lead addendum to the quality assurance ...by quality assurance section (qas) on january 31, 1989,...

) b O 0 000 3 2

^tO STjf.? \ UNITED STATES ENVIRONMENTAL PROTECTION AGENCY

1 REGION 5? 230 SOUTH DEARBORN ST.

,< CHICAGO, ILLINOIS 60604R E P L V TO THE ATTENTION OF

5SMQA

Kanorandum

Date: FE3 1 4 1990

Subject: Approval of the PRP-Lead Addendum to the Quality AssuranceProject Plan (QAPjP) for Renv^dial Investigation/FeasibilityStudy (RI/FS) Activities at the Fadrowski Drum Disposal Site,Franklin, Wisconsin

From: Valerie J. Jones, Chief.y , Monitor ing and Quality Assurance Bran

/ •/!'I'D: Joim Kelly, Acting Chief /Reniedial and Qnergency Response Branch

Attention: Fred Micke, Ri vl

I am providing approval of the Addendum to the QAPjP for RI/FSActivities at Fadrowski Drum Disposal Si.te, Franklin, Wisconsin, receivedby Quality Assurance Section (QAS) on January 31, 1989, (QAS Log-in No. 1146).

To facilitate this QAPjP for approval, QAS staff made the followingcorrections:

1. Section 4, pages 1 and. 2.

a. Name of the Remedial Project Manager was changed to Fred Micke.

b. Contract Project Manageiient Section was deleted from the QAPjPdue to the reorganization in Central Regional Laboratory.

2. Cover page for analytical methods used by War z in.

a. "Instrument detection limit (2XIDL)" was changed to " Detectionlimit (2XDL)".

b. Limits of ±10% were applied for the 2XDL standard.

EPA Region 5 Records Ctr.

208100

-2-

3. Attachment 1.

a. Check standard (2XDL), limits and frequency were added forchloride, total alkalinity and sulfate analysis in Attachment 1.

b. Limit for alkalinity was changed from "<10 ppm" to "<5 ppm".

4. Total Cyanide, page CNAAHC-1.

Following was added to the sample liandling section: "Read as soon aspossible, no later than three days after distillation".

5. Table 3-4a, note 5.

Following was added: "CLP SOW 7/88 (metals, cyanide) and SOW 2/88(VOC, ENAs, PEST/PCBs) or most recent procedures will be followed".

A copy of corrected pages is attached for your use and should beincorporated in all copies of this QAPjP.

The signed approval page is attached to this memorandum. Please havethe Remedial Project Manager provide final sign-off and send us a copy of thecomplete signature page.

rRCri : NGINEERING 312 3B6 2591 FEB 13, 1332

QUALITY ASSURANCE PROJECT PLAN (QAPP)

Fadrowski Drum Disposal SiteRemedial Investigation/Feasibility Study

Franklin, Wisconsin

Prepared by:

Warzyn Engineering Inc.Milwaukee, Wisconsin

Prepared for:

Acme Printing Ink CompanyMilwaukee, Wisconsin

o Revision: 3January 26, 1990

Approved: Date:PRP Representative

Approved: Date:Warzyn Site Project Manager

Approved:

r~J Approved:

Approved:

Warzyn Quality Assurance Manager

U.S. EPA Remedial Project Manager

•$ • /Htfyf

on VU.3. EPA Region'V Qua]Assurance Officer

Date:

Date:

Date:

[sss-600-22][vlr-400-84]25389.00

Fadrowski Drum Disposal QAPPSection: 4Revision: 3Date: January 26, 1990Page: 1 of 2

4.0 PROJECT ORGANIZATION AND RESPONSIBILITY

4.1 OVERALL RESPONSIBILITY

• Acme Printing Ink Company

• Michael J. Radcliffe, Project ManagerWarzyn Engineering Inc.

. Mr. Fred Micke,r Remedial Project ManagerU.S. EPA, Region V

• RI/FS Reports and Technical Memorandumprepared by Warzyn Engineering Inc.

4.2 MONITORING AND SAMPLING OPERATIONS AND QC

• Principal Engineering Firm - Warzyn Engineering Inc.

• Drilling - Exploration Technology, Inc.

• Sampling, Monitoring and Survey - Warzyn Engineering Inc.

• Quality Control - Richard W. Maurer, Warzyn Engineering Inc.

4.3 LABORATORY ANALYSES AND QC

• Analysis of test pit, soil, sediment, surface water and groundwatermatrix samples for EPA TCL VOCs, BNAs, Pest/PCBs.

- CompuChem Laboratories

• Analysis of test pit, soil, sediment for cyanide and EPA TCL metals; andsurface water and groundwater for cyanide, alkalinity, sulfate,chloride, field pH, field specific conductance and EPA TCL metals.

Warzyn Engineering Inc.

4.4 SPECIALIZED RESPONSIBILITIES FOR LABORATORY SERVICES

• CompuChem Laboratories

- analytical protocol specified - Warzyn Engineering Inc.

- review of analytical protocol - U.S. EPA Region V Quality AssuranceSection (QAS) and Central Regional Laboratory (CRL),

Fadrowski Drum Disposal QAPPSection: 4Revision: 3Date: January 26, 1990Page: 2 of 2

- Review and approval of performing laboratory - U.S. EPA Region V CRL,

- Internal QA/QC - CompuChem Staff

- Final data review and validation - Warzyn Engineering Inc.

- Review of tentatively Identified compounds and assessment of need forconfirmation - Warzyn Engineering Inc.

• Warzyn Engineering Inc.

- Review of analytical protocol - USEPA Region V QAS and CRL

- Review and approval of performing laboratory - U.S. EPA Region V CRL,

- Internal QA/QC - Warzyn Engineering Inc.


4.5 QUALITY ASSURANCE

• Overall QA Responsibility

- Warzyn Quality Assurance Officer

• Warzyn Subcontracted Activities- Warzyn Engineering Inc.

• Review of QAPP- U.S. EPA Region V QAS and CRL

• Field Analysis- Warzyn Engineering Inc.

4.6 PERFORMANCE AND SYSTEMS AUDITS

• Field Operations

- QAO, Warzyn Engineering Inc.- U.S. EPA Oversight Contractor

• Analytical Laboratories- U.S. EPA CRL

• Evidence Audits- QAO, Warzyn Engineering Inc.

An organization chart is shown in Figure 4-1.

ANALYTICAL METHODS USED BY WARZYN

FOR THE FADROWSKI DRUM DISPOSAL SITE

The following are standard operating procedures (SOPs) for analyses to beperformed by Warzyn on samples collected the Fadrowski Drum Disposal Site.

Method detection l i m i t s and number of QC samples to be performed are

summarized, but SOPs do not specify performance standards. The followingtable lists performance standards for quality control samples. If

calibration standards or EPA reference standards do not meet performance

criteria, the analysis will be stopped and the method problems will beresolved prior to re-calibration. If standards s t i l l are not met, the

laboratory QA officer is to be notified. When an analyte concentration

exceeds the calibrated or linear range, re-analysis of the prepared sample

after appropriate dilution is required.

Standards at twice the detection l i m i t (2X DL) are required for

automated sulfate, chloride and alkalinity analysis. The standards will

not be used for instrument calibration, but will be used as a quality

control sample. The 2X DL standard will be analyzed at the beginning ofeach run. Results will be considered acceptable if within plus or minus 10%

the true concentration of the standard. If data are not acceptable,

method resolution and/or recalibration will be performed.

Data deliverables for analyses to be performed by Warzyn Engineering will

include chain of custody records, final analytical results, a summary ofall quality control data and raw data for all analyses. The complete data

package will be included in the final evidence file maintained by Warzyn

Engineering Inc.

[Vari an-Mi sc]

QUALITY CONTROL REQUIREMENTS FOR ANALYSES PERFORMEDBY WARZYN AT THE FADROWSKI DRUM DISPOSAL SITE

Attachment 1

PARAMETER AUDIT FREQUENCY' LIMITS

Metals (except Hg) Lab blank

Duplicate

1 per set

1 per 10 samples

Check Standard 1 per 10 samplesand end of run

Matrix spike 1 per 10 samples

EPA QC Reference 1 per setStandard

< detection l i m i t

20% RPD for waters(l)35% RPD for all other(l)

matrices

90-110% recovery

85-115% recovery for waters75-125% recovery for allother matrices

80-120% recovery

Mercury Lab blank

Duplicate

1 per set

1 per 10 samples

Check Standard 1 per 10 samplesand end of run


EPA QC Reference 1 per setStandard

< detection 1 i m i t

20% RPD for waters(l)35% RPO for all(l)

other matrices

85-115% recovery


80-120% recovery

Chloride Lab blank

Check Standard

(2X DL)Check standard

Duplicate

1 per 10

1 per run

1 per 10 samplesand end of run

1 per 10 samples


<1 mg/L

90-110% recovery

90-110% recovery

20% RPD for waters(l)35% RPO for all other

matrices(l)

85-115% recovery for waters75-125% recovery for a l lother matrices

80-120% recoveryEPA QC Reference 1 per setStandard

*Frequencies apply to each i n d i v i d u a l matrix.

(1) When sample concentrations are w i t h i n 5 times the detection l i m i t theacceptable duplicate range is 2 times the detection l i m i t , as discussedin SOW 7/88.

QUALITY CONTROL REQUIREMENT FOR ANALYSi '.» H.Kh>fBY WARZYN AT THE FADROWSKI DRUM DISPOSAL S I T f

PARAMETER AUDIT FREQUENCY* L I M I T S

Total A l k a l i n i t y Lab blank

Check Standard(2X DL)

Check Standard

Duplicate

Matrix Spike

EPA QC ReferenceStandard

1 per 10 samples

1 per 10 samples

1 per 10 samples

1 per set

<5 mg/L

90-110% recovery

90-110% recovery

20% RPO for waters(l)35% RPD for all other(l)

matrices

85-115% recovery for waters75-125% for all othermatrices

80-120% recovery

Sulfate Lab blankCheck Standard

(2X DL)Check Standard

Duplicate

Matrix spike


1 per 101 per run


1 per 10 samples

1 per 10 samples

1 per set

<5 mg/L90-110% recovery

90-110% recovery

20% RPD for waters(l)35% RPD for all other(l)

matrices


80-120% recovery

Total Cyanide Lab blank

Duplicate

Check standard

Matrix spike


1 per 10 samples <0.005 mg/L

1 per 10 samples


1 per 10 samples

1 per set

STD (Distilled) 1 per set

Blank (Distilled) 1 per set

*Frequencies apply to each individual matrix.

20% RPD for waters(l)35% RPO for all other

matrices(l)

85-115% recovery


80-120% recovery

85-115% recovery

<0.005 mg/L

1) When sample concentrations are within 5 times the detection l i m i t theacceptable d u p l i c a t e range is 2 times the detection l i m i t , as discussed

Effective Date:

TOTAL CYANIDE - AUTOANALYZER - (HEATED METHOD)

Scope and Application: This method is applicable to d i s t i l led groundwater,drinking water, wastewater, sediments and soils. Allsamples must be distilled prior to analysis with theautoanalyzer. (Refer to SOP # CNDISC.)

Reference: EPA, 1983, Method 335.3Lachat Instruments, 1986, Method 10-204-00-1-AStandard Methods, 16th Edition, pages 337-338

strument Detection L i m i t : 0.005 mg/L

Optimum Concentration Range: 0.005 - 0.40 mg/L

Sample Handling: Samples should be capped and refrigerated at 4°C afterdis t i l l a t i o n . Read as soon as possible no later than3 days after d i s t i l l a t i o n .

Instrument Conditions:

1. Pump speed: 352. Cycle period: 50 seconds3. Load period: 20 seconds4. Inject period: 15 seconds5. Inject to start of peak period: 30 seconds6. Inject to end of peak period: 78 seconds7. Gain: 4208. Zero: 3509. Interference filter: 570 mm10. Sample loop: 150 cm (0.80 mm i.d.)11. Standards for calibration: 0, 0.02, 0.04, 0.10, 0.20, 0.40 mg/L12. Water Bath 45"C (Position A).

Reagent Preparation: (Prepare fresh every 6 months unless otherwise noted.)

1. Degassed Mil 1i-Q-water - 2 options:

a. Boil Milli-Q water vigorously for 5 minutes. Cool and store incubitainer.

b. Bubble helium, using the fritted gas dispersion tube, through 20 LM i l l i - Q water for 15-20 minutes. Store in cubitainer.

2. Carrier - 0.25N NaOH:

In a 1 L volumetric flask, dissolve 10.0 g NaOH in 900 mL DI water.Dilute to the mark and invert several times. Filter through 0.45micron filter paper. Store in a plastic bottle.

[INORGSOP]CNAAHC-1

Table 3-4a

Additional RI SamplingFadrowski Drum Disposal Site

Matrix!1)

SoilSoilSoilSoilSoil

SedimentSedimentSedimentSedimentSediment

GroundwaterGroundwaterGroundwaterGroundwater

Lab(2)

CompuChemCompuChemCompuChemWarzynWarzyn

CompuChemCompuChemCompuChemWarzynWarzyn

FieldCompuChemWarzynWarzyn

No. OfSamples

11111

11111

8888

FieldDuplicates

11111

11111

Field(3) Matrix(4)Blanks SPK/DUP

00000

00000

Total*Samples

22222

22222

121010

Test Parameters

EPA TCL VOCsEPA TCL BNAsEPA TCL PEST/PCBsEPA TAL METALSCYANIDE

EPA TCL VOCsEPA TCL BNAsEPA TCL PEST/PCBsEPA TAL METALSCYANIDE

pH, CONDUCTIVITY, TEMPERATUREEPA TCL VOCsEPA TAL METALS (MERCURY ONLY)(6)ALKALINITY, CHLORIDE, SULFATE

(1) Soil, sediment and water matrix samples will be considered low concentration samples. Samples from excavations w i l lbe considered medium level samples.

(2) CompuChem: CompuChem Laboratories, 3308 Chapel H111, Nelson Highway, Research Triangle Park, NC 27709Warzyn: Warzyn Analytical Laboratory, 1 Science Court, Madison, WI 53711Field: Field Analysis - performed on-site

(3) A trip blank for purgeables will be Included with each shipment for leachate and groundwater samples.

(4) Water matrix VOCs require triple the normal volume for a MS/MSD sample and water matrix extractables (BNAs,Pesticides/PCBs) require double the normal volume at a frequency of one per 20 or fewer samples per concentrationlevel.

(5) See Appendix B for EPA TCL and TAL analyte 11st. See Appendix C for water quality parameter SOPS. Conductivity, pHand temperature will be determined in the field for surface and groundwater. CLP SOW 7/88fmetals Cyanide^ andSOW 2 /88 fVOC, BNAs , PEST/PCBs) or the most recent procedures will be followed. "

(6) Samples should be filtered in the field for mercury analysis.

STS/vlr/MJR[dlk-401-40]25389.20

WARZYN

January 25, 1990

Mr. Fred MickeRemedial Project ManagerU.S. Environmental Protection AgencyRegion V (5HE-12)230 South Dearborn StreetChicago, Illinois 60604

Re: Addendum to Quality Assurance Project Plan (QAPP)QAS Log-In No. 1106Fadrowski Drum Disposal Site (FDDS) RI/FSFranklin, Wisconsin

Dear Mr. Micke:

On January 8, 1990 Warzyn received a facsimile transmission of the January 1,1990 Quality Assurance Section (QAS) review of the above mentioned QAPPaddendum. It was Warzyn's understanding that the purpose of the QAPP addendumwas to document the change in the project Contract Laboratory Program (CLP)analytical laboratory, not to reiterate the project objectives. This letteris in response to comments made by QAS regarding the FDDS Site QAPP Addendum.

This response should be reviewed in conjunction with the original QAPPdocument. The addendum is not intended as a stand alone document. EPAinquiries are identified in bold type; followed by Warzyn's response instandard print.

I. The addendum to the QAPjP should contain following information:

1. Project Objectives

The objectives of the additional sampling program proposed isto evaluate the potential impact from surface runoff from theFDDS. Soil sediment from SD-5 (refer to Figure 1 attached)will represent potential contaminant movement via surfacerunoff from the FDDS fill area. A surface water sedimentsample, SW-5 (shown on figure 1) will evaluate potentialimpacts on stream sediments from surface runoff from the FDDS.On additional round of groundwater samples wi l l be collectedfrom each of the 5 groundwater table wells and 3 piezometers(refer to Figure 1). These additional groundwater samples arerequired to complete groundwater characterization forpreparation of the RI report.

Fadrowski Drum Disposal Site (FDDS) RI/FS Page 2January 25, 1990

2. Sample Network and Rationale

The rationale behind the sample network has been previouslysubmitted in the Final RI/FS QAPP and Work Plan. Therationale for additional soil, sediment and groundwatersamples is discussed above and in Warzyn's letter to Mr. FredMicke, RPM dated October 6, 1989.

3. Map of Sampling locations

A map (Figure 1) is attached which shows the locations of theproposed additional sampling locations.

4. Intended Data Uses

The data will be utilized to finalize contaminant migrationwork associated with the FDDS as discussed in I.I above andthe RI/FS QAPP and work plan.

5. Table with required detection limits for target compoundsincluding water quality indicators

The detection limits for each target compound and waterquality indicator parameter are presented in Table B-l of theQAPP (Appendix B).

II. Following correction should be made in Table 3-4a:

1. Please reference the methods used for organic/inorganicanalysis.

Refer to revised footnote 5 on Table 3-4a.

2. Please note that groundwater samples designated for MS/MSDanalysis should be collected at the triple the normal samplevolumes for VGA analysis. Please correct,

MS/MSD footnote has been changed to include volumerequirements. Refer to footnote 4.

3. Please state whether groundwater samples should be fieldfiltered for Hg analysis.

Footnote added to Table 3-4a to indicate that groundwatersamples should be field filtered for Hg analysis (footnote 6).

4. "EPA TCL Metals" should be changed to "EPA TAL Metals".

Revised table reflects this change.

WARZYN


III. The detection limits provided in SOPs are different from detectionlimits in Table B-l, Appendix B of the QAPjP approved on 10.13.88.Please submit a table with required detection limits.

Contract required detection limits (CRDL) and contract requiredquantisation limits (CRQL) are provided in Table B-l, eachinstrument detection limit must achieve these required maximumlevels.Actual instrument detection limits (IDL) may be lowerthan CRDL and are recorded in the individual SOPs. The CRDLcontract requirements wil l be reported when applicable.

IV. SOPs submitted for metals and water quality parameters requiredfollowing correction:

A. Alkalinity SOP.

1. Drying temperature for Na2C03 in the referenced method is250°C not 140°C. Please explain.

Omission in revision. Corrected SOP attached.

2. Concentration of the first calibration standard (exceptblank) should be closer to the detection limit (at least 5ppm).

Calibration will be as stated in the SOP. To check forlinearity near the detection limit, we will run anadditional standard at the start of the analysis at alevel of twice the instrument detection limit. Seeintroductory text of Appendix C.

3. The control limits for the method blank, matrix spike,duplicate analysis, laboratory control samples (LCS), etc.must be provided in the SOP.

All water quality parameters have been addressed in atable containing a summary of quality control requirementsand associated quality control limits (see Appendix C).

4. The data deliverables should be specified in the SOP.

See inductory test of Appendix C.

B. Chloride SOP.

1. Drying temperature for NAC1 in the referenced method is1409C not 103°C. Please explain.

Omission in revision. Corrected SOP attached.

WARZYN


2. Concentration of the first calibration standard (exceptblank) should be closer to the detection limit. Pleasecorrect.

See response to Alkalinity SOP comment number 2.

3. The control limits for method blank, matrix spike,duplicate analysis, laboratory control sample (LCS), etc.must be provided in the SOP.



See inductory test of Appendix C.

C. Cyanide SOP.

1. Standard cyanide solution (5 mg/1) and all calibrationstandards must be prepared daily at the time of analysis,not weekly.

Cyanides will be analyzed as per Statement of Work (SOW)7/88 requirements.

2. They cyanide detection limit in the approved QAPjP wasdifferent from detection limit provided in the SOP.Please correct the discrepancy.

The detection limit included in the approved QAPjPrepresents a contract required detection limit (CRDL), andthe instrument detection limit (IDL) must be at or belowthis level. The detection limit noted in the SOPrepresents the IDL. The CRDL wil l be reported as per SOW7/88.

3. Please provide equation for calculations and describe thereporting units in the SOP.

Omission incurred in revision, corrected SOP included.

4. The control limits for method blank, duplicate analysis,matrix spike, laboratory control sample, initial andcontinuing calibration verification standard, etc. must beprovided.



See inductory text of Appendix C.

WARZYN


D. Sulfate SOP.

1. Concentration of the first calibration standard (exceptblank) should be closer to the detection limit (10 mg/1).Please correct.


2. The control limits for method blank, matrix spike,duplicate analysis, laboratory control samples, etc. mustbe provided in the SOP.



See introductory text of Appendix C.

E. Metals SOPs.

1. Acid digestion for sediments, sludges and soil samples.Please explain how samples in 200 ml volumetric flask canbe diluted to 100 ml (A-ll, B-4). Please correct this ifthis is a typo.

Corrected SOP attached.

2. All calibration standards for metals analysis (flame,furnace) must be prepared at time of analysis (CLP SOW7/87, Exhibit D).

Omission in revision, all SOPS corrected and attached.

3. The data deliverables for metals analysis should bespecified in each SOP.

See inductory text of Appendix C.

4. The control limits for method blank, matrix spike,duplicate analysis, initial calibration blank, continuingcalibration blank, initial calibration verification,continuing calibration verification, laboratory controlsample, etc. must be provided in each SOP.


5. Please explain what does "Duplicate are to be averaged"mean. Does it mean duplicate analysis, duplicate burns orduplicate samples.

Revisions to SOP quality control sections were omittedfrom original copies. SOPs with correctly revised qualitycontrol section are attached.

WARZYN


6. Concentration of the first calibration standard should beslightly above the detection limits for all metalsanalyzed by flame AA.

We calibrate the instrument according to manufacturer'srecommendations, as is suggested in SOW 7/88 exhibit E.To check for linearity near the instrument detection limit(IDL) we will analyze a standard at twice the IDL at thebeginning of the analysis.

7. The detection limits in the SOPs differ from the detectionlimits provided in the QAPjP. Please correct thediscrepancy.

See response to Cyanide SOP comment number 2. CRDLresults will be reported.

8. Please state that the holding time for mercury should be26 days.

Omission in revisions. Corrected SOP attached.

9. For every sample analyzed, by furnace, verification isnecessary to determine that method of standard addition isnot required. Please use attachment I for all furnaceanalysis.

The criteria used to determine if method of standardaddition is necessary were omitted from the qualitycontrol section of the SOPs and has since been included.Corrected SOPs are attached.

If you have any questions, please contact Mike Radcliffe, Project Manager orKim Finner, Laboratory Manager, for further clarification. Please provide uswith verbal and/or written approval expeditiously so that we may proceed withthe additional field sampling component of the FDDS RI.

Sincerely,

WARZYN ENGINEERING INC.,

Steve^ C. Termont-Schenk, P.E.Task Manager

Michael J. RadcliffeProject Manager

STS/MJR/vlr/KDF[vlr-101-75]25389 WARZYN

WARZYN

Report Quality Assurance25389 Project Plan (QAPP)

Fadrowski Drum Disposal SiteFranklin, Wisconsin

Prepared for:


Prepared by:


June 1988

WARZYN

Engineers & ScientistsEnvironmental Services

Waste ManagementWater Resources

Site DevelopmentSpecial Structures

Geotechnical Analvs.s

June 29, 198825389.00

Mr. Robert WhippoRemedial Project ManagerU.S. Environmental Protection AgencyRegion V 5HE-12230 S. Dearborn StreetChicago, IL 60604

Dear Mr. Whippo:

Attached are five copies of the Final RI/FS Quality Assurance Project Plan(QAPP) for the Fadrowski Drum Disposal Site. As required under the ConsentOrder, two copies are also being mailed to Mark Giesfeldt (WONR-Mad1son) andFrank Schultz (WDNR-Southeast District). The QAPP has been revised based onreview comments made by the U.S. EPA and the WDNR.

If you have any questions, please call.

Sincerely,

WARZYN ENGINEERING INC.

, uWrRobert C. Wendt, Ph.D.Project Chemist

Michael J. RadcliffeProject Manager

Enclosures: As Stated

cc: Mark Giesfeldt, WDNR-Mad1son (w/2 encl)Frank Schultz, WDNR-Southeast District (w/2 encl)Randy Walbrun, Acme Ink Co. (w/1 encl)William Roush, Esq. (w/1 encl)

RCW/bcn/MJR[guest-105-64]

Warzyn Engineering IncOne Science Court

University Research ParkPO Sox 5385

Madison. Wisconsin 53705

|608| 273-0440

WARZYN

Quality AssuranceProject Plan (QAPP)

Fadrowski Drum Disposal SiteFranklin, Wisconsin

June 1988

QUALITY ASSURANCE PROJECT PLAN (QAPP)

Fadrowski Drum Disposal SiteRemedial Investigation/Feasibility Study

Franklin, Wisconsin

Prepared by:


Prepared for:


Approved:

Approved:

Approved:

Approved:

Approved:

Revision: 2June 28, 1988

tepresentaytTve PRp Steeri ngCommittee

\- •r

Warzyn Site Project Manager

Warzyn Quality Assurance Manager

U.S. EPA Remedial Project Manager

U.S. EPA Region V QuaTttiAssurance Officer

Date:

Date:

Date:

Date:

[sss-600-22]

Fadrowski Drum Disposal QAPPSection: 1Revision: 2Date: June 28, 1988Page 1 of 1

1.0 INTRODUCTION

The United States Environmental Protection Agency (USEPA) requires that

potentially responsible party (PRP) - lead Investigations under CERCLA have an

approved Quality Assurance Project Plan (QAPP). This requirement applies to

project environmental monitoring and measurement efforts mandated or supported

by the USEPA. It is the responsibility of the respondents or their

representatives to implement procedures to achieve and document data

precision, accuracy, completeness and representativeness.

This QAPP presents the organization, objectives, functional activities andspecific Quality Assurance (QA) and Quality Control (QC) activities associated

with the Remedial Investigation/ Feasibility Study (RI/FS) at the Fadrowski

Drum Disposal Site near Franklin, Wisconsin. The QAPP 1s designed to achieve

the specific data quality goals of the RI/FS.

This QAPP has been prepared using the following guidance documents:

1. USEPA, Region V, December 1985, Preparation of Federal-Lead RemedialInvestigation Quality Assurance Project Plans for Region V (Ref.l).

2. USEPA, December 1980, Interim Guidelines and Specifications forPreparing Quality Assurance Project Plans, QAMS-005/80 (Ref.2).

3. USEPA, June 1986, Data Quality Objectives for the RI/FS Process, Doc.No. 9355.0-7A (Ref.3).

Fadrowski Drum Disposal QAPPSection: 2Revision: 2Date: June 28, 1988Page: 1 of 4

2.0 TABLE OF CONTENTS

Section

1.0 TITLE PAGEINTRODUCTION

2.0 TABLE OF CONTENTS

3.0 PROJECT DESCRIPTION

4.0 PROJECT ORGANIZATION ANDRESPONSIBILITIES

5.0 QUALITY ASSURANCE OBJECTIVESFOR DATA MEASUREMENT

6.0 SAMPLING PROCEDURES

7.0 SAMPLE CUSTODY

8.0 CALIBRATION PROCEDURES ANDFREQUENCY, AND PREVENTATIVEMAINTENANCE FOR FIELD INSTRUMENTS

9.0 ANALYTICAL LABORATORY PROCEDURES

10.0 DATA REDUCTION, VALIDATION ANDREPORTING

11.0 INTERNAL QUALITY CONTROL CHECKS

12.0 PERFORMANCE AND SYSTEM AUDITS

13.0 PREVENTATIVE MAINTENANCE

14.0 SPECIFIC ROUTINE PROCEDURES USEDTO ASSESS DATA PRECISION, ACCURACYAND COMPLETENESS

Revision Date

1-1

2-1

3-1

4-1

5-1

6-1

7-1

8-1

9-1

10-1

11-1

12-1

13-1

14-1

2

2

2

2

2

2

2

2

2

2

2

2

2

2

June 28, 1988

June 28, 1988

June 28, 1988

June 28, 1988

June 28, 1988

June 28, 1988

June 28, 1988

June 28, 1988

June 28, 1988

June 28, 1988

June 28, 1988

June 28, 1988

June 28, 1988

June 28, 1988


15.0 CORRECTIVE ACTION 15-1 2 June 28, 1988

16.0 QUALITY ASSURANCE REPORTS TOMANAGEMENT 16-1 2 June 28, 1988

17.0 REFERENCES 17-1 2 June 28, 1988

18.0 GLOSSARY OF TERMS 18-1 2 June 28, 1988

LIST OF TABLES

Table FollowsNo. Title Page Revision Date

3-1 Maximum Concentration of Contaminants 3-5 2 June 28, 1988

3-2 Private Well and Surface Water MetalsResults 3-5 2 June 28, 1988

3-3 Private Well and Surface WaterOrganlcs Results 3-5 2 June 28, 1988

3-4 Sample Type and Estimated NumberSamples 5-5 2 June 28, 1988


LIST OF FIGURES

FigureNo. Title

3-1

3-2

4-1

7-1

7-2

7-3

7-4

Site Layout

Schedule of Tasks forDisposal RI/FS

Fadrowski Drum

Project Organization Chart

Cha1n-of -custody Record

Cha1n-of-custody Seal

Sample Identification

Sample Identification

Record

Record

FollowsPaqe Revision Date

2-5

5-5

2-2

7-1

7-2

7-3

7-3

2

2

2

2

2

2

2

June

June

June

June

June

June

June

28,

28,

28,

28,

28,

28,

28,

1988

1988

1988

1988

1988

1988

1988


LIST OF APPENDICES

Appendix Title Revision Date

A Sampling and Analysis Plan 2 June 28, 1988

B U.S. EPA CLP Target Compound List 2 June 28, 1988

C Autoanalyzer Operating Procedures 2 June 28, 1988for Alkalinity Chloride, Sulfate,and Total Cyanide Analyses

D Internal Cha1n-of-CustodyProcedure for Warzyn 2 June 28, 1988

E Internal Cha1n-of-CustodyProcedure for HazletonLaboratories America 2 June 28, 1988

F Document Control and theEvidentiary File System 2 June 28, 1988

G Field Measurement of pH andoperation Instructions Orion Model211 pH Meter 2 June 28, 1988

H Field Measurement of SpecificConductance and Temperature andOperating Instructions YSI Model 3333 Conductivity Meter 2 June 28, 1988

I Calibration and Maintenance ofPhotovac TIP 2 June 28, 1988

J Operation Procedure for HNU ModelPI 101 Photo1on1zat1on Analyzer 2 June 28, 1988

K Field Measurement of Hydraulic 0 June 10, 1988Conductivity - Slug Tests


3.0 PROJECT DESCRIPTIONThe RI/FS 1s designed to gather specific Information necessary to (1)

determine 1f the site presents a hazard to human health or to the environment,and (2) to evaluate potentially feasible remedial alternatives. The tasks andsubtasks are directed toward accomplishment of these primary objectives. TheFDD site 1s a PRP - lead Investigation.

3.1 BACKGROUND

The Fadrowski Drum Disposal (FDD) Site encompasses approximately 20 acres ofsemi-rural land 1n southeastern Wisconsin. It 1s located in the southeastquarter of section 1, T5N, R9E, 1n southern Milwaukee County. The address 1s6865 South 27 Street, Franklin, Wisconsin. The site 1s bounded by Menards,Inc. (Menards) on the north, by a tree line on the south, by 27th Street onthe east, and by an unnamed stream on the west (Figure 3-1).

From 1970 to 1981, Edward Fadrowski of Ed's Masonry and Trucking Inc.,operated the site as a landfill for demolition and construction waste. OnJuly 6, 1981, the Wisconsin Department of Natural Resources (WDNR) received acomplaint from Marda Smith, former secretary of Ed's Masonry and Trucking,who alleged that the property had been used for burial of hazardous waste.Smith said she had records to show that several hundred drums had been burledon the site, and several hundred cubic yards of lubricant sludge had been

burled. In June 1983, several burled drums were ruptured by earthmovlngequipment that were moving fill from the site for construction at Menards.Samples were collected and analyzed by the Wisconsin Department of NaturalResources (WDNR). The samples were found to contain Volatile Organic Compounds(VOCs), chromium, lead and traces of arsenic. One sample of oil sludge wasfound to contain the pesticide DDT. See Table 3-1 of QAPP for summary ofconcentrations.


Of potential environmental concerns are (1) contamination of soil on theproperty, which could act as a long term source of contamination to theenvironment, (2) potential contamination of shallow domestic wells 1n the

area, and (3) possible contaminant migration off site by way of the stream atthe western end of the property.

3.1.1 Surface Features of the SiteThe surface of the Fadrowski Drum Disposal Site can be divided Into threegeneral areas: the fill area, the staging area, and the unfilled area (Figure3-1). The fill area 1s about 200 feet by 600 feet, consisting of a mound ofconstruction debris, Including large sections of broken concrete withprotruding re-bar. It extends over one-third of the site and 1s located along

the eastern half of the southern boundary. The staging area, approximately

400 feet by 150 feet, 1s located between the fill area and the northernboundary and 1s the area 1n which barrels and trucks were apparently unloadedand where waste may have been burled.

A small pond, located near the middle of the site, appears to mark the end ofthe filled area. The western half of the site appears to be unfilled,although the surface has been graded and contoured to allow drainage towardthe stream.

3.1.2 Contamination Problem at the Site Based on Past Data.No previous detailed Investigations have been conducted at the Fadrowski DrumDisposal Site. The existing site Information consists of testimony by Ms.Smith, the report of drums being ruptured during earthwork at the site In June1983, and the results of 12 samples collected and analyzed by the WisconsinDNR. As described above, those samples were found to contain traces of VOC,heavy metals and DDT. A summary of past data 1s presented 1n Table 3-1. TheVOC analysis was a total VOC scan. No specific compounds were quantified orreported.

SOUTH 27TH STREET

— SITE INVESTIGATION BOUNDARY

—. — —— APPROXIMATE PROPERTY LINE

FENCE

FIGURE 3-1SITE LAYOUT

QUALITY ASSURANCE PROJECT PLANREMEDIAL INVCSTlGATION/FEASIBIUTr STUOTFADROWSKI DRUM DISPOSAL SITEFRANKLIN, WISCONSIN


Additional data were collected as part of a FIT Investigation conductedSeptember 25 and 26, 1985. Water quality results are listed 1n Tables 3.2 and3.3. The quality of metals data 1s suspect due to relatively high levels ofseveral metals 1n blank samples (Table 3.2). Most organic analytes wereundetected, with the exception of typical laboratory contaminants (Table 3.3).

3.2 PROJECT OBJECTIVES AND USE OF DATAThe objectives of the RI recommended for the Fadrowski Drum Disposal Site areto gather and assess Information needed to accomplish the following generalobjectives:

• Determine the characteristics and extent of contaminants,

• Define the pathways of contaminant migration,

• Define the physical features that could affect contaminant migration,containment or remediation,

• Quantify the risk to public health and the environment, and

• Gather Information necessary to support the FS.

The tasks, subtasks and activities are directed toward the accomplishment ofthese primary objectives.

The currently available data and information concerning the Fadrowski DrumDisposal Site are Insufficient to allow the development, screening andevaluation of remedial action alternatives. The full extent and concentrationof contaminants located 1n the surface and subsurface soils, groundwater,surface water and sediments on and near the site have not been determined.The determination of the adequacy of data will be done as part of the RIreport.

Once the data have been obtained and evaluated 1n the RI report, the followingtasks will be performed as part of the FS:

• Develop viable remedial action alternatives,

• Evaluate remedial action alternatives,

TABLE 3-1

MAXIMUM CONCENTRATIONS OF CONTAMINANTSFADROWSKI DRUM DISPOSAL SITE

SAMPLE

Green Sludge

White Sludge

Black Sludge

01 ly Water (7)

01 ly Water

Soil, Sludge

Paint Waste (10)

Paint Waste (11)

TotalMetals (PPM)

As,Pb,Cr,

As,Pb,

As,Pb,

Pb,

Pb,Cr,

< 532,7006,800

ND

<51,200

ND

ND

<5700

900

400< 100

EP MetalsTOX (PPM)

ND18ND

ND

ND2

ND

ND

ND0.6

1.8

NDND

FLASH POINT CF

95

98

>200

139

128

106

78

96

VOC1

Yes

ND

Yes

Yes

ND

Yes

ND

Yes

PESTICIDE

ND

ND

ND

DDT, 1,450

DDT, 21.1

ND

ND

ND

1 Only the presence or absence of VOCs are reported.

ND = not detected

RCW/SSS/SGW2[sss-600-21b]

TABLE 3.2

PRIVATE WELL AND SURFACE WATER METAL CONCENTRATIONSSEPTEMBER 25 AND 26, 1985

FADROWSKI DRUM DISPOSAL SITE

SampleDescription Borzokowski

EPA Sample t ME4880

Aluminum 227

Antimony 88

Arsenic 9u

Barium [53]

Beryllium 1.3u

Cadmiun 2.3u

Calcium 30,400

Chromium 3.4u

Cobalt 4.7u

Copper [17]

Iron 717

Lead 4.5u

Magnesium 22,500

Manganese 15

Mercury 0.8

Nickel [6.2]

Potassium [965]

Selenium 2u

Silver [9.4]

Sodium 49,100

Thallium 5u

Tin 14u

Vanadium [12]

Zinc 92

Concentrations are in ug/L.

Augie'sRestaurant

ME4882

623

130

9u

75

1.3u

2.3u

42,600

3.4u

4.7u

526

9,120

16

28,900

105

1.2

[4-3]

1,050

2u

5.2u

48,700

5u

14u

[7.7]

5,050

The three field blanks indicate varyingGenerally, sample concentrations < 5 x s

25389.00SGW2/SSS/SGU2[sss-600-21c]

Rate Puetz

ME4883 ME4885

[160] [183]

100 101

9u 9u

[29] 2.1u

1.3u 1.3u

2.3u 2.3u

21,400 [201]

3.4u 3.4u

4.7u 4.7u

[9.7] 7.8u

428 1084.5u 4.5u

12,600 [167]

[9.9] 1.2u

0.9 0.4

4.0u 4.0u

[520] 80u

2u 2u

5.2u [5.5]

49,400 [374]

5u 5u

14u 14u

[6.2] [5.6]

143 [3.5]

St. PaulSchool

ME4886

201

154

9u

[56]

1.3u2.3u

66,400

3.4u

4.7u

[9.6]

104

4.5u

53,600

[13]

0.9

4.0u

1,140

2u

[8.1]13,500

5u

50

[12]

145

ZignegoConstr.

ME4890

308

99

9u

[36]

1.3u

2.3u

47,800

3.4u

4.7u

7.8u

814

7.3

33,100

174

1.3

[6.9]

[965]

2u

[7.1]30,700

5u

14u

[9.3]

74

levels of contamination for Al. Sbthe amount found in any blank are

Surface 1

ME4887

4,740

101

9u

[139]

1.3u

2.3u

154,000

[6.1]4.7u

34

10,700

12

91,900

1,940

0.8

80

16,200

2u

5.2u

97,900

5u

14u

[18]

426

Surface 2

ME4892

9,320

70

9u

203

1.3u

2.3u

182,000

15

[6.6]

78

19,400

22

91,900

268

0.5

[37]

17,000

2u

5.2u

93,800

5u

[32]

[25]

767

, Ba, Ca, Cu, Fe, Pb, Mgnot considered positive

Surface

ME4888

24,500

92

9u

[154]

1.3u

2.3u

12,000

28

[13]42

28,700

12

66,800

483

0.9

[38]11,000

[2.3]5.2u

58,700

5u

14u

53

128

, Mn, Hgvalues.

3 Surface 4

ME4889

2,340

95

9u

[33]

1.3u

2.3u

29,300

[4.6]

4.7u

[17]2,650

15

11,800

59

1.1

133

[2.370]

2u

[7.7]

19,600

5u

51

[13]68

, Ni, K, Ag, NaMuch of this

FieldBlank

ME4881

378

72

9u

[57]

1.3u

2.3u

30,000

3.4u

4.7u

[23]

964

5.8

23,300

[14]2.2

[20]

[880]

2u

[8.3]

42,300

5u

14u

[11]100

, Snmetals

FieldBlank

ME4884

[148]

9u

9u

[51]1.3u

2.3u

40,700

3.4u

4.7u

7.8u

712

4.5u

28,200

23

1.7

4.0u

965

2u

5.2u

43,100

5u

[39]

[5.4]

78

V and Zn.data is

FieldBlank

ME4891

235

99

9u

2.1u

1.3u

2.3u

1,404

3.4u

4.7u

7.8u

[77]

4.5u

465

[2.7]

0.4

4.0u

80u

2u

[9.4]

[667]

5u

14u

[8-4]

31

suspect

TABLE 3.3

RESULTS OF PRIVATE WELL AND SURFACE WATER ORGANICS ANALYSISSEPTEMBER 25 AND 26, 1985. FADROUSKI DRUM DISPOSAL SITE

Location

PRIVATE WELLS

Borzokowski

Augies Restaurant

Katz

Volatiles

Compound Cone, (ppb)

ND

ND

ND

Semi-Volatiles


Puetz

St. PaulSchool

ZignegoConstr.

Methylene chloride

Methylene chloride

Methylene chloride

SURFACE WATER

Surface 1 ND

Surface 2 Methylene chloride

Surface 3 Methylene chloride

Surface 4 ND

ND

3 KDi(n)butylphalate

ND

110 Bis(2-ethylhexyl)phthalate 4 K

6 K ND

4 K ND

ND

76 ND

6 K ND

ND

Pesticides/PCBs


ND

ND

ND

ND

ND

ND

ND

ND

ND

ND

ND - Not Detected

K - Data qualifier indicating common laboratory contaminants at less than 10 times the amount found in blanks.

RCW/sss/SGW2[sss-600-21 a]


• Recommend the most cost-effective alternatives, and

• Prepare a conceptual design for the selected alternative.

3.3 OBJECTIVES OF SPECIFIC PROJECT ELEMENTSThe RI/FS Includes nine general tasks which are summarized 1n the Work Plan.The focus of this QAPP 1s limited to the data collection and environmentalmonitoring of RI Task 5, the Site Characterization. This task will focus onthe evaluation of the character and extent of contamination, the potentialroutes and extent of migration, and the environment 1n which the contaminantsexist. Data will be obtained 1n each of the following subtasks to support thescreening of alternatives and detailed evaluation of candidate remedial

alternatives:

• Waste characterization,

• Surface water and sediment Investigation,

• Site hydrogeologlc Investigation,

• Soils Investigation, and

• A1r Investigation.

The specific objectives of the subtasks are outlined as follows:

Waste Characterization

• Locate and Identify drummed waste, and

• Identify other sources of waste.

Surface Water and Sediment Investigation

• Assess the Impact of runoff from the site on the quality of the adjacentsurface water stream, and

• Determine the degree of contamination of the sediments and surfacewaters of the on-s1te pond.


Site Hydroqeoloqlc Investigation

• Install monitoring wells to Identify groundwater flow direction andgradient,

• Calculate groundwater seepage velocity, and

• Identify environmental Impact of burled waste on the groundwater system.

Soils Investigation

• Define the characteristics of materials dumped at the site,

• Determine the volumes and concentration levels of chemicals 1n soilsdistributed over the site area; assess the spatial variability ofchemical occurrence,

• Define naturally occurring background concentration ranges of chemicalsin soils 1n the Immediate site vicinity and 1n similar ecosystems sothat comparisons with residual on-s1te concentrations can be evaluated,and

• Assess the physical characteristics of the soils at the site.

A1r Investigation

• Establish background levels through on-s1te ambient air qualitymonitoring

Complete descriptions of the Site Investigation subtasks are provided 1n theSampling and Analysis Plan (SAP), attached 1n Appendix A. The SAP describesthe field activities Involved 1n sample collection during performance of theRemedial Investigation at the Fadrowski Drum Disposal Site. A listing of testparameters, sample types and estimated sample numbers 1s presented in Table3-4.

3.4 SCHEDULEA project schedule 1s presented 1n Figure 3-2. The final RI report should becomplete within approximately 9 months after Initiation of field work and theFS within an additional 9 months. Quality assurance systems audits arescheduled during both the RI and FS phases.

TABLE 3-4SAMPLE TYPES AM) ESTIMATE]) SAMPLE NUMBERS


(1)MATRIX

TEST PITSTEST PITSTEST PITSTEST PITSTEST PITS

SOILSOILSOILSOILSOIL

SEDIMENTSEDIMENTSEDIMENTSEDIMENTSEDIMENT

SURFACE WATERSURFACE WATERSURFACE WATERSURFACE WATERSURFACE WATERSURFACE WATERSURFACE WATER

GROUNDWATERGROUNDWATERGROUNDWATERGROUNDWATERGROUNDWATERGROUNDWATERGROUNDWATER

(2)LAB

HAZLETONHAZLETONHAZLETONHAZLETONWARZYN



FIELDHAZLETONHAZLETONHAZLETONHAZLETONWARZYNWARZYN


NO. OFSAMPLES

444A

4

2625262626

2626262626

4444A

4A

888a888

FIELDDUPLICATES

111\1

33333

aa333

—j111\1

—111111

(3)FIELDBLANKS

0000O

O0OOO

OOOOO

—111111

—111111

WMATRIXSPK/DUP

00000

O0O00

00000

—21j

———

—211

——~~

TOTALSAMPLES

66666

2828282828

2828282828

4877006

g

121111101O1O

toTEST PARAMETERS

EPA TCL VOCsEPA TCL BNAsEPA TCL PEST/PCBsEPA TCL METALSCYANIDE

EPA TCL VOCsEPA TCL BNAsEPA TCL PEST/PCB.EPA TCL METALSCYANIDE


pH, CONDUCTIVITY, TEMPERATUREEPA TCL VOCsEPA TCL BNAsEPA TCL PEST/PCBsEPA TCL METALSCYANIDEALKALINITY, CHLORIDE, SULFATE


(1) Sot I, sediment and water matrix samples w t l I be considered low concentration samples.Samples from excavations w l 1 1 be considered medium level samples.

(2) HAZLETON: Hazleton Laboratories AmericaWARZYN: Warzyn Analytical LaboratoryFIELD: Field Analysis

(3) A trip blank for purgeables w i l l be included with each shipment for leachate andgroundwater samples.

(4) Sample numbers reflect extra volumes required for matrix spike/matrix spikeduplicate analysis.

(5) See Appendix B Tor EPA TCL analyte list. pH, conductivity and temperature w i l l bedetermined in the field for surface and groundwater.

MSR/msr/RCW[MSR-VAX, 6/28/88]

FIGURE 3-2. SCHEDULE OF TASKS FOR REMEDIAL INVESTIGATION AT FAOROWSKI

TASK ^EEK

Initial Project Scoping

Planning 4 ManagementWork PlanOAPPSampling 4 Analysis PlanData flanage»ent PlanEndangertent Assessment Plan

Initial Activities

Site Characterization

Site Investigation AnalysisTechnical leisoranda No. 1Technical Memoranda No. 2Technical Memoranda No. 3Technical fleioranda No. 4

Endangerient Assessment

QA/OC 4 Manageient

Draft RI Report

Agency Review

Public Cowent on Draft RI

Final RI Report

Draft FS Report

Agency Review

Conceptual Design

Agency Review

•"ublic Cowient

Final FS Report

Monthly Report

1 2 3 4

f»*m

*t+i++t++t+t*+mt

t*++++*+t+++

t

1 2 3 4

5 6 7 8

mOOOOOOOOOtt+000000000H+000000000H+000000000mOOOOOOOOO

t

5 6 7 8

9 10 11 i:

000/H++++OOO+'W'H000+H+++000++H+*000++++++

+M

++•

f

9 10 11 1;

65 66 67 68

000000000000

t

65 66 67 68

69 70 71 72

000000000000

+

69 70 71 72

73 74 75 76

tm++H-m+

t

73 74 75 76

77 78 79 80

t

77 78 79 80

81 32 83 84

t -f + +

t

81 82 83 84

LEGEND:» = Uarzyn0 = Agency ReviewL = Laboratory Analysis


4.0 PROJECT ORGANIZATION AND RESPONSIBILITY4.1 OVERALL RESPONSIBILITY

• Acme Printing Ink Company

• Michael J. Radcliffe, Project ManagerWarzyn Engineering Inc.

• Robert E. Whippo, Remedial Project ManagerU.S. EPA, Region V

• RI/FS Reports and Technical Memorandumprepared by Warzyn Engineering Inc.

4.2 MONITORING AND SAMPLING OPERATIONS AND QC

• Principal Engineering Firm - Warzyn Engineering Inc.

• Drilling - Exploration Technology, Inc.

• Sampling, Monitoring and Survey - Warzyn Engineering Inc.

• Quality Control - Richard W. Maurer, Warzyn Engineering Inc.

4.3 LABORATORY ANALYSES AND QC

• Analysis of test pit, soil, sediment, surface water and groundwatermatrix samples for EPA TCL VOCs, BNAs, Pest/PCBs and metals

- Hazleton Laboratories America

• Analyses test pit, soil, sediment for cyanide and surface water andgroundwater for cyanide, alkalinity, sulfate, chloride, field pH andfield specific conductance.

- Warzyn Engineering Inc.

4.4 SPECIALIZED RESPONSIBILITIES FOR LABORATORY SERVICES

• Hazleton

- analytical protocol specified - Warzyn Engineering Inc.

- review of analytical protocol - U.S. EPA Region V Quality AssuranceSection (QAS) and Central Regional Laboratory (CRL), Contract ProgramManagement Section (CPMS)


- Review and approval of performing laboratory - U.S. EPA Region V CPMS,CRL

- Internal QA/QC - Hazleton Staff


- Review of tentatively Identified compounds and assessment of need forconfirmation - Warzyn Engineering Inc.

• Warzyn Engineering Inc.

- Review of analytical protocol - USEPA Region V QAS and CPMS, CRL

- Review and approval of performing laboratory - U.S. EPA Region V CPMS,CRL

- Internal QA/QC - Warzyn Engineering Inc.


4.5 QUALITY ASSURANCE

• Overall QA Responsibility

- Warzyn Quality Assurance Officer

• Warzyn Subcontracted Activities- Warzyn Engineering Inc.

• Review of QAPP- U.S. EPA Region V QAS and CPMS, CRL

• Field Analysis- Warzyn Engineering Inc.


• Field Operations

- QAO, Warzyn Engineering Inc.- U.S. EPA Oversight Contractor

• Analytical Laboratories- U.S. EPA CPMS, CRL

• Evidence Audits- QAO, Warzyn Engineering Inc.

An organization chart is shown 1n Figure 4-1.

U.S. EPA REGION V

R. Whippo

ACME PRINTING INK CO.

PROJECT MANAGER

CORPORATE HEALTHAND SAFETY

0. WoodsWarzyn

QUALITY ASSURANCEOFFICER

M. RadcliffeWarzyn

R. MaurerWarzyn

REMEDIAL INVESTIGATION FEASIBILITY STUDY REMEDIAL DESIGN SUBCONTRACTORS

0. LawtonWarzyn

R. HuMfordWarzyn

M. RMlchWarzyn

HazletonETI

FIGURE 4-1

IUIO

YN

I »O

SI

DWN"d£, APPDMS.R. DATE fc/21/88 25389 A13

WARZYN PROJECT OHOAMZATION CHART

QUALITY ASSURANCE PROJECT PLANREMEDIAL INVESTIGATION/FEASIBILITY STUDYFAOROWSKI DRUM DISPOSAL SITEFRANKLIN. WISCONSIN


5.0 QUALITY ASSURANCE OBJECTIVES FOR DATA MEASUREMENTThe overall QA objective 1s to develop and Implement procedures for fieldsampling, cha1n-of-custody, laboratory analysis and reporting that willprovide legally defensible results in a court of law. Specific procedures tobe used for sampling, cha1n-of- custody, calibration, laboratory analysis,reporting, Internal quality control, audits, preventative maintenance andcorrective actions are described 1n other sections of this QAPP. This sectiondefines the goals for levels of QC effort:

• Accuracy, precision and sensitivity of analyses;

• Completeness, representativeness, and comparability of measurement datafrom project analytical laboratories, and

• Quality assurance objectives for field measurement methods.

5.1 LEVEL OF QC EFFORTField duplicate, matrix spike and matrix spike duplicate, field blank and tripblank samples will be taken and submitted to the analytical laboratories toprovide the means to assess the quality of the data resulting from the fieldsampling program. Duplicate samples will be analyzed to check for samplingand analytical reproduc1bH1ty. Blank samples will be analyzed to check forprocedural contamination and/or ambient conditions at the site that may causesample contamination.

The general level of QC effort for sample matrices will be one field duplicateper 10 investigative samples and both one matrix spike/matrix spike duplicateand one field blank per 20 Investigative samples. A trip blank for volatileorganlcs will be included with each volatlles shipment. The specific level ofQC effort for the Fadrowski Drum Disposal Site RI/FS 1s described 1n Section3-4.


Surface water, sediment, soil and groundwater samples collected at the sitewill be analyzed using Contract Laboratory Program (CLP) protocols for CLP

target volatile, semi-volatile and pest1c1de/PCB compounds and Inorganics(metals and cyanide) listed 1n Appendix B. The level of QC effort for the CLP

protocol analyses 1s described for organlcs and Inorganics in CLP SOW 7/87 (ormost recent).

The level of QC effort for analysis of water quality Indicator parameters,Including alkalinity, chloride and sulfate, are described 1n methods provided1n Appendix C. The level of QC effort for field measurement of pH consists ofpremeasurement calibration and a post-measurement verification using twostandard reference solutions. QC effort for field determination of specificconductance will Include Initial and continuing calibration of the Instrumentusing a standard solution of known specific conductance.

5.2 ACCURACY. PRECISION AND SENSITIVITY OF ANALYSESThe QA objectives of analyses with respect to accuracy, precision andsensitivity are to achieve acceptable data based on specified performancecriteria. Accuracy and precision requirements and method detection limits forCLP protocol analyses are described 1n CLP SOW 7/87 (or most recent).Accuracy and precision criteria and required detection limits for other

proposed analyses are listed with method descriptions 1n Appendix C.

The accuracy of field measurements of pH and conductivity will be assessedthrough premeasurement calibrations and post-measurement verifications asdescribed 1n Appendix D and F, respectively. Precision will be assessedthrough duplicate measurements (the electrode will be withdrawn, rinsed withdeionlzed water, and re- Immersed between each duplicate). The calibration

and verification will be done before the first duplicate and after the last.

The level of QC effort for ambient air monitoring with the HNu Phot1on1zer(10.2 eV lamp) or Photoval TIP will consist of premeasurement calibration.Maintenance and procedures for operation are given 1n Appendices I and J for

the TIP and HNu, respectively.


5.3 COMPLETENESS. REPRESENTATIVENESS. AND COMPARABILITYIt 1s anticipated that at least 95X of analyses will provide results meetingacceptance criteria. Sampling methods and locations are designed to provideresults representative of the matrix at the sampling point. The samplingmethods, analytical methods and level of QC effort used will providecomparable data, which will supplement prior data collected at the site.


6.0 SAMPLING PROCEDURES

Specific sampling procedures used are documented in the Sampling and AnalysisPlan (SAP) (Appendix A). Sample quantities, preservatives, packaging methods,test parameters and laboratory designations are summarized 1n Tables 2-1 and2-2 of the SAP.


7.0 SAMPLE CUSTODYProject samples will be collected under cha1n-of-custody procedures. Chain-of-Custody protocol will follow National Enforcement Investigation Center(NEIC) policies (Ref. 5) and User's Guide to the Contract Laboratory Program(Ref. 4) Including use of chain- of-custody forms, custody seals, sampleIdentification records, sample tags, container labels and field notebooks forsample documentation. Standard forms, including cha1n-of-custody recordforms, sample labels, sample Identification record forms and cha1n-of-custodyseals, will be maintained.

7.1 Chain-of-Custody RecordA copy of the cha1n-of-custody form to be used for the Fadrowski Drum DisposalSite RI/FS 1s shown in Figure 7-1. Form Requirements:

- One form per shipping container (steel/foam cooler)

- Carrier service does not need to sign form, 1f custody seals remainintact during shipment

- Use for each project sample

7.2 Cha1n-of-Custody SealAn example of the cha1n-of-custody seal to be used for sample shipping for theFadrowski Drum Disposal Site RI/FS 1s shown 1n Figure 7-2. Seal Requirements:

- Two (2) seals per shipping container attached to the cooler I1d toprovide evidence that samples within have not been tampered with.

- Cover seals with clear tape prior to shipping sample containers.

- Record seal numbers on cha1n-of-custody forms as well as sampleIdentification record forms.

WARZYN

CHAIN OF CUSTODY RECORD

Wnzyn Engine-rung meOne Science Couit

Univcilily Rcsc.vcti P.<i>CO Bo« S3B';

adnon U/nconjin 5370!)(608) 273-0-HO

PRO). NO I'KOirCTNAME

SAMPLERS:

LAB NO. DATE TIME STATION LOCATION

NO.

OF

CON-

TAINERS

REMARKS

Relinquished by:

l by: H;/;H,II

D.ilc / Time Received by . (Si(;M.iim<.-j

RolilK|llisllL'(l by: /^i^n.tl

D.ue /

O.ile / I line

Received by: i

KIM.'I'lved by:

Relinf|uislu-(l by: (•"/.•"•"

Remarks

!<!(•(civ(r( I for I .ib< n ,i l< >i y by: fS^-d


7.3 SAMPLE LABELS

A copy of the sample label to be used for the Fadrowski Drum Disposal SiteRI/FS is shown In Figure 7-3. Label Requirements:

• Each sample container must have a sample label affixed to 1t. Labelwill specify parameters for analysis and preservative used.

• Record sample label numbers on the cha1n-of-custody and sampleIdentification record forms.

• Use for each project sample.

7.4 Sample Identification Record FormAn example of the sample Identification record form to be used for theFadrowski Drum Disposal Site RI/FS 1s shown 1n Figure 7-4. The form is toprovide the means of recording critical shipping and tracking Information.The form will include Information such as:

• Sample number• Sample matrix• Sample location code• Sample round• Chain of custody• Lab code• Date sampled• Date shipped• Airbill number• Sample label number

The documentation accompanying the samples shipped to the laboratory win besealed 1n a plastic bag taped to the Inside of the cooler lid. Thisdocumentation 1s to Include: a cha1n-of-custody record for the accompanyingsamples, sample labels attached to each sample, and two chain-of-custody sealsplaced over the cooler lid. The lid of the sample cooler will be securelytaped shut prior to shipment. The Field Data Coordinator (FDC) and theSampling Manager (SM) will be responsible for collecting the sample,completing the sample documentation and properly packaging the samples forshipment to the laboratory.

uac.

I

r\j WARZYN

O

C

Oa.

5 0 3

CHAIN OF CUSTODY SEALWARZYN ENGINEERING INC.

ONE PIERCE PLACESUITE 1110 W.

ITASCA, IL 60143-2681(312)773-8484

ft)a>


Once in the laboratory's possession, sample custody will be the responsibilityof the laboratory sample custodian.

7.5 LABORATORY CHAIN-OF-CUSTODYLaboratory analyses will be performed by either CLP RAS or CLP SAS protocols,as approved by the Central Regional Laboratory, Contract Project ManagementSection for USEPA Region V. Under the CLP program, performing laboratoriesare required to have written and approved standard operating proceduresdetailing Internal cha1n-of-custody. These procedures are outlined forHazleton 1n Appendix E. The Internal laboratory chain-of-custody requirementsfor Warzyn's analytical laboratory are detailed 1n Appendix D.

7.6 FINAL EVIDENCE FILEOriginal data generated through Hazel ton will be retained by Warzyn. Copies

of Hazel ton data and original field data will be retained by Warzyn. Warzynwill maintain the final evidence file. Warzyn's document control andevidentiary file system 1s described 1n detail in Appendix F. Upon completionof the project, Warzyn will audit the evidence file for completeness.

AN

ALY

TIC

AL

SER

VIC

ESW

AR

ZY

NE

HO

IME

6B

INC

IH

C

On

o S

clo

nco

C

ou

rtU

nlv

ors

lly R

ese

arc

h P

ark

P.O

. B

ox 5

38

5M

ad

iso

n,

Wl

53

70

5(6

08)

27

3-0

44

0

Project *

Sampla Name

Date Collected

Parameters)

Preservatives)

Lab a

By

F i g u r e 7 - 3 S a m p l e l a b e l

O „'

; 3:

cc.Q

-J a:M UJco aa; r

•< 2

Qu

U a,H a,< HQ X

Qu

Id J£-1 a.< EQ <

U,0 >

Q2 OM £-,< inX DO (J

uto m< EJ D

2

fflJ

w o£^ ua, caz s< Ov> 2

XH

E-

a0 a;

to Zoo D< 2U

]

j1

1

]

-

F i g u r e 7 - 4 S a m p l e I d e n t i f i c a t i o nRecord.


8.0 CALIBRATION PROCEDURES, FREQUENCY ANDPREVENTATIVE MAINTENANCE FOR FIELD INSTRUMENTS

Instruments will be Inspected and calibrated at Warzyn's analytical laboratoryprior to being taken to the field. Calibration and maintenance of pH andspecific conductance meters are detailed 1n Appendices G and H. In the field,the pH meter will be calibrated using the two-buffer standardization methodprior to use. Calibration will be verified using a pH 7 buffer every fifthsample. The conductivity meter will be tested dally using a check standard.If readings vary more than 5% from expected values, the unit will be replaced.

Calibration of survey instruments used for health and safety purposes willfollow procedures recommended by the manufacturer (Appendices I and J). TheHNu and TIP will be calibrated to read in benzene equivalents at the beginningof each work day using standard calibration gas (isobutylene) supplied by HNu.

The calibration for laboratory instruments used for CLP protocol analyses will

be consistent with CLP SOW 7/87 or the most recent procedures. Operatingprocedures for the Indicator parameter analyses (alkalinity, chloride andsulfate) are contained in Appendix C.


9.0 ANALYTICAL LABORATORY PROCEDURES9.1 HAZELTON LABORATORIES AMERICA. INC.

Samples analyzed by Hazelton for CLP target volatiles, sem1-volat1les,pest1c1des/PCBs and Inorganics (see appendix B for parameter list) will followCLP protocols outlined 1n CLP SOW 7/87 or the most recent procedures.

9.2 WARZYN ENGINEERING INC.Analytical and calibration procedures are documented 1n the Individual SOPs inAppendix C.


10.0 INTERNAL QUALITY CONTROL CHECKS

Internal quality control for CLP protocol analyses will follow specificationsin CLP SOW 7/87 or the most recent procedures.

Required internal quality control analyses and their frequencies for Indicatorparameters are specified 1n methods descriptions in Appendix C.


11.0 DATA REDUCTION, VALIDATION AND REPORTINGData reduction for CLP protocol analyses will follow CLP SOW 7/87 or the mostrecent procedures. Data reduction methods for general water quality Indicatorparameters are listed with method descriptions 1n Appendix C.

Validation of organlcs data will be performed using guidelines developed 1nTechnical Directive Document No. HQ-8410-01, Laboratory Data Validation,Functional Guidelines for Evaluating Organics Analyses, May 1985 (Ref. 6).Inorganics data validation will be performed based on Laboratory Data

Validation, Functional Guidelines for Evaluating Inorganics Analyses,November, 1985 (Ref. 7). Data validation for general water quality Indicatorparameters will consist of comparisons of results of quality control sampleswith stated performance criteria. If results meet performance criteria, datawill be considered acceptable.

Data for CLP protocol analyses will be presented 1n CLP data package format.For general water quality Indicator parameters, raw data will be reported,Including results of calibration standards, duplicates, blanks, matrix spikesand performance evaluation samples. The specific reporting format 1sunspecified.



USEPA Region V, Central Regional laboratory, Contract Project ManagementSection (CPMS) will audit performing laboratories as a basis for approval ordisapproval for the requested analyses. Performance audits are to beperformed as specified In CLP SOW 7/87 for analyses by CLP protocols.Performance audits with Independent QC samples are to be performed asspecified 1n Individual SOP descriptions found 1n Appendix C.

The Quality Assurance Manger (QAM) will monitor and audit performance of theQA procedures, so that the project 1s performed 1n accordance with approvedquality assurance procedures. Audits may be scheduled at various times toevaluate the execution of sample Identification, sample control, cha1n-of-custody, field notebooks and sampling procedures.


13.0 PREVENTATIVE MAINTENANCEPreventative maintenance of instrumentation will be performed as stated 1nSection 3.0 and Appendices G, H, I, J and K.


14.0 SPECIFIC ROUTINE PROCEDURESUSED TO ASSESS DATA PRECISION ACCURACY AND COMPLETENESS

Data assessment will be performed by Warzyn. Assessment of organlcs data willbe performed using guidelines developed 1n Technical Directive Document No.HQ-8410-01, Laboratory Data Validation, Function Guidelines for EvaluatingOrganlcs Analyses, May 1985 (Ref. 6). Inorganics data assessment will beperformed based on guidelines in Laboratory Data Validation, FunctionGuidelines for Evaluating Inorganics Analyses, November, 1985 (Ref. 7).Accuracy and precision definitions are described 1n the CLP SOW 7/87 foranalyses performed using CLP protocols.

Routine procedures for assessing results of quality control samples forgeneral water quality Indicator parameters will Include relative percentdifference for duplicate samples and percent recoveries for matrix spike andany performance evaluation (PE) samples that are analyzed.


15.0 CORRECTIVE ACTIONIf quality control audits result 1n detection of unacceptable conditions ordata, the Warzyn QAM will be responsible for developing and initiatingcorrective action. Corrective action may Include:

• Re-analysis of the sample 1f holding time criteria permits,

• Resampling and re-analysis,

• Evaluating and amending sampling and analytical procedures, and

• Accepting data, acknowledging the level of uncertainty.


16.0 QUALITY ASSURANCE REPORTS TO MANAGEMENTA separate QA report for this project 1s not anticipated. The final RI reportand FS report will contain separate QA sections that summarize project dataquality.


17.0 REFERENCES

1. USEPA, 1985, "Preparation of Federal-Lead Remedial InvestigationQuality Assurance Program Plans for Region V," Draft, Region V QualityAssurance Office, April.

2. USEPA, 1980, "Interim Guidelines and Specifications for Preparing QualityAssurance Project Plans," QAMS-005/80, December.

3. USEPA, 1986, "Data Quality Objectives for the RI/FS Process," DocumentNo. 9355.0-7A.

4. USEPA, 1984, "User's Guide to the EPA Contract Laboratory Program," SampleManagement Office, October.

5. USEPA, 1983, "NEIC Policies and Procedures," National EnforcementInvestigations Center, EPA-330/9-78-001-R, May 1978, Revised February1983.

6. USEPA, 1985, "Laboratory Data Validation, Functional Guidelines forEvaluating Organlcs Analyses," Hazardous Site Control Division, TechnicalDirective Document No. HQ-8410-01, May.

7. USEPA, 1985, "Laboratory Data Validation, Functional Guidelines forEvaluating Inorganics Analyses," Office of Emergency and RemedialResponse, November.


18.0 GLOSSARY OF TERMS

ACCURACY - The degree of agreement of a measurement (or an average ofmeasurements of the same thing), X, with an accepted reference or true value,T, usually expressed as the difference between the two values, X-T, or thedifference as a percentage of the reference or true value, 100 (X-T)/T, andsometimes expressed as a ratio, X/T. Accuracy 1s a measure of the bias 1n asystem.

AUDIT - A systematic check to determine the quality of operation of somefunction or activity. Audits may be of two basic types: (1) system auditsthat consist of a review of the quality control system to ensure that acomprehensive set of quality'control methods, procedures, reviews, and sign-off approvals 1s established or in place, and (2) performance audits in whichproject activities are observed 1n process for their compliance with theestablished quality control procedures and requirements.

COMPARABILITY - Expresses the confidence with which one data set can becompared to another.

COMPLETENESS - A measure of the amount of valid data obtained from ameasurement system compared to the amount that was expected to be obtainedunder normal conditions.

DATA VALIDATION - A systematic process for reviewing a body of data against aset of criteria to provide assurance that the data are adequate for theirIntended use. Data validation consist of data editing, screening, checking,auditing, verification, certification, and review.

ENVIRONMENTALLY RELATED MEASUREMENTS - A term used to describe field andlaboratory Investigations that generate data Involving (1) the measurement ofchemical, physical, or biological parameters in the environment; (2) thedetermination of the presence or absence of criteria or priority pollutants inwaste streams; (3) assessment of health and ecological effect studies; (4)conduct of clinical and ep1dem1olog1cal Investigations; (5) performance ofengineering and process evaluations; (6) study of laboratory simulation ofenvironmental events; and (7) study of measurement on pollutant transport andfate, Including diffusion models.

PRECISION - A measure of mutual agreement among Individual measurements of thesame property, usually under prescribed similar conditions. Precision is bestexpressed 1n terms of the standard deviation. Various measures of precisionexist depending upon the "prescribed similar conditions".

QUALITY ASSURANCE - The total Integrated program for assuring the reliabilityof monitoring and measurement data. A system for Integrating the qualityplanning, quality assessment, and quality Improvement effort to meet userrequirements.


QUALITY ASSURANCE PROGRAM PLAN - An orderly assemblage of management policies,objectives, principles and general procedures by which an agency or laboratoryoutlines how it Intends to produce data of known and accepted quality.

QUALITY ASSURANCE PROJECT PLAN - An orderly assemblage of detailed andspecific procedures which delineates how data of known and accepted qualityare produced for a specific project (a given agency or laboratory would haveonly one quality assurance program plan, but would have a quality assuranceproject plan for each of Its projects.)

QUALITY CONTROL - The routine application of procedures for obtainingprescribed standards of performance 1n the monitoring and measurement process.

REPRESENTATIVENESS - Expresses the confidence with which one data set can becompared to another.

[sss-600-21]

APPENDIX A

SAMPLING AND ANALYSIS PLAN

REVISION: 2

TABLE OF CONTENTS

PAGE

1.0 INTRODUCTION 11.1 SAMPLING MEMBERS RESPONSIBILITIES 1

1.1.1 Sampling Manager 11.1.2 Sampling Team Members 11.1.3 Field Data Coordinator 11.1.4 Site Health and Safety Coordinator 2

2.0 GENERAL SAMPLING INFORMATION 22.1 SCOPE 22.2 SAMPLE SHIPMENT 32.3 QUALITY CONTROL REQUIREMENTS 3

2.3.1 Field Duplicates (FD) 32.3.2 Field Blanks 42.3.3 Trip Blanks (TP) 42.3.4 Matrix Spike and Matrix Spike

Duplicates (MS/MSD) 4

3.0 SAMPLING LOCATIONS AND PROCEDURES 53.1 WASTE CHARACTERIZATION 53.2 SURFACE WATER SAMPLING 63.3 SEDIMENT SAMPLING 73.4 SOILS SAMPLING 83.5 SITE HYDROGEOLOGIC SAMPLING 8

3.5.1 Monitoring Well Installation 83.5.2 Groundwater Sampling 93.5.3 Aquifer Characteristics 10

3.6 AIR SAMPLING 103.7 FIELD TESTS OF pH, TEMPERATURE AND CONDUCTIVITY 10

4.0 DECONTAMINATION PROCEDURES 114.1 PERSONNEL DECONTAMINATION 114.2 EQUIPMENT DECONTAMINATION 114.3 SAMPLE BOTTLE DECONTAMINATION 124.4 RI GENERATED WASTES 12

5.0 DOCUMENTATION 135.1 FIELD LOG BOOKS 135.2 SAMPLE IDENTIFICATION DESIGNATION 14

5.2.1 Project Identifier 145.2.2 Sample Type and Location Code 145.2.3 Sampling Event 155.2.4 Example of Sample Numbers 15

5.3 PHOTOGRAPHS 155.4 SAMPLE DOCUMENTATION 15

TABLES

Table 2-1 Sample Quantities, Bottles, Preservation, PackagingRequirements for Water, Sediment, and Soil Samples

Table 2-2 Sample Type and Estimated Number

LIST OF FIGURES

FollowsPage

FollowsPage

Figure 2-1 Summary of Phased Approach to RI/FSat the Fadrowski Drum Disposal Site

Figure 3-1 Proposed Test Locations for Waste Characterization

Figure 3-2 Proposed Surface Water & Sediment Sample Location

Figure 3-3 Proposed Preliminary Locations for Soil Borings

Figure 3-4 Proposed Locations for Phase I Monitoring Wells

5

6

8

8

[sss-600-20b]

Fadrowski Drum Disposal QAPPAppendix ARevision: 2Date: June 28, 1988Page: 1 of 16

1.0 INTRODUCTIONThis Sampling and Analysis Plan (SAP) describes the field activities Involvedin sample collection during performance of the Remedial Investigation (RI) atthe Fadrowski Drum Disposal Site 1n Franklin, Wisconsin. The plan documentsthe procedures which the sampling team personnel will follow.

1.1 SAMPLING MEMBERS RESPONSIBILITIES

Field sampling will be performed by Warzyn Engineering Inc. (Warzyn).Responsibilities of the sampling members are described below.

1.1.1 Sampling ManagerThe Sampling Manager (SM) will be responsible for the sampling efforts. TheSM will make available and maintain sampling equipment and materials, and will

provide for shipping and packing materials. The SM will supervise thecompletion of cha1n-of-custody records and the proper handling and shipping ofthe samples collected. The SM will be responsible for the accurate completionof field log books and provide close coordination with the Field DataCoordinator (FDC).

1.1.2 Sampling Team MembersThe Sampling Team Members (STM) will perform field measurements, collectsamples and transfer them for shipping. The STM will decontaminate samplingequipment as directed by the SM.

1.1.3 Field Data CoordinatorThe Field Data Coordinator (FDC) will remain 1n the Support Area and willassume custody of samples from the sampling team. The FDC will be responsiblefor the completion of cha1n-of-custody and sample traffic control forms. TheFDC will also be responsible for maintaining communications with on-s1te andoff-site personnel.


1.1.4 Site Health and Safety CoordinatorThe Site Health and Safety Coordinator (SHSC) 1s responsible for dallysupervision and documentation of safety, decontamination, environmentalmonitoring, and field medical monitoring activities. The SHSC 1s responsiblefor directing field personnel to comply with the provisions of the Site Healthand Safety Plan and has the authority to stop work 1n the event of safetyviolations. The SHSC 1s responsible for designating and marking restrictedareas during various site activities and for redeslgnatlng these areas asunrestricted, as appropriate.

2.0 GENERAL SAMPLING INFORMATION

2.1 SCOPEThe site Investigation at Fadrowski Drum Disposal Site will Involve collectingsoil, sediment, surface water and groundwater samples. If necessary, a secondphase of investigation will be designed for contaminated areas Identifiedduring the first phase (See Figure 2.1). It 1s probable that Phase II sampleswould only be analyzed for Indicator parameters. An air quality survey of theFadrowski Drum Disposal Site will evaluate the general quality of the ambientair within the site. The designated number of stations for each type ofsampling during the RI/FS per phase 1s as follows:

Sample Type Number of Sampling Stations

Soil Samples 25Waste Samples 4Surface Water Samples 4Sediment Samples 4Monitoring Wells 8

The planned sampling effort Includes one round of sampling at each designated

station. The location of stations and the procedures for collection andcompositing of samples are discussed 1n Section 3.0 for each samplingactivity.

SUMMARY OF PHASED APPROACH TO RI/FSFKKWSKI DRUM DISPOSAL SITE

FRANKLIN, WISCONSIN

REMEDIAL INVESTIGATIONPHASE I

REMEDIAL INVESTIGATION REMEDIAL INVESTIGATIONPHASE III FEASIBILITY STUDY

Evaluate potentialcontamination 1n:

A1rSurface WaterSedimentSoilGroundwater

\/

Delineate <contanrinatlregions shecontaminatePhase I in\

octent ofon 1njwn to beidln the(estlgatlon.

\/

Examine complexcontaminantdistributions andInvestigate complexInteractions withinthe natural system.

\/

\/\/

Conduct a FeasibilityStudy based on thedata base developed1n the previousphases.

PHASE I GOALS;

SURFACE WATER• Define upgradientand downgradlentwater quality andsediment quality.

SOIL• Detect near-surfacezones of contamin-ation and sourcesof hazardouschemicals.

GROUrCUATER• Determine 1f upper

aquifer 1s contaminated.Determine verticaland horizontaldirections andgradients.

ow

AIR QUALITY• Evaluate site-wide

air quality.• Identify sources of

air pollution.

PHASE II GOALS;

SURFACE WATER• Pinpoint sources of

contaminationdetected 1n Phase I.

SOIL• Delineate horizontaland vertical extent ofcontamination Incontaminated zonesIdentified In Phase I.

GRDUTCUATER• Delineate vertical andhorizontal contaminantplime distribution 1nshallow aquifer.

• Determine characteristicsof upper aquifer.

PHASE III GOALS:

SOILRefine delineation ofcontamination to minimizeremediation costs.

GROUMMTER• Simulate groundwater flow

and contaminant transport1n aquiferircdeTHng.

FEASIBILITY STUDY GOALS:

• Develop remedial actionalternatives.

• Evaluate the alternatives.

• Recarmend the "best"altematlve(s).

• Prepare a conceptualdesign for the selectedaTtemat1ve(s).


2.2 SAMPLE SHIPMENT

Following sample collection, the sample bottles will be decontaminated 1n theContamination Reduction Zone. The SM and/or STM will help the FDC preparedocumentation and package the bottles for shipment. Bottles will be labeledwith all required Information and this information recorded. Sample bottleswill be placed in coolers for storage and shipment as Indicated in Table 2-1.Ice will be sealed in plastic bags to prevent leakage. The bottles will be

cushioned using plastic foam, vermlculite or other similar packing material.Samples will be shipped to designated laboratories as indicated 1n Table 2-2.

2.3 QUALITY CONTROL REQUIREMENTSThe sampling activities will Include the following procedures for purposes ofquality control:

• Collection of field duplicates,

• Collection of field blanks,

• Inclusion of trip blanks 1n sample shipments, and

• Collection of extra sample volumes and/or labeling for matrix spikeduplicate QC procedures in the laboratory.

The general requirements for these procedures are described 1n the following

paragraphs. The anticipated QC effort associated with specific samplingactivities is shown on Table 2-2.

2.3.1 Field Duplicates (FD)For water, sediment and soil samples, one duplicate (of the same type andcontainer size) will be collected for every 10 samples (or portion thereof)from each sampling activity. Duplicate samples will be collected byalternately filling two sets of sample bottles from the same sample unit(e.g., ball of water, scoop of sediment, spoon of soil, flowing water source)for each set of parameters.

TABLE 2-1

SAMPLE QUANTITIES, BOTTLES, PRESERVATION AND PACKAGINGREQUIREMENTS FOR WATER, SEDIMENT AND SOIL SAMPLES

FADROWSKI DRUM-DISPOSAL SITE

BOTTLES AND JARS PRESERVATIONANALYSIS

MONITORING WELLAND SURFACE WATER

CLP PROTOCOLVolatiles *Two 40-ml volatile organic Iced to 4 C

analysis (VOA) vials

BNA Extractables **Two 1-liter glass amber Iced to 4 Cbottles (Teflon-Lined Caps)

Pesticides/PCBs **Two 1-liter glass amber Iced to 4 Cbottles (Teflon-Lined Caps)

InorganicsMetals

Cyanide

One 1-Liter high densityPolyethylene Bottle

One 1-Liter high densityPolyethylene Bottle

Field filter .45 urn(groundwater only)5-ml/L 1:1 HN03 topH <2, Iced to 4 C

5-ml/L 5N NaOHto pH >12

HOLDING TIME

7 days

7 days untilextraction, 40 daysafter extraction

VOLUME OFSAMPLE

Fill Completelyno air bubbles

Fill bottle toneck

7 days until Fill bottle toextraction, 40 days neckafter extraction

SHIPPING

Federal ExpressPriority 1-Daily Basis

Federal ExpressPriority 1


6 months Fill to shoulder Federal Express(Hg-28 days) of bottle Priority 1

14 days Fill to shoulder Federal Expressof bottle Priority 1

PACKAGING

No. 1 foam lineror vermiculite





INDICATOR PARAMETERS

Alkalinity

Chloride

Sulfate

One 1-Liter high densityPolyethyleneOne 1-Liter high densityPolyethylene BottleOne 1-Liter high densityPolyethylene

Iced to 4 C

None Required

Iced to 4

14 days

28 days

28 days

Fill to shoulderof bottleFill to shoulderof bottleFill to shoulderof bottle



SEDIMENTS, SOIL AND WASTE

two 4-oz. wide mouth glass jar Iced to 4 CCLP Protocol

Volatiles

Semi-Volatiles One 8-oz. wide mouth glass jar Iced to 4 CPesticides/PCBs

Inorganicsmetals/cyanide

One 8-02. wide mouth glass jar Iced to 4 C

14 days Fill completelyNo headspace

7 days extraction, Fill 3/4 full40 days afterextraction

6 months Fill 3/4 full

Federal Express No. 1 foam linerPriority 1 - Daily Basis or vermiculite





NOTE: * - Triple normal volume should be collected for matrix spike and matrix spike duplicate samples.** - Double normal volume should be collected for matrix spike and matrix spike duplicate samples.

OC10O rv\


2.3.2 Field Blanks

For sediment and soil samples, no field blanks will be collected due to theunavailability of suitable blank material. For water samples, one field blank

will be prepared (for each type and container size). Field blanks will beprepared according to the following schedule for each sampling activity:

• One blank for every 20 or fewer samples of water collected.

• For each sampling period, a minimum of one blank for each group forparameters per sample matrix should be collected.

The field blank sample will be prepared using deionlzed water stored inpolyethylene containers. The water will be routed through the bailer formonitoring well samples or through decontaminated surface water samplingequipment for surface water samples before transfer to the container.

2.3.3 Trip Blanks (TB)A trip blank for volatile organic analysis (VGA) will be included in eachsample shipment containing water matrix samples for VOA. The trip blank willconsist of 2 40-ml VOA vials filled with deionlzed water with a M1111-Qcleanup. It will be prepared in the office or laboratory, transported to thefield and shipped with the other samples to the designated laboratory withoutbeing opened. It will be packaged using standard procedures as for othersample bottles.

2.3.4 Matrix Spike and Matrix Spike Duplicates (MS/MSD)For water samples, one sample per group of 20 or fewer samples collected forVOA and extractable organlcs analysis during each sampling activity will beselected for matrix spike/matrix spike duplicate (MS/MSD) analysis. For BNAsand Pest/PCBs, double the normal samle volume will be collected (I.e., two,

one-liter bottles for each). For VOCs, triple the normal sample volume willbe collected.

TABLE 2-2SAMPLE TYPES AM) ESTIMATE) SAMPLE NUMBERS


(1)MATRIX

TEST PITSTEST PITSTEST PITSTEST PITSTEST PITS

SOILSOILSOILSOILSOIL

SEDIMENTSEDIMENTSEDIMENTSEDIMENTSEDIMENT

SURFACE WATERSURFACE WATERSURFACE WATERSURFACE WATERSURFACE WATERSURFACE WATERSURFACE WATER

GROUNDWATERGROUNDWATERGROUNDWATERGROUNDWATERGROUNDWATERGROUNDWATERGROUNDWATER

(2)LAB






NO. OFSAMPLES

44444

2625252525

2626262626

4A

44444

8888888

FIELDDUPLICATES

1111<

33333

33333

—111

-

111

(3)FIELDBLANKS

0000O

00000

OO00O

—111111

—111111

<*)MATRIXSPK/DUP

OOOOO

OOOOO

O0OOO

—211

———

—211

——--

TOTALSAMPLES

66666

2828282828

2828282828

487700a

81211111O1O1O

(6)TEST PARAMETERS

EPA TCL VOC»EPA TCL BNAsEPA TCL PEST/PCBsEPA TCL METALSCYANIDE

EPA TCL VOC«EPA TCL BNAsEPA TCL PEST/PCBsEPA TCL METALSCYANIDE




(1) Soil, sediment and water matrix samples wl 1 1 be considered low concentration samp I*Samples from excavations w l 1 1 be considered medium level samples.

(2) HAZLETON: Hazleton Laboratories AmericaWARZYN: Warzyn Analytical LaboratoryFIELD: Field Analysis

(3) A trip blank for purgeablea w i 1 1 be included with each shipment for leachate andgroundwater samples.

(4) Sample numbers reflect extra volumes required for matrix spike/matrix spikeduplicate analysis.

(6) See Appendix B for EPA TCL analyte list. pH, conductivity and temperature w i I I bedetermined in the field for surface and groundwater.

USR/msr/RCWFMSR-VAX, 6/28/881


«

3.0 SAMPLING LOCATIONS AND PROCEDURES

3.1 WASTE CHARACTERIZATION

Records produced by Mrs. Smith, an employee of Fadrowski, Indicated that drumscontaining printing waste and lubricant sludges may have been buried at theFadrowski site. Samples collected at the Fadrowski site by the WDNR Indicatedthat there were significant concentrations of lead (Pb), chromium (Cr) andvolatile organic compounds (VOC) at several locations across the site. Also,

a concentration of 1450 parts per million (ppm) of DDT was detected 1n onesample collected from an oily sludge. Records provided by WDNR do not providedetailed identification of sampling locations.

A geophysical survey will be conducted on a grid pattern across the site usingan electromagnetic (EM) tool and a magnetometer to develop a subsurfaceprofile. The area to be included in the grid is shown on Figure 3-1. Aninstrument will be used which can yield resolution extending to a depth of 10feet. The anomalies which are judged to Indicate the presence of buried drumsor other metallic sources will be checked by boring or test pit Investigation.

Up to four trenches or test pits will be excavated. Each pit will be extendedto a depth of 12 feet (Figure 3-1). If an apparent contaminant source 1s

found, a representative sample will be collected and submitted for analysisfor purposes of waste characterization.

Waste samples will be collected using a stainless steel spatula or clam shellsampler. Samples will be checked for compatibility and a representativesample composited for analysis from each source location. Waste samples forVOA will not be mixed, but will be placed directly in the sample container.Other waste samples will be composited 1n a stainless steal container ormixing bowl using a stainless steel spatula, prior to placement 1n the sample

jars. Sampling and compositing equipment will be decontaminated betweensampling locations using the previously described decontamination fluids anddistilled water rinses. Samples will be considered as low and medium hazard.

27TH STREET

PROPOSED TEST PIT LOCATION

AREA TO BE INVESTIGATED BY GEOPHYSICALSURVEY

SITE INVESTIGATION BOUNDARY

APPROXIMATE PROPERTY LINE

FENCE

FIGURE 3-1PROPOSED TEST LOCATIONS FORWASTE CHARACTfRKATIOMSAMPLING AND ANALYSIS PLANREMEDIAL INVESTIGATION/FEASIBILITY STUDYFAOROWSU DRUH DISPOSAL SITEFRANKLIN, WISCONSIN


One field duplicate will be collected during the waste sampling activity. Nofield blanks will be collected.

Sample bottles required for this activity are listed in Table 2-1.

Samples will be shipped dally to the designated laboratories listed on Table2-2. Waste samples will be tested for CLP target Inorganic and organicparameters listed in Appendix B. Additional waste characterization may beconducted through the soil boring program described 1n Section 3.3.

3.2 SURFACE WATER SAMPLING

Representative samples of surface water and sediment will be collected fromthe site drainage areas to determine if contaminants are being transported bysurface water movement. A set of samples, including a sediment sample and awater sample, will be collected from each location. Proposed samplinglocations are shown on Figure 3-2. It is proposed that one sample set becollected from each of the following locations: 1) the pond near the edgeadjacent to the construction debris mound, 2) upstream of the site, 3)downstream of the site 1n the creek, and 4) the toe of the fill area along thesouth boundary. The samples at the fourth location will consist of erodedsediment and, 1f present, a sample of leachate.

Surface water samples will be collected within the upper 1 foot of water byusing a stainless steel dipper or by Immersing the sample container. Grabsamples will be taken from the shoreline with the sampling dipper or containerconnected to a stainless steel pole. In flowing water, the neck of the samplebottle will be oriented toward the upstream direction. In standing water,surface tension will be broken by slowly swirling the sample bottle in thewater prior to Immersion. The sample will be collected from below the watersurface to minimize collection of floating purtlculate matter. Specific

conductivity, temperature and pH will be measured In the field at the time ofsampling, in accordance with Section 3.7.

SOUTH 27TH STREET

PROPOSED SURFACE HATER ANO SEDIMENTSAMPLING LOCATION



FENCE

FIGURE 3-2PROPOSED SURFACE WATER!SAMPLE LOCATIONS

E 01 MINT

SAMPLING ANO ANALYSIS PLANREMEDIAL INVESTIGATION/FEASIBILITY STUDYFAOROUSKI DRUM DISPOSAL SITEFRANKLIN. WISCONSIN


One field duplicate, one field blank and one matrix spike/matrix spikeduplicate sample will be collected during the surface water sampling activity,

according to the guidelines 1n Section 2.3.

Sample bottles and sample preservation required for this activity are listedIn Table 2-1. Sample bottles may be pre-preserved, or preservative may beadded after the sample 1s collected. Surface water samples will not be fieldfiltered for any parameters. Surface water samples will be shipped dally tothe designated laboratories. Surface water samples will be tested for the CLPTarget Inorganic and organic parameters listed 1n Appendix B and the indicatorparameters in Table 2-1.

3.3 SEDIMENT SAMPLINGSediment samples will be collected at the same locations as the surface watersamples described in Section 3.2.

Surface sediment samples will be collected using a 2-1nch diameter stainlesssteel hand corer or clam shell sampler to a depth of no more than 6 Inches.Samples will consist of four composite samples taken at representative pointsin the pond or stream. Sampling conditions (e.g., frozen 1n winter) maydictate modifications to the compositing scheme. Sediment samples analyzedfor volatHes will be placed directly Into the sample Jars. Other sedimentsamples will be placed in a stainless steel beaker or mixing bowl and quicklymixed using a stainless steel spatula or spoon, prior to placement in thesample Jars.

Sampling and compositing equipment will be decontaminated between samplinglocations using the previously described decontamination fluids and distilledwater rinses.

One field duplicate sample will be collected during the sediment samplingactivity, according to the guidelines in Section 2.3.


Samples will be shipped daily to the designated laboratories. Surfacesediment samples will be tested for CLP Target inorganic and organicparameters shown in Appendix B.

3.4 SOILS SAMPLINGTo investigate the potential of soil contamination at the site, 25 soilborings will be made, each to a depth of ten feet. Proposed boring locationsare shown on Figure 3-3. These locations were selected on the basis ofpreliminary information, so it 1s likely that some boring locations will bemodified as more detailed site Information 1s collected during the course ofthe Investigation. Each boring will be advanced with continuous sampling

procedures. Soil core samples will be obtained using a 2-inch O.D. split-spoon sampler. Core samples will be field screened with an HNU, and thesamples Identified as most likely to contain contamination will be collectedand submitted for CLP Target parameter analysis. The soil samples will becollected from the split-spoon sampler using a stainless steel spatula orspoon. The volatile portion of samples will be placed directly 1n sample jars

with no mixing. Other soil samples will be placed into a stainless steelmixing bowl for mixing, prior to placement Into the sample jars. The drillingand sampling equipment used will be decontaminated between each boring.

Three field duplicates will be collected during soil sampling activity,according to the guidelines in Section 2.3.

Samples will be shipped dally to the designated laboratories as shown 1n Table2-2. Soil samples will be analyzed for CLP target parameters listed 1nAppendix B.

3.5 SITE HYDROGEOLOGIC SAMPLING3.5.1 Monitoring Well Installation

During the first phase of Investigation, monitoring wells will be constructedat five locations across the site (Figure 3-4). One well will be placed up-gradient to act as a background well. The other locations were selected

because they are adjacent to areas of greatest potential contamination.

SOUTH 27TH STREET

PROPOSED SOIL BORING LOCATION

POSSIBLE ADDITIONAL SOIL BORINGLOCATION



FENCE

FIGURE 3-3PROPOSED LOCATIONS FOR SOIL BOM NO J

SAMPLING ANO ANALYSIS PLANREMEDIAL INVESTIGATION/FEASIBILITY STUDYFAOROWSKI DRUM DISPOSAL SITEFRANKLIN, WISCONSIN

SOUTH 27TH STREET

PROPOSED MONITORING WELL LOCATIONANO NUMBER

PROPOSED PIEZOMETER WELL LOCATIONANO NUMBER



FENCE

IllID

VN

* fO

JI

Ht»

n

0SCALE:

* L0 L-

1"=300'

OWN 3(S AppoM^.

|

DATEC./14 «8 25389 A12

I' FIGURE 3-4

WARZYNPROPOSED LOCATIONS FOR PHASE 2

iMOMTORINQ WELLSSAMPLING AND ANALYSIS PLANREMEDIAL INVESTIGATION/FEASIBILITY STUDYFAOROWSKI DRUM DISPOSAL S ITEFRANKLIN, WISCONSIN


Locations MW-1 to MW-3 are arranged in a triangular pattern; each locationwill contain two wells screened at different depths. The triangular layoutwill be used to determine the horizontal groundwater gradient and flowdirection. The well nests will be used to determine vertical hydraulicgradients at the site.

A drilling method suitable to site conditions will be selected. To avoidsubsequent contamination of borings, drilling Implements will be steam cleanedbetween borings. A shallow well, with screen placed to Intersect the watertable, will be placed at each of the five locations. At the three locationsfor nested wells, the additional well will act as a piezometer, screened inthe next lower zone of relatively high permeability. Each monitoring wellwill be constructed of 2-inch Inside diameter, flush threaded PVC pipe and0.010 Inch slotted PVC screen. Ten-foot screens will be used for the fiveshallow wells and two-foot screens will be use on the three deeper wells. Theeight wells will be completed with the installation of a gravel pack aroundeach screen, a 2-foot bentonlte seal above the gravel pack, and a bentonitegrout to the surface. Each boring will be fitted with a locking, steelprotecting casing, and each well will be developed by balling.

3.5.2 Groundwater SamplingWhen the monitoring wells have equilibrated after construction anddevelopment, a water sample will be collected from each and submitted forlaboratory analysis for the constituents on the CLP Target Compound List 1nAppendix B and the water quality Indicators listed in Table 2-1. Groundwatersamples will be collected using a stainless steel bailer. Each monitoringwell to be sampled will be purged of three well volumes of water prior to

collecting each sample. Specific conductivity, temperature, and pH will bemeasured in the field at the time of sampling, 1n accordance with Section 3.7.

One field duplicate, one field blank and one matrix spike/matrix spike

duplicate sample will be collected during the groundwater sampling activity,

according to the guidelines 1n Section 2.3.


Sample bottles and sample preservation required for this activity are listedin Table 2-1. Sample bottles may be pre-preserved, or preservative may beadded after the sample 1s collected. Groundwater samples will be fieldfiltered for metals. Preservative will not be added prior to filtering.Groundwater samples will be shipped dally to the designated laboratories asshown on Table 2-2. The analytical results will be used for the EndangermentAssessment, the Feasibility Study, and to define additional groundwaterInvestigation which may be necessary 1n Phase II.

3.5.3 Aquifer Characteristics.Geologic cross sections will be developed from the soil boring and welldrilling logs to show the subsurface conditions. Water levels will becollected at each of the monitoring wells weekly during the fieldInvestigation. Bail tests will be used at each of the monitoring wells toprovide an estimate of the hydraulic conductivity of the screened unit. Apotentiometric map will be developed for the water table.

3.6 AIR SAMPLING

No air quality data are currently available to define ambient air conditionsat the site; however, samples collected by WDNR indicate the presence of VOCsin the waste.

A1r quality will be monitored before commencement of field activities (for thepurposes of establishing background levels) and during the sampling anddrilling program. Photo-1onizat1on detectors (HNu's or TIP's) will be usedduring the Investigation to monitor air quality and to help determine levelsof protection for on-s1te personnel. The actual monitoring procedures andequipment required to characterize the extent of atmospheric contaminationwill not be known until completion of the site heath and safety assessment.However, when those parameters have been determined, the ambient air qualityacross the site will be characterized 1n conjunction with the analysis oflocal wind patterns.


3.7 FIELD TESTS OF pH. TEMPERATURE AND CONDUCTIVITYSpecific conductivity, temperature and pH will be measured in the field usingportable Instruments at the time of sampling each monitoring well and surfacewater location. The conductivity meter will be zeroed according to proceduresspecified for the instrument, prior to recording measurements. Buffersolutions bracketing the reading will be used to calibrate the pH meter priorto and after each use. A small volume of sample will be taken from the sourceand poured Into polyethylene or glass containers and the Instrument probesplaced into the water. Following readings, the water samples will bediscarded and the Instrument probes decontaminated. Measurements, includingcalibration data will be recorded 1n the field notebook.

4.0 DECONTAMINATION PROCEDURES

Procedures to decontaminate equipment and personnel are described below and inthe Fadrowski Drum Disposal Site Health and Safety Plan.

4.1 PERSONNEL DECONTAMINATIONA personnel decontamination station will be set up at the edge of the SupportArea. Personnel will become thoroughly familiar with the decontaminationprocedure before work begins. The procedure is as follows:

1. Place equipment and/or samples in area designated; move to next area(areas marked with signs, 1f necessary),

2. Wash boots using: (1) soap (alconox or equivalent) in water solutionand (11) potable water rinse,

3. Remove disposable coveralls, booties and outer gloves and place 1nplastic bags (1n 55-gallon drum),

4. Remove hard hat and respirator (if used) and store 1n appropriateplace,

5. Remove disposable Inner gloves (1f used) and place 1n plastic bag (1n55-gallon drum) and

6. Wash hands and face with water and soap.


4.2 EQUIPMENT DECONTAMINATIONDecontamination of large equipment (vehicles, drill rigs and associatedequipment) will be performed at a cleaning station adjacent to a shallowexcavated sump lines with double layers of plastic sheeting. Cleaning willconsist of tr1-sodium phosphate (TSP) solution and water wash and potable

water rinse using a high pressure hot water or steam cleaning unit.Additional scrubbing may be required to remove encrusted materials.Decontaminated equipment will be stored on plastic sheeting and/or platformsabove the ground surface.

Drill rigs will be protected with plastic sheeting at the soil samplingstations to minimize contamination of major body parts. Any parts of the rigwhich are encrusted with dirt or mud or are suspected of having been splashedwith materials at a sampling stations will be washed prior to moving to thenext borehole location. Drill rigs will be fully decontaminated prior toboring at each new monitoring well location. Drill rigs and other vehicleswill be fully decontaminated prior to leaving the site.

Sampling equipment (including bailers) will be decontaminated prior to use,and reusable non-dedicated equipment (scoops, buckets, triers, thlefs, splitspoons) will be decontaminated between samples and before removal from thesite. The procedure 1s as follows:

• Soap and water wash,• Potable water rinse,• Acetone or methanol (reagent grade) rinse, and• Distilled water rinse, twice.

4.3 SAMPLE BOTTLE DECONTAMINATIONSample bottles will be decontaminated by immersing the bottle up to the neckin (a) soap (TSP or equivalent) In water solution and (b) potable or distilledwater rinse. Solvents will not be used to wash sample bottles.


4.4 RI GENERATED WASTES

Disposable protective clothing and disposable sampling equipment will beplaced Into plastic bags. Liquids generated by decontamination procedureswill be disposed of on-slte. Drill cutting from soil borings will remain inplace at each hole.

5.0 DOCUMENTATION

5.1 FIELD LOG BOOKS

Field log books will provide the means of recording data collection activitiesperformed. As such, entries will be described 1n sufficient detail, sopersons going to the site could reconstruct a particular situation withoutreliance on memory.

Bound field survey books will be used to record field logs. Log books will beassigned to field personnel, but will be stored In the document control centerwhen not in use. Each log book will be Identified by the project-specificdocument number.

The title page of each notebook will contain:

• Person or organization to whom the book is assigned,• Book number,• Project name,• Start date, and• End date.

Entries Into the log book will contain a variety of information. At thebeginning of each entry, the date, start time, weather, names of sampling teammembers present, level of personal protection being used, and the signature ofthe person making the entry will be entered. The names of visitors to thesite and the purpose of their visit will be recorded 1n the field log book.


Measurements made and samples collected will be recorded. Entries will bemade in ink and no erasures will be made. If an incorrect entry 1s made, theInformation will be crossed out with a single strike mark. Wherever a sample1s collected or a measurement 1s made, a detailed description of the locationof the station, which includes compass and distance measurements, shall berecorded. The number of the photographs taken of the station will also benote. Equipment used to make measurements will be Identified, along with thedate of calibration.

Samples will be collected following the procedures documented 1n this SAP.The equipment used to collect samples will be noted, along with the time ofsampling, sample description, depth at which the sample was collected, volumeand number of containers. Sample identification numbers will be assignedprior to sample collection. Duplicates, which will receive a separate sampleIdentification number, will be noted under sample description.

5.2 SAMPLE IDENTIFICATION DESIGNATION

A sample numbering system will be used to identify each sample, includingduplicates and blanks. Each sample Identifier will have three components: aproject identifier; a sample type and location code; and a numerical codeIndicating the sampling event. A listing of sample Identification will bemaintained in a log book kept by the Warzyn Field Manager.

5.2.1 Pro.lect IdentifierA two-letter designation will be used to Identify the sample collection site.For this project, the designation will be FD, which represents Fadrowski DrumDisposal.

5.2.2 Sample Type and Location CodeEach sample collected will be Identified by a two-digit alpha codecorresponding to the type of sample, followed by the sample location number.The alpha codes are as follows:


• GW-Mon1tor1ng Well Groundwater Sample• SW-Surface Water Sample• SD-Sed1ment Sample• SS-Surface Soil Sample• SB-Soil Boring Soil Sample• TP-Tr1p Blank• FB-F1eld Blank• FD-F1eld Duplicate

A three-digit numbering system will be used to Indicate the sampling location.The Identification system will require that sampling locations be givenseparate numbers. The number associated with each sampling location as wellas other pertinent data will be kept 1n the field sampling notebook.

5.2.3 Sampling EventSamples will have an identifier to indicate sampling event ("01", "02", etc.).Duplicate samples will be Identified by "91" for the first sampling event,"92" for the second sampling and so on.

5.2.4 Example of Sample NumbersAn example of a sample number 1s:

FD-GW011-02

Fadrowski Drum Disposal Site ~ groundwater sample from location Oil, secondsampling event.

Other pertinent data relating to the sampling event will be Included 1n thesampling notebook.

5.3 PHOTOGRAPHSRepresentative photographs will be taken of sampling stations to showsurrounding area and used to locate the station. The picture number and rollnumber will be logged 1n the field log book to identify which sampling site isdepicted in the photograph. The film roll number will be Identified by takinga photograph of an informational sign on the first frame of the roll, with thejob and film roll number written on the sign.


For example:

Fadrowski Drum DisposalRoll Number 1Frame Number 1 of 361 August 1987 - 8 August 1987

5.4 SAMPLE DOCUMENTATIONSamples will be collected under chain-of-custody procedures in accordance withNational Enforcement Investigation Center policies (Ref. 4 of QAPP). Standardforms Including sample tags, traffic reports, cha1n-of-custody forms andcustody seals similar to those used for CLP sample tracking will bemaintained. Pertinent information regarding the samples will be recorded 1nthe site log book maintained by the SM and 1n logs maintained by each samplingcrew. The Information will Include sampling time, location, tag numbers,weather conditions and field modifications to sampling strategy. The log bookwill be maintained in Ink, unless weather conditions dictate otherwise.Photographs with the time, date and location noted in the photo may be takenat each sampling location.

[sss-600-20]

APPENDIX B

CLP TARGET COMPOUND LIST

REVISION 2

TABLE B-l

TARGET COMPOUND LIST (TCL) ANDCONTRACT REQUIRED QUANTITATION LIMITS (CRQL)*

Detection

Volatiles CAS Number

1. Chloromethane 74-87-32. Bromomethane 74-83-93. Vinyl Chloride 75-01-44. Chloroethane 75-00-35. Methylene Chloride 75-09-2

6. Acetone 67-64-17. Carbon D1sulf1de 75-15-08. l,l-D1chloroethene 75-35-49. 1,1-01Chloroethane 75-35-3

10. Total-1,2-Dichloroethene 156-60-5

11. Chloroform 67-66-312. 1,2-01Chloroethane 107-06-213. 2-Butanone 78-93-314. 1,1,1-Trlchloroethane 71-55-615. Carbon Tetrachloride 56-23-5

16. Vinyl Acetate 108-05-417. Bromodlchloromethane 75-27-418. 1,1,2,2-Tetrachloroethane 79-34-519. 1,2-01chloropropane 78-87-520. trans-l,3-D1chloropropene 10061-02-6

21. Trichloroethene 79-01-622. Dlbromocloromethane 124-48-123. 1,1,2-TriChloroethane 79-00-524. Benzene 71-43-225. ds-l,3-D1chloropropene 10061-01-5

27. Bromoform 75-25-228. 2-Hexanone 591-78-629. 4-Methyl-2-pentanone 108-10-130. Tetrachloroethene 127-18-4

31. Toluene 108-88-332. Chlorobenzene 108-90-733. Ethyl Benzene 100-41-434. Styrene 100-41-435. Total Xylenes 100-42-5

Low Water (2)ua/1

101010105

105555

551055

105555

55555

510105

55555

Low SoilSediment C3)

uq/kq

101010105

105555

551055

105555

55555

510105

55555

Volatiles

Table B-l, Continued

CAS Number

Detection L1m1ts(1)

Low Water(2)uq/1

Low SoilSediment(3)

uq/kq

36.37.38.39.40.

41.42.43.44.45.

46.47.48.49.50.

51.52.53.54.55.

56.57.58.59.

60.

61.62.63.64.65.

66.67.68.69.70.

71.72.73.74.75.

Phenolb1 s (2-Chl oroethyl ) ether2-Chl orophenol1 , 3-D1 chl orobenzene1 , 4-D1 ch 1 orobenzene

Benzyl Alcohol1 , 2-D1 chl orobenzene2-Methyl phenolb1 s (2-Chl orol sopropyl ) ether4-Methyl phenol

N-N1 troso-D1 propy 1 ami neHexachloroethaneNitrobenzeneIsophorone2-N1trophenol

2 , 4-D1 methyl phenolBenzole Acidb1 s (2-Chl oroethoxy) methane2 , 4-D1 chl orophenol1 , 2 , 4-Tri chl orobenzene

Naphthalene4-Chloroan1l1neHexachl orobutadi ene4-Chloro-3-methyl phenol

(para-chloro-meta-cresol )2-Methyl naphthal ene

Hexachl orocycl opentadi ene2,4, 6-TH chl orophenol2, 4, 5-Tr1 chl orophenol2-Chl oronaphthal ene2-N1troanil1ne

Dimethyl Ph thai ateAcenaphthylene3-N1troan1l1neAcenaphthene2,4-D1n1trophenol

4-N1trophenolDibenzofuran2,4-D1nitrotoluene2,6-D1n1trotolueneDlethylphthalate

108-95-2111-44-495-57-8541-73-1106-46-7

100-51-695-50-195-48-739638-32-9106-44-5

621-64-767-72-198-95-378-59-188-75-5

105-67-965-85-0111-91-1120-83-2120-82-1

91-20-3106-47-887-68-359-50-7

91-57-6

77-47-488-06-295-95-491-58-788-74-4

131-11-3208-96-899-09-283-32-951-28-5

100-02-7132-64-9121-14-2606-20-284-66-2

1010101010

1010101010

1010101010

1050101010

10101010

10

1010501050

1010501050

5010101010

330330330330330

330330330330330

330330330330330

3301600330330330

330330330330

330

33033016003301600

33033016003301600

1600330330330330

VolatHes


CAS Number

Detection Limitst1)

Low Water(2)uq/1

Low Soil %Sed1mentC3)

uq/kq

76.77.78.79.80.

81.82.83.84.85.

86.87.88.89.90.

91.92.93.94.95.

96.97.98.99.100.

101.102.103.104.105.

106.107.108.109.110.

111.112.113.114.115.

4-Chlorophenyl Phenyl etherFluorene4-N1troan1l1ne4, 6-D1 n1 tro-2-methyl phenolN-n1 trosodl phenyl ami ne

4-Bromophenyl Phenyl etherHexachl orobenzenePentachl orophenolPhenanthreneANTHRACENE

D1 -n-butyl phthal ateFluoranthenePyreneButyl Benzyl Phthal ate3 , 3 ' -D1 chl orobenzldl ne

Benzo (a) anthraceneb1 s (2-ethy 1 hexyl ) phthal ateChryseneDi-n-octyl Phthal ateBenzo (b) f 1 uoranthene

Benzo (k)fluorantheneBenzo(a)pyreneIndeno(l,2,3-cd)pyreneDibenz (a, h) anthraceneBenzo (g , h , 1 ) peryl ene

alpha-BHCbeta-BHCdelta-BHCgamma-BHC (Lindane)Heptachlor

AldrlnHeptachlor EpoxldeEndosulfan IDieldrin4, 4 '-DDE

EndrinEndosulfan II4,4-DDDEndosulfan Sulfate4,4'-DDT

7005-72-386-73-7100-01-6534-52-186-30-6

101-55-3118-74-187-86-585-01-8120-12-7

84-74-2206-44-0129-00-085-68-791-94-1

56-55-3117-81-7218-01-9117-84-0205-99-2

207-08-950-32-8193-39-553-70-3191-24-2

319-84-6319-85-7319-86-858-89-976-44-8

309-00-21024-57-3959-98-860-57-175-55-9

72-20-833213-65-972-54-81031-07-850-29-3

1010505010

1010501010

1010101020

1010101010

1010101910

0.050.050.050.050.05

0.050.050.050.100.10

33033016001600330

3303301600330330

330330330330660

330330330330330

330330330330330

0.0.,10,10

0.100.100.10

8.08.08.016.016.0

16.016.016.016.016.0

Volatiles


CAS Number

Detection LimltsU)

Low Water(2)uq/1

Low Soil xSed1ment(3)

uq/kq

116. Endrln Ketone117. Methoxychlor118A. Alpha Chlordane118B. Gamma Chlordane119. Toxaphene120. AROCLOR-1016

121. AROCLOR-1221122. AROCLOR-1232123. AROCLOR-1242124. AROCLOR-1248125. AROCLOR-1254126. AROCLOR-1260

53494-70-572-43-5

8001-35-212674-11-2

11104-28-211141-16-553469-21-912672-29-611097-69-111096-82-5

0.100.50.0..5.5

1.00.5

1.01.0

16.080.080.80.160.

.0

.0

.080.0

80.80.80.80.160.0160.0

.0

.0

.0

.0

NOTES

(1) Detection limits listed for soil/sediment are based on net weight. Thedetection limits calculated by the laboratory for soil/sediments will beon dry weight basis and will be higher.

(2) Medium Water Contract Required Quantltation Limits (CRQL) for VolatileTargert Compound List (TCL) Compounds are 100 times the Individual LowWater DL.

(3) Medium Soil/Sediment CRQL for Volatile TCL Compounds are 100 times theIndividual Low Water CRQL.

(4) Medium Water CRQL for Semi-Volatile TCL Compounds are 100 times theindividual Low Water CRQL.

(5) Meidum Soil/Sediment CRQL for Semi-Volatile HSL Compunds are 60 times theindividual Low Soil/Sediment CRQL.

(6) Medium Water CRQL for Pesticide TCL Compounds are 100 times theindividual Low Water CRQL.

(7) Medium Soil/Sediment CRQL for Pesticide TCL Compunds are 15 times theindividual Low Soil/Sediment CRQL.

Specific detection limits are highly matrix dependent. The detectionlimit listed herein are provided for guidance and may not always beachievable.

[jpl-401-54]

TABLE B-l

ELEMENTS DETERMINED BYINDUCTIVELY COUPLED PLASMA EMISSIONOR ATOMIC ABSORPTION SPECTROSCOPY

RequiredDetection Level U)

Metal uq/1

Aluminum 200Antimony 60Arsenic 10Barium 200Beryllium 5Cadmium 5Calcium 5000Chromiurn 10Cobalt 50Copper 25Iron 100Lead 5Magnesium 5000Manganese 15Mercury 0.2Nickel 40Potassium 5000Selenium 5Silver 10Sodium 5000Thallium 10Vanadium 50Zinc 20

Other

Cyanide 10

NOTES

(1) Any analytical method specified 1n Exhibit D of IFB WA 84-J091/J092 maybe utilized as long as the documented instrument or method detectionlimits meet the CRQL requirements. Higher detection levels may only beused 1n the following circumstances.

If the sample concentration exceeds two times the detection limit ofthe instrument or method 1n use, the value may be reported eventhough the Instrument or method detection limit may not equal theCRQL.

[jpl-401-53]

APPENDIX C

REQUESTED ANALYSIS METHODS

FADROWSKI DRUM DISPOSAL QAPP

REVISION: 2

AUTOANALYZER

Scope and Appl icat ion: Ions can be readily analyzed by a f low-inject ionautoanalyzer. The flow injection design givesthe system excel lent washout characterist ics, toprevent carry over and cross contamination. Theautoanalzyer is generally more sensi t ive andaccurate than the manual wet-chemistry techniques.

Method: Flow injection

References: Lachat Instruments, 1986.

Sample Handling: See separate S O P ' s for requirements.

Reagents and Appartus:

1. Lachat 3-channel autoanalyzer2. Stock and standard ion solutions3. Class A volumetric f lasks4. Class A volumetric pipets5. Milli-Q water6. Required interference filters7. Disposable 4 ml cups8. Automatic sampler9. Proportioning pump

10. Injection module11. Colorimeters12. Manifolds13. Columns - if needed14. Helium gas15. Computer16. Printer

Procedure:

A. Instrument Set-up

1. Depress red power switch on power strip located behind thecomputer terminal. This will turn on the computer, thescreen, and the printer.

2. Depress red power switch on rear power strip on Lachat system.

LAA-1

4. Select manifold and make appropriate hydraulic connections.

Hydraulic connections:

a. Use correct sample loop length to connect.Lines 1, 4.

b. Line 2 is carrier line.

c. Line 3 goes to manifold.

d. Line 5 goes to waste container.

e. Line 6 comes from sample probe.

f. Connect manifold to flow through cell.

Tension levers should be up when pump tubing is inserted.Snap pump tubing cartridges into place.

5. Insert correct filter.

6. Pump Milli-Q water through lines for 5 minutes by depressingthe pump ON button. Check for leaks.

7. Computer - At the C> type in "quikcalc". This calls up theLachat software and puts you at the master menu. Press <enter>,

8. Put lines into reagents and/or degassed Milli-Q water.

9. Computer - Select "Load/Stop Background Method" on the mastermenu. Press <enter>.

10. Select appropriate method. Press <enter>.

11. Printer should be set at FONT 0.

12. Pump reagents until a steady baseline is achieved.

13. When using a method with a column ($64 or N03), the columnmay be inserted at this point. See method S O P ' s for moredetai Is.

14. For each analytical channel, adjust zero knob so that thebaseline is near the bottom of the screen (between .000 -.030).

LAA-2

15. Adjust gain while injecting top standard.

a. P lace autosampler probe into the highest standard bottle.

b. A f te r 20-30 seconds, press cycle button on front panelso that LED light is red. This is the load posit ion.

c. A f te r 25 seconds (or less depending on sample loop s ize ) ,press cycle button so that LED light is green. This isthe inject position,

d. Adjust gain knob on detector so that peak reading onthe colorimeter is 1.700-1.950.

e. Repeat until gain is properly adjusted.

f. Wipe probe and replace the autosampler probe into thesampler.

16. Select menu item by going into foreground. (Press and holdA l t key, then press Esc key).

a. Select "Sample Tray Information and Start Analysis" onmaster menu. Press <Enter>.

b. Press <Enter> or type in sample tray reference number ifit is a tray which has already been typed in.

c. Enter tray ID and operator. Check "Display StandardsPosit ion in Tray" to insure the tray is set-up properly.

d. Select "Enter Sample ID's". Press <enter>.

e. Type in sample information. Check standards willautomatically be placed in the tray informationportion.

f. Press Esc once to return to menu.

17. Put tray with samples in appropriate cup locat ions onautosampler. Position tray to the cup containing standardA (usually #35 or so). Select "Start Analys is . " Press<enter>.

18. The second screen will ask if the tray has standards or not.If you standardized the first tray of the run and all the checkstandards are within QC ranges, recalibration for the next trayis not necessary. Select appropriate option. Press <enter>.

LAA-3

19. Press A l t , Esc keys together, to get back to background toview the calibration peaks.

Af ter cal ibrat ion is complete:

- go into the foreground (Press Al t , Esc keys )

- select "display calibration graph" (Press <enter>)

- review the data

- return to the background (Press Alt, Esc keys)

- press "G" for good calibration. Ana lys is will continue.

- press "R" for re-calibration. Remember to refill standardcups and reposition sample tray before pressing "R" !

B. Instrument Shut-Down

1. Press Al t /Esc keys to get to the foreground. Select "Load/StopBackground Method". Press <enter>. To question-"Stop background( Y / N ) ? " Press "Yes". Press Esc key to main menu.

2. If column is used, stop the pump and disconnect from manifold.

3. Pull l ines from reagents into a wash beaker of D.I..

4. Pump D.I. through lines for 2-5 minutes.

5. Pump air through lines until manifold is dry.

6. Turn off pump.

7. Release tubing cartridges and lower tension levers.Release tubing.

8. Turn off main switch on rear power strip.

9. Empty and rinse waste containers, if necessary.

10. Perform back-up on current data files, once a week,(see section C )

11. Turn off the computer and printer.

LAA-4

C. Backing-up the Data Files

1. Ex i t to DOS

2. At O Type: cd\fialabXdata Press <enter>

3. At C> Type: copy *.rpt a: Press <enter>After everything is copied - remove disc.

4. At C> Type: del *.*. Press <enter>

5. Are you sure (Y /N)? Type: Y Press <enter>

6. At C> Type: cd\ Press <enter>

7. Turn off the red switch on the computer power strip toturn off the computer, printer and screen.

Revision Date

Michael J. Linskens 8-18-87Laboratory Manager y-a/7n

\jrr\ -'Kim D. FinnerAnaly t ica l Laboratory QA/QC Officer

Lawrence D. AndersonVice President, Technical Services

[KAW-3-10] LAA-5

ALKALINITY - AUTOANALYZER

Scope and Appl icat ion: This method is appl icable to drinking water,surface water, groundwater and wastewater.

Reference: EPA 1983, Method 310.2Lachat Instruments 1986, Method 10-303-31-1-C

Sample Handling: Refrigerate at 4°C and analyze within 14 days of collection.

Detection Limit: 5.0 mg/L as CaC03

Optimum Concentration Range: 5.0 - 500 mg/L


1. Pump speed: 352. Cycle period: 60 seconds3. Load period: 30 seconds4. Inject period: 15 seconds5. Inject to start of peak period: 10 seconds6. Inject to end of peak period: 56 seconds7. Gain: 150 x 108. Zero: 1809. Interference filter: 410 nm

10. Sample loop: 90 cm11. Standards for curve set-up: 0, 20.0, 50.0, 100, 250, 500 mg/L.

Reagent Preparation: (Prepare fresh every 6 months, unless otherwise stated.

1. Degassed Milli-Q water - 2 options:

a. Boil MilH-Q water vigorously for 5 minutes. Cool and storein cubitainer.

b. Bubble helium, using the fritted gas dispersion tube, throughthe Milli-Q water (15 min/20 L.) Store in cubitainer.

2. Stock alkalinity standard (1000 mg/L as Na?CO^): In a 1 litervolumetric f lask, dissolve 1.060 g of anhydrous primary standardgrade sodium carbonate (Na2C03~dried at 140"C for 4 hours) inapproximately 900 mL of helium purged Milli-Q water, and diluteto mark.

ALKAA-1

3. Standards: (Prepare fresh every 2 months.)

Concentrat ion Letter Volume of Di luteof Standard Identifier A l k . Standard to

0 mg/L A 0 200 mL20.0 mg/L B 4.0 200 mL50.0 mg/L C 10.0 200 mL

100 mg/L D 50.0 500 mL250 mg/L E 125.0 500 mL500 mg/L F 100.0 200 mL

NOTE: Final volumes are not the same!Computer refers to standards by letter.

4. Sodium hydroxide (0.1M): In a 1 liter f lask, dissolve 4.0 g sodiumhydroxide (NaOH) and dilute to the mark with Mil l i-Q water.

5. Hydrochloric acid (O.IM): In a 1 liter f lask, dilute 8.3 mL ofconcentrated HCL in Milli-Q water and dilute to the mark.

6. KHP buffer (25.0 mM. pH 3.1): In a 1 liter f lask, dissolve 5.10 gof potassium acid phthalate (KHP) (KHC3H404) in approximately 500 mLof helium purged Milli-Q water. Add 87.6 mL of 0.1M HCL and diluteto the mark. Adjust the pH of the buffer to 3.1 with 0.1M HCL or0.1M NaOH. STORE IN GLASS AND PREPARE MONTHLY!

7. Methyl orange reagent: In a 1 liter volumetric flask, dissolve

Notes:

Methyl orange reagent: In a 1 Mter volumetric t lask, d isso lve0.125 g of methyl orange indicator in about 700 mL of helium-purgedMilli-Q water and dilute to the mark. Store in g lass !

1. Samples must be diluted to obtain concentrations within theoptimum working range.

2. The gain and zero settings are guidelines and must be adjustedeach day to optimize.

3. The alkalinity standards can be combined with chloride andsulfate standards for use with the 3 channel method.

4. Turbidity will interfere. Samples must be filtered prior toanalysis. (Use Whatman #1 or #4. )

5. Color will interfere, dilute the sample and a lso spike thissample to confirm the quality of the result.

System Operation:

A. Refer to "Auto Analyzer Operation start-up procedure."(IOP# LAA-section A)

ALKAA-2

B. Ana lyze a blank and an EPA check standard at the beginning ofeach run.

C. Use 125 mg/L for the spike level.

D. The calibration check standard is 100 mg/L ( D ) .

E. Refer to "Auto Analyzer shut-down procedure". ( IOP# LAA-sect ion B)

Quality Control:

1. Establish a standard curve with the standards listed above.Record the check standard in the check standard book. Theconcentration should remain consistent from run to run. Ifnot, necessary troubleshooting must be performed beforecontinuing (check reagents, pump tubing, valves, etc. ) .

2. A quality control calibration standard of 100 mg/L is to be analyzed,at a minimum, after every 10 samples. If less than 10 samples areanalyzed, a calibration standard is still required. The last sampleanalyzed in the run is to be the calibration standard. Thesestandards must be within the acceptable ranges or the samples runafter the last acceptable check standard are to be reanalyzed.Record the calibration standards in the quality control book. Theacceptable limits are noted in the quality control book.

3. Duplicate and spike a minimum of 1 out of 10 samples. If less than10 samples are analyzed, a duplicate and spike are still required.Duplicates are to be averaged. Spike samples with a standard in a1:1 ratio of sample to standard. Spike recoveries and duplicatesare to be within acceptable ranges or troubleshooting must beperformed.

Calculation:

1. Calculate with Lachat QuikChem software, in the concentrationmode, using the IBM XT computer.

Revision Dates

8-18-87_Michael J. Link sensLaboratory Manager *?"<}• S~~F?

Kim D. F innerA n l y t i c a l Laboratory QA/QC Officer

Lawrence D. AndersenV ice President, Technical Services

[KAW-3-8] ALKAA-3

CHLORIDE - AUTQANALYZER

Scope and App l ica t ion : Th is method is appl icable to drinking water,surface water, groundwater, and wastewater .

References: EPA 1983, Method 325.2Lachat Instruments 1986, Method 10-117-07-1-B

Sample Handling: Refr igerate at 4°C and analyze wi th in 28 days of col lect ion.

Detection Limit: 1.0 mg/L.



1. Pump speed: 352. Cycle speed: 30 seconds3. Load period: 15 seconds4. Inject period: 15 seconds5. Inject to start of peak period: 8 seconds6. Inject to end of peak period: 35 seconds7. Gain: 2008. Zero: 2509. Interference filter; 480 nm

10. Sample loop: 20 cm11. Standards for curve set-up: 0, 10.0, 20.0, 50.0, 80.0, 100.

Reagent Preparation: (Prepare fresh every 6 months, unless otherwise noted.)

1. Degassed Milli-Q water - 2 options:

a. Boil Milli-Q water vigorously for 5 minutes. Cool and storein cubitainer.

b. Bubble helium, using the fritted gas dispersion tube, throughthe Milli-Q water. (15 min/20 L.) Store in cubitainer.

2. Stock chloride standard (1000 mg/L CD: In a 1 liter volumetricf lask, dissolve 1.648 g of primary grade sodium chloride (Nad),previously dried at 103°C, in 500 mL Milli-Q water. Dilute tothe mark and invert to mix.

C1AA-1

3. Standards: (Prepare fresh every 2 months.

Concentrationof Standard

0 mq/L10.0 mg/L20.0 mg/L50.0 mg/L80.0 mg/L100 mg/L

LetterIdentifier

ABCDEF

Volume ofCl Standard

02.04.0

25.040.020.0

D i 1 u teto

200200200500500200

Note: Final volumes are not the same!Computer refers to standards by letter.

4. Stock mercuric thiocyanate reagent: In a 1 liter volumetric f lask,dissolve 4.17g of mercuric thiocyanate ( H g ( S C N ) 2 ) in one liter ofmethanol. Invert to mix. Store in amber glass.

CAUTION: Mercury is a very toxic metal. WEAR GLOVES!

5. Stock ferric nitrate reagent (0 .5M): In a 1 liter volumetric f lask,dissolve 202.Og of ferric nitrate (Fe(N03)3 • 9H20) in approximately800 mL of deionized water. Add 25 mL of concentrated nitric acidand dilute to one liter. Invert to mix.

6. Combined color reagent: Mix 150 mL of stock mercuric thiocyanatesolution with 150 mL of stock ferric nitrate reagent and dilute to1000 mL with deionized water. Vacuum filter through a 0.45 micronmembrane filter.

Notes:

1. Samples must be diluted to obtain concentrations within the optimumworking range.

2. The gain and zero settings are guidelines and must be adjusted eachday to optimize.

3. The chloride standards may be combined with alkalinity and sulfatestandards for use with the 3 channel method.

4. Any sample with turbidity must be filtered prior to analysis. (UseWhatman #1 or #4. )

5. Color is an interference, dilute the sample and also spike thissample to confirm the quality of the result.

System Operation:

A. Refer to "Auto Analyzer Operation Start-up procedure".(IOP# LAA-SPCtion A)

C1AA-2

B. Analyze a blank and an EPA check standard at the beginning ofeach run.

C. Use a 40 ppm Cl for the spike level.

D. The cal ibrat ion check standard is 50 mg/L ( D ) .

E. Refer to "Auto Analyzer Shut-down procedure".( IOP# LAA-sect ion B)

Quality Control:

1. Establ ish a standard curve wi th the standards listed above.Record the check standard in the check standard book. Theconcentration should remain consistent from run to run. Ifnot, necessary troubleshooting must be performed beforecontinuing (check reagent, pump tubing, valves, etc.) .

2. A quality control calibration standard of 50.0 mg/L is to beanalyzed, at a minimum, after every 10 samples. If less than 10samples are analyzed, a calibration standard is still required.The last sample analyzed in the run is to be the calibrationstandard. These standards must be within the acceptable rangesor the samples run after the last acceptable check standard areto be reanalyzed. Record the calibration standards in the qualitycontrol book. The acceptable limits are noted in the qualitycontrol book.

3. Duplicate and spike a minimum of 1 out of 10 samples. If less than10 samples are analyzed, a duplicate and spike are still required.Duplicates are to be averaged. Spike samples with a standard in a1:1 ratio of sample to standard. Spike recoveries and duplicatesare to be within acceptable ranges or troubleshooting must beperformed.

Calculations:

1. Calculate with Lachat QuikChem software, in the concentrationmode, using the IBM XT computer.

Revision Date

8-18-87Michael J. LinskensLaboratory Manager 7~~&

K urr\Kim D. F innerAnalyt ica l Laboratory QA/QC Off icer

V-

Lawrence D. AndersenVice President, Technical Services

[KAW-3-9] C1AA-3

SULFATE - AUTOANALYZER

Scope and Appl icat ion: This method is applicable to drinking water,surface water, groundwater, and wastewaters.

Reference: EPA, 1983, Method 375.2Lachat Instruments, 1986, QuikChem Method 10-116-10-2-B

Detection Limit: 5.0 mg/L


Sample Handling: Refrigerate at 4CC and analyze within 28 days of collection.

Instrument Condition:

1. Load time: 20 seconds2. Inject Period: 30 seconds3. Inject to peak start period: 9 seconds4. Inject to peak end period: 54 seconds5. Cycle time: 50 seconds6. Gain: 2007. Zero: 7008. Interference filter: 460 nm9. Sample loop: 10 cm

10. Standards to use for curve set-up: 0, 25.0, 50.0, 100, 150, 200 mg/L,


1. Degassing with helium - 2 options:

a. Boil Milli-Q water vigorously for 5 minutes. Cool and storein cubitainer.

b. Bubble helium, using the fritted gas dispersion tube, throughthe Milli-Q water. (15 min/20 L.) Store in cubitainer.

2. Carrier (0.3 ppm S0d=): In a 1 liter volumetric f lask, add 0.3 mL

of 1000 ppm stock sulfate solution and dilute to mark with degassedMilli-Q water.

3. Barium chloride solution (6.24M): In a 1 liter volumetric f lask,dissolve 1.526 g of barium chloride dihydrate (BaCl 2 -2H 2 0) in 500 mLof degassed Milli-Q water and dilute to 1 liter.

4. Hydrochloric acid ( l .QN): In a 100 mL volumetric f lask, containingapproximately 80 mL of Milli-Q water, add 8.3 mL of concentratedhydrochloric acid and dilute to the mark with Milli-Q water.

S04AA-1

5. Barium - MTB color reagent: (The purity of the methyl thymol blue andthe alcohol can be crit ical. USE THE SOURCES STATED B E L O W . )

In a dry 1000 mL volumetric f l ask , place 0.2364 g of methylthymolblue ( 3 ' , 3"bis-N,N-bis carboxymethyl )-amino methylthymolsul fon-ephthalein pentasodium salt (Kodak No. 8068). Add 50 mL of bariumchloride solution ("3" above). The solution may be used to aid inthe transfer of the dye. Swirl to dissolve. Add 8.0 mL of the 1.0N HC1 solution ( "4" above) and mix - solution should turn orange.Add 142 mL deionized water and dilute to 1000 mL with ethanol (Aldr ich24.511.9) Mix. The pH of this solution should be 2.5. Preparethis solution the day before use and store it refrigerated in anamber bottle.

6. Sodium hydroxide (50% stock solution): Cautiously dissolve 500 g ofof Milli-Q water. Cool and dilute

CAUTION: The solution willsodium hydroxide (NaOH) in 600 mLto 1 liter. Store in plastic bottle.become very hot!

7. Sodium hydroxide (0.18 N): In a 1 liter volumetric f lask, add14.4 mL of 502 sodium hydroxide ( "6" above) to degassed Milli-Qwater, and dilute to the mark.

8. Buffered EDTA (for cleaning manifold) : In a 1 liter volumetric flask,dissolve 6.75 g ammonium chloride (NH4C1) in 500 mL Milli-Q water.Add 57 mL concentrated ammonium hydroxide and 40.0 g tetrasodium EDTAdihydrate. Dissolve by swirling; dilute to the mark wi th Milli-Qwater.

9. Sulfate stock (1000 mg/L): Dry approximately 2 g of sodium sulfateat 105 "C for 2 hours. Cool in a desiccator. In a 1 liter

volumetric f lask, dissolve 1.479 g of the dried sodium sulfate inMilli-Q water and dilute to 1 liter. (1.0 mL = 1.0 PC S04

=).

10. Working standard: (Prepare fresh every 2 months)


0 mg/L25.0 mg/L50.0 mg/L100 mg/L150 mg/L200 mg/L

LetterIdentifier

ABCDEF

Volume of StockSulfate Standard

05.0

10.050.075.040.0

200 mL200 mL200 mL500 mL500 mL200 mL

Note: Final volumes are not the same.Computer refers to standards by letter.

S04AA-2

Preparation of Ion Exchange Column:

1. Make a slurry of approximately 0.5 g of BioRex 70, 50-100 mesh ionexchange resin in Milli-Q water.

2. Remove one column end from the glass column. Fill the column withwater, then aspirate the slurry or a l low it to sett le by gravity tooack the column. Take care to avoid trapping air bubbles in thecolumn and its fittings at this point and all subseauent operations.

3. After the resin has settled, replace the end fitting. To ensure agood seal, remove any resin particles from the threads of the glass,the column end and the end fittings. To store the column, the endsof the Tef lon tubing may be joined with a union.

4. To test the ef fect iveness of the column, make uo a standard of puresodium sul fate and compare its peak height to an identical standardwi th hardness typical of the samples added. If the column is beingdepleted, the standard with hardness will read lower because thedivalent cations are complexing the free MTB. The concentration ofthp standard should be mid-range. If depletion has occured, repackthe column with fresh resin.

5. Regenerating Resin: Batch regeneration is recommended because thehydrogen form of BioRex 70 can swell considerably more than thesodium form. Collect the used resin in a small beaker or flask.W a s h wi th dilute HC1 until the wash tests free of calcium and/ormagnesium. This procedure removes the divalent cations byconverting the carboxylate exchange group to the protonated form -COOH. Convert the resin back to the sodium form by neutralizingwith washes of 0.5M NaOH until the wash has a pH of 9 or greater.Rinse wi th deionized water for storage or repacking. A column maybe used for 3-4 Trays (approximately 150 samples) before it needsto be replaced.

Notes:


2. Sulfate standards may be combined with alkalinity and chloridestandards for use with the 3-channel method.


S04AA-3

4. Inteferences:

- The cat ion exchange column removes mult ivalent cat ions. Run amid-range sulfate standard containing a typical concentrat ion ofCaC03 periodically to check performance. Any decrease in peakheight should indicate the need to regenerate or replace theresin. (At 600 ppm CaC03, the column is good for 80 + inject ions.)

Samples with pH less <2 should be neutralized. High acidconcentrations can displace multivalent cat ions from the column.

- Color wi l l interfere. Dilute the sample and a l so spike this sampleto confirm the quality of the result.

- Turbidity - turbid samples may be filtered (use Whatman #1 or#4) prior to analysis on Lachat.

- Orthophospha te also forms a precipitate with barium at high pH.Check the response of pure orthophosphate standards, if samplesare known to be high in

5. Troubleshooting:

A. Baseline noise with reagents pumping.

1. Noise with column in line but good baseline without column.

a. Repack column, air bubbles may be causing pulsing.

b. Check flow fit connectors and end fittings on columnfor blockage or leaks.

2. Noise with and without column in line.

a. Degas carrier and/or reagents. Fine bubbles causesharp spikes on baseline.

b. Place a longer piece of manifold tubing on the outletof the flow cell leading to the waste container. Thismethod requires the use of the screw type flow cell.

c. Replace the pump tubes. The si li cone tube, used for thecolor reagent, wears faster than the PVC pump tubes.

d. W i th water pumping in the lines, check all hydraulicconnections for blockages, leaks, etc.

S04AA-4

B. Baseline drift.

1. Clean the manifold wi th the buffered EDTA.

2. Turn the gain high and use the shortest sample loop possible.This improves the linearity of the calibration curve, prolongsthe useful life of the column, and minimizes the build up ofBaS04 on the manifold tubing.

System Operat ion:

1. Refer to "Auto Analyzer Operation Start-up procedure" (SOP# LAA-SPCtion A ) .

2. Pump reagents through lines until baseline is stable. Then turn offpump and insert column.

3. Pump reagents through the lines before inserting the column. Use ashort piece of manifold tubing in place of the column. When all airhas passed and the baseline is steady, turn off the pump and insertthe column. The column should be placed in a vertical position withf low in the top and out the bottom. In this configuration, the columnwill operate effectively even if the resin packs down more to leave agap at the top. Resume pumping.

4. Analyze a blank and an EPA check standard at the beginning ofeach run.

5. Use a 75 ppm spike level. The calibration check standard is100 mg/L ( D ) .

6. To shut down, turn off pump and remove the column.

To remove the column:

a. Turn off the pump.b. Remove the column.c. Join ends of the column with a union.d. Replace the column on the manifold w i th the short teflon tubing

piece.e. Rinse manifold with Milli-Q water.f. Rinse manifold with EDTA cleaning solution.g. Rinse manifold aoain with Mill i-Q water,h. Pump dry.

Follow "Auto Analyzer Shut-down procedures" (SOP# LAA-Sect ion B).

Quality Control:

S04AA-5

A quality control calibration standard of 100 mg/L is to beanalyzed, at a minimum, after every 10 samples. If less than 10samples are analyzed, a calibration standard is still required.The last sample analyzed in the run is to be the calibration standard.These standards must be within the acceptable ranges or the samplesrun after the last acceptable check standard are to be reanalyzed.Record the calibration standards in the quality control book. Theconfidence limits are noted in the quality control book.

Duplicate and spike a minimum of 1 out of 10 samples. If less than10 samples are analyzed, a duplicate and spike are still required.Duplicates are to be averaged. Spike samples with a standard ofa 1:1 ratio of sample to standard. Spike recoveries and duplicatesare to be within acceptable ranges or troubleshooting must beperformed.

Calculations:

1. Calculate with the Lachat QuikChem software, in the concentrationmode, using the IBM-XT computer.

Revision Date

8-18-87Michael J. LinskensLaboratory Manager

•Kmm -TL/Kim D. FiI nnerAnalytical Laboratory QA/QC Officer

Lawrence D. AndersenVice President, Technical Services

[KAW-3-13] S04AA-6

2. Spikes will be distilled at a level of 0.20 mg/L. The calibrationcheck standard is 0.10 mg/L.

3. Analyze a blank and a standard at the beginning of each run. An EPAstandard is to be analyzed, at a minimum, monthly.

4. If a sample and spike are overrange:

- Dilute the sample and spike if dilution 1:5. The distilled spikestandard will still be detectable.

- Dilute the sample and do a manual spike if dilution is 1:5.

5. Refer to Auto Analyzer shut-down procedure. (SOP # LAA - Section B).

Quality Control:

1. Establish a standard curve with the standards listed above. Theconcentration should remain consistent from run to run. If not,necessary troubleshooting must be performed before continuing (checkreagents, pump tubing, etc.).

2. A quality control calibration standard of 0.10 mg/L is to be analyzedat a minimum, after every 10 samples. If less than 10 samples areanalyzed, a calibration standard is still required. The last sampleanalyzed in the run is to be the calibration standard. Thesestandards must be within the acceptable ranges or the samples runafter the last acceptable check standard are to be reanalyzed.

3. Duplicate and spike a minimum of 1 out of 10 samples. If less than 10samples are analyzed, a duplicate and spike are still required.Duplicates are to be averaged. Spike recoveries and duplicates are tobe within acceptable ranges or troubleshooting must be performed.(These samples must be carried through the distillation step.)

Calculations:

1. Calculate with Lachat QuikChem software, in the concentration mode,using the IBM XT computer. Be sure to calculate any distillationdilution into the final result.

[602-98a]CNAAC-4

8. Cyanide Standards:

Prepare by pipetting the volumes noted below into 250 mL volumetricflasks, adding 50 mL of 1.25N NaOH, and diluting to the mark with D.I,water. (The 1.25N NaOH must be added - very important!) Preparefresh weekly.


0.00 mg/L0.01 mg/L0.02 mg/L0.10 mg/L0.20 mg/L0.40 mg/L

LetterIdentifier

ABCDEF

Volume of 5 mg/Lworking standard

0 mL0.5 mL1.0 mL5.0 mL10 mL20 mL

Note: Computer refers to standards by letter.

NOTES:

1. This chemistry is temperature sensitive. It is crucial to have allreagents, samples and standards at room temperature before runningsamples or sensitivity drift will result.

2. Any sample dilutions must be diluted with 0.25N NaOH, not water. Youmay use the carrier or the zero standard for this.

3. Interferences are reduced or eliminated by the distillation procedure.Cyanide analyses suffer from many interferences. See EPA and StandardMethods references for detailed discussion. Information andrecommendations for the manual pyrldlne-barbituric add colordevelopment also apply to this automated method.



6. Color 1s an interference, dilute the sample and also manually spikethis sample to confirm the quality of the result.

System Operation:

1. Refer to "Auto Analyzer Operation Start-up Procedure" (SOP # LAA -Section A).

[602-98a]CNAAC-3

3. Phosphate Buffer - 0.86M (pH 5.2):

In a 1 L volumetric flask, dissolve 97.0 g KH2P04 in 800 mL degassedMilli-Q water. Add 8.1 mL concentrated (85%) phosphoric acid. Diluteto the mark and invert several times.

4. Chloramine-T Solution:

Dissolve 2.0 g of chloramine-T in 500 mL degassed Milli-Q. Preparefresh weekly and store refrigerated.

5. Pyri'dine - Barbituric Acid Reagent:

In the fume hood, place 15.0 g barbituric acid in a 1 L beaker and add100 mL of degassed Milli-Q water, rinsing down the sides of the beakerto wet the barbituric acid. Add 75 mL pyridine (CsHsN) while stirringwith stir bar. Mix until barbituric acid dissolves. Add 15 mLconcentrated HC1 and stir. Transfer to a 1 L volumetric flask, diluteto the mark with degassed Milli-Q water and invert several times.Refrigerate. Prepare fresh every 2 months.

6. Stock Cyanide Solution (1000 mq/L):

Dissolve 2.51 g KCN and 2.0 g KOH and dilute to 1 liter with D.I.water in a volumetric flask. Standardize against standard silvernitrate tltrant each use. Refer to Standard Methods, 16th Edition,pp. 337-338, Method 412D for the standard procedure. Solution losesstrength with time. If, upon standardizing, the solution falls below980 mg/L cyanide, the stock must be remade; otherwise, prepare freshevery 6 months. CAUTION; TOXIC!

7. Standard Cyanide Solution (5.0 mq/L):

Dilute 5 mL of stock cyanide solution to 1 liter with D.I. water usinga volumetric flask. Prepare fresh weekly.

[602-98a]CNAAC-2

TOTAL CYANIDE - AUTOANALYZER

Scope and Application: This method is applicable to distilled groundwater,drinking water, wastewater, sediments and soils. Allsamples must be distilled prior to analysis with theautoanalyzer. (Refer to SOP # CNDIS.)

Reference: EPA, 1983, Method 335.3Lachat Instruments, 1986, Method 10-204-00-1-AStandard Methods, 16th Edition, pages 337-338

Instrument Detection Limit: 0.01 mg/L

Optimum Concentration Range: 0.01 - 0.40 mg/L

Sample Handling: Samples should be capped and refrigerated at 4*C afterdistillation.


1. Pump speed: 352. Cycle period: 60 seconds3. Load period: 30 seconds4. Inject period: 30 seconds5. Inject to start of peak period: 20 seconds6. Inject to end of peak period: 75 seconds7. Gain: 140 x 10 (use lOx gain)8. Zero: 3809. Interference filter: 570 nm10. Sample loop: 150 cm (0.80 mm i.d.)11. Standards for calibration: 0, 0.01, 0.02, 0.10, 0.20, 0.40

Reagent Preparation: (Prepare fresh every 6 months unless otherwise noted.)

1. Degassed Milli-Q-water - 2 options:

a. Boil Milli-Q water vigorously for 5 minutes. Cool and store incubitainer.

b. Bubble helium, using the fritted gas dispersion tube, through 20 LMilli-Q water for 15-20 minutes. Store in cubitainer.

2. Carrier - 0.2SN NaOH;

In a 1 L volumetric flask, dissolve 10.0 g NaOH in 900 mL degassedMilli-Q. Dilute to the mark and invert several times. Store in aplastic bottle.

[602-98a]CNAAC-1

C

_C Q O L I H G W A T E R "

O U T

INLET

S C R E W C L A M P

I

J v.TO LOW V A C U U M

SOURCE

- A B S O R B E R

DISTILLING F L A S K

HEATER —

FIGURE 2

CYANIDE DISTILLATION A P P A R A T U S

CNDISC-6

Calculation:

Calculate with Lachat QuikChem software, in the concentration mode,using the IBM XT computer. (Be sure to calculate in any distillationdilution into the final result.)

[602-95a]CNDISC-5

9. Using a graduated cylinder, add 20 mL magnesium chloride solution intothe air inlet tube and rinse the tube with D.I. water.

10. Turn heating mantle on to 60-63% of scale. Watch vacuum ratecarefully and adjust as necessary maintaining a rate of one bubble persecond. As the temperature increases, bubbling increases, and thesolution can be drawn from the absorption tube or blown out the airinlet tube. Reflux for one hour after the sample comes to a boil.

11. Turn off heat and continue vacuum for 15 minutes.

12. Disconnect absorber and shut off vacuum pump.

13. Pour solution from absorber tube into a 250 mL volumetric flask.Using D.I. water, rinse the absorption tube (3 times) and add to thevolumetric flask. Dilute to mark with washings from the absorber.Mix by inverting.

14. Distillates are ready for analysis. Proceed with Lachat SOP I CNAACfor the automated colorimetric step.

Quality Control:

1. The standard curve does not need to be carried through thedistillation procedure,

2. A reagent blank is to be analyzed with each set of samples. Thisblank is to be carried through the distillation steps as a check forcontamination.

3. A quality control calibration standard of 0.10 mg/L cyanide is to beanaylzed with each set of samples. This standard is to be carriedthrought the entire procedure Including the distillation step. Thisstandard must be within acceptable ranges or the samples are to bereanalyzed.

4. Duplicate and spike a minimum of 1 out of 10 samples. If less than 10samples are anaylzed, a duplicate and spike are still required.Duplicates are to be averaged. Spike recoveries and duplicate resultsare to be within acceptable ranges.

5. Aqueous and solid/seml-solid samples are separate matrices.Duplicates and spikes are required for each matrix type.

[602-95a]CNDISC-4

3. Sulfides interfere by forming thiocyanate at a high pH. If sulfidesare believed to be present, put a drop of sample on lead acetate testpaper treated with acetic acid buffer solution at ph4. Darkening ofpaper indicates sulfides. If sulfides are present, add 50 mL ofbismuth nitrate solution after the air rate is set through the airinlet tube. Mix for 3 minutes prior to addition of H?S04.Alternatively, Cd 03)2 20, CdC03 or PbC03 can be added after thedistillation, but prior to color development. Bismuth nitrate addedprior to the distillation process is the preferred choice.

4. Fatty acids, high carbonates, and aldehydes can interfere. Refer toStandard Methods for troubleshooting.

5. High concentrations of N03 and N02 can give false positive results.If samples contain high concentrations of N03 and/or N02, add 50 mL ofsulfamic acid solution after the air rate is set through the air inlettube. Mix for 3 minutes prior to addition of H2S04.

Procedure:

1. All glassware is to be soap and water washed, tap rinsed, anddeionized rinsed prior to analyses. Dichromate and acetone may alsobe used to clean the glassware prior to the soap and water wash.

2. Connect and set up cyanide reflux distillation apparatus as shown inFigure 2. (See pg. CNDIS-6).

3. Prepare the 0.10 mg/L cyanide calibration standard as follows:

Add 5 mL of the 5 mg/L cyanide solution to 500 mL of DI water.(Prepare in the distillation flask.)

4. Pour 500 mL of sample Into cyanide distilling flask. If a solid orsemi-solid sample is to be anaylzed, use a 1-5 g sample size and add500 mL of D.I. water to the distilling flask. (Record the amount ofsample used.)

To Spike: Add 10 mL of the 5 mg/L cyanide solution to the 500 mLof sample.

5. Using a graduated cylinder, add 50 mL 1.25 N sodium hydroxide to theabsorber tube and connect.

6. Turn on vacuum pump and adjust so that one bubble per second entersthe distillation flask through the air inlet tube.

7. Add 50 mL of B1(N03)3 solution to flask.

8. Slowly add 25 mL concentrated sulfuric acid through the air inlettube. Rinse the tube with D.I. water and wait for about 2-3 minutes,until the sulfuric add has been dispersed into the sample.

[602-95a]CNDISC-3

3. Stock Cyanide Solution (1000 mq/L):

Dissolve 2.51 g KCN and 2.0 g KOH and dilute to 1 liter with D.I.water in a volumetric flask. Standardize against standard silvernitrate titrant each use. Refer to Standard Methods, 16th Edition,pp. 337-338, Method 412D for the standard procedure. Solution losesstrength with time. If, upon standardizing, the solution falls below980 mg/L cyanide, the stock must be remade; otherwise, prepare freshevery 6 months. CAUTION: TOXIC!

4. Standard Cyanide Solution (5 mq/L):

Dilute 5 mL of stock cyanide solution to 1 liter with D.I. water usinga volumetric flask. Refrigerate. Prepare fresh weekly.

5. Bismuth Nitrate Solution;

Dissolve 30.0 g of 81 03)3 in 100 mL of D.I. water. While stirring,add 250 mL of concentrated acetic acid. Stir until dissolved. Diluteto 1 liter with D.I. water.

6. Sulfamic Acid Solution; Dissolve 40.0 g of sulfamic acid in D.I.water. Dilute to 1 liter.

Notes:

1. CAUTION; Use care in handling of samples with cyanide because of thetoxlcity. Avoid skin contact, inhalation, or ingestion. ALWAYS HAVEA RESPIRATOR IN AREA WHEN DOING THIS TEST.

If a sample begins to bump or back up the tube, quickly increase theflow rate, pull out the Inlet tube, turn the heat off. Thedistillation must be repeated on a fresh sample.

If a sample does boil over, proceed as follows:

- Put on respirator- Turn heat off (For your proctection, use gloves.)- Pull inlet tube out- Put sample Into hood

2. Oxidizing agents, such as chlorine, Interfere by decomposing cyanides.If chlorine is believed to present, put a drop of sample on potassiumiodide starch paper. If paper turns bluish, add a few crystals ofsodium thlosulfate (N32S203; to the sample, mix, and retest. Continueadding sodium thlosulfate until free from chlorine. Then, add 0.1 gsodium thlosulfate in excess.

[602-95a]CNDISC-2

CYANIDE. TOTAL - DISTILLATION

Scope and Application: This method is applicable to the determination ofcyanide in drinking water, surface water, ground-water, sludges, soils and industrial wastes.

Methods: Distillation, Automated Colorimetric

Reference: EPA 1983, Method 335.2

SW-846, Method 9010

Standard Methods, 16th Edition, Method 412

Detection Limit: 0.005 mg/L

Optimum Range: 0.01 - 0.40 mg/L

Sample Handling: Preserve with sodium hydroxide to pH >12 and refrigerateat 4*C. Analyze samples within 14 days.

Reagents and Apparatus:

1. Cyanide reflux distillation apparatus2. 25 mL and 50 mL graduated cylinders3. Vacuum pump4. Heating mantle5. Thermometer6. 250 mL volumetric flasks7. Sodium hydroxide8. Sulfuric acid, concentrated9. Magnesium chloride10. Deionlzed water11. Bismuth nitrate12. Sulfamic acid13. Acetic add, concentrated14. Sodium thiosulfate, crystals


1. Sodium Hydroxide (1.25N);

Dissolve 50.0 g NaOH 1n D.I. water and dilute to 1 liter in avolumetric flask. Store in a plastic bottle.

2. Magnesium Chloride Solution:

Dissolve 510.0 g MgCl2'6H20 in D.I. water and dilute to 1 liter.Store in a plastic bottle.

[602-95a]CNDISC-1

APPENDIX D

INTERNAL CHAIN-OF-CUSTODY PROCEDURES DATAWARZYN ENGINEERING INC.

REVISION: 2

CHAIN-OF-CUSTOOYSuperfund Level

Scope and Appl icat ion: Chain-of-custody procedures are used to maintain anddocumpnt sample possession. This part icular procedureis applicable when full chain-of-custody proceduresare required for enforcement driven investigan'ons.

Reference: NEIC Pol ic ies and Procedures, May, 1978 (Revised March ,1986).EPA-330/9-7R-001-R.U.S. EPA Central Regional Laboratory (10/15/82).

Procedure: Due to the legal nature of enforcement investigations, possessionof samples must be traceable from the rime the samples are collecteduntil introduced as evidence in legal proceedings or destroyed.To maintain and document sample possession, strict chain-of-custodyprocedures are followed.

v

A sample is unacr your custody if:

1) it is in your possesion, or2) it is in your view, after being in your possession, or

L 3) it was in your possession and you locked it up, or4) it is in a designated secure area.

k Field Custody:

•• 1. As few people as possible should handle samples.

2. The field sampler is personally responsible for the care and custody,, of the samples collected until they are properly transferred or

dispatched to the appropriate laboratory.

3. Sample tags/labels shall be completed for each sample, using waterr proof ink (unless prohibited by weather conditions). For example:

a log book notation would explain that a pencil was used to fil1out the sample tag/label because a ball point pen would not function

f in freezing weather.

4. The field project coordinator determines whether proper custodyprocedures were followed during the field work and decides ifadditional samples are required.

L

IrL

1I cor.-i

^

\

I

I

I

Transfer of Custody and Shipment

1. Samples w i l l be packaged properly for shipment and d ispatched tothe appropriate laboratory for a n a l y s i s , w i t h a separate cus todyrecord accompanying each shipment. The method of shipment, couriername, and other pertinent information is entered in the "Remarks"(114) section of the custody record. Shipping containers are "sealed 1

with numbered chain-of-custody seals. The seal numbers are a lsonoted in the "Remarks" section of the custody record.

2. Samples are accompanied by a chain-of-custody record (see Figure 1).When transferring the possession of samples, field personnel wi l lcomplete the information required for II through 111 on the chain-of-custody. Any remarks pertaining to shipping are includedin 114. This information is required prior to the field personnelrelinquishing custody of the samples. This record documents samplecustody transfer from the sampler, to the mobile laboratory or adistant laboratory.

3. Each shipping container will be accompanied by a chain-of-custodyrecord identifying the contents. The original record will accompanythe shipment, and a copy wil l be retained by the field projectcoordinator.

Sample Receipt and Sample Log-In Procedures

Safety Precautions: All samples received should be considered hazardousand appropriate precautions should be taken whenhandling these samples. Under no circumstancesshould any personnel other than the sample custodianor project leader open coolers. If damage or leakageis noted, stay clear of the coolers and notify thesample custodian or project leader immediately. Allsamples will be opened in a hooded area!

Procedure:

1. The project leader will notify the sample custodian in writing ofincoming samples.

2. The custodian will receive the samples and deliver them to a hoodlocated in the analytical laboratory. The procedures describedbelow will be followed by the sample custodian:

2.1 Examine the shipping container and record the following informationin the project log book (one container per form). Refer to Figure 1.

- The presence/absence of custody seal on the shipping container.

f - The condition of the custody seal (i.e., intact, broken).L

I

ICOC-2

E\I

2.2 Open the shipping container in a well ventilated hood, remove theenclosed sample Documents, and record the following information inthp log book.

- The presence/absence of the chain-of-custody record(s).

- The presence/absence of airbills and/or bills of ladingdocumenting shipment of the samples.

2.3 Remove the samples from the container and record the followinginformation in the log book.

- Condi ton of samples (intact, broken, leaking, etc). Any brokenand/or leaking samples should be carefully repacked, labeled asBiohazard, and returned to the client.

- The presence/absence of sample tags.

- Sample tag numbers. Compare these numbers with the chain-of-custody recorrJ(s) (Figure 3). If sample taq numbers do not match,record this fact.

2.4 Compare the following docuifents to verify agreement of the informationcontained on them.

- Chain-of-custody records.

- Sample tags.

- Airbills or bills of lading.

2.5 If there are no problems with the sample shipment, sign the chain-of-custody record in the "Received for laboratory by:" box (Figure 3 -112 and 113). If problems are noted, sign for shipment and note problemsin the "Remarks" (114) box or reference other forms detailing the problemsand inform the Inorganic laboratory supervisor. The supervisor will contactthe project manager to resolve any problems.

3. Log-In the samples.

Figure 4 is an example of the form the sample custodian will use tolog-in the sample and to record the Information previously described.

Each sample is assigned a unique sequential laboratory number. Thelaboratory number is entered on the chain-of-custody (115).

The sample custodian will remove the sample tags. All tags willbe placed in sealed plastic bags and placed in the appropriateproject file.

COC-3

4. Sample Storage

4 . 1 Samples and extracts wi l l be stored in a secure area desfor chain-of-custody samples.

4.2 Damaged samples w i l l be disposed of in an appropr iate ~*nner andthe method of d isposal documented.

4.3 The storage area wi l l be kept secure at all titres. The samplecustodian wil l control access to the storage area. (Dup l i ca tekeys for locked storage areas will be maintained by the laboratorymanagement s ta f f only.

4.4 Whenever samples are removed from storage, this removal wi l l bedocumented. All transfers of samples wil l be documented on theinternal chain-of-custody records. (See example - Figure 2.)

4.5 Samples and extracts will b«» stored after completion of analysisin accordance with the contract or until instructed otherwiseby the enforcement Project Officer.

4.6 The location of stored extracts wil l be recorded,

4.7 YOA samples will be stored separately from other samples.

4.8 Standards will not be stored with samples.

4.9 Samples requiring refrigeration are stored in the Raetone refrigeratorand metal samples are to be stored on shelves in the metals lab.

5. Sample Securi ty

5.1 Samples will be stored in a secure area.

5.2 Access to the laboratory will be through a monitored area. Otheroutside-access doors to the laboratory will be kept locked.

5.3 Vis i tors will sign a visitors log (located at the reception areadesk) and be escorted while In the laboratory area.

5.4 Refrigerators, freezers, and other sample storage areas will besecurely maintained or locked.

5.5 Only the designated sample custodian and the supervisory personnelwill have keys to locked sample storage area.

COC-4

rr

r

EII

5.6 Samples w i l l remain in secure sample storage until removed forsample arepara r ion or a n a l y s i s . A l l t r ans fe r s of samples in toand out of storage w i l l be docmnentod on an internal c n a i n - o f -Ci/Stody record. An example ot an inTerna l cha in -o f -cus todyrecoro used for th is procedure is a t tached . (See Figure 2 . }

5.7 These internal custody records w i l l be maintained in the p r o j e c tf i le.

5.8 A f te r a sample has been removed from storage by the ana l ys t , theanalyst is responsible for the custody of the sample. Eachana l ys t must return the samples to the storage area before theend of the working day.

Internal Chain-of-Custody Procedure:

The following procedure for documentation of internal chain-of-custody forsamples requiring continuous custody.

1. Al l samples wi l l be stored in locked refrigerators located in thesample entry area. A list of sample numbers will be maintainedby the sample custodian.

2. Only the designated sample custodian and supervisory personnelwill have keys to the refrigerators.

3. Samples will remain in the designated refrigerators until removedfor sample preparation and/or analysis.

4. All transfer of samples into or out of the refrigerators will bedocumented on an internal chain-of-custody record (see Figure 2).These records are maintained by the sample custodian.

5. Once a sample is removed from a refrigerator by the analyst, he/sheis responsible for the custody of the sample. Each analyst mustreturn samples to the refrigerator before the end of the workingday. Samples are not allowed to sit on the bench overnight.

6. When sample analyses ana necessary quality assurance checks havebeen completed by the laboratory or after a 3 month time periodwhichever is longer, the unused portion of the sample shouldbe disposed of properly. All identifying tags, data sheets, and

COC-5

r

L

rL.

laboratory records sha l l be reta ined as part of the permanentdocumentation of rue project . T a o s and forms are never d iscarded!

Revision Date

Fb

r^

r

r

9-26-86Michael J. LinskensLabora tory Manager

Kim 0. FinnerAnajytical Lab/T'itory QA/QC Off icer

^^O^^utx ]{/£+<.Lawrence D. AndersonVice President, Technical Services

[ K A W - 5 - 4 ] COC-6

APPENDIX E

INTERNAL CHAIN-OF-CUSTODY PROCEDURES FORHAZLETON LABORATORIES AMERICA

REVISION 2

APPENDIX F

DOCUMENT CONTROL AND THE EVIDENTARY FILE SYSTEM

REVISION: 2

rrr

rEE\I

APPENDIX FDOCUMENT CONTROL AND THE EVIDENTIARY FILESYSTEM FOR FADROWSKI DRUM DISPOSAL RI/FS

ACCOUNTABLE DOCUMENTS

Accountable documents will include all logbooks, field datarecords, correspondence, sample tags, graphs, chain-of-custodyrecords, and other sample documentaiton forms used, original datincluding laboratory bench sheets, photographic prints andplanning documents.

FILE STRUCTURE

Documents will be arranged in the evidentiary file using theformat specified in Table 1 (attached).

LOGGING OF DOCUMENTS

Documents will be received by the Document Control Officer whowill log them and assign a number to each such that documentswithin each document subclass are separately serialized. Anexception to this will be items such as sample tags, chain-of-custody forms or other documents that are numbered prior toassignment for use.

DOCUMENT ACCESS

Project documents will be secured in a separate, locked filecabinet. Access will be limited by the Document Control Officerto project personnel. A check-out log will be maintained as arecord of access.

EVIDENCE FTTfE AUDIT

Upon project completion, the Warzyn Quality Assurance/QualityControl Coordinator will audit the evidence file forcompleteness. Results of the audit will be documented on theattached form and kept in the Final Evidence file.

FINAL DISPOSITION Qf FILE CONTENTS

The Final Evidence file will be maintained by Warzyn untilissuance of the record of decision (ROD) at a minimum.

rrr

TABLE 1

DOCUMENT CLASSES AND STRUCTUREFOR SUPERFUND EVIDENTIARY FILES

r

EI

Document

File Index

Contracts/Proposals/Bids

Financial

ZUfi

B

Correspondence

Work Plan Documents

Contents

Check out logs and listof active files

Proposals, contracts,purchase orders,specifications - COPIESONLY

Summary of invoicestatus; invoicescorrespondence re:accounts receivable; copyof budget and projecttask setup; COPIES ONLY

Various incoming andoutgoing letters,memorandums, diary notes

Cl-In-housecorrespondence; diarynotes and memos

C2-Outgoing lettes/memos

C3-Incomingcorrespondence

C4-Correspondence logged

Documents other thanproposals; includingHealth and Safety plans,Sampling plans, QAPPs,permit plans; specialinstructions/outlines forconducting the project;Work Plans; WEI plans andspecifications

Page 2 of 7

rr

rr

F

I

TI

L

I

QA File

Field Data

Laboratory Data

QA Work Plan and budget;project history file;sample documentationrecords, etc.

El Sample tags

E2-Chain-of CustodyRecords

E3-Receipt of Samplesforms

E4-Transfer of Samplesforms

Original fielddata/notebooks

Fl-Field boring logs

F2-Well constructiondetails

F3-Geotechnical testing

F4-Geophysical testing

F5-Water Quality testing

F6-Daily field logs

F7-Baildown testing

F8-Structural testing

F9-Miscellaneous/Other

Laboratory test data,including originalanalytical logbooks, labdata, calculations, benchrecords, graphs, etc. fororiginal data and qualitycontrol data

Gl-Analytical laboratorydata

G2-Geotechnicallaboratory data

G3-Materials testinglaboratory data

r!L

Page 3 of 7

rrr Calculations

Photographs

H

r

iii

Originals

Warzyn Reports

Warzyn Drawings

Other Reports/Drawings M

Mi seel1aneous

Checkprint

N

ii

G4-Subcontractedlaboratory data

Calculations, quantityest imates, computerprintouts of tabularizeddata

Photographs, stereopairs, site maps(published zoning,topography, geology,groundwater, bedrock,negatives)

Warzyn original reportsor drafts

Copies of the projectreport or previouspertinent WEI reports

Reference list of reportdrawings; copies orreduced copies oforiginal drawings. Note:original or reducedmylars will be storedseparately

Non-Warzyn reports anddrawings includingliterature, reference,etc.

Other file informationwhich does not fit intoother categories; filemust be named

TEMPORARY FILE ofcheckprints, draftreports or other work inprogress. File must beremoved upon jobcompletion.

Page 4 of 7

I

r

rrrr

PROJECT NO.

PROJECT LOCATION

FILE LOCATION

Yes No

Yes No

DOCUMENT AUDIT CHECKLIST*

DATE OF AUDIT

SIGNATURE OF AUDITOR

Have individual files been assembled (field in-vestigation, laboratory, other)?

Comments:

Is each file Inventoried?

Comments:

E Yes No Is there a 11st of accountable documents?

Comments:

Yes No 4. Are all accountable documents present or accountedfor?

Comments:

E

E

From NEIC Procedure Manual for the Evidence Audit of EnforcementInvestigations by Contractor Evidence Audit Teams, EPA-300/9-81-003-R,April, 1984.

I Page 5 of 7

r

r

E

i

I

Yes _ No _ 5. Is a document numbering system used?

Comments : _

Yes No 6. Has each document been assigned a document controlnumber?

Comments:

Yes No 7. Are all documents listed on the inventory accountedfor?

Comments:

Yes No 8. Are there any documents in the file which are not onF the inventory?

Comments:

Yes No 9. Is the file stored in a secure area?

Comments:

Yes _ No _ 10. Are there any project documents which have beenT declared confidential?

Comments :

I _

I -

IPage^ 6 of 7

rr

Comments:

r

Yes No 11. Are confidential documents stored In a secure areaseparate from other project documents?

Yes _ No _ 12. Is access to confidential files restricted?

Comments : _

r -Yes No 13. Have confidential documents been marked or stamped

"Confidential"?

f Comments:

E ~~II

Yes No 14. Is confidential Information inventoried?

Comments:

Yes _ No _ 15. Is confidential information numbered for documentcontrol?

f Comments:

E zL Yes No 16. Have any documents been claimed confidential under

TSCA?

Comments:

[jap-800-64a]

IPage 7 of 7

L

APPENDIX G

FIELD MEASUREMENTS OF pH AND OPERATING INSTRUCTIONSORION MODEL 211 pH METER

REVISION: 2

r

I

I

I

(Page 1 of 2)

FIELD MEASUREMENT OF pH

Method: Electronic trie

Reference: EPA 1979, Page 150.1

Sensitivity: 0.1 pH unit

Optimum Range: 1-12 pH units

Sample Handling: Determine on-site or within 6 hours.

Reagents and Apparatus:

1. pH meter (Orion Model 211 Mini pH meter).

2. Combination electrodes

3 . Beakers or plastic cups.

4. pH buffer solutions, pH 4, 7, and 10.

5. Deionized water in squirt bottle.

6. All glassware soap and water washed, fo l lowed by two hot waterrinses and two deionized water rinses.

rfriPi

Cal ibration:

L 1. Place electrode in pH7 buffer solution.

2. After allowing several minutes for meter to stabil ize, turn calibra-tion dial until a reading of 7.00 is obtained.

3. Rinse electrode with deionized water and place in pH4 or pHIO buffersolution.

4. Wait several minutes and then turn slope adjustment dial until areading of 4.00 or 10.00 is obtained.

5. Rinse electrode with deionized water and place in pH7 buffer. Ifmeter reading is not 7.00, fol low Steps 2-5 again.

Procedure:

f 1. Calibrate neter using calibration procedure.

2. Pour the sample into a clean beaker or plastic cup.

[

[

[

f

I

I

I

I

LII

(Page 2 of 2)

- 3. Rinse electrode with deionized water between samples. Recheckcalibration with pH7 buffer solution after every 5 samples.

4. Immerse electrode in solution allowing several minutes for meterto stabilize. Make sure the white KC1 junction on side of electrodeis in the solution. The level of electrode solution should be oneinch above sample to be measured.

Notes:

1. When calibrating the meter, use pH buffers 7 and 4 for samples withpH <_ 8, and buffers 7 and 10 for samples with pH >_ 8. If meterwill not read pH4 or 10, something may be wrong with the electrode.Return it to the lab with a note.

2. pH is a temperature dependent analysis. Therefore, temperatures ofbuffers and samples should be within about 2*C. For refrigeratedor cool samples, use refrigerated buffers to calibrate meter.

3. Weak organic and inorganic salts and oil and grease are interferencesin pH measurements. If oil and grease are visible, note on datasheet. Clean electrode with soap and water, followed by 101 HC1.Then recalibrate meter.

4. When not in use, the electrode should be stored in pH4 buffer.

5. Before going into the field:

a) Check batteries;b) Do a quick calibration at pH7 and 4 to check electrode;c) Obtain fresh solutions.

6. Following field measurements:

a) Report any problems;b) Compare with previous data;c) Clean all dirt off of meter and inside case;d) Make sure electrode is stored in pH4 buffer.

(Page 1 of 7)

iI

aINSTRUCTION MANUAL

model 211digital pH meter

L iLLLi

ORION RESEARCHLlil!

1 contentsi• introduction 3

! instrumentdescription 3

Instrument set-up 4

support rodpower sourcemotor check-outconnecting electrodes

measurement procedures 6

general measurement techniquepK moasurcmeni

single-butler standardizationIwo-buller standardization

balleryreplacement 8

recordoroulput 8

repair and service 8

i accessories 9 JJ

: specifications 10 <o

i notlceof compliance 11 *°o

repair/serviceFor Information on repair or replacement ol this instrument, contact OrionResearch loll Ireo Ask lor Customer Service.

ORION RESEARCH INCORPORATED

Customer Service640 Memorial DriveCambridge, Massachusetts 02139 U.S.A.800-225-1480 (Continental U.S.)617-864-5400 (Massachusetts , A l a s k a , Hawaii . Canada)Telex: 921466

OlOUOilonfUiMiclilncoipoiiied FoimiMIi iiIMOOniOM* It • i*ol»ur*dIKdtmukol 0'ion n«»i>chlnco>po»i«d Piinitumu S A

llgur* 1 ®I • At.

IOW

ORION RESEARCH model 21 (/digital pH meter

Oil

orr

ION)

TEMP *C CALID

O

legend (Q)1 stitp chart rocoidci binding posts7 OAT LOW3. LC dttplty4. lupport tod clipfr. (Knp«r»tui« Indicator contioi

il- «'•,*••"'#••

G AC line nd.iplci input7 lunchon coriliol0. calibration control9. electrode connector

tO. slope control

introductionThe Model 211 is a battery- or line-operated (110*220 V AC adapter) dignm P>Imeter lor livid or laboratory use. The meter is complete with strip chart recoidi.-'binding posts and Is supplied with an unbreakable, gel-lilted combination pitelectrode, one packet ol pH 7 bullcr powder, one bottle lor pH 7 but let. one boniclor distilled water, support rod. electrode holder, AC adapter. si« 1.5 V bancmv..shorting plug, and carrying case.

instrument descriptionSee llguro 1.

t. strip chart recorder binding posts: black post is low (ground) and red post ishigh Input side ol recorder. Sec pig* B.

2. BAT LOW: an arrow pointing lowaids DAT LOW appcurs on the dispi.iywhen battery requires replacement.

3. LC display: pH display over therangeolO - 14 with r Ol pM units resolution

4. support rod clip: holds steel rod used lo mount elcctiode holder

5. temperature Indicator control (TEMP *C); compensates lot vanation melectrode slope or temperature changes. Used in two bullet caiii>i*iion

6. AC line adapter Input: jack used to insert AC line adapict With AC i">cadapler operational, the internal bat tery is bypassed

7. function control: rocker switch with three positions • ON. OKF and (ON)Oepiess (ON) lor a momentary leading The switch wiiliciu'n loOFf whenreleased.

8. calibration control (CALIB): used lo calibialc me nicicr wiin UuMors olknown ph.

9. al*clrod« connaclor: accepts GNC connector Irom pM clccliodc

10. slope control: screwdriver adjustment used lo set second bullcr In twobullcr calibration.

0»vQ(D

Ui

O

PE T\4 PV l> tu-

instrument set-upsupport rod

1 Insert steel support rod Into the hole in the support rod clip on side ol theniblci.

2. Mount electrode holder on the rod by pinching lo compress (he spring.Release to hold In place.

power sourceThe Model 211 operate* on six non/ochargeable 1.5 voll batteries or on 110 or220 i 20V. V with an approved AC adaptor (spoclly voltage when ordering). Lowbattery is Indicated by the BAT LOW Indicator on the display.NOTE: Galleries are not rechargeable - use ol line adapter whenever possiblewilt prevent the unit's batteries from being discharged. II battery operation isrltisiicil. follow installation instructions under battery replacement.

meter check-outt. Install six AA batteries in Iho meter. Orient the ( + ) and (-) battery termi-

nals to match the orientation shown in the battery compartment.

2 Depress ON button on the Iron! panel. II llic OAT. LOW indicator on theIronl display lights up, the batteries must be replaced.

3 II battery mode Is not to be used, disregard steps 1 and 2. loser) pin end olappropriate AC line adapter Into the motor, and the other end into the ap-propriate grounded AC line receptacle.

4. Attach ONC shorting plug to ONC Input on Iho bottom side o( Iho rnclcr.Depress ON button on the Ironl panel. Turn CALIB knob so display reads• ileady 7.00. II this cannot be done consult ORION Technical Service.

b. (Wnovt the ahofllng plug. Successlul completion ol steps 1-4 show the• -:V. It teady lor use.

connecting electrode1. Insert Iho ONC connector Into the electrode jack on Hit: bottom panel ol the

meter. Turn connector clockwise until it seals llrmly.

2. Mount electrode In (he clecirode holder by spreading the electrode clipopen and sliding (he electrode into the holder so lhal the clip closes onelectrode cap. Sec figure 2.

3. Follow measurement procedures lo use the meter lo measure pH4. Dlsconnnccl electrode by turning connector counterclockwise until releas-

ed Irom pin.

figure 2

•d»iQ(0

sQuceit <> ifio.n 10 mien <iecnu>ic

measurement procedures

general measurement techniquetemperature: All sample* and buffers should bo at the same temperature, assmall variation* In temperature can cause errors In measurement. The slope olthe pH electrode, the potential ol Iho reference electrode, and Iho pH ol Iho bul-let are temperature-dependent.

cleaning electrodes: Electrode should be rinsed and shaken between measure-ments to remove drops and to prevent solution carryover.

stirring: Stir measured solutions moderately to obtain good contact betweenthe gluss bulb and the solution. Insert electrode lo a dcplh of about 3 cm.

pH measurementssingle bullor standardization(where maximum precision Is nol required)

NOTE For maximum accuracy II Is recommended thai j two bullcr calibrationho pciloimcd once at the beginning ol each day (see page 7). This procedure oniu»e4 Hie con cc I sol ling ol the slope control. Subsequent measurements duringthe dny may be made using a single point calibration.

l. Place (lie electrode in a buffer solution whose pH is near the expected pM ofthe sample. Insert electrode lo a dcplh ol about 3 cm and stir moderately.

2 Get the- temperature Indicator control to the tcmpcraluic ol the buffer

3 tii:i the function control lo ON and allow the buffer loading lo stabilize. Ad-|ir..l tin: CALIBsothal the display indir.nle-j Ihe pllol Ilichiillci Ol the solulion tumpcialuie. See Table i.

4 Hi-move the electrode Irom the buffer solution and rinse by stirringinixli.-i.iicly in distilled waif Shake oil excess chops ol walci.

'j 1'idcc uicctiodc in the sample to a dcplh ol about 3 cm and stir moderately.SIM the function control to ON and allow the lending lo stabilize flccoul the

pH leading.

Iwo-bulfor standardization(where maximum precision Is tequired)

1. Select two buffers lo bracket the expected pH of the sample, with one uoller having a pH of 7.

2. Place the electrode in the pH 7 buffer to a depth ol about 3 cm and stirmoderately. Set the temperature Indicator contiol to the temper atuio ol thebullcr. Set Iho function control lo ON and allow the reading to stabilizeTurn CALIB until the display indicates the pH of the bullcr at the solutiontemperature. See table 1.

3. Remove electrode Irom Ihe first buffer and rinse by stirring moderately indistilled water. Shake oil excess drops ol water .

4. Place Ihe electrode In Ihe second bullcr lo a depth of about 3 cm and stirmoderately. Scl the (unction control to ON and adjust the slop* control un-til Ihe pH at Ihe solution temperature is displayed. See Table 1.

5. Remove Ihe electrode and rinse by stirring moderately in distilled water.Shake oil excess drops of water.

6. Place Ihe electrode In the sample to a depth ol about 3 cm and stirmoderately. Scl the function control to ON and allow the reading tostabilize. Record Ihe steady pH reading.

oH»

-O

TABLE 1

TEMPCC) pH7.00Buller pH 4.01 Buller5 7.08 4.00

10152025

303540

50

60

7.06

7.037017.00

698698697

697

698

4004004004 0 1

4 0 2402

403

408409

pH 10.01 Buffer

102510 1810.1210.06

10.01 •

9.97 •993

989

983--

1

*>'• *

-1

battery replacementTo replace the batteries, remove the panel on the hack cl the muter. Be sure toobse/vc Hie polarity marking when inserting new ballcries.

recorder outputThe icd and block binding posls at Ihe side of Ihe molcr provide an output lorstnp rhiii recording ol absolute mV independent of lunclion mode. Foriccoiiji.-'s will) input impedance ol 100 Kllohrns or greater, Iho output Is lixed loabout lOOmV/pH.pH 14 00 output Is 1.40 V. Lower impedance recorders may beused liui lull-scale output Is reduced.

t Conned the lead Irom Iho high (input side ol the recordci) lo Ihe red bindingpoii ,-md the lead Irom Ihe low (ground) side lo Ihe black binding post.

2 Proceed according lo directions In Ihe snip chart recorder Instructionmanual

repair and servicewarranty covers failures due 10 manufacturer's workmanship or material

(lelcci from the dale ol purchase by the user. User should return the warrantycaul 10 OniON and retain prool ol purchase. Warranty is void II product has beenMiuii-ii. misused, or repairs attempted by unauthorized persons.

waiianiics herein are lor products sold/installed lor use only in Iho United Stalesand Canada For ORION products purchased lor use in all other countries consul!local in country, authorized ORION sales agent/distributor lor product warrantyinformation

A Return Authorization Number must be obtained Irom ORION Laboratory Pro-ducts Customer Service before reluming any product lor in-warranly repair,icplacemcni or credit.

"Ho Lemon" Instrument Warranty

1 lie instrument is covered by the ORION "No Lemon" warranty II the instrumenttails within twelve months Irorn dale ol purchase lor any reason other thanatiusc. HIP purchaser may elect lo have it repaired or replaced al no charge. Thiswarranty covers Ihe original or replacement/repaired meter from dale ol originalmelei puichase; Ihe warranty is not extended beyond Ihe buyer's original war-ranty date

71 d 1

accessories

015600 floss™ opoxy body, bulb guard combination pH electrode

9104BN Laboratory grade combination pH electrode (BNC connector)

910600 GX-scries cpoxy body, gel lilted combination electrode (BNCconnector)

912600 GX-sorlos epoxy body, gel-lilled Mask combination electrode(ONC connectoi)

913600 GX-series epoxy body, gel filled Hal surface combination pllelectrode (ONC connector)

915000 RX scries relillable. epoxy body combination pH electrode (ONCconnector)

9162BN Combination pH electrode with rugged bulb (ONC connector)

9I63BN Combination pH electrode with needle shape (BNC connector)

910004 pH 4 bullcr packets, box ol 25 packets, each packet making200 ml ol bullcr

910007 pH 7 buller packets, box of 25 packets, each packet making200ml ol bullcr

910009 pH 9 buller packets, box ol 25 packets, cacti packet making200 ml of buffer

910104 pH 4.01 buller. 475 rnl bottle

910107 pH 7.00 bullcr. 475ml bottle

9101 to pH 10.01 buller. 475 ml bottle

970899 Dissolved oxygen electrode

910002 Electrode holder

020030 Shorting plug

020120 110V AC line adapter

020121 220V AC line adapter

I.i>•l"

ft.Ji

specifications

Mk jl Q J ^ EJH4a l£fe*4 KA4MB ••OMB

notice of compliance

packagecontents

rang*

resolution

temperaturecompensation

isopolenllalpoint

powerrequirement

dimensions

weight

model 211 digital pH meter, with model 910GOO gel filledunbreakable combination pi I electrode, support rod, elec-trode holder, bodies lot pi I 7 bullcr and distilled water , onepacket pH 7 bullcr powdor, AC adapter, six 1.5V batteries,and carrying case

O t o 14 pH

z 01 pH

manual (Olo 100'C)

pH 7 (llxed)

six 1.5 V batteries;battery III*: 3000 ten second intermittent measurementswhen lino adapter Is nol used.

line adapter: 110 or 220 V ± 20V.. 50/60 Hz

14 cm high x 9 cm wide x 4.5 cm deep

0.4kg

• picllkilleni iub|«l lo clung* without nolki

The Model 211 may generate radio frequency energy and il nol installed andused properly, that is, in strict accordance with Ihe manufacturer's inslruclions, may cause interference lo radio and television reception. II has beentype tested and fount) to comply with the limits lor a Class B computing devicein accordance with specifications in Subparl J of Part 15 ol FCC Rules, whichare designed lo provide reasonable protection against such Interference In aresidential installation. However, (here is no guarantee that Interference willnol occur In a particular installation. II the Model 211 does cause interferencelo radio or television reception, which can be determined by turning the unitoff and on, Iho user Is encouraged to t ry to correct the intcrleience by one or•more of Ihe following measures:

- reorlcnl Iho receiving antenna

- relocate Ihe Model 211 with respect lo the receiver

- move Ihe Model 211 away Irom Ihe receiver

- plug Ihe Model 211 Into a dilferenl outlet so that the meicr and receiver areon different branch circuits

If necessary, Iho user should consult the dealer or an experienced radio/ieicvision technician lor additional suggestions. The user may Imd the followingbooklet prepared by Ihe Federal Communications Commission helpful:

"How lo Identify and Resolve Radio-TV Interference Problems"

This booklet Is available Irom Ihe U.S. Government Printing Ollicc. Washington.DC 20402, Slock No. 004 000 00345 4.

•opt(D

^J

O

APPENDIX H

FIELD MEASUREMENT OF SPECIFIC CONDUCTANCE AND TEMPERATUREOPERATING INSTRUCTIONS - YSI MODEL 33 CONDUCTIVITY METER

REVISION: 2

rr

(Pacre 1 of 2)

FIELD MEASUREMENT OF SPECIFIC CONDUCTANCEAND TEMPERATURE

Me thod: Spec i f i c Conductance, umhos t? 25*C

r Refe rence : EPA 1979, Page 120.1, Standard Me thods . 15th e d i t i o n , pp 70-73IL

Detection L i m i t : 1 umho/cm (? 25*CF^ Opt imum Range : 0.1 - 100,000 umhos/cm

Sample H a n d l i n g : Dete rmine on-site or w i t h i n 24 hours

*• Reagents and Appara tus :

r 1. Conduc t iv i ty meter ( Y S I ) and electrodes.L

2. De ion ized water in squirt bottle.

3. Standard po tass ium chloride solut ion, 0.0100 N.

Procedure:F1 i YSI Conduc t iv i t y Meter

* 1. W i t h mode switch at off posi t ion, check meter zero. If not zeroed,use meter screw and adjus t to zero.

2. P l u g probe into jack on side of meter.

* 3. Turn mode switch to red l ine , and turn red l i ne knob un t i l needlea l i g n s w i t h red l ine on d i a l . Change batteries if cannot be a l i g n e d .

4. Total ly immerse probe in sample. Do not a l l o w the probe to touchthe sample container .

[ 5. Turn mode switch to appropriate conduct iv i ty scale, X100, X10, or X I .*• Use a scale that w i l l give a mid-range output on the meter.

7" 6. W a i t for needle to s tab i l ize (about 15 sec.) and record conduc t iv i tyk m u l t i p l y i n g by scale sett ing.

«• 7. W h i l e gen t ly agi ta t ing the probe, take sample temperature ( * C ) andrecord.

8. Rinse probe w i t h deionized water.

L 9. Record spec i f ic conductivity (1st c o l u m n ) and temperature on F.O.S.sheet.

r

k.

•T

L

(Page 2 of 2)

Notes:

1. C a l c u l a t e conduc t iv i ty using f o l l o w i n g f o r m u l a :

G25 =+ 0.02Tr-257J

G2s = Conduc t iv i ty at 25*C, umhos/cm

T = Temperature of sample, "C

Gj - Conduc t iv i ty of sample at temperature T, umhos/cm

2. Report r esu l t s for the standard solution wi th each data set.

3. Record on f i e l d sheet wh ich meter and probe were used. Meter s h o u l dbe wiped c lean as necessary.

k 4. After r e tu rn ing to lab, compare results with p r ev ious data. Reportproblems to lab personnel.

T_g~s Reagent Prepara t ion :

1. Stock Potassium Chloride Solution, 1.00 N: Disso lve 74.555 g. K Clin M i l l i - Q water and di lute to 1,000 m l . in a vo lumet r i c f l a s k .

k2. Standard Potass ium Chloride Solut ion, 0 O l O O N : D i l u t e to 10.0 m i s .

~ of stock so lu t ion to 1,000 m i s . w i t h M i l l i - Q water us ing a vo lume t r i cpipet and f l a s k .

oat

.•:%*&?; *:,v,v-. v-i'.v.->.-- . - • - •

. i.V.'. -.:!-. Xii.-jCij..-.ViJ:: .1...

T A O I E O F C O N I C N I S

G E N E H A L D E S C R I P T I O N

SPEOHCATlONS

Oi ' lKATlON P i l O C E D u n E

1 Sciup

2 luii ipci i i iuie

3 Salinity

4 Coiuliicuncc

5 E H O I

CinCUlT OtSCHlPHON MAINTENANCE

AND CALIBRATION

2 MjllllOKJIICL*

3

I'MUOE

P;>0*

2

2

•«

5

5

6

99

9

9

1 2

DL-&U>|)|IUII Of VSl 3300 Coi»l.n:|1v.lv/t..-in|.,;oluiu l'i..Ut I 2

3 Puibc Use

•I Cell C.il'lii.ilxiii & Si.»iiijul Sui, ,1,1. us

YSI MODfl 33 AND 33M uSIO W I T H YSl 'j I A -j.1 AND

O X v C f N M E T E H S

I -l

0*vQn>

u-ii

G E N E R A L DESCRIPTIONTin- YSI Model 33 ami 3.TM S-C T MUIIJII me pniuhlc liauciyliowcicJ. lianniloii/cd iniiiuMicmt cli.'iMjni.'il in atcmaicly IIMMSIIICtalmiiy comliiciiviiy and tempciaiuie limy utc a piobo consoling ofa iiinijud (liaslie conductivity cell and a piucition YSI lltuimistoitiiinpuiaiuie sensor combined 10 a smijtc unitConductivity will* tlie Model 33 is c»picssod as miciomlios/ccnli-mot«r Ijimlios/cml. with die 33M. it's millisiomuns/'moiei (mS'm).These iiie munsuicmcnts ol the electrical conductance the samplewould show il measured between opposite laces ol a Icm cube.IConvcision inloimaiion I /miho/cm = 0 I inS/m ) Salinity is theiiuntbci ol ijiamt ol sali.'kilofjiam ol sample |1uo « pans perthousand) Tint mcasuiemunt assumes Ihe sample contains a "sunHind" sea waici uli innune The sample lompeiiiluie is mcasuied inilou'ccs Celsius

Salmiiy miijsuiemi'iiit aie manually lumpciaiuie compcusaiccl byduecl dial Conilm nviiy mcasuienicnis aic not tcmpt'iatuie compun-sjicil liowcvci. a iL-iiipciaiuie luncnon it piovided on ilic msiiumcnlto aid with calculation ol collections Also, whan |usi icmpcialoieand coiHtiicnviiv J'C known u it possible lo cali.nlaic salinity ant)when only luinpciaiiiic iiiul salimiy aic Known ii it possible 10CJICllljle COnUllClivily

SPECIFICATIONS

Modol 33 CunildCliviiy

Ranges

Accuracy

0 500 0 5000 , 0 SO 000iiiniiot/cni wuli YSI 3300 SuncsPiobcs INoie The ,iinlio desig-nat ions on Hie niclei aic aslioiihaiid fonn lot "innho/cm' I

I 2 5% ma< CHOI n\ 500 5 000and SO 000 plus pmbe

I 3 0% IU.IK enoi ai 250. 2.500and 25000 plus piobcSec Enoi SL-UIOM

2

2 5 !»OO

lillllJU

25 j,inim*/i.Mi on 0 000 ii.HUJC

2 5 0

Tumpuiaiuic Compensation None

Model 33M Coi-iluctivity

inlio»/c 00 000

Accuiacy

Ruadability

Tcmpciaiuie Compentanon

Salinity

Ftjityc

Accuracy

0 50 0 500 0 5000 mS-'m «nuYSI 3300 Suno Piuiic*12 5'V> nut ei-oi ji 50 500 j"iiS 000 plus pioliv1 3 OK ma> VHOI ai 75 750 .u»'2 500 plus IHOIICS..-L- CHOI SuCI-uD

025 inS/m on 50 mS'i" ian:jc2 5 mS'm on 500 inS/m onyi-25 0 niS/in on 'j 000 mS/ni i0nyo

None

•O0>

CD

to

O

TL-nt|)uroiuie Compcnsanun

0 10'10 t »5Above '1 0 7 ".piubcBvlovt 0 9piolicSc-C E < >

0 2Mjlllljl

< 4 5 ' C

in lcn'pi:i.iiinc i.hijt- ol 2C

C 10 9 •' . Ji 40 a»rt. ai 20 " ... pin* lundiiiiiviiv

4"C t I.... dl 20

° • ai JO"plui lUnd i l.v.l»

on 0 40 "u. i.iiigc

by iliiL-Ll dill fioni 2 IO

L..,.__,

tf~"* llr~T* '-a^tA v - '

Taiitpnaluf*llanijeAccmacy

Powei Supply

Piob*

Accuucy

IniliuinanlAmbient

2 10 1 00«C

±0 1*C at 2-C i06'C at 45*Cplus p'obcSoc Enoi Si.-ction10 15"C at 2«C to i037'C at15"C

Two 0 site alkalme biineiics. Evercady £95 01 uiimvalcni piovidc appioiimatcly 200 his ol operationYSI 3300 Sonet Conduciiviiy/Tein.PI.-I.HUIU PiobeNominal Piobc Constant K *• 5/cmi 2V ol liljditMj loi conductivity andS3lmilyEnoi ol 10 I 'C at 0- C andI 0 3 C at 10- C

Sanslaciuiy (IDLUIIOM 5 to I 4b*CA ma>inium unoi ol 1 0 I"., ol theluailimj put "C cliiinijt- HI intiiumcnlluinpvitiiiitc' ciin uccui Tliik L-nof ism.-ijliijililc il tin: tuvliu.ii':'.) is icad-|iiiii;(1 to lodlinc loi ouili

O P E R A T I O N P R O C E D U R E1 Setup

lal Ai||ntl illi.-ll-l /l-io til IIL-fl.-Siuiyl ll\- liilli'lll) l!ll; bjkflilCiciL'w on Hie ini:tui l;u:u so iliui Hi< nn-tui m.-i.-iiii- romcxlcstvitli tliu IL-IO on 11 ic ciinduciivily stjiu

Ilil fjlilnjlc HIL- iiirii.-i by iiiiihiiij tliL- M()()t Li.niiol toHI 1)1 INI .mil .nl|,,il.i.u ilu: HCnilNf ii.iiiiiil MI iln: IIII-IITI

needle lines up with Ihe tudlme un the mclm lacu H thiscannot bo accomplished u-placc thu bjticncs

Icl Plug the probe mio ihv piobe |JcV on ihu tide ol Ibu m»uu-inent

Id) Put the piol>c m the solution lo be mcaimed (Sec PioucUse I

2. Tciiipeialur*Set the MODE control 10 l E M i - L R A T u f l E RuJd u«tunipciaiuie on the Ixittom scale of the meter m itojieulCelsius Allow time loi the piobe icmpc'jiuie to conn- 10O(|uilibiium with that ol the wulvi boloic icjd.ny

3. Salinitylot Tunslui Hie tcmpeiatuic icjdinij liom Step 2 to MIC ' C

scale on the msiiumunt(bl Switch the MODE connol lo th< SALINI IY position <ind

mad salinity on the ted 0 40 "'*• inuioi ianu«Id Ocp'ess the CELL T E S T buttcm The mctc-i iCJ.I-mi sbouin

lati less than 2*. il iiieotui the pione is louicii j"0muasuiumunt is m CHOI Clejn Hiu inolie and ic mcji

4. Conductivity on Model 33 (Model 33M duu jn:pnientliesos.llal Switch the MODE connol to the- X 100 scale H the it--

is below 50 on the 0 500 iamjo 15 0 on the 0 00 u<switch to the XIO scale ll the lojii.ng is »tili lidov1501 switch to the XI scale Rcjd Hie mc-lei sc.Hcnuiltiply Ihe icadiiiy appMipnjtuly The ans\se> •*piosscd in |inihos/cm IniS/ml Mi'JSuicmuniS •<":icntpL-iiiiuic compL-n^tiiudExample Mcloi RcaJmg 2 4 7 l 2 4 7 l

Scale XIO

1 2 4 7 0 inS/ml

n<c

IJVI50

not

. .'t--i;.uv~i5(." i. ".-.'/.f-SivAvi;'.*''.' t..'-..

•oOl

vfl(0

• •!.'••

!•:$&*'"

Ibl WltL-n measuring on Iho XI00 and X I O scales, depress theCELL T E S T button The inutcc leading should (all less than2%. if greater, the piobe is fouled and Iho rnoasuiomcni isin enoi Clean die piobo and ic irtuasme

NOTE: The CELL T E S T does not (million mi ibc XI scale

5 EnorThe maximum CHOI m a leading can In: calculated by using diegiaphs m the following sections.Ill Teinpeiaiuit

The icmpciatuie scale is designed to give the minimumsalinity enor when die lumpcraiuie leadings are used tocompensate salinity itu-.'isiiiementsf i-juie I shovtf. total enoi loi probe and instrument vcisus*C rnoiei iuadmg

IHHOII • I—

r.ii. .-I.*?- i*/_» ,s.»_i^Exainplo: Melci nujtl

Total Enoi

Accuracy

I S'C

0 4 ° C

1 5'C 1 0 4"C loi piobejiul insliunteiil cuinbincd

121 Conduchvity on Muilol 33 (Model 33M djia are inpaiemhcscs IFiguie 2 shows the v/orsl case i oiidui.livilv CHOI J4 it luiiclion of the cnnduchvity leading loi the i<i-J>e jnd "itiruntont combined

Fiyure 2

Eiiimple. Mutui RcJilmg 300 nuihui/>.in l3G n.S'ml

S<:.ilo X I O

•;* Rejdnuj CHOI d •» 5V

Ai:cuiacy 3000 I IC2 UIM|III» -'cm1.100 Mb 2 .i.S'ml

•o0*ua(D

131 SalinityThe salinity loadings are a function ol lumpeiaiuio andconductivity, tlicivloie the uccuiacy is a (unction ol bothThe Ivmpvialuic scale and Icmpeiaiiiio cunliol have beendcsignud 10 minimne Iho Icmpi.-iatuio eiror coninbulion toIhv salmily orioi The CHOI shown in FHJUIO 3 is the total ofthe Itmpciatuic and conductivity ptobc. the lempoialuicscale and the salinity scull enoi

Figure 3

• • . . ' . ' • • .- i . • .-' ••.'•••! .1: ,,• \. ••'•;":'.•.'' .;'.'» .•': J- . . ;

tJOllQ(D

Ul

O

'OO *MI*llf AIAOIN6

Eiimpl*: Melei Reading 100/00. fe 10'C

6 5%

I0«bo i 065<Cooloi allcrrois. combined woislcase

ReadingEnor.

Accuiacy

IfciT

I.

Q O-O-O 0-0 w- i.,...Y S - I C_b«"

---

l .1" st '11" ' 9?

|i ,-b*j |

I ,»)UW »»"•*• »• «

/kir'.v «o«t-- 4Air\ }«i < , 100 OHMIMV pr "IJ'C e

r-ui'hb. ' i 7(07 >f

.0) -r:J

.11./.'OO

YSI MODEL 33 AND 33M B 03321 E

;i; a

• H i )

•oo*

v£»(D

en

O

;V:: ^

ifiC

CIRCUIT DESCRIPTION. MAINTENANCE ANO C A L I B R A T I O N1. DosciiplionThe circuit is composed ol two pans, a im.llivibidtoi and switchingtiansistors The mullivilnaior pioduccs a square wavefoim volijgcThe sqtiaio wave is applied 10 two switching uansisiois Ihcy al ter-nately apply two haitenus of opposite polamy to the piobe thusproviding AC power which mimmucs polantjhon elk-cis the meteiis in seiics with on* battery and measmcs the cuncnt liom it ThtCuircnl liom the battery is propoihonal 10 the conductance ul the c«llSalinity it measured in a special lange conductivity cucuit winch ineludes a user adjusted temperature compensator In the tempviatuicrcdlme and XI positions the mulnvibiaioi opciatet at 100 Hi In thesalinity. XI00 and X I O positions the mulliviliiatoi O|ii:iaies .u 600 M;and MI these ranges pushing lite CELL T E S T button diops the lici|uunCy lo 100 III allowing the opuratoi to judge the deijice ol (nuttepolaniaiion

2. Mainlonanc*The only maintenance icquucd is battciy ie|>l,icen\eni Two D ».;ealkaline flashlight cells, such as Eveieady E95 01 equivalent willprovide 200 his ol opeiation Accmocy will not be maintained if nnccaibon "D" cells aic used Ojt te iy iL-placemcni is milic.iicd when theledlmu adjustment cannot lie accomplishedReplace hailencs cvciy Six months to icduce Ihe danger ol cOnosiondue lo leaky batteries To replace haiicncs. icmovc the six sc icwsliom the iear plate The baiteiy hokleis arc coloi coded The PositiveH button) end musi go on ted

3. Culihiiilion ol Modol 33 (Model 33M data aio in paienlhcsos )II is possible loi the lempciaiuic Knob to h«i:ume lonsc or sl.p domUS normal position In an crneigcncy Ihe dial can be ie positioned Itmust be cmphiisi'od thai tins is an emeigi-ncy pioccdmi: i>nly andthat the instrument should be luiuincd to the lauuiy fui piopcileCAlibiation ai Ihu cailictl oppoilumly

0)

(0

-J

o

lal RI:.I.| ihu icmpoialiiie and conductivity ol the siiluinin Dutcr-iiiina Ihu salinity ol die solution by tunning a line vititically onthe gi.iph liom tins conductance value unhl il init.-is.ucis theAppiopnale *C line lintuipolaic as luiiunud loi litmpeialuiubelwucn Ihe given *C lines) Fiom tins iiiliiiscchon extend a

I I I LlUl lLIJ-l.Jl-11 I I I I l-l Ij-LI.Llll IJ.ll_JJ_C10*00 loooo 10000 toooo

lino honronl.llly to the Rdgc of the ijiaph Tins delcmiuto thesalinity loi tins sampleExample 25.000>nnhos/cm and 20"C gives a salinity ol I 7(Example 2.500 mS/m and 20*C gives a sjlmiiy ol t 7 I

|b) Remove die *C knob, switch lo SALINITY, and tum the lOnliolshall until the motor needle indicates Hit: salinity value dctuimined in Step lal. In the example given. Hie value .s I 7

Ic) Switch to TEMPERATURE (Note Tins lemjiciaiuie icailmgmust b* the tame as Step lal. il not. begin aj.im at SI..-P lal IPlace the knob on the contiol ilmlt (without tuinnig Hie lomiolshall) with the knob pointer at die J.m'e leiniKtiaime .is Hitmeter le.idmg and lighten both scl sciews secmely

At oailicst oppoitunily iccaliliiato usmg ihu lollowing jiioci-dun.- orleluin the instrument to factory lot service

la) Sol the msiiumtni lot a salunty moasuiemem as nuimaiIbl Substitute a lOOOjil capacnot and 112 7ohmO 1 \totei.me*

lesistoi loi the piobeConnect the losislor and capacitor between the giecn w.ic and n-dwiie on the jack connections inside Ihe mkiiuinent

GREEN WIRE

RED WIRE

O—

-wv-111.70

.1%1000,

Ol

CO

O

let luin Ihe leinpuiatoie dial until the mciui leads ledluieNow Htkijll tltu tempeiaiuio knob with the aiiow at 20"C Tins is aliriii|i(n.iiy ciililtiojion only Retum the instiumcnt lo the factory lotlini|n-i iei alilnanon

i -nooE1 Desiiiplion ol YSI 3300 Saiics Cunduclivity/Tcinpoiaium

PK>|J«tin: YSi 3300 Sviii-k CoiwIuChviiy Pi otic s aie designed loi licld use.fiiilHMltnig cunkln>u>oii and design lot lugged aciuiatc Suiviccf ijcli |)iol<« features a built-in cell constant ol 5 0 1500 0/MI ± 2%. •juocision VSI tlioimistor i«rn(Mii*iuie sensor ol ±0 I*C nccui.icy at0"C and ±0 3*C at 40*C and a low capacitance cable assembly 101-iiimaiing m a line* thtfiminal 025" ilia phone type connectortin; 3110 has a 10 h calil* ami the 3311 is » 50 It vcision Otheili-Mi|iti> jio av.iiljWt on special onleitin- i u i it ii- lias t iiyid P V C iKMly iilaiiimvd puic nickel electrodes.mil a n,.ur.de table piuv.dmu, ii-vikt.inr.e to a w«le umjc ol w.ncrI.HUM- MitikUiti:es

2 M.iiniiinanceIJI I'li-tfinng

WIM.-II Hit! iirll levl imlii .ili.-v luw lu.iilings IhC |iioli.llilu c.Visi- is dulyi-li:. tiiMli-k Haul maim ili:|iusits Oils and iinjjmi mallei .lie I hi: mostlit i'ly > i.i.ijmnMiusI oi » iii,cnicnl iioimjl ili:aiun<J snjk Hit; i;l«t:lM>ilus Im 5 mmulusw.lli .1 Im .illy .ivail.lblv lulhioom lid* cleaiiuig picp.ii jliun Such asO.iw (.ii,.<n«a> Oailiiuotn Cleaner llfm/on linlukiin:s Rally file-I'liitirl.iiii and Cluome Cle.'mci Juhnkiin Wai f n \ y liiil.liilCli-.im-i ui I viol n..uul Oasin Tub Tile Cle.mei

For snonger cleaning a 5 minute soak m a solution m.nle ol 10 pansdistilled water. 10 pans isnpropyl alcohol and I pan HCl can bo usedAlways rinse Ihe piobe alter cleaning and liefoic sioiageCAUTION Do not touch the electrodes inside the piuhe

Platinum lil.ick is soil and can be sciaped of fII cleaning does nol restore the piolio pciloimancc. ic pljimiimg isrequirod

fbl Ro riatiniimgEniiipincni Requited —(I) YSI (13140 PlaiHtifinn Solution. 2 II ot (3% pljimumchlondo dissolved m 0025% lead aceiatc solution)121 VSI Model 33 or 33M S C T Mole/(3) SO ml glass taieakm 01 equivalent bottle(4) Distilled waterPioccduro —I t ) Clean the piobe at m Section lal e.thei method121 Place the cell in the beakci and add sullicient YSi j|3!40

solution lo covet the electrodes Do not lovci the tnp olthe ptuue

(3) Plug tlte piobe into Ihe Model 33 01 33M iw.i, h to dieXIOO scJle to pliihnire die elecnoile Move ihu |.mbesliu'illy lo obtain Ihe luijhusl mr.-lur rojilmij .md continuejiljiiniimg lot the appioxmuiu tune klh»vn below

T.n.e(ininutesl

568

ftjvflft)

vo

O

Matoi Reading/iinhoi/cm mS/m

30.000 3 00025000 2 50020000 200015 000IOOOO

1 500I 000

I 116

(4) Alter the elajtled limn mmovo the tirobu and nnsu in lieshwater

I'j) Rctoin tho solution to us container 2 01. ol solutionshould be sufficient lor SO treatments

3. Piob* Us*la) Obsiiuclions near the piobe can disluib leadings. At Icovt two

mcliiis ol cleaianc* must be allowed liom non-metallic un-ileiwjici obj' ctt Metallic objects such as pieit 01 weightsshould be kept ai least 6 inches liom the proba.

ll>) Weights aie attached to the cable ol the YSI 3310 and 3311Piobes The YSI 3327 Weights aio supplied in pans with atotal weight ol 4 ounces per pail. Should it become necessaryto add mote weight 10 overcome water cuncnis. we suggestlimiting Ihe total wen)1'! lo two pounds 18 pairs) Foi weightsin excess ol two pounds us* an independent suspensioncaul* In eilhei cat*, weights must be kupl at toast 6 inchesaway liom the piobt

kl Gentle agitation by insmg and lowenng the piobe scvuialtunes duimg ( rncasuremenl insuies How ol specimen solu-tion through the piobe and improves the lime icsponsu ol Ihelempeiatiire sensor

4 Cell Calibialion & Standard SolutionsThe YSI |3300 Sends Cells aie cadbiaied to absolute accuiacy ol-t I 5% li»kud on a standard solution Since the litcialuic on conduc-tivity ikies nol indicate * consistently accepted siaiulaidiiahonmethod we have chukun Ihe 001 denial KCI solution method atileleiinined by Jonct and Bi*<lshaw in 1937 as our slundaid Recentii!»ibuokt. at well as the ASTM standards, concur with this choiceThe solution is pirpaied by diluting 0 745 giams ol pure dry KCI withdislrlled water until the solution is t kilogiam Ihe table billow showsthe values ol conductivity tins solution would have il the distilledwaici weie non conductive However since even high pinny distilled

waici is slightly r.onduciivo. the mciisuied conductivity wilt lieby an amount equal to the watci 's conductivity

Tampoiiilui*151617IB192021222324252627282930

Conductivity/inihos/cm mS/m

I 141 5 1 1 4 21 1 6 7 5 I 1C 81 193 6 1 1 9 41 2 1 9 9 1 2 2 01246 4 1 2 4 61 2 7 3 0 1 2 7 31299 7 1300I 3 2 G 6 I 32 713536 US 413808 13811408 1 14081-136 5 1 4 3 71 4 6 3 2 1 4 6 314909 I-19 l10 I B 7 l >j 1 915-167 104 7

0*

n

oo

The operator may use the siandaid solution and the t.iliie to . icuiacy ol a cell's constant 01 10 deteimmu an unknown <.u>i»uloimula is shown below

-i t .u.lite

R 1C- + CMtb»

R(S. + S i

whcie KRC.C,

Cell constantMeasured lesistancc m '.!Conductivity in fjinhos/cmConduclivily in |iinhns/im of the do'.II.used to ii'/ikc solution

^f?&^^£&''?&$& y* "^ ^ • • • • ' •

.1** • * • • • • • ;i_ ? • • • . . • .. » * . f i •• • . «

S> • Conductivity in mS/mSi • Conductivity m mS/m ol ihu distilled water used

10 make the solution

R. C< and Ci. 01 Si and Si. must eilbei b* duiuimii.i:.! at the sameti.-iiipeialuie 01 concciud lo the same lempuratuic to make the co.ua••on validNoi«. foi luiihoi iiiloimalion on conductivity and the above stan-dard mloiination. icier to ASIM Standaids Pan 23 — StandardMethods ol Test lot Elecliical Conductivity or Waiei and IndustnalWaste Water — ASTM Designation 01125 64

YSI MODEL 33 ANO 33M USED WITH YSI 51A. 54 and 57OXYGEN METERSII the »*imiiy measurcm*nt it to bo used lot salinity collection on the5IA ihe leading should be convened to Chloiosny The lonnula is

Salinity '•.«• -003PPM ChlOiosily

1 8- « i o «

for thes* insiruinunis ihe 003 can he neglected so ihu equation

SS 'v. « 10'PPM CI T8

II 17 3G

— I — I

For salinity collection when using the Model 57 use the >almnyleading direct Irom ihe Model 33 or 33M No conversion isnecessaryModel 33 and 33M salinity leadings taken m conjunction with Model54 dissolved oxygen readings can be used to COHCCI the Moilyl 54 forsalinity and to make post-measurement salinity conechoni to dis-solved oxygen data Coucchon tables aio available horn the lactoiy

WARRANTYAll YSI products cany a one year unconditional \v.i <ly onworkmanship and pans exclusive ol lianrines Damage tiuough .itcident, misuse, or tampering will be icpaned at a nonun.il i Ionic

II you aie cipcnencing dilliCully with any YSI product >i >»;iy berelu/nod to an auihon/ed YSI dealer lot repair even il the \vanamyh*t uxpued II you need factory atsistancu foi any H.MIOII ronlacl

Service Dcpaiin\*ntYellow Spnngt Invlrumtm Co IncPO Oox 279Yellow Springs Ohio U S APhone (5131 767 7 2 4 1

(0

5.000 10.000 IS.buO 70.0OO I'I'MCL

• .r*- '•

APPENDIX I

CALIBRATION AND MAINTENANCE OF PHOTOVAC TIP

REVISION: 2

(Page 1 of 3)

CALIBRATION AND MAINTENANCE OF PHOTOVAC TIP

. CALIBRATIONl h. ^^_^^^^^^_

Two basic calibration operations must be performed. These are adjustment of

zero and the adjustment of span.u

The zero adjustment is the easiest. Under conditions where accuracy is very

*• important and sensitivity is less important, it may be sufficient to zero ther instrument using outdoor air. In other cases, office area or indoor may prove

«. to be clean enough for zeroing purposes. When rigorously done, a source of

"Zero Air" or "Ultra Zero Air" is necessary. These are high purity grades ofcompressed air available in bottled form. The bottle is fitted with a

regulator and can be connected directly to the TIP's input fitting. A very

low rate of flow should be used with pressure applied never exceeding 1 psi

(6 kPa.).

4 Having adjusted zero (this is best done with the "Span" control at maximum),

r we will now turn to span calibration. To assess a situation where there is a

I high ionizable loading in the air consisting of a mixture of many components,it must be recognized that any reading obtained will be a composite of the

| various components. With photoionization, response factors vary greatly fromcompound to compound. This makes the reading on TIP dependent upon both

: concentration and nature of the mixture involved. TIP, in this case, works as

a scoping tool; the user can move around the contaminated area seeking "hot

spots".k

- HNu calibration gas will be used to calibrate the TIP. The TIP probe will beinserted into the gas cylinder feeder base and the gas released. The TIP willthen be adjusted to the gas concentration (generally 52 ppm).

MAINTENANCE

Routine maintenance requirements for TIP are minimal. All that is required is

to assure the batteries remain close to full charge (during periods of

• non-use) and to assure that the inlet frit-filter is kept clear of debris.

The frit is a sintered, stainless type and must be periodically replaced to

r assure free-flow of air to the detector.

rr

rrrr

(Page 2 of 3)

Replacement of the frit is indicated when the inlet flow falls below140 mL/min.

Referring to the TIP pictorial diagram, remove the four cover mounting screws

holding the detector cover in place. Remove any inlet probe that may have

been installed. Make sure the unit is switched "Off". Lift the detectorcover straight off the front of TIP with a twisting motion to overcome

friction against the seal. Take the cover and place it upside down against asoft, but firm, surface such as a block of wood, so that the inlet fittingwill not be damaged. From the inside of the fitting, press out the filter

with a tool such as a l/16th inch hex screwdriver.

Turn the cover right side up and position the new filter squarely in the inletfitting. Press it into position with the same tool.

Make sure that the black PIO seal is in place in its recess in the TIP

j, detector and slip the detector cover into position, twisting it over theseal. Replace the four cover mounting screws.

JFurther maintenance operations that can be performed by the user involve the

cleaning of the ion chamber and the lamp window, replacement of the lamp and

replacement of the battery pack.

L The ion chamber is reached by removing the detector cover (as previously

described), unplugging the yellow collector wire from the printed circuit

t board of the UHF driver, releasing the red repeller wire at its attachmentpoint on the PID (loosen the small screw and pull gently free) and finally,

f unscrewing the PID from the lamp holder by grasping gently but firmly the body

of the PID and rotating counterclockwise. The lamp will pop up on a spring* and may be lifted out for cleaning/replacement. The interior of the ion

L chamber contains a very delicate wire mesh and must not be touched with any

solid object. The lamp window may be cleaned with a cotton swab dipped in

methanol and the interior of the ion chamber may be blown free of dust using a

gentle compressed air jet. The lamp (or its replacement) is simply put back

f into the lamp holder and the PIO screwed back into place being very careful to

avoid "cross threading". The two wires are replaced as before. It is vital

(Page 3 of 3)

to assure that the PID seal is replaced in its seat before putting the coverback onto the detector.

If the pump and LEDs stay off for longer than a minute or so on a fullycharged TIP, the detector lamp driving circuit may need adjustment. Removethe detector cover after which the pump and LEDs should come on as a result ofambient light hitting the photo resistor on the exposed circuit UHF drivercircuit board.

Locate the ceramic trimming capacitor on the UHF driver; it has a screwdriveradjustment slot on the top of it. Be sure TIP is switched off, and make apencil mark on the trimmer capacitor to indicate its original position. Turnthe trimmer adjustment slightly (five degrees or so) in one direction or theother, then replace the detector cover and turn TIP "On". Repeat thisprocedure until the lamp starts. After TIP has run for two minutes or so,turn it off and set the trimmer back to its original position, or very nearit, replace the detector cover, and use TIP.

If the lamp will not start regardless of the trimmer capacitor setting, thelamp likely needs replacing. Set the trimmer to its original position andreplace the lamp as previously described. Lamp replacement is also indicatedif, with fully charged batteries, TIP response drops drastically from one dayto the next. Normally, a slight ozone smell will be present at the TIPvent. A failed lamp will not produce ozone.

T

APPENDIX J

OPERATION PROCEDURE FOR HNu MODEL PI 101PHOTOIONIZATION ANALYZER

EXTRACTED FROM PROTOTYPE PROCEDUREBY

CHEN-WEN TSAI, USEPA QAS

REVISION: 0

OCTOBER 30, 1987

rI

r

ii

TABLE OF CONTENT

r I. INSTRUCTION

1.0 OPERATION PRINCIPLE

2.C INSTRUMENT SENSITIVITY AND CALIBRATION

3.0 INSTRUMENT SPECIFICATIONS

II. OPERATIONAL PROCEDURE

1.0 INSTRUMENT CHECKOUT

2.0 FIELD OPERATION

2.1 CALIBRATION

2.1.1 EQUIPMENT AND MATERIALS

2.1.2 CALIBRATION FREQUENCY

2.1.3 CALIBRATION PROCEDURE

2.2 SAMPLE MEASUREMENTS

III. MAINTENANCE AND TROUBLE SHOOTING

1.0 BATTERY RECHARGING

*• 2.0 GENERAL FAULTS DETERMINATION AND CORRECTION

3.0 SPECIFIC FAULTS

rrrr

rr

EC

OPERATION PROCEDURE FORHNu MODEL PI 101

PHOTOIONIZATION ANALYZER

I. INTRODUCTION

1.0 Operation Principle

The HNu Model 101 photoionization detector has been designedto measure the concentration of trace gases in many industrialor plant atmospheres. The instrument has similar capabilitiesoutdoors. The analyzer employs the principle ofphotoionization for detection. This process is termedphotoionization because the absorption of ultraviolet light (aphoton) by a molecule leads to ionization via:

RH + hv RH+ + e

where RH = trace gashv = a photon with an energy greater than or

equal to an ionization potential of RH.

The sensor consists of a sealed ultraviolet light source thatemits photons which are energetic enough to ionize many tracespecies (particularly organics), but do not ionize the majorcomponents of air such as 02/ N2, CO, CO2 or H2O. A chamberadjacent to the ultraviolet light source contains a pair ofelectrodes. When a positive potential is applied to oneelectrode, the field created drives any ions, formed byabsorption of UV light, to the collector electrode where thecurrent (proportional to concentration) is measured. Theuseful range of the instrument is from a fraction of a ppm toabout 2,000 ppm.

2.0 Instrument Sensitivity and Calibration

The instrument responds to atmospheric compounds withionization potentials equal to or less than the ionizationenergy of the UV light source. If a compound in air has anionization potential greater than the energy source of thelamp, it will not be detected. Table 1 presents organic andinorganic compounds and the light sources that should be usedto detect each compound. The instrument is capable of using 1of the 3 light sources - 9.5, 10.2, and 11.7 ev lamps. Inaddition, not all compounds respond equally to each lightsources and thus they vary in their sensitivity to ionization.As a result of varying sensitivities to photoionization, theresponse given by the instrument may or may not reflect theactual atmospheric concentration of the compound beingdetected. Table 2 represents the relative sensitivities forvarious gases relative to a 10.2 ev light source. Use thistable to determine the approximate response of the instrument

" to a compound of interest, and to select the appropriate lighti (lamp) source.

There are two types of operations that are used fort calibration. For Type 1 Operation, a non-regulatory (or non-

target) compound such as isobutylene is used for calibration.r In this case, the instrument reading is reported in terms

relative to the calibration compound used for calibration.'• For the type 2 operation, the target compound or compounds are

used for calibration. As a result, the instrument isr calibrated to respond directly in ppm by volume of the target». compound (s) .

r 3.0 Instrument Specifications

~" 3.1 Performance

o Range: 0.1 to 2000 ppm

o Detection Limit: 0.1 ppmr

o Sensitivity (max.): 0 to 2 ppm FSD over 100division meter scale

r

, o Repeatability: ± 1% of FSD

o Linear Range: 0.1 to 600 ppm

* o Useful Range: 0.1 to 2000 ppm

7 o Response Time: less than 3 seconds to reachi 90% full scale

-r o Ambient humidity: up to 95% relative humidity

' o Operating Temperature: Ambient to 40"C„ (instrument is temperature compensated so that

a 20'C change in temperature corresponds to a*• change in reading of + 2% full scale at maximum

sensitivity.

k 3.2 Power Requirements and Operating Times

* o Continuous use on battery: approximately 10 hoursk o Continuous use with HNu recorder reduces instrument

battery operating time to approximately 5 hours

* o Recharge time: less than 14 hours; a 3 hours chargewill charge up to 90% full charge

L o Recharge Current: maximum 0.4 amps at 15 VDC

i II. OPERATIONAL PROCEDURE

{IT

t 1.0 Instrument Check-Out

r 1.1 Remove instrument box cover by pulling up onk fasteners.

, 1.2 On the instrument panel, there will be a label containing

L information on light source, calibration date,calibration gas, and span setting.

1.2.1 If the instrument has not been calibratedin the last 14 days or since its last fielduse, it should be recalibrated. Check the

r instrument log, which should be maintained withthe instrument, for the instrument status andits calibration history. For general use, the

.. instrument should be calibrated to isobutylene* at a span setting of 9.8.

1.2.2 Check the label for light source and refer toTable 1 for ionization potentials of variouscompounds. If the compound you wish to detect isnot listed for the light sources provided withinstrument, then the light source will have to bechanged. Use the probe with the proper lightsource for the compounds to be detected.

1.2.3 Once it has been determined that the instrumenthas the correct lamp, the instrument may need tobe recalibrated for the specific compound ofinterest. Use Procedure under 2.1.3 of thisSection to calibrate the instrument.

III

1.2.4 check the battery supply by connecting the probeto the instrument box, and turning the functionswitch to the battery check position (Figure l).

. (Note: The battery check indicator will notF function unless the probe is attached.) The meter*• needle should deflect to the far right or above

the green zone. If the needle is below or justf within the green zone or the red LED indicator isk on, the battery should be recharged. Follow the

procedure described in Section III (Maintenanceand Trouble shooting) to recharge the battery.

1.2.5 Repack the instrument for shipment to the field.

2.0 Field Operation

2.1 Ca1ibration

2.1.1 Equipment and Materials

o Calibration Gas (2 ranges)

Low range 0-20 ppm and mid-range 20-200 ppm ofisobutylene gas are used for standard fieldoperation when contaminants are unknown or amixture of gases is present. The isobutylenegas is used for general calibration because ofthe instrument's relatively high sensitivityto it and the non-toxic nature of the gas.Note: A specialty gas may be required if asingle atmospheric contaminant is present andthe contaminant has a sensitivity differentfrom that of the calibration gas(isobutylene) .

o Tubing and fittings (see Figure 1) .

o Rotometer or bubble flow meter.

o Field Log, calibration form, and datareporting form.

o Table 1 for ionization potentials forcompounds of interest.

2.1.2 Calibration Frequency

This instrument should be calibrated after eachfield use and prior to each field use.Continuous calibration check should beperformed frequently during field operation(for example, check the instrument zero andcalibration after every 10 measurements) anddocument the results properly. Caution ; DoNot Change the Settings.

2.1.3 Calibration Procedure

2.1.3.1 Use a three-points procedure tofacilitate the proper instrumentcalibration over appropriateoperating ranges. Distinct mixturesof calibration gas with knownconcentration for selective operatingrange should be used for calibration.Each mixture should give a 3/4 scaledeflection in its respectiveoperating range.

2.1.3.2 Instrument Setup.

r

r

r

iii

t

LL

Step 1: Remove Instrument cover by pulling upon the side straps.

Step 2: Prior to calibration, check thefunction switch (Figure 2) on thecontrol panel to make sure it is inthe OFF position. The probe nozzleis stored inside the instrumentcover. Remove cover plate by pullingup on the pins that fasten the coverplate.

Step 3: Remove the nozzle from the cover.Assemble probe by screwing nozzleinto casing.

Step 4: Attach probe cable to instrument boxinserting 12 pin interface connectorof the probe cable into the connectoron the instrument panel. Match thealignment keys and insert connector.Turn connector in clockwise directionuntil a distinct snap and lock isfelt.

Step 5: Turn the function switch to theBattery Check position. When thebattery is charged, the needle shouldread within or above the greenbattery arc on the scale plate. Ifthe needle is below the green arc orthe red LED light comes on, theinstrument should be recharged priorto making any measurements.Implement steps in Section III torecharge battery.

Step 6: Turn the function switch to the ONposition. In this position, the UVlight source should be on. Toverify, gaze at the end of the probefor a purple glow. Do Not LookDirectly at the Lamp Itself. If thelamp does not come on refer toMaintenance Step in 2.2 (SectionIII) .

Step 7: To zero the instrument, turn thefunction switch to the standbyposition and rotate the zeropotentiometer until the meter readszero. Clockwise rotation of the zeropotentiometer produces an upscaledeflection while counter clockwise

L

rotation yields a downscaledeflection. (Note: No zero gas isneeded since this is an electroniczero adjustment.) If the spanadjustment is changed duringinstrument calibration, the zeroshould be rechecked and adjusted. Ifnecessary, wait 15 to 20 seconds toensure that the zero reading isstable. Readjust as necessary.

2.1.3.3 Calibration Steps

Step 1: Insert one end of T tube (Figure 1)into probe. Insert second end ofprobe into calibration gas in the 20-200 ppm range. The third end ofprobe should have the rotometer(bubble meter) attached.

Step 2: Set the function switch in the 0-200ppm range. Crack the valve on thepressured calibration gas containeruntil a slight flow is indicated onthe rotometer. The instrument willdraw in the volume required fordetection with the rotometerindicating excess flow.

Step 3: Adjust the span potentiometer so thatthe instrument is reading the exactvalue of the calibration gas.(Calibration gas value is labeled onthe cylinder).

Step 4: Turn instrument switch to the standbyposition and check the electroniczero. Reset zero potentiometer asnecessary following step 7 of2.1.3.2.

Step 5: Record on form and field log alloriginal and readjusted settings asspecified in the form.

^ Step 6: Next, set the function switch to the0-20 ppm. Remove the mid-range (20-200 ppm) calibration gas cylinder andattach the low range (0-20 ppm)calibration gas cylinder as describedabove.

Step 7: Do not adjust the span potentiometer.The observed reading should be ±2 ppm

I

rrr

rr

of the concentration specified forthe low range calibration gas. ifthis is not the case, recalibrate themid range scale repeating Step l thru6 above. If the low range readingconsistently falls outside therecommended tolerance range, theprobe light source window likelyneeds cleaning. Clean windowfollowing Step 2 under 2.3 (SectionIII). When the observed reading iswithin the required tolerances, theinstrument is fully calibrated.

2.2 Sample Measurement

EE

L

II

Step 1: Place function switch in 0-20 ppmrange for field monitoring. Thiswill allow for the most sensitive,quick response in detecting airbornecontaminants.

Step 2: Before entering a contaminated area,determine background concentration.This concentration should be used asa reference to readings made in thecontaminated area. Under nocircumstance should one attempt toadjust the zero or span adjustmentswhile the instrument is beingoperated in the field.

Step 3: Take measurements in contaminatedarea, recording readings andlocations. Should readings exceedthe 0-20 scale, switch the functionswitch to the 0-200 or 0-2,000 rangeas appropriate to receive a directreading. Return the instrumentswitch to the 0-20 range whenreadings are reduced to that level.Record measurements in notebook or onan appropriate form.

Step 4: Keep in mind health and safety actionguidelines for the level ofprotection you are wearing.Sustained readings above a certainlevel may force you to vacate an areaor upgrade your level of protection.

Note; The instrument will not functionproperly in high humidity or when thewindow to the light housing is dirty. If

rr

rr

ii

t

the instrument response is erratic orlower than expected.

Step 5: When finished, use the reverse Steps1 thru 5 of Section 2.1.3.2(Instrument Setup) to shut down theinstrument.

III. MAINTENANCE AND TROUBLE-SHOOTING

1.0 Battery Recharging

1.1 The instrument should be recharged 1 hour for each hourof use or overnight for a full day's use. (The batterywill last 10 hours on a full charge.)

1.2 To recharge the battery (or instrument):

1.2.1 Turn the function switch to the off position.

1.2.2 Remove the charger from the instrument topcompartment.

1.2.3 Place the charger plug into the jack on the leftside of the instrument box.

1.2.4 Connect the charger unit to a 120 V AC supply.

1.2.5 Check charger function by turning the instrumentswitch to the battery check position. The metershould go upscale if the charger is working and iscorrectly inserted into the jack.

1.2.6 Place instrument in instrument mode and charge forthe appropriate time period.

1.2.7 Turn the instrument off following the rechargecycle. When disconnecting charger, remove from120 V AC supply before removing the mini phoneplug.

2.0 General Fault Determination and Correction

2.1 Battery level is low. Recharge if necessary implementingsteps described under 1.0 (Section III). If the batterywill not recharge, it will have to be replaced.

2.2 UV Lamp function - Gaze at sample inlet when mode switchis on an instrument function position and observe forpurple glow of lamp. If the lamp does not glow in any ofthe three instrument function positions, it may be burnedout and will have to be replaced. To replace the lamp:

rrr

r

E

IIL

1. Turn the function switch to the off position anddisconnect the probe connector from the readoutunit.

2. Remove the exhaust screw found near the base of theprobe (Figure 3).

3. Grasp the end cap in one hand and the probe shell inthe other and gently pull to separate the end capand lamp housing from the shell.

4. Loosen the screws on the top of the end cap andseparate the end cap and ion chamber from the lampand lamp housing. Care must be taken so that theion chamber does not fall out of the end cap and thelamp does not slide out of the lamp housing.

5. Turn the end cap over in your hand and tap on thetop of it; the ion chamber should fall out of it.

6. Place one hand over the top of the lamp housing andtilt slightly. The light source will slide out ofthe housing.

7. Replace lamp with one of same energy source as theone removed by sliding it into the housing. Note:The amplifier board and instrument circuitry arecalibrated for one light energy.

8. Place the ion chamber on top of the lamp housing,checking to ensure that the contacts are aligned.

9. Place the end cap on top of the ion chamber andreplace the two screws. The screws should betightened only enough to seal the "0" ring. Do notovertighten.

10. Line up the pins on the base of the lamp housingwith the pins inside the probe shell. Gently slidethe housing assembly into the probe shell. Do notforce the assembly as it only fits one way.

11. Replace and tighten the exhaust screw.

12. Reconnect the 12 pin connector and turn instrumentmode switch to a function position. Check for glowof lamp. If lamp still does not function, theinstrument has an electrical short or other problemthat will have to be corrected at the factory.

2.3 Instrument appears to be functional, but responses arelower than expected or erratic. The window of the lightsource may be dirty and need to be cleaned. To clean thelight source window:

1. Disassemble the probe assembly by repeating Steps lthru 6 under 2.2 above.

2. Clean the window of the light source using compoundprovided with instrument and soft clean cloth.Important: Use cleaning compound on the window ofthe 10.2 eV lamp only. The cleaning compound maydamage the windows of the 9.5 and 11.7 eV lamps.

3. Reassemble the probe assembly repeating Step 7through 12 above.

r 3.0 Specific Faults

* 3.1 No meter response in any switch position (including BATTCHK)

-* 1. Broken meter movement: Tip instrument rapidly fromside to side. Meter needle should move freely, and

' return to zero.

2. Electrical connection to meter is broken: Check all• wires leading to meter and clean the contacts ofj quick-disconnects.

. 3. Battery is completely dead: Disconnect battery andj check voltage with a volt-ohm meter.L

4. Check 2 amp fuse.-y

t, 5. If none of the above solves the problem, consult thefactory.

T

3.2 Meter responds in BATT CHK position, but reads zero ornear zero for all others.

1. Power supply defective: Check power supply voltagesk per Figure 4. If any voltage is out of

specification, consult the factory.T

k 2. Input transistor or amplifier has failed: Rotatezero control; meter should deflect up/down as

* control is turned. Open probe; both transistors-, should be fully seated in sockets.

r 3. Input signal connection broken in probe or readout:' Check input connector on printed circuit board.* Should be firmly pressed down. Check components on

back side of printed circuit board. All connections* should be solid, and no wires should touch any other,. object. Check all wires in readout for solid

connections.

f 3.3 Instrument responds correctly in BATT CHK, and STBY, butI. not in measuring mode.

r 1. Check to see the light source is on (See Sectionj 2.2).

2. Check high voltage power supply (See Figure 4).

'• 3. Open end of probe, remove lamp and check highvoltage on lamp contact ring.

4. If high voltage is present at all above points,light source has most likely failed. Consult thefactory.

*" 3.4 Instrument responds correctly in all positions, butsignal is lower than expected.

«- 1. Check span setting for correct value.

P 2. Clean window of light source (See 2.3).

3. Double check preparation of standards.

4. Check power supply 180 V output. See Figure 4.

5. Check for proper fan operation. Check fan voltage.A See Figure 4.

6. Rotate span setting. Response should change if spanI? pot is working properly.

3.5 Instrument responds in all switch positions, but is noisyp (erratic meter movement).

1. Open circuit in feedback circuit. Consult thefactory.

it 2. Open circuit in cable shield or probe shield.Consult the factory.

I 3.6 Instrument response is slow and/or irreproducible.

«• 1. Fan operating improperly. Check fan voltage. SeeI Figure 4.

2. Check calibration and operation.

L 3.7 Low battery indicator.

r 1. Indicator comes on.if battery charge is low.

2. Indicator also comes on if ionization voltage is too, high.

APPENDIX K

FIELD MEASUREMENT OF HYDRAULIC CONDUCTIVITY SLUG TEST

REVISION: 2

FIELD MEASUREMENT OF HYDRAULIC CONDUCTIVITYSLUG TEST

INTRODUCTION

The objective is to determine hydraulic parameters (transm1ss1v1ty,storativlty, hydraulic conductivity) of the water-bearing strata. Single wellaquifer tests are used because they may be conducted using a minimum ofequipment, personnel, and time. They may also be done at many points withinan aquifer and may be used to better plan a full-scale pumping test.

PROCEDURES

Each slug test is conducted by measuring the static water level with anelectric water level Indicator or fiberglass tape with attached soundingdevice, placing a pressure transducer (connected to a Hermit data logger*),below the water level, and Introducing a solid slug Into the well. Therecovery of the water level back to the static level is recorded over thenecessary period of time, using a logarltmic sampling mode on the data logger.

The electric water level tape and transducer are wiped, first with methanoland then with deionlzed water as they are placed in the wells, to preventcross-contamination between wells. The solid slug 1s lowered with an attached1/8-Inch stainless steel cable. The solid slug and cable are decontaminatedbetween uses by washing and rinsing with Llquinox soap and water, rinsingthree times with methanol, and rinsing three times with deionlzed water. Thesolid slug and cable are then allowed to air-dry on steel supports and arecovered with new sheet plastic.

DATA REDUCTION

The data accumulated during the slug tests are used to calculate hydraulicparameters using several published methods. Hydraulic conductivity 1scalculated for shallow, unconflned wells using the Bouwer and R1ce method(1976). The NAVFAC method (1971) 1s used for comparison. Transm1ss1v1t1esand storat1v1t1es for confined wells are determined using the curve matchingmethod described by Cooper, et al. (1967). For comparison, hydraulicconductivities are also calculated using the Hvorslev method (1951). Methodsassume an Infinite, homogenous, 1 so tropic aquifer and an Instantaneous change1n head 1n the well.

The method described by Bouwer and Rice (1976) is based upon modifications tothe Thiem equation, with the use of an analog model. A straight line 1s drawnthrough a semi-log plot of relative head versus time, and the hydraulicconductivity is calculated using the slope of that line and the geometry ofthe well and aquifer. The formulation assumes that draw-down of the watertable around the well 1s negligible, that flow 1n the capillary fringe may beIgnored, and that well losses are negligible. It 1s applicable to completelyor partially penetrating wells 1n unconflned aquifers, but may be used forconfined aquifers that receive water from the upper confining layer.

Environmental Data Logger, Model SE1000B,In-S1tu, Inc., Laramle, Wyoming 82070

-2-

In the NAVFAC method (1971), a straight line 1s also drawn through a semi-logplot of recovery data for unconflned aquifers. The method 1s based on theHvorslev method. It assumes that the well 1s cased below the water table, andthe ratio of the screen length to the well radius (L/R) 1s greater than eight.

The Cooper, et al. (1967) formulation calculates the transm1ss1v1ty of anaquifer by matching a plot of relative head (linear scale) versus time(logarithmic scale) to one of a set of type curves. The method assumes thatthe change 1n head after a known volume of water 1s Injected or removed 1sInstantaneous and that the (non-flowing) well 1s screened over the entirethickness of an arteslon aquifer. It 1s directly applicable to fullypenetrating screened wells 1n confined aquifers, but may be used to determinethe transm1ss1v1ty of the portion of an aquifer over which a partiallypenetrating well is screened, assuming no vertical flow occurs.

The Hvorslev method (1951) 1s based on a solution of the LaPlace equation anddoes not account for aquifer storage. A straight line Is drawn through asemi-log plot of relative head versus time. The time that would be requiredfor complete equalization of head difference 1f the original rate of Inflowwere maintained (defined as the basic time lag, T0, and equal to the time whenH-h/H-Ho = 0.37) 1s used to calculate the hydraulic conductivity. The valueof T0 1s measured graphically, and the ratio of the piezometer length toradius 1s assumed to be greater than eight (L/R>8).

RCW/sss/AJS[sss-600-20c]^Hermit Environmental Data Logger, Model SE1000B,In-S1tu, Inc., Laramle, Wyoming 82070

REFERENCES CITED

Bouwer, H. and R1ce, R.C., 1976, A Slug Test for Determining HydraulicConductivity of Unconflned Aquifers with Completely or PartiallyPenetrating Wells. Water Resources Research, Vol. 12, No. 3, p. 423-428.

Cooper, H.H., Jr., J.D. Bredehoeft, and I.S. Papadopulos, 1967, Response of aFinite Diameter Well to an Instantaneous Charge of Water, Water ResourcesResearch 3, p. 263-269.

Hvorslev, M.J., 1951, Time Lag and Soil Permeability 1n GroundwaterObservations, U.S. Army Corps of Engineers, Waterways Exp. Sta. Bull 36,Vlcksburg, MS.

Papadopulos, S.S., Bredehoeft, J.D., and Cooper, H.H., Jr., 1973, On theAnalysis of 'Slug Test1 Data. Water Resources Research, Vol. 9, No. 4.,P. 1087-1089.

United States Department of the Navy, Design Manual: Soil Mechanics,Foundations, and Earth Structures, NAVFAC DM-F, March 1971, p. 7-4-9.

RCW/sss/AJS[sss-600-20d]

r

WARZYN

MADISONMILWAUKEEMINNEAPOLISCHICAGODETROIT