DATE 01/08/16 PAGE B-6

SYMBOL

ANALYTE

METHOD

TECHNIQUE

PQL (mg/kg)

MDL (mg/kg)

Hg

Mercury

7470A

CV

0.16

0.012

UNCONTROLLED COPY



WET CHEMISTRY METHODS

APPENDIX B

Revision 8


PAGE B-7

ANALYTE

METHOD

TECHNIQUE

PQL

MDL

WATER (mg/L)

SOIL

(mg/kg)

WATER (mg/L)

SOIL (mg/kg)

Alkalinity

EPA 310.1

SM2320B

Titrimetric

4.1 mg/L as

CaCO3

NA

4.1

NA

Ammonia - N (distilled)

EPA 350.1

SM4500-NH3N

Colorimetric

0.05

10

0.025

5

Ammonia - N (distilled)

EPA 350.1

SM4500-NH3N

Colorimetric

0.05

-

0.02

-

BOD

SM 5210B

EPA 405.1

Membrane

Electrode

1.0

30

1.0

30

Bromide

EPA 300.0

IC

0.1

1

0.049

0.36

Chloride

EPA 300.0

IC

0.5

5

0.037

0.33

COD

SM5220D,

EPA 410.4

Colorimetric

25

200

3.5

100

Cyanide

EPA 335.1,

EPA335.4/9010

Color - Man

0.0032

1.0

0.005

0.5

Cyanide

EPA 335.2,

EPA335.3/9012A

Color - Auto

0.005

NA

0.0032

NA

Dissolved Oxygen

EPA 360.1

SM 4500-G

Membrane

Electrode

0.5

NA

0.5

NA

EC

EPA9050/120.1

Meter

1mhos/cm

NA

1mhos/cm

NA

Fluoride

EPA 300.0

IC

0.05

0.5

0.011

0.081

Hex. Chromium

EPA 7196A

Colorimetric

0.002

1.0

0.001

0.5

MBAS

SM5540C,

EPA 425.1

Colorimetric

0.1

0.05

0.039

0.02

Nitrate - N

EPA 300.0

IC

0.1

1

0.018

0.11

Nitrate/Nitrite-N

EPA 353.2

Colorimetric

0.1

0.5

0.05

0.12

Nitrite - N

SM4500-NO3F

EPA 353.2

Colorimetric

0.05

0.5

0.01

0.12

Phenols

EPA 420.2

Colorimetric

10

0.5

5

0.25

pH

EPA 9045

EPA 9040 / 150.1

Meter

0.05

0.05

0.05

0.05

Total phosphorus

EPA 365.4

Colorimetric

0.05

10

0.02

4

UNCONTROLLED COPY



WET CHEMISTRY METHODS

APPENDIX B

Revision 8


PAGE B-8

ANALYTE

METHOD

TECHNIQUE

PQL

MDL

WATER (mg/L)

SOIL

(mg/kg)

WATER (mg/L)

SOIL (mg/kg)

Ortho-Phosphate

SM4500-PF

EPA 365.1

Colorimetric

0.02

0.2

0.01

0.1

Residual Chlorine

EPA330.4 /

SM 4500cl F

Tit. DPD

0.1

NA

0.1

NA

Settleable Solids

SM2540F

EPA 160.5

IMHOFF CONE

0.1

NA

0.1

NA

Total Dissolved Solids

SM2540C

EPA 160.1

Grav.

10

NA

10

NA

Total Suspended Solids

SM2540D

EPA 160.2

Filter

0.5

NA

0.5

NA

Sulfate

EPA 300.0

IC

1

10

0.11

0.79

TKN

EPA 351.2

Colorimetric

0.2

40

0.1

20

TOC

SM5310C

EPA 415.1

Carbon Analyzer

1.0

NA

0.37

NA

Perchlorate

EPA 314.0

IC

0.004

.04

.00046

.003

Total Solids

EPA 160.3,SM2540B

Grav

10

NA

10

NA

Volatile Solids

EPA 160.4

Grav

10

NA

10

NA

Sulfide

EPA 376.1, 376.2,

SM4500S-D,E

Spectronic 20

Genesys

1

0.1

0.5

.05

Turbidity

EPA 180.1, SM2130B

Hach meter

0.1NT. Unit

NA

0.1 NT.

Units

NA

UNCONTROLLED COPY



ORGANIC METHODS

APPENDIX B

Revision 8


PAGE B-9

ANALYTE

METHOD

TECHNIQUE

PQL

MDL

WATER

(g/L)

SOIL (mg/kg)

WATER (g/L)

SOIL (mg/kg)

2,4-D

515/615/8151A

GC ECD

.4

.020

.012

.00098

2,4-DB

515/615/8151A

GC ECD

3

.04

.011

.002

DALAPON

515/615/8151A

GC ECD

10

.01

.58

.00058

DICAMBA

515/615/8151A

GC ECD

.08

0.002

.074

.000061

DICHLOROPROP

515/615/8151A

GC ECD

.5

0.02

.021

.00011

DINOSEB

515/615/8151A

GC ECD

.2

.007

.031

.000064

2,4,5-T

515/615/8151A

GC ECD

.09

.003

.005

.000053

2,4,5-TP

515/615/8151A

GC ECD

.07

.003

.0036

.000065

BENTAZON*

515/615/8151A

GC ECD

.8

.050

.031

.00082

PENTACHLOROPHENOL*

515/615/8151A

GC ECD

0.05

0.002

.0012

.000011

PICLORAM

515/615/8151A

GC ECD

0.05

0.003

.003

.0025

ALPHA-BHC

508/608/8080/8081A

GC ECD

0.005

.0005

.0017

.000047

HCB (HEXACHLOROBENZENE)*

508/608/8080/8081A

GC ECD

0.02

.002

.0051

.00029

BETA-BHC

508/608/8080/8081A

GC ECD

0.005

.0005

.0037

.00025

GAMMA-BHC

508/608/8080/8081A

GC ECD

0.005

.0005

.0017

.000060

DELTA-BHC

508/608/8080/8081A

GC ECD

0.005

.0005

.0009

.000076

CHLOROTHALONIL*

508/608/8080/8081A

GC ECD

0.024

------

0.05

-----

HEXACHLOROCYCLOPENTADIENE*

508/608/8080/8081A

GC ECD

0.0032

------

0.05

-----

HEPTACHLOR

508/608/8080/8081A

GC ECD

0.005

.0005

.0044

.00019

ALDRIN

508/608/8080/8081A

GC ECD

0.005

.0005

.0014

.00024

HEPTACHLOR EPOXIDE

508/608/8080/8081A

GC ECD

0.005

.0005

.0019

.00025

ENDOSULFAN I

508/608/8080/8081A

GC ECD

0.005

.0005

.0016

.000081

PP-DDE

508/608/8080/8081A

GC ECD

0.005

.0005

.0015

.000068

DIELDRIN

508/608/8080/8081A

GC ECD

0.005

.0005

.0021

.000054

ENDRIN

508/608/8080/8081A

GC ECD

0.005

.0005

.0022

.000044

ENDOSULFAN II

508/608/8080/8081A

GC ECD

0.005

.0005

.0031

.00015

PP-DDD

508/608/8080/8081A

GC ECD

0.005

.0005

.0024

.000047

ENDRIN ALDEHYDE

508/608/8080/8081A

GC ECD

0.01

.0005

.0022

.000043

ENDOSULFAN SULFATE

508/608/8080/8081A

GC ECD

0.005

.0005

.0019

.000063

PP-DDT

508/608/8080/8081A

GC ECD

0.005

.0005

.0019

.000055

UNCONTROLLED COPY



ORGANIC METHODS

APPENDIX B

Revision 8


PAGE B-10

ANALYTE

METHOD

TECHNIQUE

PQL

MDL

WATER

(g/L)

SOIL (mg/kg)

WATER (g/L)

SOIL (mg/kg)

METHOXYCHLOR

508/608/8080/8081A

GC ECD

0.005

.0005

.0036

.00014

KEPONE*

508/608/8080/8081A

GC ECD

0.01

.005

.016

.0025

MIREX*

508/608/8080/8081A

GC ECD

0.01

0.0005

.0016

.00026

CHLORDANE

508/608/8080/8081A

GC ECD

.5

.05

.38

.015

TOXAPHENE

508/608/8080/8081A

GC ECD

2.0

.05

.42

.0074

ALL PCB'S

508/608/8080/8082

GC ECD

0.2

0.01

0.1

0.005

TREFLAN*

508/608/8080/8081A

GC ECD

0.01

0.0005

-----

-----

AZINPHOS METHYL

8140/8141A

GC TSD

.2

.01

.055

.0019

BOLSTAR

8140/8141A

GC TSD

.2

.01

.055

.0014

CHLORPYRIFOS

8140/8141A

GC TSD

.2

.01

.024

.0008

COUMAPHOS

8140/8141A

GC TSD

.2

.01

.054

.0022

DEMETON

8140/8141A

GC TSD

.2

.01

.026

.0015

DIAZINON

8140/8141A

GC TSD

.2

.01

.044

.0006

DICHLORVOS

8140/8141A

GC TSD

.2

.01

0.07

.0062

DISULFOTON

8140/8141A

GC TSD

.5

.01

.039

.0011

ETHOPROP

8140/8141A

GC TSD

.2

.01

.025

.0008

FENSULFTHION

8140/8141A

GC TSD

.2

.01

.088

.0054

FENTHION

8140/8141A

GC TSD

.2

.01

.033

.001

MERPHOS

8140/8141A

GC TSD

.2

.01

.058

.0011

MEVINPHOS

8140/8141A

GC TSD

.2

.01

.053

.0014

NALED

8140/8141A

GC TSD

.2

.01

.072

.0017

PARATHION METHYL

8140/8141A

GC TSD

.2

.01

.074

.0021

PHORATE

8140/8141A

GC TSD

.2

.01

.041

.0006

RONNEL

8140/8141A

GC TSD

.2

.01

.067

.0016

STIROPHOS

8140/8141A

GC TSD

.2

.01

.046

.0025

TOKUTHION

8140/8141A

GC TSD

.2

.01

.032

.001

TRICHLORONATE

8140/8141A

GC TSD

.2

.01

.038

.0011

MALATHION*

8140/8141A

GC TSD

.2

.01

.063

.003

UNCONTROLLED COPY



ORGANIC METHODS

APPENDIX B

Revision 8


PAGE B-11

ANALYTE

METHOD

TECHNIQUE

PQL

MDL

WATER

(g/L)

SOIL (mg/kg)

WATER (g/L)

SOIL (mg/kg)

THIONAZIN*

8140/8141A

GC TSD

.2

.01

.041

.0014

HEXACHLOROCYCLOPENTADIENE

525.2

GC/MS

3

-----

1

-----

DIMETHYLPHTHALATE

525.2

GC/MS

1.0

-----

.038

-----

ACENAPHTHYLENE

525.2

GC/MS

0.1

-----

.037

-----

DIETHYLPHTHALATE

525.2

GC/MS

3.0

-----

.19

-----

FLORENE

525.2

GC/MS

2.0

-----

.029

-----

HEXACHLOROBENZENE

525.2

GC/MS

1.0

-----

.016

-----

SIMAZINE

525.2

GC/MS

.3

-----

.07

-----

ATRAZINE

525.2

GC/MS

.3

-----

.05

-----

PENTACHLOROPHENOL

525.2

GC/MS

1.0

-----

.35

-----

LINDANE

525.2

GC/MS

0.1

-----

0.039

-----

PHENANTHRENE

525.2

GC/MS

0.1

-----

.022

-----

ANTHRACENE

525.2

GC/MS

0.1

-----

.085

-----

ALACHLOR

525.2

GC/MS

0.2

-----

.13

-----

HEPTACHLOR

525.2

GC/MS

0.1

-----

.059

-----

DI-N-BUTYLPHTHALATE

525.2

GC/MS

1.0

-----

.18

-----

ALDRIN

525.2

GC/MS

0.5

-----

.039

-----

HEPTACHLOR EPOXIDE

525.2

GC/MS

0.1

-----

.055

-----

GAMMA-CHLORDANE

525.2

GC/MS

0.5

-----

0.128

-----

PYRENE

525.2

GC/MS

0.1

-----

.024

-----

ALPHA-CHLORDANE

525.2

GC/MS

0.5

-----

0.094

-----

TRANS-NANOCHLOR

525.2

GC/MS

.2

-----

.048

-----

ENDRIN

525.2

GC/MS

1

-----

.75

-----

BUTYLBENZYLPHTHALATE

525.2

GC/MS

4

-----

3.9

-----

DI(2-ETHYLHEXYL)ADIPATE

525.2

GC/MS

1.0

-----

0.250

-----

BENZ(A)ANTHRACENE

525.2

GC/MS

.2

-----

.042

-----

CHRYSENE

525.2

GC/MS

0.3

-----

.044

-----

DI(2-ETHYLHEXYL)PHTHALATE

525.2

GC/MS

4.0

-----

1.631

-----

UNCONTROLLED COPY



ORGANIC METHODS

APPENDIX B

Revision 8


PAGE B-12

ANALYTE

METHOD

TECHNIQUE

PQL

MDL

WATER

(g/L)

SOIL (mg/kg)

WATER (g/L)

SOIL (mg/kg)

BENZO(B)FLUORANTHENE 525.2 GC/MS 0.3 ----- .063 -----

BENZO(K)FLUORANTHENE

525.2

GC/MS

0.3

-----

.053

-----

BENZO(A)PYRENE

525.2

GC/MS

.1

-----

.026

-----

PERYLENE

525.2

GC/MS

0.4

-----

0.206

-----

INDENO(1,2,3-CD)PYRENE

525.2

GC/MS

0.3

-----

.028

-----

DIBENZ(A,H)ANTHRACENE

525.2

GC/MS

0.3

-----

.016

-----

BENZO(G,H,I)PERYLENE

525.2

GC/MS

0.3

-----

.034

-----

METHOXYCHLOR

525.2

GC/MS

.3

-----

.036

-----

AMINOCARB

632

HPLC UV

5

-----

1.0

-----

BARBAN

632

HPLC UV

5

-----

.71

-----

CARBARYL

632

HPLC UV

20

-----

11

-----

CARBOFURAN

632

HPLC UV

20

-----

6.4

-----

CHLORPROPHAM

632

HPLC UV

1

-----

.73

-----

DIURON

632

HPLC UV

1

-----

.3

-----

FENURON

632

HPLC UV

1

-----

.37

-----

FENURON TCA*

632

HPLC UV

2

-----

1.0

-----

FLUOMETURON

632

HPLC UV

1

-----

.8

-----

LINURON

632

HPLC UV

.5

-----

.16

-----

METHIOCARB

632

HPLC UV

5

-----

1.0

-----

METHOMYL

632

HPLC UV

5

-----

1.4

-----

MEXACARBATE

632

HPLC UV

5

-----

1.0

-----

MONURON

632

HPLC UV

.5

-----

.16

-----

NEBURON

632

HPLC UV

.30

-----

.15

-----

OXAMYL

632

HPLC UV

5

-----

.64

-----

PROPHAM

632

HPLC UV

3

-----

1.4

-----

PROPOXUR

632

HPLC UV

20

-----

8.1

-----

SIDURON

632

HPLC UV

1

-----

.35

-----

SWEP

632

HPLC UV

5

-----

1.0

-----

UNCONTROLLED COPY



ORGANIC METHODS

APPENDIX B

Revision 8


PAGE B-13

ANALYTE

METHOD

TECHNIQUE

PQL

MDL

WATER

(g/L)

SOIL (mg/kg)

WATER (g/L)

SOIL (mg/kg)

EDB (ETHYLENE DIBROMIDE) 504.1 GC ECD 0.01 .35 .0016 .088

DBCP (1,2-DIBROMO-3-

CHLOROPROPANE)

504.1

GC ECD

0.01

.35

.0023

.084

AR-1260

8080/8082

GC ECD

0.2

0.01

.024

.0022

AR-1254

8080/8082

GC ECD

0.2

0.01

.042

.00078

AR-1248

8080/8082

GC ECD

0.2

0.01

.025

.0012

AR-1242

8080/8082

GC ECD

0.2

0.01

.095

.0016

AR-1232

8080/8082

GC ECD

0.2

0.01

.09

.0012

AR-1221

8080/8082

GC ECD

0.2

0.01

.089

0.005

AR-1016

8080/8082

GC ECD

0.2

0.01

.048

.0027

NAPHTHALENE

610/8310

HPLC UV

1

.005

.23

.000225

ACENAPHTHYLENE

610/8310

HPLC UV

2

.05

.32

.000313

ACENAPHTHENE

610/8310

HPLC UV

3

.1

.55

.000542

FLUORENE

610/8310

HPLC UV

.4

.01

.045

.000044

PHENANTHRENE

610/8310

HPLC UV

.1

.01

.025

.000025

ANTHRACENE

610/8310

HPLC UV

.02

.001

.012

.000012

FLUORANTHENE

610/8310

HPLC UV

0.4

.02

.068

.000067

PYRENE

610/8310

HPLC UV

.6

.02

.098

.000097

BENZO(A)ANTHRACENE

610/8310

HPLC UV

.2

.01

.035

.000035

CHRYSENE

610/8310

HPLC UV

.3

.01

.029

.000028

BENZO(B)FLUORANTHENE

610/8310

HPLC UV

0.1

.06

.03

.00003


610/8310

HPLC UV

0.2

.01

.072

.000072

BENZO(A)PYRENE

610/8310

HPLC UV

.4

.02

.031

.000031


610/8310

HPLC UV

.1

.06

.31

.0003


610/8310

HPLC UV

.5

.02

.11

.0001


610/8310

HPLC UV

0.2

.01

.063

.000062

N-NITROSODIMETHYLAMINE

625/8270C

GC/MS

2

0.1

.053

.038

PYRIDINE*

625/8270C

GC/MS

10

.5

.22

.0021

UNCONTROLLED COPY



ORGANIC METHODS

APPENDIX B

Revision 8


PAGE B-14

ANALYTE

METHOD

TECHNIQUE

PQL

MDL

WATER

(g/L)

SOIL (mg/kg)

WATER (g/L)

SOIL (mg/kg)

PHENOL 625/8270C GC/MS 2 0.1 .30 .057

ANILINE

625/8270C

GC/MS

5

0.2

1.8

.023

BIS(2-CHLOROETHYL)ETHER

625/8270C

GC/MS

2

0.1

.49

.049

2-CHLOROPHENOL

625/8270C

GC/MS

2

0.1

.39

.052

1,3-DICHLOROBENZENE

625/8270C

GC/MS

2

0.1

.35

.052

1,4-DICHLOROBENZENE

625/8270C

GC/MS

2

0.1

.25

.051

1,2-DICHLOROBENZENE

625/8270C

GC/MS

2

0.1

.35

.042

BENZYL ALCOHOL

625/8270C

GC/MS

2

0.1

.44

.054

2-METHYLPHENOL

625/8270C

GC/MS

2

0.1

1.3

.052

BIS(2-CHLOROISOPROPYL)ETHER

625/8270C

GC/MS

2

0.1

.57

.049

4-METHYLPHENOL

625/8270C

GC/MS

2

.2

1.4

.12

N-NITROSO-DI-N-PROPYLAMINE

625/8270C

GC/MS

2

0.1

.88

.052

HEXACHLOROETHANE

625/8270C

GC/MS

2

0.1

.29

.046

NITROBENZENE

625/8270C

GC/MS

2

0.1

.37

.046

ISOPHORONE

625/8270C

GC/MS

2

0.1

.31

.047

2-NITROPHENOL

625/8270C

GC/MS

2

0.1

.33

.047

2,4-DIMETHYLPHENOL

625/8270C

GC/MS

2

0.1

1.5

.047

BIS(2-CHLOROETHOXY)METHANE

625/8270C

GC/MS

2

0.1

1.6

.049

2,4-DICHLOROPHENOL

625/8270C

GC/MS

2

0.1

.37

.054

BENZOIC ACID

625/8270C

GC/MS

10

.5

.61

.035

1,2,4-TRICHLOROBENZENE

625/8270C

GC/MS

2

0.1

0.26

.050

NAPHTHALENE

625/8270C

GC/MS

2

0.1

.30

.047

4-CHLOROANILINE

625/8270C

GC/MS

2

0.1

.99

.037

HEXACHLOROBUTADIENE

625/8270C

GC/MS

1

0.1

.40

.050

4-CHLORO-3-METHYLPHENOL

625/8270C

GC/MS

5

0.2

.39

.053

2-METHYLNAPHTHALENE

625/8270C

GC/MS

2

0.1

.27

.056

HEXACHLOROCYCLOPENTADIENE

625/8270C

GC/MS

2

0.1

.36

.034

2,4,6-TRICHLOROPHENOL

625/8270C

GC/MS

5

0.2

.47

.071

UNCONTROLLED COPY



ORGANIC METHODS

APPENDIX B

Revision 8


PAGE B-15

ANALYTE

METHOD

TECHNIQUE

PQL

MDL

WATER

(g/L)

SOIL (mg/kg)

WATER (g/L)

SOIL (mg/kg)

2,4,5-TRICHLOROPHENOL 625/8270C GC/MS 5 0.2 .37 .063

2-CHLORONAPHTHALENE

625/8270C

GC/MS

2

0.1

.41

.059

2-NITROANILINE

625/8270C

GC/MS

2

0.1

.82

.053

DIMETHYPHTHALATE

625/8270C

GC/MS

2

0.1

.32

.061

2,6-DINITROTOLUENE

625/8270C

GC/MS

2

0.1

.48

.052

ACENAPHTHYLENE

625/8270C

GC/MS

2

0.1

.32

.058

3-NITROANILINE

625/8270C

GC/MS

2

0.1

1.6

.050

ACENAPHTHENE

625/8270C

GC/MS

2

0.1

.35

.065

2,4-DINITROPHENOL

625/8270C

GC/MS

10

0.5

.35

.022

4-NITROPHENOL

625/8270C

GC/MS

2

0.2

.35

.054

DIBENZOFURAN

625/8270C

GC/MS

2

0.1

.37

.062

2,4-DINITROTOLUENE

625/8270C

GC/MS

2

0.1

.39

.052

2-NAPHTHYLAMINE

625/8270C

GC/MS

20

3

5.3

.047

DIETHYLPHTHALATE

625/8270C

GC/MS

2

0.1

.34

.080

FLUORENE

625/8270C

GC/MS

2

0.1

.36

.044

4-CHLOROPHENYL-PHENYL ETHER

625/8270C

GC/MS

2

0.1

.33

.061

4-NITROANILINE

625/8270C

GC/MS

2

0.2

.82

.052

4,6-DINITRO-2-METHYLPHENOL

625/8270C

GC/MS

10

.5

2.5

.028

N-NITROSODIPHENYLAMINE

625/8270C

GC/MS

2

0.1

.42

.061

ALPHA-BHC

625/8270C

GC/MS

2

0.1

.42

.060

BETA-BHC

625/8270C

GC/MS

2

0.1

.46

.058

GAMMA-BHC

625/8270C

GC/MS

2

0.1

.35

.058

DELTA-BHC

625/8270C

GC/MS

2

0.1

.28

.058

HEPTACHLOR

625/8270C

GC/MS

2

0.1

.53

.046

ALDRIN

625/8270C

GC/MS

2

0.1

.47

.057

HEPTACHLOR EPOXIDE

625/8270C

GC/MS

2

0.1

.24

.060

ENDOSULFAN I

625/8270C

GC/MS

10

.2

2.3

.049

PP-DDE

625/8270C

GC/MS

3

0.1

.52

.055

UNCONTROLLED COPY



ORGANIC METHODS

APPENDIX B

Revision 8


PAGE B-16

ANALYTE

METHOD

TECHNIQUE

PQL

MDL

WATER

(g/L)

SOIL (mg/kg)

WATER (g/L)

SOIL (mg/kg)

DIELDRIN 625/8270C GC/MS 3 0.1 .52 .022

ENDRIN

625/8270C

GC/MS

2

.2

0.68

.047

ENDOSULFAN II

625/8270C

GC/MS

10

.2

1.6

.049

PP-DDD

625/8270C

GC/MS

2

0.1

.38

.052

ENDRIN ALDEHYDE

625/8270C

GC/MS

10

.5

3.6

.054

ENDOSULFAN SULFATE

625/8270C

GC/MS

3

0.1

.67

.055

PP-DDT

625/8270C

GC/MS

2

0.1

.36

.046

4-BROMOPHENYLPHENYL ETHER

625/8270C

GC/MS

2

0.1

.40

.067

HEXACHLOROBENZENE

625/8270C

GC/MS

2

0.1

.35

.064

PENTACHLOROPHENOL

625/8270C

GC/MS

10

0.2

.55

.062

PHENANTHRENE

625/8270C

GC/MS

2

0.1

.29

.070

ANTHRACENE

625/8270C

GC/MS

2

0.1

.27

.067

DI-N-BUTYLPHTHALATE

625/8270C

GC/MS

2

0.1

.40

.0088

FLUORANTHENE

625/8270C

GC/MS

2

0.1

.30

.066

BENZIDINE

625/8270C

GC/MS

20

3

4.7

1.5

PYRENE

625/8270C

GC/MS

2

0.1

.29

.060

BUTYBLENZYLPHTHALATE

625/8270C

GC/MS

2

0.1

.32

.060

BENZO(A)ANTHRACENE

625/8270C

GC/MS

2

0.1

.34

.057

3,3´-DICHLOROBENZIDINE

625/8270C

GC/MS

10

0.2

1.5

.044

CHRYSENE

625/8270C

GC/MS

2

0.1

.30

.063

BIS(2-ETHYLHEXYL)PHTHALATE

625/8270C

GC/MS

4

0.2

.98

.068

DI-N-OCTYLPHTHALATE

625/8270C

GC/MS

2

0.1

.41

.081

BENZO(B)FLUORANTHENE

625/8270C

GC/MS

2

0.1

.38

.061


625/8270C

GC/MS

2

0.1

.47

.064

BENZO(A)PYRENE

625/8270C

GC/MS

2

0.1

.45

.053


625/8270C

GC/MS

2

0.1

.47

.075


625/8270C

GC/MS

3

0.1

.48

.058


625/8270C

GC/MS

2

0.1

.56

.046

UNCONTROLLED COPY



ORGANIC METHODS

APPENDIX B

Revision 8


PAGE B-17

ANALYTE

METHOD

TECHNIQUE

PQL

MDL

WATER

(g/L)

SOIL (mg/kg)

WATER (g/L)

SOIL (mg/kg)

DIESEL 8015-M GC FID 200 10 31 2.6

KEROSENE

8015-M

GC FID

200

10

51

2.2

JP-4

8015-M

GC FID

200

10

100

5

JP-5

8015-M

GC FID

200

10

100

5

JP-6

8015-M

GC FID

200

10

100

5

JP-8

8015-M

GC FID

200

10

100

5

MOTOR OIL

8015-M

GC FID

500

20

90

10

WASTE OIL

8015-M

GC FID

500

20

200

10

CRUDE OIL

8015-M

GC FID

500

20

72

4.6

STODDARD

8015-M

GC FID

200

20

100

5

HYDRAULIC OIL

8015-M

GC FID

500

20

200

10

BENZENE

602/624/8240B

GC/MS

0.5

0.005

.31

.0014

BROMODICHLOROMETHANE

601/624/8240B

GC/MS

0.5

0.005

.3

.0011

BROMOFORM

601/624/8240B

GC/MS

0.5

0.005

.27

.0023

BROMOMETHANE

601/624/8240B

GC/MS

1

.005

.49

.0019

CARBON TETRACHLORIDE

601/624/8240B

GC/MS

0.5

0.005

.31

.0018

CHLOROBENZENE

601/624/8240B

GC/MS

0.5

0.005

.26

.0011

CHLOROETHANE

601/624/8240B

GC/MS

.5

.005

.27

.0016

CHLOROFORM

601/624/8240B

GC/MS

0.5

0.005

.3

.0011

CHLOROMETHANE

601/624/8240B

GC/MS

.5

.005

.32

.0017

DIBROMOCHLOROMETHANE

601/624/8240B

GC/MS

0.5

0.005

.28

.00096

1,2-DCB

601/624/8240B

GC/MS

0.5

0.005

.27

.00091

1,3-DCB

601/624/8240B

GC/MS

0.5

0.005

.29

.0012

1,4-DCB

601/624/8240B

GC/MS

0.5

0.005

.28

.0013

1,1-DICHLOROETHANE

601/624/8240B

GC/MS

0.5

0.005

.3

.0012

1,2-DICHLOROETHANE

601/624/8240B

GC/MS

0.5

0.005

.26

.00099

1,1-DICHLOROETHENE

601/624/8240B

GC/MS

0.5

0.005

.32

.0017

1,2-DICHLOROETHENE (TOTAL)

601/624/8240B

GC/MS

.1

.01

.58

.0029

UNCONTROLLED COPY



ORGANIC METHODS

APPENDIX B

Revision 8


PAGE B-18

ANALYTE

METHOD

TECHNIQUE

PQL

MDL

WATER

(g/L)

SOIL (mg/kg)

WATER (g/L)

SOIL (mg/kg)

1,2-DICHLOROPROPANE 601/624/8240B GC/MS 0.5 0.005 .26 .00079

CIS-1,3-DICHLOROPROPENE

601/624/8240B

GC/MS

0.5

0.005

.27

.00085

TRANS-1,3-DICHLOROPROPENE

601/624/8240B

GC/MS

0.5

0.005

.24

.0011

ETHYLBENZENE

602/624/8240B

GC/MS

0.5

0.005

.27

.0013

METHYLENE CHLORIDE

601/624/8240B

GC/MS

1

0.01

.24

.0024

1,1,2,2-TETRACHLORETHANE

601/624/8240B

GC/MS

0.5

0.005

.26

.0013

TETRACHLOROETHENE (PCE)

601/624/8240B

GC/MS

0.5

0.005

.3

.0013

TOLUENE

602/624/8240B

GC/MS

0.5

0.005

.29

.0012

1,1,1-TRICHLOROETHANE

601/624/8240B

GC/MS

0.5

0.005

.3

.0012


601/624/8240B

GC/MS

0.5

0.005

.24

.0012

TRICHLOROETHENE (TCE)

601/624/8240B

GC/MS

0.5

0.005

.29

.0013

TRICHLOROFLUOROMETHANE

601/624/8240B

GC/MS

0.5

0.005

.29

.0017

VINYL CHLORIDE

601/624/8240B

GC/MS

.5

.005

.31

.0021

XYLENES (TOTAL)

602/624/8240B

GC/MS

.5

0.01

.78

.0037

TRIHALOMETHANES (TOTAL)

601/624/8240B

GC/MS

2

.02

1.2

.0054

ACETONE*

624/8240B

GC/MS

10

.02

6.2

.015

2-BUTANONE*

624/8240B

GC/MS

10

0.2

1.45

0.0084

METHYL ISOBUTYL KETONE*

624/8240B

GC/MS

10

0.05

3.4

0.0064

ACRYLAMIDE*

624/8240B

GC/MS

50

0.05

-----

-----

ACROLEIN*

624/8240B

GC/MS

20

0.05

3.7

.00048

ACROLONITRILE*

624/8240B

GC/MS

50

.02

2

.0062

ETHANOL*

624/8240B

GC/MS

250

1

57

.13

METHYL-T-BUTYL ETHER*

624/8240B

GC/MS

0.5

0.005

0.13

0.0012

BENZENE

524.2/8260B

GC/MS

0.5

0.005

.12

.0014

BROMOCHLOROMETHANE

524.2/8260B

GC/MS

0.5

0.005

.18

.0009

BROMODICHLOROMETHANE

524.2/8260B

GC/MS

0.5

0.005

0.13

.0011

BROMOFORM

524.2/8260B

GC/MS

0.5

0.005

.22

.0023

BROMOMETHANE

524.2/8260B

GC/MS

1.0

0.005

.31

.0019

UNCONTROLLED COPY



ORGANIC METHODS

APPENDIX B

Revision 8


PAGE B-19

ANALYTE

METHOD

TECHNIQUE

PQL

MDL

WATER

(g/L)

SOIL (mg/kg)

WATER (g/L)

SOIL (mg/kg)

CARBON TETRACHLORIDE 524.2/8260B GC/MS 0.5 0.005 .089 .0018

CHLOROBENZENE

524.2/8260B

GC/MS

0.5

0.005

.11

.0011

CHLOROETHANE

524.2/8260B

GC/MS

0.5

0.005

.12

.0016

CHLOROFORM

524.2/8260B

GC/MS

0.5

0.005

.098

.0011

CHLOROMETHANE

524.2/8260B

GC/MS

0.5

0.005

.14

.0017

DIBROMOCHLOROMETHANE

524.2/8260B

GC/MS

0.5

0.005

.12

.00096

1,2-DCB

524.2/8260B

GC/MS

0.5

0.005

.13

.00091

1,3-DCB

524.2/8260B

GC/MS

0.5

0.005

.14

.0012

1,4-DCB

524.2/8260B

GC/MS

0.5

0.005

.12

.0013

1,1-DICHLOROETHANE

524.2/8260B

GC/MS

0.5

0.005

.11

.0012

1,2-DICHLOROETHANE

524.2/8260B

GC/MS

0.5

0.005

.098

.00099

1,1-DICHLOROETHENE

524.2/8260B

GC/MS

0.5

0.005

.12

.0017

CIS-1,2-DICHLOROETHENE

524.2/8260B

GC/MS

0.5

0.005

.11

.0014

TRANS-1,2-DICHLOROETHENE

524.2/8260B

GC/MS

0.5

0.005

.14

.0015

1,2-DICHLOROPROPENE

524.2/8260B

GC/MS

0.5

0.005

.11

.00079

CIS-1,3-DICHLOROPROPENE

524.2/8260B

GC/MS

0.5

0.005

.086

.00085

TRANS-1,3-DICHLOROPROPENE

524.2/8260B

GC/MS

0.5

0.005

.11

.0011

ETHYLBENZENE

524.2/8260B

GC/MS

0.5

0.005

.13

.0013

METHYLENE CHLORIDE

524.2/8260B

GC/MS

1

0.01

.16

.0024

1,1,2,2-TETRACHLORETHANE

524.2/8260B

GC/MS

0.5

0.005

.22

.0011

TETRACHLOROETHENE (PCE)

524.2/8260B

GC/MS

0.5

0.005

0.11

.0013

TOLUENE

524.2/8260B

GC/MS

0.5

0.005

.12

.0012


524.2/8260B

GC/MS

0.5

0.005

.27

.0012


524.2/8260B

GC/MS

0.5

0.005

.12

.0012

TRICHLOROETHENE (TCE)

524.2/8260B

GC/MS

0.5

0.005

.13

.0013

TRICHLOROFLUOROMETHANE

524.2/8260B

GC/MS

0.5

0.005

.14

.0017

VINYL CHLORIDE

524.2/8260B

GC/MS

0.5

0.005

.14

.0021

XYLENES (TOTAL)

524.2/8260B

GC/MS

1

0.01

.33

.0037

UNCONTROLLED COPY



ORGANIC METHODS

APPENDIX B

Revision 8


PAGE B-20

ANALYTE

METHOD

TECHNIQUE

PQL

MDL

WATER

(g/L)

SOIL (mg/kg)

WATER (g/L)

SOIL (mg/kg)

TRIHALOMETHANES (TOTAL) 524.2/8260B GC/MS 2 .02 .47 .0054

2,2-DICHLOROPROPANE

524.2/8260B

GC/MS

0.5

0.005

.14

.0013

1,1-DICHLOROPROPANE

524.2/8260B

GC/MS

0.5

0.005

.11

.0015

1,2-DIBROMOETHANE

524.2/8260B

GC/MS

0.5

0.005

.13

.0011

1,1,1,2-TETRACHLOROETHANE

524.2/8260B

GC/MS

0.5

0.005

.19

.0013

STYRENE

524.2/8260B

GC/MS

0.5

0.005

.15

.0012

ISOPROPYLBENZENE

524.2/8260B

GC/MS

0.5

0.005

.15

.0014

1,2,3-TRICHLOROPROPANE

524.2/8260B

GC/MS

1

0.005

.42

.0026

N-PROPYLBENZENE

524.2/8260B

GC/MS

0.5

0.005

.11

.0012

BROMOBENZENE

524.2/8260B

GC/MS

0.5

0.005

.09

.0008

O-CHLOROTOLUENE

524.2/8260B

GC/MS

0.5

0.005

0.15

.00091

P-CHLOROTOLUENE

524.2/8260B

GC/MS

0.5

0.005

.16

.0011

1,3,5-TRIMETHYLBENZENE

524.2/8260B

GC/MS

0.5

0.005

.093

.0015

T-BUTYLBENZENE

524.2/8260B

GC/MS

0.5

0.005

.097

.0013

1,2,4-TRIMETHYLBENZENE

524.2/8260B

GC/MS

0.5

0.005

.14

.0012

SEC-BUTYLBENZENE

524.2/8260B

GC/MS

0.5

0.005

0.12

.0013

P-ISOPROPYL TOLUENE

524.2/8260B

GC/MS

0.5

0.005

0.12

.0014

N-BUTYLBENZENE

524.2/8260B

GC/MS

0.5

0.005

.19

.0015


524.2/8260B

GC/MS

0.5

0.005

.18

.0015

HEXACHLOROBUTADIENE

524.2/8260B

GC/MS

0.5

0.005

.31

.0017


524.2/8260B

GC/MS

0.5

0.005

.19

.0012

NAPHTHALENE

524.2/8260B

GC/MS

0.5

0.005

.27

.0013

BENZENE

8020/8021B

GC PID

0.3

0.005

.033

.00074

TOLUENE

8020/8021B

GC PID

0.3

0.005

.047

.00098

ETHYL-BENZENE

8020/8021B

GC PID

0.3

0.005

.033

.00087

XYLENES (TOTAL)

8020/8021B

GC PID

.6

0.01

.12

.0031

MTBE*

8020/8021B

GC PID

1

.02

.033

.00065

Oil and Grease

EPA 1664

Grav.

5

50

1.9

27

UNCONTROLLED COPY



ORGANIC METHODS

APPENDIX B

Revision 8


PAGE B-21

ANALYTE

METHOD

TECHNIQUE

PQL

MDL

WATER

(g/L)

SOIL (mg/kg)

WATER (g/L)

SOIL (mg/kg)

TPH-GASOLINE

8015-M

GC FID

50

1

9.3

0.1

HMX

8330

HPLC

5

.5

.53

.097

RDX

8330

HPLC

5

.5

.29

.14

1,3,5-Trinitrobenzene

8330

HPLC

5

.5

.47

.086

1,3-Dinitrobenzene

8330

HPLC

5

.5

.34

.089

Tetryl

8330

HPLC

5

.5

.98

NA

Nitrobenzene

8330

HPLC

5

.5

.48

.21

2,4,6-Trinitrotoluene

8330

HPLC

5

.5

.71

.13

4-Amino-2,6-Dinitrotoluene

8330

HPLC

5

.5

.8

NA

2,4-Dinitrotoluene

8330

HPLC

5

.5

.38

.032

2,6-Dinitrotoluene

8330

HPLC

5

.5

1.2

NA

2-Nitrotoluen

8330

HPLC

5

.5

1.1

NA

3-Nitrotoluene

8330

HPLC

5

.5

1.2

NA

4-Nitrotoluene

8330

HPLC

5

.5

.62

NA

* ALL COMPOUNDS THAT HAVE AN ASTERISK BESIDE THEM ARE NOT NORMALLY RUN BY THIS METHOD BUT CAN

BE UPON REQUEST.

Note: Appropriate analyses are updated in element with new MDL study result.

Note: Appendix B has been Reviewed on 01/08/2016 (No Changes were made)

MDL’S listed in this Appendix B may not be the current MDL’S. Please contact

BC Labs to confirm sensitivity.

UNCONTROLLED COPY



APPENDIX C

APPENDIX C Rev. 5 EFFECTIVE DATE 01/08/16 PAGE 1

UNCONTROLLED COPY



APPENDIX C


UNCONTROLLED COPY



APPENDIX C


Note: Appendix C was review on 01/08/16 (No changes were made)

UNCONTROLLED COPY



APPENDIX D

APPENDIX D EFFECTIVE DATE 01/08/16

PAGE D-1

Analyze initial calibration standards

r> or = to 0.995?Please note that r should be

>0.999.

Initiate Corrective

Action

Options

Recalibrate,Reanalyze the standard(s) which adversely affect linearity, Prepare new standards,Correct instrumentation malfunctions,Calibrate at a more appropriate level,Notify Supervisor

No

Continue analytical run

Analyze the ICV

ICV % recovery within 90-110%

window?

Initiate Corrective

Action

Options

Recalibrate, Prepare new standard(s),Correct instrumentation malfunctions,Notify Supervisor

No

Yes

Yes

Initial Calibration Logic for Continuous Flow, IC, Ion Specific,

TOC and Manual Spectrometer Methods

Calculate the correlation coefficient

(r)

Reanalyze the ICVICV % recovery within 90-110%

window?

No

yes

UNCONTROLLED COPY



APPENDIX D


PAGE D-2

Analyze at least five calibration standards at different concentration

levels

%RSD < or = 15 for all analytes?

Analyze the ICV

±30%diff or ±30%drift criteria

met?

Continue the run

Reanalyze the standard(s) which adversely affect

linearity and recalculate %RSD.

%RSD criteria met for all analytes?

Initiate Corrective Procedures

(SIF)Options

Prepare new standards,Correct instrumentation malfunctions,

Consult Supervisor,Review SOP,

Review calculations,Check maintenance log for a record

on replacement components

No

Yes

Yes

Reanalyze the ICV %diff criteria met?

Initiate Corrective

Action(SIF)

No

Yes

No

Options

Verify standards,Generate a new initial calibration

curve,Correct instrument malfunctions,

Consult the supervisor,Prepare new standards,

Check for calculation errors,Reevaluate instrument setup,

Consult the SOP

Initial Calibration Logic for GC/MS Methods

Create a least squares linear regression model

for the analyte which does not meet linearity

protocols.Do not force zero.

Calculate the mean RSD using all RSD values for all analytes of the

curve or go directly to *.

Mean RSD < 15%?

r > 0.99?

Notify the client by adding a comment

which states that there is greater uncertainty for analytes of which the %RSD is greater

than 15.

Create a quadratic or or 3rd order polynomial

regression model Do Not Force Zero

Please note:Quadratic curve: 6 standards

3rd order polynomial curve: 7 standards

COD > 0.99?

Yes

No

Yes

No

Yes

Quantitation must take

place within calibration

range.

No

Yes



range.

No

SPCC and CCC criteria met?

Yes

Corrective Action is required

No

*

UNCONTROLLED COPY



APPENDIX D


PAGE D-3

Analyze initial calibration standard(s)

after profiling the instrument.

Is the RSD < or = to 3% for all analytes of interest?

Initiate Corrective

Action

Options

Re-profile,Reanalyze the standard(s), Correct instrumentation malfunctions,Notify Supervisor

No


Analyze the CCV standard(s).

ICV % recovery within 95-105% window?

Initiate Corrective

Action

Options


No

Yes

Yes

Initial Calibration Logic for ICP Methods

Check the RSD of the 4 integrations for

analytes of interest.

Reanalyze the ICV ICV % recovery within 95-105% window?

No

yes

Analyze the ICV standard(s).

CCV % recovery within 90-110% window? Reanalyze the CCV CCV % recovery within

90-110% window?

Yes

No

Initiate Corrective

Action

Options


No

If instrument was re-profiled

UNCONTROLLED COPY



APPENDIX D


PAGE D-4


levels


Analyze the ICV


met?

Continue the run





(SIF)Options





No

Yes

Yes


Initiate Corrective

Action(SIF)

No

Yes

No

Options




Check for calculation errors,Reevaluate instrument parameter

setup,Consult the SOP

Initial Calibration Logic for GC/HPLC Methods





curve.

Mean RSD < 20%?

r > 0.99?



than 20.





COD > 0.99?

Yes

No

Yes

No

Yes



range.

No

Yes



range.

No

If time permits, you may

not choose to follow the

proceeding steps.

Notify the department

supervisor or the team

leader before proceeding

Optional ProcessPlease contact the Department Supervisor

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APPENDIX D


PAGE D-5

Analyze continuing calibration verification

standard

±20%diff or ±20%drift criteria met?

Generate a new initial calibration

curve

Correctinstrumentation malfunctions as necessary,

Consult Supervisor, as necessary,

Yes


GC/MS Continuing Calibration Logic

Use professional judgement in the assessment of continuing the run.Contact the department supervisor for guidance and/or approval.

Calculate the mean %diff or

mean %drift of all analytes in the

curve

Mean %diff or %drift <20?

No

Were there any detections for analytes that failed %diff/%drift criteria in any environmental or

QC sample?

Reanalyze the samples with constituency

between two(2) CCVs that are compliant for

the analytes of interest.

Flag the PQLs for low recovered analytes.

Flag - V11

NoWere any CCV

analyte recoveries low?

Yes

Yes

No

Yes

Option: If no hits were detected

in any samples and the

recoveries for analytes in

the CCV outside the ±20%

window are high, you may

continue the run.

General RulesDo not make any system modifications prior to analyzing any CCV.

CCVs should be analyzed once every twelve hours prior to sample analysis.

An ICV may be used as the initial CCV after a new set of calibration standards.

CCVs are incremented until a new curve has been approved. (ex. CCV1, CCV2, etc.)

If adverse conditions are known or suspected at any time during the analytical run, analysts should reanalyze samples during the time of adverse conditions even if CCV(s) are compliant.

Reanalyze the CCV

SPCC and CCC criteria met?

Yes

SPCC and CCC criteria met?Yes

No

Evaluate the %diff/%drift for non-CCCs

No

No


If not feasible, flag data PQL-9G or add a comment which denotes calibration status related to the sample of interest.

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APPENDIX D


PAGE D-6

Analyze continuing calibration verification

standard

±15%diff or ±15%drift criteria met?

Initiate Corrective

Action

Options

Generate a new initial calibration curve


Consult Supervisor,See SOP,

Qualify data if necessary

No

Yes


GC/HPLC Continuing Calibration Logic


Calculate the mean %diff or

mean %drift of all analytes in the

curve

Mean %diff or %drift <15?

No

Were there any detections for analytes that failed %diff/%drift criteria in any environmental or

QC sample?

Reanalyze the samples with constituency

between two(2) CCVs that are compliant for

the analytes of interest.

Flag the PQLs for low recovered analytes.

Flag - V11

NoWere any CCV

analyte recoveries low?

Yes

Yes

No

Yes

Option: If no hits were detected

in any samples and the

recoveries for analytes in

the CCV outside the ±15%

window are high, you may

continue the run.

General RulesDo not make any system modifications prior to analyzing any CCV.

CCV frequency is ten(10) percent. CCVs must be analyzed before and after every ten samples or less. Samples are defined as any aliquot injected into the instrument other than a calibration standard used in the calibration curve, ICV, ICB, CCV, CCB, or IB.

An ICV may be used as the initial CCV after a new set of calibration standards.

CCVs are incremented until a new curve has been approved. (ex. CCV1, CCV2, etc.)

If adverse conditions are known or suspected at any time during the analytical run, analysts should reanalyze samples during the time of adverse conditions even if CCV(s) are compliant.

Reanalyze the CCV

±15%diff or ±15%drift

criteria met?Yes

No

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APPENDIX D


PAGE D-7

Analyze the continuing calibration verification

standard

%recovery within acceptable limits and

%RSD <5%?

Initiate Corrective

ActionCCV analysis is not

acceptable.Previous samples

must be reanalyzed.

Some Options

Recalibrate, verify calibration and analyze samples associated

with the incompliant CCV.

Reanalyze the CCV, if compliant, reanalyze all samples associated


Prepare new standards,

Correct instrumentation malfunctions,

Consult Supervisor,

Qualify data if necessary, the supervisor must be infomed in

cases of qualifying data

No

Yes

Continue analytical runResults are acceptable

Continuing Calibration Logic for ICP

Methods

Reanalyze the CCV

Please note that no special modifications should be made to the instrument or CCV standard prior to the analysis of any CCV

which is used to validate prior samples.

CCV frequency is ten(10) percent. CCVs must be analyzed before and after every ten samples or less. Samples are defined as

any aliquot other than calibration standards, an ICV, ICB, CCV or CCB

Results of samples which were associated with an incompliant CCV are considered estimated at best. Please consult the

department supervisor in cases of reporting results with associated incompliant CCV(s).

If adverse conditions are known at any time during an analytical run, analysts should reanalyze samples during the time of

adverse conditions even if CCV(s) are compliant.

All samples following the last acceptable CCV must be reanalyzed.

Yes

%recovery within acceptable limits and %RSD

<5%?

No

Were any samples analyzed between the

incompliant and compliant CCVs?

Reanalyze all samples between

two acceptable CCVs

No

Yes

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APPENDIX D


PAGE D-8


standard

%recovery within acceptable limits?

Initiate Corrective



must be reanalyzed.

Some Options







Consult Supervisor,

Qualify data if necessary, the supervisor must be informed in


No

Yes


Continuing Calibration Logic for Continuous

Flow, IC, TOC, Ion Specific, and Manual

Spectrometer Methods

Reanalyze the CCV

Please note that no special modifications should be made to the instrument or CCV standard prior to the analysis of any CCV which is used to

validate prior samples.

CCV frequency is ten(10) percent. CCVs must be analyzed before and after every ten samples or less. Samples are defined as any aliquot other than

a calibration standard used in the calibration curve, ICV, ICB, CCV or CCB.

Results of samples which were associated with an incompliant CCV are considered estimated at best. Please consult the department supervisor in

cases of reporting results with associated incompliant CCV(s).

If adverse conditions are known at any time during an analytical run, analysts should reanalyze samples during the time of adverse conditions even

if CCV(s) are compliant.


No

%recovery within acceptable limits?

Reanalyze all samples between two

acceptable CCVs.



Yes

Yes

No

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APPENDIX D


PAGE D-9


standard

%recovery within acceptable limits and %RSD(if applicable)

<10%?

Initiate Corrective



must be reanalyzed.

Some Options







Consult Supervisor,

Qualify data if necessary, the supervisor must be infomed in


No

Yes


GFAA, AA, CV and GHAA Continuing

Calibration Logic

Reanalyze the CCV

Please note that no special modifications should be made to the instrument or CCV standard prior to the analysis of any CCV

which is used to validate prior samples.

CCV frequency is ten(10) percent. CCVs must be analyzed before and after every ten samples or less. Samples are defined as

any aliquot other than calibration standards, an ICV, ICB, CCV or CCB

Results of samples which were associated with an incompliant CCV are considered estimated at best. Please consult the

department supervisor in cases of reporting results with associated incompliant CCV(s).

If adverse conditions are known at any time during an analytical run, analysts should reanalyze samples during the time of

adverse conditions even if CCV(s) are compliant.


Yes

If instrument reslope was performed before CCV analysis;Is the absolute value of the reslope blank absorbance

greater than the PQL standard absorbance?

Yes

Hg by CV technique?

No

No

%recovery within acceptable limits and

%RSD(if applicable) <10%?

No





Reanalyze all samples between

two acceptable CCVs

Yes

No

Yes

Yes

No

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APPENDIX D


PAGE D-10

Prepare an analytical batch

Are recoveries within acceptable

limits?

Continue analysis of the analytical batch


Reanalyze the Laboratory Control

Sample

Analyze the Laboratory Control Sample

Within acceptable limits?

Yes

No

Yes

Corrective Action Logic for Laboratory Control

Samples

Check prior position runs,Check for carryover,Check instrumentation, Check calibration, (sensitivity, linearity, etc.),Check spike soln. (integrity, conc.),Check dilution scheme,Look for contamination sources,Check digestion/extraction logother

Initiate Quality

Improvement form,

Check for reagent bias,Check glassware cleaning procedures,Check for cross contamination possibilities,Check the source standard,Evaluate the preparation procedure,Validate calibration,Review SOP

See Dept Supervisor, QA Officer, or Project Manager

for guidance.Analyze the analytical/Prep

batch if guidance not available and no reason for

discrepancy is known.

Reprepare the entire analytical

batch

No

CA_LCS.vsdRev. 3

05/05/06

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APPENDIX D


PAGE D-11

Recovery(ies) acceptable?

Continue analysis of the analytical batch


Reanalyze the Laboratory Control

Sample

Analyze the Laboratory Control Sample

Acceptable?

Yes

No

Yes

Options

Check instrumentation, Check calibration, (sensitivity, linearity, etc.),Check spike soln. (integrity, conc.),Verify micro-pipette calibration,Look for contamination sources,other

Initiate Quality Improvement form,

Check for reagent bias,Check glassware cleaning

procedures,Check for cross

contamination possibilities,Check the source standard,

Evaluate the preparation procedure,

Validate calibration,Review SOP,

Consult the Department Supervisor

See Dept Supervisor, QA Officer, or Project Manager for guidance.Analyze the analytical batch if guidance not available and no reason for discrepancy can be found.

Initiate corrective ActionNo

Analyze 1 LCSW per every 20 samples.The LCSW should be spiked to the midpoint of the calibration curve unless noted otherwise in the respective SOPThe LCSW must be acceptable in order to report data.Use time logic when batching LCSWs with samples.

Corrective Action Logic for Laboratory Control

Samples

(unprepared LCS's)

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APPENDIX D


PAGE D-12

Analyze matrix spike/matrix spike duplicate

Accuracy/Precision Controls Met?

Analyze the entire analytical batch

Laboratory Control Sample Compliant?

Report data properly.

Instrument Problems?

Initiate Corrective Action/ Restore

acceptable instrument performance/

Reanalyze matrix spike/matrix spike

duplicate

Qualify affected data when accuracy and/or precision requirements

are not metAccuracy/Precision Controls met?

Refer to Specific Project QC

Requirements

Yes

No

Yes

Re-extract/Re-prepare the analytical

batch, Initiate corrective

action

No

Analyze the sample used for spiking

purposes

Concentration >4 times the spike level?

Analyze MS/MSD and/or sample/duplicate to

validate precision.(Dilute if necessary)

Yes

No

LCS compliant?

Yes

Re-extract/Re-prepare

the analytical batch if

applicable

No

Yes

No

Certain projects will require confirmation of matrix interferences by repreparing and reanalyzing the analytical batch in cases of MS/MSD failure.If time or workload allows, reprepare and reanalyze the set if no project specific requirements are documented.

Project specific qualifiersLaboratory qualifiersComments

Initiate documentation of corrective action,

Notify the Department Supervisor

Corrective Action Logic for Matrix Spikes

Laboratory Control sample must be compliant,Please refer to the corrective action flowchart for LCSs.

No

See Corrective Action Logic Flowchart for Laboratory

Control Samples

Yes

Precision in control?

yes

Continue the run. Flag data appropriately.

Ues professional judgement in deciding whether or not to initiate corrective action

No

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APPENDIX D


PAGE D-13

Prepare an analytical batch

Concentration < 0.5(PQL)?

Continue analysis of the analytical batch.

Check instrumentation for contamination

sources. Evaluate the preparation process

Reanalyze the method blank

Analyze the method blank

Concentration < the 0.5(PQL)?

No

Yes

Assessment of Method Blanks

Check prior position runs,Check for carryover,

Check instrumentation

Options

Initiate Quality Improvement form,

Check for reagent bias,Check glassware cleaning

procedures,Check for cross

contamination possibilities,other

Corrective action may not be necessary,

See MB Assessment

Check instrumentation, environment and/or sample

containment for contamination sources.

Evaluate the preparation process.

(May be necessary to stop the analytical run.)

NoContinue

analytical run(See MB Assessment)

Use professional judgement when deciding to continue or stop the runTypically the method blank

concentration will be reported as "trace"

Are sample results >10x the

PQL?

NO

Report data with the appropriate qualifier

Reprepare the analytical batch for all samples that were <10

times the PQL(See MB Assessment)

Yes

Yes

0.5(PQL)<MB<PQL?

0.5(PQL)<MB<PQL?

If the MB concentration was between 0.5(PQL) and the PQL, contact contact the Department Supervisor before the initiation of repreparation

Method blank Assessment:Qualify data if bias would significantly affect sample results.General, if the MB is > or = to 10% of the sample concentration, this should be considered as a significant bias. Consult the department supervisor when qualifying data.

Yes

Yes

Consult with the department

supervisor. Continue the anaytical run

No

Should open a QIF

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APPENDIX D


PAGE D-14

Batching Procedure for Prepared Samples

Samples are prepared together in a

preparation batch

Analyze QC samples

Anlayze the balance of the preparation batch and batch together

Are the MB and LSC compliant?

Make instrument corrections if

necessary, then reanalyze QC samples.

Are the MB and LSC compliant?

It is very good practice to analyze the entire prepared batch on one instrument over the course of one day.

Yes

No

Yes

Re-prepare the entire preparation batch

No

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APPENDIX D


PAGE D-15

QC sample matrices defined

(water or soil)

Evaluate constituency given the available information. Also

evaluate background as noted from the method blank and/or indicative

CCBs/IBs

Are samples from the same submission or

field origin as the sample spiked?

Batching Logic for Unprepared Samples

Are samples relatively close in

constituency?

Batch together

Batch option is open, however batching

samples from the same submission will ease data processing and

reporting

Does the constituency,matrix,

and relative instrument conditions of given samples match the

sample spiked?

Batch together

Batch together with the QC sample that most closely

resembles the given samples in matrix and constituency, and is affected in the same magnitude by the relative

instrument conditions.

Are the given samples within the calibration block as the samples

spiked?

Evaluate constituency given the available information. Also

evaluate background as noted from the method blank and/or indicative

CCBs/IBs

Yes

No Yes

No

Yes

No

Yes

No

Run completed

Initially, samples must be batched according to matrix type: Aqueous - Non-Aqueous

Matrix here is more specific than aqueous/non-aqueous

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APPENDIX D


PAGE D-16

Obtain the analyte response(s) which will be used for reporting.

Is the analyte concentration(s)

below its associated MDL?

Is the analyte concentration(s) equal to or above its associated

MDL and below its IQL?

Is the analyte concentration equal to or above the IQL and

below the PQL?

Report analyte concentration(s) as

"none detected".

Report the concentration or note the concentration as a

"trace" and attach the appropriate flag (A7).

Does the sample require the MDL/PQL

(trace) reporting format?

Report the concentration with lab defaulted PQL/MDL.

Yes

No

Yes

Yes

No

No

Yes

Low Level Reporting Policy Flowchart

Reduce the response(s) to final concentration terms.

Find the sample analyte MDL(s)/IQL(s)/PQL(s) by factoring in any sample dilutions and/or sample weight to

volume ratios which differ from those used for the analyte MDL/PQL study.

Does the sample require special reporting

limit that is below the PQL?

Does the sample require the MDL/PQL

(trace) reporting format?

Report the concentration or note the concentration as a

"trace" and attach the appropriate flag (A7).

No No

Report analyte concentration(s) as

"none detected" with lab defaulted PQL(s).

Does the sample require reporting limits

below laboratory PQLs?No

Report the IQL or MDL as the Reporting Limit.

Yes

Does the sample require reporting limits

below laboratory PQLs?

YesYes

The analyte concentration must be at or above the PQL.

No

No

Please verify the method of reporting a trace - Text or value

Please verify the method of reporting a trace - Text or value

Yes

Use the sample MDL as the reporting limit and

report the concentration with an appropriate flag

(A8).

Report the concentration and report the IQL as the

PQL or use the client specified reporting limit.

Yes

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APPENDIX D


PAGE D-17

Note: This section was review on 01/08/16 (No changes were made)

Notes Q02/Q03

Matrix spikes are outside QC Limits.Accuracy and/or

Precision

Flag all concerned analytes with note

Q03.

Are spike recoveries low?

Flag positive concerned sample

results with note Q03.No

Yes

Precision or Accuracy Controls

Exceeded?

Flag concerned analytes with note

Q02.

Are results with associated

incompliant QC positive?

Use descretion in determining if effects

will be significant.

Accuracy

Precision Yes

No

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APPENDIX E

APPENDIX E


PAGE E-1

Process Samples Data

Bottle Order

LOG-IN

Preparation/Analysis

Data Reduction/Processing

Data Review

Data Submittal

Laboratory Assumes Custody

Refrigerator Containment

Internal COC

Secondary Containment

Archive

Disposal

Submission Files

Raw Data

Diskettes

Tapes

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APPENDIX E

APPENDIX E


PAGE E-2

Sample

Receiving

Preparation

Department

Supervisor

LOGIN

Preparation

Department

Technicians

Analytical

Department

Supervisors

Analysts

CommunicationWork Orders, Hardcopy Work Lists, On-Screen Work Lists, COCs

COCs for short holding/turnaround times and 5-day or less rushes are

distributed

Samples are logged into the

system

Enter samples into the sample

flow(see rush process)

Enter samples into the sample flow (see rush

process)

Rush

Work orders are automatically

generated

Work is monitored

Non-Prep analyses is completed

LIMS

Monitoring

QA

Department

Work is monitored

Preparation is completed

Samples are collected into

method specific LIMS

work lists



work lists

Approval

ApprovalApproval

Approval

Approval

Work lists are printed or

observed on-screen


observed on-screen

Preparation information

is processedApproval

Analysis information

is processed

Prepped analyses is completed

Worklists are

updated

Worklists are

updated

Day 1

Split samples (if applicable)

Day 2 Day 7

If QC is not acceptable

Turnaround time,

Redundant entry

Holding time,Turnaround time,

Redundant sample prep


Redundant analysis,LCS failuresMB failures

Day 6Day 5Day 4Day 3

Performance data is

assessed.

Performance data is

assessed.

Performance data is

assessed.

2 hours

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APPENDIX E

APPENDIX E


PAGE E-3

A request for bottles isissued by the Client

Representative.

A Bottle Order Form iscompleted by the

Project Manager.Bottles are processedaccording to COCs.

The Bottle Order Formand COC are

submitted to theSample Control

Supervisor

The Bottle Prep. Tech.completes the bottle

orderBottle order is checked by

peer review

The completed bottleorder is placed in the

Sample ReceivingArea.

Containers and coolersare transported to

designated site or kept inSample Receiving Area

until the ClientRepresentative assumes

custody

Bottle Orders arechecked by the Client

Representative

Bottle OrderCorrect?

End

Yes

No

Bottle Ordering

Flowchart

Sample Labels arecollated and submittedwith the Bottle OrderForm and COC to the

Bottle PreparationTech.

Do sampleanalyses andsample labels

match?

No

Yes

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APPENDIX E

APPENDIX E


PAGE E-4

Complete Chain of

Custody Form

Take a representativetemperature of the

sample(s)

Unpack ice chests and/or place all samples in

order on the backcounter

Cross-check samplelabel descriptions withthe COC. Also discern

any sample integrityproblems

Conduct proper samplecustody procedures by

logging samples intorefrigerators and completing

sample refrigerator logs.Use the "Distribution" stampon the COC to acknowledge

COC distribution.

Are samples on anaccelerated turnaround

or are holding times inperil?

Place original COC'saccordingly in the

LOGIN tray.

Complete the CoolerReceipt Form (CRF).

Submit COC and CRFto Client Services

Submit a copy of theCOC with a note

stating the problem toClient Services.

Make a copy of theCOC and submit to the

appropriate ClientService representative.

Problems?

Number the samples (if possible) and stamp theCOC with the "numbering

checked by" stamp. Have apeer review the numbering

and acknowledge byinitialing the stamp. Place

samples in the LOGINrefrigerator until problem is

resolved.

Make a copy of theCOC for theappropriate

departments andconduct sample

custody procedures

Temperature withinthe acceptable

range?

See Client ServiceSample ReceivingAnomaly Handling

Flow Chart

No

Yes

Yes

No

Yes

Number the samples(if possible) and stamp theCOC with the "numbering


and acknowledge byinitialing the stamp.

No

Sample Receiving Flowchart

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APPENDIX E

APPENDIX E


PAGE E-5

Client Servicesreceives a copy of a

COC from the SampleCustodian

Is the problemrelated to sample

integrity ornumber?

Client service attemptscontact w ith the client

COC anomalies inregards toanalyses?

Quote or any otherproject information

available?

Client contacted?

Inf ormation is communicatedto Sample Custodian.

Inf ormation and/orconf irmation of c lient

requests are written on theoriginal COC (if project

protocols allow).

Correspondance isdocumented on a

Phone Log.Y es Y es

No

No

Y es Y es

No

Can the problembe solved reliably

w ithout clientcontact?

Yes No

No

Go to the appropriatestep of the particular

f low chart.

Sample Receiving Anomaly Handling Flow Chart

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APPENDIX E

APPENDIX E


PAGE E-6

Analyst secures samples following internal tracking

procedures

Is Sample Preparation required?

Water or Soil?

Sample Preparation Tech secures samples

following internal tracking procedures

Sample Preparation is conductedTesting is conducted

Data is reduced Digests or extracts are submitted to analysts

Sample Splitting is conducted

Organic Testing? Volatiles?Soil

Water No

YesYes

No

No

Yes

Basic Sample Preparation Process Flow

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APPENDIX E

APPENDIX E


PAGE E-7

AnalyticalWorksheet(s) areturned into Client

Services

Analyses are markedout on ProjectCoordinator

Acknowledgements.Dates are recorded.

Worksheets aresubmitted to DataControl. Dates are

recorded.

Worksheets and CARs

are submitted to ClientServices

Fax Required?

CARs and worksheetsare submitted to Data

Control

CARs and worksheets areplaced into submission files.The appropriate analysis iscrossed off and dated on the

acknowledgement form.

CARs are faxed. Thefax record is placed

into the worksheet file


Acknowledgements.Dates are Recorded.

Are all submissionanalyses

completed?

Continue the processuntil all CARs arechecked off on the

acknowledgement form

Remove the submissionfile and complete the

Data Control CompletedSubmission Logbook.Dates are Recorded.Complete submissionlogout on the LIMS.

The Submission folder

is submitted to Client

Services

Coversheet or CaseNarrative is produced. Allappropriate deliverables arecopied and placed into a pre-addressed envelope, or sentby courier if required. Dates

are recorded.

Is QC ReportingRequired?

The entiresubmission file is

turned into theinvoice clerk.Dates arerecorded.

See InvoiceProcess Flowchart

See TheQC

ReportingFlow chartDates arerecorded.

See the Data

Control Flow Chart

Completed Worksheet Flow Diagram

No

No

No

Yes

Yes

No

CorrectionsRequired?

Yes

Yes

Is custom reportingrequired? EDDs?

Custom Reportand/or EDDs

are produced.See EDD

Process Flowchart

No

Yes

Is custom invoicingrequired?

Custom

invoices are

produced.

Yes

No

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR... IT'S TIME FOR...

IT'S TIME FOR...

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APPENDIX E

APPENDIX E


PAGE E-8

Obtain COCs fromtrays. Prioritize

Logging.

Initiate Log-inprocedures

Ambiguous or lackof information?

The original COC anda note with specific

questions is submittedto client services. Seethe Logging AnomalyHandling Flow Chart

Complete samplelogging procedure.

Print worksheets

Organics?

Metals Rushes?

Place worksheets inorange manila

folders.

Distribute paperworkto the appropriate

areas

Go to Prep/AnalysisFlow Charts

Place worksheets inblue/red/plain colored

folders.

All other tests(wet chem,non-rush metals) do notrequire manila folders.Organize by submission.

Discrepanciesfound?

Submit organizedworksheets to the DataControl Supervisor for

review

Worksheets are datedand initialed by the

Data ControlSupervisor

Yes

Yes

No

No

No

Thediscrepantworksheets

arecorrected

Yes

No

Yes

Sample Log-in Procedures

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

Dates/Times shouldbe recorded

Dates should be

recorded

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APPENDIX E

APPENDIX E


PAGE E-9

Worksheets are placedin the black bin in theData Control Room

Worksheets are date -stamped

Worksheets areprioritized and placed

into stacking trays

A portion of work istaken by Data Control

Specialists for dataentry. The samplenumber is entered.

Data from the entireportion of worksheets

taken are entered into theLIMS. Comments areused to decipher theextent of data entry.

Are processedvalues in the

system?

Submit the worksheets tothe appropriatesupervisor for

investigation. Appropriatechanges are made (if

applicable).

Do processed valuesmatch worksheet

values?

The worksheets areseparated to prepare for

printing. Printing tasks arebased on knowledge, a

cheat sheet and/or printingcategory description

LLNL Reports?

Report requiresState Forms?

Reports need to beprinted on recycled

paper?

Place landscape letterheadinto printer cartridge as

needed. Print report thenturn the printer off then on.Place standard letterhead

printer cartridge into printerIf appropriate.

Place plain paper into aprinter cartridge as

needed. Print report thenplace standard letterheadprinter cartridge into the

printer if appropriate.

Standard Report?

Worksheets andprinted reports are

collected into folders.

Folders are placed intothe proofreading bin orsubmitted to a peer for

review.

Discrepanciesfound?

Folders are distributedto the General

Manager and/or Dept.Supervisors for

approval.

Place recycled paper intoa printer cartridge as



Place standard letterheadprinter cartridge into theprinter as needed. Print

report then placestandard letterhead

printer cartridge into theprinter if appropriate.

Discrepanciesfound?

See the appropriate step inthe Completed Worksheet

Flow Diagram.

No

Yes

Yes

Yes

Yes

Yes

No

No

Yes No

Yes

Yes

Data Control Flow Chart

IT'S TIME

FOR...

IT'S TIME

FOR...

IT'S TIME

FOR...

IT'S TIME

FOR...

IT'S TIME

FOR...

IT'S TIME FOR...

IT'S TIME FOR...

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APPENDIX E

APPENDIX E


PAGE E-10

Bench Level Review

Technical Review

Department SupervisorReview

Project CoordinatorReview

Report ApprovalReview

QA/QC Review

Project CoordinatorFinal Review

Conducted by bench analyst:1. QC Parameters - MBs,

dupls, MS/MSD, LCS,Calibration, instrumentperformance

2. Holding times3. Project Protocol4. Data Processing

Conducted by the Dept.Sup., Peer, Team Leader,or QA Dept Personnel,1. Comprehensive (100%)

review of raw data andreporting

2. Documented onspecialized checklists

Conducted by the TechnicalDirector, Dept Sup. or theQA Officer

1. Transcription of results2. Overall integrity of the

final report

Conducted by the QA/QCDept personnel during QCReporting procedures.(Approximately 50 % of thetotal work)

1. DQOs2. Reasonableness of data3. Report formating4. QC Reporting

Data Deliverables

Conducted by respectiveDept. Sup.

1. Transcriptions onto worksheets2. DQOs3. Methodology4. Reasonableness of results

Conducted by ProjectManager or Coordinator

1. DQOs2. Report formating3. Reasonableness of

results

Data Review Process

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APPENDIX E

APPENDIX E


PAGE E-11

Laboratory assumes custody

(Documented on the Chain of Custody Form)

Samples are placed in the appropriate refrigerators.

(Documented on refrigerator logs)

Prep/Analysis conducted

(Document custody on refrigerator logs and preparation/run logs)

Samples are removed from refrigerators after analyses are complete

(Document removal on refrigerator logs)

Containers are stored in on-site Sea-Trains for at least thirty days

(Document custody on a sample tracking log)

Sample disposal is conducted

(Documented on a sample tracking log)

Waste disposal container/drum

contents is profiled or verified

Waste disposal carriers remove waste containers and

transport to proper designations

(documented on manifests)

Laboratory

assumes

custody(documented on

Chain of Custody

Forms)

Samples are

housed in the

walk-in

refrigerator(Documented on the

refrigerator log)

Samples

requiring

inorganic's

testing are split

and housed in

reach in

refrigerators(documented on

refrigerator logs)

Samples and

splits are

removed from

cold storage after

analyses are

completed, and

processed

according to

waste type

Samples are held

in boxes for at

least 30 days

then disposed of

through proper

waste streams(Documented on

sample tracking logs)

Sample TrackingAqueous Matrices

Sample TrackingNon-Aqueous Matrices

Documented on refrigerator logs and on sample tracking logs.

Prep/Analysis

Conducted(document custody on

refrigerator logs and

preparation/run logs)

Samples are placed back into refrigerators from which they were

taken.(Document on refrigerator logs)

Documented in the LIMS

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APPENDIX E

APPENDIX E


PAGE E-12

Data Collection Station

File Server

Instrument Work Station

Internet or

IntranetHardcopy Reports

Client Local or Network StationAuthorization/Data

Request Station

Data Processing Station

Data is produced by the

instrument

Data is collected into the LIMS.

Data is then processed by data

processing specialists

Data is stored and accessed

Data

Diskette

Op

tio

ns

Data Processing for Electronic Data Delivery

Instrument have direct

and/or indirect links to

the Laboratory

Information

Management System

(LIMS)

All data processing is

reviewed by a second

person

All electronic data is reviewed prior to final submittal

All files on diskettes are verified as to type and content.

Virus checks are conducted on all disks

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APPENDIX E

APPENDIX E


PAGE E-13

Orientation All new employees

IDC ChecklistOn the Job

TrainingAll new analysts or a change

in responsibility

Training Process

Orientation

Checklist

Internal

Training Modules

Continuous Training

Based on job description

Certificates of

Completion

Enter the external

training programEmployee discretion

Diploma, Certificate

of Completion,

Record of attendance

Continuous Training

Training Documentation

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APPENDIX E

APPENDIX E


PAGE E-14


levels


Analyze the ICV


met?

Continue the run




Initiate Corrective

Procedures(SIF)Options





No

Yes

Yes


Initiate Corrective

Action(SIF)

No

Yes

No

Options






Initial Calibration Logic for GC/HPLC MethodsIC_GCHPLC.vsd

Rev. 404/07/05





curve.

Mean RSD < 20%?

r > 0.99?



than 20.





COD > 0.99?

Yes

No

Yes

No

Yes



range.

No

Yes



range.

No



proceeding steps.





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APPENDIX E

APPENDIX E


PAGE E-15

Instrument run is completed

The analyst reviews the data

Problems found?Problems are

documented on a review sheet

Reviewed data with the review sheet are

submitted back to the analyst

Analyst collects worksheets

Analyst enters results and other information

onto worksheets

The analyst submits the analytical run to a

peer for review

Worksheets are submitted to the Dept Supervisor for review

and approval.

Go to the Completed Worksheet Flow

Diagram


Analyst downloads the run onto the LIMS

The analyst reviews the run and completes

a review sheet

The analytical run and the review sheet is submitted

to a data processing specialist (DPS).

The analytical run is processed and

reviewed by a Data Processing Specialist.

The processed run information and raw

data is submitted to a designated technical

reviewer.

The technical reviewer reviews the raw data and the processed

information.

Problems with the analytical run?

Information is communicated to the analyst and corrective

action is initiated (if applicable).

The processed run, raw data and review sheets

are submitted to the analyst for approval. All

disagreements are midigated by the Dept.

Supervisor.

Problems with the data processing?

Information is communicated to the DPS and corrective action is initiated (if

applicable).

Results are posted.

Sample and QC results are sent

electronically to the Department Supervisor

for review and approval.

Certified analytical reports are printed

No

Yes

Yes

No

No

Analytical Review, Reporting and Approval Flow chart for ICP Analyses

Current Process Proposed/Parallel ProcessIT'S TIME FOR...

IT'S TIME FOR...

Dates are recorded

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

Dates/times should be recorded

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APPENDIX E

APPENDIX E


PAGE E-16

24 Hours

BC Laboratories, Inc.

Samples are submitted by Client Representatives and chain of custody procedures are initiated

Lab analytical worksheets are filled out by the Bac-T analyst

Well

100 mls of sample set up with with Colilert reagent. Sample is kept in an incubator for 24 hours. If yellow color is formed, sample is positive for total coliform. A check for fluorescence is conducted to indicate presence of E. Coli.

Wastewater Samples 5,5,5 with Lauryl Tryptose Broth (presumptive) followed by Total Coliform confirmation (Brilliant Green Bile)Presumptive Test takes 24 - 48 hours, confirmation another 24 - 48 hours.

48 Hours

Disposal

Media/samples are autoclaved prior to disposal

Notification

Positives are called in by a BC Laboratories, Inc. Representative

Reports

Certified analytical reports are mailed.

Interpretation and Action

Corrective action, if necessary is conducted by Client personnel

Disclosure

State government is notifed on results and/or actions taken

Process Quality ControlBacteriological

Testing

Positive/negative culture controls on each lot of Colilert productIncubator temperature checked twice per day.Thermometers checked annually against NIST reference thermometer.Certified sample containers

Positive/negative culture controls for each media.Pipet sterility checkAutoclave sterility checksAutoclave temperature and temperature distribution checksMedia control check after autoclave


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APPENDIX E

APPENDIX E


PAGE E-1

Process Samples Data

Bottle Order

LOG-IN

Preparation/Analysis

Data Reduction/Processing

Data Review

Data Submittal

Laboratory Assumes Custody

Refrigerator Containment

Internal COC

Secondary Containment

Archive

Disposal

Submission Files

Raw Data

Diskettes

Tapes

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APPENDIX E

APPENDIX E


PAGE E-2

Sample

Receiving

Preparation

Department

Supervisor

LOGIN

Preparation

Department

Technicians

Analytical

Department

Supervisors

Analysts

CommunicationWork Orders, Hardcopy Work Lists, On-Screen Work Lists, COCs

COCs for short holding/turnaround times and 5-day or less rushes are

distributed

Samples are logged into the

system

Enter samples into the sample

flow(see rush process)

Enter samples into the sample flow (see rush

process)

Rush

Work orders are automatically

generated

Work is monitored

Non-Prep analyses is completed

LIMS

Monitoring

QA

Department

Work is monitored

Preparation is completed



work lists



work lists

Approval

ApprovalApproval

Approval

Approval


observed on-screen


observed on-screen

Preparation information

is processedApproval

Analysis information

is processed

Prepped analyses is completed

Worklists are

updated

Worklists are

updated

Day 1

Split samples (if applicable)

Day 2 Day 7

If QC is not acceptable

Turnaround time,

Redundant entry


Redundant sample prep


Redundant analysis,LCS failuresMB failures

Day 6Day 5Day 4Day 3

Performance data is

assessed.

Performance data is

assessed.

Performance data is

assessed.

2 hours

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APPENDIX E

APPENDIX E


PAGE E-3

A request for bottles isissued by the Client

Representative.

A Bottle Order Form iscompleted by the

Project Manager.Bottles are processedaccording to COCs.

The Bottle Order Formand COC are

submitted to theSample Control

Supervisor

The Bottle Prep. Tech.completes the bottle

orderBottle order is checked by

peer review

The completed bottleorder is placed in the

Sample ReceivingArea.

Containers and coolersare transported to

designated site or kept inSample Receiving Area

until the ClientRepresentative assumes

custody

Bottle Orders arechecked by the Client

Representative

Bottle OrderCorrect?

End

Yes

No

Bottle Ordering

Flowchart

Sample Labels arecollated and submittedwith the Bottle OrderForm and COC to the

Bottle PreparationTech.

Do sampleanalyses andsample labels

match?

No

Yes

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APPENDIX E

APPENDIX E


PAGE E-4

Complete Chain of

Custody Form

Take a representativetemperature of the

sample(s)

Unpack ice chests and/or place all samples in

order on the backcounter

Cross-check samplelabel descriptions withthe COC. Also discern

any sample integrityproblems

Conduct proper samplecustody procedures by

logging samples intorefrigerators and completing

sample refrigerator logs.Use the "Distribution" stampon the COC to acknowledge

COC distribution.

Are samples on anaccelerated turnaround

or are holding times inperil?

Place original COC'saccordingly in the

LOGIN tray.

Complete the CoolerReceipt Form (CRF).

Submit COC and CRFto Client Services

Submit a copy of theCOC with a note

stating the problem toClient Services.

Make a copy of theCOC and submit to the

appropriate ClientService representative.

Problems?

Number the samples (if possible) and stamp theCOC with the "numbering


and acknowledge byinitialing the stamp. Place

samples in the LOGINrefrigerator until problem is

resolved.

Make a copy of theCOC for theappropriate

departments andconduct sample

custody procedures

Temperature withinthe acceptable

range?

See Client ServiceSample ReceivingAnomaly Handling

Flow Chart

No

Yes

Yes

No

Yes

Number the samples(if possible) and stamp theCOC with the "numbering


and acknowledge byinitialing the stamp.

No

Sample Receiving Flowchart

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APPENDIX E

APPENDIX E


PAGE E-5

Client Servicesreceives a copy of a

COC from the SampleCustodian

Is the problemrelated to sample

integrity ornumber?

Client service attemptscontact w ith the client

COC anomalies inregards toanalyses?

Quote or any otherproject information

available?

Client contacted?

Inf ormation is communicatedto Sample Custodian.

Inf ormation and/orconf irmation of c lient

requests are written on theoriginal COC (if project

protocols allow).

Correspondance isdocumented on a

Phone Log.Y es Y es

No

No

Y es Y es

No

Can the problembe solved reliably

w ithout clientcontact?

Yes No

No

Go to the appropriatestep of the particular

f low chart.

Sample Receiving Anomaly Handling Flow Chart

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APPENDIX E

APPENDIX E


PAGE E-6

Analyst secures samples following internal tracking

procedures

Is Sample Preparation required?

Water or Soil?

Sample Preparation Tech secures samples

following internal tracking procedures

Sample Preparation is conductedTesting is conducted

Data is reduced Digests or extracts are submitted to analysts

Sample Splitting is conducted

Organic Testing? Volatiles?Soil

Water No

YesYes

No

No

Yes

Basic Sample Preparation Process Flow

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APPENDIX E

APPENDIX E


PAGE E-7

AnalyticalWorksheet(s) areturned into Client

Services


Acknowledgements.Dates are recorded.

Worksheets aresubmitted to DataControl. Dates are

recorded.

Worksheets and CARs

are submitted to ClientServices

Fax Required?

CARs and worksheetsare submitted to Data

Control

CARs and worksheets areplaced into submission files.The appropriate analysis iscrossed off and dated on the

acknowledgement form.

CARs are faxed. Thefax record is placed

into the worksheet file


Acknowledgements.Dates are Recorded.

Are all submissionanalyses

completed?

Continue the processuntil all CARs arechecked off on the

acknowledgement form

Remove the submissionfile and complete the

Data Control CompletedSubmission Logbook.Dates are Recorded.Complete submissionlogout on the LIMS.

The Submission folder

is submitted to Client

Services

Coversheet or CaseNarrative is produced. Allappropriate deliverables arecopied and placed into a pre-addressed envelope, or sentby courier if required. Dates

are recorded.

Is QC ReportingRequired?

The entiresubmission file is

turned into theinvoice clerk.Dates arerecorded.

See InvoiceProcess Flowchart

See TheQC

ReportingFlow chartDates arerecorded.

See the Data

Control Flow Chart

Completed Worksheet Flow Diagram

No

No

No

Yes

Yes

No

CorrectionsRequired?

Yes

Yes

Is custom reportingrequired? EDDs?

Custom Reportand/or EDDs

are produced.See EDD

Process Flowchart

No

Yes

Is custom invoicingrequired?

Custom

invoices are

produced.

Yes

No

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR... IT'S TIME FOR...

IT'S TIME FOR...

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APPENDIX E

APPENDIX E


PAGE E-8

Obtain COCs fromtrays. Prioritize

Logging.

Initiate Log-inprocedures

Ambiguous or lackof information?

The original COC anda note with specific

questions is submittedto client services. Seethe Logging AnomalyHandling Flow Chart

Complete samplelogging procedure.

Print worksheets

Organics?

Metals Rushes?

Place worksheets inorange manila

folders.

Distribute paperworkto the appropriate

areas

Go to Prep/AnalysisFlow Charts

Place worksheets inblue/red/plain colored

folders.

All other tests(wet chem,non-rush metals) do notrequire manila folders.Organize by submission.

Discrepanciesfound?

Submit organizedworksheets to the DataControl Supervisor for

review

Worksheets are datedand initialed by the

Data ControlSupervisor

Yes

Yes

No

No

No

Thediscrepantworksheets

arecorrected

Yes

No

Yes

Sample Log-in Procedures

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

Dates/Times shouldbe recorded

Dates should be

recorded

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APPENDIX E

APPENDIX E


PAGE E-9

Worksheets are placedin the black bin in theData Control Room

Worksheets are date -stamped

Worksheets areprioritized and placed

into stacking trays

A portion of work istaken by Data Control

Specialists for dataentry. The samplenumber is entered.

Data from the entireportion of worksheets

taken are entered into theLIMS. Comments areused to decipher theextent of data entry.

Are processedvalues in the

system?

Submit the worksheets tothe appropriatesupervisor for

investigation. Appropriatechanges are made (if

applicable).

Do processed valuesmatch worksheet

values?

The worksheets areseparated to prepare for

printing. Printing tasks arebased on knowledge, a

cheat sheet and/or printingcategory description

LLNL Reports?

Report requiresState Forms?

Reports need to beprinted on recycled

paper?

Place landscape letterheadinto printer cartridge as

needed. Print report thenturn the printer off then on.Place standard letterhead

printer cartridge into printerIf appropriate.

Place plain paper into aprinter cartridge as



Standard Report?

Worksheets andprinted reports are

collected into folders.

Folders are placed intothe proofreading bin orsubmitted to a peer for

review.

Discrepanciesfound?

Folders are distributedto the General

Manager and/or Dept.Supervisors for

approval.

Place recycled paper intoa printer cartridge as



Place standard letterheadprinter cartridge into theprinter as needed. Print

report then placestandard letterhead

printer cartridge into theprinter if appropriate.

Discrepanciesfound?

See the appropriate step inthe Completed Worksheet

Flow Diagram.

No

Yes

Yes

Yes

Yes

Yes

No

No

Yes No

Yes

Yes

Data Control Flow Chart

IT'S TIME

FOR...

IT'S TIME

FOR...

IT'S TIME

FOR...

IT'S TIME

FOR...

IT'S TIME

FOR...

IT'S TIME FOR...

IT'S TIME FOR...

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APPENDIX E

APPENDIX E


PAGE E-10

Bench Level Review

Technical Review

Department SupervisorReview

Project CoordinatorReview

Report ApprovalReview

QA/QC Review

Project CoordinatorFinal Review

Conducted by bench analyst:1. QC Parameters - MBs,

dupls, MS/MSD, LCS,Calibration, instrumentperformance

2. Holding times3. Project Protocol4. Data Processing

Conducted by the Dept.Sup., Peer, Team Leader,or QA Dept Personnel,1. Comprehensive (100%)

review of raw data andreporting

2. Documented onspecialized checklists

Conducted by the TechnicalDirector, Dept Sup. or theQA Officer

1. Transcription of results2. Overall integrity of the

final report

Conducted by the QA/QCDept personnel during QCReporting procedures.(Approximately 50 % of thetotal work)

1. DQOs2. Reasonableness of data3. Report formating4. QC Reporting

Data Deliverables

Conducted by respectiveDept. Sup.

1. Transcriptions onto worksheets2. DQOs3. Methodology4. Reasonableness of results

Conducted by ProjectManager or Coordinator

1. DQOs2. Report formating3. Reasonableness of

results

Data Review Process

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APPENDIX E

APPENDIX E


PAGE E-11

Laboratory assumes custody

(Documented on the Chain of Custody Form)

Samples are placed in the appropriate refrigerators.

(Documented on refrigerator logs)

Prep/Analysis conducted

(Document custody on refrigerator logs and preparation/run logs)

Samples are removed from refrigerators after analyses are complete

(Document removal on refrigerator logs)

Containers are stored in on-site Sea-Trains for at least thirty days

(Document custody on a sample tracking log)

Sample disposal is conducted

(Documented on a sample tracking log)

Waste disposal container/drum

contents is profiled or verified

Waste disposal carriers remove waste containers and

transport to proper designations

(documented on manifests)

Laboratory

assumes

custody(documented on

Chain of Custody

Forms)

Samples are

housed in the

walk-in

refrigerator(Documented on the

refrigerator log)

Samples

requiring

inorganic's

testing are split

and housed in

reach in

refrigerators(documented on

refrigerator logs)

Samples and

splits are

removed from

cold storage after

analyses are

completed, and

processed

according to

waste type

Samples are held

in boxes for at

least 30 days

then disposed of

through proper

waste streams(Documented on

sample tracking logs)

Sample TrackingAqueous Matrices

Sample TrackingNon-Aqueous Matrices

Documented on refrigerator logs and on sample tracking logs.

Prep/Analysis

Conducted(document custody on

refrigerator logs and

preparation/run logs)

Samples are placed back into refrigerators from which they were

taken.(Document on refrigerator logs)

Documented in the LIMS

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APPENDIX E

APPENDIX E


PAGE E-12

Data Collection Station

File Server

Instrument Work Station

Internet or

IntranetHardcopy Reports

Client Local or Network StationAuthorization/Data

Request Station

Data Processing Station

Data is produced by the

instrument

Data is collected into the LIMS.

Data is then processed by data

processing specialists

Data is stored and accessed

Data

Diskette

Op

tio

ns

Data Processing for Electronic Data Delivery

Instrument have direct

and/or indirect links to

the Laboratory

Information

Management System

(LIMS)

All data processing is

reviewed by a second

person

All electronic data is reviewed prior to final submittal

All files on diskettes are verified as to type and content.

Virus checks are conducted on all disks

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APPENDIX E

APPENDIX E


PAGE E-13

Orientation All new employees

IDC ChecklistOn the Job

TrainingAll new analysts or a change

in responsibility

Training Process

Orientation

Checklist

Internal

Training Modules

Continuous Training

Based on job description

Certificates of

Completion

Enter the external

training programEmployee discretion

Diploma, Certificate

of Completion,

Record of attendance

Continuous Training

Training Documentation

UNCONTROLLED COPY



APPENDIX E

APPENDIX E


PAGE E-14


levels


Analyze the ICV


met?

Continue the run




Initiate Corrective

Procedures(SIF)Options





No

Yes

Yes


Initiate Corrective

Action(SIF)

No

Yes

No

Options






Initial Calibration Logic for GC/HPLC MethodsIC_GCHPLC.vsd

Rev. 404/07/05





curve.

Mean RSD < 20%?

r > 0.99?



than 20.





COD > 0.99?

Yes

No

Yes

No

Yes



range.

No

Yes



range.

No



proceeding steps.





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APPENDIX E

APPENDIX E


PAGE E-15


The analyst reviews the data

Problems found?Problems are

documented on a review sheet

Reviewed data with the review sheet are

submitted back to the analyst

Analyst collects worksheets

Analyst enters results and other information

onto worksheets

The analyst submits the analytical run to a

peer for review

Worksheets are submitted to the Dept Supervisor for review

and approval.

Go to the Completed Worksheet Flow

Diagram


Analyst downloads the run onto the LIMS

The analyst reviews the run and completes

a review sheet

The analytical run and the review sheet is submitted

to a data processing specialist (DPS).

The analytical run is processed and

reviewed by a Data Processing Specialist.

The processed run information and raw

data is submitted to a designated technical

reviewer.

The technical reviewer reviews the raw data and the processed

information.

Problems with the analytical run?

Information is communicated to the analyst and corrective

action is initiated (if applicable).

The processed run, raw data and review sheets

are submitted to the analyst for approval. All

disagreements are midigated by the Dept.

Supervisor.

Problems with the data processing?

Information is communicated to the DPS and corrective action is initiated (if

applicable).

Results are posted.

Sample and QC results are sent

electronically to the Department Supervisor

for review and approval.

Certified analytical reports are printed

No

Yes

Yes

No

No

Analytical Review, Reporting and Approval Flow chart for ICP Analyses

Current Process Proposed/Parallel ProcessIT'S TIME FOR...

IT'S TIME FOR...

Dates are recorded

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

IT'S TIME FOR...

Dates/times should be recorded

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APPENDIX E

APPENDIX E


PAGE E-16

24 Hours


Samples are submitted by Client Representatives and chain of custody procedures are initiated

Lab analytical worksheets are filled out by the Bac-T analyst

Well

100 mls of sample set up with with Colilert reagent. Sample is kept in an incubator for 24 hours. If yellow color is formed, sample is positive for total coliform. A check for fluorescence is conducted to indicate presence of E. Coli.

Wastewater Samples 5,5,5 with Lauryl Tryptose Broth (presumptive) followed by Total Coliform confirmation (Brilliant Green Bile)Presumptive Test takes 24 - 48 hours, confirmation another 24 - 48 hours.

48 Hours

Disposal

Media/samples are autoclaved prior to disposal

Notification

Positives are called in by a BC Laboratories, Inc. Representative

Reports

Certified analytical reports are mailed.

Interpretation and Action

Corrective action, if necessary is conducted by Client personnel

Disclosure

State government is notifed on results and/or actions taken

Process Quality ControlBacteriological

Testing

Positive/negative culture controls on each lot of Colilert productIncubator temperature checked twice per day.Thermometers checked annually against NIST reference thermometer.Certified sample containers

Positive/negative culture controls for each media.Pipet sterility checkAutoclave sterility checksAutoclave temperature and temperature distribution checksMedia control check after autoclave


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APPENDIX F

APPENDIX F


PAGE F-1

Ethics Agreement


ETHICS AND DATA INTEGRITY AGREEMENT

I. I, (Name), State that I understand

the high standards of integrity required of me with regard to the duties I perform and

the data I report in connection with my employment at BC Laboratories, Inc.

II. I agree that in the performance of my duties at BC Laboratories, Inc:

a. I shall not intentionally report data values that are not the actual values

obtained;

b. I shall not intentionally report the dates and times of

samples/standards/reagent preparation that are not the actual dates and

times of samples/standards/reagents preparation.

c. I shall not intentionally report the dates and times of data analyses that are

not the actual dates and times of data analyses.

d. I shall not intentionally represent another individual=s work as my own; and

e. I shall abide by the Code of Ethics Policy listed in the BC Laboratories, Inc.

QAPP (Located in the Conference Room).

III. I agree to inform BC Laboratories, Inc. of any accidental reporting of non-authentic

data by myself in a timely manner.

IV. I agree to inform BC Laboratories, Inc. of any accidental or intentional reporting of

non-authentic data by other employees.

(Signature)

(Date)

Note: Appendix F was review on 01/13/15 (No changes were made)

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APPENDIX G

APPENDIX G


PAGE G-1

USER FLAGS Qualifiers

*A Absent

*Fail Fail

*I Not Ignitable

*P Present

*Pass Pass

*R [Custom Value]

< <[Custom Value]

<=2 <= 2

<1 < 1

<1.1 < 1.1

<2 < 2

> >[Custom Value]

> 140 >140

>23 > 23

A01 PQL's and MDL's are raised due to sample dilution.

A02 The difference between duplicate readings is less than the PQL.

A03 The sample concentration is more than 4 times the spike level.

A04 Method of Standard Additions used to calculate result.

A05 Unable to report specific MPN due to insufficient dilutions.

A06 The sample was preserved within 24 hours of the collection time.

A09 PQL's were raised due to high concentration of target analytes requiring sample dilution.

A10 PQL's and MDL's were raised due to matrix interference.

A11 PQL's and/or MDL's were raised due to inadequate sample size received.

A12 PQL's were raised due to high concentrations of hydrocarbons present requiring sample dilution.

A14 All phenolic compound results are affected due to low phenol surrogate recoveries caused by matrix.

A17 Surrogate not reportable due to sample dilution.

A18 Surrogate not reportable due to matrix interference.

A19 Surrogate is high due to matrix interference. Interferences verified through second extraction/analysis.

A20 Surrogate is low due to matrix interference. Interference verified through second extraction/analysis.

A22 Associated surrogate recovery is low.

A23 Associated surrogate recovery is high.

A26 Sample received past holding time.

A39 Sample received at pH greater than 2.

A40 Initial calibration linearity criteria not met.

A41 Results confirmed by GC/MS.

A43 Primary/Confirmation column ratios do not agree, results may be biased.

A48 Matrix spike interferences may be associated with this analyte.

A51 Chromatogram not typical of Diluent.

A52 Chromatogram not typical of diesel.

A53 Chromatogram not typical of gasoline.

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APPENDIX G

APPENDIX G


PAGE G-2


A54 Chromatogram not typical of kerosene.

A55 Chromatogram not typical of crude oil.

A56 Chromatogram not typical of stoddard solvent.

A57 Chromatogram not typical of motor oil.

A58 Chromatogram not typical of hydraulic oil.

A59 Results calculated on a dry weight basis.

A61 Result is estimated a coeluting compound is also present at same retention time.

A66 Method blank for {%1} detected at {%2}.

A68 Presence of MTBE not confirmed by GC/MS.

A70 Surrogate recovery calculated from the confirmation column due to matrix interferences on the primary column.

A71 TBOS result subtracted from diesel range for final diesel result.

A72 PQL's and/or MDL's were raised due to high moisture content.

A74 A negative reading whose absolute value is greater than the MDL was obtained for the method blank.

A79 Prepared by EPA Method 5035.

A81 The result is below the calibration limit of the instrument. Due to the calibration technique used, a numerical result cannot be reported.

A83 Result based on tentatively identified compound search.

A84 Compound is a Non-Target Analyte

A85 Analyte is a Tentatively Identified Compound

A87 Carry over from a previously analyzed sample.

A88 Unable to report specific number. Insufficient dilutions to accommodate high concentration.

A89 TPH C4-C12

A90 TPPH does not exhibit a "gasoline" pattern. TPPH is entirely due to MTBE.

A91 TPH does not exhibit a "gasoline" pattern. TPH is entirely due to MTBE.

B Analyte found in blank sample (CLP Flag)

B01 Analyte detected in the Continuing Calibration Blank (CCB) at a level greater than the PQL.

B02 Analyte detected in the Continuing Calibration Blank (CCB) at a level between the PQL and 1/2 the PQL.

B03 Analyte detected in the Continuing Calibration Blank (CCB) at a level between the PQL and the MDL.

B04 The batch size for the Continuing Calibration Blank (CCB) exceeds the control limit.

B05 The time interval between Continuing Calibration Blank exceeds the control limit.

B06 The number of consecutive analyses of the Continuing Calibration Blank exceeds the control limit.

B07 The analytical sequence did not contain a Continuing Calibration Blank at the end.

C01 The calibration curve did not contain the minimum number of standards.

C02 The relative standard deviation of the calibration curve response factors exceeds the control limit.

C03 The correlation coefficient for the calibration was below the minimum control limit.

C04 The standards for the calibration were not analyzed on the same day.

C05 The standards for the calibration were not analyzed consecutively.

C06 The average of the calibration curve response factors exceeds the control limit.

C07 The response factor for a System Performance Check Compound (SPCC) is below the acceptable limit.

C08 The relative standard deviation of the calibration curve response factors for a Calibration Check Compound (CCC) exceeds the control limit.

D Dilution Used (CLP Flag)

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APPENDIX G

APPENDIX G


PAGE G-3


D01 Recovery of a standard ath the PQL exceeded the control limit.

F1 Diesel range is C12-C14

F2 Motor Oil range is C25-C36

F3 WD-40 range is C8-C16

F4 Av Gas range is C6-C12

F5 Jet Fuel JP8 range is C6-CC14

F6 Kerosene range is C10-C20

FT01 Field sampled by certified personnel

I1 Baseline adjustment

I2 Peak correction

I3 Rider removal

I4 Retention time

J Estimated Value (CLP Flag)

L01 The Laboratory Control Sample Water (LCSW) recovery is not within laboratory established control limits.

L02 The Laboratory Control Sample Water (LCSW) recovery is not within method established control limits.

L03 The batch size for the Laboratory Control Sample Water (LCSW) exceeds the control limit.

L04 The matrix of the sample does not match the Laboratory Control Sample Water (LCSW)

L05 The Laboratory Control Sample Water (LCSW) was not analyzed prior to all the samples in the batch.

L06 The relative percent difference between the Laboratory Control Sample Water (LCSW) and the LCSW Duplicate exceeds the control limit.

L07 The Laboratory Control Sample (LCS) recovery is not within laboratory established control limits.

L08 The relative percent difference between the Laboratory Control Sample (LCS) and the LCS Duplicate exceeds the control limit.

L21 The Laboratory Control Sample Soil (LCSS) recovery is not within laboratory established control limits.

L22 The Laboratory Control Sample Soil (LCSS) recovery is not within method established control limits.

L23 The batch size for the Laboratory Control Sample Soil (LCSS) exceeds the control limit.

L24 The matrix of the sample does not match the Laboratory Control Sample Soil (LCSS)

L25 The Laboratory Control Sample Soil (LCSS) was not analyzed prior to all the samples in the batch.

L26 The relative percent difference between the Laboratory Control Sample Soil (LCSS) and the LCSS Duplicate exceeds the control limit.

M01 Analyte detected in the Method Blank at or above the PQL.

M02 Analyte detected in the Method Blank at a level between the PQL and 1/2 the PQL.

M03 Analyte detected in the Method Blank at a level between the PQL and the MDL.

M04 The batch size for the Method Blank exceeds the control limit.

M05 The Method Blank was not analyzed prior to all the samples in the batch.

M06 The internal standard on the Method Blank was not within the control limits.

M07 The surrogate recovery on the Method Blank for this compound was not within the control limits.

N01 This analyte exceeded the PQL in the beginning interference check standard.

N02 Recovery of this analyte in the beginning spiked interference check standard was not within the control limits.

N03 The beginning interference check standard was not analyzed prior to this sample.

N11 This analyte exceeded the PQL in the ending interference check standard.

N12 Recovery of this analyte in the ending spiked interference check standard was not within the control limits.

N13 The ending interference check standard was not analyzed after this sample.

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APPENDIX G

APPENDIX G


PAGE G-4


ND ND

NoObO No Obs Odor

NR Non-Reactive

NR2 Non-Reactive

NTA Non Target Analyte

P01 Post spike recovery was not within the control limits.

P02 The batch size for the Post Spike exceeds the control limit.

P03 The relative percent difference between the duplicate Post Spikes exceeds the control limit.

PD Sample container was preserved on [Custom Value]

pH1:1 pH result reported on a 1:1 dilution of sample



pHdil pH result reported on a 1:[Custom Value] dilution of sample

pHsat pH result reported on a saturated paste of sample

pHstr pH result reported on a straight aliquot of sample

Q01 Sample precision is not within the control limits.

Q02 Matrix spike precision is not within the control limits.

Q03 Matrix spike recovery(s) is (are) not within the control limits.

Q04 The batch size for the QC set exceeds the control limit.

Q05 The matrix of the sample does not match that of the spike samples.

Q06 The dilutions of the quality control set are not consistent.

R01 The sample result is between the MDL and PQL.

R11 Per client request the reported PQL is less than the laboratory PQL but above the laboratory MDL.

S01 Sample result is not within the quantitation range of the method.

S02 The relative percent difference between duplicate instrument readings exceeds the control limit.

S03 A negative reading whose absolute value is greater than the PQL was obtained for the sample.

S04 The instrument reading for the sample was not a numeric value.

S05 The sample holding time was exceeded.

S06 There was an excessive amount of time between the prior sample and this sample in the analytical run.

S07 This sample result may contain carry over from the prior analytical sample.

S08 The internal standard on the sample was not within the control limits.

S09 The surrogate recovery on the sample for this compound was not within the control limits.

S10 The analyte in the Method Blank is greater than the laboratory PQL and the sample result is less than 10 times the Method Blank.

S11 The analyte in the Method Blank is greater than the laboratory PQL but the sample result is greater than 10 times the Method Blank.

S12 The Method Blank bias is greater than the PQL

U Analyte Not Detected at or above the reporting limit (CLP Flag)

V01 The Initial Calibration Verification (ICV) recovery is not within established control limits.

V02 Not all of the calibration standards were analyzed prior to the Initial Calibration Verification (ICV).

V03 The internal standard on the Initial Calibration Verification (ICV) was not within the control limits.

V11 The Continuing Calibration Verification (CCV) recovery is not within established control limits.

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APPENDIX G

APPENDIX G


PAGE G-5


V12 More than the acceptable numbers of samples were analyzed between Continuing Calibration Verification (CCV) standards.

V13 The time interval between Continuing Calibration Verification standards exceeds the control limit.

V14 The Continuing Calibration Verification (CCV) standard was reanalyzed more than the acceptable number of times.

V15 There was no Continuing Calibration Verification (CCV) at the end of the analytical sequence.

V16 The internal standard on the Continuing Calibration Verification (CCV) was not within the control limits.

V17 The percent deviation between the Continuing Calibration Verification (CCV) and the original calibration exceeds the control limit.

V18 The instrument response for a System Performance Check Compound (SPCC) on the Continuing Calibration Verification (CCV) is below

the control limit. V19 The relative standard deviation of the calibration curve response factors for a Calibration Check Compound (CCC) in the Continuing

Calibration Verification (CCV) exceeds the control limit.

V20 For EPA 200.8 analyses the acceptable recovery is 85% - 115% for a CCV following sample analysis.

W1 Analysis performed by Weck Laboratories, Inc.

Z1 [Custom Value]

Z2 [Custom Value]

Z3 [Custom Value]

Z4 [Custom Value]

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APPENDIX H

APPENDIX H


REVISED 03/15/16

PAGE H-1

SOPs Table List Of SOP (Initial The SOP that pertains to your Job duties or responsibilities)

Inorganic Dept.

SOP ID SAVED AS SOP TITLE REV

Analyst Int.

BCGEN004 ALKALSOPR7 Carbonate, Bicarbonate, Alkalinity, 310.1/SM 2320B 7

BCGEN005 COLOR5 Color/ 110.2/SM 2120B 5

BCGEN007 DSOXYGENR5 Dissolved Oxygen/360.1 SM4500-06 5

BCGEN009 SETTEABLR7 Settleable Solids/160.5/SM 2540F 7

BCGEN010 CHLORINER6 Residual Chlorine/330.4/SM 4500-CLF 6

BCGEN011 ECR6 Specific Conductance (EC)9050 120.1 SM 2510B 6

BCGEN013 TDSR8 Total Dissolved Solids Filterable Residue 160.1/SM 2540C 8

BCGEN014 TURBIDITR5 Turbidity/180.1/SM 2130B 5

BCGEN016 WCBACTERRev13 Bacteriology (Coliform/Fecal) 13

BCGEN017 BODR8 Analyte: Biochemical Oxygen 405.1 SM5210B 8

BCGEN020 SULF376_1R7 Sulfide 376.1/SM 4500/9030 7

BCGEN021 MBASR8 MBAS/EPA 425.1/ SM 5540C 8

BCGEN022 TSSR6 Total Suspended Solids/EPA 160.2/SM 2540 D 6

BCGEN024 ODOR6 Odor/EPA 140.1/SM 2150 6

BCGEN026 COD410_4R8 Chemical Oxygen Demand Colormetric, Manual/410.4/SM 5220D 8

BCGEN033 PHREV8 PH/EPA 150.1/9040 8

BCGEN035 REACTSULREV7 Reactive Sulfide\\EPA Method 7.3.4.1 7

BCGEN039 WCTOCR15 Total Organic Carbon (TOC)/ SW 5310C/EPA 415.1 15

BCGEN040 SULF376_2R7 Sulfide Method 376.2 7

BCGEN043 160.4R5 Fixed and Volatile Solids, 160.4/SM 2540E 5

BCGEN044 GLASSWR6 General Glassware Washing 6

BCGEN046 TOTRESR4 Total Residue 160.3 SW 2540B 4

BCGEN048 EPA300R10 Determination of Anion in water and solid by Dionex IC DX500/EPA 300.0 (9056) 10

BCGEN049 EPA314.0R9 Perchlorate / 314.0 9

BCGEN050 DEWAPRODR2 Deionized Water Productiion-Nanopure water 2

BCGEN051 KLORTH_365.1R5 ORTHOPHOSPHATE EPA 365.1 5

BCGEN052 KLHEXACROMR6 KONELAB HEXAVALENT CHROMIUM-7196 A 6

BCGEN053 PhSOLIDR4 EPA METHOD 9040C, 9045D 4

BCGEN055 KLNOR5 KONELAB NITRITE NITROGEN EPA 353.2 5

BCGEN056 HEXCR_218.6R6 HEXAVALENT CHROMIUM EPA 218.6/7199 6

BCGEN057 KLNCYNR7 KONELAB CYANIDE EPA 335.2/33.4/9012A/SM4500-CN-G, I (same as 9010) 7

BCGEN058 SC_NO3-NR4 Smartchem Nitrogen, Nitrate-Nitrite/EPA Method 353.2 4

BCGEN059 SC_TKN-NR5 Smartchem Total Kjeldahl Nitrogen/EPA Method 351.2 5

BCGEN060 SC_TOT_PR4 Smartchem Total Phosphorus/EPA Method 365.4/SM 4500-P 4

BCGEN061 SC_NH3-NR4 Smartchem Ammonia - Nitrogen/EPA method 350.1 (SM-4500-NH3-G) 4

BCGEN062 KLPHENOLR5 Konelab Total Recoverable Phenolics EPA 420.4 5

BCGEN063 REACTCYANR1 Reactive Cyanide\\EPA Method 7.3.3.2 1

BCGEN064 SC_PHENOLR0 Smartchem Total Recoverable Phenolics EPA 420.4 (Inactive SOP 4-13-10) 0

BCGEN065 METROHMR2 Electrical Conductivity, pH, Alkalinity// EPA 9050/120.1/SM 2510B, EPA 9040/150.1/SM 4500HB, EPA 310.1/ SM 2320B 2

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APPENDIX H

APPENDIX H


REVISED 03/15/16

PAGE H-2

Inorganic Dept.


Analyst Int.

BCGEN066 CO2_R1 Free Carbon Dioxide in Water-SM4500 1

BCGEN067 ORP_R1 Oxidation-Reduction Potential in Water 1

BCGEN068 SM3500_FeR0 SM 3500 FeD - Ferrous Iron 0

BCGEN069 FLASHPOINTR0 Flash Point by Pensky-Martens Closed Tester/ASTM D-93, EPA Method 1010 0

BCGEN070 IGNIT_EPA1030R0 IGNITABILITY OF SOLIDS-EPA Method 1030 0

BCGEN071 EPA300M-FATTYAR0

DETERMINATION OF ORGANIC ACIDS IN WATER BY DIONEX IC/EPA 300.0M (Fatty Acid) 0

BCGEN072 pHSM4500-HBR0 pH Method-SM 4500 H&B (Agar Media) 0

BCPREP006 3010R10 Acid Digestion of Aqueous Samples and Extracts for Total Metals for Analysis by ICP Spectroscopy/Method 3010A 10

BCPREP008 TCLP_EXTR2 TCLP Extraction 2

BCPREP009 SPLP_EXTR0 SYNTHETIC PRECIPITATION LEACHING PROCEDURE (SPLP) EPA 1312 (Inorganic TTLC) 0

BCPREP011 WET_EXTR2 Wet Extraction-STLC 2

BCPREP014 SPLITR6 Splitting and Refrigerating Samples 6

BCPREP015 3050R17 Acid Digestion of Sediments, Sludges and solids for analysis by FLAA or ICP Spectroscopy/Method 3050A 17

BCPREP017 2002BLOKR6

HOT BLOCK DIGESTION OF WATERS FOR TOTAL RECOVERABLE METALS FOR ANALYSIS BY GFAA, ICP SPECTROSCOPY, OR ICP MASS SPECTROSCOPY METHOD 200.2 / 3005 6

BCPREP018 FREELIQDETR2 Free Liquid Determination (TCLP) 2

BCPREP019 3060AR1 EPA METHOD 3060A 1

BCPREP021 EPA1320R0 METHOD 1320 MULTIPLE EXTRACTION PROCEDURE 0

BCSAM002 LOGISLR15 Sample Loging - In - Prep (BarCode Scanning) 15

Metals Dept.


Analyst Int.

BCMET006 EPA200GFR8 GRAPHITE FURNACE EPA 200/7000A 8

BCMET010 HG_7470R15 MERCURY (Hg) // EPA 7470A/EPA 245.1 15

BCMET011 HG_7471R19 MERCURY (Hg) // EPA 7471 / 245.5 19

BCMET013 6010METALR19 Determination of Metals and Trace Elements in Soil, Water and Waste Waters by ICP-AES 200.7/6010 19

BCMET025 MOISTURER3 % Moisture/ % Solids/SM2540G 3

BCMET035 METSPE1R10 (Sb, As, Pb, Se) EPA 200.9/7000A PE-1 10

BCMET037 6100ELANR13 EPA METHOD 200.8 USING ELAN 6100 ICP-MS 13

BCMET038 EPA6020AR12 EPA 6020A 12

Extraction Dept.


Analyst Int.

BCDOC004 XLOGR6 Extraction Log 6

BCDOC011 XREAGLOGR2 Extractions Reagent Log 2

BCDOE004 REAGPFR4 REAGENT PURITY/FITNESS FOR USE 4

BCMIS007 XROUMAINR4 Extractions Routine Maintenance 4

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APPENDIX H

APPENDIX H


REVISED 03/15/16

PAGE H-3

Extraction Dept.


Analyst Int.

BCORG016 ZHEREV7 Zero Head Space Extraction for Volatiles/EPA 1311 (Volatile TTLC) 7

BCORG026 EPA1664R9 Method 1664- Oil and Grease 9

BCORG040 ORGCR3 ORGANIC GLASSWARE CLEANING 3

BCORG047 ExtrtPreScreeninR1 Extract Pre-screening 1

BCORG057 SCREENXPLR0 SCREENIN FOR EXPLOSIVES IN SOIL 0

BCORG065 SYRINGER1 Glass Syringe Accuracy Determination 1

BCPREP001 EX3510R15 Extractions-Waters by EPA 3510 & All Methods 15

BCPREP002 OR3550r13 Organics Extractions - EPA 3550/Ultrasonic Extractions All Methods 13

BCPREP016 SILICA-3630CR5 Silica Gel Cleanup for PAH's\EPA 3630C 5

BCPREP020 SILICA-3630MR1 Silica Gel Cleanup for EPA 3630-Modified 1

Semi-Volatiles


Analyst Int.

BCORG001 549.2R7 Epa 549.2 Diquat and Paraquat 7

BCORG002 515815R13 EPA 515.1, 615, 8150B, 8151 13

BCORG004 8140R10 EPA METHOD 8140/8141/614 10

BCORG005 TPHFELR14 LUFT TPH(FUELS)/ EPA 8015M-Diesel (FFP)(Hydraulic Oil/Motor, Mineral Oil)(DRO) 14

BCORG006 548R6 Determination of Endothal in drinking water 548 6

BCORG008 525_2R5 Determination of Organic Compounds in Drinking Water by Liquid-Solid Extraction and Capillary Column, Gas Chromatography/Mass Spectrometry. EPA 525.2 5

BCORG009 504R12 EPA 504.1 (Instrument GC-04) 12

BCORG011 8310REV14 Polynuclear Aromatic Hydrocarbons by HPLC/EPA 8310/610 14

BCORG014 508R15 Organchlorine Pesticides and PCB's by Gas Chromatography EPA 508/608/8080/8081 15

BCORG018 632R5 High Performance Liquid Chromatography for Carbamate and Urea Pesticides in Wastewater/EPA 632 5

BCORG019 8082R14 Gas Chromatography EPA 8082-PCB Water 14

BCORG020 625827R15 GC/MS for Semi-Volatiles/EPA 625/8270(PAH, Phthalates, Phenols) 15

BCORG029 8330R10 Nitroaromatics and Nitroamines by High Performance Liquid Chromatography Method 8330 (Explosives) 10

BCORG042 525_2SPER3 SOLID PHASE EXTRACTION/EPA METHOD 525.2 3

BCORG053 8270SIMR5 EPA 8270C SIM PNA/NDMA 5

BCORG055 GCMSLUFTR4 GC/MS FOR SEMI-VOLATILES/ 8015B Diesel-TPH 4

BCORG058 DETERHAA5R4 Determination of HAA5 in Drinking Water by Liquid, Liquid Microextraction-552 4

BCORG059 8015B-METHETHR3 EPA Method 8015B-Methanol and Ethanol 3

BCORG060 556R3 EPA METHOD 556 3

BCORG070 AK102_103R2 AK102 & 103: Determination of Diesel and Motor Oil Range Organics (DRO C10-C25 & RRO C25-C36) 2

BCORG071 AK103R0 AK103: Residual Range Organics 0

Volatiles


Analyst Int.

BCDOC007 VOL_GCRLR6 Volatiles GC Run Log 6

BCDOC008 VOL_STANR5 Volatiles Standard Log 5

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APPENDIX H

APPENDIX H


REVISED 03/15/16

PAGE H-4

BCDOC010 DETERTCPR1 1, 2, 3 – TCP DRINKING WATER BY P & TRAP GC/MS 1

BCORG003 TPHGASR21 LUFT TPH(GA) BTEX/8015M,8020,8021B,602(Gasoline-GRO) 21

BCORG025 5035R6 Closed System Purge & Trap (5035) (same as (5030A)) 6

BCORG045 8260PPHR6 EPA METHOD 8260 TPPH 6

BCORG049 624R14 EPA METHOD 624 14

BCORG051 8240_8260R11 EPA METHOD 8240/8260w/s 11

BCORG054 524R8 EPA METHOD 524.2 8

BCORG056 ORGVAPR2 Mercury and Oragnic Vapor Monitor Analysis 2

BCORG061 AIRTO14_15R3 AIR TESTING METHOD TO-14A AND TO-15 3

BCORG062 CANISTER2 Canister Cleaning 2

BCORG063 DYNAMICR0 DYNAMIC DILUTION 0

BCORG064 FIXGASR4 FIXED GAS ANALYSIS -Air Testing 3C/ASTM D-1946 4

BCORG066 SULF307.91R1 307.9 M Sulfur Compunds Methods 1

BCORG067 RSK175M_R3 RSK-175 -Dissolved Gas Analysis in Water for Methane/Ethane/Ethene 3

BCORG068 TO3_R1 AIR TESTING METHOD TO-3 1

BCORG069 AK101R1 AK101: Determination of Gasoline Range Organics (GRO C6-C10) 1

QC Dept


Analyst Int.

BCQC002 QCTHRMR19 QC - Thermometer Monitoring 19

BCQC005 QCFRDGR16 QC - Refrigerator Monitoring 16

BCQC007 QCOVENR13 QC - Oven Monitoring 13

BCQC008 QCBLNCR17 QC - Balance Monitoring 17

BCQC011 QCDILMONR5 QC-DILUTER MONITORING 5

BCQC013 QCEPPENDORFR0 QC - EPPENDORF PIPETTE CALIBRATION 0

Client Service


Analyst Int.

BCDOC002 COCR4 Chain of Custody 4

BCMIS009 SHIPPINGR9 Shipping 9

BCREC001 RECEPTR6 RECEPTIONIST 6

BCSAM005 LOGISRV21 Sample Receiving 21

BCSER001 BOTPRER14 Bottle Prep (bottleware) 14

BCSER006 COCTRACKR3 COC & Tracking 3

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APPENDIX H

APPENDIX H


REVISED 03/15/16

PAGE H-5

Employee SOP Acknowledgement and Agreement Form

Personnel Training Record

Of

Standard Operation Procedure (SOPs)

This is to acknowledge and agree that I have read and understand the latest version of Standard

Operation Procedure(s) applicable to my job responsibilities/duties (See appendix H SOP

Table).

_______________________________ ______________________

Employee Name (Print) Date

____________________________

Employee Signature

_______________________________ ______________________

Supervisor Name (Print) Date

____________________________

Supervisor Signature

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SECTION VI REVISION 7 EFFECTIVE DATE 01/08/16 Page VI-1

Quality

Assurance

Protocols

Manual


4100 Atlas Court

Bakersfield, CA 93308

Carolyn Jackson Sara Guron

President Quality Assurance Officer

(661) 327-4912 Ext. 213 (661) 327-4912 Ext. 288

Effective Date: 01/08/2016 .

UnControlled Copy:

Issued to:

Date:

Location:

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QUALITY ASSURANCE PROTOCOLS MANUAL

TABLE OF CONTENTS

QUALITY ASSURANCE PROTOCOL MANUAL OF


Approved by Signed by

Date

CEO/President:

Technical Director:

Quality Assurance

Officer:

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TABLE OF CONTENTS

Table of Contents

1 Introduction ...................................................................................................................... I-1 thru I-4

2 Definition of Terms ....................................................................................................... II-1 thru II-6

3 Training ....................................................................................................................... III-1 thru III-7

3.1 Overview

3.2 Orientation

3.3 Process

3.4 Internal Training Program

3.5 External Training Program

3.6 Safety

3.7 Performance Evaluations

3.8 Employment

4 Laboratory Information Management System............................................................ IV-1 thru IV-5

4.1 Introduction

4.2 Access

4.3 General Rules

4.4 Crashes

5 Creation, Modification, Distribution and Maintenance of

Laboratory Controlled Documents ................................................................................ V-1 thru V-6

5.1 Scope and Application

5.2 Creation

5.3 Modification

5.4 Distribution

5.5 Management

6 Sample Procedure ...................................................................................................... VI-1 thru VI-5

6.1 Overview

6.2 Sample Containers

6.3 Sample Storage Before Analysis

6.4 Preservation Techniques

6.5 Holding Times

6.6 Analysis Reference Chart

7 Custody .................................................................................................................... VII-1 thru VII-9


7.2 Summary

7.3 Potential Problems

7.4 Custody

7.5 Secured Facility

7.6 Alarm System

7.7 Visitors

7.8 Sample Custody Procedures

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TABLE OF CONTENTS

8.0 Standard and Reagent Handling ............................................................................ VIII-1 thru VIII-4

8.1 Introduction

8.2 Qualification

8.3 Receiving

8.4 Preparation

8.5 Expiration Date

8.6 Preservation and Storage

8.7 Documentation

8.8 Disposal

9.0 Glassware ................................................................................................................... IX-1 thru IX-7

9.1 Overview

9.2 Types

9.3 Glassware Colors

9.4 Cleaning

9.5 Organics Testing

9.6 High Concentration Samples

9.7 Metals

9.8 Wet Chemistry

9.9 How to Measure Containment

9.10 Delivery and Containment Glassware Types

10.0 Measuring ..................................................................................................................... X-1 thru X-2

10.1 Weight

10.2 Accuracy

10.3 Safety

10.4 Containment

10.5 Cross-Contamination

10.6 Capacity

10.7 Alignment

10.8 Appropriateness

10.9 Liquids Measuring

10.10 Important Safety Practices

11.0 Microliter Pipette Calibration .................................................................................... XI-1 thru XI-3


11.2 Summary of Method

11.3 Apparatus and Materials

11.4 Procedure

11.5 Compliance Limits

11.6 Documentation

11.7 References

12.0 MDL/PQL Determinations ...................................................................................... XII-1 thru XII-8


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TABLE OF CONTENTS


12.3 Required Apparatus and Materials

12.4 Reagents and Standards

12.5 General MDL/PQL Procedure

12.6 Procedures by Test

12.7 Detection Limits for Soil Matrix

12.8 Documentation, Approval and Reporting

12.9 References

13.0 Reporting ............................................................................................................. XIII-1 thru XIII-10

13.1 Reporting Procedures for Qualified Data

13.2 Rounding Rules for Reporting Data

13.3 Quality Control Parameter Evaluation

13.4 Low Level Reporting

13.5 Manual Integration

13.6 Manual Integration Labeling

14.0 Audit Handling Procedures .................................................................................. XIV-1 thru XIV-3




14.4 Reagents and Standard Solutions

14.5 Solution Preparation

14.6 Working Standards

14.7 Sample Collection, Preservation and Handling

14.8 Procedure

14.9 Forms

14.10 Safety

15.0 Technical Reviews .................................................................................................. XV-1 thru XV-2



15.3 Materials

15.4 Procedure

15.5 Quality Control

16.0 Control Charting .................................................................................................. XVI-1 thru XVI-2

16.1 Introduction

16.2 Monitoring of LCSW

16.3 Development of Control Charts

16.4 Maintenance of Control Charts

16.5 Calculation Controls

17.0 Corrective Action/Quality Improvement ........................................................... XVII-1 thru XVII-7

17.1 Introduction

17.2 When to Initiate

17.3 Determining the Root Cause

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TABLE OF CONTENTS

17.4 Constructing a Basic Cause-and-Effect Diagram

18.0 Preventive Maintenance .................................................................................. XVIII-1 thru XVIII-3

18.1 Overview

18.2 Part Maintenance

18.3 Preventive Maintenance Schedules

18.4 Preventive Maintenance Logs

18.5 Service Contracts

18.6 Service Calls

18.7 Tagging Out

18.8 Verification of Working Status

19.0 Procurement ......................................................................................................... XIX-1 thru XIX-3

19.1 Overview

19.2 Responsibilities

19.3 Requisition Forms

19.4 Supply Receiving

19.5 Standard Receiving

19.6 Reagent Receiving

19.7 Receiving Products Which Can be Calibrated

20.0 Method Modifications ........................................................................................... XX-1 thru XX-12

20.1 Introduction

20.2 Modification Process

21.0 Security ................................................................................................................ XXI-1 thru XXI-3

21.1 Security System

21.2 How to Obtain an Access Code

21.3 How to Obtain a Password

21.4 How to Activate/Deactivate the Security System

21.5 How to Use the Intercom

21.6 What to do When Working Odd Hours

21.7 How to Contact Kern Securities

21.8 How to Answer Phone Calls

21.9 Responsibility

21.10 Keys

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INTRODUCTION

SECTION I REVISION 3 EFFECTIVE DATE 01/08/16 Page I-1

The intention of the QA Protocols Manual (QAPM) is to act as a working laboratory protocol/process

reference. This reference contains information essential to control various laboratory processes and to

communicate quality policy to the bench level. Designed as a policy communication tool, the QAPM,

administered by the QA Officer, is an integral part of the QA system.

The QAPM can be considered an organized collection of SOPs, which are needed by all employees to

conduct those common tasks, which are not addressed in detail in individual analytical SOPs. Because

of the difficulty in maintaining the system and at the same time increase communication and thus

promote improved quality. BCL employees should refer to this guide prior to contacting their

department supervisor or QA Officer when questions arise regarding quality, policy or procedure.

This manual is maintained under a controlled status, thus only one copy will be distributed to each

employee. All updates will be processed and distributed by the QA/QC department. Please refer to

Section V for more details on controlled documentation. BCL employees should keep this manual on

site to refer and use at will.

The quality program consists of five essential components:

1) Prevention

2) Assessment

3) Validation

4) Corrective Action

5) Improvement.

The QAPM falls into the prevention category since it was designed to communicate policy, provide

essential information, and promote good laboratory practices. If used properly, the QAPM will reduce

the chance for error and promote better understanding. Section I of the QAPP discusses the components

of the quality system in more detail.

The QA Officer is responsible for the maintenance of the QAPM. Review of this plan should take place

each year. All revisions and additions will be reviewed and approved prior to distribution. Once

approved, affected section revision number(s) are sequentially incremented and the approval date is

updated accordingly. All revised sections are distributed to laboratory personnel. Acknowledgement of

receipt signatures is required as a record of transfer of information.

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INTRODUCTION


Figure 1.1 illustrates how the QAPM fits into the QA document scheme.

QAPP

QAPM

SOPs

Polic

y

Proc

edur

e

Less detailed

Detailed

Figure 1.1

Establishes Quality

Policy and Goals.

Describes the quality

system.

Practical analyst working

manual for those

procedures other than

analytical methods

which are critical to the

order and control of the

quality system.

Written procedures

which describes

practices for a given

procedure or activity.

As noted above, SOPs should supply the most detailed information in regards to specific tasks, thus

SOPs are referenced by this manual and the QAPP. SOPs are distributed on an as needed basis to the

supervisor/analyst that the SOP directly affects. Access to SOPs is limited and specific rules will apply

(see section V).

The QAPP, on the other hand, is less detailed but provides the standards by which our quality system

must operate. Quality policy, set through goals and objectives, is stated and mandated to comply with

regulatory, client, project and internal requirements.

Objectives: To provide QA/QC guidelines to:

1) assure the data produced is of known quality

2) ensure our organization is capable of providing results which are of value to our customers

3) ensure the system can consistently perform under adverse conditions

4) Comply with quality goals and objectives set forth in government and industry standards.

Policy Statement: BC Laboratories, Inc. is an organization committed to providing data that is

technically valid and in accordance with professional standards and government regulations. The

management and staff of BC Laboratories, Inc. are committed to use all available resources to supply

accurate, precise, timely and fully documented results which should withstand legal challenge. BCL’s

goal is to provide analytical results and services which are of value to our customers.

Employees are encouraged to access the QAPP by contacting their department supervisor or the QA

Officer.

Please note that if conflicts exist among or between this manual and other documents, employees are

urged to contact their department supervisor and/or the QA Officer to resolve the differences.

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ACRONYMS


AA Atomic Absorption LOD Limit of Detection

AAII Auto Analyzer LOQ Limit of Quantitation

BCL BC Laboratories, Inc. MB Method Blank

BFB Bromofluorobenzene MCL Maximum Contaminant Level

CCB Continuing Calibration Blank MDL Method Detection Limit

CCC Calibration Check Compound MS Matrix Spike

CCV Continuing Calibration Verification MSD Matrix Spike Duplicate

CLP Contract Laboratory Program PQL Practical Quantitation Limit

COC Chain of Custody QAPP Quality Assurance Project Plan

CRDL Contract Required Detection Limit QAPM Quality Assurance Protocols Manual

CRMDL Contract Reporting Method Detection

Limit

QAPP Quality Assurance Program Plan

CRPQL Contract Reporting Practical

Quantitation Limit

RFP Request for Proposal

CV Cold Vapor RFQ Request for Quotation

DFTPP Decafluorotriphenylphosphine RL Reporting Limit

DLR Detection Limit Reporting RLS Reporting Limit Standard

DQO Data Quality Objective RPD Relative Percent Difference

Dup Duplicate RSD Relative Standard Deviation

EB Equipment Blank SIF System Improvement Form

GC Gas Chromatography/Chromatograph SM Standard Methods

GC/MS Gas Chromatography/Mass

Spectrometry

SMC System Monitoring Compound

GFAA Graphite Furnace Atomic Absorption SOP Standard Operating Procedure

GHAA Gaseous Hydride Atomic Absorption SOW Statement of Work

IB Instrument Blank SPCC System Performance Check Compound

IC Ion Chromatography/Chromatograph SRM Standard Reference Material

ICB Initial Calibration Blank STLC Soluble Threshold Limit Concentration

ICP Inductively Coupled Plasma TB Trip/Travel Blank

ICP/MS Inductively Coupled Plasma/Mass

Spectrometry

TCLP Toxicity Characteristic Leaching

Procedure

ICV Initial Calibration Verification TOX Total Organic Halides

IDC Initial Demonstration of Competency TTLC Total Threshold Limit Concentration

IDL Instrument Detection Limit UCL Upper Control Limit

IS Internal Standard WET Waste Extraction Test

LCL Lower Control Limit WPS Word Processing Specialist

LCS Laboratory Control Sample ZHE Zero Headspace Extraction

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CONVERSION TABLES


Temperature Given In °C °K °F

°C C C + 273.15 1.8C + 32

°K K – 273.15 K 1.8K + 459.4

°F 0.556F – 17.8 0.556F + 255.3 F

Factor Prefix Symbol

10-12 Pico p

10-9 Nano n

10-6 Micro µ

10-3 Milli m

103 Kilo k

To Convert Into Multiply

µg/L (ppb) mg/l (ppm) 0.001

mg/L (ppm) µg/L (ppb) 1000

µg/kg (ppb) mg/kg (ppm) 0.001

mg/kg (ppm) µg/kg (ppb) 1000

µg/ml (ppm) mg/l (ppm) 1

µg/g (ppm) mg/kg (ppm) 1

Note: Section I was review on 01/08/16 (No changes were made)

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DEFINITION OF TERMS

SECTION II REVISION 3 EFFECTIVE DATE 01/08/16 Page II-1

Aliquot-a measured portion of a sample taken for analysis

Analytical Sample-any solution or media introduced into an instrument or analyzed on an apparatus

excluding instrument calibration, initial calibration verification, initial calibration blank,

continuing calibration verification, and continuing calibration blank.

Background Correction-a technique to compensate for variable background contribution to the

instrument signal in the determination of trace elements

Batch-a set of environmental samples and QC samples of similar matrix which are processed: 1) as a

unit, 2) within a prescribed 24 hour time span, 3) with the same method manipulations and 4)

with the same lots of reagents and standards. Batch size is method dependent with a maximum

number of field samples per batch set at 20. QC samples, such as method blanks, laboratory

control samples, duplicates, and matrix spikes, are not counted when figuring batch size.

Calibration-the establishment of an analytical curve based on the absorbance, emission, intensity, or

other measured characteristic of known standards. The calibration standards must be prepared

using the same type of acid or concentration of acids as used in the sample preparation.

Calibration Factor-a factor derived by taking the response of an analyte or set of analytes in a standard

divided by the concentration of the standard. Used in calculation models not using least squares

techniques.

Case Narrative-portion of the data package which includes project codes, sample and field information,

and descriptive documentation of any problems encountered in processing the sample, along with

problem resolution or qualifying narratives.

Continuing Calibration Blank-(CCB) an instrument blank analyzed after each continuing calibration

verification. Used to monitor and verify the instrument baseline.

Continuing Calibration Verification-(CCV) a mid-point standard prepared from a separate source than

that of the standard curve. Used to verify accuracy of the standard curve. (4)

Control Limits-control limits may be specified in a reference method (either as mandatory or guidance

limits), or may be developed by the laboratory using internal performance data. Control limits

represent acceptance criteria for determining whether an analytical system is in control. Also

described as a range within a specific measurement, results must fail to be compliant. Control

limits may be mandatory, requiring corrective action if exceeded, or advisory, requiring that

noncompliant data be flagged.

Correlation Coefficient-a number (r) which indicates the degree of dependence between two variables.

The more dependent they are, the closer the value to one. Determined on the basis of the least

squares line.

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DEFINITION OF TERMS


Data Quality Objective-(DQO) project specific requirements which supercede internal quality goals.

Detection Limit Standard-a standard analyzed at the practical quantitation level. Used to verify daily

instrument low level performance.

Dilution-having combined a diluent and a concentrated source to produce less concentrated solution.

Dilution Factor-numerical representation of a dilution. If a dilution is not made, the dilution factor is 1.

The number which you multiply a diluted sample result to derive the final result.

Dissolved Metals-analyte elements which have not been digested prior to analysis and which will pass

through a 0.45 µm filter.

Duplicate-a sample which is one of two replicates. Used to measure sample precision. Types of

duplicates include field, matrix, and matrix spike duplicates. Laboratory duplicates are prepared in

the laboratory as split samples, and carried through the entire measurement process as independent

samples.

Equipment/Rinsate Blank-analyte-free water which is poured over or into field sampling equipment.

Used to monitor equipment cleanliness and the adequacy of the decontamination process. (4)

Field Blank-aliquot of analyte-free water or solvent brought to the field in a sealed container. Opened

in the field to monitor conditions at the time of sampling. (4)

Field Sample-a portion of material received to be analyzed.

Holding Time-the storage time allowed between sample collection and sample analysis when the

designated preservation and storage techniques are employed.

IDL-(Instrument Detection Limit) the smallest signal above background noise that an instrument can

reliably detect. Determined by multiplying the standard deviation of replicate reagent blanks by 3.

The calculation provides for a 99% confidence level that the IDL is not zero (if blank readings

average zero).

Independent Check Standard-a standard solution that is composed of analytes from a different source

that those used in the standards for the initial calibration.

Initial Calibration Blank-(ICB) an instrument blank analyzed after an initial calibration verification.

Used to monitor and verify the instrument baseline.

Initial Calibration Verification-(ICV) a mid-point standard prepared from a separate source than that

of the standard curve. Used to verify accuracy of the standard curve. (4)

Injection-introduction of a sample into the instrument system.

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DEFINITION OF TERMS


Instrument Calibration-analysis of analytical standards for a series of different specified

concentrations; used to define the quantitative response, linearity, and the calibration range of the

instrument to target analytes.

Interference Check Sample-a solution containing both interfering and analyte elements of known

concentration that can be used to verify background and interelement correction factors.

Interference Check Standards-standards used to monitor spectral interferences for inductively coupled

argon plasma analysis.

Interferents-substances which affect the analysis for the element of interest.

Internal Standards-compounds added at a known concentration to all GC/MS samples.

Instrument Spike Level-the concentration of the spike addition without consideration to applicable

sample weight ratio, sample volume ratios, or dilution schemes.

IQL- (Instrument Quantitation Limit) a level set lower than accepted analyte PQL’s which still meets

PQL derivation standards. Used as an internal compliance tool for a typical low level reporting.

Laboratory Control Sample-(LCS) a beginning matrix (deionized water, baked sand), spiked with the

same spiking solution used for matrix spikes, is used to validate the accuracy of the analytical

system under ideal matrix conditions. This QC parameter, known as the Laboratory Control

Sample, is a required QC sample which is prepared and analyzed with each batch at a frequency

set per method. The LCS contains the same analytes at the same concentrations as spiked in

matrix spikes. LCS validity is assessed through percent recoveries compared against statistically

based control limits unless general criteria has been defaulted. If any LCS analytes are outside

acceptable limits, associated sample data should be considered estimated, thus the entire batch

should be reprepared and reanalyzed unless it can be proven that effects can solely be attributed

to the LCS and no other QC indicators show possible quality compromise.

Laboratory Performance Check Sample-a solution described in certain drinking water methods which

is used to verify acceptable chromatography.

Linear Range-the concentration range over which the analytical curve remains linear.

Matrix-the predominant material of which the sample to be analyzed is composed. A sample matrix is

either aqueous or non-aqueous as described in the LIMS. Matrix identifying should be more

detailed at the preparation and/or the analytical levels. Detailed descriptions of sample matrices

should be documented in preparation logs.

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DEFINITION OF TERMS


Matrix Spike/Matrix Spike Duplicate-(MS/MSD) samples with an addition of a predetermined

quantity of stock solution(s) containing certain analytes. The addition of stock takes place before

any preparation steps to verify either matrix effects and/or preparation efficiency.

MCL-(Maximum Contaminant Level) the maximum permissible level of a contaminant in water which

it delivered to any user of a public water system. (2)

MDL-(Method Detection Limit) the lowest concentration level that can be determined to be statistically

different from the blank with consideration placed on routine sample preparation. The MDL is

determined by multiplying the standard deviation of prepared replicate samples spiked at 3 to 5

times the estimated detection limit by a corresponding students’t value. This value is at the 99%

confidence level with n-1 degrees of freedom. See the “Table of Students’t Values at the 99%

Confidence Level” in Appendix B 40 CFR Part 136. (1)

Method of Standard Addition-(MSA) the addition of increments of standard solution (spikes) to

sample aliquots of the same size. Measurements are made on the original and after each

addition. The slope, x-intercept, and y-intercept are determined by least squares analysis.

Modifier-salts used in metals testing which lesson the effects of chemical interferences, viscosity, and

surface tension.

M/Z-mass to charge ratio.

Percent Difference-the percent difference indicates both the direction and the magnitude of the

comparison of two values, one of which is used as a reference.

Percent Drift-used to describe GC/MS calibration status.

Percent Moisture-an approximation of the amount of water in a soil/sediment sample made by drying

an aliquot of the sample.

Performance Evaluation Sample-a sample from an outside source which is used to verify the control

of an analytical method.

Post Spike/Post Spike Duplicate-(PS/PSD) samples, digests or extracts which have been spiked after

the preparation process. Used to evaluate matrix interferences caused from the digest or extract

matrix. (3)

PQL-(Practical Quantitation Limit) the level above which quantitative results may be obtained with a

specific degree of confidence. The value for the PQL 10r (r is the standard deviation obtained

from the MDL study) is recommended, which corresponds to an uncertainty of + 30% in the

measured value.

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DEFINITION OF TERMS


Preparation Blank (PB)/Method Blank (MB)-an artificial sample designed to monitor the introduction

of artifacts into the process. Reagent water is used as the preparation blank matrix. (3)

Relative Percent Difference-a term used to describe precision.

Relative Response Factor-a measure of the relative mass spectral response of an analyte compared to

its internal standard

Relative Standard Deviation-statistic used to describe the variation among calibration curve standards.

Replicate-a sample prepared by dividing a sample into two or more separate aliquots. (4)

Reporting Limit-the analyte concentration below which a laboratory will not report the analyte as

having been detected. A laboratory’s reporting limit for any given analyte in a specific matrix must

be greater than or equal to the experimentally determined MDL for the same matrix.

Resolution-the separation between peaks on a chromatogram or strip chart. Calculated by dividing the

depth of the valley between peaks by the peak height of the smaller peak being resolved, multiplied

by 100.

Spike Level-concentration of the spike addition. Sample weights and dilution schemes are involved in

the calculation of the spike level.

Standard Curve-curve which plots concentrations of known analyte standard versus the instrument

response to the analyte. (4)

Standard Operating Procedure-SOP is an approved, controlled document which describes practices

for a given procedure or activity, in sufficient detail that a qualified individual could use the SOP to

conduct the procedure.

Stock Solution-a solution which can be diluted to derive standards or reagents.

Surrogate-organic compounds similar to analytes of interest in chemical composition, extraction, and

chromatography, but not normally found in environmental samples. These compounds are

spiked into each sample of a prepared batch and are used to validate accuracy on a sample

specific level. (4)

System Monitoring Compounds-compounds added to every blank, sample, matrix spike, matrix spike

duplicate, and standard for GC/MS analyses. These compounds are brominated or deuterated

compounds not expected to be detected in environmental media.

Target Analytes-compounds or elements which are project of method specified.

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DEFINITION OF TERMS


Temperature Blank-a deionized water filled receptacle that accompanies samples in ice chests which is

used to determine temperature upon receipt.

Tentatively Identified Compounds-compounds detected in samples that are not target compounds,

calibrated analytes, responsive analytes, internal standards, system monitoring compounds, or

surrogate.

Total Metals-metal measurement (dissolved and suspended) where the sample is not filtered and

digested prior to analysis. Metals are also considered total if the turbidity of the sample without

filtration is < 1 NTU.

Travel/Trip Blank-a sealed aliquot of analyte-free water which is transported in with field samples.

Used to identify the presence of volatile compound contamination attributable to transfer across a

sample container septum during shipping and storage of samples. (4)

Turnaround Time-the elapsed time expressed in days from the date of receipt of the sample by a

laboratory representative until the date of reporting. The form of the report and the method of

submission of the results are stipulated by the client. Turnaround time can also be expressed as a

time limit by which all results are due.

Twelve Hour Time Period-for GC/MS: the moment of a specific injection of BFB or DFTPP analysis

until twelve hours have elapsed according to the system clock. For GC: the twelve hour time

period in the analytical sequence begins at the moment of the injection of a specified initial or

calibration verification until the end of the twelve hour time period.

(1) 40 CFR Part 136 Appendix B

(2) 40 CFR Part 141

(3) CLP SOW

(4) SW-846, September 1994

(5) Navy Installation Restoration Laboratory Quality Assurance Guide

Note: Section II was reviewed on 01/08/16 (No Changes were made)

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TRAINING

SECTION III REVISION 7 EFFECTIVE DATE 01/08/16 Page III- 1

3.1 Overview

One of the key elements of a sound quality system is training. Training allows for effective communication

of policy and procedure and provided a mechanism to increase the knowledge base of the organization.

Training is a continuous process with distinct programs and objectives:

3.1.1 Orientation

Safety

“Right to Know”

Evacuation Process

Fire Prevention

Job Specific Safety

Laboratory Employee Policies

3.1.2 On the Job Training

Job specific duties and responsibilities

Job specific quality control

3.1.3 Internal Training Modules

Laboratory Process Training

Good Laboratory Practices

Continuous Training


General Procedure Training

3.1.4 External Training

Advanced instrument/method/process training

Industry standards

Personal advancement

3.1.5 Safety Meetings

Lab Safety Policy

Safety Awareness

Safe Practices

Each of the aforementioned components of the training program are described in detail in the following

sections.

3.2 Orientation

A safety orientation must be performed for all new permanent employees and temporary employees prior to

job specific duties. When job responsibilities that cross department lines change, department supervisors

must conduct department specific safety orientations. Respective department supervisors are responsible for

conducting orientations for their department employees. The Health and Safety Coordinator can conduct

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TRAINING


orientations in lieu of the department supervisor. The orientation consists of a structured interview, a film

viewing, a laboratory tour and a question/answer session.

3.3 Process

3.3.1 Film Viewing

The film “Laboratory Right to Know” should be viewed prior to the interview. A VCR is available in the

lunchroom. If applicable, the trainee should also view one or more of the following safety films:

Laboratory Spills and Waste

Laboratory Housekeeping and Personal Hygiene

Working with Asbestos

3.3.2 Interview

The Health and Safety Coordinator obtains an orientation kit from the Safety department. The kit includes

the following:

QA Protocols Manual

Employee Safety Manual

Emergency Evacuation Plan

Fire Prevention Plan

Respirator Program Plan

Waste Disposal SOP

Worker’s Compensation Pamphlet

Laboratory Map

MSDS Example

Lab Coat

Safety Glasses

The interview, conducted in an area of limited disruptions, will follow topics found on the Orientation

checklist. Each subject should be discussed thoroughly. The trainee acknowledges discussion of each topic

by initialing the proper space of the orientation form. If certain topics were not discussed or if a full

understanding of the subject is not obtainable or if additional time is required to fulfill the subject matter, the

trainee should not initial the form until he/she is fully confident to do so. All components of the orientation

kit should be distributed during the interview. A copy of the acknowledgement in the back of the

employee’s policy should be signed by the new employee.

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3.3.3 Laboratory Tour

Once the interview is completed, the Health and Safety Coordinator should conduct a tour of the laboratory

which focuses on laboratory safety features. Fire extinguisher and safety/eyewash shower locations should

be pointed out as well as all exits.

3.3.4 Question and Answer

A question and answer session will follow the tour. Once completed, the Health and Safety Coordinator

should place the orientation checklist and laboratory policy in the employee’s file.

3.3.5 On the Job Training

A controlled copy of all pertinent SOPs must be requisitioned from the QA Department then submitted to

the trainee. The trainee should read all pertinent SOPs prior to hands on training. The department

supervisor will conduct on-the-job training or will designate this responsibility to a suitable analyst or

technician. The trainer should demonstrate all aspects of technical and physical skills needed to perform job

specific tasks at or above current efficiency and accuracy levels. When the trainer and/or department

supervisor feels confident that the new employee can conduct job duties competently, the department

supervisor will schedule an initial demonstration of competency, if applicable.

3.3.6 Initial Demonstration of Competency (IDC)

Employees are to complete method specific IDCs before they are allowed to report results solo. IDC

requirements should include all duties and responsibilities associated with specific jobs or methods. IDC

tasks can include:

Preparation of standards

Preparation of reagents

LCSW preparation

LCSW analysis

MDL studies

Data Reduction

Documentation

An IDC form should be completed to acknowledge the trainee is method/task competent. When the form is

completed and approved, the analyst is designated fit for duty. Original IDC forms are placed in employee

IDC/ADC file in QA Department.

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3.4 Internal Training Program

Basic skills and training knowledge are conducted through in-house programs and/or subcontract programs.

The in-house program includes an initial orientation, on the job training module program, which covers

various aspects of laboratory operations.

In-House Training Modules

MODULE TOPICS JOB TITLES

(attendance is required)

TRAINER

A-1 Orientation for New Hires

Basic Laboratory Operations

Math and Science Basics

Introduction to Quality Control

Introduction to Laboratory Analyses

Physical Properties

New Hires Steve Bennett

Glassware

Types

Using Burettes and Pipettes

Calibration

Safety, Cleaning, and Storage

Weighing and Measuring

Mass Measurements

Volumetric Measurements

Linear Measurement

Temperature Measurements


Analysis Terms

Procedure

Data Generation

B Laboratory Math I

Units of Measurement

Significant Figures and Rounding

Percents

Exponential Numbers

Analyst/Prep Technician

Richard Penner

C-1 Quality Assurance, Quality Control

Concepts

Parameters

Basic Tasks

Measurement and Assessment

Documentation and Audits

Corrective Logic

All

Sara Guron

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TRAINING


MODULE TOPICS JOB TITLES

(attendance is required)

TRAINER

C-2

Data Management

Recordkeeping Procedures

Responsibilities

Storage

All Sara Guron

C-3

Quality Improvement-Corrective

Action


When to Initiate Corrective Procedures

Procedures

Identifying the Error

Implementing Corrective Action

Demonstrating Corrective Action

Closure

Documentation

All Sara Guron

D Ethics

Industry Standards

Case Studies


All

Sara Guron

E Sexual Harassment All Steve Bennett

F LIMS I

Logging on through Passwords

Security

Features

Policy

All Keith Vogel

Training module attendance is job dependent. Each job description has associated minimum training

requirements. Trainees must pass training examinations before acknowledgement of successful completion

of pertinent training modules.

Module training will be appropriately scheduled to accommodate both working shifts. Effort will be put

forth to provide a flexible and workable schedule to prevent any significant disruption of work flow.

Individual module presentations should be posted on the memo board near the time clock at least one week

prior to each training session. Employees are required to sign the attendance ledger on the posted schedule.

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JOB TITLES

1. President

2. Technical Director

3. Director of Human Resources

4. Health + Safety Officer/Radiological Safety

Officer

5. Service Technician

6. Client/Field Services Manager

7. Project Manager

8. Client Services Representative

9. Field Services Representative

10. Courier

11. Lab Technician I (Non Production Data)

12. Sample Custodian

13. Billing Clerk

14. Receptionist

15. Accounts Payable Clerk

16. Accounts Receivables Clerk

17. Inorganics Manager

18. Supervisor (Production Inorganics)

19. Lab Technician I (Inorganics)

20. Lab Technician I (Organics)

21. Lab Technician II (Inorganics)

22. Lab Technician II (Organics)

23. Analyst I (Inorganics)

24. Analyst I (Organics)

25. Analyst II (Inorganics)

26. Analyst II (Organics)

27. LIMS Manager

29. LIMS Programmer

30. LIMS Specialist

31. Volatile Organic Manager

32. Quality Assurance Officer

33 Quality Assurance Specialist

34. Sales & Marketing Director

35. Salesperson

36. Laboratory Coordinator

37. Semi-Volatile Organic Supervisor

38. Semi-Volatile Extraction Supervisor

39. Word Processor Specialist

3.5 External Training Program

External training is conducted through manufacturer’s instrument training programs, various independent

seminars, California State University Bakersfield (CSUB), and Bakersfield College. External training is

addressed under the Educational Assistance section of the Employee Policy Manual.

Each supervisor is encouraged to attend at least one outside services seminar or training session per year,

which would enhance his/her job performance or knowledge. In order to attend, supervisors must be granted

an approval by the President.

3.6 Safety

Safety training begins with the new employee orientation. Safety meetings are held to provide for

continuing training regarding safety related updates and to ensure safe working conditions by providing

reiterated safety practice and policy information. All employees, unless absence is approved by the Health

and Safety Coordinator are required to attend safety meetings. Additional information is listed in the Safety

Module Training SOP.

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3.7 Performance Evaluations

To monitor employee progress and efficiency, department supervisors evaluate each specialist within three

months of job duties initiated and annually thereafter. These screenings are conducted on a one-on-one

basis with supervisors rating employees’ performance on various job-related subjects. During these

interviews, goals are set to provide for deficiencies or to help employees further their training and skills.

Review of pertinent SOPS should also be covered during the annual review. Evaluation forms used are

exclusive for each laboratory department. Completed performance evaluations are maintained in employee

files.

3.8 Employment

BC Laboratories, Inc. offers a comprehensive benefit package for each employee to ensure a productive and

efficient work force. All agreements and particulars are addressed in the BC Laboratories, Inc. Employee

Policy Manual.

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LABORATORY INFORMATION MANAGEMENT SYSTEM (LIMS)

SECTION IV REVISION 4 EFFECTIVE DATE 01/08/16 Page IV-

1

4.1 Introduction

The Laboratory Information Management System (LIMS) is a 100-user Novell/Advanced Revelation

computer network with approximately 90 workstations. The laboratory has an equal number of computers

as stand-alone systems such as instrument computers, notebooks, accounts payable and accounts receivable.

The system is developed and maintained by the LIMS Manager and his assistants. The LIMS is a tool by

which laboratory information is processed and reported to our clients. It also serves as an internal and

external communication tool. Most computers utilized in the lab are linked to the LIMS, however there are

some instrument computers which are not directly connected. All general rule specifics outlined in this

section should apply to all computers.

4.2 Access

4.2.1 Password

In order to gain access to the network, one needs to have a password. The LIMS Manager is responsible for

the password maintenance system. New employees must contact the LIMS Manager personally to set up

passwords, which should be six (6) characters or more. The LIMS Manager also needs employee initials.

Three initials are required. If an employee does not have middle initial, use “n” as the middle initial.

Passwords should be set up as soon as possible.

New User Account

User Name:

User Initials (Must be 3 characters)

Password: (Must be 6 or more characters)

Department:

Computer ID: (See label affixed to computer)

4.2.2 LIMS Access Time

LIMS access time for new employees is Monday through Friday, 0730 – 1800. If access time is not

conductive to employee work activities, the employee should contact their department supervisor to approve

modified access time. The department supervisor will contact the LIMS Manager to initiate the change.

4.2.3 Logging On/Off

4.2.3.1 WINDOWS 95 USERS

4.3.1.1 Log-in

a. When prompted for password by Novell, enter your account password.

b. When Windows asks for a password, enter password provided by the

LIMS manager.

c. To access the LIMS, click the icon that contains the word

“ELEMENT”.

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2

d. The LIMS will ask for a password; enter your account password again.

e. Your supervisor will provide training to use the system.

f. When done, select exit from the main menu.

4.3.1.2 Log-off

a. Make sure you have properly exited from the LIMS software.

b. Click Start, Shut Down, Yes.

c. Leave computer on.

d. Turn monitor off.

4.2.3.2 WINDOWS 3.xx USERS

4.2.3.2.1 Log-in

a. When prompted for name enter, your initials followed by a

space then the word “windows”.

b. When prompted for a password, enter your account

password.

c. You will be logged in, and windows will start.

d. When windows asks for a password, enter password

provided by the LIMS manager.

e. To access the LIMS, click the icon that contains the word

“ELEMENT”.

f. The LIMS will ask for a password; enter your account

password again.

g. Your supervisor will provide training to use the system.

h. When done, select exit from the main menu.

4.2.3.2.2 Log-off

a. Make sure you have properly exited from the LIMS

software.

b. Press alt-F4, click Yes. You will now exit windows.

c. Type “Logout”.

d. Leave computer on.

e. Turn monitor off.

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3

4.2.3.3 DOS USERS

4.2.3.3.1 Log-in

a. When prompted for name, enter your initials followed by a

space, then the word “lims”.

b. When prompted for a password, enter your account

password.

c. You will be logged in, and the LIMS software will start.

d. The LIMS will ask for a password; enter your account

password again.

e. Your supervisor will provide training to use the system.

f. When done, select exit from the main menu.

4.2.3.3.2 Log-off

a. Make sure you have properly exited from the LIMS

software.

b. Type “Logout”.

c. Leave computer on.

d. Turn monitor off.

4.3 General Rules

4.3.1 Foreign software may not be initialized without LIMS Manager Approval.

4.3.2 No foreign floppy disks may be placed into use unless the LIMS Manager has granted

approval. All electronic files (including word processing and spreadsheets) brought to the

LIMS must be scanned for viruses prior to usage on the LIMS.

4.3.3 Employees cannot change any computer stations’ configuration in any way unless the LIMS

Manager has granted approval.

4.3.4 Non-work related internet use must be discussed with the LIMS Manager prior to accessing

the internet.

4.3.5 Non-work related computer use cannot take precedence to work related activities.

4.3.6 Passwords are of exclusive use. Passwords may not be revealed to anyone.

4.3.7 Any hardware or software problems must be reported to the LIMS Department as soon as

possible. Use the form labeled “Crashes” (see page IV-5).

4.3.8 LIMS use is exclusive to BCL employees.

4.3.9 There is no unauthorized entrance allowed in the computer room.

4.3.10 Network non-work related printing is not allowed unless permission is granted by the LIMS

Manager.

4.3.11 When you must leave your computer for more than 15 minutes, your must log off the system

prior to leaving.

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4

4.3.12 If possible, all documents (WordPerfect, Excel, Visio) must be saved on the File Server (not

on local C: or D: hard drives). If you are in doubt, please contact a staff member of the LIMS

department.

4.4 Crashes

It is imperative that you communicate that your workstation is not in working order to the LIMS staff.

Communication is documented through the “crashes” worksheet. (See next page.) Each workstation crash,

other than network crashes or power failure, must be documented.

Process:

1. Complete the “crashes” worksheet.

2. Contact a member of the LIMS staff.

3. Follow directions given to you by the LIMS staff representative.

If the LIMS personnel are not available, document the crash as accurately as possible, then re-boot your

computer.

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5

Crashes

Employee:

Date/Time:

Operating System:

Cause: Network OS Application LIMS Program

Other: ________________________________

Description of problem. Must be filled in by the user.

Description of problem. Must be filled in by Keith Vogel or Rick Penner.

Describe how the problem was resolved. Must be filled in by Keith Vogel or Rick Penner.

Note: Section IV was reviewed on 01/08/16 (No changes were made)

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CREATION, MODIFICATION, DISTRIBUTION AND MAINTENANCE OF LABORATORY CONTROLLED DOCUMENTS

SECTION V REVISION 7 EFFECTIVE DATE 01/08/16 Page V-1


The following procedures will address the maintenance and control of BCL’s controlled

documentation. Documents under controlled status include:

QAPP – Quality Assurance Program Plan

SOPs – Standard Operating Procedures

Logbooks

Employee Policy

QAPM – Quality Assurance Protocols Manual

A document is considered under control when:

it has been through a structured approval process

material is specifically kept esoteric

distribution is monitored and maintained

periodic or necessary modifications are made, reviewed, and counted

earlier versions are destroyed less at least one copy which is archived

It is extremely important to maintain certain documents under a controlled status in order to assure

information is conveyed accurately and maintained current.

All employees will have controlled documents in their possession, thus it is very important to

understand the process to keep our documentation sound and accurate.

5.2 Creation

5.2.1 QAPP/QAPM

The QAPP should be written and maintained by the QA Officer. The QA Officer should interview

appropriate personnel for information on process while consulting references to validate the

appropriateness of laboratory processes and procedures. The QAPP is revisited at least annually,

however when major modifications are made which would necessitate revisions, all personnel with

information or ownership of the new or revised process should contact the QA Officer to ensure

timely and accurate modifications. The QAPP should be approved by the management staff of BCL

on an annual basis.

5.2.2 SOPs

SOPs should be written by a person who has an adequate level of expertise in the subject matter.

Please see the SOP template in this document for guidance when creating analytically based

Standard Operating Procedures.

Write the SOP in rough draft form. The rough draft should be submitted to the Word Processing

Specialist (WPS) to initiate document maintenance. The WPS will then submit the rough draft to the

author for review. The author should then make any correction(s), if necessary, before submitting

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the SOP to his/her department supervisor. The department supervisor will then make any necessary

changes before submitting the SOP to the QA Officer. The QA Officer will review and make proper

modifications as necessary before submitting the SOP back to the WPS. The same review process

will follow a second time. When all modifications are performed and the SOP is deemed acceptable,

the department supervisor and the QA Officer will sign an approval sheet to verify the acceptability

of the document.

Objectives of Reviews

Analyst Review

Grammar

Content

Department Supervisor Review

Grammar

Accuracy of the procedure to actual process

Content

QA Officer Review

Grammar

Comparability to referenced method

5.2.3 Logbooks

Logbooks should be created by the person(s) with an extensive working knowledge of the process to

be monitored. This will ensure minimal changes, short term and long term. All logbooks designs

are submitted to the WPS for creation. The WPS will then submit the logbook sheet to the creator

for review. The log sheet should be reviewed by respective department supervisors before all

logbooks are formed. When acceptable, log sheets will be numbered sequentially and bound by the

WPS. A descriptive title and logbook number should be documented on a cover sheet for each

logbook.

5.2.4 Employee Manuals

Employee manuals outline workers rules of conduct, policies and benefits. It was written by the

management staff of BCL. This document is reviewed and updated annually by the management

staff of BCL.

5.3 Modification

5.3.1 QAPP

The QA Officer will forward all modifications to the WPS. The WPS will then submit the modified

material to the QA Officer for review. The QA Officer should consult all personnel who are

impacted by the modifications for approval. When approved, the modified section of the QAPP is

distributed to those all personnel who are on the distribution list.

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5.3.2 SOPs

SOPs should be reviewed on at least annually (every year) basis. Prior to respective employee

annual performance evaluations, all pertinent SOPs should be reviewed and modified as necessary.

These SOPs should be brought to the performance evaluation interview to be discussed. All

modified SOPs should then be submitted to the WPS. The same review process will follow as

discussed for SOP creation.

5.3.3 Logbooks

Laboratory logbooks review frequency has been established to be performed on a quarterly basis.

Department supervisor or authorized personnel will review standards, reagents and maintenance log

at least on a monthly basis. Review of logbooks performed for completeness and legibility purposes.

All Wet Chemistry analysis for manual tests review is performed in the element as a supervisor

review. All non-manual test (e.g. metals, organics) logbooks review will follow as stated above.

Keep logbook in appropriate place in the same vicinity where the analysis or prep work is to take

place. When logbooks are completed, get a new one from the word processor and put preceding

number of logbook on the front cover. Give the completed logbook to the quality assurance

department. The quality assurance department then puts the logbook number into a tracking system.

The book then goes into a storage shelf for that particular prep or analysis in the data storage room.

When the data storage shelf is full, the logbooks are stored at the storage facility where they will

remain until a seven year period has passed.

5.3.4 Employee Manual

Modifications are discussed during one or more sessions of supervisor meetings; The Director of

Human Resources gathers the information and makes changes. When acceptable, the Human

resources submit modifications to the WPS for distribution.

5.4 Distribution

5.4.1 QAPP

Distributions of controlled copies of QAPP are distributed to the management staff of BCL.

Uncontrolled copies are readily available to BCL clients; however, controlled copies can be

approved for distribution if absolutely necessary. Controlled copies which are distributed to

department supervisors should be made readily available to all employees. One controlled copy is

assigned to the conference room which is readily available to all employees. It is important that all

BCL employees recognize and understand the policies within the QAPP in order to foster an

environment conducive to quality improvement. Distribution is documented on acknowledgement

sheets which are signed by all personnel receiving controlled copies.

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5.4.2 QAPM

Controlled copies of the QAPM are distributed to the management staff of BCL. Each department

supervisor should request a copy from the QA Officer and/or WPS. The WPS is responsible for

tracking and distribution of the manuals. Distribution is documented on acknowledgement sheets

which are signed by the party receiving a controlled copy.

5.4.3 SOPs

Controlled copy distribution is restricted to all personnel directly associated to respective procedures

and to the pertinent department supervisor. Controlled copies should be restricted within the

laboratory. Clients requesting copies of SOPs should be given the latest approved uncontrolled SOP

version. Documentation of distribution of SOPs is in the form of acknowledgement sheets which are

signed by parties receiving controlled copies.

5.4.4 Employee Manuals

All employees of BCL should be given a controlled copy of the BCL Employee Manual. Employees

are required to sign an acknowledgement which verifies distribution.

5.5 Management

5.5.1 QAPP/QAPM

Distribution acknowledgements are maintained by the Word Processor Specialist (WPS). When all

personnel receive an updated section or version of the QAPP/QAPM, the old revision should be

return to the WPS to be destroyed. The WPS archives all versions of the QAPP in electronic form as

a record of policy and procedure within certain blocks of time. Approval from the QA Officer must

be granted prior to releasing a controlled copy of the QAPP or QAPM. The WPS maintains a

database of the distribution of controlled copies.

5.5.2 SOPs

Distribution acknowledgements are maintained by the WPS. When any BCL personnel receive an

updated section of version of an SOP, the old version is returned to the WPS to be destroyed. The

WPS archives all versions of SOPs in electronic form as a record of policy and procedure within

certain block of time. The WPS maintains a database recording the distribution of controlled copies.

5.5.3 Employee Safety Manual

Distribution and control of the Employee Safety Manual is handled through the Director of Human

Resources and the WPS. Content is managed by the management staff of BCL while PAS is

responsible for document production and archival.

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5.5.5 Logbooks

Keep logbook in appropriate place in the same vicinity where the analysis or prep work is to take

place. Before the logbooks are completed a form needs to fill out a form to request replacements

from the Word Processor Specialist. However, at least one week notice have to be giving to the

WPS for creation of new logbooks. The WPS adds on the cover page a word-processing ID (Exp.

WCS001) and also a QC ID (Exp 13L001). The Word Processor Specialist enters the word-

processing ID and the QC ID into an Access tracking database. The completed logbooks are also

recorded in the access tracking database as received; and then go into a label box (Exp. 12-L018

“Year End 2012”) and store into the QC data storage room. Logbook boxes are kept in to data

storage room for two years and then transfer to the on-site storage facility where they will remain

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STANDARD OPERATING PROCEDURES TEMPLATE


1.0 SCOPE AND APPLICATION*

2.0 SUMMARY OF METHOD*

3.0 INTERFERENCE AND THEIR CORRECTIVE ACTION

4.0 APPARATUS AND MATERIALS*

4.1 APPARATUS

4.2 INSTRUMENT PARAMETERS

5.0 REAGENTS AND STANDARD SOLUTIONS

5.1 REAGENTS – NAME AND SOURCE

5.2 SOLUTIONS – DILUTION SCHEMES

5.3 WORKING STANDARDS

5.4 SPIKES

6.0 SAMPLE COLLECTION, PRESERVATION AND HANDLING

7.0 PROCEDURE*

8.0 QUALITY CONTROL

8.1 DETERMINATION OF IDL, MDL, AND PQL

8.2 METHOD BLANKS

8.3 QC SETS – DUPLICATES & SPIKES

8.4 CONTROL CHARTS

8.5 LOGBOOKS

9.0 CALCULATIONS

10.0 FORMS*

10.1 QC SHEETS

10.2 OTHER FORMS

11.0 METHOD PERFORMANCCE

12.0 GENERAL MAINTENANCE

13.0 WASTE MANAGEMENT

14.0 POLLUTION PREVENTION

15.0 SAFETY

16.0 REFERENCES *SOP sections that should also appear as part of Non-analytical SOP’s.

Note: Section V was reviewed on 01/08/16(No Changes were made)

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SAMPLE PROCEDURES

SECTION VI REVISION 7 EFFECTIVE DATE 01/08/16 Page VI-1

6.1 Overview

There are many aspects regarding the subject of sample handling such as sampling, sample preservation, sample

containment, sample logging, custody, tracking and sample disposal. The following section addresses these issues.

The quality of a sample result is dependant upon how the sample was handled from a physical standpoint as well as

from a documentation perspective. If the sample was mishandled physically, the quality of sample result would be

compromised accordingly. If sample handling documentation is corrupt, the quality would be questionable and thus

would be compromised also. Proper physical handling and documentation of this handling goes hand in hand in

providing for quality results.

6.2 Sample Containers

Excerpts from Standard Methods 19th

edition

The type of sample container is of utmost importance. Containers are typically made of plastic or glass, but one

material may be preferred over the other. For example, silica and sodium may be leached from glass but not plastic,

and trace levels of metals may sorb onto the walls of glass containers. For samples containing organic compounds,

avoid plastic containers except those made of fluorinated polymers such as polytetrafluoroethylene (TFE).

Some volatile compounds in samples may dissolve into the walls of plastic containers or may even leach substances

from plastic. Use glass containers for all organics analyses such as volatile organics, semi-volatile organics,

pesticides, PCBs and oil and grease. Avoid plastics wherever possible because of potential contamination from

phthalate esters contained in the plastics. Container caps, typically plastics, also can be a problem. Use foiled or

teflon-lined lids appropriately.

Refer to the Analysis Reference Chart for appropriate container use per method.

6.3 Sample Storage Before Analysis

Nature of sample changes: Some determinations are more likely than others to be affected by sample storage

before analysis. Certain cations are subject to loss by absorption on, or ion exchange with, the walls of glass

containers. These include aluminum, cadmium, chromium, copper, iron, lead, manganese, silver and zinc, which

are best collected in a separate clean bottle and acidified with nitric acid to pH below 2.0 to minimize precipitation

and absorption on container walls.

Temperature changes quickly; pH may change significantly in a matter of minutes; dissolved gases (oxygen, carbon

dioxide) may be lost. Because changes in such basic water quality properties may occur so quickly, determine

temperature, pH and dissolved gases in the field immediately after taking sample.

Changes in the pH-alkalinity-carbon dioxide balance may cause calcium carbonate to precipitate, decreasing the

values for calcium and total hardness.

Iron and manganese are readily soluble in their lower oxidation states; therefore, these cations may precipitate or

they may dissolve from a sediment, depending on the redox potential of the sample. Micorbiological activity may

be responsible for changes in the nitrate-nitrite-ammonia content, for decreases in phenol concentration and in

BOD, or for reducing sulfate to sulfide. Residual chlorine is reduced to chloride. Sulfide, sulfite, ferrous iron,

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SAMPLE PROCEDURES

SECTION VI

REVISION NO. 20


PAGE VI-2

iodide and cyanide may be lost through oxidation. Color, odor and turbidity may increase, decrease or change in

quality. Sodium, silica and boron may be leached from the glass container. Hexavalent chromium may be reduced

to chromic ion.

Biological changes taking place in a sample may change the oxidation state of some constituents. Soluble

constituents may be converted to organically bound materials in cell structures, or cell lysis may result in release of

cellular material into solution. The well-known nitrogen and phosphorus cycles are examples of biological

influences on sample composition.

Zero headspace is important in preservation of samples with volatile organic compounds. Avoid loss of volatile

materials by collecting sample in a completely filled container. Achieve this by carefully filling so the top of the

meniscus is above the top of the bottle rim. Take care not to dilute preservatives by overfilling. Serum vials with

septum caps are particularly useful in that a sample portion for analysis can be taken through the cap by using a

syringe, although the effect of pressure reduction in the headspace must be considered.

Time interval between collection and analysis: In general, the shorted the time that elapses between collection of a

sample and its analysis, the more reliable will be the analytical results. For certain constituents and physical values,

immediate analysis in the field is required. For composited samples it is common practice to use the time at the end

of composite collection as the sample collection time.

It is impossible to state exactly how much elapses time may be allowed between sample collection and analysis; this

depends on the character of the sample, the analyses to be made, and the conditions of storage. Changes caused by

growth of mico-organisms are greatly retarded by keeping the sample in the dark and at a low temperature (<4°C

but above freezing). When the interval between sample collection and analysis is long enough to produce changes

in either the concentration or the physical state of the constituent to be measured, follow the preservation practices

given in the Analysis Reference Chart. Record time elapsed between sampling and analysis, and which

preservative, if any, was added.

6.4 Preservation Techniques

To minimize the potential for volatilization or biodegradation between sampling and analysis, keep samples as cool

as possible without freezing. Preferably pack samples in crushed or cubed ice or commercial ice substitutes before

shipment. Avoid using dry ice because it will freeze samples and may cause glass containers to break. Dry ice may

also effect a pH change in samples. Keep composite samples cool with ice or a refrigeration system set at 6°C

during compositing. Analyze samples as quickly as possible upon arrival at the laboratory. If immediate analysis is

not possible, storage at 0-6°C is recommended for most samples.

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SAMPLE PROCEDURES

SECTION VI

REVISION NO. 20


PAGE VI-3

Use chemical preservatives only when they are shown not to interfere with the analysis being made. When they are

used, add then to the sample bottle initially so that all sample portions are preserved as soon as collected. No single

method of preservation is entirely satisfactory; choose the preservative with due regard to the determinations to be

made. Because a preservation method for one determination may interfere with another one, samples for multiple

determinations may need to be split and preserved separately. All methods of preservation may be inadequate when

applied to suspended matter.

Methods of preservation are relatively limited and are intended generally to retard biological action, retard

hydrolysis of chemical compounds and complexes, and reduce volatility of constituents.

Preservation methods are limited to pH control, chemical addition, the use of amber and opaque bottles,

refrigeration, filtration and freezing. The Analysis Reference Chart lists preservation methods by constituent.

6.5 Holding Times

Sample analysis must take place prior to the allotted maximum storage times per method. This maximum storage

time is referred to as the holding time. Our performance goal is to meet 100% of the holding times. Holding times

are regulatory, thus they are extremely important. As stated in an earlier section, analysis should take place as soon

as possible. If we operate just meeting sample holding times, we will be in a precarious position when sample loads

increase, thus try to analyze samples as soon as possible.

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ANALYSIS REFERENCE CHART

SECTION VI

REVISION NO. 20


PAGE VI-4

6.6 Table 1 MAXIMUM HOLDING TIME AND CONTAINER CHART

GENERAL / INORGANIC CHEMISTRY

ANALYSIS WATER (< 6°C) SOIL (< 6°C)

Max HT1 in Days

(unless noted) Min Sample Quantity2

Container Type Preservative Container Water Soil Water (ml) Soil (gm)

Alkalinity Pint P -- 8 oz. jar 14 -- 100 10

Ammonia (NH3) Pint P H2SO4; pH<2 8 oz. jar 28 28 100 5

BOD Quart (H) P -- 8 oz. jar 48 Hrs. 48 Hrs. 1000 150

Bromide Pint P -- 8 oz. jar 28 28 50 30

Chloride Pint P -- 8 oz. jar 28 28 50 30

Chlorine (Residual) Pint (H) P -- -- 15 Min. -- 500 --

COD Pint P H2SO4 pH<2 8 oz. jar 28 28 50 25

Color Pint AG/P -- -- 48 Hrs. -- 100 --

Cyanide (Total) Pint P NaOH; pH>12 8 oz. jar 14 14 200 20

Cyanide (Reactive) Pint P -- 8 oz. jar ASAP ASAP 50 50

Dissolved Oxygen Quart (H) P -- -- 15 Min. -- 500 --

Dissolved Organic Carbon 4 oz. AG -- -- 28 -- 100 --

Electrical Conductivity (EC) Pint P -- 8 oz. jar 28 28 200 --

Flashpoint Pint AG -- 8 oz. jar -- -- 500 100

Fluoride Pint P -- 8 oz. jar 28 28 50 30

Gross Alpha Quart P HNO3 <2 or Upres 8 oz. jar 6 Mo. 6 Mo. 1000 250

Gross Beta Quart P HNO3 <2 or Upres 8 oz. jar 6 Mo. 6 Mo. 1000 250

Hardness Pint P -- -- 28 -- 200 --

Hexavalent Chromium (Cr+6) 2 oz. P Borate/HCO3/CO3 -- 5 30 Days till Ext. 50 --

Pint P -- 8 oz. jar 24 Hrs. 7 Days to run 50 20

Iodide Pint P -- 8 oz. jar ASAP 28 Days 50 30

Nitrate/Nitrite (NO3/NO2) 2oz p H2SO4; pH <2 8 oz. jar 28 28 Days After Ext. 50 30

Nitrite (NO2) Pint P -- 8 oz. jar 48 Hrs. 48 Hrs. After Ext. 50 30

Nitrate as NO3 Pint P -- 8 oz. jar 48 Hrs. 48 Hrs. After Ext. 50 30

Odor Pint AG -- -- -- -- 500 --

ORP Pint (H) P -- -- ASAP -- 100 --

Perchlorate Pint P -- 8 oz. jar 28 28 50 30

pH Pint P -- 8 oz. jar 15 Min. -- 100 50

Phenols 4 oz. A H2SO4; pH <2 8 oz. jar 28 28 200 10

Total Phosphorous Pint P H2SO4; pH <2 8 oz. jar 28 28 100 10

Ortho- Phosphorous Pint P -- 8 oz. jar 48 Hrs. 48 Hrs. After Ext. 50 30

TDS Quart P -- -- 7 -- 500 --

TSS Quart P -- -- 7 -- 1000 --

Settleable Solids Quart P -- -- 48 Hrs. -- 1000 --

Total Solids Quart P -- 8 oz. jar 7 7 500 50

Specific Gravity Pint P -- 8 oz. jar 28 28 500 10

Sulfate Pint P -- 8 oz. jar 28 28 50 30

Sulfide (Total) Pint P Zn Acetate 8 oz. jar 7 -- 200 --

Sulfide (Reactive) Pint P -- 8 oz. jar ASAP ASAP 50 50

Surfactants (MBAS) Quart P -- -- 48 Hrs. -- 500 --

Coliforms 8 oz. GN Na2S2O3 -- 6, 30 Hr. -- 125 --

Total Kjeldahl Nitrogen (TKN) Pint P H2SO4; pH <2 8 oz. jar 28 28 100 10

Total Organic Carbon (TOC) 4 oz. A H2SO4; pH <2 8 oz. jar 28 28 100 25

Total Organic Halide (TOX) Pint A H2SO4; pH <2 8 oz. jar 7 Not specified 500 50

Turbidity Pint AG, P -- -- 48 Hrs. -- 50 --

METALS

ANALYSIS Container Type Preservative Max HT (1) Min. Sample Vol.

(mls)(2)

WATER

Total Metals Pint P HNO3 6 Months ( 28 Days -Hg/Si) 100

Dissolved Filtered in Field Pint P HNO3 6 Months ( 28 Days -Hg/Si) 100

Dissolved not filtered Quart P 6 Months ( 28 Days -Hg/Si) 250

Organic Lead Quart AG Chill to <°6 C 14 Days 1000

200.8 Copper and Lead5 Quart P HNO3 in lab pH<2 6 Months 1000

ANALYSIS Container Type Preservative Max HT1 Min Quantity (gms)2

SOIL

Total Metals 8 oz. Jar G Chill to <°6 C 6 Months ( 28 Days -Hg) 50

WET/STLC As needed G Chill to <°6 C 6 Months ( 28 Days -Hg) 50

TCLP As needed G Chill to <°6 C 6 Months ( 28 Days -Hg) 150

SPLP As needed G Chill to <°6 C 6 Months ( 28 Days -Hg) 150

Hexavalent Chromium 8 oz. Jar G Chill to <°6 C 30 Days / 7 Days from Ext. 50

Organic Lead 8 oz. Jar G Chill to <°6 C 14 Days 50

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ANALYSIS REFERENCE CHART

SECTION VI

REVISION NO. 20


PAGE VI-5

A= Amber

AG= Amber Glass with Teflon lined Cap

AP= Amber Plastic

G= Glass

GN= Sterilized Glass or Nalgene

H= Headspace Free

HT= Holding Time

P= Plastic

VOA= 40 ml Glass Vials with Teflon lined Cap


ORGANIC CHEMISTRY

ANALYSIS

WATER (< 6°C)

SOIL (<

6°C)

Max HT(1) in Days

(unless noted)

Water Soil

Min Sample

Quantity(2)

Container Type Preservative Container Extract Analysis Extract Analysis Water Soil (gms)

504 2x VOA G Na2S2O3 (3) 8 oz. Jar 14 1 14 14 1 VOA 10

508 Liter AG Na2S2O3 (3) 8 oz. Jar 7 14

1 L 50

524.2/ TCP/THMS 2x VOA (H) G Ascorbic/HCl in field -- -- 14 -- -- 1 VOA --

525.2/507 Liter AG Na2SO3/HCl in field -- 14(4) 30 -- -- 1 L --

548 2 x 250ml AG Na2S2O3 (3) -- 7 21 -- -- 200 mls --

549 Liter AP Na2S2O3 (3) -- 7 21 -- -- 200 mls --

552.3 125 ml AG NH4Cl -- 14 28 -- -- 1 VOA --

556 2 x VOA A NH4Cl/CuSO4 -- 7 40 -- -- 1 VOA --

632 Liter AG (3) 8 oz. Jar 7 40 14 40 1 L 50

8015B Gasoline Range 2x VOA (H) G HCl(3) 8 oz. Jar 14 14 -- 14 1 VOA 10

8015B Diesel Range Liter AG -- 8 oz. Jar 14 40 14 40 1 L 50

8015 Ethanol/Methanol

2x VOA (H) G -- 8 oz. Jar -- 14 -- 14 1 VOA 10

8021 BTEX/MTBE 2x VOA (H) G HCl(3) 8 oz. Jar -- 14 -- 14 1 VOA 10

8081/8082/608 Liter AG Na2S2O3 (3) 8 oz. Jar 7 40 14 40 1 L 50

8141 Liter AG (3) 8 oz. Jar 7 40 14 40 1 L 50

8151/615/515.1 Liter AG Na2S2O3 (3) 8 oz. Jar 7 40 14 40 1 L 50

8260/8240/624 2x VOA (H) G Ascorbic (6)/HCl in field 8 oz. Jar -- 14 -- 14 1 VOA 10

8270/625 2 x Liter AG (3) 8 oz. Jar 7 40 14 40 1 L 50

8310/610 Liter AG -- 8 oz. Jar 7 40 14 40 1 L 50

8330 Liter AG -- 8 oz. Jar 7 40 14 40 1 L 50

1664 Oil and Grease Liter AG HCl 8 oz. jar 28 -- 28 -- 1 L 50

1664 TPH Liter AG HCl 8 oz. jar 28 -- 28 -- 1 L 50

TCLP Volatiles 8 oz. G -- 8 oz. Jar 14 7 14 7 1 L 50

TCLP Semi Volatiles Liter (Each test) AG -- 8 oz. Jar 7 40 14 Days until TCLP Leaching

AIR / VAPOR

ANALYSIS Container

Keep from Light Max HT1 Min Mass (L)

ASTM D-1946 Fixed Gases Tedlar Bag 3 1

Summa Canister 30 5

25C Landfill Gases TGNMO Tedlar Bag 3 1

Summa Canister 30 5

TO-3 TPH Gas Tedlar Bag 3 1

Summa Canister 30 5

TO-14A/TO-15 VOCs Tedlar Bag 3 1

Summa Canister 30 5

NOTES:


(1) = Calculated from time the sample is collected.

(2) = Amount needed to achieve normal method detection limits or regulatory requirements.

(3) = Samples containing residual chlorine must be dechlorinated at the time of sampling.

(4)= 7 Days if Diazonin is requested.

(5)= First Draw sample after 6 - 12 Hour idle period.

(6)= Ascorbic only if from chlorinated source

Fill all containers as much as possible.

TCLP and STLC extractions cannot be conducted on acid-treated containers.

Keep all Air/Vapor samples out of light.

8 oz. Jars all have Teflon lined Caps

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SECTION VII REVISION 5 EFFECTIVE DATE 01/08/16 Page VII-1


This section describes the methods of chain of custody for samples delivered or couriered to the fixed

laboratory, as well as internal laboratory chain of custody of samples and digests/extracts.

7.2 Summary

Chain of custody forms are completed by each client delivering samples to the laboratory. Each COC

contains fields such as Report To, Sample Description, Date and Time Sampled, Matrix, Analysis

Requested, Sample Receipt Conditions, TAT Info, Container Types, Billing Info., Disposal Info.,

Comments, and the Chain of Signatures of Custodians. Each time a sample changes hands between our

client’s personnel or a BC Laboratories courier or BC Laboratories personnel, the COC form is signed and

dated as to when the change of hands took place thus creating a chronological progression of possession of

the sample.

Internal chain of custody for samples is maintained through check out logs indicated on the sample

refrigerators and through disposal logs and manifests. Any individual retrieving and/or replacing samples

document pertinent information onto these logs. Extracts/digest custody transfers are documented on

preparation logs.

7.3 Potential Problems

Sometimes during the shipping or transporting of samples, COCs are rendered illegible due to sample

container breeches or water from ice wetting the COCs. In this case a client must be notified as to the

problem and a new COC is generated by the client. The client keeps a copy of the COC. Our COCs contain

3 copies: white, yellow and pink.

Any time a customer wishes to change any parameter on a COC form, the log-in department or authorized

person does such on our originals and denotes who requested the change, on what date, of which company

and for what reason the change was made. Also the change is initiated and dated as to who at BC

Laboratories made the change and on what the change was actually made.

If samples are received non-intact or are deemed corrupt in some form, the person receiving the samples

must contact a client service representative for resolution.

7.4 Custody

All samples must remain under custody from the time of sample analysis to the time of disposal. A sample

is considered under custody if:

1) It is in one’s possession verified by some form of documentation

2) It was in one’s possession and he/she locked it or placed it in a sealed container to prevent

tampering, or

3) It is within the laboratory grounds.

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7.5 Secured Facility

Please note that in order to define the lab as a “secured” area, we must keep the facility and the facility

grounds under locked conditions and accessed by authorized personnel. Unauthorized people may enter the

facility but only under monitored conditions. All doors and the perimeter fence should be locked by the

night shift supervisor at 1800 hrs.

7.6 Alarm System

The laboratory contracts Kern Securities to maintain the alarm system and to monitor after hours activities.

Employees must enter their numerical code to activate and deactivate the alarm system. The alarm system

needs to be activated by the last person leaving the facility on a given day.

Two codes or passwords are required to fully comply with the alarm system. The numerical code will allow

employees to activate and deactivate the alarm. A password is needed as a second line of security. If

working after hours, employee(s) will be required to disclose their password(s) to Kern Securities

representatives when these representatives call in to verify codes and activities.

In cases when the alarm goes off for no valid reason (i.e. no unauthorized entrance or no fire), the employee

must enter their numerical code into one of the alarm pads which are located at the main entrance and the

side entrance.

Codes and passwords must be obtained from the Director of Human Resources. These codes and passwords

are of exclusive use of each employee. Codes and passwords must not be shared.

7.7 Visitors

All visitors must log in and out of the Visitor Log-In Book which is kept by the receptionist. All

unauthorized people must be escorted by a BC Laboratories employee. Unauthorized people, other than

maintenance or instrument repair people may not be allowed to tamper with any laboratory instruments or

computers. All visitors entering analytical laboratory areas must use proper protective equipment.

7.8 Sample Custody Procedures

7.8.1 Procedure for Recording Sample Temperatures Upon Receipt

Objective: Ensure that personnel responsible for taking sample temperatures understand the importance of

sample temperatures in relation to the validity of data and to ensure that trainees can obtain and record

sample temperatures properly.

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7.8.2 The Importance of Sample Temperatures (0-6°C)

Samples maintained refrigerated to 0-6°C are considered preserved under conditions outlined in State and

Federal Regulations. Any temperature excursions outside 0-6°C allows for data of questionable validity.

The extent of the temperature excursion will determine the level of unreliability of the data.

A temperature range of 0-6°C was set to allow comparability of data and to provide a guideline for good

laboratory and sampling practices which prevent or deter alternative refrigeration/non-refrigeration

scenarios.

7.8.3 The Problem

Regulators tend to look at numbers and fit them into control limits or acceptable limits. If a number is not

within a limit, a regulator can invalidate data sometimes without regard to common sense. This is either

because they are not informed people or the data is highly visible or important and they do not want to stick

their neck out.

Some of our clients make sure potential temperature problems will not be variables by packing samples

properly. When we fail to properly record sample temperatures, we expose ourselves as incompetent. After

all, how easily is it to take a temperature.

7.8.4 Procedure

7.8.4.1 For Brass/Stainless Sleeves

7.8.4.1.1 Use the Thermocouple thermometer (Thermometer #THTTR2).

7.8.4.1.2 Pick a “representative” sample from the cooler.

7.8.4.1.3 Wipe the surface of the sleeve where you intend to take the

temperature. 7.8.4.1.4 Turn the thermometer on.

7.8.4.1.5 Verify the settings on the face of the thermometer are set to

“°C”.

7.8.4.1.6 Place the contact probe onto the sleeve. (Verify the contact

spring within the probe is in contact with the sleeve.)

7.8.4.1.7 Note the temperature. Disregard any zeros preceding whole

numbers.

7.8.4.1.8 Use common sense in judging whether or not the temperature is

accurate.

7.8.4.1.9 If the temperature is outside 0-6°C, either use another sample

(if available) or rotate the sample and take another reading.

7.8.4.1.10 If the temperature is still outside 0-6°C, record the lower

temperature on a Sample Receipt Form. See the section

“Sample Receipt Form Completion.”

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7.8.4.2 For All Other Containers

7.8.4.1.2.1 Use the FLUKE Non-Contact Infrared Thermometer

(Thermometer #208).

7.8.4.1.2.2 Pick a “representative” sample from the cooler.

7.8.4.1.2.3 Wipe the surface of the sample container where you intend

to take the temperature reading.

7.8.4.1.2.4 Press the button on the handle to turn the thermometer on.

7.8.4.1.2.5 The emissivity must be set according to the container type

you intend to take the temperature reading.

7.8.4.1.2.6 To set the emissivity, press the “Menu” button, then press

“Ɛ” and “No” keys to alter the reading until you reach the

desired setting. (See the table below.)

7.8.4.1.2.7 Once the emissivity is set, point laser at a section on the

sample bottle which represents the surface type that the

emissivity was set. (the IR gun has to touch the sample)

7.8.4.1.2.8 Note the “°C” at the upper right portion of the display. The

thermometer is taking readings. If a “°F” is noted, change

the setting to centigrade by pressing the “Menu” button 3

times, then press “C” keys until switches to the right

setting.

7.8.4.1.2.9 Note the temperature. Use common sense in judging

whether or not the temperature is accurate.

7.8.4.1.2.10 If the temperature is outside 0-6°C, first verify the

emissivity reading then check if the low battery warning is

flashing in the display.

7.8.4.1.2.11 If an accurate reading was taken and was outside 0-6°C,

choose another sample and take another temperature

making sure to follow the steps above.

7.8.4.1.2.12 If the temperature is still outside the acceptable range,

record the lower temperature on the Sample Receipt Form.

See the section “Sample Receipt Form Completion.”

7.8.4.1.2.13 For special containers other than the ones listed on the

label, see Emissivity Table on IR gun

Example of IR Gun Label

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Example of Emissivity Settings

Container Type Emissivity Temperature Correction

PE 0.97 Within ±1C range

Amber 0.98 Within ±1C range

Glass Clear 0.98 Within ±1C range

Bac-T Bottle 0.97 Within ±1C range

VOA Vial 0.95 Within ±1C range

*Please check with the QA/QC Department for individual IR gun calibration setting.

If an emissivity setting has not been verified by BCL, use the manufacturer’s guidelines noted in the owner’s

manual.

7.8.5 Sample Receipt Form Completion

7.8.5.1 Field Services Department

7.8.5.1.1 Check off the appropriate shipping information block.

7.8.5.1.2 Complete the Shipping Container section.

7.8.5.1.3 Check the appropriate refrigerant.

7.8.5.1.4 If custody seals were used, check appropriate boxes.

7.8.5.1.5 Enter pertinent information regarding sample temperatures for

each ice chest we are to receive.

7.8.5.1.6 If any anomalies are observed, please enter this information on

the comments section.

Example: Sample temperature was 10°C, but an adequate amount of blue ice was observed. This

information can be entered into comments. “Samples were refrigerated with an adequate amount of

blue ice, however the samples were kept under these conditions for x hours, thus the refrigerant

potential to keep sample temperatures at 0-6°C had been exhausted.

7.8.5.1.7 Any temperatures noted outside 0-6°C must be communicated

to Client Services. Submit the Sample Receipt Form to the

appropriate CSR. If the proper CSR is unavailable, either place

the form on his/her keyboard or submit to Client Service

Manager. Please use common sense…if a CSR is on vacation

don’t place it on his/her keyboard, etc.

7.8.5.1.8 The CSR must initial and date the form.

7.8.5.2 Sample Receiving Department

7.8.5.2.1 Fill in Submission Number and Project Code if available.

7.8.5.2.2 Check off the appropriate shipping information block.

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7.8.5.2.3 Complete the Shipping Container Section.

7.8.5.2.4 Check the appropriate Refrigerant.

7.8.5.2.5 If custody seals were used check the appropriate boxes.

7.8.5.2.6 Complete the sample custody check section.

7.8.5.2.7 Enter pertinent information regarding sample temperatures for

each ice chest we are to receive.

7.8.5.2.8 Complete the sample containers per ice chest section.

7.8.5.2.9 Sign and date the form at the bottom.

7.8.5.2.10 If any anomalies are observed, please enter this information in

the comments section.

Example: Sample temperature was 10°C, but an adequate amount of blue ice was observed. This

information can be entered into comments. “Samples were refrigerated with an adequate amount of

blue ice, however the samples were kept under these conditions for x hours, thus the refrigerant

potential to keep sample temperatures at 0-6°C had been exhausted.

7.8.5.2.11 Any temperatures noted outside 0-6°C must be communicated

to Client Services. Submit the Sample Receipt Form to the

appropriate CSR. If the proper CSR is unavailable, either place

the form on his/her keyboard or submit to Client Service

Manager. Please use common sense…if a CSR is on vacation

don’t place it on his/her keyboard, etc.

7.8.5.2.12 The CSR must initial and date the form.

7.8.6 Client to Laboratory

First, the samples are taken and with all pertinent information labeled by a customer or BC Laboratories

field service department. A chain of custody form is completed by the customer or at the customers request

by BC Laboratories personnel. All pertinent information is entered on the COC form, Report to, Project

info., Matrix, Analyses requested, TAT info., any comments, Billing info., and sample disposal information.

The relinquisher and receiver sign and date the COC at the time of the sample custody switch.

Upon completion of the COC forms the samples are shipped or couriered to the fixed lab, at which time the

samples are received, inspected and dated by the receiving individual.

7.8.7 Within the Laboratory

At the time of receipt the temperature of the sample(s) are taken. The pH of samples needing preservation

are checked and noted by preparation technicians and/or analysts. Also custody seals, if present, are noted.

Any sample breeches or anomalies in shipping containers are also noted. Information is noted on the Log-In

Sample Receipt Form.

Next the samples are assigned a unique laboratory number for identification throughout the labs. These

numbers are checked by a second person. A rubber stamp has been produced to be used to provide a

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template to document number checking.

The sample containers are labeled with this number and all COC information present on the sample

containers is cross checked with the COC itself. If any discrepancies are found, the client is notified and

corrective action takes place. Distribution of samples takes place and is documented on the COC.

All pertinent information such as sampling dates, times, container types and numbers, analyses requested,

sample description, matrices, client specific information, etc. are entered into the LIMS for sample tracking,

data sheet generation, final report generation and billing.

All worksheets for the tests requested are generated by the Log-In department and distributed throughout the

lab.

Samples are stored in refrigerators that have a check-in/out log associated with it. Samples are placed in

shelves and must be logged out when removed, or logged back in when they are returned.

Copies of the COC forms are made to accompany worksheets for each department. The original is kept on

file by client service representatives and then is sent with the final report to the client.

BC Laboratories has the capability of sending pre-completed COC forms along with sample containers to

clients who know what tests are needed in advance of sampling. These forms contain: Customer info.,

Project info., Analyses requested, Matrices, Billing info., as well as sample description pre-entered for a

clients ease of use.

7.8.8 Laboratory to Subcontractors

COCs are completed by BC Laboratories for any samples that are sent out to a subcontract laboratory.

Normal COC procedures are followed.

Non-BC Laboratories COC forms are treated just as our own. All normal COC procedures are followed.

7.8.9 Disposal

7.8.9.1 Aqueous Samples

Once analyses have been completed, samples ready for removal can be logged out of holding refrigerators.

Acknowledgement of final removal of samples from refrigerators is noted on respective refrigerator logs.

Samples are then temporarily stored in various areas within the lab until the person who assumed custody

can relinquish samples to a designated person who has waste archiving/disposal responsibilities. Transfer of

custody should be documented on sample tracking logs. Samples are then archived and temporarily stored

in a sea-train. When appropriate, personnel who have waste disposal responsibilities dispose of samples

according to waste stream type. Waste sample disposal should be documented on sample tracking logs.

7.8.9.2 Non-Aqueous Samples

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Once analyses have been completed, samples ready for removal can be logged out of the walk-in

refrigerators. Acknowledgement of final removal of samples from refrigerators is noted on the walk-in

refrigerator log. Samples and splits are then temporarily stored into boxes which are kept in the caged area

in the back of the laboratory. Tracking of samples and splits into boxes is conducted through the LIMS:

Cursor to “More” enter; then “Misc” enter; then “Sample Storage” enter. Enter box ID, date, then

sample IDs.

Samples are disposed of in boxed lots according to potential hazard approximately 60 days after collected

into boxes. Disposal is recorded into a sample disposal log which cross references waste drum IDs or other

disposal containers to box IDs.

7.8.10 Quality Control

As stated above, all sample information present on sample container is cross checked by sample receiving

personnel. All sample transport containers are checked for: temperature, damage or sample breeches.

Notes of such are placed on COC forms. Custody seals are noted on COC forms. Only indelible ink may be

used to complete a COC form. If an error is made, we request that clients make a single line through the

entry as well as initialing and dating the new entry. BC Laboratories personnel follow this policy. No

changes to a COC form may be made without first contacting the client. When a client requests or OKs a

change, the change is noted, dated and who OK’d the changes is noted. Also, the person physically making

the change to the COC must initial and date the change.

7.8.12 Sample Digest/Extract Tracking

Sample digests and extracts are tracked through digestion and run logs. Analysts acknowledge receiving

prepared samples from sample preparation personnel by signing respective preparation logs. Once in their

possession, analysts must store prepared samples in designated areas until sample analyses are complete.

Prepared samples must be archived into waste containers then disposed of through proper waste streams.

Documentation should be accurate enough to trace digests/extracts to a waste drum or waste receptacle.

7.8.12 Documentation

As mentioned earlier in this section, sample custody and tracking must be documented on chain of custody

forms, refrigerator logs, Sample tracking logs, sample disposal logs and manifests.

7.8.12.1 General Rules Pertaining to Logs:

7.8.12.1.1 Use indelible black ink only.

7.8.12.1.2 Follow proper error correction procedure-line through, initial

and date.

7.8.12.1.3 Write legibly.

7.8.12.1.4 Keep logs away from potential damaging sources like water.

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7.8.12.1.5 Proceed in sequential page order.

7.8.12.1.6 Keep logs in their designated areas.

7.8.12.1.7 Turn logs into the QA/QC Department when full or damaged.

7.8.12.2 How to Obtain Documentation Forms

Chain of Custody Forms – Sample Receiving Area

Logs – The Word Processing Specialist. See Controlled Documents section

Manifests – Copies are kept by the President of BC Laboratories.

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STANDARD AND REAGENT HANDLING

SECTION VIII REVISION 3 EFFECTIVE DATE 01/08/16 Page VIII-1

8.1 Introduction

The quality, validity and documentation of standard materials are critical to data quality since all

identification and quantitation of results, as well as judgment about the quality of data, rely on values for the

standard materials. The following section outlines procedures on how to qualify, prepare, validate, store and

document standards and reagents.

8.2 Qualification

It is extremely important that stock standards and reagents are appropriate for use. There are numerous

purity grades of chemicals and these grades are classified or named differently by vendors. Please refer to

the Purity Translation Table for some guidance on the appropriateness of chemicals for use with your

particular methods. Generally, the less pure a chemical, the less the price. Since some impurities may not

affect certain tests, “general use” chemicals may be appropriate for use.

Whenever possible, chemicals should be NIST traceable and ACS approved. Chemicals should be

purchased from vendors who are ISO 9001 or ISO 9002 certified.

Purity Translation Table

Manufacturer Grade Application

Aldrich ACS Most analytical applications

Baker Baker Analyzed Does not necessarily meet ACS standards. General lab use.

Baker Ultrex/Ultrex II Trace level metals. Ultra high purity.

Baker Instra-Analyzed Trace element analysis.

Baker Analyzed-HPLC HPLC applications

Baker Resi-Analyzed Residue and volatiles analyses

Baker Purified General use. Glassware cleaning.

Baker BAKER General laboratory use

Baker Practical General laboratory use

Baker Technical General laboratory use

Fisher GC Resolv Gas Chromatography

Fisher Optima HPLC, GC, plasma/ICP, spectrophotometery and pesticide residue

analysis

Fisher HPLC HPLC and spectrophotometry procedures

Fisher Pesticide GC with electron capture detector

Fisher Spectranalyzed Ultraviolet and visible wavelength detectors

Fisher TraceMetals Primarily used for digestion of samples prior to ICP analysis

Fisher Certified ACS Plus Analytical application with tighter metal specifications

Fisher Certified ACS Analytical application requiring tight specifications

Fisher Certified General analytical

Fisher Laboratory and

Technical

Manufacturing and general laboratory use

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Malinckrodt ACS Meets requirements of the American Chemical Society Committee

on Analytical Reagents

Malinckrodt AR* General laboratory use

Malinckrodt AR* Primary

Standard

Standardizing volumetric solutions and preparing reference

standards

Malinckrodt AR Select* ACS quality standards for trace metals

Malinckrodt AR Select # Plus Specifically purified by sub-boiling distillation. Nearly all trace

level impurities are less than 1 ppb.

Malinckrodt Nanograde Solvent reagent quality

Malinckrodt StandARd* Atomic absorption

Malinckrodt Technical General industrial use

Malinckrodt UltimAR* Specialty solvents distilled to purity levels exceeding the

requirements for HPLC, TLC, GC and pesticide residue analysis.

Please contact your department supervisor if you are ordering “general use” grade chemicals for new

applications. Please see the procurement section of this manual for details on ordering standards and

reagents.

8.3 Receiving

Immediately upon receipt, standards and reagents must be checked against the requisition form or the

expiring or old standard or reagent to verify suitability. If the standard or reagent is from a different vendor

or if the grade has changed, contact your department supervisor before proceeding.

Standard and reagents must be systematically labeled with the dates of receipt and expiration (if not noted

on the label). Immediately upon opening, standards and reagents must be labeled with the date of opening.

Labeling must be specific and legible enough to discern the difference between receiving, opening and

expiration dates. If information cannot fit onto the container, please use tape as a label flag or provide

information on a small label to direct where label information can be found.

All standards should be received with a Certificate of Analysis. This record acts as a traceability record and

a purity verification. Keep an orderly log of these records in your work area. If you do not receive a

Certificate of Analysis with the ordered standard, contact your department supervisor to secure a copy.

8.4 Preparation

Standard and reagent solutions must be prepared using Class A volumetric glassware or internally calibrated

volumetrics and pipettes. Automatic pipettes and gas tight syringes used to prepare standards must be

checked for conformance to calibration specifications prior to use. Standards prepared in the laboratory

must be labeled with the contents (analyte and concentration), initials of the preparer, standard code, date of

preparation, date of expiration and potential hazard.

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8.5 Expiration Date

Expiration dates must be assigned and documented for all standard, reagent and quality control materials.

All standards and reagents must be labeled with expiration dates. Expiration dates can be figured or

assigned in different ways.

Manufacturer Set: Expiration dates set for stock materials are set by the manufacturer. Assigned expiration

dates for purchased materials must not exceed the manufacturer’s expiration dates. Assigned expiration

dates for laboratory-prepared stock and diluted standards must not exceed the most limiting expiration date

of a component stock solution or material.

Method Set: Standard and reagent expiration dates are set according to method references.

Laboratory Set: If the analytical method does not provide guidelines for standard material shelf life, the

expiration date must be assigned based on professional judgment, and in consideration of the stability and

concentration of the constituents and storage conditions. These expiration dates must be discussed in

method SOPs.

Prepare a standard orreagent from a stock

solution

Note the expirationdate of the analyte(s)of the stock solution

Does any analyte fromthe stock expire prior tothe expiration date set

by the method orlaboratory SOP?

Figure the expiration dateof the prepared standard

or reagent set by theref erenced method or thelaboratory . Ref er to the

method SOP.

The expiration date isdefaulted to the stock

expiration date.

The expiration date isset according to the

referenced method orlaboratory method

SOP.

Yes

No

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Prior to initial use, the quality and accuracy of standards must be accessed through comparison with

reference standard materials of known composition. Newly made standards must not exceed five (5) percent

difference from the reference standard.

8.6 Preservation and Storage

Preservation use and storage conditions must comply with manufacturer’s recommendations, method

protocols or with good laboratory practices as to maintain standard or reagent integrity. One must consider

storage container types, potential for cross contamination sources and temperature when storing reagents and

standards. Preservative use should take sample matrix matching situations into consideration. Please refer to

respective method SOPs for specific details.

8.7 Documentation

Laboratory logbooks must document the preparation of each standard and reagent from original stock

materials, including subsequent dilutions. A unique identifier must be assigned to each original stock

material and to each subsequent dilution. Logbook entries must include the prepared concentration and

unique identifier of the prepared material, the dates of preparation and expiration, the amount and the lot

numbers or unique identifiers of the materials and solvents used to prepare the material, and the identity of

the person who prepared the materials. The reference comparison check may also be included in the

standard log.

Organic Department personnel should refer to SOPs for details on the preparation and nomenclature of

standards and reagents. Inorganic standards and reagent preparation and nomenclature should be addressed

in individual method SOPs.

8.8 Disposal

When standards and/or reagents have expired, they must be pulled out of service. The remainder of the

standard/reagent must be disposed of properly through one of our waste streams. Please refer to the Waste

Disposal SOP or consult your department supervisor.

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GLASSWARE

SECTION IX REVISION 3 EFFECTIVE DATE 01/08/16 Page IX-1

9.1 Overview

The proper handling and use of laboratory glassware will assure the accuracy and validity of data to a

certain extent. For example, when we use proper glassware for standard preparation, we are assuring the

standard was made up with a prescribed tolerance or error. Our standard operating procedures include

specified glassware to be utilized because of the need to standardize operations and to allow our

analytical systems to reproduce results. We must also prescribe to diligently and properly clean

glassware to minimize the probability of introducing contamination and interfering artifacts. The

following section deals with good laboratory practices associated with glassware. Glassware includes

receptacles which are not only glass, but made of teflon or other materials.

9.2 Types

For our purposes we will define only two classes of volumetric glassware:

9.2.1 Class A glassware – Volumetric glassware that meets volume tolerance levels as

specified in ASTM E 288, E 542, and E 694. This glassware is exclusively used to

prepare standard materials and can be used for titration analyses.

9.2.2 Non-Class A – Any glassware that is not Class A. Used for general lab use such as

preparing reagents and can be used to prepare standards if proper calibration verification

studies deem volume deliveries or capacity meets Class A standards.

Class A Volumetric Flasks

Flask Capacity (mls) Tolerance (mls)

5 +0.02

10 +0.02

25 +0.03

50 +0.05

100 +0.08

200 +0.10

500 +0.20

1000 +0.30

2000 +0.50

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Class A Volumetric Pipettes

Capacity (mls) Accuracy (mls)

0.5 +0.006

1.0 +0.006

2.0 +0.006

4.0 +0.01

5.0 +0.01

10.0 +0.02

15.0 +0.03

20.0 +0.03

25.0 +0.03

50.0 +0.05

100.0 +0.08

9.2.3 Pipettes Types

9.2.3.1 Disposable Transfer pipette: Single unit with a built-in pipette bulb.

9.2.3.2 Pasteur Pipette: Pipettes with a long narrow tip, typically not graduated,

which require a bulb to receive liquid.

9.2.3.3 Serological and Mohr Pipettes: Long cylindrical graduated pipettes that

can be used to deliver various volumes.

9.2.3.4 Volumetric Pipettes: Used to deliver a specified volume. Has a

distinctive bulge in its design.

9.2.3.5 Repipette Dispensers: Adjustable delivery dispensers which are attached

to reagent containers.

9.2.3.6 Repeater Pipetters: A fixed volume delivery system that includes a pipette

head which connects to a flask. Volume is delivered by first filling the

pipette head by tilting the flask back then tilting the flask forward to empty

the contents.

9.2.3.7 Micro-pipettes: A plunger-type gadget with a disposable tip which is used

to deliver fixed volumes.

9.2.3.8 Syringe: A graduated opened end tube with plunger

9.2.4 Flask Types

9.2.4.1 Volumetric: Fixed volume flasks which are used to prepare or contain

samples, reagents or standards. This flask has a relatively long cylindrical

neck with a blown-out lower body. Designed to accept either teflon or

glass caps.

9.2.4.2 Erlenmeyer: All purpose graduated flask used for multiple purposes such

as reagent and sample preparation activities. This flask comes in many

sizes and is shaped like a rounded pyramid. The top can have a fitted cap

or can come with optional fittings or stems which allow for vacuum

processes.

9.2.4.3 Distillation: Rounded bottomed flask which was designed for efficient

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distillation through heat containment design or heating mantle fit and

continued sample dynamics by physical dispersion. A flask holder must be

used to house these flasks because they cannot stand on their own.

9.2.5 Funnels

9.2.5.1 Separatory: Rounded body receptacle equipped with a fitted top, long

stem and stopcock. Used to separate layers within solutions.

9.2.5.2 General Purpose Filtering: Wide angled funnel with long cylindrical stem.

Used to house filter paper used for gravity filtrations. Also used to

introduce materials into receptacles with narrow orifices.

9.2.5.3 Buchner: Funnels which are used when filtrates attack filter papers.

Designed for vacuum filtration.

9.2.5.4 Millipore: A four piece unit: (stem with a filter housing, cylindrical body,

clamp and filter screen), which fits onto a large Erlenmeyer flask. Used to

filter samples under vacuum.

9.2.6 Tubes

9.2.6.1 Test: Typically non-graduated, these receptacles are long and cylindrical

with a rounded end.

9.2.6.2 Centrifuge: Conical bottomed tubes which are designed to withstand the

rigors of a centrifuge. Usually graduated with screw top closure

capabilities.

9.2.6.3 Kuderna: Danish Concentrator: A graduated tube which is used in

conjunction with a flask with two orifices and a cooling column chamber

or condenser for the concentration of trace amounts of samples dissolved

in solvents.

9.2.7 Burets

Long, cylindrical, graduated open-ended tube equipped with a stopcock. Used to deliver and measure

liquid delivery for titrations.

9.2.8 Beakers

9.2.8.1 Griffin: Non-tapered cylindrical wide-mouthed container typically with

graduations that is used for preparing reagents and samples. The top

usually has a flared spout for easy pouring.

9.2.8.2 Berzelius: Taper cylindrical wide-mouthed container which is narrower

than a Griffin beaker. Use is generally the same as for the Griffin beaker.

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9.2.9 Watch Glasses

9.2.9.1 Non-ribbed: Beaker covers used to prevent excess splatter, control cross-

contamination and to speed up preparation processed which require a

heating step.

9.2.9.2 Ribbed: Beaker covers used to prevent excess splatter, control cross-

contamination and to speed up. Ribbed design permits reflux of digestate

and escape of excess vapor, thus preventing vapor build up. Ribs also

prevent watch glasses from sticking together when wet.

9.2.10 Graduated Cylinder

9.2.10.1Graduated Cylinder: Graduated tube with a flattened bottom which

allows it to stand upright. Used to prepare and measure samples and

reagents. Not highly accurate, thus use accordingly.

9.3 Glassware Colors

Glassware used in the laboratory typically comes in two colors, amber and flint. There are advantage

and disadvantages in housing samples or standard materials in amber or flint colored receptacles.

9.3.1 Amber: Brown colored receptacles used to slow the breakdown of light sensitive

components.

9.3.2 Flint: Clear colored receptacles which allow for clear viewing of sample or standard

material.

9.4 Cleaning

Because we report concentrations for many analytes at the part per billion level, it is important to wash

glassware thoroughly prior to use. Glassware cleaning should be thorough, appropriate, systematic and

consistent in order to maintain control of your process. Any artifacts left on glassware brought into

contact with a sample or standard material can cause adverse effects. Contamination is not the only

problem here; artifacts can interfere with certain tests thus causing compromised results. Certain tests

may require special cleaning and glassware preparation procedures, so always refer to the method SOP

for details.

As a general rule, if water drops adhere to the sides of containers and inside pipettes after rinsing, this

indicates that glassware is dirty.

9.5 Organics Testing

In the analysis of samples containing components in the parts per billion range, the preparation of

scrupulously clean glassware is mandatory. Failure to do so can lead to a myriad of problems in the

interpretation of the final chromatograms due to the presence of extraneous peaks resulting from

contamination. Particular care must be taken with glassware such as Soxhlet extractors, Kuderna-

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Danish evaporative concentrators or any other glassware coming in contact with an extract that will be

evaporated to a smaller volume. The process of concentrating the compounds of interest in this

operation may similarly concentrate the contaminating substance(s), which may seriously distort the

results.

The basic cleaning steps are:

1. Removal of surface residuals immediately after use;

2. Hot soak to loosen and float most particulate material;

3. Hot water rinse to flush away floated particulates;

4. Soak with an oxidizing agent to destroy traces of organic compounds;

5. Hot water rinse to flush away materials loosened by the deep penetrant soak;

6. Distilled water rinse to remove metallic deposits from the tap water;

7. Alcohol (e.g., isopropanol or methanol) rinse to flush out any final traces of organic

materials and remove the water; and

8. Flushing the item immediately before use with some of the same solvent that will be used

in the analysis.

Each of these eight fundamental steps will be discussed in the order in which they appear.

1. As soon as possible after glassware (i.e., beakers, pipettes, flasks, or bottles) has come in

contact with sample or standards, the glassware should be flushed with alcohol before

being placed in the hot detergent soak. If this is not done, the soak bath may serve to

contaminate all other glassware placed therein.

2. The hot soak consists of a bath of a suitable detergent in water of 50°C or higher. The

detergent, powder of liquid, should be entirely synthetic and not a fatty acid base. There

are very few areas of the country where the water hardness is sufficiently low to avoid the

formation of some hard-water scum resulting from the reaction between calcium and

magnesium salts with scum or curd would have an affinity particularly for many

chlorinated compounds, and being almost wholly water-insoluble, would deposit on all

glassware in the bath in a thin film.

There are many suitable detergents on the wholesale and retail market. Most of the

common liquid dishwashing detergents sold at retail are satisfactory but are more

expensive than other comparable products sold industrially.

3. No comment required.

4. The most common and highly effective oxidizing agent for removal of traces of organic

compounds is the traditional chromic acid solution made up of concentrated sulfuric acid

and potassium or sodium dichromate. For maximum efficiency, the soak solution should

be hot (40-50°C). Safety precautions must be rigidly observed in the handling of this

solution. Prescribed safety gear should include safety goggles, rubber gloves, and apron.

The bench area where this operation is conducted should be covered with fluorocarbon

sheeting because spattering will disintegrate any unprotected surfaces.

The potential hazards of using chromic sulfuric acid mixture are great and have been well

publicized. There are now commercially available substitutes that posses the advantage

of safety in handling. These are biodegradable concentrates with a claimed cleaning

strength equal to the chromic acid solution. They are alkaline, equivalent to ca. 0.1 N

NaOH upon dilution, and are claimed to remove dried blood, silicone greases, distillation

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residues, insoluble organic residues, etc. They are further claimed to remove radioactive

traces and will not attack glass or exert a corrosive effect on skin or clothing.

5. No comments required.



8. There is always a possibility that between the time of washing and the next use, the

glassware could pick up some contamination from either the air or direct contact. To

ensure against this, it is good practice to flush the item immediately before use with some

of the same solvent that will be used in the analysis.

The drying and storage of the cleaned glassware is of critical importance to prevent the beneficial effects

of the scrupulous cleaning from being nullified. Pegboard drying is not recommended. It is

recommended that laboratory glassware and equipment be dried at 100°C. Under no circumstances

should such small items be left in the open without protective covering. The dust cloud raised by the

daily sweeping of the laboratory floor can most effectively re-contaminate the clean glassware.

As an alternative to solvent rinsing, the glassware can be heated to no higher than 300°C to vaporize any

organics. Do not use this high temperature treatment on volumetric glassware, glassware with ground

glass joints, or sintered glassware.

9.6 High Concentrated Samples

Contamination of low-level samples may occur when prepared in the same laboratory with highly

concentrated samples. Ideally, if both type samples are being handled, glassware dedicated solely to the

preparation of highly concentrated samples would be available for this purpose. If this is not feasible, as

a minimum when preparing highly concentrated samples, disposable glassware should be used or, at

least, glassware dedicated entirely to the high concentration samples. Avoid cleaning glassware used for

both trace and high concentration samples in the same area.

9.7 Metals

Cleaning sample containers used for metals analyses involves a tap rinse, an addition of 1:1 HNO3, and

a final rinse with metal-free water. For quartz or glass containers housing samples or standard materials

for metals, use a concentrated solution using HNO3 and HCL, or aqua regia (3 parts conc HCL + 1 part

HNO3) for soaking. After soaking, thoroughly rinse with metal-free water. Chromic acid may be used

to remove organic deposits, however we suggest not to use chromic acid for plastic containers or if

chromium is to be determined.

9.8 Wet Chemistry

Thoroughly clean containers with a phosphate-free detergent, then rinse with copious amounts of Type II

water. Chromic acid may be used to remove organic deposits from glass containers, however do to

safety hazard, and use this reagent with care.

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9.9 How to Measure Containment

In order to properly measure liquids contained in glassware, you must fill until the liquids’ meniscus

touches the fill line or the desired graduation. The meniscus is the curved upper surface of a liquid.

9.10 Delivery and Containment Glassware Types

9.10.1 To contain: hold the exact volume of liquid specified.

9.10.2 To deliver/blow out: must be allowed to drain, then the drop that remains must be blown

out and added to the original delivery to equal the exact amount.

9.10.3 To deliver: must be held vertically with the tip against the side of the receiving vessel

and allowed to be drained completely. The stated volume is obtained when draining

stops.

Note: Section IX was reviewed on 01/08/16(No changes were made)

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MEASURING

SECTION X REVISION 3 EFFECTIVE DATE 1/08/16 Page X-1

10.1 Weight

When weighing a component, one must consider the following variables:

Accuracy

Safety

Containment

10.2 Accuracy

Analytical balances are capable of accurately measuring the weight of a component to within 0.5 mg.

Instances where weighing using an analytical balance include:

Gravimetric testing requiring a high degree of accuracy

Weighing of standards and/or reagents

Micro-pipette calibration

Others

The analytical balance with the digital display is not as accurate as the other analytical balances, thus it is

highly recommended that you consider using an appropriate analytical balance dependant upon your

accuracy requirements.

Top-loading balances can accurately measure the weight of components to 0.1 to 0.001 g depending on

which model top-loader you use. Some top-load balances have two ranges, low and high. Be sure to set

the balance range, if applicable, to the most accurate setting possible for each measurement.

10.3 Safety

Some substances are highly toxic, thus you must take certain precautions when weighing because you

are in close contact. If the danger is from inhalation, you should weigh under a laboratory hood. Only

use top loading balances under hoods; analytical balances should not be moved. Please contact the QA

Officer and you department Supervisor when moving balances.

It is imperative that proper cleaning procedures are used at all times after using balances. All artifacts

and/or liquids must be removed from on top and around the balance before and after use. This will

minimize your exposure and will also reduce the possibility of cross-contamination. If you have any

questions regarding how to clean a balance in cases of unknown substances, contact the QA Officer.

10.4 Containment

The choice of the container or device you use to weigh substances into is extremely important. You

must consider cross-contamination potential, capacity, alignment and appropriateness.

10.5 Cross-Contamination

One must consider what testing is being conducted and what analytes are being reported per preparation

or analytical event. For example, it is not appropriate to weigh samples requiring metals into a metal

pan or using plastic containers to weigh samples for EPA 8270 tests because of potential phthalate

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MEASURING

SECTION X REVISION 3 EFFECTIVE DATE 1/08/16 Page X-2

contamination. Consult your Department Supervisor to discuss good practices regarding this issue.

10.6 Capacity

Each container has a maximum capacity that is dependant upon the matrix of the material being

weighed, and the container geometry. It is important that there is 100% containment of the material

being weighed because the weight may be accurate, but the amount of the material used for testing may

not be accurate of there is spillage and because of safety issues. Please note that you should not

necessarily fill the container to capacity or exceed capacity because of the same issues discussed earlier.

10.7 Alignment

All weighing should take place in the middle of balance pans. Ensure that the pan is properly placed or

affixed to the balance before each use. Keep all materials away from the top or within balances to

reduce the probability of inaccurate weighing.

10.8 Appropriateness

Other than container capacity, appropriateness deals with other common sense issues regarding

containment choice. For example, containers with narrow orifices should not be used for relatively high

particle size components unless an appropriate funnel is used. Also, the container the material is being

weighed into should fit onto the pan, or top of the balance without contact with any other surfaces.

There are too many other scenarios not mentioned here, so please use common sense in your decisions.

10.9 Liquids Measuring

One must first consider accuracy, appropriateness and safety when deciding measuring techniques and

apparatus for volume measurements. Please refer to the Glassware section of this document for accuracy

and appropriateness issues. Again, use common sense when deciding how, what, when and where you

measure liquids. It is especially critical to know what you are drawing or pouring because you can

increase you chance of exposure if you use inappropriate measuring tools and improper PPE and

environmental controls.

10.10 Important Safety Practices

1. Always use a bulb to draw liquids

2. Check the compatibility of the liquid with the container

3. Check the capacity of the container and verify the amount you are measuring

4. Add acid to water, never water to acid

5. Properly clean glassware before and after use, do not flick liquid from containers

Note: Section X was reviewed on 01/08/16(No Changes were made)

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EPPENDORF PIPETTE CALIBRATION

SECTION XI REVISION 4 EFFECTIVE DATE 01/08/16 Page XI-1


It is necessary to verify micro liter pipette calibration prior to laboratory use. Tolerances are

established to provide accuracy goals. Pipettes that do not meet specifications listed in section 11.4

will not be used until deemed acceptable and in good working order.


Calibration of pipettes will be conducted through gravimetric testing. Testing will be done by

weighing a prescribed volume of di-ionized water on a sufficiently sensitive analytical balance.


11.3.1 Eppendorf Unipipettes 10 µl

20 µl

50 µl

100 µl

200 µl

500 µl

1000 µl

5000

11.3.2 ASTM Type II water

11.3.3 Analytical Balance

11.3.4 Digital Thermometer

11.4 Procedure

11.4.1 Test Room (Room # 15)

11.4.2 Use balance #8 in Room 15 weighing within 0.0001g

11.4.3 Use Digital Thermometer # 158 in Room 15

11.4.4 The test room should have a constant temperature between 15°C and 30°C at a constant

temperature of ±0.5C. (according to EN ISO 8655)

11.5 Temperature differences

11.5.1 Before the test, the device to be tested and test liquid must have stood in the test room for a

sufficient amount of time, at least 2 hours, in order to reach equilibrium with the storage

conditions

11.5.2 Take five separate weighing at each calibration volumes (see Form 2)

11.5.3 The color of the control button usually indicates the color of the appropriate pipette tip.

Volumes less than or equal to 10 µl should be rinsed from an unwetted pipette tip. If

volumes are > 10 µl, it is recommended that water be aspirated and dispensed two or three

times when a new pipette tip is used. Important: The Laboratory water, weighing vessel,

pipette tips, and pipette must have reached the same temperature prior to calibration.

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11.5.4 First secure the pipette to be calibrated. You will need a supply of ASTM Type II water, a

vessel, and an analytical balance. Weigh the vessel, preferably a two ounce plastic cup, on

the analytical balance. Record the weight of the vessel. Now attach a pipette tip tightly (pay

attention to the color code). Press control button down to first stop (measuring stroke).

Hold pipette vertically and immerse tip approximately 3 mm, release control button slowly.

Slide tip out of the water along the inside of the container. Wipe any droplets with lint-free

tissue. Ensure that no liquid is aspirated out of the tip. Hold the tip at an angle against the

inside of the weighed vessel. Press the control button slowly down to the first stop

(measuring stroke) and wait approximately 1-3 seconds.

11.5.5 Press down to the second stop to empty tip completely. Hold down control button and slide

tip up against the inside of the weighed vessel. Weigh and record new vessel weight.

Subtract initial weight from the final weight to measure uncorrected volume dispensed. Five

measurements are sufficient for accuracy control of initial use. To calculate volumes, divide

the weight of the water measurements by its density at 20°C: 0.9982. For daily use, conduct

1 measurement. Record micro liter calibration in a log along with the date of calibration.

11.6 Compliance Tolerance Limits

Eppendorf Series 2000 and Finnepipette Fixed Volume

Volume Inaccuracy Imprecision Inaccuracy(±µl) Imprecision

5 µl ±2% 1% 0.1 0.05

10 µl ±2% 1% 0.2 0.10

20 µl ±2% 1% 0.4 0.2

50 µl ±2% 1% 1.0 0.5

100 µl ±2% 1% 2.0 1.0

200 µL ±2% 1% 4.0 2.0

500 µl ±2% 1% 10.0 5.0

1000 µl ±2% 1% 20.0 10.0

2000 µl ±2% 1% 40.0 20.0

5000 µL ±2% 1% 100.0 50.0

Please refer to the following tables for recommended ranges. Weights consistently outside the

recommended range should initiate corrective procedures. If a micro-pipette is not in good

working order or not in calibration, please submit the pipette to the QA/QC Department. It is

imperative that incompliant pipettes are not in use.

11.7 Documentation

Gravimetric checks are to be documented on respective prep log and/or run logs. Accuracy

verified ± 2%

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11.8 References

Eppendorf Micro – pipette Series 2000 Reference Fixed – Volume and Finnepipette instruction manuals.

Eppendorf Series 2000 Reference Fixed – Volume pipette. Tests carried out in accordance with

Piston pipettes ISO 8655-2:2002.

Temp. °C-Water Temp 15°C and 30°C, constant to ± 0.5°C

Using ASTM Type II Water

Cal of Eppendorf Acceptance Criteria

Weight of Verified at ±2%

20 µL 0.0196 – 0.0204

50 µL 0.049-0.051

100 µL 0.098-0.102

200 µL 0.196-0.204

500 µL 0.490-0.510

1.0 mL 0.980-1.020

5 ml 4.900-5.100

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TABLE OF STUDENT’S T VALUES AT THE 99% CONFIDENCE LEVEL

SECTION XII REVISION 4 EFFECTIVE DATE 01/08/16 Page XII-1


The MDL for an analytical procedure may vary as a function of sample type. The procedure

requires a complete, specific, well-defined analytical method. It is essential that all sample-

processing steps of the analytical method be included in the determination of the method detection

limit. The MDL obtained by this procedure is used to judge the significance of a single

measurement of a future sample. The MDL procedure was designed for applicability to a broad

variety of physical and chemical methods. To accomplish this, the procedure was made device-or-

instrument independent.


The Method Detection Limit is defined as the minimum concentration of a substance that can be

identified, measured and reported with 99% confidence that the analyte concentration is greater

than zero and determined from analysis of a sample in a given matrix containing analyte. Initially

the method utilizes a series of ways to estimate the detection limit; then using statistical

justification, the procedure verifies the reasonableness of the estimated MDL.

12.3 Required Apparatus and Materials

All instruments requiring MDL and IDL determinations and acceptable precision and accuracy

ranges. Calculators with statistical packages will be helpful. A table of student’s t values or a

table of normal values will be needed where applicable.

Instrument parameters - parameters will be set at routine analysis settings. MDLs may be

determined at practical concentrations thus not adhering to extreme constraints. Determinations

for pH and EC are examples of MDL=PQL.

12.4 Reagents and Standards

Reagents will be made up with high purity water and reagent grade chemicals. Standards will be

made up with high purity water and reagent grade chemicals with special emphasis on matching

matrices with samples used in the determination of MDLs of respective analyses.

Working standards – standards used will be made up with high purity water or treated water for

specific tests (i.e. Organic free water). Standard stock sources include manufactured and in-house

reagent grade standards. Matrix matching between samples and standards is essential for proper

determination of MDLs for each respective analysis. Special attention should be placed on the

linearity of the standard curve. The correlation of coefficient or (r) should be >=.995 but emphasis

should be placed on the lower end of the curve where MDL detections will be quantified. You

should check for a change in slope at the detection level.

Spikes – samples used for the determination of MDLs will be spiked at:

The concentration value that corresponds to an instrument signal/noise ration in the range

of 2.5 to 5. If the criteria for qualitative identification of the analyte is based upon pattern

recognition techniques, the least abundant signal necessary to achieve identification must

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be considered in making the estimate, or

The concentration value that corresponds to three times the standard deviation of replicate

instrumental measurements for the analyte in reagent water, or

The concentration value that corresponds to the region of the standard curve where there

is a significant change in sensitivity at low analyte concentrations (i.e. a break in the slope

of the standard curve), or

The concentration value that corresponds to known instrumental limitations.

It is recognized that the experience of the analyst is important to this process.

12.5 General MDL/PQL Procedure

12.5.1. Prepare reagent (blank) water that is free of analyte as possible. Reagent or interference

free water is defined as a water sample in which analyte and interferant concentrations are

not detected at the method detection limit of each analyte of interest. Interferences are

defined as systematic errors in the measured analytical signal of an established procedure

caused by the presence of interfering species (interferant). The interferant concentration is

presupposed to be normally distributed in representative samples of a given matrix.

12.5.2. If an MDL is to be determined in reagent water (blank), prepare a laboratory standard

(analyte in reagent water) at a concentration which is at least equal to or in the same

concentration range as the estimated MDL (recommended between 1 and 5 times the

estimated MDL). Proceed to step 12.5.6.

12.5.3. If the MDL is to be determined in another sample matrix, analyze the sample. If the

measured level of the analyte is in the recommended range of 1 to 5 times the MDL,

proceed to step 12.5.6.

12.5.4. If the measured concentration of analyte is less than the estimated MDL, add a known

amount of analyte to bring the concentration of analyte to between 1 and 5 times the MDL.

In the case where an interference is co-analyzed with the analyte.

12.5.5. If the measured level of analyte is greater than 5 times the estimated MDL, there are two

options:

12.5.5.1 Obtain another sample of lower level of analyte in the same matrix if

possible.

12.5.5.2 The sample may be used as is for determining the MDL if the analyte level

does not exceed 10 times the MDL of analyte in reagent water. The variance

of the analytical method changes as the analyte concentration increases from

the MDL, hence the MDL determined under these circumstances may not

truly reflect method variance at lower analyte concentrations.

12.5.6 Take a minimum of seven aliquots of the sample to be used to calculate the MDL and

process each through the entire analytical method. Make all computations according to the

defined method with final results in the method reporting units. If blank measurements are

required to calculate the measured level of analyte, obtain separate blank measurements for

each sample aliquot analyzed. The average blank measurement is subtracted from the

respective sample measurements.

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12.5.7 It may be economically desirable to evaluate the estimated MDL before proceeding. This

will: (1) prevent repeating this entire procedure when the costs of analyses are high and (2)

insure that the procedure is being conducted at the correct concentration. It is quite

possible that an incorrect MDL can be calculated from data obtained as many times the real

MDL even through the background concentration of analyte is less than 5 times the

calculated MDL. To insure that the estimate of the MDL is a good estimate, it is necessary

to determine that a lower concentration of analyte will not result in a significantly lower

MDL. Take two aliquots of the sample to be used to calculate the MDL and process each

through the entire method, including blank measurements as described above in 12.5.6.

Evaluate this data:

12.5.7.1 If these measurements indicate the sample is in the desirable range for

determining the MDL, take five additional aliquots and proceed. Use all

seven measurements to calculate the MDL.

12.5.7.2 If these measurements indicate the sample is not in the correct range, re-

estimate the MDL, obtain new sample as in 12.5.5 and repeat either 12.2.6

or 12.5.7.

12.5.8 Reporting - the analytical method used must be specifically identified by number or title

and the MDL for each analyte expressed in the appropriate method reporting units. If

the analytical method permits options which affect the method detection limit, these

conditions must be specified with the MDL value. The sample matrix used to determine

the MDL must also be identified with the MDL value. Report the mean analyte level

with the MDL. If a laboratory standard or a sample that contained a known amount of

analyte was used for this determination, report the mean recovery, and indicate if the

MDL determination was iterated.

12.5.9 If the level of the analyte in the sample matrix exceeds 10 times the MDL of the analyte

in reagent, do not report a value for the MDL. PQL values are calculated by multiplying

the standard deviation obtained through MDL studies by 5 – 10, then rounded up to a

number with 1’s, 2’s or 5’s.

12.6 Procedures by Test

ICP/AA/GFAA/Hydride/ICP-MS

Spike reagent water at levels outlined in Section 12.5.

Dissolved Metals: Analyze at least seven (7) low levels spikes (without digestion), on three non-

consecutive days.

Total Metals: Digest at least seven (7) low level spikes. Analyze the digested spikes.

Obtain standard deviation and mean of low level spikes. The mean should agree with the true value of

appropriate student’s t value to obtain the MDL. Multiply the standard deviation by ten (10) and round

up to the nearest 1, 2, or 5 to obtain the PQL.

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Hg by Cold Vapor

Spike reagent water at the current PQL level. In this case, spike at the established PQL level of 0.08

g/L for PQL determination. Analyze at least seven (7) low level spikes.

known value of the low level spike. Multiply the standard deviation by the appropriate student’s t

value to obtain the MDL. Multiply the standard deviation by ten (10) and round up to the nearest 1, 2,

or 5 to obtain the PQL.

The MDL can be determined by continuously spiking low level standards lower and lower until the

spike recovery is not discernable from the baseline or the method blank.

Autoanalyzer Analytes

If conducting a PQL/MDL study for the first time, spike reagent water at levels outline in Section

12.5.2. Otherwise, use the current respective method MDL=s as the spike levels. Analyze at least

seven low level spikes.

Obtain the standard deviation and mean of the low level spikes. The mean should be 10% of the

known value of the low level spike. Multiply the standard deviation by ten (10) and round up to the

nearest 1, 2, or 5 to obtain the PQL.

The MDL can be determined by continuously spiking low level standards lower and lower until the

spike recovery is not discernable from the baseline.

pH, EC

PQL=s and MDL=s for these individual tests will be defined the same. MDL=s are established by the

manufacturer.

Gravimetric Procedures

The MDL will be based on the sensitivity of the balance used for analysis. Generally, the spike level

should be such that the net weight is 1 mg otherwise spike reagent water at levels outlined in Section

12.5.2. If new PQL is to be established, analyze seven (7) reagent blanks, then compute the spike level

based on the three times the standard deviation of the reagent blank.

Obtain the standard deviation and mean of the low level spikes. The mean

known value of the low level spike. Multiply the standard deviation by ten (10) and round up to the

nearest 1, 2, or 5 to obtain the PQL.

Gas Chromatography and GC/MS

Spike reagent water at levels outlined in Section 12.5.2. Analyze at least seven (7) low level spikes.

Compute the standard deviation of the low level spikes. Multiply the standard deviation by the

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corresponding 99% Confidence Level Student=s t value for n-1 degrees of freedom to find the MDL.

Compute the mean recovery for the low level spikes. The mean must be 65-135% of the known value,

unless the department supervisor approves differently. Multiply the standard deviation five to ten

times and round to the nearest 1, 2, or 5 to find the PQL.

Digital Spectrometer Techniques

Spike reagent water at levels outlined in Section 12.5.2. Analyze at least (7) low level spikes.

Compute the standard deviation of the low level spikes. Multiply the standard deviation by the

corresponding 99% Confidence Level Student=s t value for n-1 degrees of freedom to find the MDL.

Compute the mean recovery for the low level spikes. The mean must be 80-120% of the known value.

Multiply the standard deviation five to ten times and round to the nearest 1, 2, or 5 to find the PQL.

12.7 Detection Limits for Soil Matrix

Follow procedures outlined in earlier sections except substitute sand or inert solid for reagent water.

12.8 PQL Deviations

In all cases PQLs can be arbitrarily set above official PQL findings. Reasons for this policy are: 1) to

accommodate routine reporting, 2) eliminate uncertainty in regards to matrix interferences and 3)

provide for reporting a PQL achievable based on true instrument limitations.

12.9 Documentation, Approval and Reporting

Record MDL studies on either or the forms on pages XII-8 or XII-9, or on a spreadsheet. If you choose

to use a spreadsheet, please include all data which is found on the following pages. Submit a copy of

your documentation and a copy of the raw data to your department supervisor for approval. The

department supervisor will review the data and the findings and then approve, if appropriate, by

signing report form or spreadsheet. The data will be submitted to the QA Officer. A copy of data will

be submitted to the laboratory coordinator to enter the MDL(s) and into the LIMS. The LIMS print out

is submitted to the QA Officer for review.

12.10 References

Gaser, J.I.; Forest, D.I.; Mckee, G.d.; Quave, S.a.; Budde, W.I. Environ. Sci. Technol. 1981, 15, 1426-

1435.

Long, G.I.; Winefordner, J.D. Anal. Chem. 1983, 55, 721a-724a. Anal. Chem., 55, 2210-2218.

40 CFR Part 136, Appendix B.

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PQL/MDL DETERMINATIONS

Analyst:

Analyte:

Method:

Run Date:

Instrument ID:

Matrix:

Units:

Prep Date:

MDL Study No:

__/__/__-___________-____-________

DATE INSTR ID SEQ MATRIX

NO (W,S)

Analyst:

Analyte:

Method:

Run Date:

Instrument ID:

Matrix:

Units:

Prep Date:

MDL Study No:

__/__/__-___________-____-________


NO (W,S)

Analyst:

Analyte:

Method:

Run Date:

Instrument ID:

Matrix:

Units:

Prep Date:

MDL Study No:

__/__/__-___________-____-________


NO (W,S)

MDL Std. ID

Conc.

Response

MDL Std. ID

Conc.

Response

MDL Std. ID

Conc.

Response

1

1

1

2

2

2

3

3

3

4

4

4

5

5

5

6

6

6

7

7

7

MDL Std Concentration:

_

x = s = 3.29(s) =

t(n-1, .99)s= MDL =

10s = PQL =


_

x = s = 3.29(s) =

t(n-1, .99)s= MDL =

10s = PQL =


_

x = s = 3.29(s) =

t(n-1, .99)s= MDL =

10s = PQL =

Standard Curve r= r2=



1st Order

2nd Order

3rd Order

1st Order

2nd Order

3rd Order

1st Order

2nd Order

3rd Order

Stand. ID

Conc.

Response

Stand. ID

Conc.

Response

Stand. ID

Conc.

Response

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MDL/PQL DETERMINATIONS

Analyte: Study No: Std Concentration Used:

_

x = s = 3.29(s) =

t(n-1, .99)s= t(n-1, .99)=

10s =

Dates: Run No. 1

Run No. 2

Run No. 3

Analyst: Blank Response Data:

_

x = s = 3.29(s) =

3s =

10s=

Instrument:

Method:

Matrix:

Units: STANDARD CURVE

Standard ID Conc. Response

Instrument Parameters:

Standard Calibration Setting:

Flowcell Length: 1st Order 2nd Order 3rd Order

Program Method ID: Correlation Coefficient:

Date of Preparation: PQL: MDL:

Run No. 1 Run No. 2

MDL STD. ID RESPONSE CONC. MDL STD. ID RESPONSE CONC.

1. 1.

2. 2.

3. 3.

4. 4.

5. 5.

6. 6.

7 7

8 8

Run No. 3 Blank Determination

MDL STD. ID RESPONSE CONC. BLANK ID RESPONSE CONC.

1. 1.

2. 2.

3. 3.

4. 4.

5. 5.

6 6

7 7

8 8

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Number of Degrees of

Replicates Freedom (n-1) t(n-1, 1- =.99)

7 6 3.143

8 7 2.998

9 8 2.896

10 9 2.821

12 10 2.764

16 15 2.602

21 20 2.528

26 25 2.485

31 30 2.457

60 60 2.390

2.326

Note: Section XII was reviewed on 01/08/16(No Changes were made)

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REPORTING

SECTION XIII REVISION 4 EFFECTIVE DATE 01/08/16 Page XIII-1

Reporting

It is extremely important to properly report data onto worksheets. Reported values must be technically

valid and accurate. The accuracy of the reported data will depend upon the analytical process and the

mathematical manipulations used to reduce data. The technical validity of the data depends on the

assessment of the QC parameters and thus will depend on the accuracy of the flagging or qualifying

process.

13.1 Reporting Procedures for Qualified Data

13.1.1 Holding time exceeded – If holding times are exceeded, qualify results as estimated. Add a

comment to the final report and/or other pertinent deliverables which explain the qualifier.

13.1.2 GC/MS Initial Calibration Incompliance – If %RSD is greater than 30.0% and the initial

calibration RRFs greater than or equal to 0.05, qualify positive results as estimated, and non-

detected target compounds using professional judgment. If any calibration RRF is less than

0.05, qualify positive results that have acceptable mass spectral identification as estimated

and non-detected analytes as unusable.

13.1.3 GC/MS Continuing Calibration Incompliance – If the %D is outside +20.0% criterion and

the continuing calibration RRF is greater than or equal to 0.05, qualify positive results as

estimated. If the %D is outside +20.0% criterion and the continuing calibration RRF is

greater than or equal to 0.05:

Qualify non-detect target compounds as estimated if –20%.

Do not qualify non-detect target compounds if +20%.

13.1.4 Blanks Incompliance – If a compounds is detected in the sample and in the blank, the sample

result is qualified if the sample concentration is less than ten (10) times the associated PQL.

Report method blank bias for associated sample concentrations >10 respective PQLs.

Results must not be corrected by subtracting any blank value, unless method references state

otherwise.

13.1.5 Surrogate Incompliance – If a surrogate has a recovery greater than the upper acceptance

limit, detected target compounds are qualified while results for non-detected target

compounds should not be qualified. If a surrogate has a recovery greater than or equal to

10% but less than the lower acceptance limit, detected target compounds are qualified while

non-detected compounds quantitation limits are qualified as approximate. If surrogate

recovery is less than 10% and less than the lower acceptance limit, detected compounds are

qualified and non-detected target compounds may be qualified as unusable.

13.1.6 Matrix Spike/Matrix Spike Duplicate Incompliance – No action is taken on MS/MSD data

alone unless informed professional judgment is used in conjunction with other QC criteria.

13.1.7 Laboratory Control Samples Incompliance – Action on the LCS recovery should be based on

both the number of compounds that are outside of the recovery and the magnitude of the

exceedance of the criteria. If the LCS recovery criteria are not met, then the LCS results

should be used to qualify samples data for the specific compounds that are in the LCS

solution. If the LCS recovery is greater than the UCL, then positive results for the particular

compounds should be qualified. If LCS compounds are below associated LCLs, then

affected results should be rated unusable. If more than half the compounds in the LCS are

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REPORTING


not within the required recovery criteria, then all of the associated detected target

compounds should be qualified unusable. Please note that the proximity of recoveries to

100% should be considered in assessment.

13.1.8 Internal Standard Incompliance – If an IS area count is outside –50% or +100% of the area

for associated standard, positive results for compounds quantitated using that IS should be

qualified, non-detected compounds quantitated using an IS area count greater than 100%

should not be qualified, non-detected compounds quantitated using an IS area count less than

50% are reported with an approximated quantitation limit.

13.1.9 Initial Calibration Incomplaince (GC) – If %RSD is greater than 20%, qualify all positive

results as estimated and use professional judgment is assessing non-detected target analytes.

13.1.10Continuing Calibration Incompliance – If % diff is greater than 15%, qualify positive results

as estimated. If % diff is less than –15%, qualify positive results as estimated and

approximate the non-detect target analytes quantitation limits.

13.1.11Initial Calibration Incompliance (Inorganics) – If the minimum number of standard were not

used for initial calibration, or if the instrument was not calibrated daily and each time the

instrument was set up, qualify the data as unusable. Please note that the Ion

Chromatography procedures mandate that an initial curve is validated by continuing

calibration checks. If the correlation coefficient is <0.995, qualify results as estimated.

13.1.12Continuing Calibration Incompliance (Inorganics) – If the CCV or ICV %R falls outside the

acceptance windows, use professional judgment to qualify all associated data.

13.1.13Interference Check Sample – For samples with concentration of Al, Fe, Ca, and Mg which

are comparable to or greater than their respective levels in the Interference Check Sample:

1. If the ICS recovery for an element is >120%, qualify detected results.

2. If the ICS recovery for an element falls between 50 and 79%, qualify detected and

non-detected results.

3. If ICS recovery results are <50%, qualify data as unusable.

13.1.14Duplicate Incompliance – If duplicate analysis results for a particular analyte fall outside the

appropriate control windows, qualify the results for that analyte in all associated samples of

the same matrix as estimated.

13.1.15Post Spike Incompliance – If sample absorbance is <50% of the post digestion spike

absorbance then:

1. If the post spike recovery is not within 85-125%, qualify results as estimated.

2. If method of standard additions is required but has not been done, qualify the sample

results as estimated.

3. If MSA spike levels are not appropriate, qualify data, and

4. If MSA correlation coefficient is <0.995, qualify data as estimated.

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REPORTING


13.2 Rounding Rules for Reporting Data

13.2.1 Significant figure and rounding rules for Inorganics analyses:

Values between Report to the nearest Example

0.00001 – 0.00099 0.00001 0.00075

0.001 – 0.00999… 0.0001 0.0010

0.01 – 0.0999… 0.001 0.053

0.1 – 0.999… 0.01 0.27

1.0 – 9.999… 0.1 7.3

10 – 99.9… 1 87

100 – 999.99… 1 562

1000 – 999.99… 10 6720

10000 – 99999.99… 100 15600

>100000 3 significant digits

All values are rounded to 2 significant digits until they get above 100 when they are rounded to 3

significant digits.

Rounding off numbers is the process of dropping digits that are not significant. In order to round off a

number to a particular place holder (for example, to the nearest 10) one looks at the next smallest place

holder (the 1’s place). If the next smallest place holder is a 6, 7, 8 or 9, then increase the preceding digit by

one and drop the digits to the right (if to the right of the decimal) or replace them with zeros (if to the left of

the decimal). If the next smallest place holder is a 1, 2, 3 or 4, then do not change the preceding digit and

drop the digits to the right or replace with zeros. If the next smallest place holder is a 5 and any number to

the right of the 5 is not zero, then treat it as 6, 7, 8 or 9 as above. If the next smallest place holder is a 5 and

all digits to the right of this digit are zero, then round the preceding digit to the nearest even number (0, 2,

4, 6, 8) and drop the digits to the right or replace with zeros. Thus, 2.250001 becomes 2.3 and 2.250000

becomes 2.2, and 6.750 becomes 6.8.

When rounding values, do not round off values that have been previously rounded. In other words, do not

round off during a preliminary calculation. Carry as many digits as possible until the final value has been

calculated and then round off as needed.

13.2.2 Significant figure and rounding rules for organics analyses:

Two significant figures are used as a rule for organics. Rounding rules are the same as for inorganics

testing.

13.3 Quality Control Parameter Evaluation

Before evaluating a number for being in control or out of control of a certain limit, the number evaluated

must be rounded using EPA rounding rules to the significance reported for that limit. For instance, the

control limit for an ICV is plus or minus 10% of the true value. A reported percent recovery value of 120.4

would be considered in control while a reported value of 120.6 would be considered out of control. In

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REPORTING


addition, a calculated value of 120.50 would be in control while a calculated value of 120.51 would be out

of control.

13.4 Low Level Reporting

“Reliable analytical measurements of environmental samples are an essential ingredient of sound decisions

involving many facets of society including safeguarding the public health, improving the quality of the

environment, and facilitating advances in technology”. Analytical objectives for environmental samples

typically require reliable measurements at part per billion levels. At these levels, it is important to properly

evaluate the significance and reliability of results at or near the detection and quantitation limits. In order to

properly assess the reliability of low level results, one must have a working knowledge of analytical

techniques, EPA method protocols and procedures, statistics and environmental regulations.

Our laboratory uses the terms MDL and PQL for reporting the sensitivity of particular methods or analyses.

Definitions

MDL: The minimum concentration of a substance that can be measured and reported with a 99%

confidence that the analyte concentration is greater than zero and is determined from analysis of a

sample in a given matrix containing the analyte. Operationally the same as the Limit of Detection

(LOD).

PQL: The lowest level that can be reliably achieved within specified limits of precision and accuracy

during routine laboratory operating conditions. Operationally the same as the Limit of Quantitation

(LOQ).

MDLs are determined using the procedures outlined in 40 CFR Part 136 Appendix B. PQLs are then

determined by the procedure listed in the “Principles of Environmental Analysis” and/or are determined

using the expertise of BC Laboratories, Inc’ analysts and chemists. When setting PQLs, analysts must

consider meeting precision and accuracy goals as set in referenced methods.

Excerpts from the “Principles of Environmental Analysis”, Analytical Chemistry, Volume 55, Pages

2210 - 2218, Dec. 1983

Table I. Guidelines for Reporting Data

Analyte Concn. in units of (S(t) - S(b)

<3 region of questionable detection(and therefore

unacceptable)

3 limit of detection(LOD)

3 to 10 region of less-certain quantitation

10 limit of quantitation(LOQ)

>10 region of quantitation

: Represents the standard deviation of replicate low level standards and blanks.

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REPORTING


±3 ±3

Region of HighUncertainty

Region of LessCertain

Quantitation

Region ofQuantitation

Total Signal

(S(t))

Zero PQL/LOQMDL/LOD

-3 -2 -1 0 1 2 3 4 5 6 7 8 10 11 12 13 14S(b)

9

(S(b) +3 ) (S(b) + 10)

“Signals below 3 should be reported as “not detected”(ND)” ....”Signals in the region of less-certain

quantitation (3 to 10) should be reported as detections with the limit of detection given in parenthesis.“

“... Data measured at or near the limit of detection have two problems. The uncertainty can approach and

even equal the reported value. Furthermore, confirmation of the species reported is virtually impossible;

hence the identification must depend solely on the selectivity of the methodology and knowledge of the

absence of possible interferents. These problems diminish when measurable amounts of analytes are

present. Accordingly, quantitative interpretation, decision-making, and regulatory actions should be

limited to data at or above the limit of quantitation. “.

Excerpt from Standard Methods for the Examination of Water and Wastewater 19th edition, 1995,

page 1-12.

The practical quantitation limit (PQL) has been proposed as the lowest level achievable among laboratories

within specified limits during routine laboratory operations. The PQL is significant because different

laboratories will produce different MDLs even though using the same analytical procedures,

instruments and sample matrices.

The curve labeled B is representative of the background or blank signal distribution. As Shown, the

distribution of the blank signals is nearly as broad as for the other distributions, that is (B) = (I) = (L).

As blank analyses continue, this curve will become narrower because of increased degrees of freedom. The

curve labeled I represents the IDL. Its average value is located k(B) units distant from the blank curve,

and k represents the value of t (from the one-sided t distribution) that corresponds to the confidence level

chosen to describe instrument performance. The overlap of the B and I curves indicates the probability of

not detecting a constituent when it is present (Type II error). The curve at the extreme right represents the

LLD. Because only a finite number of determinations are used for calculating the IDL and LLD, the curves

are broader than the blank, but are similar, so it is reasonable to choose (I) = (L). Therefore, the LLD is

k(I) + k(L) = 2k(l) from the blank curve.

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REPORTING


B I L

+kr(b) -kr(l) +kr(l)

Detection limit relationship

Comments

Please note in order for these statements to be considered valid, the variability of blank responses must

equal the variability of the low level standards used to compute MDLs. Since this is not always

determined, the MDL can be statistically computed low, thus widening the level of uncertainty between the

MDL and PQL.

In practice, an indication of whether an analyte is detected by an instrument is sometimes based on the

extent to which the analyte signal exceeds peak-to-peak noise. The question of a given analyte is often one

of the most important decisions in low-level analysis. The question which must be answered is whether a

measured value is significantly different from that found for the sample blank.

References

40 CFR Part 136 Appendix B

Long, G.L.; Winefordner, J.D. Anal. Chem. 1983, 55, 712A-724A

Revision to “Guidelines for Data Acquisition and Data Quality Evaluation in Environmental Chemistry”

Anal. chem. 1980, 52, 2242-2249, Reprinted from Anal. Chem, 1983 Vol. 55,

13.5 Manual Integration

Instrument software applications for chromatographic analyses allows for automated integration of analyte

peaks. Automated integration does not work 100% time due to many reasons, thus it is necessary to

conduct manual integrations. The following section deals with general integration practices.

13.6 Manual Integration Labeling

Manual integrations must be flagged, initialed and dated by analysts. Typically the instrument software will

automatically label manual integrations with an “m” or indicate change in quantitations by flagging

chromatograms “reprocessed”. A good laboratory practice is to be more descriptive in the labeling practice

of manual integrations. Analysts should use the following list of integration flags:

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M Manual integration due to irregular peak shape

MS Manual integration due to split peak

MR Manual integration due to retention time shift

MI Manual integration of correct isomer or peak

MT Manual integration due to peak tailing

MB Manual integration due to irregular baseline

1. All lone > or = to 90% baseline resolved peaks are to be integrated valley to valley

2. All peaks with adjacent peaks <90% resolved must be integrated baseline to

baseline; dropping a perpendicular at the minimum.

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REPORTING


3. All peaks with shoulders will be integrated in the beat manner possible.

Analysts' judgement. (Tangential skim or Perpendicular drop)

4. In a busy chromatogram, the analysts' judgement, subject to approval, as to

the best integration technique will supercede techniques 1 through 3.

5. All Manual re-integrations are printed and reviewed during the technical

review process. All controversial integrations (technique is not agreeable to both

the analyst and technical reviewer) must be approved by the department

supervisor.

6. Manual integrations are documented by the software being used. HP

Chemstation places an "m" by each peak that was manually integrated. The

Dionex software states that the run was reprocessed and the date upon which the

reprocessing occurred.

7. Be consistent between integrating standard peaks and like peaks in samples.

8. No peak shaving is to be observed or practiced.

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13.7 Manual Integration Discussion

When manual integrations are performed, raw data records include a quantitation report. A

quantitation report shows the results of manual integration labeled with “m” chromatograms of

manually integrated peaks. Each quantitation report is printed with date, time and initial of person

performing the manual integration. For Navy project, a case narrative will be provided with an

analytical report. A case narrative shall include all data qualifiers of flags. All samples and analytes

for which manual integration occurred, will be discussed in the case narrative under discussion, (i.e.

case narrative).

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Note: Section XII was reviewed on 01/08/16 (No Changes were made)

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AUDIT HANDLING PROCEDURES

SECTION XIV REVISION 6 EFFECTIVE DATE 01/08/16 Page XIV-1


The purpose of this operating procedure is to document the steps taken to conduct, receive, and/or report

results regarding internal and external Performance Evaluation (PE) samples.


Internal Audits (PE) samples– the QA/QC Department prepares audit samples purchased from Absolute

Standards and ERA. These samples are submitted to the Log-In Department. Chain-of-custody is prepared

to accompany batch of samples received.

Received Audits – the QA Officer examines the submitted audit for any irregularities regarding sample

containment or analysis requirements. The audit is then placed into the sample flow. Data review is

conducted by responsible supervisors before submitted to the QA Officer. The QA Officer reviews the data

and records the completed results onto Vendors Website.


Apparatus

Volumetric flasks (various volumes)

Volumetric pipettes (various deliveries)

Micro-pipettes (variable)

Sample containers (plastic and glass)

14.4 Reagents and Standard Solutions

Reagents – Name and Source

Organic free water – located in the AA room near the nanopure water system.

Nitric acid – located in the bottle preparation room. Use the acid for preserving metals.

Sulfuric acid – located in the bottle preparation room.

Hydrochloric acid – located in the bottle preparation room.

All preservatives are made from reagent acid stocks. A log is kept, by the Bottle Prep. Dept., that

includes information on preservative preparation.

14.5 Solution Preparation

The directions for standard audit (PE) samples preparations should be followed; however, if a

decision is made to alter sample dilution, this should be documented at the time of preparation.

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14.6 Working Standards

Internal audit standards proficiency testing are purchased from:

Absolute Standards ERA Sigma-Aldrich

P.O. Box 5585 6000 W. 54th

Street 2931 Soldier Springs Road

Hamden, CT 06518-0585 Arvada, CO 80002 Laramie, WY 82070

(800) 368-1231 (800) 372-0122 (800) 576-5690

www.Absolutestandards.com (303) 421-0159 Fax www.RT-Corp.com

www.eraqc.com

14.7 Sample Collection, Preservation and Handling

Audit samples should be prepared as soon as possible. If this is not practical, store samples or

ampuls according to specifications included in respective preparation method instructions.

Preserve audit solutions according to method preparation instructions, and/or laboratory guidelines.

Handle concentrated ampul solutions with care. Read associated MSDS sheets for more

information on safe handling of each material.

When analyses are completed, discard samples and remaining ampul contents according to

laboratory waste disposal protocols.

14.8 Procedure

14.8.1 Internal Audits (conducted by the QA/QC Dept.)

Purchase audit samples from ERA and Absolute Standards of an as needed basis. When the

audits samples arrive, prepare and process them immediately. If this cannot be done, store

the samples inside the walk-in refrigerator. Follow preparation procedures and fill out

chain-of-custody forms under fictitious client identifications. Document these sample

identifications and notify the billing department of the audit samples so they are not billed.

The most anonymous method of submitting samples is to pack the sample batch into an ice

chest or box. Then leave it overnight in the walk-in refrigerator. The samples will be

logged in the following morning. When analyses are completed, retrieve data and report on

vendor website. Process the results in report form as part of the quarterly report to upper

management. Process an unacceptable results open SIF section that includes: sample IDs,

methods, analytes, reasons or cause for discrepancies, and corrective action.

14.8.2 External Audits

Examine all aspects of sample condition when the audit arrives. If any discrepancies are

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found, contact the responsible parties for further instruction or action. After examination of

samples and instructions, initiate the analytical process. Review all pertinent raw data after

respective supervisor validations. If any discrepancies are found, allow the responsible

supervisor to correct the problem. When all data is acceptable and complete, hand in the

data package to the Data Control Department. Review of data transferal is conducted by the

Data Control Supervisor.

14.9 Forms

Preparation Forms

Sample Constituency Forms

Analyte Concentrations Reports

Chain-of-Custody

14.10 Safety

Follow any precautions listed in the MSDS associated for each sample. Always wear a lab coat,

gloves and safety glasses.

Note: Section XIV was reviewed on 01/08/16(No Changes were made)

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TECHNICAL REVIEWS

SECTION XV REVISION 4 EFFECTIVE DATE 01/08/16 Page XV-1


This section describes the process by which the technical review of analytical data is carried out

throughout the lab.


Upon completion of a test method, each individual analyst reviews all parameters governing the

acceptability and correctness of the data generated. (Quality control, calculations, method protocols,

holding time, and reasonableness of data.) A second level 100% technical review is carried out by a

qualified peer which is a repeat of the first level of review plus the review of the raw data. A third

level of review, typically by department supervisor, is carried out to ensure completeness, QC

control, protocols, and reasonableness of data.

When a peer is either absent of extremely busy, the back-up reviewer will be assigned review duties.

15.3 Materials

Indelible ink pen

All raw data and worksheets associated with a given run

Quality control criteria

Technical review sheet

15.4 Procedure

Preparation task reviews – all extraction and preparation tasks must be reviewed and approved.

Technical reviews should be conducted by qualified personnel. Reviewed parameters should

include:

Sample numbering

Reagents

Standards

Proper documentation

Data entry into the LIMS

Review completion is verified in the LIMS and via initials on either preparation logs or review

sheets. Refer to the appropriate processing SOP for more details.

Upon completion of testing, the first level of review takes place. The first level of review entails

checking all quality control parameters, calibration, blanks accuracy and precision. All calculations,

identifications, method protocols and holding times are also checked at this time. The analyst who

performed the analyses conducts this first level of review. All sample preparation reviews are

conducted by person(s) not directly associated with the task of concern.

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TECHNICAL REVIEWS

SECTION XV REVISION 4 EFFECTIVE DATE 01/08/16 Page XV-2

A second level 100% technical review must take place within 24 hours following the first review or

before the data is submitted to our clients. All raw data as well as a technical review sheet are given

to the assigned reviewer. The reviewer is a qualified peer who has conducted the analyses he/she is

reviewing.

The second level of review contains all the elements of the first review plus a review of the raw

data. Review sheets for specific tests have been constructed in order to guide and maintain a record

of all such 100% technical reviews.

If upon review a problem/mistake is found, the analyst who performed the testing is approached to

correct the matter. The problem is noted on the review sheet and the analyst signs and dates the

review sheet as to his acceptance of any changes or problems.

The raw data and worksheets are returned to the analyst who files the raw data according to protocol

and turns in the worksheets as well as review sheets for final review by his/her supervisor.

Each department supervisor conducts the third level of review. This review entails checking QC

controls and protocols and reasonableness of the data. All comments and qualifying flags are also

reviewed and corrected as required.

A fourth level of review is completed by the Quality Assurance Department if QC reporting is

required. The QC review includes quality control acceptance, deliverables and possibly historical

trending.

15.5 Quality Control

Only indelible ink pen must be used to complete QC forms, data sheets, and technical review sheets.

If an error is made, a single line is drawn through it and the correction made. The correction must

be initialed and dated as to when the correction was made. There will be no obliterations.

In the event of an assigned reviewer being absent or extremely busy, a backup reviewer who is also

a qualified peer may be assigned review duties during their absence.

A qualified peer is:

1. An analyst/tech who has conducted the analysis and has passed the respective IDC,

2. A senior analyst who was responsible for the method at one time,

3. A team leader within his/her responsibility scope, or

4. A department supervisor within his/her responsibility scope.

Reviews will be monitored periodically by respective department supervisors and QA/QC

department personnel.

Note: Section XV was reviewed on 01/08/16(No Changes were made)

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CONTROL CHARTING

SECTION XVI REVISION 4 EFFECTIVE DATE 03/15/16 Page XVI-1

16.1 Introduction

A tool that is commonly used to monitor and control process variations on an ongoing basis is

control chart. Control charts are used to ensure that the process is in control and capable of

repeatedly meeting requirements. Control charts are based on the statistical theories of the normal

curve. By turning the normal curve 90°, the relationship between the normal curve and control

charts become more evident. The upper control limit represents +3 standard deviations from the

mean. The central line represents the mean and the lower control limit represents –3 standard

deviations from the mean. These lines representing +2 standard deviations from the means are

commonly called warning limits.

A process is in control when the following conditions are met:

All points on a control chart are within the control limits.

No patterns are formed by the points on the control chart. Patterns may be runs, cycles, trends and

so on.

When a process is out of control when any one of the following conditions exist.

Points exceed the upper or lower control limits.

Points within the control limits form a pattern.

One common pattern is a run. A run is a series of consecutive points that fall on one side of the

central line. Runs can be defined by any one of the following conditions:

Seven (7) consecutive points fall on one side of the central line.

Ten (10) of eleven (12) consecutive points fall on one side of the central line.

Twelve (12) of fourteen (14) consecutive points fall on one side of the central line.

A run indicates that the process mean has shifted or a change has occurred in the process. When

this occurs, the process should be investigated to identify and remove the cause of the changes.

Another common pattern is a trend. A trend is a steady progression of points in one direction. If a

trend continues, a point will eventually exceed control limits. Trends usually indicate equipment

wear, or standard/reagent degradation.

When patterns exist and/or points exceed control limits, a special or assignable cause of variation is

usually present.

16.2 Monitoring of LCSW

The Laboratory Control Sample Water is the QC spiked parameter of choice to be monitored

through control charting.

Charting of Multi-Analyte Methods – In cases where charting organic multi-analyte methods is not

feasible, a select subset of analytes should be identified and charted. Those analytes chosen should

represent the entire retention time range and must represent normal analytical activity or

performance (i.e., do not chart abnormally stable or unstable analytes).

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CONTROL CHARTING

SECTION XVI REVISION 4 EFFECTIVE DATE 03/15/16 Page XVI-2

16.3 Development of Control Charts

A minimum of 30 data points is required in order to administer statistical manipulations to a

particular QC parameter. Once at least thirty data points are obtained, the standard deviation and

mean of the data set can be calculated. The mean plus or minus two sigma will define warning

limits while the mean plus or minus three sigma will represent LCS control limits. Please contact

the QA Officer for guidance or for additional charting options.

16.4 Maintenance of Control Charts

16.4.1 Electronic Charting

Instrument data which is processed via Element, control limits are calculated by analyst

using QA admin in Element then select control charts. Recalculations of control limits shall

be monitored on an on-going basis (at least quarterly) for shifts in mean recovery, changes in

standard deviation, and development of trends. The recalculated limits should be submitted

to the QA/QC Department for LIMS updating.

16.5 Calculation Controls

It is important that control limits are properly calculated to correctly assessed control of the system

and to validate presence of interferences and bias.

General Rules

Include all recoveries unless outliers are validated.

If significant changes are made, reestablish control limits by initiating a new data set.

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CORRECTIVE ACTION/SYSTEM IMPROVEMENT

SECTION XVII REVISION 4 EFFECTIVE DATE 01/08/16 Page XVII-1

17.1 Introduction

It is inevitable that problems will be encountered. When these problems occur, it is imperative that

we prevent future similar mistakes by incorporating a corrective action program. Corrective action

is a process by which errors are corrected in such a way to prevent future errors of the same nature

or type. Corrective action should be systematic, documented and monitored.

System improvement is used to describe preemptive positive actions or process modifications that

increase the level of quality and customer satisfaction. This differs from corrective action.

Corrective action is reactive while system improvement is proactive.

17.2 When to Initiate

Corrective action should be initiated when:

1. A client requests

2. An out of control situation is detected on a control chart

3. An unacceptable result is found on a PE study

4. QC anomalies arise (see flow charts)

5. Significant process/procedural problems occur

6. Communication problems occur

7. Instruments fail

8. Persistent “minor” problems exist

9. Project specific anomalies occur

10. Reagent/equipment problems are detected

11. Problems are found associated with the LIMS

12. Procurement anomalies occur

13. Subcontractors do not perform to our standards

14. Policies conflict

System Improvement Forms can be initiated anytime you have a good idea. Please document

system improvement and corrective actions on SIFs.

17.3 DEFINITIONS

17.3.1 Corrective Action (CA)

A process by which a critical error is corrected in such a way as to prevent future errors of the same

nature or type.

Some examples of when to initiate corrective action:

S Calculation errors.

S Client Request.

S Out of control trend

S Significant QA/QC anomalies

S Unacceptable PE results.

S Poor curve linearity.

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S Dilution error (if sample is diluted).

S Equipment malfunction.

S Improper methodology for sample matrix.

S Contamination.

S Incorrect report formatting.

S Clerical discrepancies.

S Invoicing problems.

S Field service problems.

S Inherent or chronic problems with methodology.

17.3.2 Corrective Action Process

Corrective action steps for reporting and correcting problems for non conformance

measurement or instruments

1. Identify the problem: A problem must be identified in a clear and concise term.

2. Evaluation (Root Cause): A root cause of the problem must be determined to see whether the

problem is local or systematic.

3. Extent of Problem: Extent of the problem must be specific to the area of the problem; so that

it can be addressed appropriately.

4. Develop Action: Develop a through action plan to address the problem in question

5. Implementation of Corrective Action: A plan needs to be designed that reflect how this plan

was implemented that demonstrates the outcome of implementation.

6. Expected Completion Date: A problem expected completion date ought to be assigned

7. Evaluation of Effectiveness of Corrective Action: Develop a plan (test) to evaluate the

effectiveness of the corrective action

8. Criteria for Verification: A criteria needs to be set up in order to verify whether your action

was effective

9. Documentation: All Corrective Action must be documented for future reference

PROCESS

Please refer to Appendix D for background on initiation of analytically based corrective action.

Implement

Corrective

Action(s)

Demonstrate

correction of

the problem

Close the

corrective action

process

(documentation)

END

Identify what

went wrong

Identify the

root cause

Extent of

problem

Develop Action

Expected

Completion Date

Evaluate the

effectiveness of

Corrective Action

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SECTION XVII REVISION 4 EFFECTIVE DATE 01/08/16 Page XVII- 4

BC Laboratories Inc.

Customer Complain Form

Date: Filled out by:

Company Name: Contact Name:

Complain via: Affected Lab#/Invoice #:

Complaint:

TAT Courier Service Web Service/IT Other

Quality of Data Invoicing Issues Missed holding times Clerical

Customer Service Incorrect Tests/Methods Bottle Orders D.L’s

QC Issues (Flagging) Reporting Issues

Explanation of Customer Complaint:

Action Taken:

Reviewed by: Date::

(Management)

Reviewed by: Date::

(Authorized Signature)

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17.4 Determining the Root Cause

Quality problems can be the result of complex causes. Once a problem has been identified on a

process, the potential causes need to be determined before any corrective actions are taken.

The cause and effect diagram is one of the tools that can be used to identify all of the potential

causes. The cause and effect diagram is also used to describe the relationship between the various

causes and the effect (problem) on the process. The left side of the diagram lists the primary causes

the variation. This half of the diagram is the cause side. The right side of the diagram lists the

problem or quality characteristic to be improved. This half is the effect side. The major purpose of

the cause and effect diagram is to identify the relationships that exist between each of the various

causes and to determine their overall effect on the problem.

All things vary. That is, each result or item differs to some degree from the others produced by the

process. These differences are the result of various causes in the process. Causes of variation can be

categorized as common or assignable.

Common causes of variation result from normal events operating within the process. Common

causes cannot be eliminated entirely, but their effect on the quality of items can be controlled.

Assignable causes, on the other hand, are the result of abnormal or unnatural events in the process.

Assignable causes can be detected, corrected, and eliminated.

Common causes of variation are usually grouped into five major categories; people, machinery,

methods, materials, and environment.

People: Since every person is unique, individual performance and perceptions vary from one

person to the next. Even when established procedures are used to perform a specific task, no two

people perform tasks in the exact same manner. Given this, variation occurs as a result of the

people involved in the process.

Machinery (instrumentation): The performance of instrumentation and equipment used in

processes changes daily. These changes are due to mechanical functions, wear, calibration, and so

on. Variation naturally occurs as a result of equipment, instrumentation and so on.

Methods: On the surface, method of operation appears to be fairly consistent, yet differences exist.

These differences may occur between shifts, supervisors, pressures, location and so on. The

methods used in a process are based on interpretation. Various interpretations of methods affect the

variation of the process.

Materials: The basic composition and measurements of raw materials vary. In addition, the

materials delivered by various suppliers also vary. Therefore, the materials used in any process vary

to some degree.

Environment: The events that naturally make up the environment, such as organizational culture,

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management, humidity, temperature pollution and so on, all affect the variation in the process.

When these factors are combined in a process a certain level of variation will occur in the process.

These causes of variation are referred to as common cause variation, which cannot be entirely

eliminated.

In addition to common cause variation in the process, assignable causes may also be present.

Assignable causes of variation are the result of abnormal or unnatural events. Any factor outside the

realm of a common cause can be defined as an assignable cause.

Examples of assignable causes:

Environmental factors such as air conditioner breakdowns, power outages, or abnormally high

levels of pollution.

Measurement devices or gauge malfunctions.

Equipment malfunctions.

Whenever an attempt is made to condense or reduce the amount of time normally required to do a

job or perform a given task, variation in the process increases.

For the most part, both common and assignable causes of variation are present in all processes.

These combined levels of variation directly affect the quality of the items produced by the process.

The higher the level of variation, the poorer the quality. To improve quality, the variation of the

process must be monitored and controlled. Any assignable cause of variation should be eliminated

and common cause variation can be reduced by improving the process continuously.

The cause and effect diagram can be used to identify the causes of variation in the process. This

information allows you to identity the major causes of variation that can be controlled or eliminated.

The net effect of these efforts will enable you to reduce variation in the process and improve

quality.

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17.5 Constructing a Basic Cause-and-Effect Diagram

Step 1: Identify a problem or quality characteristic

Once a specific problem has been identified, draw a box on the right side of the paper and write the

problem in the box.

Step 2: Draw a line pointing to the problem identified

After one problem has been identified, draw a perpendicular horizontal line pointing to the problem.

Step 3: Determine the major causes of the problem

Identify the major causes of the problem that have been identified and list each major cause in a box

around the main line. Then draw an arrow pointing toward the main line.

Step 4: Determine the minor causes of the problem

Minor causes are the causes associated with the major cause. Isolate each major cause and

determine all the factors that contribute to each major cause. Then list each minor cause around the

major cause and draw an arrow pointing to the major cause.

Step 5: Identify the sub-causes for each minor cause

The primary purpose of the cause and effect diagram is to illustrate the interactions among various

causes of variation in a given process. Therefore, it is necessary to break cause down, in a step-by-

step fashion, from the most major to the most minor aspects of each cause. For example, if

equipment is listed as the major cause, a specific piece of equipment could be listed a minor cause;

the condition of the equipment could be a sub-cause; and the measurements or characteristics or

calibration could be another sub-cause. List all of the sub-causes around the minor cause and draw

an arrow from the sub-cause to the minor cause to illustrate their relationship.

Step 6: Review the cause-and-effect diagram

When you review the diagram, be sure that all of the items contributing to the problem have been

identified.

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PREVENTIVE MAINTENANCE

SECTION XVIII REVISION 4 EFFECTIVE DATE 01/08/16 Page XVIII- 1

18.1 Overview

Preventive maintenance is an orderly program of positive actions (equipment cleaning, lubricating,

reconditioning, adjustment and/or testing, etc.) done to prevent the failure of measurement systems

or support equipment. The goal is to ensure that analytical systems are in control and to prevent any

nonconformance due to instrument malfunction from occurring before or during any procedure. In

order for preventive maintenance to function properly, analysts and technicians need to maintain and

reference maintenance documentation. Documentation should be in the form of Preventive

Maintenance Schedules or Preventive Maintenance Logs. Use of preventive maintenance logs for

each analytical measurement system and support apparatus aids in the foretelling of possible

problems while preventive maintenance schedules are used to prevent problems from occurring.

Periodic preventive maintenance (PM) routines by outside services are contracted to extend

instrument/apparatus life and to verify current and future working status. Many instruments are

maintained under service contracts, thus PM calls should be made on a regular basis.

18.2 Part Maintenance

Every instrument has parts which are routinely exhausted, refurbished or cleaned. These parts

should have replacement parts readily available. Replacement inventory should be maintained

according to replacement part use and life. Information on part life can be obtained from Preventive

Maintenance Logs. Since some of the personnel have multiple responsibilities, including running

different instruments, it is important to maintain a centralized area for replacement parts and a

working inventory. A minimum number of each replacement part should be designated to act as a

reordering point. Refer to section XIX for details on supply ordering.

18.3 Preventive Maintenance Schedules

It is important to maintain instrumentation in good working order to limit down time. Following a

preventive maintenance schedule can prevent down time and also can prevent QC anomalies. In

order to produce a Preventive Maintenance Schedule, one needs to be extremely familiar with the

instrumentation or apparatus. Please follow the steps below:

1. Record specific instrument maintenance routines.

2. Figure a frequency for maintenance routines based on experience and information on

Preventive Maintenance Logs.

3. Construct a Table that has the maintenance tasks as rows and times (in days) in columns.

4. Have this table or schedule sheet approved by your department supervisor. Please make sure

“BC Laboratories, Inc.” is written on the top of the draft sheet.

5. Submit the table to the Word Processor (WP).

6. Review the WP’s work and approve the sheet when all corrections, if necessary, are

completed.

7. Tell the WP the number of sheets needed for your log. The WP will bind the log.

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SECTION XVIII REVISION 4 EFFECTIVE DATE 01/08/16 Page XVIII-

2

Preventive Maintenance Logs

A Preventive Maintenance Log is used to document preventive measures conducted on a day-to-day

basis. These logs can be paginated composition books or any paginated bound notebook. Maintenance

logs should be instrument specific. Entries into these logs should be periodically checked by

respective department supervisors.

18.5 Service Contracts

Service contracts are maintained for various instruments. These contracts entitle us to unlimited corrective

labor and parts. Preventive maintenance is also covered on each service contract, thus it is imperative to

schedule a PM for insured instruments on an annual basis.

18.6 Service Calls

All service calls are subject to approval by department supervisors. Once approved, analysts should contact

service personnel as soon as possible to schedule corrective work or preventive maintenance. When a firm

date has been set, analysts should relay the date information to the department supervisor.

18.7 Tagging Out

In cases when instrumentation or equipment is not operational, they must be labeled “out of service, do not

use”. A label with the aforementioned quote should be affixed to all non-operational instruments or

equipment. The same labeling convention should be used in cases of temporarily out of service situations.

Labels are available from the QA/QC Department.

Non-operational status should be documented on either a Preventive Maintenance Log or a Preventive

Maintenance Schedule.

18.8 Verification of Working Status

When an instrument or apparatus is placed back into service after being tagged out, analysts must verify

working condition prior to use. Condition verification can be an acceptable calibration, an acceptable

performance check, service technician performance check documentation, or any other record that verifies

the instrument or apparatus is functioning properly. Entries in Preventive Maintenance logs or schedules

should allude to the performance verification records. Analysts or technicians should always document

working status after tag out on either a Preventive Maintenance Log or a Preventive Maintenance Schedule.

Note: Section XVIII was reviewed on 01/08/16(No Changes were made)

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SECTION XVIII REVISION 4 EFFECTIVE DATE 01/08/16 Page XVIII- 3

Maintenance Request Form

General Manager Use Only

Request No.:

Priority Rating:

Employee:

Date of request:

Requested date of maintenance completion:

ASAP

1 week

At earl iest convenience

Specific Date: ____________

Maintenance Request:

Problem(s) if not corrected:

Maintenance Dept. use only

Estimated Cost: $_____________

Supplies:

Department: Supervisor Approval:

Date:

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PROCUREMENT

SECTION XIX REVISION 3 EFFECTIVE DATE 01/08/16 Page XIX- 1

19.1 Overview

An important aspect of the overall quality of a system is its interaction with outside services. The

quality of supplies has a direct relation with the quality of finished work. Our goal is to conduct

business with reputable, reliable vendors and to have an ordering system of high quality and

efficiency. Every order or service provided by a subcontracted vendor must be accounted for by

some form of documentation (requisition forms) which will be used for cost analysis and quality

control purposed. Utilizing, archiving and scrutinizing requisition forms will prove for many by-

products such as analytical consistency, cost analysis, theft tracking, vendor quality measurement,

workload monitoring, and test pricing.

19.2 Responsibilities

19.2.1 Technicians/Analysts

19.2.1.1 Complete a requisition form

19.2.1.2 Submit a completed requisition form to the appropriate department supervisor

19.2.1.3 Receive the orders (communicate to the purchasing agent)

19.2.1.4 Submit orders on a timely basis

19.2.1.5 Monitor inventory

19.2.1.6 Ensure the quality of products meets quality goals

19.2.2 Purchasing Agent

19.2.2.1 Place orders

19.2.2.2 Track orders

19.2.2.3 Ensure the quality of products meet quality goals

19.2.2.4 Mitigate procurement anomalies

19.2.2.5 Receive the orders

19.2.2.6 Cost analysis

19.2.3 President

19.2.3.1 Order approval

19.2.3.2 Purchases are in-line with company mission

19.2.3.3 Reasonableness of purchases

19.2.3.4 Budgeting

19.2.4 Department Supervisors

19.2.4.1 Interpreting the Requisition Forms

19.2.4.2 Approve orders

19.2.4.3 Monitor orders (number, cost)

19.2.4.4 Ensure the quality of products meet quality goals

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METHOD MODIFICATIONS

SECTION XIX REVISION 5 EFFECTIVE DATE: 01/08/16 Page XIX- 2

19.2.5 QA Officer

19.2.5.1 Monitor the quality of the ordering system

19.2.5.2 System audit

19.2.5.3 Calibration of new measuring products

19.3 Requisition Forms

Requisition forms are used to place orders. These forms, which are department dependant, are

available from department supervisors.

19.3.1 Obtain a requisition form from your department supervisor.

19.3.2 Place your name and the date in the appropriate fields.

19.3.3 Fill in the “date needed by” field. Please do not use terms such as “ASAP” or

“normal”. Please keep rush orders to a minimum.

19.3.4 Fill in the total number of units required under the Quantity field.

19.3.5 Enter the part number (if available) into the proper field.

19.3.6 Enter the product description under the proper field. Be descriptive. If information

cannot fit into appropriate boxes, use the back of the form or the next row under the

appropriate column.

19.3.7 Enter the vendor under the appropriate field.

19.3.8 Fill in the “Use” field. Be descriptive. Method number should be entered here also

(if appropriate).

19.3.9 Figure the frequency of use to the best of your knowledge.

19.3.10 Enter the PO# if applicable. Typically this field will be left blank.

19.3.11 Write in the number from the legend which represents the reason for purchase. If

none of the choices represent the reason for purchase adequately, use “8” for other

and describe accordingly.

19.3.12 If a service is required, rather than a product, enter the required information in the

fields located near the bottom of the requisition form.

19.3.13 When the form has been completed, submit to your department supervisor. If you

like, you can keep a copy for tracking and for a reference for future ordering.

19.3.14 Some of the orders are submitted by the Technical director, either under his name or

supervisor’s name.

19.4 Supply Receiving

Please follow the steps for receiving ordered products:

19.4.1 Sample custodian will receive the orders and the Technical Director will approve them.

19.4.2 Pick up your order in the sample receiving area. A page will be placed by the sample

custodian or receptionist for order pickups.

19.4.3 All containers are received by the Technical Director, this means he has accounted for

receiving the product, and thus it is available for use without any further communication.

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SECTION XIX REVISION 5 EFFECTIVE DATE: 01/08/16 Page XIX- 3

19.4.4 Open the packaging and inspect the product.

19.4.5 Verify the product is what you ordered in type and number.

19.4.6 Sign/initial and date the shipping paperwork to accept custody of items.

19.4.7 If a discrepancy was found, please contact your department supervisor.

19.5 Standard Receiving

Follow the receiving steps noted above. Locate the Certificate of Analysis and store according to

supervisor specifications. Label the standard (if possible) or standard paperwork with your initials

and the date received. Also record the date the standard was put into use.

19.6 Reagent Receiving

Follow the receiving steps outlined in the section labeled “Supply Receiving.” Write the date

received and your initials on the container label. Write the date the reagent is opened on the label.

19.7 Receiving Products Which Can Be Calibrated

Any device used for measuring can qualify as a product which can be calibrated. Follow the

receiving steps outlined in the section labeled “Supply Receiving.” Submit the device or glassware

to the QA/QC Department or supervisor for fitness of use approval.

Please note that if any supplies, standards, reagents, etc., received are not the usual products or

product brands you usually use, you need to scrutinize your work very closely to tie in possible

improved or degraded quality. If you have time, pre-qualify the new products through investigative

testing. Contact your department supervisor or the QA Officer for guidance.

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SECTION XX REVISION 5 EFFECTIVE DATE 01/08/16 Page XX- 1

20.1 Introduction

All methods utilized by BCL must be tested, documented and approved. We must have stringent

control on our approved methods and on our modification process. Communication, approval and

capability must be assured. If an employee makes changes to a method and does not effectively

communicate these changes, significant mistakes can occur during their absence. Also if the

changes are not approved, gross errors may occur because the chemistry or instrument is not

functioning properly. The capability of methods after modification must be checked to verify

compliance with referenced methods and internal controls. It is extremely important that all

employees follow the following method modification process to keep our system in control.

20.2 Modification Process

The method modification process includes the following steps:

1. Method modification petition

2. Petition approval

3. SOP revision and approval

4. Method modification capability study

5. Capability study approval

6. Method modification approval

20.2.1 Method Modification Petition

A request for a method modification must be placed in writing and submitted to a

department supervisor or to the President. This petition should have the following elements:

1. Method Identification

2. Instrument/Equipment IDs

3. Statement of the Problem

4. Proposed modification

5. Effects of the modification

6. Explanatory comments

20.2.2 Petition Approval

The department supervisor, Technical Director or can approve petitions by signature.

Additional requests or requirements can be added to the petition at any time during the

modification process. The original petition should be kept by the department supervisor and

a copy o the petition should be made and kept by the person responsible for carrying out the

modification.

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20.2.3 SOP Revision and Approval

Refer to section 5.3.

20.2.4 Method Modification Capability Study

The capability of a method must be verified after every method modification. Method

capability includes sensitivity, accuracy, precision and efficiency.

Sensitivity

An MDL study must be conducted.

Accuracy

4 replicates of a laboratory control sample must be analyzed and accessed.

Precision

The RPD/Standard Deviation of the 4 replicates of a laboratory control sample must be

accessed.

Efficiency

A logical metric must be used to express efficiency. Examples include, but are not restricted

to, samples/hour, samples per day, dollars per run/day. A comparison must be made

between the efficiency of the method prior to and after the modification.

20.2.5 Capability Study Approval

The capability study must be place in writing to the department supervisor for approval. The

department supervisor and the President should both sign the capability study. If not

approved, a subset of the capability study may require re-work.

20.2.6 Method Modification Approval

Once the capability study has been approved, the method is ready for use. Please note that it

is important to train all personnel responsible for the modified method.

20.2.7 New Methods

The State of California requires all laboratories requesting the use of methods off of their

respective certification lists to submit formalized data packages. Please refer to the

following sections for details.

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ENVIRONMENTAL LABORATORY ACCREDITATION PROGRAM (ELAP)

CALIFORNIA DEPARTMENT OF HEALTH SERVICES

850 Marina Bay Park Way 500 North Central Avenue Ste. 50

Building P 1st Floor M0512 Glendale, CA 91203

Richmond, CA 94804, (818) 551-2047

(510) 620-3155

______________________________________________________________________________________

DATA PACKAGE GUIDELINES

INTRODUCTION

The following guidelines are to be used by laboratories when submitting a Data Package if requested by

ELAP as a demonstration of laboratory competency

This format is to be used when submitting packets for the following instrumental methods: Gas

Chromatography (GC), Gas Chromatography/Mass Spectrometry (GC/MS), High Pressure Liquid

Chromatography (ICP/MS), Ion Chromatography (IC), Flame Atomic Absorption Spectrometry (FAA), and

Graphite Furnace Atomic Absorption Spectrometry (GFAA) and related instrumental techniques.

The laboratory must demonstrate that requirements for instrumentation, quality control, performance

criteria, procedures and reagents as specified in the method are complied with. Modification is allowed

only where permitted in the method.

As a document necessary for the verification of your laboratory’s competency for certification, a Data

Package must provide clear evidence of compliance with method standards and practices. To assist in our

determination or your competency, please be sure that all information is legible (preferably typewritten), all

pages of the document are numbered and that the Data Package is bound. Each method applied for must be

presented in a separate package.

A Data Package consists of a concise tabular summary of the key elements necessary to demonstrate

method proficiency. The basic format described in this document must be followed. Variations in the

presentation style and combining of tabular results are permitted, but the package must include complete

documentation of all required elements and the package must be well-organized. All raw data, including

chromatograms and instrument printouts, that support Data Package results should also be included for

ELAP review.

Incomplete, unsigned or disorganized packages will be returned to the laboratory unprocessed.

Data Packages are just one portion of the certification process and other factors such as an application, PE

samples and fees may be involved. Written approval from ELAP is necessary before the method applied

for can be employed for regulatory analysis.

Refer to the ELAP Guidelines and the Appendices for specific details, tips and/or additional details for the

particular method(s) you are preparing the data package(s) for.

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IF YOU HAVE ANY QUESTION REGARDING PREPARATION OF A DATA PACKAGE FOR

ANY METHOD, CONTACT YOUR ELAP CONSULTANT FOR FURTHER INFORMATION.

DATA PACKAGE FORMAT

Data packages submitted to ELAP should be presented in the following sections:

1. Cover Page

2. Table of Contents

3. Instrument Operating Conditions/Parameters

4. Standard and Sample Preparation Summary

5. Quality Control Limits

6. Summary of Data:

a. Calibration

b. Method Blank

c. Sample Analysis

d. Matrix Spike/Matrix Spike Duplicate

e. Method Detection Limit/Reporting Limit

f. External Reference Sample Analysis

7. Information/Comments

8. Raw Data

1. Cover Page

The Cover Page should include the following:

A. Full laboratory name and ELAP certificate/application number

B. Method Reference Number and Title of Method

C. Printed name and dated signature of Laboratory Director

D. Printed name and dated signature of analyst(s) who prepared data package

NOTE: All data packages must be reviewed for content and accuracy by the Laboratory

Director prior to submission. The director must sign and date the data package and

attest to the following statement (please print statement on cover page):

“I have reviewed this data package and found it to be accurate and complete.

All work was completed at our facility by the analyst and instrument as listed

in this document.”

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2. Table of Contents

The Table of Contents must list all items in the data package with page reference.

3. Instrument Operating Conditions/Parameters

A complete listing of all instruments operating condition should be described.

Chromatographic Methods – Instrument manufacturer and model number, detector(s), columns,

flow rates, carrier, temperature conditions and run times.

Atomic Absorption/Emission Methods – Instrument manufacturer and model number,

wavelength(s), gases, matrix modifiers, and temperatures for drying, ashing and atomization (if

appropriate).

Variances are allowed only if demonstrated as equivalent to the original method practice and as

allowed for in the method. Data packages with improperly modified procedures are not in

compliance with the method and certification will be denied.

4. Standard and Sample Preparation Summary

Procedures involved in the preparation of Standards and Samples should be summarized in tables

for the Data Package.

Standard Preparation should cover all steps involved in the preparation of the working calibration

standards, and include the following information:

Source of standard, lot number, dilutions, final concentrations preparer and date prepared.

Sample Preparation should cover all steps involved in the preparation of the sample for analysis

and include the following information:

Sample ID number, matrix sample preparer, date, initial weight or volume for sample, pretreatment

(sitting, milling), preparation (extraction, digestions, clean-up) and final volume for analysis.

The method of sample introduction into the analytical instruments should be described.

5. Quality Control Limits

Acceptance ranges for calibration linearity, response factors, recoveries, replicates and reference

standard. Analyses must be presented in the Data Package.

For Hazardous Waste instrumental methods acceptance limits for both solid and liquid matrices are

required.

Please present acceptance limits by analyte in a table form. Quality control limits may be combined

with analytical results which are evaluated against the acceptance criteria in the Data Package.

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In addition, control charts may be included in the quality control section.

NOTE: Quality control acceptance limits should be established by the following criteria:

Limits as described in the method.

Limits as described in the Code of Federal Registers

Limits derived by statistical procedures in the “Handbook for Analytical

Quality Control in Water and Wastewater Laboratories” EPA-600/4-79-019.

6. Summary of Data

A. Calibration

The calibration data for the method must be included in the Data Package.

Calibration curves must be presented for all compounds of interest. For the specific calibration

procedure requirements, refer to the individual method. In general, a calibration blank and three (3)

to five (5) calibration points as specified in the method must be presented in a summary form along

with peak areas/heights and appropriate statistical evaluation of linearity including response factors

and % relative standard deviations. If linearity is evaluated by graphic methods, the graph must be

included. All internal and surrogate standards should be identified.

NOTE: If one point calibration is used as the daily calibration check for the method, please

include the results of the daily RF and % difference from the RF derived form the

calibration curve.

Calibration information must be presented for all compounds being evaluated. All results must be

referenced to the chromatograms, printouts, etc. in the Raw Data section of the Data Package.

NOTE: Compounds To Be Analyzed For Multiple Analyte Methods

For initial certification, at a minimum all regulated analytes and/or analytes to be reported by the

method must be analyzed. Any common compounds that may coelute or interfere with target

analytes must also be tested for.

If no analytes to be evaluated by a method are regulated (i.e., certain 600 and 8000 series methods),

analyze at a minimum:

1. All analytes if the method list has ten (10) compounds or less.

2. If the method list has eleven (12) to thirty nine (39) analytes, evaluate at least ten (10)

analytes representative of early, mid-range and late elutors.

3. If the method list has more than forty (40) analytes, evaluate at least 25% of the analytes

representative of early, mid-range and late elutors.

B. Method Blank

The result of a Method Blank must be included in the Data Package.

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List any compound(s) and/or contaminant(s) identified in the method blank. Results may be

combined in the summary with calibration and sample results. Contamination above reporting

limits should be noted.

NOTE: A method blank is processed through the entire method and includes all surrogate

and internal standards, if used.

C. Sample Analysis

The results of a sample analysis must be included in the Data Package.

List the sample results in appropriate reporting units in a table. Results may be combined with the

Method Blank, Calibration and Matrix Spike results. All results must be referenced to the

chromatograms, printouts, etc. in the Raw Data section of the Data Package.

A local soil sample is recommended for hazardous waste methods and a tap water sample is

recommended for drinking water and wastewater methods. The sample does not necessarily have to

contain the analytes of interest. Inert sand or reagent water should not be used.

D. Matrix Spike/Matrix Spike Duplicate

The result of a Matrix Spike/Matrix Spike Duplicate must be included in the Data Package.

List the results of the matrix spike/matrix spike duplicate in a table. The spike is to be added to the

sample prior to any preparation steps necessary for analysis. Source of spiking solution, amount and

concentration of stock added, final concentration in sample, percent recovery, relative percent

difference and acceptance limits should be included.

NOTE: For multi-analyte methods, spike all analytes as specified in the method. If not

specified in the method, analyze at a minimum of three compounds or 10% of

analytes listed in the method, whichever is greater.

E. Method Detection Limit (MDL)/Reporting Limit (RL)

The results of the Method Detection Limit determination and Reporting Limits to be used when

employing the method must be included in the Data Package.

List the MDL’s and summarize all determination procedures in a table. Reference the results to

chromatograms and printouts.

For details on how to determine the MDL, consult the ELAP Information Appendices Guidelines or

refer to Glaser, J.A., Forest, D.L., McKee, G.D., Quave, S.A. and Budde, W.L., “Trace Analysis For

Waste Waters,” Environmental Science and Technology, 15, 1426, 1981.

The Reporting Limit (RL) is considered to be the minimum quantifiable level that the laboratory can

detect and is to be used when reporting results. The RL should be greater than or equal to the MDL.

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Reporting limits must conform to Regulatory Agency requirements.

Reporting limits must be verified. The RL is verified by spiking a matrix free of target analytes at

the reporting level. The spike is taken through all steps of the analytical process and is then

analyzed as a sample. Spiked values and actual recoveries should be indicated.

For Hazardous Materials methods, RLs should be defined for both soils and aqueous matrices.

F. External Reference Sample Analysis

The results of an External Reference Sample must be included in the Data Package.

Summarize the results of External Reference Sample analysis. Include the source (vendor and lot

number), a description of the matrix (if applicable), true values, concentration found, percent

recovery and acceptance limits.

If your laboratory has recently participated in any sort of Performance Evaluation (PE) study either

through EPA or another organization, please submit a copy of the results along with the acceptance

limits (if available).

For Hazardous Materials instrumental methods, a Laboratory Control Sample (LCS) is also required

in the Data Package. An LCS is a reference sample made from a matrix representative of the

samples being analyzed, and spiked with the analytes of interest.

7. Additional Information/Comments

Other information such as examples of calculations or Standard Operating Procedures may be

included in the package. Please feel free to submit any other information that will help us to

evaluate your proficiency in performing the method.

Comments (or footnotes) on various items in the data package may be included in this section.

8. Raw Data: Chromatograms, Printouts, Quantitation Reports

Submit copies of all relevant chromatograms, printouts, quantitation reports, etc., that support

results summarized in the previous sections. Chromatograms may be reduced in size by

photocopying to accommodate binding. Do not obscure any of the information printed on the raw

data. Paginate all raw data for easy reference.

All chromatograms and printouts must be clearly identified and referenced. All compounds must be

clearly identified. Integrator printouts must list relative retention times, peak areas, response factors

and concentrations. All surrogate and/or internal standard compounds should be identified.

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Appendix

DATA PACKAGE ELEMENTS

The following items are required for a complete data package.

Inorganic Analysis

EPA 200 Series Methods – Metals in drinking water and wastewater

1. Calibration

2. Method blank

3. Tap water sample analysis

4. Duplicate matrix spike of sample

5. MDL determination

6. DLR verification

7. External Reference Sample

NOTE: Primary standards for drinking water: use Office of Drinking Water (ODW)

reporting limits.

EPA 7000 Series Methods – Metals in Hazardous Wastes

1. Calibration

2. Method blank

3. Soil sample analysis


5. MDL determination must be presented for both soil and liquid matrices

6. RL verification must be presented for both soil and liquid matrices


8. Laboratory Control Sample

EPA 6010 Inductively Coupled Plasma (ICP)

1. Calibration

2. Method blank







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9. Analysis of an interference check standard. The interference check standard used must be as

specified in the method or made according to the following:

Analytes (mg/L) Interferant (mg/L)

Ag 1.0 Al 500

Ba 0.5 Ca 500

Be 0.5 Fe 200

Cd 1.0 Mg 500

Co 0.5

Cr 1.0

Cu 0.5

Mn 0.5

Ni 1.0

Pb 5.0

Ti 1.0

V 0.5

Zn 1.0

EPA 200.8, 6020 Inductively Coupled Plasma/Mass Spectrophotometry (ICP/MS)

1. Calibration

2. Method blank

3. Tap water (200.8) or soil (6020) sample analysis

4. Duplicate matrix spike or sample


6. RL/DLR verification



9. Analysis of a tuning solution for evaluating isotopic resolution in the 20 – 200 AMU range

(Be, Mg, Co, In, Pb).

ORGANIC ANALYSES

EPA 500/600 GC Methods

1. Calibration

2. Mid-range check standard for daily run

3. Method blank


5. Duplicate Matrix spike of sample

NOTE: For Purge and Trap methods, a Duplicate Laboratory Fortified Blank (Section 3.7 –

500 Series Methods) may be substituted for a matrix spike.



8. Mass spectra and relative ion abundance as specified in the method turning criteria using

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BFB (Purge and Trap) or DFTPP (Extractions) must be generated for GC/MS procedures.

EPA 524, 525, 624, 625 GC/MS Methods

1. Calibration


3. Method blank




7. DLR verification




EPA 8000 GC Methods

1. Calibration


3. Method blank







For PCBs (EPA 8080)

Complete demonstration of proficiency is required for PCBs 1016 and 1260. A mid-range check standard

for PCBs 1221, 1232, 1242, 1298, and 1254 is required.

Please summarize quantitation procedures for PCBs in the Instrument Operating Conditions Section.

For Total Petroleum Hydrocarbons (TPH)

Analysis of both Gasoline and Diesel Fuels is required.

For Gasoline Fuel Analysis by FID, a PID profile of BTEX in gasoline is also required (EPA 8020).

Please summarize quantitation procedures for all fuels analyzed in the Instrument Operating Conditions

Sections.

EPA 8240, 8260, 8270 GC/MS

1. Calibration


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3. Method blank









NOTE: For calibration of GC/MS methods, Calibration Check Compounds (CCC) RSDs

and System Performance Check Compounds (SPCC) RFs must be evaluated.

Results and acceptance criteria should be included in the calibration table and

should be highlighted or in bold.

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SECURITY

SECTION XXI REVISION 3 EFFECTIVE DATE 01/08/16 Page XXI-

1

21.1 Security System

Our security system is maintained through Kern Securities, Inc. Kern Securities is responsible for the

maintenance of the hardware, monitoring of activated system, and initiating fire and/or police response. In

order to activate and deactivate the security system, employees need to obtain an access number and a

clearance password.

21.2 How to Obtain an Access Code

Access codes are available through Human Resources. Contact your Department Supervisor for approval

prior to obtaining an access code from the Human Resources. Temporary employees and employees under

probation are not qualified to obtain access codes.

21.3 How to Obtain a Password

When obtaining an access code, you must have a password in mind that you will use as a clearance or abort

code. The password can be any length, but please note that you must remember this password when Kern

Securities representatives call for clearance. Be discrete with your password and access code. Other than

you and Human Resources, only Kern Securities should be privy to this information.

21.4 How to Activate/Deactivate the Security System

21.4.1 Deactivation

When opening the laboratory, the system should initially be armed, thus you need to deactivate the alarm

system. Upon entering the building, find an alarm keypad within 45 seconds and enter your access code

number. This should deactivate the alarm. If the access code is not acceptable or there was a discrepant

keypad entry, the alarm will go off after 45 seconds. If the alarm goes off, enter your six digit access code,

then call Kern Securities to explain the situation.

21.4.2 Activation

In order to activate the alarm, first verify all exits are locked and secure, then verify no other employees are

in the laboratory by using the intercom system or by conducting a search of the entire premises. If all exits

are secure and you are the only employee on the laboratory grounds, activate the alarm by entering your six

digit access code. Please wait until the digital display on the keypad reads “Ready to Arm” before you enter

your access code. If this prompt does not appear, a door may not be locked or secured. When you

successfully activate the alarm system, the prompt “All secure, please exit” will appear in the keypad

display. You must exit within 45 seconds.

Kern Securities must be contacted whenever the alarm goes off. Representatives from Kern Securities call

for police response, thus you must contact Kern Securities whenever the alarm goes off.

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SECURITY

SECTION XXI REVISION 3 EFFECTIVE DATE 01/08/16 Page XXI-2

21.5 How to Use the Intercom

Locate a phone that is connected to the phone network. Pick up the receiver, enter “810”, wait for the

acknowledgement tone, then speak into the receiver.

21.6 What to do When Working Odd Hours

Whenever working on weekends or late hours, please contact Kern Securities to communicate how long

you expect to work. If you leave prior to another employee also working odd hours, please tell him/her the

expected exit time you gave to Kern Securities, so he/she can correct the expected exit time.

21.7 How to Contact Kern Securities

When contacting Kern Securities, you must be ready to give them you access code number and password.

Contact Kern Securities at 588-HELP or 588-4357.

21.8 How to Answer Phone Calls

When the night service function is activated on the phone system, all incoming calls are acknowledged

through the intercom system. If you hear the intercom phone call acknowledgement, pick up the receiver of

the nearest phone and enter “73290”. An appropriate greeting would be “BC Laboratories. How can I help

you?” It is extremely important to answer the phone because Kern Securities calls numerous times to verify

system status. If calls from Kern Securities are not answered, the police or management will be called.

21.9 Responsibility

It is the responsibility of all employees to do their best in following proper procedures listed here regarding

the security system. The last person entering their code into the security system is responsible for security

of the laboratory. In order to transfer responsibility, the responsible employee must secure a written

verification of the transfer of responsibility from another employee. Transfer of responsibility

documentation must be submitted to the President by the following work shift.

An example of a Transfer of Responsibility Form is attached.

21.10 Keys

You must request the use of a laboratory key through your Department Supervisor. If the Department

Supervisor is not available, contact either Human Resources or the Team Leader within your department. If

you require a copy of a laboratory key, please contact Human Resources. Laboratory keys may not be

copies unless prior approval is granted by the President. Sharing of keys is not acceptable. You are subject

to disciplinary procedures if you are found to share your key.

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SECURITY

SECTION XXI REVISION 3 EFFECTIVE DATE 01/08/16 Page XXI-3

Transfer of Responsibility Form

Relinquished by: Date/Time:

Assumed by: Date/Time:

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Comments:

Note: Section XXI was reviewed on 01/08/16 (No Changes were made)

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