ANALYTICAL REPORT

Job Number: 280-21985-1

Job Description: WWK - Phase III Sampling

For:

E.I. du Pont de Nemours and Company ADQM

c/o URS Corporation

Iron Hill Corporate Center

4051 Ogletown Road, Suite 300

Newark, DE 19713

Attention: Michael Aucoin

_____________________________________________

Approved for release.

Michelle Johnston

Project Manager I

11/7/2011 8:04 AM

Michelle Johnston

Project Manager I

michelle.johnston@testamericainc.com

11/07/2011

cc: Ms. Kelly Rinehimer

The test results in this report relate only to the samples in this report and meet all requirements of NELAC, with any

exceptions noted. Pursuant to NELAP, this report shall not be reproduced except in full, without the written approval of

the laboratory. All questions regarding this report should be directed to the TestAmerica Denver Project Manager.

The Lab Certification ID# is E87667.

LBIO-66421

92017720100CVD05F52605

Release TAL27943

Reporting limits are adjusted for sample size used, dilutions and moisture content if applicable.

TestAmerica Laboratories, Inc.

TestAmerica Denver 4955 Yarrow Street, Arvada, CO 80002

Tel (303) 736-0100 Fax (303) 431-7171 www.testamericainc.com

Page 1 of 272
Table of Contents

Cover Title Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

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

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

Manual Integration Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

Sample Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8

Executive Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

Method Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

Method / Analyst Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

Sample Datasheets . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12

Surrogate Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14

QC Data Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

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

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

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

Reagent Traceability . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

Certification Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31

Organic Sample Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32

LCMS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32

8321A_PFC_Du . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32

8321A_PFC_Du QC Summary . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33

8321A_PFC_Du Sample Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39

Standards Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47

8321A_PFC_Du ICAL Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47

8321A_PFC_Du CCAL Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 82

Raw QC Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131

8321A_PFC_Du Tune Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 131

Page 2 of 272
Table of Contents

8321A_PFC_Du Blank Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 146

8321A_PFC_Du LCS/LCSD Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 158

8321A_PFC_Du MS/MSD Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 170

8321A_PFC_Du Duplicate/Triplicate Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 174

8321A_PFC_Du Run Logs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 182

8321A_PFC_Du Prep Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 183

Inorganic Sample Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 249

General Chemistry Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 249

Gen Chem Cover Page . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 250

Gen Chem MDL . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 251

Gen Chem Analysis Run Log . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 252

Gen Chem Raw Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 255

Gen Chem Prep Data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 256

Shipping and Receiving Documents . . . . . . . . . . . . . . . . . . . . . . . . . . . 257

Client Chain of Custody . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 258

Sample Receipt Checklist . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 259

Interlab Coc (where applicable) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 260

Page 3 of 272
CASE NARRATIVE

Client: E. I. DuPont

Project: WWK Phase III Sampling

Report Number: 280-21985-1

With the exceptions noted as flags or footnotes, standard analytical protocols were followed in the analysis of the samples and no 

problems were encountered or anomalies observed. In addition all laboratory quality control samples were within established control 

limits, with any exceptions noted below. Each sample was analyzed to achieve the lowest possible reporting limit within the constraints of 

the method. In some cases, due to interference or analytes present at high concentrations, samples were diluted. For diluted samples, 

the reporting limits are adjusted relative to the dilution required.

Calculations are performed before rounding to avoid round-off errors in calculated results.

All holding times were met and proper preservation noted for the methods performed on these samples, unless otherwise detailed in the 

individual sections below.

The PFC method DV-LC-0012 is an isotope dilution method; therefore, the internal standards are added prior to the extraction process. 

This technique inherently corrects for variability in the extraction efficiency due to sample matrix. Dilution of samples beyond the ability of 

the instrument to detect the internal standards is not recommended. Analyses performed at a dilution level requiring additional internal 

standard to be added after the extraction step in order to quantitate results has been shown to yield results with a significant low bias. As 

a result, data may have been reported over the calibration range. In this case the data will be qualified (E) as estimated.

The PFC method is an isotope dilution method where the internal standards are added prior to extraction and used to quantitate results; 

therefore, the use of dilution factors is inappropriate. Application of dilution factors would yield results that are artificially high. Reporting 

limits and method detection limits are not adjusted for dilutions unless samples are fortified with additional internal standard, which is not 

recommended.

Internal standard abundances may vary depending upon both recovery and the dilution at which the analysis is performed. This is an 

inherent feature of the isotope dilution technique and is not indicative of bias to the reported results.

Sample Arrival and Receipt

The one soil sample presented in this report was received at the TestAmerica Denver laboratory at a temperature of 5.2°C on October 25, 

2011. The sample containers were received in an acceptable condition. No anomalies were observed during sample receipt.

Standards

Analytical standards were prepared using the acid form of the compound perfluorooctanoic acid (PFOA).

The surrogate compound, Perfluoro-n-[1,2,3,4-13C4]octanoic acid was introduced at the extraction step and was used as an internal 

standard for quantitation of PFOA. The concentration of the surrogate spike is 0.2 ug/L in water samples or 50 ug/kg in soil samples.

Sample Extraction and Analysis

The samples presented in this report were extracted for the target analyte by TestAmerica Denver’s SOP DV-OP-0019, Rev. 2 and 

analyzed for the target analytes by TestAmerica Denver’s SOP DV-LC-0012, Rev. 9, with the exceptions of the items indicated in the 

DuPont QAS. Sample WWK-S-WWM-1(0-.2) (280-21985-1) was chosen to be analyzed as a duplicate and also to be spiked with the 

target analyte.

For solid samples ten grams of sample are extracted in 50 mL of basified methanol in a sonication bath for three hours, followed by 

tumbling end over end for 24 hours. Each sample was spiked with the internal standard, prior to extraction. After the sample is extracted, 

centrifuged, and filtered, it is analyzed by LC/MS/MS.

For water samples a 250 mL aliquot of each sample is extracted using solid phase extraction technique with methanol conditioned Weak 

Anion Exchange cartridges. Each sample is spiked with the internal standard, prior to extraction. After the sample is passed through the 

cartridge, the analytes are eluted with 4 mL of 10% ammonium hydroxide in methanol. The final volume is brought to 5 mL using reagent 

water and the extract is analyzed by LC/MS/MS.

The target analyte is separated from other components on a high-performance liquid chromatography (HPLC) C18 column with a mobile 

phase mixture of water containing 0.1% ammonium acetate and methanol. The mass spectrometer detector is operated in the 

electrospray (ESI) negative ion mode. The instrument is calibrated at 7 concentration levels (0.2, 0.5, 1.0, 2.0, 5.0, 10 and 20 ug/L). The 

target analyte is detected as the perfluorooctanoate anion with the parent ion of 413 amu. The daughter ions used for analysis by 

LC/MS/MS are at 369 and 169 amu. The ratio of the peak areas to the two ions must be ±20% of the ion ratios in the mid-point ICAL for 

qualitative identification. Sample results are quantitated using the internal standard method.

Tuning and Calibration

The instrument is tuned with a solution of the target analyte such that mass assignments are within ±0.5 amu of the daughter ions. The 

instrument is calibrated with seven concentration levels from 0.2 ug/L to 20 ug/L. Linear regression (y=ax+b) or quadratic functions 

(y=ax+cx2+b) are used with a correlation coefficient or coefficient of determination 30.990.

Following initial calibration (ICAL), an initial calibration blank (ICB) is tested, which consists of methanol spiked with the surrogate. The 

Page 4 of 272
result for the target analyte must be less than the limit of detection (PFOA LOD = 0.0020 ug/L for waters and 0.50 ug/kg for soils) to 

proceed.

Next an initial calibration verification (ICV) standard is tested. This is a mid-level concentration standard from a different vendor from the 

ICAL standard. If a different vendor is not available then, a different lot number from the same vendor is used. The ICV must be within 

80-120% of the true value.

The quantitation limit verification standard (PFOA LOQ = 0.010 ug/L for water and 2.5 ug/kg for solids) is a standard from the same 

source as the ICAL tested run at the LOQ level to determine accuracy near the detection limit. This recovery must be within 70-130%.

Continuing calibration verification (CCV) standards are tested every 10 injections and are from the same source as the ICAL and are at 

mid-level concentration. The recovery of the CCVs must be 70-130% or recalibration is necessary.

A closing calibration of the seven standards is also done to verify instrument drift and to verify the correlation coefficient. The recoveries 

of the 0.5 standard must be 70-130%, the 2.0 and 20 ug/L standards must be 80-120%.

Method QC Samples

The Method Blank is processed reagent water spiked with internal standard and prepared with each batch of 20 samples of the same 

matrix. All samples in the batch are processed at the same time and with the same reagents. The method blank must be less than the 

LOD or associated batch samples must be re-extracted and reanalyzed.

Each batch is prepared with a low- and a mid-level concentration spike Laboratory Control Samples (LCS). The recoveries of these 

samples must be within 70-130% or associated batch samples must be re-extracted and reanalyzed. If the recovery is biased high and 

samples are non-detect, results can be reported without re-extraction.

Calculations

Sample Result Calculation

For internal standard quantitation,

PFOA Response = Area of PFOA * PFOA 1,2,3,4-13C4 concentration / area of PFOA 1,2,3,4-13C4

Concentration in waters, ug/L = (Cex Vt)/(Vo)

Where:

Cex = Concentration measured in sample extract from the target analyte response (ng/mL)

Vt = Volume of total extract (mL)

Vo = Volume of water extracted (mL)

2. Percent Recovery Calculation

Spike Recovery = (SSR-SR)/(SA)x100%

Where:

SSR = Spike sample result

SR = Sample result

SA = Spike added

3. Relative Percent Difference Calculation

RPD = (SR - DR)/(1/2(SR+DR))x100

Where:

SR = Sample result

DR = Duplicate result

PFOA/APFO Analysis Anomalies

Sample WWK-S-WWM-1(0-.2) (280-21985-1) was analyzed for PFCs by LC/MS/MS in accordance with DV-LC-0012. The sample was 

prepared on 10/31/2011 and analyzed on 11/02/2011.

The MS performed on sample WWK-S-WWM-1(0-.2) (280-21985-1) in prep batch 280-94049 exhibited a surrogate recovery below the 

QC control limits for 13C4 PFOA. The acceptable low- and mid-level LCS analysis data indicated that the analytical system was 

operating within control; therefore, corrective action is deemed unnecessary.

Refer to the QC report for details.

No other difficulties were encountered during the PFC analysis.

All other quality control parameters were within the acceptance limits.

Percent Solids

Sample WWK-S-WWM-1(0-.2) (280-21985-1) was analyzed for percent solids in accordance with EPA SW846 3550C. The sample was 

Page 5 of 272
analyzed on 10/26/2011.

No difficulties were encountered during the % solids analysis.

All quality control parameters were within the acceptance limits.

Page 6 of 272
Lab Name: Job No.:

SDG No.:

LCMS MANUAL INTEGRATION SUMMARY

TestAmerica Denver 280-21985-1

Instrument ID: LC_LCMS5 Analysis Batch Number: 94589

Lab Sample ID: Client Sample ID:

Date Analyzed: Lab File ID:

COMPOUND NAME RETENTION

TIME

MANUAL INTEGRATION

REASON ANALYST DATE

STD0002 280-94589/2 IC

11/02/11 13:49 PC511K02008.d GC Column: Gemini-NX ID:

Ammonium Perfluorooctanoate 

(APFO)

4.45 Baseline bonnettj 11/03/11 10:25

Perfluorooctanoic acid (PFOA) 4.45 Baseline bonnettj 11/03/11 10:25

Lab Sample ID: Client Sample ID:

Date Analyzed: Lab File ID:

COMPOUND NAME RETENTION

TIME

MANUAL INTEGRATION

REASON ANALYST DATE

280-21985-1 WWK-S-WWM-1(0-.2)

11/02/11 15:45 PC511K02023.d GC Column: Gemini-NX ID:

Ammonium Perfluorooctanoate 

(APFO)

4.44 Baseline williamst 11/03/11 14:44

Perfluorooctanoic acid (PFOA) 4.44 Baseline williamst 11/03/11 14:44

Lab Sample ID: Client Sample ID:

Date Analyzed: Lab File ID:

COMPOUND NAME RETENTION

TIME

MANUAL INTEGRATION

REASON ANALYST DATE

280-21985-1 DU WWK-S-WWM-1(0-.2) DU

11/02/11 16:01 PC511K02025.d GC Column: Gemini-NX ID:

Ammonium Perfluorooctanoate 

(APFO)

4.43 Baseline williamst 11/03/11 14:45

Perfluorooctanoic acid (PFOA) 4.43 Baseline williamst 11/03/11 14:45

Lab Sample ID: Client Sample ID:

Date Analyzed: Lab File ID:

COMPOUND NAME RETENTION

TIME

MANUAL INTEGRATION

REASON ANALYST DATE

CCVL 280-94589/22

11/02/11 16:24 PC511K02028.d GC Column: Gemini-NX ID:

Ammonium Perfluorooctanoate 

(APFO)

4.42 Baseline bonnettj 11/03/11 10:27

Perfluorooctanoic acid (PFOA) 4.42 Baseline bonnettj 11/03/11 10:27

DV-LC-0012

Page 7 of 272
SAMPLE SUMMARY

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

Lab Sample ID Client Sample ID Client Matrix Sampled Received

Date/Time Date/Time

280-21985-1 WWK-S-WWM-1(0-.2) Solid 10/24/2011 0728 10/25/2011 0830

280-21985-1MS WWK-S-WWM-1(0-.2) Solid 10/24/2011 0728 10/25/2011 0830

280-21985-1DU WWK-S-WWM-1(0-.2) Solid 10/24/2011 0728 10/25/2011 0830

TestAmerica Denver Page 8 of 272
Executive Summary

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

DV-LC-0012 PFOA and PFOS

Analyte Result (ug/Kg) MDL RL

Individual Final

Lab Sample ID Client Sample ID Result (ug/Kg)

Ammonium 0.69 3.5

Perfluorooctanoate 

(APFO)

280-21985-1 WWK-S-WWM-1(0-.2) ND 1.07

Ammonium 0.70 3.5

Perfluorooctanoate 

(APFO)

280-21985-1 DU WWK-S-WWM-1(0-.2) NQ

Perfluorooctanoic 0.69 3.5

acid (PFOA)

280-21985-1 WWK-S-WWM-1(0-.2) ND 0.983

Perfluorooctanoic 0.70 3.5

acid (PFOA)

280-21985-1 DU WWK-S-WWM-1(0-.2) NQ

Method DEN-LC-0012

DUP or REP indicates a laboratory duplicate.

ND= Compound not detected at or below the detection limit (LOD)

NQ= Compound detected at a level between the LOD and reporting limit (LOQ); result is not quantifiable

(a)

(b)

(c)

Note: ND<LOD<NQ<LOQ

(d) If the sample and laboratory duplicate are both greater than 5X the LOQ and the relative percent difference (RPD) is less than 20, the average

value is reported. If the RPD is greater than 20, the higher of the sample and laboratory duplicate value is reported. If the sample/and or

laboratory duplicate are less than 5X the LOQ, and the absolute difference is less than the LOQ, the average value is reported. If the absolute

difference is greater than the LOQ, the higher of the sample and laboratory duplicate value is reported. If either the sample or the duplicate

 result is greater than or equal to the LOQ and the other is less than the LOQ, then the higher of the two is reported.

(e) Moisture Determined by EPA Method 160.3 MOD

(f)

(g)

Reporting Limit (RL) = LOQ adjusted for actual sample weight. See the case narrative concentration calculation.

LOQ = Limit of Quantitation = 5 times LOD.

Detection Limit (MDL) = LOD adjusted for actual sample weight.

TestAmerica Denver Page 9 of 272
METHOD SUMMARY

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

Description Lab Location Method Preparation Method

Matrix: Solid

PFOA and PFOS TAL DEN TAL-DEN DV-LC-0012

Leaching procedure for PFCs TAL-DEN DV-OP-0019

Percent Moisture TAL DEN ASTM D 2216

Lab References:

TAL DEN = TestAmerica Denver

Method References:

ASTM = ASTM International

TAL-DEN = TestAmerica Laboratories, Denver, Facility Standard Operating Procedure.

TestAmerica Denver Page 10 of 272
METHOD / ANALYST SUMMARY

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

Method Analyst Analyst ID

TAL-DEN DV-LC-0012 Bonnett, Jaqueline C JCB

ASTM D 2216 Berry III, Paul B PBB

TestAmerica Denver

Page 11 of 272
Analytical Data

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

Client Sample ID:

Lab Sample ID:

WWK-S-WWM-1(0-.2)

Client Matrix: % Moisture: 28.1

280-21985-1

Solid

Date Sampled: 10/24/2011 0728

Date Received: 10/25/2011 0830

DV-LC-0012 PFOA and PFOS

Dilution:

10/31/2011 1440

11/02/2011 1545

1.0

DV-LC-0012

Injection Volume:

Final Weight/Volume:

Initial Weight/Volume:

Lab File ID:

Instrument ID:

PC511K02023.d

10.04 g

50 mL

20 uL

DV-OP-0019

LC_LCMS5

Analysis Date:

Prep Date:

Analysis Batch:

Prep Batch:

280-94589

280-94046

Analysis Method:

Prep Method:

Analyte DryWt Corrected: Y Result (ug/Kg) Qualifier MDL RL

Ammonium Perfluorooctanoate (APFO) ND 0.69 3.5

Perfluorooctanoic acid (PFOA) ND 0.69 3.5

Surrogate %Rec Qualifier Acceptance Limits

13C4 PFOA 53 50 - 200

TestAmerica Denver Page 12 of 272
Analytical Data

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

General Chemistry

Client Sample ID:

Lab Sample ID:

WWK-S-WWM-1(0-.2)

Client Matrix:

280-21985-1

Solid

Date Sampled: 10/24/2011 0728

Date Received: 10/25/2011 0830

Analyte Result Qual Units RL RL Dil Method

Percent Moisture 28 % 0.10 0.10 1.0 D 2216

Analysis Batch: 280-93110 Analysis Date: 10/26/2011 0715 DryWt Corrected: N

TestAmerica Denver Page 13 of 272
Quality Control Results

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

Surrogate Recovery Report

DV-LC-0012 PFOA and PFOS

Client Matrix: Solid

Lab Sample ID Client Sample ID

PFOA

%Rec

280-21985-1 WWK-S-WWM-1(0-.2

)

53

MB 280-94046/1-A 92

LCS 280-94046/2-A 91

LLCS 280-94046/3-A 95

280-21985-1 MS WWK-S-WWM-1(0-.2

) MS

49X

280-21985-1 DU WWK-S-WWM-1(0-.2

) DU

51

DLCK 280-94589/13 101

Surrogate Acceptance Limits

PFOA = 13C4 PFOA 50-200

TestAmerica Denver

Page 14 of 272
Quality Control Results

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

Client Matrix: Solid

Dilution: 1.0

Lab Sample ID:

Method Blank - Batch: 280-94046

Instrument ID:

Lab File ID:

Initial Weight/Volume:

Final Weight/Volume:

PC511K02020.d

10.08 g

Units: ug/Kg 50 mL

Method: DV-LC-0012

Preparation: DV-OP-0019

MB 280-94046/1-A LC_LCMS5

Analysis Date: 11/02/2011 1522

Analysis Batch:

Prep Batch:

Leach Batch: N/A

280-94589

280-94046

Prep Date: Injection Volume: 20 uL

Leach Date:

10/31/2011 1440

N/A

Analyte Result Qual MDL RL

Ammonium Perfluorooctanoate (APFO) ND 0.50 2.5

Perfluorooctanoic acid (PFOA) ND 0.50 2.5

Surrogate % Rec Acceptance Limits

13C4 PFOA 92 50 - 200

Solid

1.0

Lab Control Sample - Batch: 280-94046

Client Matrix:

Lab Sample ID:

Dilution:

Instrument ID:

Lab File ID:

Initial Weight/Volume:

Final Weight/Volume:

PC511K02021.d

10.00 g

Units: ug/Kg 50 mL

Method: DV-LC-0012

Preparation: DV-OP-0019

LCS 280-94046/2-A LC_LCMS5

Analysis Date: 11/02/2011 1530

Analysis Batch:

Prep Batch:

Leach Batch:

280-94589

280-94046

N/A

Prep Date: Injection Volume: 20 uL

Leach Date:

10/31/2011 1440

N/A

Analyte Spike Amount Result % Rec. Limit Qual

Ammonium Perfluorooctanoate (APFO) 52.0 58.0 111 70 - 130

Perfluorooctanoic acid (PFOA) 50.0 55.5 111 70 - 130

Surrogate % Rec Acceptance Limits

13C4 PFOA 91 50 - 200

Solid

1.0

Low Level Control Sample - Batch: 280-94046

Client Matrix:

Lab Sample ID:

Dilution:

Instrument ID:

Lab File ID:

Initial Weight/Volume:

Final Weight/Volume:

PC511K02022.d

10.12 g

Units: ug/Kg 50 mL

Method: DV-LC-0012

Preparation: DV-OP-0019

LLCS 280-94046/3-A LC_LCMS5

Analysis Date: 11/02/2011 1538

Analysis Batch:

Prep Batch:

Leach Batch:

280-94589

280-94046

N/A

Prep Date: Injection Volume: 20 uL

Leach Date:

10/31/2011 1440

N/A

Analyte Spike Amount Result % Rec. Limit Qual

Ammonium Perfluorooctanoate (APFO) 5.14 5.73 111 70 - 130

Perfluorooctanoic acid (PFOA) 4.94 5.48 111 70 - 130

Surrogate % Rec Acceptance Limits

13C4 PFOA 95 50 - 200

TestAmerica Denver Page 15 of 272
Quality Control Results

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

Solid

1.0

Matrix Spike - Batch: 280-94046

Lab Sample ID:

Client Matrix:

Dilution:

Instrument ID:

Lab File ID:

Initial Weight/Volume:

Final Weight/Volume:

PC511K02024.d

10.09 g

Units: ug/Kg 50 mL

Method: DV-LC-0012

Preparation: DV-OP-0019

280-21985-1 LC_LCMS5

Analysis Date: 11/02/2011 1553

Analysis Batch: 280-94589

Prep Batch: 280-94046

Leach Batch: N/A

Prep Date: Injection Volume: 20 uL

Leach Date:

10/31/2011 1440

N/A

Analyte Sample Result/Qual Spike Amount Result % Rec. Limit Qual

Ammonium Perfluorooctanoate (APFO) ND 71.7 77.9 109 70 - 130

Perfluorooctanoic acid (PFOA) ND 68.9 75.1 109 70 - 130

Surrogate % Rec Acceptance Limits

13C4 PFOA 49 X 50 - 200

Units: ug/Kg

Solid

Dilution: 1.0

Duplicate - Batch: 280-94046

Lab Sample ID:

Client Matrix:

Instrument ID:

Lab File ID:

Initial Weight/Volume:

Final Weight/Volume:

PC511K02025.d

10.06 g

50 mL

Method: DV-LC-0012

Preparation: DV-OP-0019

280-21985-1 LC_LCMS5

Analysis Date: 11/02/2011 1601

Analysis Batch:

Prep Batch:

Leach Batch:

280-94589

280-94046

N/A

Prep Date: Injection Volume: 20 uL

Leach Date:

10/31/2011 1440

N/A

Analyte Sample Result/Qual Result RPD Limit Qual

Ammonium Perfluorooctanoate (APFO) ND 1.07 NC 20 J

Perfluorooctanoic acid (PFOA) ND 0.983 NC 20 J

Surrogate % Rec Acceptance Limits

13C4 PFOA 51 50 - 200

TestAmerica Denver Page 16 of 272
Quality Control Results

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

Solid

1.0

Detection Limit Check Standard - Batch: 280-94589

Client Matrix:

Lab Sample ID:

Dilution:

Instrument ID:

Lab File ID:

Initial Weight/Volume:

Final Weight/Volume:

PC511K02019.d

1 mL

Units: ug/L

Method: DV-LC-0012

Preparation: N/A

DLCK 280-94589/13 LC_LCMS5

Analysis Date: 11/02/2011 1514

Analysis Batch:

Prep Batch:

Leach Batch:

280-94589

N/A

N/A

Prep Date: Injection Volume: 20 uL

Leach Date:

N/A

N/A

Analyte Spike Amount Result % Rec. Limit Qual

Ammonium Perfluorooctanoate (APFO) 0.520 0.488 94 70 - 130 J

Perfluorooctanoic acid (PFOA) 0.500 0.468 94 70 - 130 J

Surrogate % Rec Acceptance Limits

13C4 PFOA 101 50 - 200

TestAmerica Denver Page 17 of 272
Quality Control Results

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

Units: %

Solid

Dilution: 1.0

Duplicate - Batch: 280-93110

Lab Sample ID:

Client Matrix:

Instrument ID:

Lab File ID:

Initial Weight/Volume:

Final Weight/Volume:

Method: D 2216

Preparation: N/A

N/A

280-21985-1 No Equipment 

Analysis Date: 10/26/2011 0715

Analysis Batch:

Prep Batch:

Leach Batch:

280-93110

N/A

N/A

Prep Date:

Leach Date:

N/A

N/A

Analyte Sample Result/Qual Result RPD Limit Qual

Percent Moisture 28 29 4 20

TestAmerica Denver Page 18 of 272
DATA REPORTING QUALIFIERS

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

Lab Section Qualifier Description

LCMS

Result is less than the RL but greater than or equal to the MDL 

and the concentration is an approximate value.

J

X Surrogate is outside control limits

TestAmerica Denver

Page 19 of 272
Quality Control Results

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

QC Association Summary

Lab Sample ID Client Sample ID Client Matrix Method Prep Batch

Report

Basis

LCMS

Prep Batch: 280-94046

LCS 280-94046/2-A Lab Control Sample T Solid DV-OP-0019

LLCS 280-94046/3-A Low Level Control Sample T Solid DV-OP-0019

MB 280-94046/1-A Method Blank T Solid DV-OP-0019

280-21985-1 WWK-S-WWM-1(0-.2) T Solid DV-OP-0019

280-21985-1DU Duplicate T Solid DV-OP-0019

280-21985-1MS Matrix Spike T Solid DV-OP-0019

Analysis Batch:280-94589

DLCK 280-94589/13 Detection Limit Check Standard T Solid DV-LC-0012

LCS 280-94046/2-A Lab Control Sample T Solid DV-LC-0012 280-94046

LLCS 280-94046/3-A Low Level Control Sample T Solid DV-LC-0012 280-94046

MB 280-94046/1-A Method Blank T Solid DV-LC-0012 280-94046

280-21985-1 WWK-S-WWM-1(0-.2) T Solid DV-LC-0012 280-94046

280-21985-1DU Duplicate T Solid DV-LC-0012 280-94046

280-21985-1MS Matrix Spike T Solid DV-LC-0012 280-94046

Report Basis

T = Total

General Chemistry

Analysis Batch:280-93110

280-21985-1 WWK-S-WWM-1(0-.2) T Solid D 2216

280-21985-1DU Duplicate T Solid D 2216

Report Basis

T = Total

TestAmerica Denver

Page 20 of 272
Quality Control Results

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

Laboratory Chronicle

10/25/2011 08:30

Lab ID:

Method Bottle ID Run

Analysis 

Batch Prep Batch

Date Prepared / 

Analyzed Dil Lab Analyst

Client ID:

Sample Date/Time: 10/24/2011 07:28 Received Date/Time:

280-21985-1 WWK-S-WWM-1(0-.2)

P:DV-OP-0019 280-21985-A-1-A 280-94589 280-94046 10/31/2011 14:40 1 TAL DEN CDC

A:DV-LC-0012 280-21985-A-1-A 280-94589 280-94046 11/02/2011 15:45 1 TAL DEN JCB

A:D 2216 280-21985-B-1 280-93110 10/26/2011 07:15 1 TAL DEN PBB

10/25/2011 08:30

Lab ID:

Method Bottle ID Run

Analysis 

Batch Prep Batch

Date Prepared / 

Analyzed Dil Lab Analyst

Client ID:

Sample Date/Time: 10/24/2011 07:28 Received Date/Time:

280-21985-1 WWK-S-WWM-1(0-.2)

P:DV-OP-0019 280-21985-A-1-B MS 280-94589 280-94046 10/31/2011 14:40 1 TAL DEN CDC

A:DV-LC-0012 280-21985-A-1-B MS 280-94589 280-94046 11/02/2011 15:53 1 TAL DEN JCB

10/25/2011 08:30

Lab ID:

Method Bottle ID Run

Analysis 

Batch Prep Batch

Date Prepared / 

Analyzed Dil Lab Analyst

Client ID:

Sample Date/Time: 10/24/2011 07:28 Received Date/Time:

280-21985-1 WWK-S-WWM-1(0-.2)

P:DV-OP-0019 280-21985-A-1-C DU 280-94589 280-94046 10/31/2011 14:40 1 TAL DEN CDC

A:DV-LC-0012 280-21985-A-1-C DU 280-94589 280-94046 11/02/2011 16:01 1 TAL DEN JCB

A:D 2216 280-21985-B-1 DU 280-93110 10/26/2011 07:15 1 TAL DEN PBB

Lab ID:

Method Bottle ID Run

Analysis 

Batch Prep Batch

Date Prepared / 

Analyzed Dil Lab Analyst

Client ID:

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

MB N/A

P:DV-OP-0019 MB 280-94046/1-A 280-94589 280-94046 10/31/2011 14:40 1 TAL DEN CDC

A:DV-LC-0012 MB 280-94046/1-A 280-94589 280-94046 11/02/2011 15:22 1 TAL DEN JCB

Lab ID:

Method Bottle ID Run

Analysis 

Batch Prep Batch

Date Prepared / 

Analyzed Dil Lab Analyst

Client ID:

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

LCS N/A

P:DV-OP-0019 LCS 280-94046/2-A 280-94589 280-94046 10/31/2011 14:40 1 TAL DEN CDC

A:DV-LC-0012 LCS 280-94046/2-A 280-94589 280-94046 11/02/2011 15:30 1 TAL DEN JCB

Lab ID:

Method Bottle ID Run

Analysis 

Batch Prep Batch

Date Prepared / 

Analyzed Dil Lab Analyst

Client ID:

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

LLCS N/A

P:DV-OP-0019 LLCS 280-94046/3-A 280-94589 280-94046 10/31/2011 14:40 1 TAL DEN CDC

A:DV-LC-0012 LLCS 280-94046/3-A 280-94589 280-94046 11/02/2011 15:38 1 TAL DEN JCB

TestAmerica Denver A = Analytical Method P = Prep Method 

Page 21 of 272
Quality Control Results

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

Laboratory Chronicle

Lab ID:

Method Bottle ID Run

Analysis 

Batch Prep Batch

Date Prepared / 

Analyzed Dil Lab Analyst

Client ID:

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

DLCK N/A

A:DV-LC-0012 DLCK 280-94589/13 280-94589 11/02/2011 15:14 1 TAL DEN JCB

Lab References:

TAL DEN = TestAmerica Denver

TestAmerica Denver A = Analytical Method P = Prep Method 

Page 22 of 272
REAGENT TRACEABILITY SUMMARY

Lab Name:

SDG No.:

TestAmerica Denver Job No.: 280-21985-1

Reagent ID

Exp

Date Date

Prep Dilutant

Used

Reagent

Final

Volume

Parent Reagent

Reagent ID

Volume

Added Analyte Concentration

PFOA/S-Cal0_00037 11/16/11 11/02/11 80:20 Methanol : H2O, 1 mL PFOA/S-IS_LC_00003 20 uL 13C4 PFOA 10 ug/L

Lot J29E57:K02E01

13C4 PFOS 9.56 ug/L

.PFOA/S-IS_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C4PFOAStock_00013 0.1 mL 13C4 PFOA 0.5 ug/mL

13C4PFOSStock_00013 0.1 mL 13C4 PFOS 0.478 ug/mL

..13C4PFOAStock_00013 06/22/13 Wellington, Lot MPFOA0610 (Purchased Reagent) 13C4 PFOA 50 ug/mL

..13C4PFOSStock_00013 09/08/13 Wellington, Lot MPFOS0910 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL

PFOA/S-Cal1_00035 11/16/11 11/02/11 80:20 Methanol : H2O, 1 mL PFOA/S-IS_LC_00003 20 uL 13C4 PFOA 10 ug/L

Lot J29E57:K02E01

13C4 PFOA (IS) 10 ug/L

13C4 PFOS 9.56 ug/L

13C4 PFOS (IS) 9.56 ug/L

Ammonium Perfluorooctanoate 

(APFO)

PFOA/S_CALwSk_00013 10 uL 0.20812 ug/L

Perfluorooctanoic acid (PFOA) 0.2 ug/L

Perfluorooctanoic Sulfonate 0.1912 ug/L

13C8 PFOA 0.2 ug/L

13C8 PFOS 0.1912 ug/L

.PFOA/S-IS_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C4PFOAStock_00013 0.1 mL 13C4 PFOA 0.5 ug/mL

13C4 PFOA (IS) 0.5 ug/mL

13C4PFOSStock_00013 0.1 mL 13C4 PFOS 0.478 ug/mL

13C4 PFOS (IS) 0.478 ug/mL

..13C4PFOAStock_00013 06/22/13 Wellington, Lot MPFOA0610 (Purchased Reagent) 13C4 PFOA 50 ug/mL

13C4 PFOA (IS) 50 ug/mL

..13C4PFOSStock_00013 09/08/13 Wellington, Lot MPFOS0910 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL

13C4 PFOS (IS) 47.8 ug/mL

PFOA/S_Spike_00004 Ammonium Perfluorooctanoate 

(APFO)

.PFOA/S_CALwSk_00013 11/02/11 07/03/11 80:20 Methanol : H2O, 10 mL 0.4 mL 20.812 ug/L

Lot J29E57:K02E01

Perfluorooctanoic acid (PFOA) 20 ug/L

Perfluorooctanoic Sulfonate 19.12 ug/L

PFOA/S_Sur_LC_00003 0.4 mL 13C8 PFOA 20 ug/L

13C8 PFOS 19.12 ug/L

PFOA-stock_00002 Ammonium Perfluorooctanoate 

(APFO)

..PFOA/S_Spike_00004 11/02/11 11/02/10 Methanol, Lot J29E57 100 mL 1 mL 0.5203 ug/mL

Perfluorooctanoic acid (PFOA) 0.5 ug/mL

PFOS-Stock_00002 1 mL Perfluorooctanoic Sulfonate 0.478 ug/mL

06/01/12 (Purchased Reagent) Ammonium Perfluorooctanoate 

(APFO)

...PFOA-stock_00002 Wellington, Lot PFOA0609 52.03 ug/mL

Perfluorooctanoic acid (PFOA) 50 ug/mL

...PFOS-Stock_00002 05/05/12 Wellington, Lot LPFOS0409 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL

..PFOA/S_Sur_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C8PFOA-stk_00006 0.1 mL 13C8 PFOA 0.5 ug/mL

13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL

...13C8PFOA-stk_00006 01/29/13 Wellington Laboratories, Lot M8PFOA0110 (Purchased Reagent) 13C8 PFOA 50 ug/mL

...13C8PFOS-stk_00006 05/06/13 Wellington Laboratories, Lot M8PFOS0510 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL

PFOA/S-Cal2_00034 11/02/11 11/02/11 80:20 Methanol : H2O, 1 mL PFOA/S-IS_LC_00003 20 uL 13C4 PFOA 10 ug/L

Lot J29E57:K02E01

13C4 PFOA (IS) 10 ug/L

13C4 PFOS 9.56 ug/L

13C4 PFOS (IS) 9.56 ug/L

Page 23 of 272
REAGENT TRACEABILITY SUMMARY

Lab Name:

SDG No.:

TestAmerica Denver Job No.: 280-21985-1

Reagent ID

Exp

Date Date

Prep Dilutant

Used

Reagent

Final

Volume

Parent Reagent

Reagent ID

Volume

Added Analyte Concentration

Ammonium Perfluorooctanoate 

(APFO)

PFOA/S_CALwSk_00013 25 uL 0.5203 ug/L

Perfluorooctanoic acid (PFOA) 0.5 ug/L

Perfluorooctanoic Sulfonate 0.478 ug/L

13C8 PFOA 0.5 ug/L

13C8 PFOS 0.478 ug/L

.PFOA/S-IS_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C4PFOAStock_00013 0.1 mL 13C4 PFOA 0.5 ug/mL

13C4 PFOA (IS) 0.5 ug/mL

13C4PFOSStock_00013 0.1 mL 13C4 PFOS 0.478 ug/mL

13C4 PFOS (IS) 0.478 ug/mL

..13C4PFOAStock_00013 06/22/13 Wellington, Lot MPFOA0610 (Purchased Reagent) 13C4 PFOA 50 ug/mL

13C4 PFOA (IS) 50 ug/mL

..13C4PFOSStock_00013 09/08/13 Wellington, Lot MPFOS0910 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL

13C4 PFOS (IS) 47.8 ug/mL

PFOA/S_Spike_00004 Ammonium Perfluorooctanoate 

(APFO)

.PFOA/S_CALwSk_00013 11/02/11 07/03/11 80:20 Methanol : H2O, 10 mL 0.4 mL 20.812 ug/L

Lot J29E57:K02E01

Perfluorooctanoic acid (PFOA) 20 ug/L

Perfluorooctanoic Sulfonate 19.12 ug/L

PFOA/S_Sur_LC_00003 0.4 mL 13C8 PFOA 20 ug/L

13C8 PFOS 19.12 ug/L

PFOA-stock_00002 Ammonium Perfluorooctanoate 

(APFO)

..PFOA/S_Spike_00004 11/02/11 11/02/10 Methanol, Lot J29E57 100 mL 1 mL 0.5203 ug/mL

Perfluorooctanoic acid (PFOA) 0.5 ug/mL

PFOS-Stock_00002 1 mL Perfluorooctanoic Sulfonate 0.478 ug/mL

06/01/12 (Purchased Reagent) Ammonium Perfluorooctanoate 

(APFO)

...PFOA-stock_00002 Wellington, Lot PFOA0609 52.03 ug/mL

Perfluorooctanoic acid (PFOA) 50 ug/mL

...PFOS-Stock_00002 05/05/12 Wellington, Lot LPFOS0409 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL

..PFOA/S_Sur_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C8PFOA-stk_00006 0.1 mL 13C8 PFOA 0.5 ug/mL

13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL

...13C8PFOA-stk_00006 01/29/13 Wellington Laboratories, Lot M8PFOA0110 (Purchased Reagent) 13C8 PFOA 50 ug/mL

...13C8PFOS-stk_00006 05/06/13 Wellington Laboratories, Lot M8PFOS0510 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL

PFOA/S-Cal3_00034 11/02/11 11/02/11 80:20 Methanol : H2O, 1 mL PFOA/S-IS_LC_00003 20 uL 13C4 PFOA 10 ug/L

Lot J29E57:K02E01

13C4 PFOA (IS) 10 ug/L

13C4 PFOS 9.56 ug/L

13C4 PFOS (IS) 9.56 ug/L

Ammonium Perfluorooctanoate 

(APFO)

PFOA/S_CALwSk_00013 50 uL 1.0406 ug/L

Perfluorooctanoic acid (PFOA) 1 ug/L

Perfluorooctanoic Sulfonate 0.956 ug/L

13C8 PFOA 1 ug/L

13C8 PFOS 0.956 ug/L

.PFOA/S-IS_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C4PFOAStock_00013 0.1 mL 13C4 PFOA 0.5 ug/mL

13C4 PFOA (IS) 0.5 ug/mL

13C4PFOSStock_00013 0.1 mL 13C4 PFOS 0.478 ug/mL

13C4 PFOS (IS) 0.478 ug/mL

..13C4PFOAStock_00013 06/22/13 Wellington, Lot MPFOA0610 (Purchased Reagent) 13C4 PFOA 50 ug/mL

13C4 PFOA (IS) 50 ug/mL

..13C4PFOSStock_00013 09/08/13 Wellington, Lot MPFOS0910 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL

13C4 PFOS (IS) 47.8 ug/mL Page 24 of 272
REAGENT TRACEABILITY SUMMARY

Lab Name:

SDG No.:

TestAmerica Denver Job No.: 280-21985-1

Reagent ID

Exp

Date Date

Prep Dilutant

Used

Reagent

Final

Volume

Parent Reagent

Reagent ID

Volume

Added Analyte Concentration

PFOA/S_Spike_00004 Ammonium Perfluorooctanoate 

(APFO)

.PFOA/S_CALwSk_00013 11/02/11 07/03/11 80:20 Methanol : H2O, 10 mL 0.4 mL 20.812 ug/L

Lot J29E57:K02E01

Perfluorooctanoic acid (PFOA) 20 ug/L

Perfluorooctanoic Sulfonate 19.12 ug/L

PFOA/S_Sur_LC_00003 0.4 mL 13C8 PFOA 20 ug/L

13C8 PFOS 19.12 ug/L

PFOA-stock_00002 Ammonium Perfluorooctanoate 

(APFO)

..PFOA/S_Spike_00004 11/02/11 11/02/10 Methanol, Lot J29E57 100 mL 1 mL 0.5203 ug/mL

Perfluorooctanoic acid (PFOA) 0.5 ug/mL

PFOS-Stock_00002 1 mL Perfluorooctanoic Sulfonate 0.478 ug/mL

06/01/12 (Purchased Reagent) Ammonium Perfluorooctanoate 

(APFO)

...PFOA-stock_00002 Wellington, Lot PFOA0609 52.03 ug/mL

Perfluorooctanoic acid (PFOA) 50 ug/mL

...PFOS-Stock_00002 05/05/12 Wellington, Lot LPFOS0409 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL

..PFOA/S_Sur_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C8PFOA-stk_00006 0.1 mL 13C8 PFOA 0.5 ug/mL

13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL

...13C8PFOA-stk_00006 01/29/13 Wellington Laboratories, Lot M8PFOA0110 (Purchased Reagent) 13C8 PFOA 50 ug/mL

...13C8PFOS-stk_00006 05/06/13 Wellington Laboratories, Lot M8PFOS0510 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL

PFOA/S-Cal4_00035 11/02/11 11/02/11 80:20 Methanol : H2O, 1 mL PFOA/S-IS_LC_00003 20 uL 13C4 PFOA 10 ug/L

Lot J29E57:K02E01

13C4 PFOA (IS) 10 ug/L

13C4 PFOS 9.56 ug/L

13C4 PFOS (IS) 9.56 ug/L

Ammonium Perfluorooctanoate 

(APFO)

PFOA/S_CALwSk_00013 100 uL 2.0812 ug/L

Perfluorooctanoic acid (PFOA) 2 ug/L

Perfluorooctanoic Sulfonate 1.912 ug/L

13C8 PFOA 2 ug/L

13C8 PFOS 1.912 ug/L

.PFOA/S-IS_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C4PFOAStock_00013 0.1 mL 13C4 PFOA 0.5 ug/mL

13C4 PFOA (IS) 0.5 ug/mL

13C4PFOSStock_00013 0.1 mL 13C4 PFOS 0.478 ug/mL

13C4 PFOS (IS) 0.478 ug/mL

..13C4PFOAStock_00013 06/22/13 Wellington, Lot MPFOA0610 (Purchased Reagent) 13C4 PFOA 50 ug/mL

13C4 PFOA (IS) 50 ug/mL

..13C4PFOSStock_00013 09/08/13 Wellington, Lot MPFOS0910 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL

13C4 PFOS (IS) 47.8 ug/mL

PFOA/S_Spike_00004 Ammonium Perfluorooctanoate 

(APFO)

.PFOA/S_CALwSk_00013 11/02/11 07/03/11 80:20 Methanol : H2O, 10 mL 0.4 mL 20.812 ug/L

Lot J29E57:K02E01

Perfluorooctanoic acid (PFOA) 20 ug/L

Perfluorooctanoic Sulfonate 19.12 ug/L

PFOA/S_Sur_LC_00003 0.4 mL 13C8 PFOA 20 ug/L

13C8 PFOS 19.12 ug/L

PFOA-stock_00002 Ammonium Perfluorooctanoate 

(APFO)

..PFOA/S_Spike_00004 11/02/11 11/02/10 Methanol, Lot J29E57 100 mL 1 mL 0.5203 ug/mL

Perfluorooctanoic acid (PFOA) 0.5 ug/mL

PFOS-Stock_00002 1 mL Perfluorooctanoic Sulfonate 0.478 ug/mL

06/01/12 (Purchased Reagent) Ammonium Perfluorooctanoate 

(APFO)

...PFOA-stock_00002 Wellington, Lot PFOA0609 52.03 ug/mL

Perfluorooctanoic acid (PFOA) 50 ug/mL

...PFOS-Stock_00002 05/05/12 Wellington, Lot LPFOS0409Page 25 of 272(Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL
REAGENT TRACEABILITY SUMMARY

Lab Name:

SDG No.:

TestAmerica Denver Job No.: 280-21985-1

Reagent ID

Exp

Date Date

Prep Dilutant

Used

Reagent

Final

Volume

Parent Reagent

Reagent ID

Volume

Added Analyte Concentration

..PFOA/S_Sur_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C8PFOA-stk_00006 0.1 mL 13C8 PFOA 0.5 ug/mL

13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL

...13C8PFOA-stk_00006 01/29/13 Wellington Laboratories, Lot M8PFOA0110 (Purchased Reagent) 13C8 PFOA 50 ug/mL

...13C8PFOS-stk_00006 05/06/13 Wellington Laboratories, Lot M8PFOS0510 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL

PFOA/S-Cal5_00035 11/02/11 11/02/11 80:20 Methanol : H2O, 1 mL PFOA/S-IS_LC_00003 20 uL 13C4 PFOA 10 ug/L

Lot J29E57:K02E01

13C4 PFOA (IS) 10 ug/L

13C4 PFOS 9.56 ug/L

13C4 PFOS (IS) 9.56 ug/L

Ammonium Perfluorooctanoate 

(APFO)

PFOA/S_CALwSk_00013 250 uL 5.203 ug/L

Perfluorooctanoic acid (PFOA) 5 ug/L

Perfluorooctanoic Sulfonate 4.78 ug/L

13C8 PFOA 5 ug/L

13C8 PFOS 4.78 ug/L

.PFOA/S-IS_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C4PFOAStock_00013 0.1 mL 13C4 PFOA 0.5 ug/mL

13C4 PFOA (IS) 0.5 ug/mL

13C4PFOSStock_00013 0.1 mL 13C4 PFOS 0.478 ug/mL

13C4 PFOS (IS) 0.478 ug/mL

..13C4PFOAStock_00013 06/22/13 Wellington, Lot MPFOA0610 (Purchased Reagent) 13C4 PFOA 50 ug/mL

13C4 PFOA (IS) 50 ug/mL

..13C4PFOSStock_00013 09/08/13 Wellington, Lot MPFOS0910 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL

13C4 PFOS (IS) 47.8 ug/mL

PFOA/S_Spike_00004 Ammonium Perfluorooctanoate 

(APFO)

.PFOA/S_CALwSk_00013 11/02/11 07/03/11 80:20 Methanol : H2O, 10 mL 0.4 mL 20.812 ug/L

Lot J29E57:K02E01

Perfluorooctanoic acid (PFOA) 20 ug/L

Perfluorooctanoic Sulfonate 19.12 ug/L

PFOA/S_Sur_LC_00003 0.4 mL 13C8 PFOA 20 ug/L

13C8 PFOS 19.12 ug/L

PFOA-stock_00002 Ammonium Perfluorooctanoate 

(APFO)

..PFOA/S_Spike_00004 11/02/11 11/02/10 Methanol, Lot J29E57 100 mL 1 mL 0.5203 ug/mL

Perfluorooctanoic acid (PFOA) 0.5 ug/mL

PFOS-Stock_00002 1 mL Perfluorooctanoic Sulfonate 0.478 ug/mL

06/01/12 (Purchased Reagent) Ammonium Perfluorooctanoate 

(APFO)

...PFOA-stock_00002 Wellington, Lot PFOA0609 52.03 ug/mL

Perfluorooctanoic acid (PFOA) 50 ug/mL

...PFOS-Stock_00002 05/05/12 Wellington, Lot LPFOS0409 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL

..PFOA/S_Sur_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C8PFOA-stk_00006 0.1 mL 13C8 PFOA 0.5 ug/mL

13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL

...13C8PFOA-stk_00006 01/29/13 Wellington Laboratories, Lot M8PFOA0110 (Purchased Reagent) 13C8 PFOA 50 ug/mL

...13C8PFOS-stk_00006 05/06/13 Wellington Laboratories, Lot M8PFOS0510 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL

PFOA/S-Cal6_00037 11/02/11 11/02/11 80:20 Methanol : H2O, 1 mL PFOA/S-IS_LC_00003 20 uL 13C4 PFOA 10 ug/L

Lot J29E57:K02E01

13C4 PFOA (IS) 10 ug/L

13C4 PFOS 9.56 ug/L

13C4 PFOS (IS) 9.56 ug/L

Ammonium Perfluorooctanoate 

(APFO)

PFOA/S_CALwSk_00013 500 uL 10.406 ug/L

Perfluorooctanoic acid (PFOA) 10 ug/L

Page 26 of 272 Perfluorooctanoic Sulfonate 9.56 ug/L
REAGENT TRACEABILITY SUMMARY

Lab Name:

SDG No.:

TestAmerica Denver Job No.: 280-21985-1

Reagent ID

Exp

Date Date

Prep Dilutant

Used

Reagent

Final

Volume

Parent Reagent

Reagent ID

Volume

Added Analyte Concentration

13C8 PFOA 10 ug/L

13C8 PFOS 9.56 ug/L

.PFOA/S-IS_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C4PFOAStock_00013 0.1 mL 13C4 PFOA 0.5 ug/mL

13C4 PFOA (IS) 0.5 ug/mL

13C4PFOSStock_00013 0.1 mL 13C4 PFOS 0.478 ug/mL

13C4 PFOS (IS) 0.478 ug/mL

..13C4PFOAStock_00013 06/22/13 Wellington, Lot MPFOA0610 (Purchased Reagent) 13C4 PFOA 50 ug/mL

13C4 PFOA (IS) 50 ug/mL

..13C4PFOSStock_00013 09/08/13 Wellington, Lot MPFOS0910 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL

13C4 PFOS (IS) 47.8 ug/mL

PFOA/S_Spike_00004 Ammonium Perfluorooctanoate 

(APFO)

.PFOA/S_CALwSk_00013 11/02/11 07/03/11 80:20 Methanol : H2O, 10 mL 0.4 mL 20.812 ug/L

Lot J29E57:K02E01

Perfluorooctanoic acid (PFOA) 20 ug/L

Perfluorooctanoic Sulfonate 19.12 ug/L

PFOA/S_Sur_LC_00003 0.4 mL 13C8 PFOA 20 ug/L

13C8 PFOS 19.12 ug/L

PFOA-stock_00002 Ammonium Perfluorooctanoate 

(APFO)

..PFOA/S_Spike_00004 11/02/11 11/02/10 Methanol, Lot J29E57 100 mL 1 mL 0.5203 ug/mL

Perfluorooctanoic acid (PFOA) 0.5 ug/mL

PFOS-Stock_00002 1 mL Perfluorooctanoic Sulfonate 0.478 ug/mL

06/01/12 (Purchased Reagent) Ammonium Perfluorooctanoate 

(APFO)

...PFOA-stock_00002 Wellington, Lot PFOA0609 52.03 ug/mL

Perfluorooctanoic acid (PFOA) 50 ug/mL

...PFOS-Stock_00002 05/05/12 Wellington, Lot LPFOS0409 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL

..PFOA/S_Sur_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C8PFOA-stk_00006 0.1 mL 13C8 PFOA 0.5 ug/mL

13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL

...13C8PFOA-stk_00006 01/29/13 Wellington Laboratories, Lot M8PFOA0110 (Purchased Reagent) 13C8 PFOA 50 ug/mL

...13C8PFOS-stk_00006 05/06/13 Wellington Laboratories, Lot M8PFOS0510 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL

PFOA/S-Cal7_00034 11/02/11 11/02/11 80:20 Methanol : H2O, 1 mL PFOA/S-IS_LC_00003 20 uL 13C4 PFOA 10 ug/L

Lot J29E57:K02E01

13C4 PFOA (IS) 10 ug/L

13C4 PFOS 9.56 ug/L

13C4 PFOS (IS) 9.56 ug/L

Ammonium Perfluorooctanoate 

(APFO)

PFOA/S_Spike_00004 40 uL 20.812 ug/L

Perfluorooctanoic acid (PFOA) 20 ug/L

Perfluorooctanoic Sulfonate 19.12 ug/L

PFOA/S_Sur_LC_00003 40 uL 13C8 PFOA 20 ug/L

13C8 PFOS 19.12 ug/L

.PFOA/S-IS_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C4PFOAStock_00013 0.1 mL 13C4 PFOA 0.5 ug/mL

13C4 PFOA (IS) 0.5 ug/mL

13C4PFOSStock_00013 0.1 mL 13C4 PFOS 0.478 ug/mL

13C4 PFOS (IS) 0.478 ug/mL

..13C4PFOAStock_00013 06/22/13 Wellington, Lot MPFOA0610 (Purchased Reagent) 13C4 PFOA 50 ug/mL

13C4 PFOA (IS) 50 ug/mL

..13C4PFOSStock_00013 09/08/13 Wellington, Lot MPFOS0910 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL

13C4 PFOS (IS) 47.8 ug/mL

PFOA-stock_00002 Ammonium Perfluorooctanoate 

(APFO)

.PFOA/S_Spike_00004 11/02/11 11/02/10 Methanol, Lot J29E57 100 mL 1 mL 0.5203 ug/mL

Perfluorooctanoic acid (PFOA) 0.5 ug/mL

PFOS-Stock_00002 1 mL Perfluorooctanoic Sulfonate 0.478 ug/mL Page 27 of 272
REAGENT TRACEABILITY SUMMARY

Lab Name:

SDG No.:

TestAmerica Denver Job No.: 280-21985-1

Reagent ID

Exp

Date Date

Prep Dilutant

Used

Reagent

Final

Volume

Parent Reagent

Reagent ID

Volume

Added Analyte Concentration

06/01/12 (Purchased Reagent) Ammonium Perfluorooctanoate 

(APFO)

..PFOA-stock_00002 Wellington, Lot PFOA0609 52.03 ug/mL

Perfluorooctanoic acid (PFOA) 50 ug/mL

..PFOS-Stock_00002 05/05/12 Wellington, Lot LPFOS0409 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL

.PFOA/S_Sur_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C8PFOA-stk_00006 0.1 mL 13C8 PFOA 0.5 ug/mL

13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL

..13C8PFOA-stk_00006 01/29/13 Wellington Laboratories, Lot M8PFOA0110 (Purchased Reagent) 13C8 PFOA 50 ug/mL

..13C8PFOS-stk_00006 05/06/13 Wellington Laboratories, Lot M8PFOS0510 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL

PFOA/S-Cal8_00022 11/02/11 11/02/11 80:20 Methanol : H2O, 1 mL PFOA/S-IS_LC_00003 20 uL 13C4 PFOA 10 ug/L

Lot J29E57:K02E01

13C4 PFOA (IS) 10 ug/L

13C4 PFOS 9.56 ug/L

13C4 PFOS (IS) 9.56 ug/L

Ammonium Perfluorooctanoate 

(APFO)

PFOA/S_Spike_00004 100 uL 52.03 ug/L

Perfluorooctanoic acid (PFOA) 50 ug/L

Perfluorooctanoic Sulfonate 47.8 ug/L

PFOA/S_Sur_LC_00003 100 uL 13C8 PFOA 50 ug/L

13C8 PFOS 47.8 ug/L

.PFOA/S-IS_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C4PFOAStock_00013 0.1 mL 13C4 PFOA 0.5 ug/mL

13C4 PFOA (IS) 0.5 ug/mL

13C4PFOSStock_00013 0.1 mL 13C4 PFOS 0.478 ug/mL

13C4 PFOS (IS) 0.478 ug/mL

..13C4PFOAStock_00013 06/22/13 Wellington, Lot MPFOA0610 (Purchased Reagent) 13C4 PFOA 50 ug/mL

13C4 PFOA (IS) 50 ug/mL

..13C4PFOSStock_00013 09/08/13 Wellington, Lot MPFOS0910 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL

13C4 PFOS (IS) 47.8 ug/mL

PFOA-stock_00002 Ammonium Perfluorooctanoate 

(APFO)

.PFOA/S_Spike_00004 11/02/11 11/02/10 Methanol, Lot J29E57 100 mL 1 mL 0.5203 ug/mL

Perfluorooctanoic acid (PFOA) 0.5 ug/mL

PFOS-Stock_00002 1 mL Perfluorooctanoic Sulfonate 0.478 ug/mL

06/01/12 (Purchased Reagent) Ammonium Perfluorooctanoate 

(APFO)

..PFOA-stock_00002 Wellington, Lot PFOA0609 52.03 ug/mL

Perfluorooctanoic acid (PFOA) 50 ug/mL

..PFOS-Stock_00002 05/05/12 Wellington, Lot LPFOS0409 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL

.PFOA/S_Sur_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C8PFOA-stk_00006 0.1 mL 13C8 PFOA 0.5 ug/mL

13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL

..13C8PFOA-stk_00006 01/29/13 Wellington Laboratories, Lot M8PFOA0110 (Purchased Reagent) 13C8 PFOA 50 ug/mL

..13C8PFOS-stk_00006 05/06/13 Wellington Laboratories, Lot M8PFOS0510 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL

PFOA/S-Cal9_00022 11/02/11 11/02/11 80:20 Methanol : H2O, 1 mL PFOA/S-IS_LC_00003 20 uL 13C4 PFOA 10 ug/L

Lot J29E57:K02E01

13C4 PFOA (IS) 10 ug/L

13C4 PFOS 9.56 ug/L

13C4 PFOS (IS) 9.56 ug/L

Ammonium Perfluorooctanoate 

(APFO)

PFOA/S_Spike_00004 250 uL 130.075 ug/L

Perfluorooctanoic acid (PFOA) 125 ug/L

Perfluorooctanoic Sulfonate 119.5 ug/L

PFOA/S_Sur_LC_00003 250 uL 13C8 PFOA 125 ug/L

Page 28 of 272 13C8 PFOS 119.5 ug/L
REAGENT TRACEABILITY SUMMARY

Lab Name:

SDG No.:

TestAmerica Denver Job No.: 280-21985-1

Reagent ID

Exp

Date Date

Prep Dilutant

Used

Reagent

Final

Volume

Parent Reagent

Reagent ID

Volume

Added Analyte Concentration

.PFOA/S-IS_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C4PFOAStock_00013 0.1 mL 13C4 PFOA 0.5 ug/mL

13C4 PFOA (IS) 0.5 ug/mL

13C4PFOSStock_00013 0.1 mL 13C4 PFOS 0.478 ug/mL

13C4 PFOS (IS) 0.478 ug/mL

..13C4PFOAStock_00013 06/22/13 Wellington, Lot MPFOA0610 (Purchased Reagent) 13C4 PFOA 50 ug/mL

13C4 PFOA (IS) 50 ug/mL

..13C4PFOSStock_00013 09/08/13 Wellington, Lot MPFOS0910 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL

13C4 PFOS (IS) 47.8 ug/mL

PFOA-stock_00002 Ammonium Perfluorooctanoate 

(APFO)

.PFOA/S_Spike_00004 11/02/11 11/02/10 Methanol, Lot J29E57 100 mL 1 mL 0.5203 ug/mL

Perfluorooctanoic acid (PFOA) 0.5 ug/mL

PFOS-Stock_00002 1 mL Perfluorooctanoic Sulfonate 0.478 ug/mL

06/01/12 (Purchased Reagent) Ammonium Perfluorooctanoate 

(APFO)

..PFOA-stock_00002 Wellington, Lot PFOA0609 52.03 ug/mL

Perfluorooctanoic acid (PFOA) 50 ug/mL

..PFOS-Stock_00002 05/05/12 Wellington, Lot LPFOS0409 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL

.PFOA/S_Sur_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C8PFOA-stk_00006 0.1 mL 13C8 PFOA 0.5 ug/mL

13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL

..13C8PFOA-stk_00006 01/29/13 Wellington Laboratories, Lot M8PFOA0110 (Purchased Reagent) 13C8 PFOA 50 ug/mL

..13C8PFOS-stk_00006 05/06/13 Wellington Laboratories, Lot M8PFOS0510 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL

PFOA/S-CALicv_00034 11/16/11 11/02/11 80:20 Methanol : H2O, 1 mL PFOA/S-IS_LC_00003 20 uL 13C4 PFOA 10 ug/L

Lot J29E57:K02E01

13C4 PFOS 9.56 ug/L

Ammonium Perfluorooctanoate 

(APFO)

PFOA/S_ICVWSk_00006 100 uL 2.0812 ug/L

Perfluorooctanoic acid (PFOA) 2 ug/L

13C8 PFOA 2 ug/L

13C8 PFOS 1.912 ug/L

.PFOA/S-IS_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C4PFOAStock_00013 0.1 mL 13C4 PFOA 0.5 ug/mL

13C4PFOSStock_00013 0.1 mL 13C4 PFOS 0.478 ug/mL

..13C4PFOAStock_00013 06/22/13 Wellington, Lot MPFOA0610 (Purchased Reagent) 13C4 PFOA 50 ug/mL

..13C4PFOSStock_00013 09/08/13 Wellington, Lot MPFOS0910 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL

PFOA/S_ICVStk_00003 Ammonium Perfluorooctanoate 

(APFO)

.PFOA/S_ICVWSk_00006 04/18/12 07/03/11 80:20 Methanol : H2O, 10 mL 0.2 mL 20.812 ug/L

Lot J57E02

Perfluorooctanoic acid (PFOA) 20 ug/L

PFOA/S_Sur_LC_00003 0.4 mL 13C8 PFOA 20 ug/L

13C8 PFOS 19.12 ug/L

PFOA_ICVStk_00003 Ammonium Perfluorooctanoate 

(APFO)

..PFOA/S_ICVStk_00003 07/03/12 07/03/11 Methanol, Lot 5.76.1 10 mL 0.1 mL 1040.6 ug/L

Perfluorooctanoic acid (PFOA) 1000 ug/L

11/02/20 (Purchased Reagent) Ammonium Perfluorooctanoate 

(APFO)

...PFOA_ICVStk_00003 Accustandard, Lot 210041455-01 104.06 ug/mL

Perfluorooctanoic acid (PFOA) 100 ug/mL

..PFOA/S_Sur_LC_00003 04/18/12 04/19/11 Methanol, Lot J29E57 10 mL 13C8PFOA-stk_00006 0.1 mL 13C8 PFOA 0.5 ug/mL

13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL

...13C8PFOA-stk_00006 01/29/13 Wellington Laboratories, Lot M8PFOA0110 (Purchased Reagent) 13C8 PFOA 50 ug/mL

...13C8PFOS-stk_00006 05/06/13 Wellington Laboratories, Lot M8PFOS0510 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL

PFOA-stock_00002 Ammonium Perfluorooctanoate 

(APFO)

PFOA/S_Spike_00004 11/02/11 11/02/10 Methanol, Lot J29E57 100 mL 1 mL 0.5203 ug/mL

Perfluorooctanoic acid (PFOA) 0.5 ug/mL Page 29 of 272
REAGENT TRACEABILITY SUMMARY

Lab Name:

SDG No.:

TestAmerica Denver Job No.: 280-21985-1

Reagent ID

Exp

Date Date

Prep Dilutant

Used

Reagent

Final

Volume

Parent Reagent

Reagent ID

Volume

Added Analyte Concentration

PFOS-Stock_00002 1 mL Perfluorooctanoic Sulfonate 0.478 ug/mL

06/01/12 (Purchased Reagent) Ammonium Perfluorooctanoate 

(APFO)

.PFOA-stock_00002 Wellington, Lot PFOA0609 52.03 ug/mL

Perfluorooctanoic acid (PFOA) 50 ug/mL

.PFOS-Stock_00002 05/05/12 Wellington, Lot LPFOS0409 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL

PFOA/S_Sur/IS_00003 04/19/12 04/19/11 Methanol, Lot J29E57 100 mL 13C4PFOAStock_00015 1 mL 13C4 PFOA 0.5 ug/mL

13C4 PFOA (IS) 0.5 ug/mL

13C4PFOSStock_00015 1 mL 13C4 PFOS 0.478 ug/mL

13C4 PFOS (IS) 0.478 ug/mL

13C8PFOA-stk_00008 1 mL 13C8 PFOA 0.5 ug/mL

13C8PFOS-stk_00008 1 mL 13C8 PFOS 0.478 ug/mL

.13C4PFOAStock_00015 05/12/14 Wellington, Lot MPFOA0511 (Purchased Reagent) 13C4 PFOA 50 ug/mL

13C4 PFOA (IS) 50 ug/mL

.13C4PFOSStock_00015 05/05/14 Wellington, Lot MPFOS0511 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL

13C4 PFOS (IS) 47.8 ug/mL

.13C8PFOA-stk_00008 05/12/14 Wellington Laboratories, Lot M8PFOA0511 (Purchased Reagent) 13C8 PFOA 50 ug/mL

.13C8PFOS-stk_00008 05/06/13 Wellington Laboratories, Lot M8PFOS0510 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL

Page 30 of 272
Certification Summary

Client: E.I. du Pont de Nemours and Company ADQM TestAmerica Job ID: 280-21985-1

Project/Site: WWK - Phase III Sampling

Laboratory Authority Program EPA Region Certification ID

TestAmerica Denver A2LA DoD ELAP 2907.01

TestAmerica Denver A2LA ISO/IEC 17025 2907.01

TestAmerica Denver Alabama State Program 4 40730

TestAmerica Denver Alaska Alaska UST 10 UST-30

TestAmerica Denver Arizona State Program 9 AZ0713

TestAmerica Denver Arkansas State Program 6 88-0687

TestAmerica Denver California State Program 9 2513

TestAmerica Denver Colorado State Program 8 N/A

TestAmerica Denver Connecticut State Program 1 PH-0686

TestAmerica Denver Florida NELAC 4 E87667

TestAmerica Denver Georgia State Program 4 N/A

TestAmerica Denver Idaho State Program 10 CO00026

TestAmerica Denver Illinois NELAC 5 200017

TestAmerica Denver Iowa State Program 7 370

TestAmerica Denver Kansas NELAC 7 E-10166

TestAmerica Denver Louisiana NELAC 6 30785

TestAmerica Denver Maine State Program 1 CO0002

TestAmerica Denver Maryland State Program 3 268

TestAmerica Denver Minnesota NELAC 5 8-999-405

TestAmerica Denver Nevada State Program 9 CO0026

TestAmerica Denver New Hampshire NELAC 1 205310

TestAmerica Denver New Jersey NELAC 2 CO004

TestAmerica Denver New Mexico State Program 6 N/A

TestAmerica Denver New York NELAC 2 11964

TestAmerica Denver North Carolina North Carolina DENR 4 358

TestAmerica Denver North Dakota State Program 8 R-034

TestAmerica Denver Oklahoma State Program 6 8614

TestAmerica Denver Oregon NELAC 10 CO200001

TestAmerica Denver Pennsylvania NELAC 3 68-00664

TestAmerica Denver South Carolina State Program 4 72002

TestAmerica Denver Tennessee State Program 4 TN02944

TestAmerica Denver Texas NELAC 6 T104704183-08-TX

TestAmerica Denver USDA USDA P330-08-00036

TestAmerica Denver Utah NELAC 8 QUAN5

TestAmerica Denver Washington State Program 10 C1284

TestAmerica Denver West Virginia West Virginia DEP 3 354

TestAmerica Denver Wisconsin State Program 5 999615430

Accreditation may not be offered or required for all methods and analytes reported in this package. Please contact your project manager for the laboratory’s 

current list of certified methods and analytes.

Page 31 of 272 TestAmerica Denver
8321A_PFC_Du

PFOA and PFOS

Page 32 of 272
FORM II

LCMS SURROGATE RECOVERY

Lab Name: Job No.: 280-21985-1

SDG No.:

Matrix: Solid Level: Low

TestAmerica Denver

GC Column (1): Gemini-NX ID:

Client Sample ID Lab Sample ID PFOA #

WWK-S-WWM-1(0-.2) 280-21985-1 53

MB 280-94046/1-A 92

LCS 

280-94046/2-A

91

LLCS 

280-94046/3-A

95

WWK-S-WWM-1(0-.2) 280-21985-1 MS

MS

49 X

WWK-S-WWM-1(0-.2) 280-21985-1 DU

DU

51

DLCK 

280-94589/13

101

QC LIMITS

PFOA = 13C4 PFOA QC LIMITS 50-200

FORM II DV-LC-0012

# Column to be used to flag recovery values

Page 33 of 272
LCMS LAB CONTROL SAMPLE RECOVERY

FORM III

Lab Name: Job No.:

SDG No.:

Matrix: Level:

Matrix:

Low

280-21985-1

Solid Lab File ID: PC511K02021.d

Lab ID: LCS 280-94046/2-A Client ID:

TestAmerica Denver

REC 

%

REC

QC

CONCENTRATION LIMITS

(ug/Kg)

SPIKE

ADDED

(ug/Kg)

#

LCS LCS

COMPOUND

Ammonium Perfluorooctanoate 

(APFO)

52.0 58.0 111 70-130

Perfluorooctanoic acid (PFOA) 50.0 55.5 111 70-130

FORM III DV-LC-0012

# Column to be used to flag recovery and RPD values

Page 34 of 272
LCMS LOW LEVEL CONTROL SAMPLE RECOVERY

FORM III

Lab Name: Job No.:

SDG No.:

Matrix: Level:

Matrix:

Low

280-21985-1

Solid Lab File ID: PC511K02022.d

Lab ID: LLCS 280-94046/3-A Client ID:

TestAmerica Denver

REC 

%

REC

QC

CONCENTRATION LIMITS

(ug/Kg)

SPIKE

ADDED

(ug/Kg)

#

LLCS LLCS

COMPOUND

Ammonium Perfluorooctanoate 

(APFO)

5.14 5.73 111 70-130

Perfluorooctanoic acid (PFOA) 4.94 5.48 111 70-130

FORM III DV-LC-0012

# Column to be used to flag recovery and RPD values

Page 35 of 272
LCMS MATRIX SPIKE RECOVERY

FORM III

Lab Name: Job No.:

SDG No.:

Matrix: Level:

Matrix:

Low

280-21985-1

Solid Lab File ID: PC511K02024.d

Lab ID: 280-21985-1 MS Client ID: WWK-S-WWM-1(0-.2) MS

TestAmerica Denver

LIMITS

COMPOUND

CONCENTRATION %

REC

QC

REC

SAMPLE

CONCENTRATION

SPIKE

ADDED

(ug/Kg) (ug/Kg) (ug/Kg)

#

MS MS

Ammonium Perfluorooctanoate 71.7 77.9 70-130

(APFO)

ND 109

Perfluorooctanoic acid (PFOA) 68.9 ND 75.1 109 70-130

FORM III DV-LC-0012

# Column to be used to flag recovery and RPD values

Page 36 of 272
LCMS DETECTION LIMIT CHECK STANDARD RECOVERY

FORM III

Lab Name: Job No.:

SDG No.:

Matrix: Level:

Matrix:

Low

280-21985-1

Solid Lab File ID: PC511K02019.d

Lab ID: DLCK 280-94589/13 Client ID:

TestAmerica Denver

REC 

%

REC

QC

CONCENTRATION LIMITS

(ug/L)

SPIKE

ADDED

(ug/L)

#

DLCK DLCK

COMPOUND

Ammonium Perfluorooctanoate 

(APFO)

0.520 0.488 J 94 70-130

Perfluorooctanoic acid (PFOA) 0.500 0.468 J 94 70-130

FORM III DV-LC-0012

# Column to be used to flag recovery and RPD values

Page 37 of 272
FORM IV

LCMS METHOD BLANK SUMMARY

Lab Name:

SDG No.:

TestAmerica Denver Job No.: 280-21985-1

Instrument ID:

Level:(Low/Med)

Date Extracted:

Date Analyzed: 11/02/2011 15:22

10/31/2011 14:40

Low

LC_LCMS5

Lab File ID: PC511K02020.d Lab Sample ID: MB 280-94046/1-A

Matrix: Solid

THIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES:

LAB SAMPLE ID

LAB

CLIENT SAMPLE ID FILE ID DATE ANALYZED

PC511K02021 11/02/2011 15:30

.d

LCS 280-94046/2-A

PC511K02022 11/02/2011 15:38

.d

LLCS 280-94046/3-A

PC511K02023 11/02/2011 15:45

.d

WWK-S-WWM-1(0-.2) 280-21985-1

PC511K02024 11/02/2011 15:53

.d

WWK-S-WWM-1(0-.2) MS 280-21985-1 MS

PC511K02025 11/02/2011 16:01

.d

WWK-S-WWM-1(0-.2) DU 280-21985-1 DU

FORM IV DV-LC-0012

Page 38 of 272
FORM I

LCMS ORGANICS ANALYSIS DATA SHEET Form 1

Client Sample ID:

Lab Name: Job No.:

WWK-S-WWM-1(0-.2)

SDG No.:

280-21985-1

Lab Sample ID: 280-21985-1

Matrix: Lab File ID: PC511K02023.d

Analysis Method: DV-LC-0012 Date Collected:

Solid

TestAmerica Denver

10/24/2011 07:28

Con. Extract Vol.:

Volume:

Injection Volume:

GPC Cleanup:(Y/N)

Date Extracted:

Date Analyzed:

Dilution Factor: 1

Extraction Method: DV-OP-0019 10/31/2011 14:40

11/02/2011 15:45

50(mL)

20(uL)

Sample wt/vol: 10.04(g)

% Moisture: 28.1

GC Column: Gemini-NX ID:

N

Analysis Batch No.: 94589 Units: ug/Kg

CAS NO. COMPOUND NAME RESULT Q RL MDL

3825-26-1 Ammonium Perfluorooctanoate (APFO) ND 3.5 0.69

335-67-1 Perfluorooctanoic acid (PFOA) ND 3.5 0.69

CAS NO. SURROGATE %REC Q LIMITS

STL00990 13C4 PFOA 53 50-200

FORM I DV-LC-0012

Page 39 of 272
Report Date: 03-Nov-2011 14:45:20 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02023.d

Lims ID: 280-21985-A-1-A Client ID: WWK-S-WWM-1(0-.2)

Inject. Date: 02-Nov-2011 15:45:51 Dil. Factor: 1.0000 

Sample Type: Client

Sample ID: 280-21985-a-1-a, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 17

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 14:45:19 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC308

First Level Reviewer: williamst Date: 03-Nov-2011 14:44:09

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.440 4.433 0.007 1.000 9774712 10.5

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.441 4.434 0.007 11345925 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.441 4.434 0.007 11345925 5.27

 3 Ammonium Perfluorooctanoate (APFO) M

 413.0 > 368.9 4.442 4.435 0.007 1.000 203458 0.0838 0.70- 1.30 1.00 M

 413.0 > 169.0 4.442 4.435 0.007 1.000 47473 3.72- 6.92 4.29 M

 1 Perfluorooctanoic acid M

 413.0 > 368.9 4.442 4.435 0.007 1.000 215126 0.0897 0.70- 1.30 1.00 M

 413.0 > 169.0 4.442 4.435 0.007 1.000 43544 3.72- 6.92 4.94 M

$ 6 13C8 PFOS

 506.9 > 80.0 4.588 4.586 0.002 1.000 3221622 10.3

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.580 4.586 -0.006 0.998 93653 0.1435 0.70- 1.30 1.00

 498.9 > 98.9 4.580 4.586 -0.006 0.998 40487 1.30- 2.42 2.31

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.588 4.586 0.002 3425245 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.588 4.586 0.002 3425245 6.22

QC Flag Legend

Review Flags

M - Manually Integrated

Page 40 of 272
Report Date: 03-Nov-2011 14:45:20 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02023.d

Injection Date: 02-Nov-2011 15:45:51 Limit Group: LC - PFOA DuPont

Client ID: WWK-S-WWM-1(0-.2) Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 17

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

28

Y ( X100000)

C511K02023[MS QQQ Chro]:m/z 421.0 > 375.9 4.440

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

5

10

15

20

25

30

Y ( X100000)

C511K02023[MS QQQ Chro]:m/z 417.0 > 371.9 4.441

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

5

10

15

20

25

30

Y ( X100000)

C511K02023[MS QQQ Chro]:m/z 417.0 > 371.9 4.441

 3 Ammonium Perfluorooctanoate (APFO) (M)

2.9 3.9 4.9

Min

46

54

62

70

78

86

94

102

Y ( X1000)

C511K02023[MS QQQ Chro]:m/z 413.0 > 368.9 4.442

 3 Ammonium Perfluorooctanoate (APFO) (M)

2.9 3.9 4.9

Min

41

43

45

47

49

51

53

Y ( X1000)

C511K02023[MS QQQ Chro]:m/z 413.0 > 169.0 4.442

 1 Perfluorooctanoic acid (M)

2.9 3.9 4.9

Min

46

54

62

70

78

86

94

102

Y ( X1000)

C511K02023[MS QQQ Chro]:m/z 413.0 > 368.9 4.442

 1 Perfluorooctanoic acid (M)

2.9 3.9 4.9

Min

41

43

45

47

49

51

53

Y ( X1000)

C511K02023[MS QQQ Chro]:m/z 413.0 > 169.0 4.442

$ 6 13C8 PFOS

3 4 5

Min

4

16

28

40

52

64

76

88

Y ( X10000)

C511K02023[MS QQQ Chro]:m/z 506.9 > 80.0 4.588

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

41

44

47

50

53

56

59

62

Y ( X1000)

C511K02023[MS QQQ Chro]:m/z 498.9 > 79.9 4.580

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

41

43

45

47

49

51

53

55

Y ( X1000)

C511K02023[MS QQQ Chro]:m/z 498.9 > 98.9 4.580

* 5 13C4 PFOS (IS)

3 4 5

Min

4

16

28

40

52

64

76

88

Y ( X10000)

C511K02023[MS QQQ Chro]:m/z 502.9 > 80.0 4.588

$ 8 13C4 PFOS

3 4 5

Min

4

16

28

40

52

64

76

88

Y ( X10000)

C511K02023[MS QQQ Chro]:m/z 502.9 > 80.0 4.588

Page 41 of 272
Report Date: 03-Nov-2011 14:45:20 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02023.d

Page 42 of 272
Report Date: 03-Nov-2011 14:45:20 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Manual Integration/User Assign Peak Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02023.d

Injection Date: 02-Nov-2011 15:45:51 Limit Group: LC - PFOA DuPont

Client ID: WWK-S-WWM-1(0-.2) Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 17

Operator ID: TW/JB Injection Vol: 20.00 ul

 3 Ammonium Perfluorooctanoate (APFO), Signal: 1, m/z: 413.0 > 368.9 Type: quant, RT: 4.44

Processing Integration Results

RT: 4.44

Response: 164511

Amount: 0.050333

4.15

Min

50

54

58

62

66

70

74

78

82

86

90

94

98

102

106

Y ( X1000)

C511K02023[MS QQQ Chro]:m/z 413.0 > 368.9 4.442

Manual Integration Results

RT: 4.44

Response: 203458

Amount: 0.083838

4.16

Min

50

54

58

62

66

70

74

78

82

86

90

94

98

102

106

Y ( X1000)

C511K02023[MS QQQ Chro]:m/z 413.0 > 368.9 4.442

Reviewer: williamst, 03-Nov-2011 14:44:09

Audit Action: Manually Integrated

Audit Reason: Baseline

Page 43 of 272
Report Date: 03-Nov-2011 14:45:20 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Manual Integration/User Assign Peak Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02023.d

Injection Date: 02-Nov-2011 15:45:51 Limit Group: LC - PFOA DuPont

Client ID: WWK-S-WWM-1(0-.2) Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 17

Operator ID: TW/JB Injection Vol: 20.00 ul

 3 Ammonium Perfluorooctanoate (APFO), Signal: 2, m/z: 413.0 > 169.0 Type: qualifier, RT: 4.44

Processing Integration Results

RT: 4.44

Response: 17258

Amount: 0

4.15

Min

41

42

43

44

45

46

47

48

49

50

51

52

53

54

Y ( X1000)

C511K02023[MS QQQ Chro]:m/z 413.0 > 169.0 4.442

Manual Integration Results

RT: 4.44

Response: 47473

Amount: 0

4.15

Min

41

42

43

44

45

46

47

48

49

50

51

52

53

54

Y ( X1000)

C511K02023[MS QQQ Chro]:m/z 413.0 > 169.0 4.442

Reviewer: williamst, 03-Nov-2011 14:44:09

Audit Action: Manually Integrated

Audit Reason: Baseline

Page 44 of 272
Report Date: 03-Nov-2011 14:45:20 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Manual Integration/User Assign Peak Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02023.d

Injection Date: 02-Nov-2011 15:45:51 Limit Group: LC - PFOA DuPont

Client ID: WWK-S-WWM-1(0-.2) Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 17

Operator ID: TW/JB Injection Vol: 20.00 ul

 1 Perfluorooctanoic acid, Signal: 1, m/z: 413.0 > 368.9 Type: quant, RT: 4.44

Processing Integration Results

RT: 4.44

Response: 164511

Amount: 0.047851

2.8 3.8 4.8

Min

45

49

53

57

61

65

69

73

77

81

85

89

93

97

101

105

Y ( X1000)

C511K02023[MS QQQ Chro]:m/z 413.0 > 368.9 4.442

Manual Integration Results

RT: 4.44

Response: 215126

Amount: 0.089695

2.8 3.8 4.8

Min

45

49

53

57

61

65

69

73

77

81

85

89

93

97

101

105

Y ( X1000)

C511K02023[MS QQQ Chro]:m/z 413.0 > 368.9 4.442

Reviewer: williamst, 03-Nov-2011 14:44:09

Audit Action: Manually Integrated

Audit Reason: Baseline

Page 45 of 272
Report Date: 03-Nov-2011 14:45:20 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Manual Integration/User Assign Peak Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02023.d

Injection Date: 02-Nov-2011 15:45:51 Limit Group: LC - PFOA DuPont

Client ID: WWK-S-WWM-1(0-.2) Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 17

Operator ID: TW/JB Injection Vol: 20.00 ul

 1 Perfluorooctanoic acid, Signal: 2, m/z: 413.0 > 169.0 Type: qualifier, RT: 4.44

Processing Integration Results

RT: 4.44

Response: 17258

Amount: 0

4.16

Min

41

42

43

44

45

46

47

48

49

50

51

52

53

54

Y ( X1000)

C511K02023[MS QQQ Chro]:m/z 413.0 > 169.0 4.442

Manual Integration Results

RT: 4.44

Response: 43544

Amount: 0

4.16

Min

41

42

43

44

45

46

47

48

49

50

51

52

53

54

Y ( X1000)

C511K02023[MS QQQ Chro]:m/z 413.0 > 169.0 4.442

Reviewer: williamst, 03-Nov-2011 14:44:09

Audit Action: Manually Integrated

Audit Reason: Baseline

Page 46 of 272
FORM VI

Lab Name: Job No.:

Calibration ID:

SDG No.:

Instrument ID: Heated Purge: (Y/N)

LCMS INITIAL CALIBRATION DATA

TestAmerica Denver 280-21985-1

LC_LCMS5

Analy Batch No.: 94589

Calibration Start Date: 11/02/2011 13:49 Calibration End Date: 7699

N

11/02/2011 14:51

GC Column: Gemini-NX ID:

EXTERNAL STANDARD RETENTION TIME SUMMARY

Calibration Files:

LEVEL: LAB SAMPLE ID: LAB FILE ID:

Level 1 STD0002 280-94589/2 PC511K02008.d

Level 2 STD0005 280-94589/3 PC511K02009.d

Level 3 STD0010 280-94589/4 PC511K02010.d

Level 4 STD0020 280-94589/5 PC511K02011.d

Level 5 STD0050 280-94589/6 PC511K02012.d

Level 6 STD0100 280-94589/7 PC511K02013.d

Level 7 STD0200 280-94589/8 PC511K02014.d

Level 8 STD0500 280-94589/9 PC511K02015.d

Level 9 STD1250 280-94589/10 PC511K02016.d

ANALYTE LVL 1 LVL 2 LVL 3 LVL 4 LVL 5 LVL 6 LVL 7 LVL 8 LVL 9 RT WINDOW AVG RT

13C4 PFOA 4.450 4.441 4.441 4.432 4.432 4.432 4.432 4.423 +++++ 3.934 - 4.934 4.434

13C4 PFOS 4.606 4.597 4.597 4.588 4.588 4.579 4.579 4.571 +++++ 4.086 - 5.086 4.586

FORM VI DV-LC-0012 Page 47 of 272
FORM VI

Lab Name: Job No.:

Calibration ID:

SDG No.:

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

LCMS INITIAL CALIBRATION DATA

TestAmerica Denver 280-21985-1

LC_LCMS5

Analy Batch No.: 94589

Calibration Start Date: 11/02/2011 13:49 Calibration End Date: 7699

N

11/02/2011 14:51

Gemini-NX ID:

EXTERNAL STANDARD CURVE EVALUTION

Calibration Files:

LEVEL: LAB SAMPLE ID: LAB FILE ID:

Level 1 STD0002 280-94589/2 PC511K02008.d

Level 2 STD0005 280-94589/3 PC511K02009.d

Level 3 STD0010 280-94589/4 PC511K02010.d

Level 4 STD0020 280-94589/5 PC511K02011.d

Level 5 STD0050 280-94589/6 PC511K02012.d

Level 6 STD0100 280-94589/7 PC511K02013.d

Level 7 STD0200 280-94589/8 PC511K02014.d

Level 8 STD0500 280-94589/9 PC511K02015.d

Level 9 STD1250 280-94589/10 PC511K02016.d

MIN R^2

OR COD

R^2 #

OR COD

MAX

%RSD

COEFFICIENT # %RSD #

B M1 M2

CURVE

TYPE

LVL 1 LVL 2 LVL 3 LVL 4

ANALYTE CF MIN CF

LVL 5 LVL 6 LVL 7 LVL 8

LVL 9

13C4 PFOA 2296718 2223037 2279793 2326392 Ave 9.9 30.0

2241184 2181743 1978105 1700225

+++++

2153399.50

13C4 PFOS 555482 565703 581890 580327 Ave 7.7 30.0

568480 571212 524933 455059

+++++

550385.735

FORM VI DV-LC-0012

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

Page 48 of 272
FORM VI

Lab Name: Job No.:

Calibration ID:

SDG No.:

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

LCMS INITIAL CALIBRATION DATA

TestAmerica Denver 280-21985-1

LC_LCMS5

Analy Batch No.: 94589

Calibration Start Date: 11/02/2011 13:49 Calibration End Date: 7699

N

11/02/2011 14:51

Gemini-NX ID:

INTERNAL STANDARD CURVE EVALUTION

ANALYTE RRF

LVL 1 LVL 2 LVL 3 LVL 4 LVL 5

CURVE

TYPE

COEFFICIENT

B M1 M2

# %RSD # MAX

%RSD

R^2

OR COD

# MIN R^2

OR COD

MIN RRF

LVL 6 LVL 7 LVL 8 LVL 9

Ammonium Perfluorooctanoate (APFO) 1.3782 1.3238 1.0737 1.0673 1.0426 Lin1 0.9990

1.0232 1.0730 1.0109 +++++

0.0934 1.0245 0.9900

Perfluorooctanoic acid (PFOA) 1.4387 1.3776 1.1173 1.1106 1.0850 Lin1 0.9990

1.0647 1.1165 1.0520 +++++

0.0940 1.0661 0.9900

Perfluorooctanoic Sulfonate 1.7363 1.5399 1.3577 1.3919 1.3879 Lin1 1.0000

1.3656 1.4172 1.3545 +++++

0.0650 1.3684 0.9900

13C8 PFOA 1.0343 0.9261 0.8995 0.8451 0.8652 Lin1 0.9980

0.8435 0.8646 0.7883 +++++

0.0622 0.8143 0.9900

13C8 PFOS 1.0470 0.9368 0.8850 0.9360 0.9054 Lin1 0.9980

0.8939 0.9221 0.8456 +++++

0.0435 0.8710 0.9900

FORM VI DV-LC-0012

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

Page 49 of 272
FORM VI

Lab Name: Job No.:

Calibration ID:

SDG No.:

Instrument ID: Heated Purge: (Y/N)

LCMS INITIAL CALIBRATION DATA

TestAmerica Denver 280-21985-1

LC_LCMS5

Analy Batch No.: 94589

Calibration Start Date: 11/02/2011 13:49 Calibration End Date: 7699

N

11/02/2011 14:51

GC Column: Gemini-NX ID:

EXTERNAL STANDARD RESPONSE AND CONCENTRATION

Calibration Files:

LEVEL: LAB SAMPLE ID: LAB FILE ID:

Level 1 STD0002 280-94589/2 PC511K02008.d

Level 2 STD0005 280-94589/3 PC511K02009.d

Level 3 STD0010 280-94589/4 PC511K02010.d

Level 4 STD0020 280-94589/5 PC511K02011.d

Level 5 STD0050 280-94589/6 PC511K02012.d

Level 6 STD0100 280-94589/7 PC511K02013.d

Level 7 STD0200 280-94589/8 PC511K02014.d

Level 8 STD0500 280-94589/9 PC511K02015.d

Level 9 STD1250 280-94589/10 PC511K02016.d

CURVE

TYPE

ANALYTE RESPONSE CONCENTRATION (UG/L)

LVL 1 LVL 2 LVL 3 LVL 4 LVL 5 LVL 1 LVL 2 LVL 3 LVL 4 LVL 5

LVL 6 LVL 7 LVL 8 LVL 9 LVL 6 LVL 7 LVL 8 LVL 9

13C4 PFOA Ave 22967180

21817429

22230365

19781051

22797925

17002248

23263924

+++++

22411838 10.0

10.0

10.0

10.0

10.0

10.0

10.0

+++++

10.0

13C4 PFOS Ave 5310411

5460786

5408117

5018364

5562864

4350363

5547924

+++++

5434672 9.56

9.56

9.56

9.56

9.56

9.56

9.56

+++++

9.56

Curve Type Legend:

Ave = Average

FORM VI DV-LC-0012 Page 50 of 272
FORM VI

Lab Name: Job No.:

Calibration ID:

SDG No.:

Instrument ID: Heated Purge: (Y/N)

LCMS INITIAL CALIBRATION DATA

TestAmerica Denver 280-21985-1

LC_LCMS5

Analy Batch No.: 94589

Calibration Start Date: 11/02/2011 13:49 Calibration End Date: 7699

N

11/02/2011 14:51

GC Column: Gemini-NX ID:

INTERNAL STANDARD RESPONSE AND CONCENTRATION

Calibration Files:

LEVEL: LAB SAMPLE ID: LAB FILE ID:

Level 1 STD0002 280-94589/2 PC511K02008.d

Level 2 STD0005 280-94589/3 PC511K02009.d

Level 3 STD0010 280-94589/4 PC511K02010.d

Level 4 STD0020 280-94589/5 PC511K02011.d

Level 5 STD0050 280-94589/6 PC511K02012.d

Level 6 STD0100 280-94589/7 PC511K02013.d

Level 7 STD0200 280-94589/8 PC511K02014.d

Level 8 STD0500 280-94589/9 PC511K02015.d

Level 9 STD1250 280-94589/10 PC511K02016.d

ANALYTE CURVE

TYPE

IS

REF

RESPONSE

LVL 1 LVL 2 LVL 3 LVL 4 LVL 5

CONCENTRATION (UG/L)

LVL 1 LVL 2 LVL 3 LVL 4 LVL 5

LVL 6 LVL 7 LVL 8 LVL 9 LVL 6 LVL 7 LVL 8 LVL 9

Ammonium Perfluorooctanoate (APFO) OA Lin1 658763 1531203 2547268 5167538 12158038

23229872 44171876 89427814 +++++

0.208 0.520 1.04 2.08 5.20

10.4 20.8 52.0 +++++

Perfluorooctanoic acid (PFOA) OA Lin1 660880 1531203 2547268 5167538 12158038

23229872 44171876 89427814 +++++

0.200 0.500 1.00 2.00 5.00

10.0 20.0 50.0 +++++

Perfluorooctanoic Sulfonate PFOS Lin1 184405 416392 755252 1544406 3771389

7457483 14223555 29463004 +++++

0.191 0.478 0.956 1.91 4.78

9.56 19.1 47.8 +++++

13C8 PFOA OA Lin1 475083 1029368 2050597 3932174 9695738

18402008 34203552 67015770 +++++

0.200 0.500 1.00 2.00 5.00

10.0 20.0 50.0 +++++

13C8 PFOS PFOS Lin1 111195 253319 492339 1038604 2460152

4881581 9255367 18393914 +++++

0.191 0.478 0.956 1.91 4.78

9.56 19.1 47.8 +++++

Curve Type Legend:

Lin1 = Linear 1/conc ISTD

FORM VI DV-LC-0012 Page 51 of 272
Report Date: 03-Nov-2011 10:28:56 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02008.d

Lims ID: std0002 Client ID:

Inject. Date: 02-Nov-2011 13:49:53 Dil. Factor: 1.0000 

Sample Type: IC Calib Level: 1

Sample ID: STD0002, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 2

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:28:56 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

First Level Reviewer: bonnettj Date: 03-Nov-2011 10:20:27

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

 1 Perfluorooctanoic acid M

 413.0 > 368.9 4.451 4.451 0.000 1.000 660880 0.1818 0.70- 1.30 1.00 M

 413.0 > 169.0 4.451 4.451 0.000 1.000 118357 3.72- 6.92 5.58

 3 Ammonium Perfluorooctanoate (APFO) M

 413.0 > 368.9 4.451 4.451 0.000 1.000 658763 0.1888 0.70- 1.30 1.00 M

 413.0 > 169.0 4.451 4.451 0.000 1.000 118357 3.72- 6.92 5.57

$ 9 13C8 PFOA

 421.0 > 375.9 4.449 4.433 0.016 1.000 475083 0.1776

$ 7 13C4 PFOA

 417.0 > 371.9 4.450 4.434 0.016 22967180 10.7

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.450 4.434 0.016 22967180 10.0

$ 6 13C8 PFOS

 506.9 > 80.0 4.605 4.586 0.019 1.000 111195 0.1799

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.607 4.586 0.021 1.000 184405 0.1951 0.70- 1.30 1.00

 498.9 > 98.9 4.607 4.586 0.021 1.000 103815 1.30- 2.42 1.78

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.606 4.586 0.020 5310411 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.606 4.586 0.020 5310411 9.65

Page 52 of 272
Report Date: 03-Nov-2011 10:28:56 Chrom Revision: 1.2 13-Jul-2011 10:43:06

QC Flag Legend

Review Flags

M - Manually Integrated

Page 53 of 272
Report Date: 03-Nov-2011 10:28:56 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02008.d

Injection Date: 02-Nov-2011 13:49:53 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 2

Operator ID: TW/JB Injection Vol: 20.00 ul

 1 Perfluorooctanoic acid (M)

2.9 3.9 4.9

Min

4

7

10

13

16

19

22

Y ( X10000)

C511K02008[MS QQQ Chro]:m/z 413.0 > 368.9 4.451

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

41

47

53

59

65

71

77

83

Y ( X1000)

C511K02008[MS QQQ Chro]:m/z 413.0 > 169.0 4.451

 3 Ammonium Perfluorooctanoate (APFO) (M)

2.9 3.9 4.9

Min

4

7

10

13

16

19

22

Y ( X10000)

C511K02008[MS QQQ Chro]:m/z 413.0 > 368.9 4.451

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

41

47

53

59

65

71

77

83

Y ( X1000)

C511K02008[MS QQQ Chro]:m/z 413.0 > 169.0 4.451

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

4

6

8

10

12

14

16

Y ( X10000)

C511K02008[MS QQQ Chro]:m/z 421.0 > 375.9 4.449

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02008[MS QQQ Chro]:m/z 417.0 > 371.9 4.450

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02008[MS QQQ Chro]:m/z 417.0 > 371.9 4.450

$ 6 13C8 PFOS

3 4 5

Min

41

46

51

56

61

66

71

76

Y ( X1000)

C511K02008[MS QQQ Chro]:m/z 506.9 > 80.0 4.605

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

41

48

55

62

69

76

83

90

Y ( X1000)

C511K02008[MS QQQ Chro]:m/z 498.9 > 79.9 4.607

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

41

45

49

53

57

61

65

69

Y ( X1000)

C511K02008[MS QQQ Chro]:m/z 498.9 > 98.9 4.607

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02008[MS QQQ Chro]:m/z 502.9 > 80.0 4.606

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02008[MS QQQ Chro]:m/z 502.9 > 80.0 4.606

Page 54 of 272
Report Date: 03-Nov-2011 10:28:56 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02008.d

Page 55 of 272
Report Date: 03-Nov-2011 10:28:56 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Manual Integration/User Assign Peak Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02008.d

Injection Date: 02-Nov-2011 13:49:53 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 2

Operator ID: TW/JB Injection Vol: 20.00 ul

 1 Perfluorooctanoic acid, Signal: 1, m/z: 413.0 > 368.9 Type: quant, RT: 4.45

Processing Integration Results

RT: 4.45

Response: 578269

Amount: 0.168099

4.1

Min

4

6

8

10

12

14

16

18

20

22

Y ( X10000)

C511K02008[MS QQQ Chro]:m/z 413.0 > 368.9 4.451

Manual Integration Results

RT: 4.45

Response: 660880

Amount: 0.181753

4.08

Min

4

6

8

10

12

14

16

18

20

22

Y ( X10000)

C511K02008[MS QQQ Chro]:m/z 413.0 > 368.9 4.451

Reviewer: bonnettj, 03-Nov-2011 10:25:28

Audit Action: Manually Integrated

Audit Reason: Baseline

Page 56 of 272
Report Date: 03-Nov-2011 10:28:56 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Manual Integration/User Assign Peak Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02008.d

Injection Date: 02-Nov-2011 13:49:53 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 2

Operator ID: TW/JB Injection Vol: 20.00 ul

 3 Ammonium Perfluorooctanoate (APFO), Signal: 1, m/z: 413.0 > 368.9 Type: quant, RT: 4.45

Processing Integration Results

RT: 4.45

Response: 578269

Amount: 0.174924

4.1

Min

4

6

8

10

12

14

16

18

20

22

Y ( X10000)

C511K02008[MS QQQ Chro]:m/z 413.0 > 368.9 4.451

Manual Integration Results

RT: 4.45

Response: 658763

Amount: 0.188767

4.09

Min

4

6

8

10

12

14

16

18

20

22

Y ( X10000)

C511K02008[MS QQQ Chro]:m/z 413.0 > 368.9 4.451

Reviewer: bonnettj, 03-Nov-2011 10:25:28

Audit Action: Manually Integrated

Audit Reason: Baseline

Page 57 of 272
Report Date: 03-Nov-2011 10:28:57 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02009.d

Lims ID: std0005 Client ID:

Inject. Date: 02-Nov-2011 13:57:37 Dil. Factor: 1.0000 

Sample Type: IC Calib Level: 2

Sample ID: STD0005, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 3

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:28:57 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

First Level Reviewer: bonnettj Date: 03-Nov-2011 10:23:08

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.442 4.451 -0.009 1.000 1531203 0.5579 0.70- 1.30 1.00

 413.0 > 169.0 4.442 4.451 -0.009 1.000 236900 3.72- 6.92 6.46

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.442 4.451 -0.009 1.000 1531203 0.5811 0.70- 1.30 1.00

 413.0 > 169.0 4.442 4.451 -0.009 1.000 236900 3.72- 6.92 6.46

$ 9 13C8 PFOA

 421.0 > 375.9 4.440 4.433 0.007 1.000 1029368 0.4922

$ 7 13C4 PFOA

 417.0 > 371.9 4.441 4.434 0.007 22230365 10.3

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.441 4.434 0.007 22230365 10.0

$ 6 13C8 PFOS

 506.9 > 80.0 4.596 4.586 0.010 1.000 253319 0.4642

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.598 4.586 0.012 1.000 416392 0.4904 0.70- 1.30 1.00

 498.9 > 98.9 4.598 4.586 0.012 1.000 226660 1.30- 2.42 1.84

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.597 4.586 0.011 5408117 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.597 4.586 0.011 5408117 9.83

Page 58 of 272
Report Date: 03-Nov-2011 10:28:57 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02009.d

Injection Date: 02-Nov-2011 13:57:37 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 3

Operator ID: TW/JB Injection Vol: 20.00 ul

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

9

14

19

24

29

34

39

Y ( X10000)

C511K02009[MS QQQ Chro]:m/z 413.0 > 368.9 4.442

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

41

50

59

68

77

86

95

104

Y ( X1000)

C511K02009[MS QQQ Chro]:m/z 413.0 > 169.0 4.442

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

9

14

19

24

29

34

39

Y ( X10000)

C511K02009[MS QQQ Chro]:m/z 413.0 > 368.9 4.442

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

41

50

59

68

77

86

95

104

Y ( X1000)

C511K02009[MS QQQ Chro]:m/z 413.0 > 169.0 4.442

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

4

8

12

16

20

24

28

Y ( X10000)

C511K02009[MS QQQ Chro]:m/z 421.0 > 375.9 4.440

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02009[MS QQQ Chro]:m/z 417.0 > 371.9 4.441

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02009[MS QQQ Chro]:m/z 417.0 > 371.9 4.441

$ 6 13C8 PFOS

3 4 5

Min

41

51

61

71

81

91

101

111

Y ( X1000)

C511K02009[MS QQQ Chro]:m/z 506.9 > 80.0 4.596

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

6

8

10

12

14

16

Y ( X10000)

C511K02009[MS QQQ Chro]:m/z 498.9 > 79.9 4.598

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

41

49

57

65

73

81

89

97

Y ( X1000)

C511K02009[MS QQQ Chro]:m/z 498.9 > 98.9 4.598

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02009[MS QQQ Chro]:m/z 502.9 > 80.0 4.597

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02009[MS QQQ Chro]:m/z 502.9 > 80.0 4.597

Page 59 of 272
Report Date: 03-Nov-2011 10:28:57 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02009.d

Page 60 of 272
Report Date: 03-Nov-2011 10:28:58 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02010.d

Lims ID: std0010 Client ID:

Inject. Date: 02-Nov-2011 14:05:21 Dil. Factor: 1.0000 

Sample Type: IC Calib Level: 3

Sample ID: STD0010, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 4

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:28:58 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

First Level Reviewer: bonnettj Date: 03-Nov-2011 10:23:13

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.440 4.433 0.007 1.000 2050597 1.03

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.441 4.434 0.007 22797925 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.441 4.434 0.007 22797925 10.6

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.442 4.446 -0.004 1.000 2547268 1.00 0.70- 1.30 1.00

 413.0 > 169.0 4.442 4.446 -0.004 1.000 510741 3.72- 6.92 4.99

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.442 4.446 -0.004 1.000 2547268 0.9599 0.70- 1.30 1.00

 413.0 > 169.0 4.442 4.446 -0.004 1.000 510741 3.72- 6.92 4.99

$ 6 13C8 PFOS

 506.9 > 80.0 4.596 4.586 0.010 1.000 492339 0.9214

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.598 4.586 0.012 1.000 755252 0.9010 0.70- 1.30 1.00

 498.9 > 98.9 4.598 4.586 0.012 1.000 422285 1.30- 2.42 1.79

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.597 4.586 0.011 5562864 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.597 4.586 0.011 5562864 10.1

Page 61 of 272
Report Date: 03-Nov-2011 10:28:58 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02010.d

Injection Date: 02-Nov-2011 14:05:21 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 4

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

4

11

18

25

32

39

46

53

Y ( X10000)

C511K02010[MS QQQ Chro]:m/z 421.0 > 375.9 4.440

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02010[MS QQQ Chro]:m/z 417.0 > 371.9 4.441

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02010[MS QQQ Chro]:m/z 417.0 > 371.9 4.441

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

13

22

31

40

49

58

67

Y ( X10000)

C511K02010[MS QQQ Chro]:m/z 413.0 > 368.9 4.442

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

6

8

10

12

14

16

18

Y ( X10000)

C511K02010[MS QQQ Chro]:m/z 413.0 > 169.0 4.442

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

13

22

31

40

49

58

67

Y ( X10000)

C511K02010[MS QQQ Chro]:m/z 413.0 > 368.9 4.442

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

6

8

10

12

14

16

18

Y ( X10000)

C511K02010[MS QQQ Chro]:m/z 413.0 > 169.0 4.442

$ 6 13C8 PFOS

3 4 5

Min

4

6

8

10

12

14

16

18

Y ( X10000)

C511K02010[MS QQQ Chro]:m/z 506.9 > 80.0 4.596

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

7

10

13

16

19

22

25

Y ( X10000)

C511K02010[MS QQQ Chro]:m/z 498.9 > 79.9 4.598

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

6

8

10

12

14

16

Y ( X10000)

C511K02010[MS QQQ Chro]:m/z 498.9 > 98.9 4.598

* 5 13C4 PFOS (IS)

3 4 5

Min

0

3

6

9

12

15

Y ( X100000)

C511K02010[MS QQQ Chro]:m/z 502.9 > 80.0 4.597

$ 8 13C4 PFOS

3 4 5

Min

0

3

6

9

12

15

Y ( X100000)

C511K02010[MS QQQ Chro]:m/z 502.9 > 80.0 4.597

Page 62 of 272
Report Date: 03-Nov-2011 10:28:58 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02010.d

Page 63 of 272
Report Date: 03-Nov-2011 10:28:59 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02011.d

Lims ID: std0020 Client ID:

Inject. Date: 02-Nov-2011 14:13:05 Dil. Factor: 1.0000 

Sample Type: IC Calib Level: 4

Sample ID: STD0020, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 5

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:28:59 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

First Level Reviewer: bonnettj Date: 03-Nov-2011 10:23:19

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.431 4.433 -0.002 1.000 3932174 2.00

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.432 4.434 -0.002 23263924 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.432 4.434 -0.002 23263924 10.8

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.433 4.445 -0.012 1.000 5167538 2.08 0.70- 1.30 1.00

 413.0 > 169.0 4.433 4.445 -0.012 1.000 991708 3.72- 6.92 5.21

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.433 4.445 -0.012 1.000 5167538 2.00 0.70- 1.30 1.00

 413.0 > 169.0 4.433 4.445 -0.012 1.000 991708 3.72- 6.92 5.21

$ 6 13C8 PFOS

 506.9 > 80.0 4.588 4.586 0.002 1.000 1038604 2.00

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.589 4.586 0.003 1.000 1544406 1.90 0.70- 1.30 1.00

 498.9 > 98.9 4.589 4.586 0.003 1.000 873693 1.30- 2.42 1.77

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.588 4.586 0.002 5547924 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.588 4.586 0.002 5547924 10.1

Page 64 of 272
Report Date: 03-Nov-2011 10:28:59 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02011.d

Injection Date: 02-Nov-2011 14:13:05 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 5

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

2

4

6

8

10

Y ( X100000)

C511K02011[MS QQQ Chro]:m/z 421.0 > 375.9 4.431

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02011[MS QQQ Chro]:m/z 417.0 > 371.9 4.432

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02011[MS QQQ Chro]:m/z 417.0 > 371.9 4.432

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02011[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

8

12

16

20

24

28

Y ( X10000)

C511K02011[MS QQQ Chro]:m/z 413.0 > 169.0 4.433

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02011[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

8

12

16

20

24

28

Y ( X10000)

C511K02011[MS QQQ Chro]:m/z 413.0 > 169.0 4.433

$ 6 13C8 PFOS

3 4 5

Min

4

8

12

16

20

24

28

32

Y ( X10000)

C511K02011[MS QQQ Chro]:m/z 506.9 > 80.0 4.588

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

10

16

22

28

34

40

46

Y ( X10000)

C511K02011[MS QQQ Chro]:m/z 498.9 > 79.9 4.589

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

8

12

16

20

24

28

Y ( X10000)

C511K02011[MS QQQ Chro]:m/z 498.9 > 98.9 4.589

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02011[MS QQQ Chro]:m/z 502.9 > 80.0 4.588

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02011[MS QQQ Chro]:m/z 502.9 > 80.0 4.588

Page 65 of 272
Report Date: 03-Nov-2011 10:28:59 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02011.d

Page 66 of 272
Report Date: 03-Nov-2011 10:29:00 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02012.d

Lims ID: std0050 Client ID:

Inject. Date: 02-Nov-2011 14:20:49 Dil. Factor: 1.0000 

Sample Type: IC Calib Level: 5

Sample ID: STD0050, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 6

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:28:59 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

First Level Reviewer: bonnettj Date: 03-Nov-2011 10:23:24

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.431 4.433 -0.002 1.000 9695738 5.24

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.432 4.434 -0.002 22411838 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.432 4.434 -0.002 22411838 10.4

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.433 4.442 -0.009 1.000 12158038 5.20 0.70- 1.30 1.00

 413.0 > 169.0 4.433 4.442 -0.009 1.000 2285249 3.72- 6.92 5.32

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.433 4.442 -0.009 1.000 12158038 5.00 0.70- 1.30 1.00

 413.0 > 169.0 4.433 4.442 -0.009 1.000 2285249 3.72- 6.92 5.32

$ 6 13C8 PFOS

 506.9 > 80.0 4.588 4.586 0.002 1.000 2460152 4.92

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.580 4.586 -0.006 0.998 3771389 4.80 0.70- 1.30 1.00

 498.9 > 98.9 4.580 4.586 -0.006 0.998 2025922 1.30- 2.42 1.86

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.588 4.586 0.002 5434672 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.588 4.586 0.002 5434672 9.87

Page 67 of 272
Report Date: 03-Nov-2011 10:29:00 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02012.d

Injection Date: 02-Nov-2011 14:20:49 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 6

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

Y ( X100000)

C511K02012[MS QQQ Chro]:m/z 421.0 > 375.9 4.431

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02012[MS QQQ Chro]:m/z 417.0 > 371.9 4.432

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02012[MS QQQ Chro]:m/z 417.0 > 371.9 4.432

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

5

10

15

20

25

30

Y ( X100000)

C511K02012[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

12

20

28

36

44

52

60

Y ( X10000)

C511K02012[MS QQQ Chro]:m/z 413.0 > 169.0 4.433

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

5

10

15

20

25

30

Y ( X100000)

C511K02012[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

12

20

28

36

44

52

60

Y ( X10000)

C511K02012[MS QQQ Chro]:m/z 413.0 > 169.0 4.433

$ 6 13C8 PFOS

3 4 5

Min

4

13

22

31

40

49

58

67

Y ( X10000)

C511K02012[MS QQQ Chro]:m/z 506.9 > 80.0 4.588

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

2

4

6

8

10

12

Y ( X100000)

C511K02012[MS QQQ Chro]:m/z 498.9 > 79.9 4.580

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

12

20

28

36

44

52

60

Y ( X10000)

C511K02012[MS QQQ Chro]:m/z 498.9 > 98.9 4.580

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02012[MS QQQ Chro]:m/z 502.9 > 80.0 4.588

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02012[MS QQQ Chro]:m/z 502.9 > 80.0 4.588

Page 68 of 272
Report Date: 03-Nov-2011 10:29:00 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02012.d

Page 69 of 272
Report Date: 03-Nov-2011 10:29:00 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02013.d

Lims ID: std0100 Client ID:

Inject. Date: 02-Nov-2011 14:28:32 Dil. Factor: 1.0000 

Sample Type: IC Calib Level: 6

Sample ID: STD0100, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 7

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:00 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

First Level Reviewer: bonnettj Date: 03-Nov-2011 10:22:29

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.431 4.433 -0.002 1.000 18402008 10.3

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.432 4.434 -0.002 21817429 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.432 4.434 -0.002 21817429 10.1

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.433 4.440 -0.007 1.000 23229872 10.3 0.70- 1.30 1.00

 413.0 > 169.0 4.424 4.440 -0.016 0.998 4461306 3.72- 6.92 5.21

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.433 4.440 -0.007 1.000 23229872 9.90 0.70- 1.30 1.00

 413.0 > 169.0 4.424 4.440 -0.016 0.998 4461306 3.72- 6.92 5.21

$ 6 13C8 PFOS

 506.9 > 80.0 4.579 4.586 -0.007 1.000 4881581 9.76

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.580 4.586 -0.006 1.000 7457483 9.49 0.70- 1.30 1.00

 498.9 > 98.9 4.580 4.586 -0.006 1.000 4015248 1.30- 2.42 1.86

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.579 4.586 -0.007 5460786 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.579 4.586 -0.007 5460786 9.92

Page 70 of 272
Report Date: 03-Nov-2011 10:29:01 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02013.d

Injection Date: 02-Nov-2011 14:28:32 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 7

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

6

12

18

24

30

36

42

48

Y ( X100000)

C511K02013[MS QQQ Chro]:m/z 421.0 > 375.9 4.431

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02013[MS QQQ Chro]:m/z 417.0 > 371.9 4.432

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02013[MS QQQ Chro]:m/z 417.0 > 371.9 4.432

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02013[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

Y ( X100000)

C511K02013[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02013[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

Y ( X100000)

C511K02013[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

$ 6 13C8 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02013[MS QQQ Chro]:m/z 506.9 > 80.0 4.579

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

3

6

9

12

15

18

Y ( X100000)

C511K02013[MS QQQ Chro]:m/z 498.9 > 79.9 4.580

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

2

4

6

8

10

12

Y ( X100000)

C511K02013[MS QQQ Chro]:m/z 498.9 > 98.9 4.580

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02013[MS QQQ Chro]:m/z 502.9 > 80.0 4.579

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02013[MS QQQ Chro]:m/z 502.9 > 80.0 4.579

Page 71 of 272
Report Date: 03-Nov-2011 10:29:01 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02013.d

Page 72 of 272
Report Date: 03-Nov-2011 10:29:01 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02014.d

Lims ID: std0200 Client ID:

Inject. Date: 02-Nov-2011 14:36:17 Dil. Factor: 1.0000 

Sample Type: IC Calib Level: 7

Sample ID: STD0200, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 8

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:01 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

First Level Reviewer: bonnettj Date: 03-Nov-2011 10:21:43

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.431 4.433 -0.002 1.000 34203552 21.2

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.432 4.434 -0.002 19781051 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.432 4.434 -0.002 19781051 9.19

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.433 4.439 -0.006 1.000 44171876 21.7 0.70- 1.30 1.00

 413.0 > 169.0 4.433 4.439 -0.006 1.000 8332659 3.72- 6.92 5.30

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.433 4.439 -0.006 1.000 44171876 20.9 0.70- 1.30 1.00

 413.0 > 169.0 4.433 4.439 -0.006 1.000 8332659 3.72- 6.92 5.30

$ 6 13C8 PFOS

 506.9 > 80.0 4.579 4.586 -0.007 1.000 9255367 20.2

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.580 4.586 -0.006 1.000 14223555 19.8 0.70- 1.30 1.00

 498.9 > 98.9 4.580 4.586 -0.006 1.000 7690600 1.30- 2.42 1.85

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.579 4.586 -0.007 5018364 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.579 4.586 -0.007 5018364 9.12

Page 73 of 272
Report Date: 03-Nov-2011 10:29:02 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02014.d

Injection Date: 02-Nov-2011 14:36:17 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 8

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

11

22

33

44

55

66

77

88

Y ( X100000)

C511K02014[MS QQQ Chro]:m/z 421.0 > 375.9 4.431

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

7

14

21

28

35

42

49

Y ( X100000)

C511K02014[MS QQQ Chro]:m/z 417.0 > 371.9 4.432

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

7

14

21

28

35

42

49

Y ( X100000)

C511K02014[MS QQQ Chro]:m/z 417.0 > 371.9 4.432

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

Y ( X1000000)

C511K02014[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

3

6

9

12

15

18

21

Y ( X100000)

C511K02014[MS QQQ Chro]:m/z 413.0 > 169.0 4.433

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

Y ( X1000000)

C511K02014[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

3

6

9

12

15

18

21

Y ( X100000)

C511K02014[MS QQQ Chro]:m/z 413.0 > 169.0 4.433

$ 6 13C8 PFOS

3 4 5

Min

0

4

8

12

16

20

24

Y ( X100000)

C511K02014[MS QQQ Chro]:m/z 506.9 > 80.0 4.579

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

5

10

15

20

25

30

35

Y ( X100000)

C511K02014[MS QQQ Chro]:m/z 498.9 > 79.9 4.580

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

3

6

9

12

15

18

21

Y ( X100000)

C511K02014[MS QQQ Chro]:m/z 498.9 > 98.9 4.580

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02014[MS QQQ Chro]:m/z 502.9 > 80.0 4.579

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02014[MS QQQ Chro]:m/z 502.9 > 80.0 4.579

Page 74 of 272
Report Date: 03-Nov-2011 10:29:02 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02014.d

Page 75 of 272
Report Date: 03-Nov-2011 10:29:02 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02015.d

Lims ID: std0500 Client ID:

Inject. Date: 02-Nov-2011 14:43:59 Dil. Factor: 1.0000 

Sample Type: IC Calib Level: 8

Sample ID: STD0500, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 9

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:02 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

First Level Reviewer: bonnettj Date: 03-Nov-2011 10:21:20

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.422 4.433 -0.011 1.000 67015770 48.3

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.423 4.434 -0.011 17002248 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.423 4.434 -0.011 17002248 7.90

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.424 4.438 -0.014 1.000 89427814 51.2 0.70- 1.30 1.00

 413.0 > 169.0 4.424 4.438 -0.014 1.000 17409476 3.72- 6.92 5.14

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.424 4.438 -0.014 1.000 89427814 49.2 0.70- 1.30 1.00

 413.0 > 169.0 4.424 4.438 -0.014 1.000 17409476 3.72- 6.92 5.14

$ 6 13C8 PFOS

 506.9 > 80.0 4.570 4.586 -0.016 1.000 18393914 46.4

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.571 4.586 -0.015 1.000 29463004 47.3 0.70- 1.30 1.00

 498.9 > 98.9 4.571 4.586 -0.015 1.000 16037149 1.30- 2.42 1.84

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.571 4.586 -0.015 4350363 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.571 4.586 -0.015 4350363 7.90

Page 76 of 272
Report Date: 03-Nov-2011 10:29:03 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02015.d

Injection Date: 02-Nov-2011 14:43:59 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 9

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

3

6

9

12

15

Y ( X1000000)

C511K02015[MS QQQ Chro]:m/z 421.0 > 375.9 4.422

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

6

12

18

24

30

36

42

Y ( X100000)

C511K02015[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

6

12

18

24

30

36

42

Y ( X100000)

C511K02015[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

3

6

9

12

15

18

21

Y ( X1000000)

C511K02015[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

6

12

18

24

30

36

42

Y ( X100000)

C511K02015[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

3

6

9

12

15

18

21

Y ( X1000000)

C511K02015[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

6

12

18

24

30

36

42

Y ( X100000)

C511K02015[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

$ 6 13C8 PFOS

3 4 5

Min

0

6

12

18

24

30

36

42

Y ( X100000)

C511K02015[MS QQQ Chro]:m/z 506.9 > 80.0 4.570

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

9

18

27

36

45

54

63

72

Y ( X100000)

C511K02015[MS QQQ Chro]:m/z 498.9 > 79.9 4.571

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

5

10

15

20

25

30

35

40

Y ( X100000)

C511K02015[MS QQQ Chro]:m/z 498.9 > 98.9 4.571

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

Y ( X100000)

C511K02015[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

Y ( X100000)

C511K02015[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

Page 77 of 272
Report Date: 03-Nov-2011 10:29:03 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02015.d

Page 78 of 272
Report Date: 03-Nov-2011 10:29:04 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Lims ID: std1250 Client ID:

Inject. Date: 02-Nov-2011 14:51:42 Dil. Factor: 1.0000 

Sample Type: IC Calib Level: 9

Sample ID: STD1250, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 10

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

First Level Reviewer: bonnettj Date: 03-Nov-2011 10:23:45

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.422 4.433 -0.011 1.000 123902997 107.1

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.423 4.434 -0.011 14194691 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.423 4.434 -0.011 14194691 6.59

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.424 4.436 -0.012 1.000 160762177 110.5 0.70- 1.30 1.00

 413.0 > 169.0 4.424 4.436 -0.012 1.000 30903572 3.72- 6.92 5.20

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.424 4.436 -0.012 1.000 160762177 106.1 0.70- 1.30 1.00

 413.0 > 169.0 4.424 4.436 -0.012 1.000 30903572 3.72- 6.92 5.20

$ 6 13C8 PFOS

 506.9 > 80.0 4.570 4.586 -0.016 1.000 32699964 104.5

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.571 4.586 -0.015 1.000 51804971 105.3 0.70- 1.30 1.00

 498.9 > 98.9 4.571 4.586 -0.015 1.000 28282048 1.30- 2.42 1.83

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.571 4.586 -0.015 3434108 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.571 4.586 -0.015 3434108 6.24

Page 79 of 272
Report Date: 03-Nov-2011 10:29:04 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Injection Date: 02-Nov-2011 14:51:42 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 10

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

28

Y ( X1000000)

C511K02016[MS QQQ Chro]:m/z 421.0 > 375.9 4.422

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

28

32

Y ( X100000)

C511K02016[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

28

32

Y ( X100000)

C511K02016[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

5

10

15

20

25

30

35

Y ( X1000000)

C511K02016[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

9

18

27

36

45

54

63

Y ( X100000)

C511K02016[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

5

10

15

20

25

30

35

Y ( X1000000)

C511K02016[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

9

18

27

36

45

54

63

Y ( X100000)

C511K02016[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

$ 6 13C8 PFOS

3 4 5

Min

0

9

18

27

36

45

54

63

72

Y ( X100000)

C511K02016[MS QQQ Chro]:m/z 506.9 > 80.0 4.570

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

2

4

6

8

10

12

Y ( X1000000)

C511K02016[MS QQQ Chro]:m/z 498.9 > 79.9 4.571

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02016[MS QQQ Chro]:m/z 498.9 > 98.9 4.571

* 5 13C4 PFOS (IS)

3 4 5

Min

4

14

24

34

44

54

64

74

Y ( X10000)

C511K02016[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

$ 8 13C4 PFOS

3 4 5

Min

4

14

24

34

44

54

64

74

Y ( X10000)

C511K02016[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

Page 80 of 272
Report Date: 03-Nov-2011 10:29:04 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Page 81 of 272
FORM VII

Lab Name: Job No.:

SDG No.:

Instrument ID:

Calibration Date:

Calib Start Date:

Lab Sample ID:

GC Column: ID: Calib End Date:

LCMS CONTINUING CALIBRATION DATA

280-21985-1

LC_LCMS5

11/02/2011 15:07

11/02/2011 13:49

11/02/2011 14:51

ICV 280-94589/12

Gemini-NX

TestAmerica Denver

Lab File ID: PC511K02018.d Conc. Units: ug/L

ANALYTE CURVE CALC SPIKE %D MAX

TYPE AMOUNT AMOUNT %D

AVE RRF RRF MIN RRF

Ammonium Perfluorooctanoate 

(APFO)

Lin1 0.9264 1.79 2.08 -14.0 20.0

Perfluorooctanoic acid 

(PFOA)

Lin1 0.9640 1.72 2.00 -14.0 20.0

Perfluorooctanoic Sulfonate Lin1 1.284 1.85 2.02 -8.4 20.0

13C8 PFOA Lin1 0.8633 2.04 2.00 2.0 20.0

13C4 PFOA Ave 2153400 2253292 10.5 10.0 4.6

13C8 PFOS Lin1 0.8917 1.91 1.91 -0.1 20.0

13C4 PFOS Ave 550386 570417 9.91 9.56 3.6

FORM VII DV-LC-0012

Page 82 of 272
Report Date: 03-Nov-2011 10:29:06 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02018.d

Lims ID: icv Client ID:

Inject. Date: 02-Nov-2011 15:07:11 Dil. Factor: 1.0000 

Sample Type: ICV

Sample ID: ICV, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 12

Sublist:

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.422 4.433 -0.011 1.000 3890502 2.04

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.423 4.434 -0.011 22532916 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.423 4.434 -0.011 22532916 10.5

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.424 4.435 -0.011 1.000 4344211 1.79 0.70- 1.30 1.00

 413.0 > 169.0 4.424 4.435 -0.011 1.000 806056 3.72- 6.92 5.39

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.424 4.435 -0.011 1.000 4344211 1.72 0.70- 1.30 1.00

 413.0 > 169.0 4.424 4.435 -0.011 1.000 806056 3.72- 6.92 5.39

$ 6 13C8 PFOS

 506.9 > 80.0 4.570 4.586 -0.016 1.000 972526 1.91

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.563 4.586 -0.024 0.998 1479752 1.85 0.70- 1.30 1.00

 498.9 > 98.9 4.571 4.586 -0.015 1.000 634846 1.30- 2.42 2.33

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.571 4.586 -0.015 5453191 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.571 4.586 -0.015 5453191 9.91

Page 83 of 272
Report Date: 03-Nov-2011 10:29:06 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02018.d

Injection Date: 02-Nov-2011 15:07:11 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 12

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

2

4

6

8

10

Y ( X100000)

C511K02018[MS QQQ Chro]:m/z 421.0 > 375.9 4.422

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02018[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02018[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

Y ( X100000)

C511K02018[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

7

10

13

16

19

22

25

Y ( X10000)

C511K02018[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

Y ( X100000)

C511K02018[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

7

10

13

16

19

22

25

Y ( X10000)

C511K02018[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

$ 6 13C8 PFOS

3 4 5

Min

4

8

12

16

20

24

28

Y ( X10000)

C511K02018[MS QQQ Chro]:m/z 506.9 > 80.0 4.570

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

8

12

16

20

24

28

32

Y ( X10000)

C511K02018[MS QQQ Chro]:m/z 498.9 > 79.9 4.563

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

6

8

10

12

14

16

18

Y ( X10000)

C511K02018[MS QQQ Chro]:m/z 498.9 > 98.9 4.571

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02018[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02018[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

Page 84 of 272
Report Date: 03-Nov-2011 10:29:06 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02018.d

Page 85 of 272
FORM VII

Lab Name: Job No.:

SDG No.:

Instrument ID:

Calibration Date:

Calib Start Date:

Lab Sample ID:

GC Column: ID: Calib End Date:

LCMS CONTINUING CALIBRATION DATA

280-21985-1

LC_LCMS5

11/02/2011 16:09

11/02/2011 13:49

11/02/2011 14:51

CCV 280-94589/20

Gemini-NX

TestAmerica Denver

Lab File ID: PC511K02026.d Conc. Units: ug/L

ANALYTE CURVE CALC SPIKE %D MAX

TYPE AMOUNT AMOUNT %D

AVE RRF RRF MIN RRF

Ammonium Perfluorooctanoate 

(APFO)

Lin1 1.051 5.25 5.20 0.9 20.0

Perfluorooctanoic acid 

(PFOA)

Lin1 1.094 5.04 5.00 0.8 20.0

Perfluorooctanoic Sulfonate Lin1 1.346 4.65 4.78 -2.7 20.0

13C8 PFOA Lin1 0.8369 5.06 5.00 1.2 20.0

13C4 PFOA Ave 2153400 2121411 9.85 10.0 -1.5

13C8 PFOS Lin1 0.9000 4.89 4.78 2.3 20.0

13C4 PFOS Ave 550386 528000 9.17 9.56 -4.1

FORM VII DV-LC-0012

Page 86 of 272
Report Date: 03-Nov-2011 10:29:12 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02026.d

Lims ID: CCV Client ID:

Inject. Date: 02-Nov-2011 16:09:03 Dil. Factor: 1.0000 

Sample Type: CCV

Sample ID: CCV, CCV L5, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 20

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:12 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.431 4.433 -0.002 1.000 8877243 5.06

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.432 4.434 -0.002 21214105 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.432 4.434 -0.002 21214105 9.85

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.424 4.435 -0.011 0.998 11605689 5.25 0.70- 1.30 1.00

 413.0 > 169.0 4.424 4.435 -0.011 0.998 2181081 3.72- 6.92 5.32

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.424 4.435 -0.011 0.998 11605689 5.04 0.70- 1.30 1.00

 413.0 > 169.0 4.424 4.435 -0.011 0.998 2181081 3.72- 6.92 5.32

$ 6 13C8 PFOS

 506.9 > 80.0 4.570 4.586 -0.016 1.000 2271484 4.89

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.571 4.586 -0.015 1.000 3395881 4.65 0.70- 1.30 1.00

 498.9 > 98.9 4.571 4.586 -0.015 1.000 1905688 1.30- 2.42 1.78

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.571 4.586 -0.015 5047678 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.571 4.586 -0.015 5047678 9.17

Page 87 of 272
Report Date: 03-Nov-2011 10:29:12 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02026.d

Injection Date: 02-Nov-2011 16:09:03 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 20

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

3

6

9

12

15

18

21

24

Y ( X100000)

C511K02026[MS QQQ Chro]:m/z 421.0 > 375.9 4.431

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02026[MS QQQ Chro]:m/z 417.0 > 371.9 4.432

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02026[MS QQQ Chro]:m/z 417.0 > 371.9 4.432

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

28

32

Y ( X100000)

C511K02026[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

12

20

28

36

44

52

60

Y ( X10000)

C511K02026[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

28

32

Y ( X100000)

C511K02026[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

12

20

28

36

44

52

60

Y ( X10000)

C511K02026[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

$ 6 13C8 PFOS

3 4 5

Min

4

13

22

31

40

49

58

67

Y ( X10000)

C511K02026[MS QQQ Chro]:m/z 506.9 > 80.0 4.570

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

16

28

40

52

64

76

88

Y ( X10000)

C511K02026[MS QQQ Chro]:m/z 498.9 > 79.9 4.571

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

11

18

25

32

39

46

53

Y ( X10000)

C511K02026[MS QQQ Chro]:m/z 498.9 > 98.9 4.571

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02026[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02026[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

Page 88 of 272
Report Date: 03-Nov-2011 10:29:12 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02026.d

Page 89 of 272
FORM VII

Lab Name: Job No.:

SDG No.:

Instrument ID:

Calibration Date:

Calib Start Date:

Lab Sample ID:

GC Column: ID: Calib End Date:

LCMS CONTINUING CALIBRATION DATA

280-21985-1

LC_LCMS5

11/02/2011 16:24

11/02/2011 13:49

11/02/2011 14:51

CCVL 280-94589/22

Gemini-NX

TestAmerica Denver

Lab File ID: PC511K02028.d Conc. Units: ug/L

ANALYTE CURVE CALC SPIKE %D MAX

TYPE AMOUNT AMOUNT %D

AVE RRF RRF MIN RRF

Ammonium Perfluorooctanoate 

(APFO)

Lin1 1.456 0.205 0.208 -1.7 30.0

Perfluorooctanoic acid 

(PFOA)

Lin1 1.499 0.193 0.200 -3.5 30.0

Perfluorooctanoic Sulfonate Lin1 1.834 0.209 0.191 9.2 30.0

13C8 PFOA Lin1 1.029 0.176 0.200 -11.8 30.0

13C4 PFOA Ave 2153400 2209935 10.3 10.0 2.6

13C8 PFOS Lin1 1.130 0.198 0.191 3.7 30.0

13C4 PFOS Ave 550386 552973 9.60 9.56 0.5

FORM VII DV-LC-0012

Page 90 of 272
Report Date: 03-Nov-2011 10:29:14 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02028.d

Lims ID: CCVL L1 Client ID:

Inject. Date: 02-Nov-2011 16:24:30 Dil. Factor: 1.0000 

Sample Type: CCVL

Sample ID: STD0002, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 22

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:13 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

First Level Reviewer: bonnettj Date: 03-Nov-2011 10:27:30

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.422 4.433 -0.011 1.000 454974 0.1764

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.423 4.434 -0.011 22099352 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.423 4.434 -0.011 22099352 10.3

 3 Ammonium Perfluorooctanoate (APFO) M

 413.0 > 368.9 4.424 4.435 -0.011 1.000 669691 0.2046 0.70- 1.30 1.00 M

 413.0 > 169.0 4.424 4.435 -0.011 1.000 115330 3.72- 6.92 5.81

 1 Perfluorooctanoic acid M

 413.0 > 368.9 4.424 4.435 -0.011 1.000 662476 0.1930 0.70- 1.30 1.00 M

 413.0 > 169.0 4.424 4.435 -0.011 1.000 115330 3.72- 6.92 5.74

$ 6 13C8 PFOS

 506.9 > 80.0 4.561 4.586 -0.025 0.998 119511 0.1982

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.563 4.586 -0.024 0.998 193917 0.2087 0.70- 1.30 1.00

 498.9 > 98.9 4.563 4.586 -0.024 0.998 93541 1.30- 2.42 2.07

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.571 4.586 -0.015 5286424 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.571 4.586 -0.015 5286424 9.60

Page 91 of 272
Report Date: 03-Nov-2011 10:29:14 Chrom Revision: 1.2 13-Jul-2011 10:43:06

QC Flag Legend

Review Flags

M - Manually Integrated

Page 92 of 272
Report Date: 03-Nov-2011 10:29:14 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02028.d

Injection Date: 02-Nov-2011 16:24:30 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 22

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

4

6

8

10

12

14

16

Y ( X10000)

C511K02028[MS QQQ Chro]:m/z 421.0 > 375.9 4.422

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02028[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02028[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

 3 Ammonium Perfluorooctanoate (APFO) (M)

2.9 3.9 4.9

Min

4

7

10

13

16

19

22

Y ( X10000)

C511K02028[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

41

46

51

56

61

66

71

Y ( X1000)

C511K02028[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

 1 Perfluorooctanoic acid (M)

2.9 3.9 4.9

Min

4

7

10

13

16

19

22

Y ( X10000)

C511K02028[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

41

46

51

56

61

66

71

Y ( X1000)

C511K02028[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

$ 6 13C8 PFOS

3 4 5

Min

41

46

51

56

61

66

71

Y ( X1000)

C511K02028[MS QQQ Chro]:m/z 506.9 > 80.0 4.561

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

41

47

53

59

65

71

77

83

Y ( X1000)

C511K02028[MS QQQ Chro]:m/z 498.9 > 79.9 4.563

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

41

45

49

53

57

61

65

69

Y ( X1000)

C511K02028[MS QQQ Chro]:m/z 498.9 > 98.9 4.563

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02028[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02028[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

Page 93 of 272
Report Date: 03-Nov-2011 10:29:14 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02028.d

Page 94 of 272
Report Date: 03-Nov-2011 10:29:14 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Manual Integration/User Assign Peak Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02028.d

Injection Date: 02-Nov-2011 16:24:30 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 22

Operator ID: TW/JB Injection Vol: 20.00 ul

 3 Ammonium Perfluorooctanoate (APFO), Signal: 1, m/z: 413.0 > 368.9 Type: quant, RT: 4.44

Processing Integration Results

RT: 4.42

Response: 604504

Amount: 0.175797

4.02

Min

4

6

8

10

12

14

16

18

20

22

24

Y ( X10000)

C511K02028[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

Manual Integration Results

RT: 4.42

Response: 669691

Amount: 0.204588

4.04

Min

4

6

8

10

12

14

16

18

20

22

24

Y ( X10000)

C511K02028[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

Reviewer: bonnettj, 03-Nov-2011 10:27:30

Audit Action: Manually Integrated

Audit Reason: Baseline

Page 95 of 272
Report Date: 03-Nov-2011 10:29:14 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Manual Integration/User Assign Peak Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02028.d

Injection Date: 02-Nov-2011 16:24:30 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 22

Operator ID: TW/JB Injection Vol: 20.00 ul

 1 Perfluorooctanoic acid, Signal: 1, m/z: 413.0 > 368.9 Type: quant, RT: 4.44

Processing Integration Results

RT: 4.42

Response: 604504

Amount: 0.168424

4.02

Min

4

6

8

10

12

14

16

18

20

22

24

Y ( X10000)

C511K02028[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

Manual Integration Results

RT: 4.42

Response: 662476

Amount: 0.193029

4.04

Min

4

6

8

10

12

14

16

18

20

22

24

Y ( X10000)

C511K02028[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

Reviewer: bonnettj, 03-Nov-2011 10:27:30

Audit Action: Manually Integrated

Audit Reason: Baseline

Page 96 of 272
FORM VII

Lab Name: Job No.:

SDG No.:

Instrument ID:

Calibration Date:

Calib Start Date:

Lab Sample ID:

GC Column: ID: Calib End Date:

LCMS CONTINUING CALIBRATION DATA

280-21985-1

LC_LCMS5

11/02/2011 16:32

11/02/2011 13:49

11/02/2011 14:51

CCVL 280-94589/23

Gemini-NX

TestAmerica Denver

Lab File ID: PC511K02029.d Conc. Units: ug/L

ANALYTE CURVE CALC SPIKE %D MAX

TYPE AMOUNT AMOUNT %D

AVE RRF RRF MIN RRF

Ammonium Perfluorooctanoate 

(APFO)

Lin1 1.224 0.530 0.520 1.9 30.0

Perfluorooctanoic acid 

(PFOA)

Lin1 1.273 0.509 0.500 1.8 30.0

Perfluorooctanoic Sulfonate Lin1 1.470 0.466 0.478 -2.5 30.0

13C8 PFOA Lin1 0.9244 0.491 0.500 -1.8 30.0

13C4 PFOA Ave 2153400 2172383 10.1 10.0 0.9

13C8 PFOS Lin1 1.025 0.513 0.478 7.2 30.0

13C4 PFOS Ave 550386 542774 9.43 9.56 -1.4

FORM VII DV-LC-0012

Page 97 of 272
Report Date: 03-Nov-2011 10:29:14 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02029.d

Lims ID: CCVL L2 Client ID:

Inject. Date: 02-Nov-2011 16:32:16 Dil. Factor: 1.0000 

Sample Type: CCVL

Sample ID: STD0005, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 23

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:14 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.422 4.433 -0.011 1.000 1004086 0.4912

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.423 4.434 -0.011 21723829 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.423 4.434 -0.011 21723829 10.1

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.424 4.435 -0.011 1.000 1383178 0.5303 0.70- 1.30 1.00

 413.0 > 169.0 4.424 4.435 -0.011 1.000 235779 3.72- 6.92 5.87

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.424 4.435 -0.011 1.000 1383178 0.5091 0.70- 1.30 1.00

 413.0 > 169.0 4.424 4.435 -0.011 1.000 235779 3.72- 6.92 5.87

$ 6 13C8 PFOS

 506.9 > 80.0 4.561 4.586 -0.025 1.000 265950 0.5126

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.563 4.586 -0.024 1.000 381316 0.4659 0.70- 1.30 1.00

 498.9 > 98.9 4.563 4.586 -0.024 1.000 214039 1.30- 2.42 1.78

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.562 4.586 -0.024 5188919 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.562 4.586 -0.024 5188919 9.43

Page 98 of 272
Report Date: 03-Nov-2011 10:29:15 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02029.d

Injection Date: 02-Nov-2011 16:32:16 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 23

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

4

8

12

16

20

24

28

Y ( X10000)

C511K02029[MS QQQ Chro]:m/z 421.0 > 375.9 4.422

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02029[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02029[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

9

14

19

24

29

34

39

44

Y ( X10000)

C511K02029[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

41

50

59

68

77

86

95

104

Y ( X1000)

C511K02029[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

9

14

19

24

29

34

39

44

Y ( X10000)

C511K02029[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

41

50

59

68

77

86

95

104

Y ( X1000)

C511K02029[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

$ 6 13C8 PFOS

3 4 5

Min

41

51

61

71

81

91

101

111

Y ( X1000)

C511K02029[MS QQQ Chro]:m/z 506.9 > 80.0 4.561

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

6

8

10

12

14

Y ( X10000)

C511K02029[MS QQQ Chro]:m/z 498.9 > 79.9 4.563

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

41

49

57

65

73

81

89

97

Y ( X1000)

C511K02029[MS QQQ Chro]:m/z 498.9 > 98.9 4.563

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02029[MS QQQ Chro]:m/z 502.9 > 80.0 4.562

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02029[MS QQQ Chro]:m/z 502.9 > 80.0 4.562

Page 99 of 272
Report Date: 03-Nov-2011 10:29:15 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02029.d

Page 100 of 272
FORM VII

Lab Name: Job No.:

SDG No.:

Instrument ID:

Calibration Date:

Calib Start Date:

Lab Sample ID:

GC Column: ID: Calib End Date:

LCMS CONTINUING CALIBRATION DATA

280-21985-1

LC_LCMS5

11/02/2011 16:39

11/02/2011 13:49

11/02/2011 14:51

CCVL 280-94589/24

Gemini-NX

TestAmerica Denver

Lab File ID: PC511K02030.d Conc. Units: ug/L

ANALYTE CURVE CALC SPIKE %D MAX

TYPE AMOUNT AMOUNT %D

AVE RRF RRF MIN RRF

Ammonium Perfluorooctanoate 

(APFO)

Lin1 1.121 1.05 1.04 0.9 30.0

Perfluorooctanoic acid 

(PFOA)

Lin1 1.166 1.01 1.00 1.0 30.0

Perfluorooctanoic Sulfonate Lin1 1.468 0.978 0.956 2.3 30.0

13C8 PFOA Lin1 0.8922 1.02 1.00 2.0 30.0

13C4 PFOA Ave 2153400 2223136 10.3 10.0 3.2

13C8 PFOS Lin1 0.9528 1.00 0.956 4.6 30.0

13C4 PFOS Ave 550386 560829 9.74 9.56 1.9

FORM VII DV-LC-0012

Page 101 of 272
Report Date: 03-Nov-2011 10:29:15 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02030.d

Lims ID: CCVL L3 Client ID:

Inject. Date: 02-Nov-2011 16:39:59 Dil. Factor: 1.0000 

Sample Type: CCVL

Sample ID: STD0010, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 24

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:15 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.413 4.433 -0.020 1.000 1983536 1.02

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.414 4.434 -0.020 22231363 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.414 4.434 -0.020 22231363 10.3

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.415 4.435 -0.020 1.000 2593215 1.05 0.70- 1.30 1.00

 413.0 > 169.0 4.415 4.435 -0.020 1.000 482610 3.72- 6.92 5.37

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.415 4.435 -0.020 1.000 2593215 1.01 0.70- 1.30 1.00

 413.0 > 169.0 4.415 4.435 -0.020 1.000 482610 3.72- 6.92 5.37

$ 6 13C8 PFOS

 506.9 > 80.0 4.561 4.586 -0.025 1.000 510829 1.00

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.563 4.586 -0.024 1.000 786956 0.9779 0.70- 1.30 1.00

 498.9 > 98.9 4.563 4.586 -0.024 1.000 426318 1.30- 2.42 1.85

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.562 4.586 -0.024 5361524 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.562 4.586 -0.024 5361524 9.74

Page 102 of 272
Report Date: 03-Nov-2011 10:29:15 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02030.d

Injection Date: 02-Nov-2011 16:39:59 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 24

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

4

11

18

25

32

39

46

53

60

Y ( X10000)

C511K02030[MS QQQ Chro]:m/z 421.0 > 375.9 4.413

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02030[MS QQQ Chro]:m/z 417.0 > 371.9 4.414

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02030[MS QQQ Chro]:m/z 417.0 > 371.9 4.414

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

13

22

31

40

49

58

67

76

Y ( X10000)

C511K02030[MS QQQ Chro]:m/z 413.0 > 368.9 4.415

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

6

8

10

12

14

16

18

Y ( X10000)

C511K02030[MS QQQ Chro]:m/z 413.0 > 169.0 4.415

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

13

22

31

40

49

58

67

76

Y ( X10000)

C511K02030[MS QQQ Chro]:m/z 413.0 > 368.9 4.415

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

6

8

10

12

14

16

18

Y ( X10000)

C511K02030[MS QQQ Chro]:m/z 413.0 > 169.0 4.415

$ 6 13C8 PFOS

3 4 5

Min

4

6

8

10

12

14

16

18

Y ( X10000)

C511K02030[MS QQQ Chro]:m/z 506.9 > 80.0 4.561

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

7

10

13

16

19

22

25

Y ( X10000)

C511K02030[MS QQQ Chro]:m/z 498.9 > 79.9 4.563

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

6

8

10

12

14

16

Y ( X10000)

C511K02030[MS QQQ Chro]:m/z 498.9 > 98.9 4.563

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02030[MS QQQ Chro]:m/z 502.9 > 80.0 4.562

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02030[MS QQQ Chro]:m/z 502.9 > 80.0 4.562

Page 103 of 272
Report Date: 03-Nov-2011 10:29:15 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02030.d

Page 104 of 272
FORM VII

Lab Name: Job No.:

SDG No.:

Instrument ID:

Calibration Date:

Calib Start Date:

Lab Sample ID:

GC Column: ID: Calib End Date:

LCMS CONTINUING CALIBRATION DATA

280-21985-1

LC_LCMS5

11/02/2011 16:47

11/02/2011 13:49

11/02/2011 14:51

CCVL 280-94589/25

Gemini-NX

TestAmerica Denver

Lab File ID: PC511K02031.d Conc. Units: ug/L

ANALYTE CURVE CALC SPIKE %D MAX

TYPE AMOUNT AMOUNT %D

AVE RRF RRF MIN RRF

Ammonium Perfluorooctanoate 

(APFO)

Lin1 1.054 2.05 2.08 -1.5 30.0

Perfluorooctanoic acid 

(PFOA)

Lin1 1.097 1.97 2.00 -1.5 30.0

Perfluorooctanoic Sulfonate Lin1 1.272 1.73 1.91 -9.5 30.0

13C8 PFOA Lin1 0.8616 2.04 2.00 2.0 30.0

13C4 PFOA Ave 2153400 2221836 10.3 10.0 3.2

13C8 PFOS Lin1 0.8984 1.92 1.91 0.4 30.0

13C4 PFOS Ave 550386 567461 9.86 9.56 3.1

FORM VII DV-LC-0012

Page 105 of 272
Report Date: 03-Nov-2011 10:29:16 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02031.d

Lims ID: CCVL L4 Client ID:

Inject. Date: 02-Nov-2011 16:47:42 Dil. Factor: 1.0000 

Sample Type: CCVL

Sample ID: STD0020, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 25

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:16 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.422 4.433 -0.011 1.000 3828522 2.04

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.423 4.434 -0.011 22218360 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.423 4.434 -0.011 22218360 10.3

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.424 4.435 -0.011 1.000 4872898 2.05 0.70- 1.30 1.00

 413.0 > 169.0 4.415 4.435 -0.020 0.998 937631 3.72- 6.92 5.20

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.424 4.435 -0.011 1.000 4872898 1.97 0.70- 1.30 1.00

 413.0 > 169.0 4.415 4.435 -0.020 0.998 937631 3.72- 6.92 5.20

$ 6 13C8 PFOS

 506.9 > 80.0 4.561 4.586 -0.025 1.000 974794 1.92

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.563 4.586 -0.024 1.000 1380417 1.73 0.70- 1.30 1.00

 498.9 > 98.9 4.563 4.586 -0.024 1.000 772038 1.30- 2.42 1.79

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.562 4.586 -0.024 5424923 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.562 4.586 -0.024 5424923 9.86

Page 106 of 272
Report Date: 03-Nov-2011 10:29:16 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02031.d

Injection Date: 02-Nov-2011 16:47:42 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 25

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

2

4

6

8

10

Y ( X100000)

C511K02031[MS QQQ Chro]:m/z 421.0 > 375.9 4.422

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02031[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02031[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02031[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

8

12

16

20

24

28

Y ( X10000)

C511K02031[MS QQQ Chro]:m/z 413.0 > 169.0 4.415

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02031[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

8

12

16

20

24

28

Y ( X10000)

C511K02031[MS QQQ Chro]:m/z 413.0 > 169.0 4.415

$ 6 13C8 PFOS

3 4 5

Min

4

8

12

16

20

24

28

32

Y ( X10000)

C511K02031[MS QQQ Chro]:m/z 506.9 > 80.0 4.561

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

9

14

19

24

29

34

39

Y ( X10000)

C511K02031[MS QQQ Chro]:m/z 498.9 > 79.9 4.563

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

7

10

13

16

19

22

25

Y ( X10000)

C511K02031[MS QQQ Chro]:m/z 498.9 > 98.9 4.563

* 5 13C4 PFOS (IS)

3 4 5

Min

0

3

6

9

12

15

Y ( X100000)

C511K02031[MS QQQ Chro]:m/z 502.9 > 80.0 4.562

$ 8 13C4 PFOS

3 4 5

Min

0

3

6

9

12

15

Y ( X100000)

C511K02031[MS QQQ Chro]:m/z 502.9 > 80.0 4.562

Page 107 of 272
Report Date: 03-Nov-2011 10:29:16 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02031.d

Page 108 of 272
FORM VII

Lab Name: Job No.:

SDG No.:

Instrument ID:

Calibration Date:

Calib Start Date:

Lab Sample ID:

GC Column: ID: Calib End Date:

LCMS CONTINUING CALIBRATION DATA

280-21985-1

LC_LCMS5

11/02/2011 16:55

11/02/2011 13:49

11/02/2011 14:51

CCV 280-94589/26

Gemini-NX

TestAmerica Denver

Lab File ID: PC511K02032.d Conc. Units: ug/L

ANALYTE CURVE CALC SPIKE %D MAX

TYPE AMOUNT AMOUNT %D

AVE RRF RRF MIN RRF

Ammonium Perfluorooctanoate 

(APFO)

Lin1 1.055 5.27 5.20 1.3 20.0

Perfluorooctanoic acid 

(PFOA)

Lin1 1.098 5.06 5.00 1.2 20.0

Perfluorooctanoic Sulfonate Lin1 1.338 4.62 4.78 -3.3 20.0

13C8 PFOA Lin1 0.8606 5.21 5.00 4.2 20.0

13C4 PFOA Ave 2153400 2159755 10.0 10.0 0.3

13C8 PFOS Lin1 0.9171 4.98 4.78 4.2 20.0

13C4 PFOS Ave 550386 556188 9.66 9.56 1.1

FORM VII DV-LC-0012

Page 109 of 272
Report Date: 03-Nov-2011 10:29:17 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02032.d

Lims ID: CCV L5 Client ID:

Inject. Date: 02-Nov-2011 16:55:27 Dil. Factor: 1.0000 

Sample Type: CCV

Sample ID: STD0050, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 26

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:17 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.413 4.433 -0.020 1.000 9293452 5.21

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.414 4.434 -0.020 21597553 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.414 4.434 -0.020 21597553 10.0

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.415 4.435 -0.020 1.000 11852498 5.27 0.70- 1.30 1.00

 413.0 > 169.0 4.415 4.435 -0.020 1.000 2266559 3.72- 6.92 5.23

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.415 4.435 -0.020 1.000 11852498 5.06 0.70- 1.30 1.00

 413.0 > 169.0 4.415 4.435 -0.020 1.000 2266559 3.72- 6.92 5.23

$ 6 13C8 PFOS

 506.9 > 80.0 4.561 4.586 -0.025 1.000 2438267 4.98

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.554 4.586 -0.032 0.998 3556163 4.62 0.70- 1.30 1.00

 498.9 > 98.9 4.563 4.586 -0.024 1.000 1937204 1.30- 2.42 1.84

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.562 4.586 -0.024 5317161 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.562 4.586 -0.024 5317161 9.66

Page 110 of 272
Report Date: 03-Nov-2011 10:29:17 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02032.d

Injection Date: 02-Nov-2011 16:55:27 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 26

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

Y ( X100000)

C511K02032[MS QQQ Chro]:m/z 421.0 > 375.9 4.413

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02032[MS QQQ Chro]:m/z 417.0 > 371.9 4.414

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02032[MS QQQ Chro]:m/z 417.0 > 371.9 4.414

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

28

32

Y ( X100000)

C511K02032[MS QQQ Chro]:m/z 413.0 > 368.9 4.415

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

12

20

28

36

44

52

60

Y ( X10000)

C511K02032[MS QQQ Chro]:m/z 413.0 > 169.0 4.415

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

28

32

Y ( X100000)

C511K02032[MS QQQ Chro]:m/z 413.0 > 368.9 4.415

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

12

20

28

36

44

52

60

Y ( X10000)

C511K02032[MS QQQ Chro]:m/z 413.0 > 169.0 4.415

$ 6 13C8 PFOS

3 4 5

Min

4

13

22

31

40

49

58

67

Y ( X10000)

C511K02032[MS QQQ Chro]:m/z 506.9 > 80.0 4.561

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

17

30

43

56

69

82

95

Y ( X10000)

C511K02032[MS QQQ Chro]:m/z 498.9 > 79.9 4.554

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

11

18

25

32

39

46

53

Y ( X10000)

C511K02032[MS QQQ Chro]:m/z 498.9 > 98.9 4.563

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02032[MS QQQ Chro]:m/z 502.9 > 80.0 4.562

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02032[MS QQQ Chro]:m/z 502.9 > 80.0 4.562

Page 111 of 272
Report Date: 03-Nov-2011 10:29:17 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02032.d

Page 112 of 272
FORM VII

Lab Name: Job No.:

SDG No.:

Instrument ID:

Calibration Date:

Calib Start Date:

Lab Sample ID:

GC Column: ID: Calib End Date:

LCMS CONTINUING CALIBRATION DATA

280-21985-1

LC_LCMS5

11/02/2011 17:03

11/02/2011 13:49

11/02/2011 14:51

CCVL 280-94589/27

Gemini-NX

TestAmerica Denver

Lab File ID: PC511K02033.d Conc. Units: ug/L

ANALYTE CURVE CALC SPIKE %D MAX

TYPE AMOUNT AMOUNT %D

AVE RRF RRF MIN RRF

Ammonium Perfluorooctanoate 

(APFO)

Lin1 1.018 10.3 10.4 -1.0 30.0

Perfluorooctanoic acid 

(PFOA)

Lin1 1.060 9.85 10.0 -1.5 30.0

Perfluorooctanoic Sulfonate Lin1 1.321 9.18 9.56 -4.0 30.0

13C8 PFOA Lin1 0.8391 10.2 10.0 2.0 30.0

13C4 PFOA Ave 2153400 2201775 10.2 10.0 2.2

13C4 PFOS Ave 550386 571245 9.92 9.56 3.8

13C8 PFOS Lin1 0.8929 9.75 9.56 2.0 30.0

FORM VII DV-LC-0012

Page 113 of 272
Report Date: 03-Nov-2011 10:29:18 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02033.d

Lims ID: CCVL L6 Client ID:

Inject. Date: 02-Nov-2011 17:03:11 Dil. Factor: 1.0000 

Sample Type: CCVL

Sample ID: STD0100, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 27

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:18 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.413 4.433 -0.020 1.000 18474100 10.2

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.414 4.434 -0.020 22017750 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.414 4.434 -0.020 22017750 10.2

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.415 4.435 -0.020 1.000 23328820 10.3 0.70- 1.30 1.00

 413.0 > 169.0 4.415 4.435 -0.020 1.000 4452211 3.72- 6.92 5.24

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.415 4.435 -0.020 1.000 23328820 9.85 0.70- 1.30 1.00

 413.0 > 169.0 4.415 4.435 -0.020 1.000 4452211 3.72- 6.92 5.24

$ 6 13C8 PFOS

 506.9 > 80.0 4.561 4.586 -0.025 1.002 4876213 9.75

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.554 4.586 -0.032 1.000 7213312 9.18 0.70- 1.30 1.00

 498.9 > 98.9 4.554 4.586 -0.032 1.000 3967726 1.30- 2.42 1.82

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.553 4.586 -0.033 5461101 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.553 4.586 -0.033 5461101 9.92

Page 114 of 272
Report Date: 03-Nov-2011 10:29:18 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02033.d

Injection Date: 02-Nov-2011 17:03:11 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 27

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

7

14

21

28

35

42

49

Y ( X100000)

C511K02033[MS QQQ Chro]:m/z 421.0 > 375.9 4.413

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02033[MS QQQ Chro]:m/z 417.0 > 371.9 4.414

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02033[MS QQQ Chro]:m/z 417.0 > 371.9 4.414

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02033[MS QQQ Chro]:m/z 413.0 > 368.9 4.415

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

Y ( X100000)

C511K02033[MS QQQ Chro]:m/z 413.0 > 169.0 4.415

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02033[MS QQQ Chro]:m/z 413.0 > 368.9 4.415

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

Y ( X100000)

C511K02033[MS QQQ Chro]:m/z 413.0 > 169.0 4.415

$ 6 13C8 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02033[MS QQQ Chro]:m/z 506.9 > 80.0 4.561

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

3

6

9

12

15

18

21

Y ( X100000)

C511K02033[MS QQQ Chro]:m/z 498.9 > 79.9 4.554

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

2

4

6

8

10

12

Y ( X100000)

C511K02033[MS QQQ Chro]:m/z 498.9 > 98.9 4.554

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02033[MS QQQ Chro]:m/z 502.9 > 80.0 4.553

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02033[MS QQQ Chro]:m/z 502.9 > 80.0 4.553

Page 115 of 272
Report Date: 03-Nov-2011 10:29:18 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02033.d

Page 116 of 272
FORM VII

Lab Name: Job No.:

SDG No.:

Instrument ID:

Calibration Date:

Calib Start Date:

Lab Sample ID:

GC Column: ID: Calib End Date:

LCMS CONTINUING CALIBRATION DATA

280-21985-1

LC_LCMS5

11/02/2011 17:10

11/02/2011 13:49

11/02/2011 14:51

CCV 280-94589/28

Gemini-NX

TestAmerica Denver

Lab File ID: PC511K02034.d Conc. Units: ug/L

ANALYTE CURVE CALC SPIKE %D MAX

TYPE AMOUNT AMOUNT %D

AVE RRF RRF MIN RRF

Ammonium Perfluorooctanoate 

(APFO)

Lin1 1.074 21.7 20.8 4.3 20.0

Perfluorooctanoic acid 

(PFOA)

Lin1 1.118 20.9 20.0 4.5 20.0

Perfluorooctanoic Sulfonate Lin1 1.356 18.9 19.1 -1.2 20.0

13C8 PFOA Lin1 0.8668 21.2 20.0 6.0 20.0

13C4 PFOA Ave 2153400 1922920 8.93 10.0 -10.7

13C8 PFOS Lin1 0.9005 19.7 19.1 3.0 20.0

13C4 PFOS Ave 550386 522306 9.07 9.56 -5.1

FORM VII DV-LC-0012

Page 117 of 272
Report Date: 03-Nov-2011 10:29:19 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02034.d

Lims ID: CCV L7 Client ID:

Inject. Date: 02-Nov-2011 17:10:55 Dil. Factor: 1.0000 

Sample Type: CCV

Sample ID: STD0200, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 28

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:18 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.413 4.433 -0.020 1.000 33334469 21.2

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.414 4.434 -0.020 19229199 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.414 4.434 -0.020 19229199 8.93

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.415 4.435 -0.020 1.000 42980700 21.7 0.70- 1.30 1.00

 413.0 > 169.0 4.415 4.435 -0.020 1.000 8308989 3.72- 6.92 5.17

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.415 4.435 -0.020 1.000 42980700 20.9 0.70- 1.30 1.00

 413.0 > 169.0 4.415 4.435 -0.020 1.000 8308989 3.72- 6.92 5.17

$ 6 13C8 PFOS

 506.9 > 80.0 4.561 4.586 -0.025 1.000 8993257 19.7

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.554 4.586 -0.032 0.998 13544804 18.9 0.70- 1.30 1.00

 498.9 > 98.9 4.554 4.586 -0.032 0.998 7463107 1.30- 2.42 1.81

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.562 4.586 -0.024 4993248 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.562 4.586 -0.024 4993248 9.07

Page 118 of 272
Report Date: 03-Nov-2011 10:29:19 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02034.d

Injection Date: 02-Nov-2011 17:10:55 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 28

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

11

22

33

44

55

66

77

88

Y ( X100000)

C511K02034[MS QQQ Chro]:m/z 421.0 > 375.9 4.413

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

7

14

21

28

35

42

49

Y ( X100000)

C511K02034[MS QQQ Chro]:m/z 417.0 > 371.9 4.414

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

7

14

21

28

35

42

49

Y ( X100000)

C511K02034[MS QQQ Chro]:m/z 417.0 > 371.9 4.414

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

Y ( X1000000)

C511K02034[MS QQQ Chro]:m/z 413.0 > 368.9 4.415

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

3

6

9

12

15

18

21

Y ( X100000)

C511K02034[MS QQQ Chro]:m/z 413.0 > 169.0 4.415

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

Y ( X1000000)

C511K02034[MS QQQ Chro]:m/z 413.0 > 368.9 4.415

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

3

6

9

12

15

18

21

Y ( X100000)

C511K02034[MS QQQ Chro]:m/z 413.0 > 169.0 4.415

$ 6 13C8 PFOS

3 4 5

Min

0

4

8

12

16

20

24

Y ( X100000)

C511K02034[MS QQQ Chro]:m/z 506.9 > 80.0 4.561

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

5

10

15

20

25

30

35

Y ( X100000)

C511K02034[MS QQQ Chro]:m/z 498.9 > 79.9 4.554

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

3

6

9

12

15

18

21

Y ( X100000)

C511K02034[MS QQQ Chro]:m/z 498.9 > 98.9 4.554

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02034[MS QQQ Chro]:m/z 502.9 > 80.0 4.562

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02034[MS QQQ Chro]:m/z 502.9 > 80.0 4.562

Page 119 of 272
Report Date: 03-Nov-2011 10:29:19 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02034.d

Page 120 of 272
FORM VII

Lab Name: Job No.:

SDG No.:

Instrument ID:

Calibration Date:

Calib Start Date:

Lab Sample ID:

GC Column: ID: Calib End Date:

LCMS CONTINUING CALIBRATION DATA

280-21985-1

LC_LCMS5

11/02/2011 17:18

11/02/2011 13:49

11/02/2011 14:51

CCVL 280-94589/29

Gemini-NX

TestAmerica Denver

Lab File ID: PC511K02035.d Conc. Units: ug/L

ANALYTE CURVE CALC SPIKE %D MAX

TYPE AMOUNT AMOUNT %D

AVE RRF RRF MIN RRF

Ammonium Perfluorooctanoate 

(APFO)

Lin1 1.016 51.5 52.0 -1.0 30.0

Perfluorooctanoic acid 

(PFOA)

Lin1 1.058 49.5 50.0 -1.0 30.0

Perfluorooctanoic Sulfonate Lin1 1.347 47.0 47.8 -1.7 30.0

13C8 PFOA Lin1 0.7935 48.6 50.0 -2.8 30.0

13C4 PFOA Ave 2153400 1744580 8.10 10.0 -19.0

13C8 PFOS Lin1 0.8515 46.7 47.8 -2.3 30.0

13C4 PFOS Ave 550386 453885 7.88 9.56 -17.5

FORM VII DV-LC-0012

Page 121 of 272
Report Date: 03-Nov-2011 10:29:19 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02035.d

Lims ID: CCVL L8 Client ID:

Inject. Date: 02-Nov-2011 17:18:37 Dil. Factor: 1.0000 

Sample Type: CCVL

Sample ID: STD0500, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 29

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:19 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.413 4.433 -0.020 1.000 69216654 48.6

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.414 4.434 -0.020 17445801 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.414 4.434 -0.020 17445801 8.10

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.415 4.435 -0.020 1.000 92245784 51.5 0.70- 1.30 1.00

 413.0 > 169.0 4.415 4.435 -0.020 1.000 17562948 3.72- 6.92 5.25

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.415 4.435 -0.020 1.000 92245784 49.5 0.70- 1.30 1.00

 413.0 > 169.0 4.415 4.435 -0.020 1.000 17562948 3.72- 6.92 5.25

$ 6 13C8 PFOS

 506.9 > 80.0 4.552 4.586 -0.034 1.000 18474613 46.7

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.554 4.586 -0.032 1.000 29215030 47.0 0.70- 1.30 1.00

 498.9 > 98.9 4.554 4.586 -0.032 1.000 16086574 1.30- 2.42 1.82

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.553 4.586 -0.033 4339142 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.553 4.586 -0.033 4339142 7.88

Page 122 of 272
Report Date: 03-Nov-2011 10:29:19 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02035.d

Injection Date: 02-Nov-2011 17:18:37 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 29

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

3

6

9

12

15

18

Y ( X1000000)

C511K02035[MS QQQ Chro]:m/z 421.0 > 375.9 4.413

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

6

12

18

24

30

36

42

Y ( X100000)

C511K02035[MS QQQ Chro]:m/z 417.0 > 371.9 4.414

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

6

12

18

24

30

36

42

Y ( X100000)

C511K02035[MS QQQ Chro]:m/z 417.0 > 371.9 4.414

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

3

6

9

12

15

18

21

Y ( X1000000)

C511K02035[MS QQQ Chro]:m/z 413.0 > 368.9 4.415

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

6

12

18

24

30

36

42

Y ( X100000)

C511K02035[MS QQQ Chro]:m/z 413.0 > 169.0 4.415

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

3

6

9

12

15

18

21

Y ( X1000000)

C511K02035[MS QQQ Chro]:m/z 413.0 > 368.9 4.415

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

6

12

18

24

30

36

42

Y ( X100000)

C511K02035[MS QQQ Chro]:m/z 413.0 > 169.0 4.415

$ 6 13C8 PFOS

3 4 5

Min

0

6

12

18

24

30

36

42

Y ( X100000)

C511K02035[MS QQQ Chro]:m/z 506.9 > 80.0 4.552

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

10

20

30

40

50

60

70

Y ( X100000)

C511K02035[MS QQQ Chro]:m/z 498.9 > 79.9 4.554

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

6

12

18

24

30

36

Y ( X100000)

C511K02035[MS QQQ Chro]:m/z 498.9 > 98.9 4.554

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

Y ( X100000)

C511K02035[MS QQQ Chro]:m/z 502.9 > 80.0 4.553

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

Y ( X100000)

C511K02035[MS QQQ Chro]:m/z 502.9 > 80.0 4.553

Page 123 of 272
Report Date: 03-Nov-2011 10:29:20 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02035.d

Page 124 of 272
FORM VII

Lab Name: Job No.:

SDG No.:

Instrument ID:

Calibration Date:

Calib Start Date:

Lab Sample ID:

GC Column: ID: Calib End Date:

LCMS CONTINUING CALIBRATION DATA

280-21985-1

LC_LCMS5

11/02/2011 17:26

11/02/2011 13:49

11/02/2011 14:51

CCVL 280-94589/30

Gemini-NX

TestAmerica Denver

Lab File ID: PC511K02036.d Conc. Units: ug/L

ANALYTE CURVE CALC SPIKE %D MAX

TYPE AMOUNT AMOUNT %D

AVE RRF RRF MIN RRF

Ammonium Perfluorooctanoate 

(APFO)

Lin1 0.8797 112 130 -14.2 30.0

Perfluorooctanoic acid 

(PFOA)

Lin1 0.9154 107 125 -14.2 30.0

Perfluorooctanoic Sulfonate Lin1 1.178 103 120 -14.0 30.0

13C8 PFOA Lin1 0.7055 108 125 -13.4 30.0

13C4 PFOA Ave 2153400 1426912 6.63 10.0 -33.7

13C8 PFOS Lin1 0.7564 104 120 -13.2 30.0

13C4 PFOS Ave 550386 367327 6.38 9.56 -33.3

FORM VII DV-LC-0012

Page 125 of 272
Report Date: 03-Nov-2011 10:29:20 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02036.d

Lims ID: CCVL L9 Client ID:

Inject. Date: 02-Nov-2011 17:26:20 Dil. Factor: 1.0000 

Sample Type: CCVL

Sample ID: STD1250, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 30

Sublist: chrom-8321_PFOA_S_Dupont*sub1

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:20 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.413 4.433 -0.020 1.000 125830388 108.2

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.414 4.434 -0.020 14269120 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.414 4.434 -0.020 14269120 6.63

 3 Ammonium Perfluorooctanoate (APFO) E

 413.0 > 368.9 4.415 4.435 -0.020 1.000 163277029 111.6 0.70- 1.30 1.00 E

 413.0 > 169.0 4.406 4.435 -0.029 0.998 31020574 3.72- 6.92 5.26

 1 Perfluorooctanoic acid E

 413.0 > 368.9 4.415 4.435 -0.020 1.000 163277029 107.2 0.70- 1.30 1.00 E

 413.0 > 169.0 4.406 4.435 -0.029 0.998 31020574 3.72- 6.92 5.26

$ 6 13C8 PFOS

 506.9 > 80.0 4.552 4.586 -0.034 1.000 33201962 103.7

 2 Perfluorooctanoic Sulfonate E

 498.9 > 79.9 4.554 4.586 -0.032 1.000 51703144 102.8 0.70- 1.30 1.00 E

 498.9 > 98.9 4.554 4.586 -0.032 1.000 28344659 1.30- 2.42 1.82

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.553 4.586 -0.033 3511649 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.553 4.586 -0.033 3511649 6.38

QC Flag Legend

Processing Flags

E - Exceeded Maximum Amount

Page 126 of 272
Report Date: 03-Nov-2011 10:29:20 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02036.d

Injection Date: 02-Nov-2011 17:26:20 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 30

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

28

Y ( X1000000)

C511K02036[MS QQQ Chro]:m/z 421.0 > 375.9 4.413

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

28

32

Y ( X100000)

C511K02036[MS QQQ Chro]:m/z 417.0 > 371.9 4.414

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

28

32

Y ( X100000)

C511K02036[MS QQQ Chro]:m/z 417.0 > 371.9 4.414

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

5

10

15

20

25

30

35

Y ( X1000000)

C511K02036[MS QQQ Chro]:m/z 413.0 > 368.9 4.415

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

9

18

27

36

45

54

63

Y ( X100000)

C511K02036[MS QQQ Chro]:m/z 413.0 > 169.0 4.406

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

5

10

15

20

25

30

35

Y ( X1000000)

C511K02036[MS QQQ Chro]:m/z 413.0 > 368.9 4.415

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

9

18

27

36

45

54

63

Y ( X100000)

C511K02036[MS QQQ Chro]:m/z 413.0 > 169.0 4.406

$ 6 13C8 PFOS

3 4 5

Min

0

9

18

27

36

45

54

63

72

Y ( X100000)

C511K02036[MS QQQ Chro]:m/z 506.9 > 80.0 4.552

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

2

4

6

8

10

12

Y ( X1000000)

C511K02036[MS QQQ Chro]:m/z 498.9 > 79.9 4.554

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02036[MS QQQ Chro]:m/z 498.9 > 98.9 4.554

* 5 13C4 PFOS (IS)

3 4 5

Min

4

14

24

34

44

54

64

74

84

Y ( X10000)

C511K02036[MS QQQ Chro]:m/z 502.9 > 80.0 4.553

$ 8 13C4 PFOS

3 4 5

Min

4

14

24

34

44

54

64

74

84

Y ( X10000)

C511K02036[MS QQQ Chro]:m/z 502.9 > 80.0 4.553

Page 127 of 272
Report Date: 03-Nov-2011 10:29:20 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02036.d

Page 128 of 272
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Page 145 of 272
FORM I

LCMS ORGANICS ANALYSIS DATA SHEET Form 1

Client Sample ID:

Lab Name: Job No.:

SDG No.:

280-21985-1

Lab Sample ID: MB 280-94046/1-A

Matrix: Lab File ID: PC511K02020.d

Analysis Method: DV-LC-0012 Date Collected:

Solid

TestAmerica Denver

Con. Extract Vol.:

Volume:

Injection Volume:

GPC Cleanup:(Y/N)

Date Extracted:

Date Analyzed:

Dilution Factor: 1

Extraction Method: DV-OP-0019 10/31/2011 14:40

11/02/2011 15:22

50(mL)

20(uL)

Sample wt/vol: 10.08(g)

% Moisture:

GC Column: Gemini-NX ID:

N

Analysis Batch No.: 94589 Units: ug/Kg

CAS NO. COMPOUND NAME RESULT Q RL MDL

3825-26-1 Ammonium Perfluorooctanoate (APFO) ND 2.5 0.50

335-67-1 Perfluorooctanoic acid (PFOA) ND 2.5 0.50

CAS NO. SURROGATE %REC Q LIMITS

STL00990 13C4 PFOA 92 50-200

FORM I DV-LC-0012

Page 146 of 272
Report Date: 03-Nov-2011 10:29:07 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02020.d

Lims ID: MB 280-94046/1-A Client ID:

Inject. Date: 02-Nov-2011 15:22:39 Dil. Factor: 1.0000 

Sample Type: MB

Sample ID: mb 280-94046/1-a, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 14

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.449 4.433 0.016 1.000 17429442 10.7

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.450 4.434 0.016 19825404 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.450 4.434 0.016 19825404 9.21

 3 Ammonium Perfluorooctanoate (APFO) 1

 413.0 > 368.9 4.435

 413.0 > 169.0 4.435

 1 Perfluorooctanoic acid 1

 413.0 > 368.9 4.435

 413.0 > 169.0 4.435

$ 6 13C8 PFOS

 506.9 > 80.0 4.596 4.586 0.010 1.000 4540517 9.76

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.586

 498.9 > 98.9 4.586

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.597 4.586 0.011 5078600 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.597 4.586 0.011 5078600 9.23

QC Flag Legend

Processing Flags

1 - Missing Peaks

Page 147 of 272
Report Date: 03-Nov-2011 10:29:07 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02020.d

Injection Date: 02-Nov-2011 15:22:39 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 14

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

6

12

18

24

30

36

42

Y ( X100000)

C511K02020[MS QQQ Chro]:m/z 421.0 > 375.9 4.449

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

7

14

21

28

35

42

49

Y ( X100000)

C511K02020[MS QQQ Chro]:m/z 417.0 > 371.9 4.450

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

7

14

21

28

35

42

49

Y ( X100000)

C511K02020[MS QQQ Chro]:m/z 417.0 > 371.9 4.450

 3 Ammonium Perfluorooctanoate (APFO) (ND)

2.9 3.9 4.9

Min

41

44

47

50

53

56

59

62

Y ( X1000)

C511K02020[MS QQQ Chro]:m/z 413.0 > 368.9 

 3 Ammonium Perfluorooctanoate (APFO) (ND)

2.9 3.9 4.9

Min

413

419

425

431

437

443

449

455

Y ( X100)

C511K02020[MS QQQ Chro]:m/z 413.0 > 169.0 

 1 Perfluorooctanoic acid (ND)

2.9 3.9 4.9

Min

41

44

47

50

53

56

59

62

Y ( X1000)

C511K02020[MS QQQ Chro]:m/z 413.0 > 368.9 

 1 Perfluorooctanoic acid (ND)

2.9 3.9 4.9

Min

413

419

425

431

437

443

449

455

Y ( X100)

C511K02020[MS QQQ Chro]:m/z 413.0 > 169.0 

$ 6 13C8 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02020[MS QQQ Chro]:m/z 506.9 > 80.0 4.596

 2 Perfluorooctanoic Sulfonate (ND)

3 4 5

Min

413

416

419

422

425

428

431

Y ( X100)

C511K02020[MS QQQ Chro]:m/z 498.9 > 79.9 

 2 Perfluorooctanoic Sulfonate (ND)

3 4 5

Min

413

415

417

419

421

423

Y ( X100)

C511K02020[MS QQQ Chro]:m/z 498.9 > 98.9 

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02020[MS QQQ Chro]:m/z 502.9 > 80.0 4.597

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02020[MS QQQ Chro]:m/z 502.9 > 80.0 4.597

Page 148 of 272
Report Date: 03-Nov-2011 10:29:08 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02020.d

Page 149 of 272
FORM I

LCMS ORGANICS ANALYSIS DATA SHEET Form 1

Client Sample ID:

Lab Name: Job No.:

SDG No.:

280-21985-1

Lab Sample ID: CCB 280-94589/11

Matrix: Lab File ID: PC511K02017.d

Analysis Method: DV-LC-0012 Date Collected:

Solid

TestAmerica Denver

Con. Extract Vol.:

Volume:

Injection Volume:

GPC Cleanup:(Y/N)

Date Extracted:

Date Analyzed:

Dilution Factor: 1

Extraction Method:

11/02/2011 14:59

20(uL)

Sample wt/vol: 1(mL)

% Moisture:

GC Column: Gemini-NX ID:

N

Analysis Batch No.: 94589 Units: ug/L

CAS NO. COMPOUND NAME RESULT Q RL MDL

3825-26-1 Ammonium Perfluorooctanoate (APFO) ND 0.50 0.052

335-67-1 Perfluorooctanoic acid (PFOA) ND 0.50 0.052

CAS NO. SURROGATE %REC Q LIMITS

STL00990 13C4 PFOA 100 50-200

FORM I DV-LC-0012

Page 150 of 272
Report Date: 03-Nov-2011 10:29:05 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02017.d

Lims ID: ccb Client ID:

Inject. Date: 02-Nov-2011 14:59:27 Dil. Factor: 1.0000 

Sample Type: CCB

Sample ID: CCB, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 11

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

First Level Reviewer: bonnettj Date: 03-Nov-2011 10:23:51

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.433

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.423 4.434 -0.011 21568424 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.423 4.434 -0.011 21568424 10.0

 3 Ammonium Perfluorooctanoate (APFO) 1

 413.0 > 368.9 4.435

 413.0 > 169.0 4.435

 1 Perfluorooctanoic acid 1

 413.0 > 368.9 4.435

 413.0 > 169.0 4.435

$ 6 13C8 PFOS

 506.9 > 80.0 4.586

 2 Perfluorooctanoic Sulfonate 1

 498.9 > 79.9 4.586

 498.9 > 98.9 4.586

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.571 4.586 -0.015 5205820 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.571 4.586 -0.015 5205820 9.46

QC Flag Legend

Processing Flags

1 - Missing Peaks

Page 151 of 272
Report Date: 03-Nov-2011 10:29:05 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02017.d

Injection Date: 02-Nov-2011 14:59:27 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 11

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA (ND)

2.9 3.9 4.9

Min

410

416

422

428

434

440

446

452

Y ( X100)

C511K02017[MS QQQ Chro]:m/z 421.0 > 375.9 

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02017[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02017[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

 3 Ammonium Perfluorooctanoate (APFO) (ND)

2.9 3.9 4.9

Min

42

46

50

54

58

62

66

70

Y ( X1000)

C511K02017[MS QQQ Chro]:m/z 413.0 > 368.9 

 3 Ammonium Perfluorooctanoate (APFO) (ND)

2.9 3.9 4.9

Min

410

418

426

434

442

450

458

466

Y ( X100)

C511K02017[MS QQQ Chro]:m/z 413.0 > 169.0 

 1 Perfluorooctanoic acid (ND)

2.9 3.9 4.9

Min

42

46

50

54

58

62

66

70

Y ( X1000)

C511K02017[MS QQQ Chro]:m/z 413.0 > 368.9 

 1 Perfluorooctanoic acid (ND)

2.9 3.9 4.9

Min

410

418

426

434

442

450

458

466

Y ( X100)

C511K02017[MS QQQ Chro]:m/z 413.0 > 169.0 

$ 6 13C8 PFOS (ND)

3 4 5

Min

410

418

426

434

442

450

458

466

Y ( X100)

C511K02017[MS QQQ Chro]:m/z 506.9 > 80.0 

 2 Perfluorooctanoic Sulfonate (ND)

3 4 5

Min

411

418

425

432

439

446

453

460

Y ( X100)

C511K02017[MS QQQ Chro]:m/z 498.9 > 79.9 

 2 Perfluorooctanoic Sulfonate (ND)

3 4 5

Min

411

415

419

423

427

431

435

Y ( X100)

C511K02017[MS QQQ Chro]:m/z 498.9 > 98.9 

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02017[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02017[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

Page 152 of 272
Report Date: 03-Nov-2011 10:29:05 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02017.d

Page 153 of 272
FORM I

LCMS ORGANICS ANALYSIS DATA SHEET Form 1

Client Sample ID:

Lab Name: Job No.:

SDG No.:

280-21985-1

Lab Sample ID: CCB 280-94589/21

Matrix: Lab File ID: PC511K02027.d

Analysis Method: DV-LC-0012 Date Collected:

Solid

TestAmerica Denver

Con. Extract Vol.:

Volume:

Injection Volume:

GPC Cleanup:(Y/N)

Date Extracted:

Date Analyzed:

Dilution Factor: 1

Extraction Method:

11/02/2011 16:16

20(uL)

Sample wt/vol: 1(mL)

% Moisture:

GC Column: Gemini-NX ID:

N

Analysis Batch No.: 94589 Units: ug/L

CAS NO. COMPOUND NAME RESULT Q RL MDL

3825-26-1 Ammonium Perfluorooctanoate (APFO) ND 0.50 0.052

335-67-1 Perfluorooctanoic acid (PFOA) ND 0.50 0.052

CAS NO. SURROGATE %REC Q LIMITS

STL00990 13C4 PFOA 98 50-200

FORM I DV-LC-0012

Page 154 of 272
Report Date: 03-Nov-2011 10:29:13 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02027.d

Lims ID: ccb Client ID:

Inject. Date: 02-Nov-2011 16:16:47 Dil. Factor: 1.0000 

Sample Type: CCB

Sample ID: CCB, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 21

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:12 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.433

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.423 4.434 -0.011 21131544 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.423 4.434 -0.011 21131544 9.81

 3 Ammonium Perfluorooctanoate (APFO) 1

 413.0 > 368.9 4.435

 413.0 > 169.0 4.435

 1 Perfluorooctanoic acid 1

 413.0 > 368.9 4.435

 413.0 > 169.0 4.435

$ 6 13C8 PFOS

 506.9 > 80.0 4.586

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.586

 498.9 > 98.9 4.586

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.571 4.586 -0.015 5181337 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.571 4.586 -0.015 5181337 9.41

QC Flag Legend

Processing Flags

1 - Missing Peaks

Page 155 of 272
Report Date: 03-Nov-2011 10:29:13 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02027.d

Injection Date: 02-Nov-2011 16:16:47 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 21

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA (ND)

2.9 3.9 4.9

Min

413

416

419

422

425

428

431

434

Y ( X100)

C511K02027[MS QQQ Chro]:m/z 421.0 > 375.9 

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02027[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02027[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

 3 Ammonium Perfluorooctanoate (APFO) (ND)

2.9 3.9 4.9

Min

41

45

49

53

57

61

65

Y ( X1000)

C511K02027[MS QQQ Chro]:m/z 413.0 > 368.9 

 3 Ammonium Perfluorooctanoate (APFO) (ND)

2.9 3.9 4.9

Min

413

419

425

431

437

443

449

Y ( X100)

C511K02027[MS QQQ Chro]:m/z 413.0 > 169.0 

 1 Perfluorooctanoic acid (ND)

2.9 3.9 4.9

Min

41

45

49

53

57

61

65

Y ( X1000)

C511K02027[MS QQQ Chro]:m/z 413.0 > 368.9 

 1 Perfluorooctanoic acid (ND)

2.9 3.9 4.9

Min

413

419

425

431

437

443

449

Y ( X100)

C511K02027[MS QQQ Chro]:m/z 413.0 > 169.0 

$ 6 13C8 PFOS (ND)

3 4 5

Min

413

418

423

428

433

438

443

Y ( X100)

C511K02027[MS QQQ Chro]:m/z 506.9 > 80.0 

 2 Perfluorooctanoic Sulfonate (ND)

3 4 5

Min

413

417

421

425

429

433

437

441

445

Y ( X100)

C511K02027[MS QQQ Chro]:m/z 498.9 > 79.9 

 2 Perfluorooctanoic Sulfonate (ND)

3 4 5

Min

413

416

419

422

425

428

431

Y ( X100)

C511K02027[MS QQQ Chro]:m/z 498.9 > 98.9 

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02027[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02027[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

Page 156 of 272
Report Date: 03-Nov-2011 10:29:13 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02027.d

Page 157 of 272
FORM I

LCMS ORGANICS ANALYSIS DATA SHEET Form 1

Client Sample ID:

Lab Name: Job No.:

SDG No.:

280-21985-1

Lab Sample ID: LCS 280-94046/2-A

Matrix: Lab File ID: PC511K02021.d

Analysis Method: DV-LC-0012 Date Collected:

Solid

TestAmerica Denver

Con. Extract Vol.:

Volume:

Injection Volume:

GPC Cleanup:(Y/N)

Date Extracted:

Date Analyzed:

Dilution Factor: 1

Extraction Method: DV-OP-0019 10/31/2011 14:40

11/02/2011 15:30

50(mL)

20(uL)

Sample wt/vol: 10.00(g)

% Moisture:

GC Column: Gemini-NX ID:

N

Analysis Batch No.: 94589 Units: ug/Kg

CAS NO. COMPOUND NAME RESULT Q RL MDL

3825-26-1 Ammonium Perfluorooctanoate (APFO) 58.0 2.5 0.50

335-67-1 Perfluorooctanoic acid (PFOA) 55.5 2.5 0.50

CAS NO. SURROGATE %REC Q LIMITS

STL00990 13C4 PFOA 91 50-200

FORM I DV-LC-0012

Page 158 of 272
Report Date: 03-Nov-2011 10:29:08 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02021.d

Lims ID: LCS 280-94046/2-A Client ID:

Inject. Date: 02-Nov-2011 15:30:22 Dil. Factor: 1.0000 

Sample Type: LCS

Sample ID: lcs 280-94046/2-a, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 15

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.449 4.433 0.016 1.000 17187234 10.7

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.450 4.434 0.016 19510836 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.450 4.434 0.016 19510836 9.06

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.451 4.435 0.016 1.000 23327029 11.6 0.70- 1.30 1.00

 413.0 > 169.0 4.451 4.435 0.016 1.000 4544796 3.72- 6.92 5.13

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.451 4.435 0.016 1.000 23327029 11.1 0.70- 1.30 1.00

 413.0 > 169.0 4.451 4.435 0.016 1.000 4544796 3.72- 6.92 5.13

$ 6 13C8 PFOS

 506.9 > 80.0 4.596 4.586 0.010 1.000 4654243 9.75

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.598 4.586 0.012 1.000 7357364 9.81 0.70- 1.30 1.00

 498.9 > 98.9 4.598 4.586 0.012 1.000 4012137 1.30- 2.42 1.83

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.597 4.586 0.011 5213188 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.597 4.586 0.011 5213188 9.47

Page 159 of 272
Report Date: 03-Nov-2011 10:29:08 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02021.d

Injection Date: 02-Nov-2011 15:30:22 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 15

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

6

12

18

24

30

36

42

Y ( X100000)

C511K02021[MS QQQ Chro]:m/z 421.0 > 375.9 4.449

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

7

14

21

28

35

42

49

Y ( X100000)

C511K02021[MS QQQ Chro]:m/z 417.0 > 371.9 4.450

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

7

14

21

28

35

42

49

Y ( X100000)

C511K02021[MS QQQ Chro]:m/z 417.0 > 371.9 4.450

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02021[MS QQQ Chro]:m/z 413.0 > 368.9 4.451

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

Y ( X100000)

C511K02021[MS QQQ Chro]:m/z 413.0 > 169.0 4.451

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02021[MS QQQ Chro]:m/z 413.0 > 368.9 4.451

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

2

4

6

8

10

12

Y ( X100000)

C511K02021[MS QQQ Chro]:m/z 413.0 > 169.0 4.451

$ 6 13C8 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02021[MS QQQ Chro]:m/z 506.9 > 80.0 4.596

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

3

6

9

12

15

18

21

Y ( X100000)

C511K02021[MS QQQ Chro]:m/z 498.9 > 79.9 4.598

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

2

4

6

8

10

12

Y ( X100000)

C511K02021[MS QQQ Chro]:m/z 498.9 > 98.9 4.598

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02021[MS QQQ Chro]:m/z 502.9 > 80.0 4.597

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

16

Y ( X100000)

C511K02021[MS QQQ Chro]:m/z 502.9 > 80.0 4.597

Page 160 of 272
Report Date: 03-Nov-2011 10:29:08 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02021.d

Page 161 of 272
FORM I

LCMS ORGANICS ANALYSIS DATA SHEET Form 1

Client Sample ID:

Lab Name: Job No.:

SDG No.:

280-21985-1

Lab Sample ID: LLCS 280-94046/3-A

Matrix: Lab File ID: PC511K02022.d

Analysis Method: DV-LC-0012 Date Collected:

Solid

TestAmerica Denver

Con. Extract Vol.:

Volume:

Injection Volume:

GPC Cleanup:(Y/N)

Date Extracted:

Date Analyzed:

Dilution Factor: 1

Extraction Method: DV-OP-0019 10/31/2011 14:40

11/02/2011 15:38

50(mL)

20(uL)

Sample wt/vol: 10.12(g)

% Moisture:

GC Column: Gemini-NX ID:

N

Analysis Batch No.: 94589 Units: ug/Kg

CAS NO. COMPOUND NAME RESULT Q RL MDL

3825-26-1 Ammonium Perfluorooctanoate (APFO) 5.73 2.5 0.49

335-67-1 Perfluorooctanoic acid (PFOA) 5.48 2.5 0.49

CAS NO. SURROGATE %REC Q LIMITS

STL00990 13C4 PFOA 95 50-200

FORM I DV-LC-0012

Page 162 of 272
Report Date: 03-Nov-2011 10:29:09 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02022.d

Lims ID: LLCS 280-94046/3-A Client ID:

Inject. Date: 02-Nov-2011 15:38:07 Dil. Factor: 1.0000 

Sample Type: LLCS

Sample ID: llcs 280-94046/3-a, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 16

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.458 4.433 0.025 1.000 17944069 10.7

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.459 4.434 0.025 20508155 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.459 4.434 0.025 20508155 9.52

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.460 4.435 0.025 1.000 2627905 1.16 0.70- 1.30 1.00

 413.0 > 169.0 4.451 4.435 0.016 0.998 456643 3.72- 6.92 5.75

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.460 4.435 0.025 1.000 2627905 1.11 0.70- 1.30 1.00

 413.0 > 169.0 4.451 4.435 0.016 0.998 456643 3.72- 6.92 5.75

$ 6 13C8 PFOS

 506.9 > 80.0 4.605 4.586 0.019 1.000 4641355 9.65

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.598 4.586 0.012 0.998 785510 1.00 0.70- 1.30 1.00

 498.9 > 98.9 4.607 4.586 0.021 1.000 402332 1.30- 2.42 1.95

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.606 4.586 0.020 5251794 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.606 4.586 0.020 5251794 9.54

Page 163 of 272
Report Date: 03-Nov-2011 10:29:09 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02022.d

Injection Date: 02-Nov-2011 15:38:07 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 16

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

6

12

18

24

30

36

42

48

Y ( X100000)

C511K02022[MS QQQ Chro]:m/z 421.0 > 375.9 4.458

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

7

14

21

28

35

42

49

Y ( X100000)

C511K02022[MS QQQ Chro]:m/z 417.0 > 371.9 4.459

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

7

14

21

28

35

42

49

Y ( X100000)

C511K02022[MS QQQ Chro]:m/z 417.0 > 371.9 4.459

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

13

22

31

40

49

58

67

Y ( X10000)

C511K02022[MS QQQ Chro]:m/z 413.0 > 368.9 4.460

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

6

8

10

12

14

16

18

Y ( X10000)

C511K02022[MS QQQ Chro]:m/z 413.0 > 169.0 4.451

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

13

22

31

40

49

58

67

Y ( X10000)

C511K02022[MS QQQ Chro]:m/z 413.0 > 368.9 4.460

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

6

8

10

12

14

16

18

Y ( X10000)

C511K02022[MS QQQ Chro]:m/z 413.0 > 169.0 4.451

$ 6 13C8 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02022[MS QQQ Chro]:m/z 506.9 > 80.0 4.605

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

7

10

13

16

19

22

25

Y ( X10000)

C511K02022[MS QQQ Chro]:m/z 498.9 > 79.9 4.598

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

6

8

10

12

14

16

Y ( X10000)

C511K02022[MS QQQ Chro]:m/z 498.9 > 98.9 4.607

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02022[MS QQQ Chro]:m/z 502.9 > 80.0 4.606

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02022[MS QQQ Chro]:m/z 502.9 > 80.0 4.606

Page 164 of 272
Report Date: 03-Nov-2011 10:29:09 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02022.d

Page 165 of 272
FORM I

LCMS ORGANICS ANALYSIS DATA SHEET Form 1

Client Sample ID:

Lab Name: Job No.:

SDG No.:

280-21985-1

Lab Sample ID: DLCK 280-94589/13

Matrix: Lab File ID: PC511K02019.d

Analysis Method: DV-LC-0012 Date Collected:

Solid

TestAmerica Denver

Con. Extract Vol.:

Volume:

Injection Volume:

GPC Cleanup:(Y/N)

Date Extracted:

Date Analyzed:

Dilution Factor: 1

Extraction Method:

11/02/2011 15:14

20(uL)

Sample wt/vol: 1(mL)

% Moisture:

GC Column: Gemini-NX ID:

N

Analysis Batch No.: 94589 Units: ug/L

CAS NO. COMPOUND NAME RESULT Q RL MDL

3825-26-1 Ammonium Perfluorooctanoate (APFO) 0.488 J 0.50 0.052

335-67-1 Perfluorooctanoic acid (PFOA) 0.468 J 0.50 0.052

CAS NO. SURROGATE %REC Q LIMITS

STL00990 13C4 PFOA 101 50-200

FORM I DV-LC-0012

Page 166 of 272
Report Date: 03-Nov-2011 10:29:07 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02019.d

Lims ID: dlck Client ID:

Inject. Date: 02-Nov-2011 15:14:54 Dil. Factor: 1.0000 

Sample Type: DLCK

Sample ID: DLCK L2, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 13

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.422 4.433 -0.011 1.000 1013527 0.4953

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.423 4.434 -0.011 21770259 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.423 4.434 -0.011 21770259 10.1

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.424 4.435 -0.011 1.000 1291480 0.4878 0.70- 1.30 1.00

 413.0 > 169.0 4.415 4.435 -0.020 0.998 231988 3.72- 6.92 5.57

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.424 4.435 -0.011 1.000 1291480 0.4683 0.70- 1.30 1.00

 413.0 > 169.0 4.415 4.435 -0.020 0.998 231988 3.72- 6.92 5.57

$ 6 13C8 PFOS

 506.9 > 80.0 4.570 4.586 -0.016 1.000 233919 0.4391

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.571 4.586 -0.015 1.000 405313 0.4918 0.70- 1.30 1.00

 498.9 > 98.9 4.571 4.586 -0.015 1.000 210969 1.30- 2.42 1.92

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.571 4.586 -0.015 5249734 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.571 4.586 -0.015 5249734 9.54

Page 167 of 272
Report Date: 03-Nov-2011 10:29:07 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02019.d

Injection Date: 02-Nov-2011 15:14:54 Limit Group: LC - PFOA DuPont

Client ID: Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 13

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

4

8

12

16

20

24

28

32

Y ( X10000)

C511K02019[MS QQQ Chro]:m/z 421.0 > 375.9 4.422

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02019[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

8

16

24

32

40

48

56

Y ( X100000)

C511K02019[MS QQQ Chro]:m/z 417.0 > 371.9 4.423

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

9

14

19

24

29

34

39

Y ( X10000)

C511K02019[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

41

50

59

68

77

86

95

104

113

Y ( X1000)

C511K02019[MS QQQ Chro]:m/z 413.0 > 169.0 4.415

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

9

14

19

24

29

34

39

Y ( X10000)

C511K02019[MS QQQ Chro]:m/z 413.0 > 368.9 4.424

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

41

50

59

68

77

86

95

104

113

Y ( X1000)

C511K02019[MS QQQ Chro]:m/z 413.0 > 169.0 4.415

$ 6 13C8 PFOS

3 4 5

Min

41

50

59

68

77

86

95

104

113

Y ( X1000)

C511K02019[MS QQQ Chro]:m/z 506.9 > 80.0 4.570

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

6

8

10

12

14

16

Y ( X10000)

C511K02019[MS QQQ Chro]:m/z 498.9 > 79.9 4.571

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

41

49

57

65

73

81

89

97

105

Y ( X1000)

C511K02019[MS QQQ Chro]:m/z 498.9 > 98.9 4.571

* 5 13C4 PFOS (IS)

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02019[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

$ 8 13C4 PFOS

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02019[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

Page 168 of 272
Report Date: 03-Nov-2011 10:29:07 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02019.d

Page 169 of 272
FORM I

LCMS ORGANICS ANALYSIS DATA SHEET Form 1

Client Sample ID:

Lab Name: Job No.:

WWK-S-WWM-1(0-.2) MS

SDG No.:

280-21985-1

Lab Sample ID: 280-21985-1 MS

Matrix: Lab File ID: PC511K02024.d

Analysis Method: DV-LC-0012 Date Collected:

Solid

TestAmerica Denver

10/24/2011 07:28

Con. Extract Vol.:

Volume:

Injection Volume:

GPC Cleanup:(Y/N)

Date Extracted:

Date Analyzed:

Dilution Factor: 1

Extraction Method: DV-OP-0019 10/31/2011 14:40

11/02/2011 15:53

50(mL)

20(uL)

Sample wt/vol: 10.09(g)

% Moisture: 28.1

GC Column: Gemini-NX ID:

N

Analysis Batch No.: 94589 Units: ug/Kg

CAS NO. COMPOUND NAME RESULT Q RL MDL

3825-26-1 Ammonium Perfluorooctanoate (APFO) 77.9 3.4 0.69

335-67-1 Perfluorooctanoic acid (PFOA) 75.1 3.4 0.69

CAS NO. SURROGATE %REC Q LIMITS

STL00990 13C4 PFOA 49 X 50-200

FORM I DV-LC-0012

Page 170 of 272
Report Date: 03-Nov-2011 10:29:11 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02024.d

Lims ID: 280-21985-A-1-B MS Client ID: WWK-S-WWM-1(0-.2)-MS

Inject. Date: 02-Nov-2011 15:53:34 Dil. Factor: 1.0000 

Sample Type: MS

Sample ID: 280-21985-a-1-b ms, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 18

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC285

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.431 4.433 -0.002 1.000 9280504 10.7

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.432 4.434 -0.002 10550504 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.432 4.434 -0.002 10550504 4.90

 3 Ammonium Perfluorooctanoate (APFO)

 413.0 > 368.9 4.433 4.435 -0.002 1.000 12367102 11.3 0.70- 1.30 1.00

 413.0 > 169.0 4.433 4.435 -0.002 1.000 2492138 3.72- 6.92 4.96

 1 Perfluorooctanoic acid

 413.0 > 368.9 4.433 4.435 -0.002 1.000 12367102 10.9 0.70- 1.30 1.00

 413.0 > 169.0 4.433 4.435 -0.002 1.000 2492138 3.72- 6.92 4.96

$ 6 13C8 PFOS

 506.9 > 80.0 4.579 4.586 -0.007 1.000 2956142 10.1

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.571 4.586 -0.015 0.998 4736886 10.3 0.70- 1.30 1.00

 498.9 > 98.9 4.571 4.586 -0.015 0.998 2543694 1.30- 2.42 1.86

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.579 4.586 -0.007 3198056 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.579 4.586 -0.007 3198056 5.81

Page 171 of 272
Report Date: 03-Nov-2011 10:29:11 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02024.d

Injection Date: 02-Nov-2011 15:53:34 Limit Group: LC - PFOA DuPont

Client ID: WWK-S-WWM-1(0-.2)-MS Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 18

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

Y ( X100000)

C511K02024[MS QQQ Chro]:m/z 421.0 > 375.9 4.431

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

28

Y ( X100000)

C511K02024[MS QQQ Chro]:m/z 417.0 > 371.9 4.432

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

28

Y ( X100000)

C511K02024[MS QQQ Chro]:m/z 417.0 > 371.9 4.432

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

0

5

10

15

20

25

30

Y ( X100000)

C511K02024[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

 3 Ammonium Perfluorooctanoate (APFO)

2.9 3.9 4.9

Min

4

13

22

31

40

49

58

67

Y ( X10000)

C511K02024[MS QQQ Chro]:m/z 413.0 > 169.0 4.433

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

0

5

10

15

20

25

30

Y ( X100000)

C511K02024[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

 1 Perfluorooctanoic acid

2.9 3.9 4.9

Min

4

13

22

31

40

49

58

67

Y ( X10000)

C511K02024[MS QQQ Chro]:m/z 413.0 > 169.0 4.433

$ 6 13C8 PFOS

3 4 5

Min

4

15

26

37

48

59

70

81

Y ( X10000)

C511K02024[MS QQQ Chro]:m/z 506.9 > 80.0 4.579

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

0

2

4

6

8

10

12

14

Y ( X100000)

C511K02024[MS QQQ Chro]:m/z 498.9 > 79.9 4.571

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

4

13

22

31

40

49

58

67

Y ( X10000)

C511K02024[MS QQQ Chro]:m/z 498.9 > 98.9 4.571

* 5 13C4 PFOS (IS)

3 4 5

Min

4

15

26

37

48

59

70

81

92

Y ( X10000)

C511K02024[MS QQQ Chro]:m/z 502.9 > 80.0 4.579

$ 8 13C4 PFOS

3 4 5

Min

4

15

26

37

48

59

70

81

92

Y ( X10000)

C511K02024[MS QQQ Chro]:m/z 502.9 > 80.0 4.579

Page 172 of 272
Report Date: 03-Nov-2011 10:29:11 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02024.d

Page 173 of 272
FORM I

LCMS ORGANICS ANALYSIS DATA SHEET Form 1

Client Sample ID:

Lab Name: Job No.:

WWK-S-WWM-1(0-.2) DU

SDG No.:

280-21985-1

Lab Sample ID: 280-21985-1 DU

Matrix: Lab File ID: PC511K02025.d

Analysis Method: DV-LC-0012 Date Collected:

Solid

TestAmerica Denver

10/24/2011 07:28

Con. Extract Vol.:

Volume:

Injection Volume:

GPC Cleanup:(Y/N)

Date Extracted:

Date Analyzed:

Dilution Factor: 1

Extraction Method: DV-OP-0019 10/31/2011 14:40

11/02/2011 16:01

50(mL)

20(uL)

Sample wt/vol: 10.06(g)

% Moisture: 29.1

GC Column: Gemini-NX ID:

N

Analysis Batch No.: 94589 Units: ug/Kg

CAS NO. COMPOUND NAME RESULT Q RL MDL

3825-26-1 Ammonium Perfluorooctanoate (APFO) 1.07 J 3.5 0.70

335-67-1 Perfluorooctanoic acid (PFOA) 0.983 J 3.5 0.70

CAS NO. SURROGATE %REC Q LIMITS

STL00990 13C4 PFOA 51 50-200

FORM I DV-LC-0012

Page 174 of 272
Report Date: 03-Nov-2011 14:45:20 Chrom Revision: 1.2 13-Jul-2011 10:43:06

TestAmerica Laboratories

Target Compound Quantitation Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02025.d

Lims ID: 280-21985-A-1-C DU Client ID: WWK-S-WWM-1(0-.2)-REP

Inject. Date: 02-Nov-2011 16:01:19 Dil. Factor: 1.0000 

Sample Type: DU

Sample ID: 280-21985-a-1-c du, Sample

Misc. Info.:

Operator: TW/JB Instrument ID: LC_LCMS5

Vol. Injected: 20.0000 ALS Bottle#: 0

Lims Batch ID: 94589 Lims Sample ID: 19

Raw Data: Smoothed

Detector: MS QQQ

Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PFOA_S_Dupont.m

Last Update: 03-Nov-2011 14:45:19 Calib Date: 02-Nov-2011 14:51:42

Quant Method: Internal/External Standard Quant By: Initial Calibration

Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d

Limit Group: LC - PFOA DuPont

Integrator: Falcon

Process Host: DENPC308

First Level Reviewer: williamst Date: 03-Nov-2011 14:45:00

Signal RT

ADJ

RT

DLT

RT

REL

RT Response

On-Col Amt

ug/L Ratio Range Ratio Flags

$ 9 13C8 PFOA

 421.0 > 375.9 4.431 4.433 -0.002 1.000 9554896 10.6

* 4 13C4 PFOA (IS)

 417.0 > 371.9 4.432 4.434 -0.002 11017193 10.0

$ 7 13C4 PFOA

 417.0 > 371.9 4.432 4.434 -0.002 11017193 5.12

 3 Ammonium Perfluorooctanoate (APFO) M

 413.0 > 368.9 4.433 4.435 -0.002 1.000 275882 0.1532 0.70- 1.30 1.00 M

 413.0 > 169.0 4.424 4.435 -0.011 0.998 47280 3.72- 6.92 5.84 M

 1 Perfluorooctanoic acid M

 413.0 > 368.9 4.433 4.435 -0.002 1.000 268207 0.1402 0.70- 1.30 1.00 M

 413.0 > 169.0 4.424 4.435 -0.011 0.998 45817 3.72- 6.92 5.85 M

$ 6 13C8 PFOS

 506.9 > 80.0 4.570 4.586 -0.016 1.000 2947347 9.81

 2 Perfluorooctanoic Sulfonate

 498.9 > 79.9 4.571 4.586 -0.015 1.000 115538 0.1985 0.70- 1.30 1.00

 498.9 > 98.9 4.571 4.586 -0.015 1.000 48967 1.30- 2.42 2.36

* 5 13C4 PFOS (IS)

 502.9 > 80.0 4.571 4.586 -0.015 3280529 9.56

$ 8 13C4 PFOS

 502.9 > 80.0 4.571 4.586 -0.015 3280529 5.96

QC Flag Legend

Review Flags

M - Manually Integrated

Page 175 of 272
Report Date: 03-Nov-2011 14:45:20 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02025.d

Injection Date: 02-Nov-2011 16:01:19 Limit Group: LC - PFOA DuPont

Client ID: WWK-S-WWM-1(0-.2)-REP Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 19

Operator ID: TW/JB Injection Vol: 20.00 ul

$ 9 13C8 PFOA

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

Y ( X100000)

C511K02025[MS QQQ Chro]:m/z 421.0 > 375.9 4.431

* 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

28

Y ( X100000)

C511K02025[MS QQQ Chro]:m/z 417.0 > 371.9 4.432

$ 7 13C4 PFOA

2.9 3.9 4.9

Min

0

4

8

12

16

20

24

28

Y ( X100000)

C511K02025[MS QQQ Chro]:m/z 417.0 > 371.9 4.432

 3 Ammonium Perfluorooctanoate (APFO) (M)

2.9 3.9 4.9

Min

46

56

66

76

86

96

106

116

126

Y ( X1000)

C511K02025[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

 3 Ammonium Perfluorooctanoate (APFO) (M)

2.9 3.9 4.9

Min

41

43

45

47

49

51

53

55

57

Y ( X1000)

C511K02025[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

 1 Perfluorooctanoic acid (M)

2.9 3.9 4.9

Min

46

56

66

76

86

96

106

116

126

Y ( X1000)

C511K02025[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

 1 Perfluorooctanoic acid (M)

2.9 3.9 4.9

Min

41

43

45

47

49

51

53

55

57

Y ( X1000)

C511K02025[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

$ 6 13C8 PFOS

3 4 5

Min

4

15

26

37

48

59

70

81

Y ( X10000)

C511K02025[MS QQQ Chro]:m/z 506.9 > 80.0 4.570

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

41

45

49

53

57

61

65

69

Y ( X1000)

C511K02025[MS QQQ Chro]:m/z 498.9 > 79.9 4.571

 2 Perfluorooctanoic Sulfonate

3 4 5

Min

41

43

45

47

49

51

53

55

Y ( X1000)

C511K02025[MS QQQ Chro]:m/z 498.9 > 98.9 4.571

* 5 13C4 PFOS (IS)

3 4 5

Min

4

16

28

40

52

64

76

88

Y ( X10000)

C511K02025[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

$ 8 13C4 PFOS

3 4 5

Min

4

16

28

40

52

64

76

88

Y ( X10000)

C511K02025[MS QQQ Chro]:m/z 502.9 > 80.0 4.571

Page 176 of 272
Report Date: 03-Nov-2011 14:45:21 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02025.d

Page 177 of 272
Report Date: 03-Nov-2011 14:45:21 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Manual Integration/User Assign Peak Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02025.d

Injection Date: 02-Nov-2011 16:01:19 Limit Group: LC - PFOA DuPont

Client ID: WWK-S-WWM-1(0-.2)-REP Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 19

Operator ID: TW/JB Injection Vol: 20.00 ul

 3 Ammonium Perfluorooctanoate (APFO), Signal: 1, m/z: 413.0 > 368.9 Type: quant, RT: 4.44

Processing Integration Results

RT: 4.43

Response: 251810

Amount: 0.131897

3.97

Min

51

56

61

66

71

76

81

86

91

96

101

106

111

116

121

126

Y ( X1000)

C511K02025[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

Manual Integration Results

RT: 4.43

Response: 275882

Amount: 0.153222

3.97

Min

51

56

61

66

71

76

81

86

91

96

101

106

111

116

121

126

Y ( X1000)

C511K02025[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

Reviewer: williamst, 03-Nov-2011 14:45:00

Audit Action: Manually Integrated

Audit Reason: Baseline

Page 178 of 272
Report Date: 03-Nov-2011 14:45:21 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Manual Integration/User Assign Peak Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02025.d

Injection Date: 02-Nov-2011 16:01:19 Limit Group: LC - PFOA DuPont

Client ID: WWK-S-WWM-1(0-.2)-REP Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 19

Operator ID: TW/JB Injection Vol: 20.00 ul

 3 Ammonium Perfluorooctanoate (APFO), Signal: 2, m/z: 413.0 > 169.0 Type: qualifier, RT: 4.44

Processing Integration Results

RT: 4.42

Response: 30674

Amount: 0

2.8 3.8 4.8

Min

41

43

45

47

49

51

53

55

57

Y ( X1000)

C511K02025[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

Manual Integration Results

RT: 4.42

Response: 47280

Amount: 0

2.8 3.8 4.8

Min

41

43

45

47

49

51

53

55

57

Y ( X1000)

C511K02025[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

Reviewer: williamst, 03-Nov-2011 14:45:00

Audit Action: Manually Integrated

Audit Reason: Baseline

Page 179 of 272
Report Date: 03-Nov-2011 14:45:21 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Manual Integration/User Assign Peak Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02025.d

Injection Date: 02-Nov-2011 16:01:19 Limit Group: LC - PFOA DuPont

Client ID: WWK-S-WWM-1(0-.2)-REP Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 19

Operator ID: TW/JB Injection Vol: 20.00 ul

 1 Perfluorooctanoic acid, Signal: 1, m/z: 413.0 > 368.9 Type: quant, RT: 4.44

Processing Integration Results

RT: 4.43

Response: 251810

Amount: 0.126234

3.97

Min

51

56

61

66

71

76

81

86

91

96

101

106

111

116

121

126

Y ( X1000)

C511K02025[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

Manual Integration Results

RT: 4.43

Response: 268207

Amount: 0.140194

3.97

Min

51

56

61

66

71

76

81

86

91

96

101

106

111

116

121

126

Y ( X1000)

C511K02025[MS QQQ Chro]:m/z 413.0 > 368.9 4.433

Reviewer: williamst, 03-Nov-2011 14:45:00

Audit Action: Manually Integrated

Audit Reason: Baseline

Page 180 of 272
Report Date: 03-Nov-2011 14:45:21 Chrom Revision: 1.2 13-Jul-2011 10:43:06

Manual Integration/User Assign Peak Report

Data File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02025.d

Injection Date: 02-Nov-2011 16:01:19 Limit Group: LC - PFOA DuPont

Client ID: WWK-S-WWM-1(0-.2)-REP Instrument ID: LC_LCMS5

Lims Batch ID: 94589 Lims Sample ID: 19

Operator ID: TW/JB Injection Vol: 20.00 ul

 1 Perfluorooctanoic acid, Signal: 2, m/z: 413.0 > 169.0 Type: qualifier, RT: 4.44

Processing Integration Results

RT: 4.42

Response: 30674

Amount: 0

2.8 3.8 4.8

Min

41

43

45

47

49

51

53

55

57

Y ( X1000)

C511K02025[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

Manual Integration Results

RT: 4.42

Response: 45817

Amount: 0

2.8 3.8 4.8

Min

41

43

45

47

49

51

53

55

57

Y ( X1000)

C511K02025[MS QQQ Chro]:m/z 413.0 > 169.0 4.424

Reviewer: williamst, 03-Nov-2011 14:45:00

Audit Action: Manually Integrated

Audit Reason: Baseline

Page 181 of 272
Lab Name: Job No.:

SDG No.:

Instrument ID:

Analysis Batch Number:

LCMS ANALYSIS RUN LOG

DILUTION

FACTOR

LAB SAMPLE ID CLIENT SAMPLE ID DATE ANALYZED LAB FILE ID COLUMN ID

TestAmerica Denver 280-21985-1

LC_LCMS5

94589

Start Date:

End Date: 11/02/2011 17:26

11/02/2011 13:42

ICB 280-94589/1 11/02/2011 13:42 1 Gemini-NX

STD0002 280-94589/2 

IC

11/02/2011 13:49 1 PC511K02008.d Gemini-NX

STD0005 280-94589/3 

IC

11/02/2011 13:57 1 PC511K02009.d Gemini-NX

STD0010 280-94589/4 

IC

11/02/2011 14:05 1 PC511K02010.d Gemini-NX

STD0020 280-94589/5 

IC

11/02/2011 14:13 1 PC511K02011.d Gemini-NX

STD0050 280-94589/6 

IC

11/02/2011 14:20 1 PC511K02012.d Gemini-NX

STD0100 280-94589/7 

IC

11/02/2011 14:28 1 PC511K02013.d Gemini-NX

STD0200 280-94589/8 

IC

11/02/2011 14:36 1 PC511K02014.d Gemini-NX

STD0500 280-94589/9 

IC

11/02/2011 14:43 1 PC511K02015.d Gemini-NX

STD1250 280-94589/10 

IC

11/02/2011 14:51 1 PC511K02016.d Gemini-NX

CCB 280-94589/11 11/02/2011 14:59 1 PC511K02017.d Gemini-NX

ICV 280-94589/12 11/02/2011 15:07 1 PC511K02018.d Gemini-NX

DLCK 280-94589/13 11/02/2011 15:14 1 PC511K02019.d Gemini-NX

MB 280-94046/1-A 11/02/2011 15:22 1 PC511K02020.d Gemini-NX

LCS 280-94046/2-A 11/02/2011 15:30 1 PC511K02021.d Gemini-NX

LLCS 280-94046/3-A 11/02/2011 15:38 1 PC511K02022.d Gemini-NX

280-21985-1 WWK-S-WWM-1(0-.2) 11/02/2011 15:45 1 PC511K02023.d Gemini-NX

280-21985-1 MS WWK-S-WWM-1(0-.2) MS 11/02/2011 15:53 1 PC511K02024.d Gemini-NX

280-21985-1 DU WWK-S-WWM-1(0-.2) DU 11/02/2011 16:01 1 PC511K02025.d Gemini-NX

CCV 280-94589/20 11/02/2011 16:09 1 PC511K02026.d Gemini-NX

CCB 280-94589/21 11/02/2011 16:16 1 PC511K02027.d Gemini-NX

CCVL 280-94589/22 11/02/2011 16:24 1 PC511K02028.d Gemini-NX

CCVL 280-94589/23 11/02/2011 16:32 1 PC511K02029.d Gemini-NX

CCVL 280-94589/24 11/02/2011 16:39 1 PC511K02030.d Gemini-NX

CCVL 280-94589/25 11/02/2011 16:47 1 PC511K02031.d Gemini-NX

CCV 280-94589/26 11/02/2011 16:55 1 PC511K02032.d Gemini-NX

CCVL 280-94589/27 11/02/2011 17:03 1 PC511K02033.d Gemini-NX

CCV 280-94589/28 11/02/2011 17:10 1 PC511K02034.d Gemini-NX

CCVL 280-94589/29 11/02/2011 17:18 1 PC511K02035.d Gemini-NX

CCVL 280-94589/30 11/02/2011 17:26 1 PC511K02036.d Gemini-NX

DV-LC-0012

Page 182 of 272
Lab Name: Job No.:

SDG No.:

LCMS BATCH WORKSHEET

280-21985-1

Batch Number: Batch Start Date: Batch Analyst:

Batch End Date:

Cokley, Cheyana D

11/02/11 10:15

94046 10/31/11 14:40

Batch Method:

TestAmerica Denver

PFC leach

Lab Sample ID Client Sample ID Method Chain Basis InitialAmount FinalAmount CalcMsg PFOA/S_Spike 

00004

PFOA/S_Sur/IS 

00003

10.08 g 50 mL CALC NOT SET TO 

RUN

MB 280-94046/1 PFC leach, 1 mL

DV-LC-0012

10.00 g 50 mL CALC NOT SET TO 

RUN

LCS 280-94046/2 PFC leach, 1 mL 1 mL

DV-LC-0012

10.12 g 50 mL CALC NOT SET TO 

RUN

LLCS 0.1 mL 1 mL

280-94046/3

PFC leach, 

DV-LC-0012

WWK-S-WWM-1(0-.2

)

10.04 g 50 mL CALC NOT SET TO 

RUN

280-21985-A-1 PFC leach, 1 mL

DV-LC-0012

T

WWK-S-WWM-1(0-.2

)

10.09 g 50 mL CALC NOT SET TO 

RUN

280-21985-A-1 1 mL 1 mL

MS

PFC leach, 

DV-LC-0012

T

WWK-S-WWM-1(0-.2

)

10.06 g 50 mL CALC NOT SET TO 

RUN

280-21985-A-1 1 mL

DU

PFC leach, 

DV-LC-0012

T

DV-LC-0012 Page 1 of 2

Page 183 of 272
Lab Name: Job No.:

SDG No.:

LCMS BATCH WORKSHEET

280-21985-1

Batch Number: Batch Start Date: Batch Analyst:

Batch End Date:

Cokley, Cheyana D

11/02/11 10:15

94046 10/31/11 14:40

Batch Method:

TestAmerica Denver

PFC leach

Batch Notes

Analyst CDC - C

Balance ID 24750836

Batch Comment Filtered by:ACF

HCl Concentration 2.4M

Lot # of hydrochloric acid 2.D.1.7

HCl Pipette ID H

MeOH Pipette # Cylinder

Methanol Lot Number K17E29

NaOH Concentration 0.2M

NaOH Lot # 2-C-1-14

NaOH pipette ID Cylinder

Nominal Amount Used 10 g

Ottawa Sand Lot # 2AB0606

PVDF Filter Lot# W465

Perform Calculation (0=No, 1=Yes) no

Sonication Start Time 10.31.11@1536

Sonication Stop Time 10.31.11@1830

SOP Number DV-OP-0019

Tumble End Time @1115*see ncm* / end time 2 @ 0930

Tumble End Date 11.1.11/ 11.2.11

Tumble Start Time 1900/ start time 2 @ 2141

Tumble Start Date 10.31.11/11.1.11

Witness Reviewer:CullenC

Basis Basis Description

T Total/NA

DV-LC-0012 Page 2 of 2

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Page 248 of 272
GENERAL CHEMISTRY

Page 249 of 272
COVER PAGE

Lab Name: Job Number: 

Client Sample ID Lab Sample ID

GENERAL CHEMISTRY

Project: WWK - Phase III Sampling

SDG No.:

TestAmerica Denver 280-21985-1

WWK-S-WWM-1(0-.2) 280-21985-1 

Comments:

Page 250 of 272
9-IN

Instrument ID: NOEQUIP

Job Number: 280-21985-1

Matrix: Solid

SDG Number:

Lab Name:

GENERAL CHEMISTRY

TestAmerica Denver

DETECTION LIMITS

Method: D 2216 RL Date: 11/01/2009 00:00

Analyte Wavelength/

Mass

RL

(%)

Percent Moisture 0.1

FORM IX - IN

Page 251 of 272
13-IN

ANALYSIS RUN LOG

Lab Name: Job No.:

SDG No.:

Instrument ID: Method:

Start Date: End Date:

TestAmerica Denver 280-21985-1

NOEQUIP

10/26/2011 07:15 10/26/2011 07:15

D 2216

GENERAL CHEMISTRY

Lab

Sample

ID

D

/

F

Time

Analytes

M

o

i

s

t

T

y

p

e

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

280-21985-1 1 T 07:15 X

280-21985-1 DU 1 T 07:15 X

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

FORM XIII-IN Page 252 of 272
13-IN

ANALYSIS RUN LOG

Lab Name: Job No.:

SDG No.:

Instrument ID: Method:

Start Date: End Date:

TestAmerica Denver 280-21985-1

NOEQUIP

10/26/2011 07:15 10/26/2011 07:15

D 2216

GENERAL CHEMISTRY

Lab

Sample

ID

D

/

F

Time

Analytes

M

o

i

s

t

T

y

p

e

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

FORM XIII-IN Page 253 of 272
13-IN

ANALYSIS RUN LOG

Lab Name: Job No.:

SDG No.:

Instrument ID: Method:

Start Date: End Date:

TestAmerica Denver 280-21985-1

NOEQUIP

10/26/2011 07:15 10/26/2011 07:15

D 2216

GENERAL CHEMISTRY

Lab

Sample

ID

D

/

F

Time

Analytes

M

o

i

s

t

T

y

p

e

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

ZZZZZZ 07:15

Prep Types

T = Total/NA

FORM XIII-IN Page 254 of 272
Sop#: Dt/-/+tC'oor,3 Analyst -P B Instrnment: 43i{.'2,

Preo Batch Batch Method Snecial Inst

-T '75.t tO rZ"^*/E lll /lt

TestAmerica Denver

Wet Chemistry Data Review Checklist For Gravimetric Methods

TestNamertvrethod#: {)'l ( tl" J ,', o- AnalvsisDate: /0/<a /r t

Lot / Sample Numbers

Comrnents:

2nd Level Reviewer :

Comments:

tg>tf\t I trtilutl

Matrix

5

I

t,

4tW/ ?t1s-{, 1lnt

z i?97" 77t0 ls.

2.1?sq, /tE

A- Balance, Oven' and DI Water QC Checks Yes No N/A 2d Level

I nas tn" U"i"nte calibration verified before and after processing samples and noted

in the ..Balance Calforation Log" foi the date(s) the sampies ivere processed? /

2lw"s the o"en temperature within method requirements and recorded in the "Oven

Temperature" logbook for the date(s) the samples were processed? L/

Wa". tl" Ouiiy conductiviry check of the deiouized water recorded in the

-Conducti vitv Lo sbook"?

,/

B. Method Requirements

L If samoie is visiblv oily, was this noted on the benchsheet? ;/

Z. Was final residue weight witirinrninimrrm/maximun reqqrsments? /

3.W-*" th" initial anC fiaai dryrn-q dates and times recorded on the benchsheet and

were ali samples dried for at ieast one hour? t/

C. Sample Results

1. TDS/Conductivrw ratio or histoncal data checked? L/

i. For % Moisture, was the Final Dried weight < the Initial Pan weight or is the

result Freater than 100%?

p3. Were sample analYses done within hoiding time? L/

4- Were speciai ciient requirements met? '/ 5. Wsre data that were manualiy trar.scribed from inst'ument pri:rtouts into TALS

verified 100% i:rcludiag significant figures and units?

//

6. Do',he prep aud anaiysis dates i:r TALS reflect the actuai dates?

Lots/Dates report checked?

l-/

l. STD/True Value information is updated and rnciuded? L./

8. Are rarn'data cooies prspared. scanned, and upioaded? t-'

D. Preparationflvlatrix QC

1. Method blank < RL or all reported sarrrfies > i0 X RL? L/-

2. Method btank <'% RL or NCM provided? <./

3. LCSiLCSD run for batch and within eC limits? !/

4. DUP run forbatch and RPD <\AV, for samples >5 X RL? //

Anal-vst: \).o. 

- -/, Date:' 1z,z,t

Revision 2.0

5/1 B/1 0

OAVdit\FORMS\Data Review\Gravimetric Review Checki isl

Page 255 of 272
Lab Name: Job No.:

SDG No.:

GENERAL CHEMISTRY BATCH WORKSHEET

280-21985-1

Batch Number: Batch Start Date: Batch Analyst:

Batch End Date:

93110 10/26/11 07:15 Berry III, Paul B

Batch Method:

TestAmerica Denver

D 2216

Lab Sample ID Client Sample ID Method Chain Basis DISH# DishWeight SampleMassWet SampleMassDry

WWK-S-WWM-1(0-.2

)

280-21985-B-1 D 2216 T 7 1.27 g 17.95 g 13.26 g

WWK-S-WWM-1(0-.2

)

280-21985-B-1 8 1.27 g 17.95 g 13.09 g

DU

D 2216 T

Batch Notes

Balance ID H31422 No Unit

Date samples were placed in the oven 10/26/11

Oven Temp when samples are put in oven 103 Degrees C

Time samples were place in the oven 1230

Date samples were removed from oven 10/27/11

Oven Temp when samples removed from oven 98 Degrees C

Time Samples were removed from oven 0645

Oven ID D / C

ID number of the thermometer Moist ove

Uncorrected In Temperature 103 Celsius

Uncorrected Out Temperature 98 Celsius

Basis Basis Description

T Total/NA

D 2216 Page 1 of 1

Page 256 of 272
Shipping and

Receiving

Documents

Page 257 of 272
Page 258 of 272
Login Sample Receipt Checklist

Client: E.I. du Pont de Nemours and Company ADQM Job Number: 280-21985-1

Login Number: 21985

Question Answer Comment

Creator: Lazarte, Noah M

List Source: TestAmerica Denver

List Number: 1

Radioactivity either was not measured or, if measured, is at or below True

background

The cooler's custody seal, if present, is intact. True

The cooler or samples do not appear to have been compromised or True

tampered with.

Samples were received on ice. True

Cooler Temperature is acceptable. True

Cooler Temperature is recorded. True

COC is present. True

COC is filled out in ink and legible. True

COC is filled out with all pertinent information. True

Is the Field Sampler's name present on COC? True

There are no discrepancies between the sample IDs on the containers and True

the COC.

Samples are received within Holding Time. True

Sample containers have legible labels. True

Containers are not broken or leaking. True

Sample collection date/times are provided. True

Appropriate sample containers are used. True

Sample bottles are completely filled. True

Sample Preservation Verified. True

There is sufficient vol. for all requested analyses, incl. any requested True

MS/MSDs

VOA sample vials do not have headspace or bubble is <6mm (1/4") in N/A

diameter.

Multiphasic samples are not present. True

Samples do not require splitting or compositing. True

Residual Chlorine Checked. N/A

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