analytical report for samples received … · analytical report job number: 480-111215-1 job...

ANALYTICAL REPORT

Job Number: 480-111215-1

Job Description: W.R. Grace, Acton

For:Tetra Tech GEO

W.R. Grace45610 Woodland Road

Suite 400Sterling, VA 20166

Attention: Ms. Anne Sheehan

_____________________________________________

Approved for release.Lisa E ShafferProject Manager II12/23/2016 12:59 PM

Designee forBecky C Mason, Project Manager II

10 Hazelwood Drive, Amherst, NY, 14228-2298(413)572-4000

[email protected]/23/2016

cc: Grady Dante

The test results in this report meet all NELAP requirements for analytes for which accreditation is required or available.Any exceptions to the NELAP requirements are noted in this report. Pursuant to NELAP, this report may not bereproduced, except in full, without the written approval of the laboratory. All questions regarding this test report shouldbe directed to the TestAmerica Project Manager who has signed this report.

TestAmerica Buffalo NELAC Certifications: CADPH 01169CA, FLDOH E87672, ILEPA 200003, KSDOH E-10187,LADEQ 30708, MDH 036-999-337, NHELAP 2973, NJDEP NY455, NHDOH 10026, ORELAP NY200003, PADEP 68-00281, TXCEQ T-104704412-10-1

TestAmerica Laboratories, Inc.

TestAmerica Buffalo 10 Hazelwood Drive, Amherst, NY 14228-2298

Tel (716) 691-2600 Fax (716) 691-7991 www.testamericainc.com

Page 1 of 116

TestAmerica THE LEADER IN ENVIRONMENTAL TESTING

mailto:[email protected]://www.testamericainc.comhttp://

Table of ContentsCover Title Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

Data Summaries . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4

Report Narrative . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4

Manual Integration Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

Sample Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

Executive Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8

Method Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

Method / Analyst Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

Sample Datasheets . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

Surrogate Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16

QC Data Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

Data Qualifiers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19

QC Association Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

Lab Chronicle . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

Certification Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

Organic Sample Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

GC/MS Semi VOA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

Method 522 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24Method 522 QC Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25Method 522 Sample Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32Standards Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52

Method 522 ICAL Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52Method 522 CCAL Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70

Raw QC Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88Method 522 Tune Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88Method 522 Blank Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91

Page 2 of 116

Table of ContentsMethod 522 LCS/LCSD Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 94Method 522 MS/MSD Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97

Method 522 Run Logs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106Method 522 Prep Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 111

Subcontracted Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 112

Shipping and Receiving Documents . . . . . . . . . . . . . . . . . . . . . . . . . . . 113

Client Chain of Custody . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 114

Sample Receipt Checklist . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115

Page 3 of 116

Job Narrative480-111215-1

CommentsNo additional comments.

Receipt The samples were received on 12/16/2016 10:00 AM; the samples arrived in good condition, properly preserved and, where required, on ice. The temperature of the cooler at receipt was 2.0 C.

GC/MS Semi VOA No analytical or quality issues were noted, other than those described in the Definitions/Glossary page.

Organic Prep No analytical or quality issues were noted, other than those described in the Definitions/Glossary page.

Page 4 of 116

Lab Name: Job No.:

SDG No.:

GC/MS SEMI VOA MANUAL INTEGRATION SUMMARY

TestAmerica Burlington 480-111215-1

Instrument ID: Analysis Batch Number:CHZ.i 112452

Lab Sample ID: Client Sample ID:

Date Analyzed: Lab File ID:

COMPOUND NAME RETENTIONTIME

MANUAL INTEGRATIONDATEANALYSTREASON

IC 200-112452/5

Z23129_05.D12/15/16 11:14 GC Column: Rxi-5ms ID: 0.25(mm)

Tetrahydrofuran-d8 Baseline snellingn 12/15/16 14:113.37





ICIS 200-112452/6


Tetrahydrofuran-d8 Baseline snellingn 12/15/16 14:113.37

522

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I

I

I I I

I I I I

I

I

I I I

I I I I

Lab Name: Job No.:

SDG No.:

GC/MS SEMI VOA MANUAL INTEGRATION SUMMARY


Instrument ID: Analysis Batch Number:CHZ.i 112677





480-111215-4 MS


Tetrahydrofuran-d8 Peak Tail bagcilars 12/22/16 14:533.441,4-Dioxane-d8 (Surr) Baseline bagcilars 12/22/16 14:534.331,4-Dioxane Peak Tail bagcilars 12/22/16 14:534.37

522

Page 6 of 116

SAMPLE SUMMARY

Client: Tetra Tech GEO Job Number: 480-111215-1

Client Sample IDLab Sample ID Client Matrix Sampled ReceivedDate/Time Date/Time

480-111215-1 ASSABET-1A Water 12/15/2016 1435 12/16/2016 1000

480-111215-2 ASSABET-2A Water 12/15/2016 1440 12/16/2016 1000

480-111215-3 CHRISTOFFERSON Water 12/15/2016 1455 12/16/2016 1000

480-111215-4 SCRIBNER Water 12/15/2016 1520 12/16/2016 1000

480-111215-4MS SCRIBNER Water 12/15/2016 1520 12/16/2016 1000

480-111215-4MSD SCRIBNER Water 12/15/2016 1520 12/16/2016 1000

480-111215-5 SCRIBNER-DUP Water 12/15/2016 1522 12/16/2016 1000

TestAmerica Buffalo Page 7 of 116

EXECUTIVE SUMMARY - Detections


Analyte ResultReporting Limit Units Method

Lab Sample ID Client Sample IDQualifier

480-111215-1 ASSABET-1A

0.20 ug/L 5221.01,4-Dioxane

480-111215-2 ASSABET-2A

0.20 ug/L 5220.411,4-Dioxane

480-111215-3 CHRISTOFFERSON

0.20 ug/L 5220.281,4-Dioxane

480-111215-4 SCRIBNER

0.20 ug/L 5220.341,4-Dioxane

480-111215-5 SCRIBNER-DUP

0.20 ug/L 5220.321,4-Dioxane


METHOD SUMMARY


Preparation MethodMethodLab LocationDescription

Matrix: Water

1,4 Dioxane (GC/MS SIM) TAL BUR EPA 522

Solid Phase Extraction (SPE) TAL BUR SW846 3535A

Lab References:

TAL BUR = TestAmerica Burlington

Method References:

EPA = US Environmental Protection Agency

SW846 = "Test Methods For Evaluating Solid Waste, Physical/Chemical Methods", Third Edition, November 1986 And Its Updates.


METHOD / ANALYST SUMMARY


Method Analyst Analyst ID

Bagcilar, Seren H SHBEPA 522

TestAmerica Buffalo

Page 10 of 116

Analytical Data


Client Sample ID:

Lab Sample ID:

ASSABET-1A

Client Matrix:

480-111215-1

Water

Date Sampled: 12/15/2016 1435

Date Received: 12/16/2016 1000

522 1,4 Dioxane (GC/MS SIM)

Dilution:

12/20/2016 1941

12/21/2016 2311

1.0

522

Injection Volume:

Final Weight/Volume:

Initial Weight/Volume:

Lab File ID:

Instrument ID:

Z23206_41.D

100 mL

2000 uL

2 uL

3535A

CHZ.i

Analysis Date:

Prep Date:

Analysis Batch:

Prep Batch:

200-112622

200-112608

Analysis Method:

Prep Method:

Analyte Result (ug/L) Qualifier MDL RL

1.0 0.200.0571,4-Dioxane

Surrogate %Rec Acceptance LimitsQualifier

85 70 - 1301,4-Dioxane-d8 (Surr)


Analytical Data


Client Sample ID:

Lab Sample ID:

ASSABET-2A

Client Matrix:

480-111215-2

Water

Date Sampled: 12/15/2016 1440



Dilution:

12/20/2016 1941

12/21/2016 2330

1.0

522

Injection Volume:



Lab File ID:

Instrument ID:

Z23206_42.D

100 mL

2000 uL

2 uL

3535A

CHZ.i

Analysis Date:

Prep Date:

Analysis Batch:

Prep Batch:

200-112622

200-112608

Analysis Method:

Prep Method:


0.41 0.200.0571,4-Dioxane


83 70 - 1301,4-Dioxane-d8 (Surr)


Analytical Data


Client Sample ID:

Lab Sample ID:

CHRISTOFFERSON

Client Matrix:

480-111215-3

Water

Date Sampled: 12/15/2016 1455



Dilution:

12/20/2016 1941

12/21/2016 2349

1.0

522

Injection Volume:



Lab File ID:

Instrument ID:

Z23206_43.D

100 mL

2000 uL

2 uL

3535A

CHZ.i

Analysis Date:

Prep Date:

Analysis Batch:

Prep Batch:

200-112622

200-112608

Analysis Method:

Prep Method:


0.28 0.200.0571,4-Dioxane


84 70 - 1301,4-Dioxane-d8 (Surr)


Analytical Data


Client Sample ID:

Lab Sample ID:

SCRIBNER

Client Matrix:

480-111215-4

Water

Date Sampled: 12/15/2016 1520



Dilution:

12/20/2016 1941

12/22/2016 1305

1.0

522

Injection Volume:



Lab File ID:

Instrument ID:

Z23228_07.D

100 mL

2000 uL

2 uL

3535A

CHZ.i

Analysis Date:

Prep Date:

Analysis Batch:

Prep Batch:

200-112677

200-112608

Analysis Method:

Prep Method:


0.34 0.200.0571,4-Dioxane


80 70 - 1301,4-Dioxane-d8 (Surr)


Analytical Data


Client Sample ID:

Lab Sample ID:

SCRIBNER-DUP

Client Matrix:

480-111215-5

Water

Date Sampled: 12/15/2016 1522



Dilution:

12/20/2016 1941

12/22/2016 1403

1.0

522

Injection Volume:



Lab File ID:

Instrument ID:

Z23228_10.D

100 mL

2000 uL

2 uL

3535A

CHZ.i

Analysis Date:

Prep Date:

Analysis Batch:

Prep Batch:

200-112677

200-112608

Analysis Method:

Prep Method:


0.32 0.200.0571,4-Dioxane


81 70 - 1301,4-Dioxane-d8 (Surr)


Quality Control Results

Job Number: 480-111215-1Client: Tetra Tech GEO

Surrogate Recovery Report


Client Matrix: Water

Lab Sample ID Client Sample ID

DXE

%Rec

480-111215-1 ASSABET-1A 85

480-111215-2 ASSABET-2A 83

480-111215-3 CHRISTOFFERSON 84

480-111215-4 SCRIBNER 80

480-111215-5 SCRIBNER-DUP 81

MB 200-112608/1-A 81

LCS 200-112608/2-A 83

480-111215-4 MS SCRIBNER MS 70

480-111215-4 MSD SCRIBNER MSD 71

Surrogate Acceptance Limits

DXE = 1,4-Dioxane-d8 (Surr) 70-130

TestAmerica Buffalo

Page 16 of 116



WaterClient Matrix:

1.0Dilution:

Lab Sample ID:

Method Blank - Batch: 200-112608

Instrument ID:

Lab File ID:



Z23206_34.D

100 mL

2000 uLUnits: ug/L

Method: 522Preparation: 3535A

CHZ.iMB 200-112608/1-A

Analysis Date: 12/21/2016 2055

Analysis Batch:

Prep Batch:

Leach Batch: N/A

200-112622

200-112608

Prep Date: Injection Volume: 2 uL

Leach Date:

12/20/2016 1941

N/A

Analyte RLMDLQualResult

ND 0.200.0571,4-Dioxane

Surrogate % Rec Acceptance Limits

1,4-Dioxane-d8 (Surr) 81 70 - 130

Water

1.0

Lab Control Sample - Batch: 200-112608

Client Matrix:

Lab Sample ID:

Dilution:

Instrument ID:

Lab File ID:



Z23206_33.D

100 mL

2000 uLUnits: ug/L


CHZ.iLCS 200-112608/2-A

Analysis Date: 12/21/2016 2035

Analysis Batch:

Prep Batch:

Leach Batch:

200-112622

200-112608

N/A

Prep Date: Injection Volume: 2 uL

Leach Date:

12/20/2016 1941

N/A

Analyte QualLimit% Rec.ResultSpike Amount

0.200 0.192 96 J70 - 1301,4-Dioxane

Surrogate % Rec Acceptance Limits

1,4-Dioxane-d8 (Surr) 83 70 - 130




Dilution:

Dilution:

Water

1.0

1.0

Client Matrix:

Instrument ID:

Lab File ID:



Injection Volume:

Instrument ID:

Lab File ID:



Injection Volume:

Client Matrix: Water

Z23228_08.D

100 mL

2000 uL

2 uL

Z23228_09.D

100 mL

2000 uL

2 uL


CHZ.i

CHZ.i

480-111215-4

480-111215-4

MS Lab Sample ID:

MSD Lab Sample ID:

Matrix Spike/Matrix Spike Duplicate Recovery Report - Batch: 200-112608

12/22/2016 1325

N/A

Analysis Date:

Prep Date:

Leach Date:

Analysis Batch:

Prep Batch:

Leach Batch:

200-112677

200-112608

N/A

Analysis Date:

Prep Date:

Leach Date:

12/22/2016 1344

12/20/2016 1941

N/A

Analysis Batch:

Prep Batch:

Leach Batch:

200-112677

200-112608

N/A

12/20/2016 1941

Analyte RPD LimitRPDLimit

% Rec.

MS MSD MS Qual MSD Qual

73 73 70 - 130 0 301,4-Dioxane

Surrogate Acceptance LimitsMS % Rec MSD % Rec

1,4-Dioxane-d8 (Surr) 70 71 70 - 130

Water

12/22/2016 1325 12/22/2016 1344

Dilution: Dilution:1.0 1.0

Client Matrix: Client Matrix: Water


Units: ug/L480-111215-4 480-111215-4MS Lab Sample ID: MSD Lab Sample ID:

Matrix Spike/Matrix Spike Duplicate Recovery Report - Batch: 200-112608

Analysis Date:

Prep Date:

Leach Date:

12/20/2016 1941

N/A

Analysis Date:

Prep Date:

Leach Date:

12/20/2016 1941

N/A

Amount

Sample

Analyte Result/Qual Amount Result/Qual Result/Qual

MS MSDMS Spike MSD Spike

0.34 2.00 2.00 1.80 1.791,4-Dioxane


DATA REPORTING QUALIFIERS


Lab Section Qualifier Description

GC/MS Semi VOA

Result is less than the RL but greater than or equal to the MDL and the concentration is an approximate value.

J




QC Association Summary

Lab Sample ID Client Sample ID Client Matrix Method Prep Batch

ReportBasis

GC/MS Semi VOA

Prep Batch: 200-112608Lab Control Sample Water 3535ALCS 200-112608/2-A TMethod Blank Water 3535AMB 200-112608/1-A T

WaterASSABET-1A 3535A480-111215-1 TWaterASSABET-2A 3535A480-111215-2 TWaterCHRISTOFFERSON 3535A480-111215-3 TWaterSCRIBNER 3535A480-111215-4 T

Matrix Spike Water 3535A480-111215-4MS TMatrix Spike Duplicate Water 3535A480-111215-4MSD T

WaterSCRIBNER-DUP 3535A480-111215-5 T

Analysis Batch:200-112622Lab Control Sample Water 200-112608522LCS 200-112608/2-A TMethod Blank Water 200-112608522MB 200-112608/1-A T

Water 200-112608ASSABET-1A 522480-111215-1 TWater 200-112608ASSABET-2A 522480-111215-2 TWater 200-112608CHRISTOFFERSON 522480-111215-3 T

Analysis Batch:200-112677Water 200-112608SCRIBNER 522480-111215-4 T

Matrix Spike Water 200-112608522480-111215-4MS TMatrix Spike Duplicate Water 200-112608522480-111215-4MSD T

Water 200-112608SCRIBNER-DUP 522480-111215-5 T

Report Basis

T = Total

TestAmerica Buffalo

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Laboratory Chronicle

12/16/2016 10:00

Lab ID:

Method Bottle ID Run

Analysis Batch Prep Batch

Date Prepared / Analyzed Dil Lab Analyst

Client ID:

Sample Date/Time: Received Date/Time:12/15/2016 14:35

480-111215-1 ASSABET-1A

P:3535A 480-111215-A-1-A 200-112622 200-112608 12/20/2016 19:41 RCKTAL BUR1

A:522 480-111215-A-1-A 200-112622 200-112608 12/21/2016 23:11 SHBTAL BUR1

12/16/2016 10:00

Lab ID:




Client ID:


480-111215-2 ASSABET-2A

P:3535A 480-111215-A-2-A 200-112622 200-112608 12/20/2016 19:41 RCKTAL BUR1

A:522 480-111215-A-2-A 200-112622 200-112608 12/21/2016 23:30 SHBTAL BUR1

12/16/2016 10:00

Lab ID:




Client ID:


480-111215-3 CHRISTOFFERSON

P:3535A 480-111215-A-3-A 200-112622 200-112608 12/20/2016 19:41 RCKTAL BUR1

A:522 480-111215-A-3-A 200-112622 200-112608 12/21/2016 23:49 SHBTAL BUR1

12/16/2016 10:00

Lab ID:




Client ID:


480-111215-4 SCRIBNER

P:3535A 480-111215-A-4-A 200-112677 200-112608 12/20/2016 19:41 RCKTAL BUR1

A:522 480-111215-A-4-A 200-112677 200-112608 12/22/2016 13:05 SHBTAL BUR1

12/16/2016 10:00

Lab ID:




Client ID:


480-111215-4 SCRIBNER

P:3535A 480-111215-A-4-B MS

200-112677 200-112608 12/20/2016 19:41 RCKTAL BUR1

A:522 480-111215-A-4-B MS

200-112677 200-112608 12/22/2016 13:25 SHBTAL BUR1

A = Analytical Method P = Prep Method TestAmerica Buffalo

Page 21 of 116



Laboratory Chronicle

12/16/2016 10:00

Lab ID:




Client ID:


480-111215-4 SCRIBNER

P:3535A 480-111215-A-4-C MSD

200-112677 200-112608 12/20/2016 19:41 RCKTAL BUR1

A:522 480-111215-A-4-C MSD

200-112677 200-112608 12/22/2016 13:44 SHBTAL BUR1

12/16/2016 10:00

Lab ID:




Client ID:


480-111215-5 SCRIBNER-DUP

P:3535A 480-111215-A-5-A 200-112677 200-112608 12/20/2016 19:41 RCKTAL BUR1

A:522 480-111215-A-5-A 200-112677 200-112608 12/22/2016 14:03 SHBTAL BUR1

Lab ID:




Client ID:

Sample Date/Time: N/A Received Date/Time: N/A

MB N/A

P:3535A MB 200-112608/1-A 200-112622 200-112608 12/20/2016 19:41 RCKTAL BUR1

A:522 MB 200-112608/1-A 200-112622 200-112608 12/21/2016 20:55 SHBTAL BUR1

Lab ID:




Client ID:

Sample Date/Time: N/A Received Date/Time: N/A

LCS N/A

P:3535A LCS 200-112608/2-A 200-112622 200-112608 12/20/2016 19:41 RCKTAL BUR1

A:522 LCS 200-112608/2-A 200-112622 200-112608 12/21/2016 20:35 SHBTAL BUR1

Lab References:TAL BUR = TestAmerica Burlington

A = Analytical Method P = Prep Method TestAmerica Buffalo

Page 22 of 116

Certification SummaryClient: Tetra Tech GEO TestAmerica Job ID: 480-111215-1Project/Site: W.R. Grace, Acton

Laboratory Authority Program EPA Region Certification ID

TestAmerica Burlington PH-0751State ProgramConnecticut 1

TestAmerica Burlington NAState ProgramDE Haz. Subst. Cleanup Act (HSCA) 3

TestAmerica Burlington E87467NELAPFlorida 4

TestAmerica Burlington L2336DoD ELAPL-A-B

TestAmerica Burlington VT00008State ProgramMaine 1

TestAmerica Burlington 050-999-436NELAPMinnesota 5

TestAmerica Burlington 2006NELAPNew Hampshire 1

TestAmerica Burlington VT972NELAPNew Jersey 2

TestAmerica Burlington 10391NELAPNew York 2

TestAmerica Burlington 68-00489NELAPPennsylvania 3

TestAmerica Burlington LAO00298State ProgramRhode Island 1

TestAmerica Burlington LE-058448-0FederalUS Fish & Wildlife

TestAmerica Burlington P330-11-00093FederalUSDA

TestAmerica Burlington VT-4000State ProgramVermont 1

TestAmerica Burlington 460209NELAPVirginia 3

Accreditation may not be offered or required for all methods and analytes reported in this package. Please contact your project manager for the laboratorys current list of certified methods and analytes.

TestAmerica BuffaloPage 23 of 116

Method 5221,4 Dioxane (GC/MS SIM) by Method

522

Page 24 of 116

FORM IIGC/MS SEMI VOA SURROGATE RECOVERY

Lab Name: Job No.: 480-111215-1

SDG No.:

Matrix: Water Level: Low

TestAmerica Burlington

GC Column (1): Rxi-5ms ID: 0.25(mm)

Lab Sample IDClient Sample ID #DXE

480-111215-1ASSABET-1A 85

480-111215-2ASSABET-2A 83

480-111215-3CHRISTOFFERSON 84

480-111215-4SCRIBNER 80

480-111215-5SCRIBNER-DUP 81

MB 200-112608/1-A

81

LCS 200-112608/2-A

83

480-111215-4 MSSCRIBNER MS 70

480-111215-4 MSDSCRIBNER MSD 71

QC LIMITSDXE = 1,4-Dioxane-d8 (Surr) 70-130

FORM II 522

# Column to be used to flag recovery values

Page 25 of 116

GC/MS SEMI VOA LAB CONTROL SAMPLE RECOVERYFORM III

Job No.:Lab Name:

SDG No.:

Level:Matrix: Low

480-111215-1

Lab File ID: Z23206_33.DWater

Lab ID: LCS 200-112608/2-A Client ID:


REC %REC

QCLIMITSCONCENTRATION

(ug/L)

SPIKEADDED(ug/L)

#LCS LCS

COMPOUND1,4-Dioxane 0.200 0.192 70-13096J

FORM III 522

# Column to be used to flag recovery and RPD values

Page 26 of 116

GC/MS SEMI VOA MATRIX SPIKE RECOVERYFORM III

Job No.:Lab Name:

SDG No.:

Level:Matrix: Low

480-111215-1


Lab ID: 480-111215-4 MS Client ID: SCRIBNER MS


LIMITSCOMPOUND

CONCENTRATION %REC

QC

REC

SAMPLECONCENTRATION

SPIKEADDED(ug/L) (ug/L) (ug/L)

#MS MS

2.00 1.80 70-1301,4-Dioxane 730.34

FORM III 522


Page 27 of 116

GC/MS SEMI VOA MATRIX SPIKE DUPLICATE RECOVERYFORM III

Job No.:Lab Name:

SDG No.:

Level:Matrix: Low

480-111215-1


Lab ID: 480-111215-4 MSD Client ID: SCRIBNER MSD


COMPOUND

SPIKEADDED CONCENTRATION %

REC%RPD

QC LIMITS

RPD REC (ug/L) (ug/L)#

MSD MSD

2.00 1.79 30 70-1301,4-Dioxane 073

FORM III 522


Page 28 of 116

FORM IVGC/MS SEMI VOA METHOD BLANK SUMMARY

Lab Name:

SDG No.:

Job No.: 480-111215-1TestAmerica Burlington

Instrument ID:

Level:(Low/Med)

Date Extracted:

Date Analyzed: 12/21/2016 20:55

12/20/2016 19:41

Low

CHZ.i

Lab File ID: Z23206_34.D Lab Sample ID: MB 200-112608/1-A

Matrix: Water

THIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES:

LAB SAMPLE IDLAB

FILE ID DATE ANALYZEDCLIENT SAMPLE ID 12/21/2016 20:35Z23206_33.DLCS 200-112608/2-A 12/21/2016 23:11Z23206_41.D480-111215-1ASSABET-1A 12/21/2016 23:30Z23206_42.D480-111215-2ASSABET-2A 12/21/2016 23:49Z23206_43.D480-111215-3CHRISTOFFERSON 12/22/2016 13:05Z23228_07.D480-111215-4SCRIBNER 12/22/2016 13:25Z23228_08.D480-111215-4 MSSCRIBNER MS 12/22/2016 13:44Z23228_09.D480-111215-4 MSDSCRIBNER MSD 12/22/2016 14:03Z23228_10.D480-111215-5SCRIBNER-DUP

FORM IV 522

Page 29 of 116

FORM V

DECAFLUOROTRIPHENYLPHOSPHINE (DFTPP)

Lab Name:

SDG No.:

Job No.: 480-111215-1

Lab File ID:

Instrument ID:

Z23129_01.D

CHZ.i

12/15/2016

10:15

BFB Injection Date:

BFB Injection Time:

M/E ION ABUNDANCE CRITERIA% RELATIVEABUNDANCE

Analysis Batch No.: 112452

50 15.0 - 40.0 % of mass 95 21.9 75 30.0 - 80.0 % of mass 95 52.0 95 Base Peak, 100% relative abundance 100.0 96 5.0 - 9.0 % of mass 95 6.8 173 Less than 2.0 % of mass 174 0.2 (0.3) 1174 >50.0 % of mass 95 74.0 175 5.0 - 9.0 % of mass 174 5.5 (7.5) 1176 >95.0 but

GC/MS SEMI VOA INTERNAL STANDARD AREA AND RETENTION TIME SUMMARY

Lab Name: Job No.:

SDG No.:

FORM VIII


Sample No.: ICIS 200-112452/6 Date Analyzed: 12/15/2016 11:30

Lab File ID (Standard): Z23129_06.D

Instrument ID: CHZ.i GC Column: Rxi-5ms ID: 0.25(mm)

Heated Purge: (Y/N) N

Calibration ID: 36223

# RT # RT # # RT ##AREA AREA AREA

UPPER LIMIT

LOWER LIMIT

289677

96559

3.37INITIAL CALIBRATION MID-POINT

3.87

2.87

193118

LAB SAMPLE ID CLIENT SAMPLE ID

ICV 200-112452/10 174233 3.38

CCVL 200-112452/11 224676 3.38

CCV 200-112622/32 170667 3.37

LCS 200-112608/2-A 177383 3.37

MB 200-112608/1-A 219466 3.40

480-111215-1 ASSABET-1A 192145 3.38

480-111215-2 ASSABET-2A 215152 3.40

480-111215-3 CHRISTOFFERSON 229249 3.38

CCV 200-112622/46 200564 3.40

CCVL 200-112677/1 232614 3.44

480-111215-4 SCRIBNER 197386 3.37

480-111215-4 MS SCRIBNER MS 237656 3.44

480-111215-4 MSD SCRIBNER MSD 218619 3.40

480-111215-5 SCRIBNER-DUP 217201 3.39

CCV 200-112677/12 200181 3.38

= Tetrahydrofuran-d8

Area Limit = 50%-150% of internal standard areaRT Limit = 0.5 minutes of internal standard RT

# Column used to flag values outside QC limits

FORM VIII 522

Page 31 of 116

FORM IGC/MS SEMI VOA ORGANICS ANALYSIS DATA SHEET

Client Sample ID:

Lab Name: Job No.:

ASSABET-1A

SDG No.:

480-111215-1

Lab Sample ID: 480-111215-1

Matrix: Z23206_41.DLab File ID:

Date Collected:522Analysis Method:

Water


12/15/2016 14:35

Level: (low/med)

Con. Extract Vol.:

Injection Volume:

GPC Cleanup:(Y/N)

Date Analyzed:

Date Extracted:

Dilution Factor:

Extract. Method: 12/20/2016 19:41

1

3535A

12/21/2016 23:11

Low2(uL)

2000(uL)

% Moisture:

Sample wt/vol: 100(mL)

N

Analysis Batch No.: 112622 ug/LUnits:

CAS NO. COMPOUND NAME RESULT Q MDLRL

0.20 0.057123-91-1 1,4-Dioxane 1.0

%RECCAS NO. LIMITSQSURROGATE

85 70-13017647-74-4 1,4-Dioxane-d8 (Surr)

FORM I 522

Page 32 of 116

I I I I I

I I I I I

I I I I

I I I I

Report Date: 22-Dec-2016 13:52:30 Chrom Revision: 2.2 05-Dec-2016 12:37:22

TestAmerica BurlingtonTarget Compound Quantitation Report

Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161221-23206.b\Z23206_41.DLims ID: 480-111215-A-1-A Client ID: ASSABET-1ASample Type: ClientInject. Date: 21-Dec-2016 23:11:30 ALS Bottle#: 40 Worklist Smp#: 41Injection Vol: 2.0 ul Dil. Factor: 1.0000 Sample Info: 200-0023206-041Operator ID: shb Instrument ID: CHZ.i

Method: \\ChromNA\Burlington\ChromData\CHZ.i\20161221-23206.b\522_MOD_Z.mLimit Group: SV_522_LimitsLast Update: 22-Dec-2016 13:51:40 Calib Date: 15-Dec-2016 12:19:30Integrator: RTE ID Type: RT Order IDQuant Method: Internal Standard Quant By: Initial CalibrationLast ICal File: \\ChromNA\Burlington\ChromData\CHZ.i\20161215-23129.b\Z23129_09.D

Column 1 : Rxi-5ms ( 0.25 mm) Det: MS SCANProcess Host: XAWRK002

First Level Reviewer: bagcilars Date: 22-Dec-2016 11:28:18

Compound SigRT

(min.)Exp RT(min.)

Dlt RT(min.) Q Response

OnCol Amtng/ul Flags

* 1 Tetrahydrofuran-d8 46 3.377 3.371 0.006 92 192145 0.5000 $ 2 1,4-Dioxane-d8 (Surr) 64 4.287 4.281 0.006 98 24804 0.0855 3 1,4-Dioxane 58 4.329 4.323 0.006 87 15157 0.0521 $ 4 BFB

Reagents:SV522ISi_00031 Amount Added: 4.00 Units: uL Run Reagent

Page 33 of 116

Report Date: 22-Dec-2016 13:52:31 Chrom Revision: 2.2 05-Dec-2016 12:37:22TestAmerica Burlington

Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161221-23206.b\Z23206_41.DInjection Date: 21-Dec-2016 23:11:30 Instrument ID: CHZ.i Operator ID: shbLims ID: 480-111215-A-1-A Lab Sample ID: 200-111215-1 Worklist Smp#: 41Client ID: ASSABET-1AInjection Vol: 2.0 ul Dil. Factor: 1.0000 ALS Bottle#: 40Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Y Scaling: Method Defined: Set to Absolute Y Value

3.0 3.3 3.5 3.8 4.0 4.3 4.5 4.8 5.0 5.3 5.5 5.8 6.0 6.3 6.5 6.8 7.0 7.3 7.5 7.8 8.0 8.3 8.5Min

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30

32

34

Y (

X10

0000

)

Z23206_41[MS SCAN Chro]:Total

* T

etra

hydr

ofur

an-d

8( 3

.377

)

Page 34 of 116


Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161221-23206.b\Z23206_41.DInjection Date: 21-Dec-2016 23:11:30 Instrument ID: CHZ.iLims ID: 480-111215-A-1-A Lab Sample ID: 200-111215-1 Client ID: ASSABET-1AOperator ID: shb ALS Bottle#: 40 Worklist Smp#: 41Injection Vol: 2.0 ul Dil. Factor: 1.0000 Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Detector MS SCAN 3 1,4-Dioxane, CAS: 123-91-1

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

0

3

6

9

12

15

18

Y (

X10

00)

Raw Spec:Scan 210(4.33)

88

58

57

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

0

3

6

9

12

15

18

Y (

X10

00)

Enhanced Spec:Scan 210(4.33), Qvalue=87

88

58

57

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

0

3

6

9

12

15

18

21

24

Y (

X10

00)

Ref Spec: 3 1,4-Dioxane @ 4.430 min.

8858

57

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

-100

-75

-50

-25

0

25

50

75

100

Y

Differenc Spec:Scan 210 @ 4.329 min.(Qvalue: 87)

Page 35 of 116

I I


Client Sample ID:

Lab Name: Job No.:

ASSABET-2A

SDG No.:

480-111215-1




Water


12/15/2016 14:40

Level: (low/med)

Con. Extract Vol.:

Injection Volume:

GPC Cleanup:(Y/N)

Date Analyzed:

Date Extracted:

Dilution Factor:

Extract. Method: 12/20/2016 19:41

1

3535A

12/21/2016 23:30

Low2(uL)

2000(uL)

% Moisture:


N



0.20 0.057123-91-1 1,4-Dioxane 0.41


83 70-13017647-74-4 1,4-Dioxane-d8 (Surr)

FORM I 522

Page 36 of 116

I I I I I

I I I I I

I I I I

I I I I



Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161221-23206.b\Z23206_42.DLims ID: 480-111215-A-2-A Client ID: ASSABET-2ASample Type: ClientInject. Date: 21-Dec-2016 23:30:30 ALS Bottle#: 41 Worklist Smp#: 42Injection Vol: 2.0 ul Dil. Factor: 1.0000 Sample Info: 200-0023206-042Operator ID: shb Instrument ID: CHZ.i




Compound SigRT

(min.)Exp RT(min.)





Page 37 of 116


Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161221-23206.b\Z23206_42.DInjection Date: 21-Dec-2016 23:30:30 Instrument ID: CHZ.i Operator ID: shbLims ID: 480-111215-A-2-A Lab Sample ID: 200-111215-2 Worklist Smp#: 42Client ID: ASSABET-2AInjection Vol: 2.0 ul Dil. Factor: 1.0000 ALS Bottle#: 41Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Y Scaling: Method Defined: Set to Absolute Y Value

3.0 3.3 3.5 3.8 4.0 4.3 4.5 4.8 5.0 5.3 5.5 5.8 6.0 6.3 6.5 6.8 7.0 7.3 7.5 7.8 8.0 8.3 8.5Min

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30

32

34

Y (

X10

0000

)


Page 38 of 116


Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161221-23206.b\Z23206_42.DInjection Date: 21-Dec-2016 23:30:30 Instrument ID: CHZ.iLims ID: 480-111215-A-2-A Lab Sample ID: 200-111215-2 Client ID: ASSABET-2AOperator ID: shb ALS Bottle#: 41 Worklist Smp#: 42Injection Vol: 2.0 ul Dil. Factor: 1.0000 Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Detector MS SCAN 3 1,4-Dioxane, CAS: 123-91-1

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

0

11

22

33

44

55

66

77

88

Y (

X10

0)


88

58

57

9664

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

0

11

22

33

44

55

66

77

88

Y (

X10

0)


88

58

57

9664

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

0

3

6

9

12

15

18

21

24

Y (

X10

00)


8858

57

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

-100

-75

-50

-25

0

25

50

75

100

Y


9657

Page 39 of 116

. /

.

.

' . . . ' . .

I '1 I '1 I .

. /

.

.

' . . . ' . .

I '1 I '1 I I I I I I I I I I I I I I I I I I I I I I -r I

. /

. ' .

.

.

. ' .

. I I

I I . I I I I I I I I I I I I I I I I I I I I I .

.

.

. . ' I /I

.

.

.

I


Client Sample ID:

Lab Name: Job No.:

CHRISTOFFERSON

SDG No.:

480-111215-1




Water


12/15/2016 14:55

Level: (low/med)

Con. Extract Vol.:

Injection Volume:

GPC Cleanup:(Y/N)

Date Analyzed:

Date Extracted:

Dilution Factor:

Extract. Method: 12/20/2016 19:41

1

3535A

12/21/2016 23:49

Low2(uL)

2000(uL)

% Moisture:


N



0.20 0.057123-91-1 1,4-Dioxane 0.28


84 70-13017647-74-4 1,4-Dioxane-d8 (Surr)

FORM I 522

Page 40 of 116

I I I I I

I I I I I

I I I I

I I I I



Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161221-23206.b\Z23206_43.DLims ID: 480-111215-A-3-A Client ID: CHRISTOFFERSONSample Type: ClientInject. Date: 21-Dec-2016 23:49:30 ALS Bottle#: 42 Worklist Smp#: 43Injection Vol: 2.0 ul Dil. Factor: 1.0000 Sample Info: 200-0023206-043Operator ID: shb Instrument ID: CHZ.i




Compound SigRT

(min.)Exp RT(min.)





Page 41 of 116


Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161221-23206.b\Z23206_43.DInjection Date: 21-Dec-2016 23:49:30 Instrument ID: CHZ.i Operator ID: shbLims ID: 480-111215-A-3-A Lab Sample ID: 200-111215-3 Worklist Smp#: 43Client ID: CHRISTOFFERSONInjection Vol: 2.0 ul Dil. Factor: 1.0000 ALS Bottle#: 42Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Y Scaling: Method Defined: Set to Absolute Y Value

3.0 3.3 3.5 3.8 4.0 4.3 4.5 4.8 5.0 5.3 5.5 5.8 6.0 6.3 6.5 6.8 7.0 7.3 7.5 7.8 8.0 8.3 8.5Min

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30

32

34

Y (

X10

0000

)


Page 42 of 116


Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161221-23206.b\Z23206_43.DInjection Date: 21-Dec-2016 23:49:30 Instrument ID: CHZ.iLims ID: 480-111215-A-3-A Lab Sample ID: 200-111215-3 Client ID: CHRISTOFFERSONOperator ID: shb ALS Bottle#: 42 Worklist Smp#: 43Injection Vol: 2.0 ul Dil. Factor: 1.0000 Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Detector MS SCAN 3 1,4-Dioxane, CAS: 123-91-1

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

0

8

16

24

32

40

48

56

64

Y (

X10

0)


88

58

57

9678

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

0

8

16

24

32

40

48

56

64

Y (

X10

0)


88

58

57

9678

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

0

3

6

9

12

15

18

21

24

Y (

X10

00)


8858

57

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

-100

-75

-50

-25

0

25

50

75

100

Y


57

Page 43 of 116

. /

.

.

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. ' .

. '1 '1

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.

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- / - ' -. . .

' . .

I I I I I I I I I I I I I I I I I I I I I I I I I I I

.

.

.

.

. . / . I

I

.

.

.

'


Client Sample ID:

Lab Name: Job No.:

SCRIBNER

SDG No.:

480-111215-1




Water


12/15/2016 15:20

Level: (low/med)

Con. Extract Vol.:

Injection Volume:

GPC Cleanup:(Y/N)

Date Analyzed:

Date Extracted:

Dilution Factor:

Extract. Method: 12/20/2016 19:41

1

3535A

12/22/2016 13:05

Low2(uL)

2000(uL)

% Moisture:


N



0.20 0.057123-91-1 1,4-Dioxane 0.34


80 70-13017647-74-4 1,4-Dioxane-d8 (Surr)

FORM I 522

Page 44 of 116

I I I I I

I I I I I

I I I I

I I I I



Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161222-23228.b\Z23228_07.DLims ID: 480-111215-A-4-A Client ID: SCRIBNERSample Type: ClientInject. Date: 22-Dec-2016 13:05:30 ALS Bottle#: 7 Worklist Smp#: 7Injection Vol: 2.0 ul Dil. Factor: 1.0000 Sample Info: 200-0023228-007Operator ID: shb Instrument ID: CHZ.i




Compound SigRT

(min.)Exp RT(min.)



* 1 Tetrahydrofuran-d8 46 3.371 3.442 -0.071 94 197386 0.5000 $ 2 1,4-Dioxane-d8 (Surr) 64 4.287 4.323 -0.036 94 23830 0.0799 3 1,4-Dioxane 58 4.323 4.365 -0.042 86 5118 0.0171


Page 45 of 116


Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161222-23228.b\Z23228_07.DInjection Date: 22-Dec-2016 13:05:30 Instrument ID: CHZ.i Operator ID: shbLims ID: 480-111215-A-4-A Lab Sample ID: 200-111215-4 Worklist Smp#: 7Client ID: SCRIBNERInjection Vol: 2.0 ul Dil. Factor: 1.0000 ALS Bottle#: 7Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Y Scaling: Method Defined: Set to Absolute Y Value

3.0 3.3 3.5 3.8 4.0 4.3 4.5 4.8 5.0 5.3 5.5 5.8 6.0 6.3 6.5 6.8 7.0 7.3 7.5 7.8 8.0 8.3 8.5Min

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30

32

34

Y (

X10

0000

)


Page 46 of 116


Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161222-23228.b\Z23228_07.DInjection Date: 22-Dec-2016 13:05:30 Instrument ID: CHZ.iLims ID: 480-111215-A-4-A Lab Sample ID: 200-111215-4 Client ID: SCRIBNEROperator ID: shb ALS Bottle#: 7 Worklist Smp#: 7Injection Vol: 2.0 ul Dil. Factor: 1.0000 Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Detector MS SCAN 3 1,4-Dioxane, CAS: 123-91-1

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

0

10

20

30

40

50

60

70

Y (

X10

0)


88

58

57

9678

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

0

10

20

30

40

50

60

70

Y (

X10

0)


88

58

57

9678

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

0

3

6

9

12

15

18

21

24

Y (

X10

00)


8858

57

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

-100

-75

-50

-25

0

25

50

75

100

Y


Page 47 of 116

/ -.

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-

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.

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I


Client Sample ID:

Lab Name: Job No.:

SCRIBNER-DUP

SDG No.:

480-111215-1




Water


12/15/2016 15:22

Level: (low/med)

Con. Extract Vol.:

Injection Volume:

GPC Cleanup:(Y/N)

Date Analyzed:

Date Extracted:

Dilution Factor:

Extract. Method: 12/20/2016 19:41

1

3535A

12/22/2016 14:03

Low2(uL)

2000(uL)

% Moisture:


N



0.20 0.057123-91-1 1,4-Dioxane 0.32


81 70-13017647-74-4 1,4-Dioxane-d8 (Surr)

FORM I 522

Page 48 of 116

I I I I I

I I I I I

I I I I

I I I I



Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161222-23228.b\Z23228_10.DLims ID: 480-111215-A-5-A Client ID: SCRIBNER-DUPSample Type: ClientInject. Date: 22-Dec-2016 14:03:30 ALS Bottle#: 10 Worklist Smp#: 10Injection Vol: 2.0 ul Dil. Factor: 1.0000 Sample Info: 200-0023228-010Operator ID: shb Instrument ID: CHZ.i




Compound SigRT

(min.)Exp RT(min.)



* 1 Tetrahydrofuran-d8 46 3.389 3.442 -0.053 90 217201 0.5000 $ 2 1,4-Dioxane-d8 (Surr) 64 4.293 4.323 -0.030 95 26735 0.0815 3 1,4-Dioxane 58 4.335 4.365 -0.030 86 5306 0.0161 $ 4 BFB


Page 49 of 116


Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161222-23228.b\Z23228_10.DInjection Date: 22-Dec-2016 14:03:30 Instrument ID: CHZ.i Operator ID: shbLims ID: 480-111215-A-5-A Lab Sample ID: 200-111215-5 Worklist Smp#: 10Client ID: SCRIBNER-DUPInjection Vol: 2.0 ul Dil. Factor: 1.0000 ALS Bottle#: 10Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Y Scaling: Method Defined: Set to Absolute Y Value

3.0 3.3 3.5 3.8 4.0 4.3 4.5 4.8 5.0 5.3 5.5 5.8 6.0 6.3 6.5 6.8 7.0 7.3 7.5 7.8 8.0 8.3 8.5Min

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30

32

34

Y (

X10

0000

)


Page 50 of 116


Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161222-23228.b\Z23228_10.DInjection Date: 22-Dec-2016 14:03:30 Instrument ID: CHZ.iLims ID: 480-111215-A-5-A Lab Sample ID: 200-111215-5 Client ID: SCRIBNER-DUPOperator ID: shb ALS Bottle#: 10 Worklist Smp#: 10Injection Vol: 2.0 ul Dil. Factor: 1.0000 Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Detector MS SCAN 3 1,4-Dioxane, CAS: 123-91-1

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

0

11

22

33

44

55

66

77

Y (

X10

0)


88

58

57

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

0

11

22

33

44

55

66

77

Y (

X10

0)


88

58

57

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

0

3

6

9

12

15

18

21

24

Y (

X10

00)


8858

57

46 50 54 58 62 66 70 74 78 82 86 90 94m/z

-100

-75

-50

-25

0

25

50

75

100

Y


Page 51 of 116

/ . .

.

' . .

' . .

' I I I I '

/ . .

.

' . .

' . .

' I I I I --. I I T I I T I I --. I I T I I --. I I --. I T I I --.

. /

. ' .

.

.

. ' .

. I I

I I ' I I I I I ' I I I I I I I I ' I I I I I

.

.

.

. .

. I '

.

.

'

FORM VI

Lab Name: Job No.:

Calibration ID:

SDG No.:

Instrument ID: GC Column: Heated Purge: (Y/N)

GC/MS SEMI VOA BY INTERNAL STANDARD - INITIAL CALIBRATION DATA


CHZ.i

Analy Batch No.: 112452

36223Calibration Start Date: Calibration End Date:12/15/2016 10:42

N

12/15/2016 12:19

0.25(mm)Rxi-5ms ID:

CURVE EVALUATION

Calibration Files:

LEVEL: LAB SAMPLE ID: LAB FILE ID:1Level IC 200-112452/9 Z23129_09.D2Level IC 200-112452/8 Z23129_08.D3Level IC 200-112452/7 Z23129_07.D4Level ICIS 200-112452/6 Z23129_06.D5Level IC 200-112452/5 Z23129_05.D6Level IC 200-112452/4 Z23129_04.D7Level IC 200-112452/3 Z23129_03.D

ANALYTE RRF

LVL 1 LVL 2 LVL 3 LVL 4 LVL 5

CURVETYPE

COEFFICIENT

B M1 M2

# %RSD # MAX%RSD

R^2OR COD

# MIN R^2OR COD

MIN RRF

LVL 6 LVL 7

1,4-Dioxane 0.8687 0.7062 0.6960 0.7799 0.7732 Ave 7.70.7303 0.7465

0.0500 15.0 0.99000.7573

1,4-Dioxane-d8 (Surr) 0.7894 0.7482 0.7708 0.7551 0.7857 Ave 4.30.7448 0.6924

15.0 0.99000.7552

FORM VI 522

Note: The m1 coefficient is the same as Ave RRF for an Ave curve type.

Page 52 of 116

FORM VI

Lab Name: Job No.:

Calibration ID:

SDG No.:

Instrument ID: Heated Purge: (Y/N)

GC/MS SEMI VOA BY INTERNAL STANDARD - INITIAL CALIBRATION DATA


CHZ.i

Analy Batch No.: 112452

36223Calibration Start Date: Calibration End Date:12/15/2016 10:42

N

12/15/2016 12:19

GC Column: Rxi-5ms ID: 0.25(mm)

RESPONSE AND CONCENTRATION

Calibration Files:

LEVEL: LAB SAMPLE ID: LAB FILE ID:Level 1 IC 200-112452/9 Z23129_09.DLevel 2 IC 200-112452/8 Z23129_08.DLevel 3 IC 200-112452/7 Z23129_07.DLevel 4 ICIS 200-112452/6 Z23129_06.DLevel 5 IC 200-112452/5 Z23129_05.DLevel 6 IC 200-112452/4 Z23129_04.DLevel 7 IC 200-112452/3 Z23129_03.D

ANALYTE CURVETYPE

ISREF

RESPONSE

LVL 1 LVL 2 LVL 3 LVL 4 LVL 5

CONCENTRATION (NG/UL)

LVL 1 LVL 2 LVL 3 LVL 4 LVL 5LVL 6 LVL 7 LVL 6 LVL 7

1,4-Dioxane Ave 3288 7516 12569 30123 56669136853 252659

0.0100 0.0200 0.0500 0.100 0.2000.400 0.800

1,4-Dioxane-d8 (Surr) Ave 149392 199079 139205 145819 143957174452 146462

0.500 0.500 0.500 0.500 0.5000.500 0.500

Curve Type Legend:Ave = Average ISTD

FORM VI 522 Page 53 of 116



Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161215-23129.b\Z23129_03.DLims ID: IC Client ID:Sample Type: IC Calib Level: 7Inject. Date: 15-Dec-2016 10:42:30 ALS Bottle#: 3 Worklist Smp#: 3Injection Vol: 2.0 ul Dil. Factor: 1.0000 Sample Info: 200-0023129-003Operator ID: shb Instrument ID: CHZ.iSublist: chrom-522_MOD_Z*sub8



First Level Reviewer: snellingn Date: 15-Dec-2016 11:11:01

Compound SigRT

(min.)Exp RT(min.)


Cal Amtng/ul


* 1 Tetrahydrofuran-d8 46 3.388 3.383 0.005 88 211524 0.5000 0.5000 $ 2 1,4-Dioxane-d8 (Surr) 64 4.293 4.293 0.000 95 146462 0.5000 0.4584 3 1,4-Dioxane 58 4.329 4.329 0.000 95 252659 0.8000 0.7887

Reagents:SV522SUi_00018 Amount Added: 10.00 Units: uLSV522CALi_00033 Amount Added: 80.00 Units: uLSV522ISi_00031 Amount Added: 4.00 Units: uL Run Reagent

Page 54 of 116


Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161215-23129.b\Z23129_03.DInjection Date: 15-Dec-2016 10:42:30 Instrument ID: CHZ.i Operator ID: shbLims ID: IC Worklist Smp#: 3Client ID:Injection Vol: 2.0 ul Dil. Factor: 1.0000 ALS Bottle#: 3Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Y Scaling: Method Defined: Set to Absolute Y Value

3.0 3.3 3.5 3.8 4.0 4.3 4.5 4.8 5.0 5.3 5.5 5.8 6.0 6.3 6.5 6.8 7.0 7.3 7.5 7.8 8.0 8.3 8.5Min

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30

32

34

Y (

X10

0000

)


Page 55 of 116







Compound SigRT

(min.)Exp RT(min.)


Cal Amtng/ul




Page 56 of 116



3.0 3.3 3.5 3.8 4.0 4.3 4.5 4.8 5.0 5.3 5.5 5.8 6.0 6.3 6.5 6.8 7.0 7.3 7.5 7.8 8.0 8.3 8.5Min

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30

32

34

Y (

X10

0000

)


Page 57 of 116







Compound SigRT

(min.)Exp RT(min.)


Cal Amtng/ul


* 1 Tetrahydrofuran-d8 46 3.365 3.383 -0.018 92 183221 0.5000 0.5000 M$ 2 1,4-Dioxane-d8 (Surr) 64 4.281 4.293 -0.012 95 143957 0.5000 0.5202 3 1,4-Dioxane 58 4.317 4.329 -0.012 95 56669 0.2000 0.2042

QC Flag LegendReview Flags M - Manually IntegratedReagents:SV522SUi_00018 Amount Added: 10.00 Units: uLSV522CALi_00033 Amount Added: 20.00 Units: uLSV522ISi_00031 Amount Added: 4.00 Units: uL Run Reagent

Page 58 of 116



3.0 3.3 3.5 3.8 4.0 4.3 4.5 4.8 5.0 5.3 5.5 5.8 6.0 6.3 6.5 6.8 7.0 7.3 7.5 7.8 8.0 8.3 8.5Min

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30

32

34

Y (

X10

0000

)


Page 59 of 116

Report Date: 15-Dec-2016 14:13:43 Chrom Revision: 2.2 05-Dec-2016 12:37:22Manual Integration/User Assign Peak Report

TestAmerica BurlingtonData File: \\ChromNA\Burlington\ChromData\CHZ.i\20161215-23129.b\Z23129_05.DInjection Date: 15-Dec-2016 11:14:30 Instrument ID: CHZ.iLims ID: IC Client ID:Operator ID: shb ALS Bottle#: 5 Worklist Smp#: 5Injection Vol: 2.0 ul Dil. Factor: 1.0000 Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Detector MS SCAN

* 1 Tetrahydrofuran-d8, CAS: 1693-74-9Signal: 1

Processing Integration ResultsRT: 3.36Area: 183662Amount: 0.500000Amount Units: ng/ul

3.0 3.2 3.4 3.6 3.8Min

0

1

2

3

4

5

6

7

8

9

10

11

12

13

14

Y (

X10

000)

m/z 46.0

3.3

65

Manual Integration ResultsRT: 3.36Area: 183221Amount: 0.500000Amount Units: ng/ul

3.0 3.2 3.4 3.6 3.8Min

0

1

2

3

4

5

6

7

8

9

10

11

12

13

14

Y (

X10

000)

m/z 46.0

3.3

65

Reviewer: snellingn, 15-Dec-2016 14:11:38Audit Action: Split an Integrated Peak Audit Reason: Baseline

Page 60 of 116



Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161215-23129.b\Z23129_06.DLims ID: ICIS Client ID:Sample Type: ICIS Calib Level: 4Inject. Date: 15-Dec-2016 11:30:30 ALS Bottle#: 6 Worklist Smp#: 6Injection Vol: 2.0 ul Dil. Factor: 1.0000 Sample Info: 200-0023129-006Operator ID: shb Instrument ID: CHZ.iSublist: chrom-522_MOD_Z*sub8




Compound SigRT

(min.)Exp RT(min.)


Cal Amtng/ul


* 1 Tetrahydrofuran-d8 46 3.365 3.365 0.000 95 193118 0.5000 0.5000 M$ 2 1,4-Dioxane-d8 (Surr) 64 4.281 4.281 0.000 97 145819 0.5000 0.4999 3 1,4-Dioxane 58 4.317 4.317 0.000 97 30123 0.1000 0.1030

QC Flag LegendReview Flags M - Manually IntegratedReagents:SV522SUi_00018 Amount Added: 10.00 Units: uLSV522CALi_00033 Amount Added: 10.00 Units: uLSV522ISi_00031 Amount Added: 4.00 Units: uL Run Reagent

Page 61 of 116


Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161215-23129.b\Z23129_06.DInjection Date: 15-Dec-2016 11:30:30 Instrument ID: CHZ.i Operator ID: shbLims ID: ICIS Worklist Smp#: 6Client ID:Injection Vol: 2.0 ul Dil. Factor: 1.0000 ALS Bottle#: 6Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Y Scaling: Method Defined: Set to Absolute Y Value

3.0 3.3 3.5 3.8 4.0 4.3 4.5 4.8 5.0 5.3 5.5 5.8 6.0 6.3 6.5 6.8 7.0 7.3 7.5 7.8 8.0 8.3 8.5Min

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30

32

34

Y (

X10

0000

)


Page 62 of 116

Report Date: 15-Dec-2016 14:13:44 Chrom Revision: 2.2 05-Dec-2016 12:37:22Manual Integration/User Assign Peak Report

TestAmerica BurlingtonData File: \\ChromNA\Burlington\ChromData\CHZ.i\20161215-23129.b\Z23129_06.DInjection Date: 15-Dec-2016 11:30:30 Instrument ID: CHZ.iLims ID: ICIS Client ID:Operator ID: shb ALS Bottle#: 6 Worklist Smp#: 6Injection Vol: 2.0 ul Dil. Factor: 1.0000 Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Detector MS SCAN

* 1 Tetrahydrofuran-d8, CAS: 1693-74-9Signal: 1

Processing Integration ResultsRT: 3.36Area: 203434Amount: 0.500000Amount Units: ng/ul

3.1 3.3 3.5 3.7Min

0

1

2

3

4

5

6

7

8

9

10

11

12

13

14

Y (

X10

000)

m/z 46.0

3.3

65

Manual Integration ResultsRT: 3.36Area: 193118Amount: 0.500000Amount Units: ng/ul

3.1 3.3 3.5Min

0

1

2

3

4

5

6

7

8

9

10

11

12

13

14

Y (

X10

000)

m/z 46.0

3.3

65

Reviewer: snellingn, 15-Dec-2016 14:11:48Audit Action: Split an Integrated Peak Audit Reason: Baseline

Page 63 of 116







Compound SigRT

(min.)Exp RT(min.)


Cal Amtng/ul




Page 64 of 116



3.0 3.3 3.5 3.8 4.0 4.3 4.5 4.8 5.0 5.3 5.5 5.8 6.0 6.3 6.5 6.8 7.0 7.3 7.5 7.8 8.0 8.3 8.5Min

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30

32

34

Y (

X10

0000

)


* T

etra

hydr

ofur

an-d

8( 3

.365

)

Page 65 of 116







Compound SigRT

(min.)Exp RT(min.)


Cal Amtng/ul




Page 66 of 116



3.0 3.3 3.5 3.8 4.0 4.3 4.5 4.8 5.0 5.3 5.5 5.8 6.0 6.3 6.5 6.8 7.0 7.3 7.5 7.8 8.0 8.3 8.5Min

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30

32

34

Y (

X10

0000

)


* T

etra

hydr

ofur

an-d

8( 3

.418

)

Page 67 of 116

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

- l ----- ~ I I I I I I I I I I I I I I I I I I I I I I







Compound SigRT

(min.)Exp RT(min.)


Cal Amtng/ul


* 1 Tetrahydrofuran-d8 46 3.359 3.365 -0.006 98 189242 0.5000 0.5000 $ 2 1,4-Dioxane-d8 (Surr) 64 4.281 4.281 0.000 92 149392 0.5000 0.5227 3 1,4-Dioxane 58 4.317 4.317 0.000 56 3288 0.0100 0.0115


Page 68 of 116



3.0 3.3 3.5 3.8 4.0 4.3 4.5 4.8 5.0 5.3 5.5 5.8 6.0 6.3 6.5 6.8 7.0 7.3 7.5 7.8 8.0 8.3 8.5Min

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30

32

34

Y (

X10

0000

)


$ 1,

4-D

ioxa

ne-d

8 (S

urr)

( 4.

281)

+

Page 69 of 116

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

I I I I I I I I I I I I I I I I I I I I I I

FORM VII

Lab Name: Job No.:

SDG No.:

Instrument ID:

Calibration Date:

Calib Start Date:

Lab Sample ID:

Calib End Date:GC Column: ID:

GC/MS SEMI VOA CONTINUING CALIBRATION DATA

0.25(mm)

480-111215-1

CHZ.i

12/15/2016 13:33

12/15/2016 10:42

12/15/2016 12:19

ICV 200-112452/10

Rxi-5ms


Lab File ID: Z23129_10.D Conc. Units: ug/L

ANALYTE CURVE CALC SPIKE %D MAXTYPE AMOUNT AMOUNT %D

AVE RRF RRF MIN RRF

1,4-Dioxane 0.72880.7573 0.0500 192 200 -3.8 20.0Ave

FORM VII 522

Page 70 of 116



Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161215-23129.b\Z23129_10.DLims ID: ICV Client ID:Sample Type: ICVInject. Date: 15-Dec-2016 13:33:30 ALS Bottle#: 10 Worklist Smp#: 10Injection Vol: 2.0 ul Dil. Factor: 1.0000 Sample Info: 200-0023129-010Operator ID: shb Instrument ID: CHZ.iSublist:




Compound SigRT

(min.)Exp RT(min.)


Cal Amtng/ul


* 1 Tetrahydrofuran-d8 46 3.377 3.365 0.011 90 174233 0.5000 0.5000 3 1,4-Dioxane 58 4.323 4.317 0.006 97 50792 0.2000 0.1925

Reagents:SV522ICVi_00011 Amount Added: 100.00 Units: uLSV522ISi_00031 Amount Added: 4.00 Units: uL Run Reagent

Page 71 of 116


Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161215-23129.b\Z23129_10.DInjection Date: 15-Dec-2016 13:33:30 Instrument ID: CHZ.i Operator ID: shbLims ID: ICV Worklist Smp#: 10Client ID:Injection Vol: 2.0 ul Dil. Factor: 1.0000 ALS Bottle#: 10Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Y Scaling: Method Defined: Set to Absolute Y Value

3.0 3.3 3.5 3.8 4.0 4.3 4.5 4.8 5.0 5.3 5.5 5.8 6.0 6.3 6.5 6.8 7.0 7.3 7.5 7.8 8.0 8.3 8.5Min

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30

32

34

Y (

X10

0000

)


Page 72 of 116

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

A ~ I I I I I I I I I I I I I I I I I I I I I I

FORM VII

Lab Name: Job No.:

SDG No.:

Instrument ID:

Calibration Date:

Calib Start Date:

Lab Sample ID:



0.25(mm)

480-111215-1

CHZ.i

12/15/2016 13:58

12/15/2016 10:42

12/15/2016 12:19

CCVL 200-112452/11

Rxi-5ms




AVE RRF RRF MIN RRF

1,4-Dioxane 0.83100.7573 0.0500 11.0 10.0 9.7 50.0Ave

1,4-Dioxane-d8 (Surr) 0.73270.7552 0.0500 485 500 -3.0 50.0Ave

FORM VII 522

Page 73 of 116



Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161215-23129.b\Z23129_11.DLims ID: CCVL Client ID:Sample Type: CCVLInject. Date: 15-Dec-2016 13:58:30 ALS Bottle#: 11 Worklist Smp#: 11Injection Vol: 2.0 ul Dil. Factor: 1.0000 Sample Info: 200-0023129-011Operator ID: shb Instrument ID: CHZ.iSublist: chrom-522_MOD_Z*sub8




Compound SigRT

(min.)Exp RT(min.)


Cal Amtng/ul




Page 74 of 116


Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161215-23129.b\Z23129_11.DInjection Date: 15-Dec-2016 13:58:30 Instrument ID: CHZ.i Operator ID: shbLims ID: CCVL Worklist Smp#: 11Client ID:Injection Vol: 2.0 ul Dil. Factor: 1.0000 ALS Bottle#: 11Method: 522_MOD_Z Limit Group: SV_522_LimitsColumn: Rxi-5ms ( 0.25 mm) Y Scaling: Method Defined: Set to Absolute Y Value

3.0 3.3 3.5 3.8 4.0 4.3 4.5 4.8 5.0 5.3 5.5 5.8 6.0 6.3 6.5 6.8 7.0 7.3 7.5 7.8 8.0 8.3 8.5Min

0

2

4

6

8

10

12

14

16

18

20

22

24

26

28

30

32

34

Y (

X10

0000

)


Page 75 of 116

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

-

I I I I I I I I I I I I I I I I I I I I I I

FORM VII

Lab Name: Job No.:

SDG No.:

Instrument ID:

Calibration Date:

Calib Start Date:

Lab Sample ID:



0.25(mm)

480-111215-1

CHZ.i

12/21/2016 20:15

12/15/2016 10:42

12/15/2016 12:19

CCV 200-112622/32

Rxi-5ms




AVE RRF RRF MIN RRF

1,4-Dioxane 0.75490.7573 0.0500 99.7 100 -0.3 30.0Ave

1,4-Dioxane-d8 (Surr) 0.76730.7552 0.0500 508 500 1.6 30.0Ave

FORM VII 522

Page 76 of 116



Data File: \\ChromNA\Burlington\ChromData\CHZ.i\20161221-23206.b\Z23206_32.DLims ID: CCV Client ID:Sample Type: CCVInject. Date: 21-Dec-2016 20:15:30 ALS Bottle#: 8 Worklist Smp#: 32Injection Vol: 2.0 ul Dil. Factor: 1.0000 Sample Info: 200-0023206-032Operator ID: shb Instrument ID: CHZ.iSublist: chrom-522_MOD_Z*sub8




Compound SigRT

(min.)Exp RT(min.)


Cal Amtng/ul



Reagents:SV522SUi_00018 Amount Added: 10.00 Units: uLSV522CALi_00033 Amount Added: 10.00 Units: uLSV522