# 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 3 0.990. Following initial calibration (ICAL), an initial calibration blank (ICB) is tested, which consists of methanol spiked with the surrogate. The 

### Page 4 of 272result 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 272analyzed 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: Analysis Batch Number: LC_LCMS5 94589 Lab Sample ID: Client Sample ID: Date Analyzed: Lab File ID:
COMPOUND NAME RETENTION TIME MANUAL INTEGRATION DATE ANALYST REASON STD0002 280-94589/2 IC
PC511K02008.d 11/02/11 13:49 GC Column: Gemini-NX ID:

Ammonium Perfluorooctanoate (APFO) Baseline bonnettj 11/03/11 10:25 4.45 Perfluorooctanoic acid (PFOA) Baseline bonnettj 11/03/11 10:25 4.45 Lab Sample ID: Client Sample ID: Date Analyzed: Lab File ID:
COMPOUND NAME RETENTION TIME MANUAL INTEGRATION DATE ANALYST REASON 280-21985-1 WWK-S-WWM-1(0-.2) PC511K02023.d 11/02/11 15:45 GC Column: Gemini-NX ID:

Ammonium Perfluorooctanoate (APFO) Baseline williamst 11/03/11 14:44 4.44 Perfluorooctanoic acid (PFOA) Baseline williamst 11/03/11 14:44 4.44 Lab Sample ID: Client Sample ID: Date Analyzed: Lab File ID:
COMPOUND NAME RETENTION TIME MANUAL INTEGRATION DATE ANALYST REASON 280-21985-1 DU WWK-S-WWM-1(0-.2) DU PC511K02025.d 11/02/11 16:01 GC Column: Gemini-NX ID:

Ammonium Perfluorooctanoate (APFO) Baseline williamst 11/03/11 14:45 4.43 Perfluorooctanoic acid (PFOA) Baseline williamst 11/03/11 14:45 4.43 Lab Sample ID: Client Sample ID: Date Analyzed: Lab File ID:
COMPOUND NAME RETENTION TIME MANUAL INTEGRATION DATE ANALYST REASON CCVL 280-94589/22
PC511K02028.d 11/02/11 16:24 GC Column: Gemini-NX ID:

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

DV-LC-0012 

### Page 7 of 272

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

Client Sample ID Lab 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 Result (ug/Kg) Lab Sample ID Client Sample ID 3.5 0.69 Ammonium Perfluorooctanoate (APFO) 1.07 280-21985-1 WWK-S-WWM-1(0-.2) ND

3.5 0.70 Ammonium Perfluorooctanoate (APFO) 280-21985-1 DU WWK-S-WWM-1(0-.2) NQ

3.5 0.69 Perfluorooctanoic acid (PFOA) 0.983 280-21985-1 WWK-S-WWM-1(0-.2) ND
3.5 0.70 Perfluorooctanoic 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. Moisture Determined by EPA Method 160.3 MOD (e) (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
Preparation Method Method Lab Location Description
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 Bonnett, Jaqueline C JCB TAL-DEN DV-LC-0012 Berry III, Paul B PBB ASTM D 2216

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 ND 3.5 0.69 Ammonium Perfluorooctanoate (APFO) ND 3.5 0.69 Perfluorooctanoic acid (PFOA) Surrogate %Rec Acceptance Limits Qualifier 53 50 - 200 13C4 PFOA

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

TestAmerica Denver 

### Page 13 of 272

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



## 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 49 X

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

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

Solid Client Matrix: 1.0 Dilution: Lab Sample ID: 

### Method Blank - Batch: 280-94046

Instrument ID: Lab File ID: Initial Weight/Volume: Final Weight/Volume: PC511K02020.d 10.08 g 50 mL Units: ug/Kg 

### Method: DV-LC-0012 Preparation: DV-OP-0019

LC_LCMS5 MB 280-94046/1-A

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 RL MDL Qual Result ND 2.5 0.50 Ammonium Perfluorooctanoate (APFO) ND 2.5 0.50 Perfluorooctanoic acid (PFOA) 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 50 mL Units: ug/Kg 

### Method: DV-LC-0012 Preparation: DV-OP-0019

LC_LCMS5 LCS 280-94046/2-A

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 Qual Limit % Rec. Result Spike Amount 52.0 58.0 111 70 - 130 Ammonium Perfluorooctanoate (APFO) 50.0 55.5 111 70 - 130 Perfluorooctanoic acid (PFOA) 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 50 mL Units: ug/Kg 

### Method: DV-LC-0012 Preparation: DV-OP-0019

LC_LCMS5 LLCS 280-94046/3-A

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 Qual Limit % Rec. Result Spike Amount 5.14 5.73 111 70 - 130 Ammonium Perfluorooctanoate (APFO) 4.94 5.48 111 70 - 130 Perfluorooctanoic acid (PFOA) Surrogate % Rec Acceptance Limits 13C4 PFOA 95 50 - 200

TestAmerica Denver 

### Page 15 of 272

## Quality Control Results

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

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 50 mL Units: ug/Kg 

### Method: DV-LC-0012 Preparation: DV-OP-0019

LC_LCMS5 280-21985-1

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

Qual Limit % Rec. Result Spike Amount Sample Result/Qual Analyte
ND 71.7 77.9 109 70 - 130 Ammonium Perfluorooctanoate (APFO) ND 68.9 75.1 109 70 - 130 Perfluorooctanoic acid (PFOA) Surrogate % Rec Acceptance Limits 13C4 PFOA 50 - 200 49 X

ug/Kg Units: 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

LC_LCMS5 280-21985-1

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 Qual Limit RPD Result Sample Result/Qual
1.07 ND NC 20 J Ammonium Perfluorooctanoate (APFO) 0.983 ND NC 20 J Perfluorooctanoic acid (PFOA) Surrogate % Rec Acceptance Limits 13C4 PFOA 51 50 - 200

TestAmerica Denver 

### Page 16 of 272

## Quality Control Results

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

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

LC_LCMS5 DLCK 280-94589/13

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 Qual Limit % Rec. Result Spike Amount 0.520 0.488 94 J 70 - 130 Ammonium Perfluorooctanoate (APFO) 0.500 0.468 94 J 70 - 130 Perfluorooctanoic acid (PFOA) Surrogate % Rec Acceptance Limits 13C4 PFOA 101 50 - 200

TestAmerica Denver 

### Page 17 of 272

## Quality Control Results

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

% 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 No Equipment 280-21985-1

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 Qual Limit RPD Result Sample Result/Qual
29 28 4 20 Percent Moisture

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
Surrogate is outside control limits X

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 Lab Control Sample Solid DV-OP-0019 LCS 280-94046/2-A T Low Level Control Sample Solid DV-OP-0019 LLCS 280-94046/3-A T Method Blank Solid DV-OP-0019 MB 280-94046/1-A T Solid WWK-S-WWM-1(0-.2) DV-OP-0019 280-21985-1 T Duplicate Solid DV-OP-0019 280-21985-1DU T Matrix Spike Solid DV-OP-0019 280-21985-1MS T
Analysis Batch:280-94589 Detection Limit Check Standard Solid DV-LC-0012 DLCK 280-94589/13 T Lab Control Sample Solid 280-94046 DV-LC-0012 LCS 280-94046/2-A T Low Level Control Sample Solid 280-94046 DV-LC-0012 LLCS 280-94046/3-A T Method Blank Solid 280-94046 DV-LC-0012 MB 280-94046/1-A T Solid 280-94046 WWK-S-WWM-1(0-.2) DV-LC-0012 280-21985-1 T Duplicate Solid 280-94046 DV-LC-0012 280-21985-1DU T Matrix Spike Solid 280-94046 DV-LC-0012 280-21985-1MS T

Report Basis T = Total
General Chemistry Analysis Batch:280-93110 Solid WWK-S-WWM-1(0-.2) D 2216 280-21985-1 T Duplicate Solid D 2216 280-21985-1DU T

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: Received Date/Time: 10/24/2011 07:28 280-21985-1 WWK-S-WWM-1(0-.2)

P:DV-OP-0019 280-21985-A-1-A 280-94589 280-94046 10/31/2011 14:40 CDC TAL DEN 1 A:DV-LC-0012 280-21985-A-1-A 280-94589 280-94046 11/02/2011 15:45 JCB TAL DEN 1 A:D 2216 280-21985-B-1 280-93110 10/26/2011 07:15 PBB TAL DEN 1

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: Received Date/Time: 10/24/2011 07:28 280-21985-1 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 CDC TAL DEN 1 A:DV-LC-0012 280-21985-A-1-B MS 280-94589 280-94046 11/02/2011 15:53 JCB TAL DEN 1

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: Received Date/Time: 10/24/2011 07:28 280-21985-1 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 CDC TAL DEN 1 A:DV-LC-0012 280-21985-A-1-C DU 280-94589 280-94046 11/02/2011 16:01 JCB TAL DEN 1 A:D 2216 280-21985-B-1 DU 280-93110 10/26/2011 07:15 PBB TAL DEN 1

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

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

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 CDC TAL DEN 1 A:DV-LC-0012 LLCS 280-94046/3-A 280-94589 280-94046 11/02/2011 15:38 JCB TAL DEN 1
A = Analytical Method P = Prep Method TestAmerica Denver 

### 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 JCB TAL DEN 1



### Lab References: TAL DEN = TestAmerica Denver

A = Analytical Method P = Prep Method TestAmerica Denver 

### Page 22 of 272

### REAGENT TRACEABILITY SUMMARY

Lab Name:

SDG No.: Job No.: 280-21985-1 TestAmerica Denver

Reagent ID Exp Date Date Prep Dilutant Used Reagent Final Volume Parent Reagent

Reagent ID Volume Added Concentration Analyte PFOA/S-IS_LC_00003 13C4 PFOA 10 ug/L 1 mL 20 uL 11/16/11 11/02/11 PFOA/S-Cal0_00037 80:20 Methanol : H2O, Lot J29E57:K02E01 13C4 PFOS 9.56 ug/L 13C4PFOAStock_00013 13C4 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 .PFOA/S-IS_LC_00003 Methanol, Lot J29E57 13C4PFOSStock_00013 0.1 mL 13C4 PFOS 0.478 ug/mL 06/22/13 (Purchased Reagent) 13C4 PFOA 50 ug/mL Wellington, Lot MPFOA0610 ..13C4PFOAStock_00013 09/08/13 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL Wellington, Lot MPFOS0910 ..13C4PFOSStock_00013 PFOA/S-IS_LC_00003 13C4 PFOA 10 ug/L 1 mL 20 uL 11/16/11 11/02/11 PFOA/S-Cal1_00035 80:20 Methanol : H2O, 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) 0.20812 ug/L PFOA/S_CALwSk_00013 10 uL 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 13C4PFOAStock_00013 13C4 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 .PFOA/S-IS_LC_00003 Methanol, Lot J29E57 13C4 PFOA (IS) 0.5 ug/mL 13C4 PFOS 0.478 ug/mL 13C4PFOSStock_00013 0.1 mL 13C4 PFOS (IS) 0.478 ug/mL 06/22/13 (Purchased Reagent) 13C4 PFOA 50 ug/mL Wellington, Lot MPFOA0610 ..13C4PFOAStock_00013 13C4 PFOA (IS) 50 ug/mL 09/08/13 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL Wellington, Lot MPFOS0910 ..13C4PFOSStock_00013 13C4 PFOS (IS) 47.8 ug/mL PFOA/S_Spike_00004 Ammonium Perfluorooctanoate (APFO) 20.812 ug/L 10 mL 0.4 mL 11/02/11 07/03/11 .PFOA/S_CALwSk_00013 80:20 Methanol : H2O, Lot J29E57:K02E01 Perfluorooctanoic acid (PFOA) 20 ug/L Perfluorooctanoic Sulfonate 19.12 ug/L 13C8 PFOA 20 ug/L PFOA/S_Sur_LC_00003 0.4 mL 13C8 PFOS 19.12 ug/L PFOA-stock_00002 Ammonium Perfluorooctanoate (APFO) 0.5203 ug/mL 100 mL 1 mL 11/02/11 11/02/10 ..PFOA/S_Spike_00004 Methanol, Lot J29E57 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) 52.03 ug/mL Wellington, Lot PFOA0609 ...PFOA-stock_00002 Perfluorooctanoic acid (PFOA) 50 ug/mL 05/05/12 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL Wellington, Lot LPFOS0409 ...PFOS-Stock_00002 13C8PFOA-stk_00006 13C8 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 ..PFOA/S_Sur_LC_00003 Methanol, Lot J29E57 13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL 01/29/13 (Purchased Reagent) 13C8 PFOA 50 ug/mL Wellington Laboratories, Lot M8PFOA0110 ...13C8PFOA-stk_00006 05/06/13 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL Wellington Laboratories, Lot M8PFOS0510 ...13C8PFOS-stk_00006 PFOA/S-IS_LC_00003 13C4 PFOA 10 ug/L 1 mL 20 uL 11/02/11 11/02/11 PFOA/S-Cal2_00034 80:20 Methanol : H2O, 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.: Job No.: 280-21985-1 TestAmerica Denver

Reagent ID Exp Date Date Prep Dilutant Used Reagent Final Volume Parent Reagent

Reagent ID Volume Added Concentration Analyte Ammonium Perfluorooctanoate (APFO) 0.5203 ug/L PFOA/S_CALwSk_00013 25 uL 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 13C4PFOAStock_00013 13C4 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 .PFOA/S-IS_LC_00003 Methanol, Lot J29E57 13C4 PFOA (IS) 0.5 ug/mL 13C4 PFOS 0.478 ug/mL 13C4PFOSStock_00013 0.1 mL 13C4 PFOS (IS) 0.478 ug/mL 06/22/13 (Purchased Reagent) 13C4 PFOA 50 ug/mL Wellington, Lot MPFOA0610 ..13C4PFOAStock_00013 13C4 PFOA (IS) 50 ug/mL 09/08/13 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL Wellington, Lot MPFOS0910 ..13C4PFOSStock_00013 13C4 PFOS (IS) 47.8 ug/mL PFOA/S_Spike_00004 Ammonium Perfluorooctanoate (APFO) 20.812 ug/L 10 mL 0.4 mL 11/02/11 07/03/11 .PFOA/S_CALwSk_00013 80:20 Methanol : H2O, Lot J29E57:K02E01 Perfluorooctanoic acid (PFOA) 20 ug/L Perfluorooctanoic Sulfonate 19.12 ug/L 13C8 PFOA 20 ug/L PFOA/S_Sur_LC_00003 0.4 mL 13C8 PFOS 19.12 ug/L PFOA-stock_00002 Ammonium Perfluorooctanoate (APFO) 0.5203 ug/mL 100 mL 1 mL 11/02/11 11/02/10 ..PFOA/S_Spike_00004 Methanol, Lot J29E57 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) 52.03 ug/mL Wellington, Lot PFOA0609 ...PFOA-stock_00002 Perfluorooctanoic acid (PFOA) 50 ug/mL 05/05/12 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL Wellington, Lot LPFOS0409 ...PFOS-Stock_00002 13C8PFOA-stk_00006 13C8 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 ..PFOA/S_Sur_LC_00003 Methanol, Lot J29E57 13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL 01/29/13 (Purchased Reagent) 13C8 PFOA 50 ug/mL Wellington Laboratories, Lot M8PFOA0110 ...13C8PFOA-stk_00006 05/06/13 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL Wellington Laboratories, Lot M8PFOS0510 ...13C8PFOS-stk_00006 PFOA/S-IS_LC_00003 13C4 PFOA 10 ug/L 1 mL 20 uL 11/02/11 11/02/11 PFOA/S-Cal3_00034 80:20 Methanol : H2O, 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) 1.0406 ug/L PFOA/S_CALwSk_00013 50 uL Perfluorooctanoic acid (PFOA) 1 ug/L Perfluorooctanoic Sulfonate 0.956 ug/L 13C8 PFOA 1 ug/L 13C8 PFOS 0.956 ug/L 13C4PFOAStock_00013 13C4 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 .PFOA/S-IS_LC_00003 Methanol, Lot J29E57 13C4 PFOA (IS) 0.5 ug/mL 13C4 PFOS 0.478 ug/mL 13C4PFOSStock_00013 0.1 mL 13C4 PFOS (IS) 0.478 ug/mL 06/22/13 (Purchased Reagent) 13C4 PFOA 50 ug/mL Wellington, Lot MPFOA0610 ..13C4PFOAStock_00013 13C4 PFOA (IS) 50 ug/mL 09/08/13 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL Wellington, Lot MPFOS0910 ..13C4PFOSStock_00013 13C4 PFOS (IS) 47.8 ug/mL 

### Page 24 of 272

### REAGENT TRACEABILITY SUMMARY

Lab Name:

SDG No.: Job No.: 280-21985-1 TestAmerica Denver

Reagent ID Exp Date Date Prep Dilutant Used Reagent Final Volume Parent Reagent

Reagent ID Volume Added Concentration Analyte PFOA/S_Spike_00004 Ammonium Perfluorooctanoate (APFO) 20.812 ug/L 10 mL 0.4 mL 11/02/11 07/03/11 .PFOA/S_CALwSk_00013 80:20 Methanol : H2O, Lot J29E57:K02E01 Perfluorooctanoic acid (PFOA) 20 ug/L Perfluorooctanoic Sulfonate 19.12 ug/L 13C8 PFOA 20 ug/L PFOA/S_Sur_LC_00003 0.4 mL 13C8 PFOS 19.12 ug/L PFOA-stock_00002 Ammonium Perfluorooctanoate (APFO) 0.5203 ug/mL 100 mL 1 mL 11/02/11 11/02/10 ..PFOA/S_Spike_00004 Methanol, Lot J29E57 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) 52.03 ug/mL Wellington, Lot PFOA0609 ...PFOA-stock_00002 Perfluorooctanoic acid (PFOA) 50 ug/mL 05/05/12 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL Wellington, Lot LPFOS0409 ...PFOS-Stock_00002 13C8PFOA-stk_00006 13C8 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 ..PFOA/S_Sur_LC_00003 Methanol, Lot J29E57 13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL 01/29/13 (Purchased Reagent) 13C8 PFOA 50 ug/mL Wellington Laboratories, Lot M8PFOA0110 ...13C8PFOA-stk_00006 05/06/13 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL Wellington Laboratories, Lot M8PFOS0510 ...13C8PFOS-stk_00006 PFOA/S-IS_LC_00003 13C4 PFOA 10 ug/L 1 mL 20 uL 11/02/11 11/02/11 PFOA/S-Cal4_00035 80:20 Methanol : H2O, 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) 2.0812 ug/L PFOA/S_CALwSk_00013 100 uL Perfluorooctanoic acid (PFOA) 2 ug/L Perfluorooctanoic Sulfonate 1.912 ug/L 13C8 PFOA 2 ug/L 13C8 PFOS 1.912 ug/L 13C4PFOAStock_00013 13C4 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 .PFOA/S-IS_LC_00003 Methanol, Lot J29E57 13C4 PFOA (IS) 0.5 ug/mL 13C4 PFOS 0.478 ug/mL 13C4PFOSStock_00013 0.1 mL 13C4 PFOS (IS) 0.478 ug/mL 06/22/13 (Purchased Reagent) 13C4 PFOA 50 ug/mL Wellington, Lot MPFOA0610 ..13C4PFOAStock_00013 13C4 PFOA (IS) 50 ug/mL 09/08/13 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL Wellington, Lot MPFOS0910 ..13C4PFOSStock_00013 13C4 PFOS (IS) 47.8 ug/mL PFOA/S_Spike_00004 Ammonium Perfluorooctanoate (APFO) 20.812 ug/L 10 mL 0.4 mL 11/02/11 07/03/11 .PFOA/S_CALwSk_00013 80:20 Methanol : H2O, Lot J29E57:K02E01 Perfluorooctanoic acid (PFOA) 20 ug/L Perfluorooctanoic Sulfonate 19.12 ug/L 13C8 PFOA 20 ug/L PFOA/S_Sur_LC_00003 0.4 mL 13C8 PFOS 19.12 ug/L PFOA-stock_00002 Ammonium Perfluorooctanoate (APFO) 0.5203 ug/mL 100 mL 1 mL 11/02/11 11/02/10 ..PFOA/S_Spike_00004 Methanol, Lot J29E57 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) 52.03 ug/mL Wellington, Lot PFOA0609 ...PFOA-stock_00002 Perfluorooctanoic acid (PFOA) 50 ug/mL 05/05/12 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL Wellington, Lot LPFOS0409 ...PFOS-Stock_00002 

### Page 25 of 272

### REAGENT TRACEABILITY SUMMARY

Lab Name:

SDG No.: Job No.: 280-21985-1 TestAmerica Denver

Reagent ID Exp Date Date Prep Dilutant Used Reagent Final Volume Parent Reagent

Reagent ID Volume Added Concentration Analyte 13C8PFOA-stk_00006 13C8 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 ..PFOA/S_Sur_LC_00003 Methanol, Lot J29E57 13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL 01/29/13 (Purchased Reagent) 13C8 PFOA 50 ug/mL Wellington Laboratories, Lot M8PFOA0110 ...13C8PFOA-stk_00006 05/06/13 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL Wellington Laboratories, Lot M8PFOS0510 ...13C8PFOS-stk_00006 PFOA/S-IS_LC_00003 13C4 PFOA 10 ug/L 1 mL 20 uL 11/02/11 11/02/11 PFOA/S-Cal5_00035 80:20 Methanol : H2O, 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) 5.203 ug/L PFOA/S_CALwSk_00013 250 uL Perfluorooctanoic acid (PFOA) 5 ug/L Perfluorooctanoic Sulfonate 4.78 ug/L 13C8 PFOA 5 ug/L 13C8 PFOS 4.78 ug/L 13C4PFOAStock_00013 13C4 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 .PFOA/S-IS_LC_00003 Methanol, Lot J29E57 13C4 PFOA (IS) 0.5 ug/mL 13C4 PFOS 0.478 ug/mL 13C4PFOSStock_00013 0.1 mL 13C4 PFOS (IS) 0.478 ug/mL 06/22/13 (Purchased Reagent) 13C4 PFOA 50 ug/mL Wellington, Lot MPFOA0610 ..13C4PFOAStock_00013 13C4 PFOA (IS) 50 ug/mL 09/08/13 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL Wellington, Lot MPFOS0910 ..13C4PFOSStock_00013 13C4 PFOS (IS) 47.8 ug/mL PFOA/S_Spike_00004 Ammonium Perfluorooctanoate (APFO) 20.812 ug/L 10 mL 0.4 mL 11/02/11 07/03/11 .PFOA/S_CALwSk_00013 80:20 Methanol : H2O, Lot J29E57:K02E01 Perfluorooctanoic acid (PFOA) 20 ug/L Perfluorooctanoic Sulfonate 19.12 ug/L 13C8 PFOA 20 ug/L PFOA/S_Sur_LC_00003 0.4 mL 13C8 PFOS 19.12 ug/L PFOA-stock_00002 Ammonium Perfluorooctanoate (APFO) 0.5203 ug/mL 100 mL 1 mL 11/02/11 11/02/10 ..PFOA/S_Spike_00004 Methanol, Lot J29E57 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) 52.03 ug/mL Wellington, Lot PFOA0609 ...PFOA-stock_00002 Perfluorooctanoic acid (PFOA) 50 ug/mL 05/05/12 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL Wellington, Lot LPFOS0409 ...PFOS-Stock_00002 13C8PFOA-stk_00006 13C8 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 ..PFOA/S_Sur_LC_00003 Methanol, Lot J29E57 13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL 01/29/13 (Purchased Reagent) 13C8 PFOA 50 ug/mL Wellington Laboratories, Lot M8PFOA0110 ...13C8PFOA-stk_00006 05/06/13 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL Wellington Laboratories, Lot M8PFOS0510 ...13C8PFOS-stk_00006 PFOA/S-IS_LC_00003 13C4 PFOA 10 ug/L 1 mL 20 uL 11/02/11 11/02/11 PFOA/S-Cal6_00037 80:20 Methanol : H2O, 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) 10.406 ug/L PFOA/S_CALwSk_00013 500 uL Perfluorooctanoic acid (PFOA) 10 ug/L Perfluorooctanoic Sulfonate 9.56 ug/L 

### Page 26 of 272

### REAGENT TRACEABILITY SUMMARY

Lab Name:

SDG No.: Job No.: 280-21985-1 TestAmerica Denver

Reagent ID Exp Date Date Prep Dilutant Used Reagent Final Volume Parent Reagent

Reagent ID Volume Added Concentration Analyte 13C8 PFOA 10 ug/L 13C8 PFOS 9.56 ug/L 13C4PFOAStock_00013 13C4 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 .PFOA/S-IS_LC_00003 Methanol, Lot J29E57 13C4 PFOA (IS) 0.5 ug/mL 13C4 PFOS 0.478 ug/mL 13C4PFOSStock_00013 0.1 mL 13C4 PFOS (IS) 0.478 ug/mL 06/22/13 (Purchased Reagent) 13C4 PFOA 50 ug/mL Wellington, Lot MPFOA0610 ..13C4PFOAStock_00013 13C4 PFOA (IS) 50 ug/mL 09/08/13 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL Wellington, Lot MPFOS0910 ..13C4PFOSStock_00013 13C4 PFOS (IS) 47.8 ug/mL PFOA/S_Spike_00004 Ammonium Perfluorooctanoate (APFO) 20.812 ug/L 10 mL 0.4 mL 11/02/11 07/03/11 .PFOA/S_CALwSk_00013 80:20 Methanol : H2O, Lot J29E57:K02E01 Perfluorooctanoic acid (PFOA) 20 ug/L Perfluorooctanoic Sulfonate 19.12 ug/L 13C8 PFOA 20 ug/L PFOA/S_Sur_LC_00003 0.4 mL 13C8 PFOS 19.12 ug/L PFOA-stock_00002 Ammonium Perfluorooctanoate (APFO) 0.5203 ug/mL 100 mL 1 mL 11/02/11 11/02/10 ..PFOA/S_Spike_00004 Methanol, Lot J29E57 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) 52.03 ug/mL Wellington, Lot PFOA0609 ...PFOA-stock_00002 Perfluorooctanoic acid (PFOA) 50 ug/mL 05/05/12 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL Wellington, Lot LPFOS0409 ...PFOS-Stock_00002 13C8PFOA-stk_00006 13C8 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 ..PFOA/S_Sur_LC_00003 Methanol, Lot J29E57 13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL 01/29/13 (Purchased Reagent) 13C8 PFOA 50 ug/mL Wellington Laboratories, Lot M8PFOA0110 ...13C8PFOA-stk_00006 05/06/13 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL Wellington Laboratories, Lot M8PFOS0510 ...13C8PFOS-stk_00006 PFOA/S-IS_LC_00003 13C4 PFOA 10 ug/L 1 mL 20 uL 11/02/11 11/02/11 PFOA/S-Cal7_00034 80:20 Methanol : H2O, 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) 20.812 ug/L PFOA/S_Spike_00004 40 uL Perfluorooctanoic acid (PFOA) 20 ug/L Perfluorooctanoic Sulfonate 19.12 ug/L 13C8 PFOA 20 ug/L PFOA/S_Sur_LC_00003 40 uL 13C8 PFOS 19.12 ug/L 13C4PFOAStock_00013 13C4 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 .PFOA/S-IS_LC_00003 Methanol, Lot J29E57 13C4 PFOA (IS) 0.5 ug/mL 13C4 PFOS 0.478 ug/mL 13C4PFOSStock_00013 0.1 mL 13C4 PFOS (IS) 0.478 ug/mL 06/22/13 (Purchased Reagent) 13C4 PFOA 50 ug/mL Wellington, Lot MPFOA0610 ..13C4PFOAStock_00013 13C4 PFOA (IS) 50 ug/mL 09/08/13 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL Wellington, Lot MPFOS0910 ..13C4PFOSStock_00013 13C4 PFOS (IS) 47.8 ug/mL PFOA-stock_00002 Ammonium Perfluorooctanoate (APFO) 0.5203 ug/mL 100 mL 1 mL 11/02/11 11/02/10 .PFOA/S_Spike_00004 Methanol, Lot J29E57 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.: Job No.: 280-21985-1 TestAmerica Denver

Reagent ID Exp Date Date Prep Dilutant Used Reagent Final Volume Parent Reagent

Reagent ID Volume Added Concentration Analyte 06/01/12 (Purchased Reagent) Ammonium Perfluorooctanoate (APFO) 52.03 ug/mL Wellington, Lot PFOA0609 ..PFOA-stock_00002 Perfluorooctanoic acid (PFOA) 50 ug/mL 05/05/12 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL Wellington, Lot LPFOS0409 ..PFOS-Stock_00002 13C8PFOA-stk_00006 13C8 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 .PFOA/S_Sur_LC_00003 Methanol, Lot J29E57 13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL 01/29/13 (Purchased Reagent) 13C8 PFOA 50 ug/mL Wellington Laboratories, Lot M8PFOA0110 ..13C8PFOA-stk_00006 05/06/13 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL Wellington Laboratories, Lot M8PFOS0510 ..13C8PFOS-stk_00006 PFOA/S-IS_LC_00003 13C4 PFOA 10 ug/L 1 mL 20 uL 11/02/11 11/02/11 PFOA/S-Cal8_00022 80:20 Methanol : H2O, 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) 52.03 ug/L PFOA/S_Spike_00004 100 uL Perfluorooctanoic acid (PFOA) 50 ug/L Perfluorooctanoic Sulfonate 47.8 ug/L 13C8 PFOA 50 ug/L PFOA/S_Sur_LC_00003 100 uL 13C8 PFOS 47.8 ug/L 13C4PFOAStock_00013 13C4 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 .PFOA/S-IS_LC_00003 Methanol, Lot J29E57 13C4 PFOA (IS) 0.5 ug/mL 13C4 PFOS 0.478 ug/mL 13C4PFOSStock_00013 0.1 mL 13C4 PFOS (IS) 0.478 ug/mL 06/22/13 (Purchased Reagent) 13C4 PFOA 50 ug/mL Wellington, Lot MPFOA0610 ..13C4PFOAStock_00013 13C4 PFOA (IS) 50 ug/mL 09/08/13 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL Wellington, Lot MPFOS0910 ..13C4PFOSStock_00013 13C4 PFOS (IS) 47.8 ug/mL PFOA-stock_00002 Ammonium Perfluorooctanoate (APFO) 0.5203 ug/mL 100 mL 1 mL 11/02/11 11/02/10 .PFOA/S_Spike_00004 Methanol, Lot J29E57 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) 52.03 ug/mL Wellington, Lot PFOA0609 ..PFOA-stock_00002 Perfluorooctanoic acid (PFOA) 50 ug/mL 05/05/12 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL Wellington, Lot LPFOS0409 ..PFOS-Stock_00002 13C8PFOA-stk_00006 13C8 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 .PFOA/S_Sur_LC_00003 Methanol, Lot J29E57 13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL 01/29/13 (Purchased Reagent) 13C8 PFOA 50 ug/mL Wellington Laboratories, Lot M8PFOA0110 ..13C8PFOA-stk_00006 05/06/13 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL Wellington Laboratories, Lot M8PFOS0510 ..13C8PFOS-stk_00006 PFOA/S-IS_LC_00003 13C4 PFOA 10 ug/L 1 mL 20 uL 11/02/11 11/02/11 PFOA/S-Cal9_00022 80:20 Methanol : H2O, 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) 130.075 ug/L PFOA/S_Spike_00004 250 uL Perfluorooctanoic acid (PFOA) 125 ug/L Perfluorooctanoic Sulfonate 119.5 ug/L 13C8 PFOA 125 ug/L PFOA/S_Sur_LC_00003 250 uL 13C8 PFOS 119.5 ug/L 

### Page 28 of 272

### REAGENT TRACEABILITY SUMMARY

Lab Name:

SDG No.: Job No.: 280-21985-1 TestAmerica Denver

Reagent ID Exp Date Date Prep Dilutant Used Reagent Final Volume Parent Reagent

Reagent ID Volume Added Concentration Analyte 13C4PFOAStock_00013 13C4 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 .PFOA/S-IS_LC_00003 Methanol, Lot J29E57 13C4 PFOA (IS) 0.5 ug/mL 13C4 PFOS 0.478 ug/mL 13C4PFOSStock_00013 0.1 mL 13C4 PFOS (IS) 0.478 ug/mL 06/22/13 (Purchased Reagent) 13C4 PFOA 50 ug/mL Wellington, Lot MPFOA0610 ..13C4PFOAStock_00013 13C4 PFOA (IS) 50 ug/mL 09/08/13 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL Wellington, Lot MPFOS0910 ..13C4PFOSStock_00013 13C4 PFOS (IS) 47.8 ug/mL PFOA-stock_00002 Ammonium Perfluorooctanoate (APFO) 0.5203 ug/mL 100 mL 1 mL 11/02/11 11/02/10 .PFOA/S_Spike_00004 Methanol, Lot J29E57 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) 52.03 ug/mL Wellington, Lot PFOA0609 ..PFOA-stock_00002 Perfluorooctanoic acid (PFOA) 50 ug/mL 05/05/12 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL Wellington, Lot LPFOS0409 ..PFOS-Stock_00002 13C8PFOA-stk_00006 13C8 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 .PFOA/S_Sur_LC_00003 Methanol, Lot J29E57 13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL 01/29/13 (Purchased Reagent) 13C8 PFOA 50 ug/mL Wellington Laboratories, Lot M8PFOA0110 ..13C8PFOA-stk_00006 05/06/13 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL Wellington Laboratories, Lot M8PFOS0510 ..13C8PFOS-stk_00006 PFOA/S-IS_LC_00003 13C4 PFOA 10 ug/L 1 mL 20 uL 11/16/11 11/02/11 PFOA/S-CALicv_00034 80:20 Methanol : H2O, Lot J29E57:K02E01 13C4 PFOS 9.56 ug/L Ammonium Perfluorooctanoate (APFO) 2.0812 ug/L PFOA/S_ICVWSk_00006 100 uL Perfluorooctanoic acid (PFOA) 2 ug/L 13C8 PFOA 2 ug/L 13C8 PFOS 1.912 ug/L 13C4PFOAStock_00013 13C4 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 .PFOA/S-IS_LC_00003 Methanol, Lot J29E57 13C4PFOSStock_00013 0.1 mL 13C4 PFOS 0.478 ug/mL 06/22/13 (Purchased Reagent) 13C4 PFOA 50 ug/mL Wellington, Lot MPFOA0610 ..13C4PFOAStock_00013 09/08/13 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL Wellington, Lot MPFOS0910 ..13C4PFOSStock_00013 PFOA/S_ICVStk_00003 Ammonium Perfluorooctanoate (APFO) 20.812 ug/L 10 mL 0.2 mL 04/18/12 07/03/11 .PFOA/S_ICVWSk_00006 80:20 Methanol : H2O, Lot J57E02 Perfluorooctanoic acid (PFOA) 20 ug/L 13C8 PFOA 20 ug/L PFOA/S_Sur_LC_00003 0.4 mL 13C8 PFOS 19.12 ug/L PFOA_ICVStk_00003 Ammonium Perfluorooctanoate (APFO) 1040.6 ug/L 10 mL 0.1 mL 07/03/12 07/03/11 ..PFOA/S_ICVStk_00003 Methanol, Lot 5.76.1 Perfluorooctanoic acid (PFOA) 1000 ug/L 11/02/20 (Purchased Reagent) Ammonium Perfluorooctanoate (APFO) 104.06 ug/mL Accustandard, Lot 210041455-01 ...PFOA_ICVStk_00003 Perfluorooctanoic acid (PFOA) 100 ug/mL 13C8PFOA-stk_00006 13C8 PFOA 0.5 ug/mL 10 mL 0.1 mL 04/18/12 04/19/11 ..PFOA/S_Sur_LC_00003 Methanol, Lot J29E57 13C8PFOS-stk_00006 0.1 mL 13C8 PFOS 0.478 ug/mL 01/29/13 (Purchased Reagent) 13C8 PFOA 50 ug/mL Wellington Laboratories, Lot M8PFOA0110 ...13C8PFOA-stk_00006 05/06/13 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL Wellington Laboratories, Lot M8PFOS0510 ...13C8PFOS-stk_00006 PFOA-stock_00002 Ammonium Perfluorooctanoate (APFO) 0.5203 ug/mL 100 mL 1 mL 11/02/11 11/02/10 PFOA/S_Spike_00004 Methanol, Lot J29E57 Perfluorooctanoic acid (PFOA) 0.5 ug/mL 

### Page 29 of 272

### REAGENT TRACEABILITY SUMMARY

Lab Name:

SDG No.: Job No.: 280-21985-1 TestAmerica Denver

Reagent ID Exp Date Date Prep Dilutant Used Reagent Final Volume Parent Reagent

Reagent ID Volume Added Concentration Analyte PFOS-Stock_00002 1 mL Perfluorooctanoic Sulfonate 0.478 ug/mL 06/01/12 (Purchased Reagent) Ammonium Perfluorooctanoate (APFO) 52.03 ug/mL Wellington, Lot PFOA0609 .PFOA-stock_00002 Perfluorooctanoic acid (PFOA) 50 ug/mL 05/05/12 (Purchased Reagent) Perfluorooctanoic Sulfonate 47.8 ug/mL Wellington, Lot LPFOS0409 .PFOS-Stock_00002 13C4PFOAStock_00015 13C4 PFOA 0.5 ug/mL 100 mL 1 mL 04/19/12 04/19/11 PFOA/S_Sur/IS_00003 Methanol, Lot J29E57 13C4 PFOA (IS) 0.5 ug/mL 13C4 PFOS 0.478 ug/mL 13C4PFOSStock_00015 1 mL 13C4 PFOS (IS) 0.478 ug/mL 13C8 PFOA 0.5 ug/mL 13C8PFOA-stk_00008 1 mL 13C8PFOS-stk_00008 1 mL 13C8 PFOS 0.478 ug/mL 05/12/14 (Purchased Reagent) 13C4 PFOA 50 ug/mL Wellington, Lot MPFOA0511 .13C4PFOAStock_00015 13C4 PFOA (IS) 50 ug/mL 05/05/14 (Purchased Reagent) 13C4 PFOS 47.8 ug/mL Wellington, Lot MPFOS0511 .13C4PFOSStock_00015 13C4 PFOS (IS) 47.8 ug/mL 05/12/14 (Purchased Reagent) 13C8 PFOA 50 ug/mL Wellington Laboratories, Lot M8PFOA0511 .13C8PFOA-stk_00008 05/06/13 (Purchased Reagent) 13C8 PFOS 47.8 ug/mL Wellington Laboratories, Lot M8PFOS0510 .13C8PFOS-stk_00008



### 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 2907.01 DoD ELAP A2LA TestAmerica Denver 2907.01 ISO/IEC 17025 A2LA TestAmerica Denver 40730 State Program Alabama 4 TestAmerica Denver UST-30 Alaska UST Alaska 10 TestAmerica Denver AZ0713 State Program Arizona 9 TestAmerica Denver 88-0687 State Program Arkansas 6 TestAmerica Denver 2513 State Program California 9 TestAmerica Denver N/A State Program Colorado 8 TestAmerica Denver PH-0686 State Program Connecticut 1 TestAmerica Denver E87667 NELAC Florida 4 TestAmerica Denver N/A State Program Georgia 4 TestAmerica Denver CO00026 State Program Idaho 10 TestAmerica Denver 200017 NELAC Illinois 5 TestAmerica Denver 370 State Program Iowa 7 TestAmerica Denver E-10166 NELAC Kansas 7 TestAmerica Denver 30785 NELAC Louisiana 6 TestAmerica Denver CO0002 State Program Maine 1 TestAmerica Denver 268 State Program Maryland 3 TestAmerica Denver 8-999-405 NELAC Minnesota 5 TestAmerica Denver CO0026 State Program Nevada 9 TestAmerica Denver 205310 NELAC New Hampshire 1 TestAmerica Denver CO004 NELAC New Jersey 2 TestAmerica Denver N/A State Program New Mexico 6 TestAmerica Denver 11964 NELAC New York 2 TestAmerica Denver 358 North Carolina DENR North Carolina 4 TestAmerica Denver R-034 State Program North Dakota 8 TestAmerica Denver 8614 State Program Oklahoma 6 TestAmerica Denver CO200001 NELAC Oregon 10 TestAmerica Denver 68-00664 NELAC Pennsylvania 3 TestAmerica Denver 72002 State Program South Carolina 4 TestAmerica Denver TN02944 State Program Tennessee 4 TestAmerica Denver T104704183-08-TX NELAC Texas 6 TestAmerica Denver P330-08-00036 USDA USDA TestAmerica Denver QUAN5 NELAC Utah 8 TestAmerica Denver C1284 State Program Washington 10 TestAmerica Denver 354 West Virginia DEP West Virginia 3 TestAmerica Denver 999615430 State Program Wisconsin 5 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.



### TestAmerica Denver 

### Page 31 of 272

# 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:

Lab Sample ID Client Sample ID # PFOA
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 49 X
280-21985-1 DU WWK-S-WWM-1(0-.2) DU 51

DLCK 280-94589/13 101



### QC LIMITS QC LIMITS PFOA = 13C4 PFOA 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

Job No.: Lab Name:
SDG No.: Level: Matrix: Matrix: Low 280-21985-1

Lab File ID: PC511K02021.d Solid
Lab ID: LCS 280-94046/2-A Client ID: TestAmerica Denver

REC % REC QC LIMITS CONCENTRATION (ug/Kg) SPIKE ADDED (ug/Kg) # LCS LCS

COMPOUND Ammonium Perfluorooctanoate (APFO) 52.0 58.0 70-130 111 Perfluorooctanoic acid (PFOA) 50.0 55.5 70-130 111

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

Job No.: Lab Name:
SDG No.: Level: Matrix: Matrix: Low 280-21985-1

Lab File ID: PC511K02022.d Solid
Lab ID: LLCS 280-94046/3-A Client ID: TestAmerica Denver

REC % REC QC LIMITS CONCENTRATION (ug/Kg) SPIKE ADDED (ug/Kg) # LLCS LLCS

COMPOUND Ammonium Perfluorooctanoate (APFO) 5.14 5.73 70-130 111 Perfluorooctanoic acid (PFOA) 4.94 5.48 70-130 111

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

Job No.: Lab Name:
SDG No.: Level: Matrix: Matrix: Low 280-21985-1

Lab File ID: PC511K02024.d Solid
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

71.7 77.9 70-130 Ammonium Perfluorooctanoate (APFO) 109 ND
68.9 75.1 70-130 Perfluorooctanoic acid (PFOA) 109 ND

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

Job No.: Lab Name:
SDG No.: Level: Matrix: Matrix: Low 280-21985-1

Lab File ID: PC511K02019.d Solid
Lab ID: DLCK 280-94589/13 Client ID: TestAmerica Denver

REC % REC QC LIMITS CONCENTRATION (ug/L) SPIKE ADDED (ug/L) # DLCK DLCK

COMPOUND Ammonium Perfluorooctanoate (APFO) 0.520 0.488 70-130 94 J Perfluorooctanoic acid (PFOA) 0.500 0.468 70-130 94 J

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.: Job No.: 280-21985-1 TestAmerica Denver

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 FILE ID DATE ANALYZED CLIENT SAMPLE ID 11/02/2011 15:30 PC511K02021 .d LCS 280-94046/2-A 11/02/2011 15:38 PC511K02022 .d LLCS 280-94046/3-A 11/02/2011 15:45 PC511K02023 .d 280-21985-1 WWK-S-WWM-1(0-.2) 11/02/2011 15:53 PC511K02024 .d 280-21985-1 MS WWK-S-WWM-1(0-.2) MS 11/02/2011 16:01 PC511K02025 .d 280-21985-1 DU WWK-S-WWM-1(0-.2) DU

FORM IV DV-LC-0012 

### Page 38 of 272

### FORM I Form 1 LCMS ORGANICS ANALYSIS DATA SHEET

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: PC511K02023.d Lab File ID:
Date Collected: DV-LC-0012 Analysis Method: 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: ID: Gemini-NX
N Analysis Batch No.: 94589 ug/Kg Units:

CAS NO. COMPOUND NAME RESULT Q MDL RL

3.5 0.69 3825-26-1 Ammonium Perfluorooctanoate (APFO) ND 3.5 0.69 335-67-1 Perfluorooctanoic acid (PFOA) ND



### SURROGATE %REC CAS NO. LIMITS Q

53 50-200 STL00990 13C4 PFOA



### 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) In j ect. Date: 02-Nov-2011 15:45:51 Dil. Factor: 1.0000 Sample T y pe: Client Sample ID: 280-21985-a-1-a , Sample Misc. In f o.: O perator: TW / J B Instrument ID: LC_LCMS5 V ol. In j ected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 94589 Lims Sample ID: 17 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 14:45:19 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant By : Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC308 First Level Revie w

er: w illiamst Date: 03-Nov-2011 14:44:09 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C8 PF O A 421.0 > 375.9 4.440 4.433 0.007 1.000 9774712 10.5

* 4 13C4 PF O A (IS) 417.0 > 371.9 4.441 4.434 0.007 11345925 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.441 4.434 0.007 11345925 5.27 3 Ammonium Per

f luorooctanoate (APF O ) 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 Per f luorooctanoic 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 PF O S 506.9 > 80.0 4.588 4.586 0.002 1.000 3221622 10.3 2 Per f luorooctanoic Sul f

onate 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 PF O S (IS) 502.9 > 80.0 4.588 4.586 0.002 3425245 9.56 $ 8 13C4 PF O S 502.9 > 80.0 4.588 4.586 0.002 3425245 6.22 QC Flag Legend Revie w Flags M - Manuall y

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: 945 8 9 Lims Sample ID: 17 Operator ID: T W / JB Injection V ol: 20.00 ul $ 9 13C 8

PFOA

2.9 3.9 4.9

Min 0 4 8 12 16 20 24 2 8Y(X100000) C511K02023 [ MS QQQ Chro ] :m /z 421.0 > 375.94.440 

### * 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min 0 5 10 15 20 25 30Y(X100000) C511K02023 [ MS QQQ Chro ] :m /z 417.0 > 371.94.441 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 5 10 15 20 25 30Y(X100000) C511K02023 [ MS QQQ Chro ] :m /z 417.0 > 371.94.441



### 3 Ammonium Per

f luorooctanoate (APFO) (M)

2.9 3.9 4.9

Min 46 54 62 70 7 8 8 6 94 102Y(X1000) C511K02023 [ MS QQQ Chro ] :m /z 413.0 > 36 8 .94.442 

### 3 Ammonium Per f luorooctanoate (APFO) (M)

2.9 3.9 4.9

Min 41 43 45 47 49 51 53Y(X1000) C511K02023 [ MS QQQ Chro ] :m /z 413.0 > 169.04.442 

### 1 Per f luorooctanoic acid (M)

2.9 3.9 4.9

Min 46 54 62 70 7 8 8 6 94 102Y(X1000) C511K02023 [ MS QQQ Chro ] :m /z 413.0 > 36 8 .94.442



### 1 Per f luorooctanoic acid (M)

2.9 3.9 4.9

Min 41 43 45 47 49 51 53Y(X1000) C511K02023 [ MS QQQ Chro ] :m /z 413.0 > 169.04.442 

### $ 6 13C 8 PFOS

3 4 5

Min 4 16 2 8 40 52 64 76 88Y(X10000) C511K02023 [ MS QQQ Chro ] :m /z 506.9 > 8 0.04.588 

### 2 Per

f luorooctanoic Sul f

onate

3 4 5

Min 41 44 47 50 53 56 59 62Y(X1000) C511K02023 [ MS QQQ Chro ] :m /z 49 8 .9 > 79.94.580



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 41 43 45 47 49 51 53 55Y(X1000) C511K02023 [ MS QQQ Chro ] :m /z 49 8 .9 > 9 8 .94.580 

### * 5 13C4 PFOS (IS)

3 4 5

Min 4 16 2 8 40 52 64 76 88Y(X10000) C511K02023 [ MS QQQ Chro ] :m /z 502.9 > 8 0.04.588 

### $ 8 13C4 PFOS

3 4 5

Min 4 16 2 8 40 52 64 76 88Y(X10000) C511K02023 [ MS QQQ Chro ] :m /z 502.9 > 8 0.04.588



### 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 B atch ID: 9 45 89 Lims Sample ID: 17 Operator ID: T W/J B Injection V ol: 20.00 ul 3 Ammonium Per

f luorooctanoate (

APFO ), Signal: 1 , m/ z : 413.0 > 36 8

. 9 Ty pe: q uant , R T : 4.44 Processing Integration Results R T : 4.44 Response: 164511 Amount: 0.050333

4.15 Min 50 54 5 8 62 66 70 74 7 8 8 2 8 6 9 0 9 4 98 102 106Y(X1000) C511K02023 [ MS QQQ Chro ] :m/ z 413.0 > 36 8

. 94.442



### Manual Integration Results R T : 4.44 Response: 20345 8 Amount: 0.0

8 3 8 3 8

4.16 Min

50 54 5 8 62 66 70 74 7 8 8 2 8 6 9 0 9 4 98 102 106Y(X1000) C511K02023 [ MS QQQ Chro ] :m/ z 413.0 > 36 8

. 94.442



### Revie w er: w illiamst , 03-Nov-2011 14:44:0

9 Audit Action: Manuall y

Integrated Audit Reason: B aseline

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 B atch ID: 9 45 89 Lims Sample ID: 17 Operator ID: T W/J B Injection V ol: 20.00 ul 3 Ammonium Per

f luorooctanoate (

APFO ), Signal: 2 , m/ z : 413.0 > 16 9 .0 Ty pe: q uali f ier , R T : 4.44 Processing Integration Results R T : 4.44 Response: 1725 8 Amount: 0

4.15 Min 41 42 43 44 45 46 47 4 8 4 9 50 51 52 53 54Y(X1000) C511K02023 [ MS QQQ Chro ] :m/ z 413.0 > 16 9 .04.442



### Manual Integration Results R T : 4.44 Response: 47473 Amount: 0

4.15 Min 41 42 43 44 45 46 47 4 8 4 9 50 51 52 53 54Y(X1000) C511K02023 [ MS QQQ Chro ] :m/ z 413.0 > 16 9 .04.442



### Revie w er: w illiamst , 03-Nov-2011 14:44:0

9 Audit Action: Manuall y

Integrated Audit Reason: B aseline

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 B atch ID: 9 45 89 Lims Sample ID: 17 Operator ID: T W/J B Injection V ol: 20.00 ul 1 Per f luorooctanoic acid , Signal: 1 , m/ z : 413.0 > 36 8

. 9 Ty pe: q uant , R T : 4.44 Processing Integration Results R T : 4.44 Response: 164511 Amount: 0.047 8 51

2. 8 3. 8 4. 8 Min 45 4 9 53 57 61 65 6 9 73 77 8 1 8 5 89 9 3 9 7 101 105Y(X1000) C511K02023 [ MS QQQ Chro ] :m/ z 413.0 > 36 8

. 94.442



### Manual Integration Results R T : 4.44 Response: 215126 Amount: 0.0

89 6 9 5

2. 8 3. 8 4. 8 Min 45 4 9 53 57 61 65 6 9 73 77 8 1 8 5 89 9 3 9 7 101 105Y(X1000) C511K02023 [ MS QQQ Chro ] :m/ z 413.0 > 36 8

. 94.442



### Revie w er: w illiamst , 03-Nov-2011 14:44:0

9 Audit Action: Manuall y

Integrated Audit Reason: B aseline

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 B atch ID: 9 45 89 Lims Sample ID: 17 Operator ID: T W/J B Injection V ol: 20.00 ul 1 Per f luorooctanoic acid , Signal: 2 , m/ z : 413.0 > 16 9 .0 Ty pe: q uali f ier , R T : 4.44 Processing Integration Results R T : 4.44 Response: 1725 8 Amount: 0

4.16 Min 41 42 43 44 45 46 47 4 8 4 9 50 51 52 53 54Y(X1000) C511K02023 [ MS QQQ Chro ] :m/ z 413.0 > 16 9 .04.442



### Manual Integration Results R T : 4.44 Response: 43544 Amount: 0

4.16 Min 41 42 43 44 45 46 47 4 8 4 9 50 51 52 53 54Y(X1000) C511K02023 [ MS QQQ Chro ] :m/ z 413.0 > 16 9 .04.442



### Revie w er: w illiamst , 03-Nov-2011 14:44:0

9 Audit Action: Manuall y

Integrated Audit Reason: B aseline

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

7699 Calibration Start Date: Calibration End Date: 11/02/2011 13:49 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 AVG RT RT WINDOW 13C4 PFOA 4.434

3.934 - 4.934 4.450 4.441 4.441 4.432 4.432 4.432 4.432 4.423 +++++ 13C4 PFOS 4.586

4.086 - 5.086 4.606 4.597 4.597 4.588 4.588 4.579 4.579 4.571 +++++



### 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

7699 Calibration Start Date: Calibration End Date: 11/02/2011 13:49 N 11/02/2011 14:51 Gemini-NX ID: EXTERNAL STANDARD CURVE EVALUTION

Calibration Files: LEVEL: LAB SAMPLE ID: LAB FILE ID: 1 Level STD0002 280-94589/2 PC511K02008.d 2 Level STD0005 280-94589/3 PC511K02009.d 3 Level STD0010 280-94589/4 PC511K02010.d 4 Level STD0020 280-94589/5 PC511K02011.d 5 Level STD0050 280-94589/6 PC511K02012.d 6 Level STD0100 280-94589/7 PC511K02013.d 7 Level STD0200 280-94589/8 PC511K02014.d 8 Level STD0500 280-94589/9 PC511K02015.d 9 Level STD1250 280-94589/10 PC511K02016.d

MIN R^2

OR COD # R^2 OR COD MAX %RSD # %RSD # COEFFICIENT
M2 M1 B CURVE TYPE LVL 4 LVL 3 LVL 2 LVL 1 CF ANALYTE MIN CF

LVL 5 LVL 6 LVL 7 LVL 8 LVL 9 13C4 PFOA Ave 9.9 30.0 2296718 2223037 2279793 2326392 2241184 2181743 1978105 1700225 +++++ 2153399.50

13C4 PFOS Ave 7.7 30.0 555482 565703 581890 580327 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

7699 Calibration Start Date: Calibration End Date: 11/02/2011 13:49 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 +++++ 0.9900 0.0934 1.0245
Perfluorooctanoic acid (PFOA) 1.4387 1.3776 1.1173 1.1106 1.0850 Lin1 0.9990 1.0647 1.1165 1.0520 +++++ 0.9900 0.0940 1.0661
Perfluorooctanoic Sulfonate 1.7363 1.5399 1.3577 1.3919 1.3879 Lin1 1.0000 1.3656 1.4172 1.3545 +++++ 0.9900 0.0650 1.3684
13C8 PFOA 1.0343 0.9261 0.8995 0.8451 0.8652 Lin1 0.9980 0.8435 0.8646 0.7883 +++++ 0.9900 0.0622 0.8143
13C8 PFOS 1.0470 0.9368 0.8850 0.9360 0.9054 Lin1 0.9980 0.8939 0.9221 0.8456 +++++ 0.9900 0.0435 0.8710



### 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

7699 Calibration Start Date: Calibration End Date: 11/02/2011 13:49 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 RESPONSE ANALYTE CONCENTRATION (UG/L)
LVL 1 LVL 1 LVL 2 LVL 2 LVL 3 LVL 3 LVL 4 LVL 4 LVL 5 LVL 5 LVL 6 LVL 6 LVL 7 LVL 7 LVL 8 LVL 8 LVL 9 LVL 9 Ave 13C4 PFOA 22967180 21817429 22230365 19781051 22797925 17002248 23263924 +++++ 22411838 10.0 10.0 10.0 10.0 10.0 10.0 10.0 +++++ 10.0

Ave 13C4 PFOS 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

7699 Calibration Start Date: Calibration End Date: 11/02/2011 13:49 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) Lin1 OA 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) Lin1 OA 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 Lin1 PFOS 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 Lin1 OA 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 Lin1 PFOS 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 V ol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 94589 Lims Sample ID: 2 Sublist: chrom-8321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:28:56 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC285 First Level Revie w

er: bonnettj Date: 03-Nov-2011 10:20:27 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags
1 Per f luorooctanoic 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 Per

f luorooctanoate (

APF O) 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 PF O A 421.0 > 375.9 4.449 4.433 0.016 1.000 475083 0.1776 $ 7 13C4 PF O A 417.0 > 371.9 4.450 4.434 0.016 22967180 10.7

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.450 4.434 0.016 22967180 10.0 $ 6 13C8 PF O S 506.9 > 80.0 4.605 4.586 0.019 1.000 111195 0.1799 2 Per f luorooctanoic Sul f

onate 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 PF O S ( IS ) 502.9 > 80.0 4.606 4.586 0.020 5310411 9.56 $ 8 13C4 PF O S 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 Revie w 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 V ol: 20.00 ul 1 Per f luorooctanoic acid ( M

)

2.9 3.9 4.9

Min 4 7 10 13 16 19 22Y(X10000) C511K02008 [ MS QQQ Chro ] :m /z 413.0 > 368.94.451 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 41 47 53 59 65 71 77 83Y(X1000) C511K02008 [ MS QQQ Chro ] :m /z 413.0 > 169.04.451 

### 3 Ammonium Per f luorooctanoate (

APFO ) ( M

)

2.9 3.9 4.9

Min 4 7 10 13 16 19 22Y(X10000) C511K02008 [ MS QQQ Chro ] :m /z 413.0 > 368.94.451



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 41 47 53 59 65 71 77 83Y(X1000) C511K02008 [ MS QQQ Chro ] :m /z 413.0 > 169.04.451 

### $ 9 13C8 PFOA

2.9 3.9 4.9

Min 4 6 8 10 12 14 16Y(X10000) C511K02008 [ MS QQQ Chro ] :m /z 421.0 > 375.94.449 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02008 [ MS QQQ Chro ] :m /z 417.0 > 371.94.450



### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02008 [ MS QQQ Chro ] :m /z 417.0 > 371.94.450 

### $ 6 13C8 PFOS

3 4 5

Min 41 46 51 56 61 66 71 76Y(X1000) C511K02008 [ MS QQQ Chro ] :m /z 506.9 > 80.04.605 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 41 48 55 62 69 76 83 90Y(X1000) C511K02008 [ MS QQQ Chro ] :m /z 498.9 > 79.94.607



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 41 45 49 53 57 61 65 69Y(X1000) C511K02008 [ MS QQQ Chro ] :m /z 498.9 > 98.94.607 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02008 [ MS QQQ Chro ] :m /z 502.9 > 80.04.606 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02008 [ MS QQQ Chro ] :m /z 502.9 > 80.04.606



### 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 - PF O A DuPont Client ID: Instrument ID: LC_LCMS5 Lims B atch ID: 94589 Lims Sample ID: 2 O perator ID: TW /J B Injection V ol: 20.00 ul 1 Per f luorooctanoic acid , Signal: 1 , m/ z : 413.0 > 368.9 Ty pe: q uant , R T : 4.45 Processing Integration Results R T : 4.45 Response: 578269 Amount: 0.168099

4.1 Min 4 6 8 10 12 14 16 18 20 22Y(X10000) C511K02008 [ MS QQQ Chro ] :m/ z 413.0 > 368.94.451



### Manual Integration Results R T : 4.45 Response: 660880 Amount: 0.181753

4.08 Min 4 6 8 10 12 14 16 18 20 22Y(X10000) C511K02008 [ MS QQQ Chro ] :m/ z 413.0 > 368.94.451



### Revie w er: bonnettj , 03-Nov-2011 10:25:28 Audit Action: Manuall y

Integrated Audit Reason: B aseline

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 - PF O A DuPont Client ID: Instrument ID: LC_LCMS5 Lims B atch ID: 94589 Lims Sample ID: 2 O perator ID: TW /J B Injection V ol: 20.00 ul 3 Ammonium Per

f luorooctanoate (

APF O), Signal: 1 , m/ z : 413.0 > 368.9 Ty pe: q uant , R T : 4.45 Processing Integration Results R T : 4.45 Response: 578269 Amount: 0.174924

4.1 Min 4 6 8 10 12 14 16 18 20 22Y(X10000) C511K02008 [ MS QQQ Chro ] :m/ z 413.0 > 368.94.451



### Manual Integration Results R T : 4.45 Response: 658763 Amount: 0.188767

4.09 Min 4 6 8 10 12 14 16 18 20 22Y(X10000) C511K02008 [ MS QQQ Chro ] :m/ z 413.0 > 368.94.451



### Revie w er: bonnettj , 03-Nov-2011 10:25:28 Audit Action: Manuall y

Integrated Audit Reason: B aseline

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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 V ol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 94589 Lims Sample ID: 3 Sublist: chrom-8321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:28:57 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC285 First Level Revie w

er: bonnettj Date: 03-Nov-2011 10:23:08 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags
1 Per f luorooctanoic 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 Per

f luorooctanoate (

APF O) 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 PF O A 421.0 > 375.9 4.440 4.433 0.007 1.000 1029368 0.4922 $ 7 13C4 PF O A 417.0 > 371.9 4.441 4.434 0.007 22230365 10.3

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.441 4.434 0.007 22230365 10.0 $ 6 13C8 PF O S 506.9 > 80.0 4.596 4.586 0.010 1.000 253319 0.4642 2 Per f luorooctanoic Sul f

onate 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 PF O S ( IS ) 502.9 > 80.0 4.597 4.586 0.011 5408117 9.56 $ 8 13C4 PF O S 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 V ol: 20.00 ul 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 9 14 19 24 29 34 39Y(X10000) C511K02009 [ MS QQQ Chro ] :m /z 413.0 > 368.94.442 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 41 50 59 68 77 86 95 104Y(X1000) C511K02009 [ MS QQQ Chro ] :m /z 413.0 > 169.04.442 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 4 9 14 19 24 29 34 39Y(X10000) C511K02009 [ MS QQQ Chro ] :m /z 413.0 > 368.94.442



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 41 50 59 68 77 86 95 104Y(X1000) C511K02009 [ MS QQQ Chro ] :m /z 413.0 > 169.04.442 

### $ 9 13C8 PFOA

2.9 3.9 4.9

Min 4 8 12 16 20 24 28Y(X10000) C511K02009 [ MS QQQ Chro ] :m /z 421.0 > 375.94.440 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02009 [ MS QQQ Chro ] :m /z 417.0 > 371.94.441



### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02009 [ MS QQQ Chro ] :m /z 417.0 > 371.94.441 

### $ 6 13C8 PFOS

3 4 5

Min 41 51 61 71 81 91 101 111Y(X1000) C511K02009 [ MS QQQ Chro ] :m /z 506.9 > 80.04.596 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 6 8 10 12 14 16Y(X10000) C511K02009 [ MS QQQ Chro ] :m /z 498.9 > 79.94.598



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 41 49 57 65 73 81 89 97Y(X1000) C511K02009 [ MS QQQ Chro ] :m /z 498.9 > 98.94.598 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02009 [ MS QQQ Chro ] :m /z 502.9 > 80.04.597 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02009 [ MS QQQ Chro ] :m /z 502.9 > 80.04.597



### 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.: O perator: T W/ J B Instrument ID: LC_LCMS5 V ol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 9 458 9 Lims Sample ID: 4 Sublist: chrom-8321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:28:58 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC285 First Level Revie w

er: bonnettj Date: 03-Nov-2011 10:23:13 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C8 PF O A 421.0 > 375. 9 4.440 4.433 0.007 1.000 20505 9 7 1.03

* 4 13C4 PF O A ( IS ) 417.0 > 371. 9 4.441 4.434 0.007 227 9 7 9 25 10.0 $ 7 13C4 PF O A 417.0 > 371. 9 4.441 4.434 0.007 227 9 7 9 25 10.6 3 Ammonium Perfluorooctanoate ( APF O) 413.0 > 368. 9 4.442 4.446 -0.004 1.000 2547268 1.00 0.70- 1.30 1.00 413.0 > 16 9 .0 4.442 4.446 -0.004 1.000 510741 3.72- 6. 9 2 4. 99 1 Perfluorooctanoic acid 413.0 > 368. 9 4.442 4.446 -0.004 1.000 2547268 0. 9 5 99 0.70- 1.30 1.00 413.0 > 16 9 .0 4.442 4.446 -0.004 1.000 510741 3.72- 6. 9 2 4. 99 $ 6 13C8 PF O S 506. 9 > 80.0 4.5 9 6 4.586 0.010 1.000 4 9 233 9 0. 9 214 2 Perfluorooctanoic Sulfonate 4 9 8. 9 > 7 9

. 9 4.5 9 8 4.586 0.012 1.000 755252 0. 9 010 0.70- 1.30 1.00 4 9 8. 9 > 9 8. 9 4.5 9 8 4.586 0.012 1.000 422285 1.30- 2.42 1.7 9

* 5 13C4 PF O S ( IS ) 502. 9 > 80.0 4.5 9 7 4.586 0.011 5562864 9 .56 $ 8 13C4 PF O S 502. 9 > 80.0 4.5 9 7 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 4 11 18 25 32 39 46 53Y(X10000) C511K02010 [ MS QQQ Chro ] :m /z 421.0 > 375.94.440 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02010 [ MS QQQ Chro ] :m /z 417.0 > 371.94.441 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02010 [ MS QQQ Chro ] :m /z 417.0 > 371.94.441



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 4 13 22 31 40 49 58 67Y(X10000) C511K02010 [ MS QQQ Chro ] :m /z 413.0 > 368.94.442 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 4 6 8 10 12 14 16 18Y(X10000) C511K02010 [ MS QQQ Chro ] :m /z 413.0 > 169.04.442 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 13 22 31 40 49 58 67Y(X10000) C511K02010 [ MS QQQ Chro ] :m /z 413.0 > 368.94.442



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 6 8 10 12 14 16 18Y(X10000) C511K02010 [ MS QQQ Chro ] :m /z 413.0 > 169.04.442 

### $ 6 13C8 PFOS

3 4 5

Min 4 6 8 10 12 14 16 18Y(X10000) C511K02010 [ MS QQQ Chro ] :m /z 506.9 > 80.04.596 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 7 10 13 16 19 22 25Y(X10000) C511K02010 [ MS QQQ Chro ] :m /z 498.9 > 79.94.598



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 6 8 10 12 14 16Y(X10000) C511K02010 [ MS QQQ Chro ] :m /z 498.9 > 98.94.598 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 3 6 9 12 15Y(X100000) C511K02010 [ MS QQQ Chro ] :m /z 502.9 > 80.04.597 

### $ 8 13C4 PFOS

3 4 5

Min 0 3 6 9 12 15Y(X100000) C511K02010 [ MS QQQ Chro ] :m /z 502.9 > 80.04.597



### 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 V ol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 94589 Lims Sample ID: 5 Sublist: chrom-8321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:28:59 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC285 First Level Revie w

er: bonnettj Date: 03-Nov-2011 10:23:19 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C8 PF O A 421.0 > 375.9 4.431 4.433 -0.002 1.000 3932174 2.00

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.432 4.434 -0.002 23263924 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.432 4.434 -0.002 23263924 10.8 3 Ammonium Per

f luorooctanoate (

APF O) 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 Per f luorooctanoic 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 PF O S 506.9 > 80.0 4.588 4.586 0.002 1.000 1038604 2.00 2 Per f luorooctanoic Sul f

onate 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 PF O S ( IS ) 502.9 > 80.0 4.588 4.586 0.002 5547924 9.56 $ 8 13C4 PF O S 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 2 4 6 8 10Y(X100000) C511K02011 [ MS QQQ Chro ] :m /z 421.0 > 375.94.431 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02011 [ MS QQQ Chro ] :m /z 417.0 > 371.94.432 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02011 [ MS QQQ Chro ] :m /z 417.0 > 371.94.432



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02011 [ MS QQQ Chro ] :m /z 413.0 > 368.94.433 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 4 8 12 16 20 24 28Y(X10000) C511K02011 [ MS QQQ Chro ] :m /z 413.0 > 169.04.433 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02011 [ MS QQQ Chro ] :m /z 413.0 > 368.94.433



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 8 12 16 20 24 28Y(X10000) C511K02011 [ MS QQQ Chro ] :m /z 413.0 > 169.04.433 

### $ 6 13C8 PFOS

3 4 5

Min 4 8 12 16 20 24 28 32Y(X10000) C511K02011 [ MS QQQ Chro ] :m /z 506.9 > 80.04.588 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 10 16 22 28 34 40 46Y(X10000) C511K02011 [ MS QQQ Chro ] :m /z 498.9 > 79.94.589



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 8 12 16 20 24 28Y(X10000) C511K02011 [ MS QQQ Chro ] :m /z 498.9 > 98.94.589 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02011 [ MS QQQ Chro ] :m /z 502.9 > 80.04.588 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02011 [ MS QQQ Chro ] :m /z 502.9 > 80.04.588



### 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.: O perator: T W/ J B Instrument ID: LC_LCMS5 V ol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 945 8 9 Lims Sample ID: 6 Sublist: chrom- 8 321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\ 8 321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:2 8 :59 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC2 8 5 First Level Revie w

er: bonnettj Date: 03-Nov-2011 10:23:24 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C 8

PF O A 421.0 > 375.9 4.431 4.433 -0.002 1.000 969573 8 5.24

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.432 4.434 -0.002 22411 8 3 8 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.432 4.434 -0.002 22411 8 3 8 10.4 3 Ammonium Perfluorooctanoate ( APF O) 413.0 > 36 8 .9 4.433 4.442 -0.009 1.000 1215 8 03 8 5.20 0.70- 1.30 1.00 413.0 > 169.0 4.433 4.442 -0.009 1.000 22 8 5249 3.72- 6.92 5.32 1 Perfluorooctanoic acid 413.0 > 36 8 .9 4.433 4.442 -0.009 1.000 1215 8 03 8 5.00 0.70- 1.30 1.00 413.0 > 169.0 4.433 4.442 -0.009 1.000 22 8 5249 3.72- 6.92 5.32 $ 6 13C 8

PF O S 506.9 > 8

0.0 4.5 88 4.5 8 6 0.002 1.000 2460152 4.92 2 Perfluorooctanoic Sulfonate 49 8 .9 > 79.9 4.5 8 0 4.5 8 6 -0.006 0.99 8 37713 8 9 4. 8 0 0.70- 1.30 1.00 49 8 .9 > 9 8 .9 4.5 8 0 4.5 8 6 -0.006 0.99 8 2025922 1.30- 2.42 1. 8 6

* 5 13C4 PF O S ( IS ) 502.9 > 8

0.0 4.5 88 4.5 8 6 0.002 5434672 9.56 $ 8 13C4 PF O S 502.9 > 8

0.0 4.5 88 4.5 8 6 0.002 5434672 9. 8 7

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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 4 8 12 16 20 24Y(X100000) C511K02012 [ MS QQQ Chro ] :m /z 421.0 > 375.94.431 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02012 [ MS QQQ Chro ] :m /z 417.0 > 371.94.432 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02012 [ MS QQQ Chro ] :m /z 417.0 > 371.94.432



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 5 10 15 20 25 30Y(X100000) C511K02012 [ MS QQQ Chro ] :m /z 413.0 > 368.94.433 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 4 12 20 28 36 44 52 60Y(X10000) C511K02012 [ MS QQQ Chro ] :m /z 413.0 > 169.04.433 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 5 10 15 20 25 30Y(X100000) C511K02012 [ MS QQQ Chro ] :m /z 413.0 > 368.94.433



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 12 20 28 36 44 52 60Y(X10000) C511K02012 [ MS QQQ Chro ] :m /z 413.0 > 169.04.433 

### $ 6 13C8 PFOS

3 4 5

Min 4 13 22 31 40 49 58 67Y(X10000) C511K02012 [ MS QQQ Chro ] :m /z 506.9 > 80.04.588 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 2 4 6 8 10 12Y(X100000) C511K02012 [ MS QQQ Chro ] :m /z 498.9 > 79.94.580



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 12 20 28 36 44 52 60Y(X10000) C511K02012 [ MS QQQ Chro ] :m /z 498.9 > 98.94.580 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02012 [ MS QQQ Chro ] :m /z 502.9 > 80.04.588 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02012 [ MS QQQ Chro ] :m /z 502.9 > 80.04.588



### 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 V ol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 94589 Lims Sample ID: 7 Sublist: chrom-8321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:00 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC285 First Level Revie w

er: bonnettj Date: 03-Nov-2011 10:22:29 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C8 PF O A 421.0 > 375.9 4.431 4.433 -0.002 1.000 18402008 10.3

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.432 4.434 -0.002 21817429 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.432 4.434 -0.002 21817429 10.1 3 Ammonium Per

f luorooctanoate (

APF O) 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 Per f luorooctanoic 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 PF O S 506.9 > 80.0 4.579 4.586 -0.007 1.000 4881581 9.76 2 Per f luorooctanoic Sul f

onate 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 PF O S ( IS ) 502.9 > 80.0 4.579 4.586 -0.007 5460786 9.56 $ 8 13C4 PF O S 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 6 12 18 24 30 36 42 48Y(X100000) C511K02013 [ MS QQQ Chro ] :m /z 421.0 > 375.94.431 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02013 [ MS QQQ Chro ] :m /z 417.0 > 371.94.432 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02013 [ MS QQQ Chro ] :m /z 417.0 > 371.94.432



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02013 [ MS QQQ Chro ] :m /z 413.0 > 368.94.433 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 2 4 6 8 10 12Y(X100000) C511K02013 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02013 [ MS QQQ Chro ] :m /z 413.0 > 368.94.433



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 2 4 6 8 10 12Y(X100000) C511K02013 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### $ 6 13C8 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02013 [ MS QQQ Chro ] :m /z 506.9 > 80.04.579 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 3 6 9 12 15 18Y(X100000) C511K02013 [ MS QQQ Chro ] :m /z 498.9 > 79.94.580



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 2 4 6 8 10 12Y(X100000) C511K02013 [ MS QQQ Chro ] :m /z 498.9 > 98.94.580 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02013 [ MS QQQ Chro ] :m /z 502.9 > 80.04.579 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02013 [ MS QQQ Chro ] :m /z 502.9 > 80.04.579



### 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.: O perator: T W/ J B Instrument ID: LC_LCMS5 V ol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 945 8 9 Lims Sample ID: 8 Sublist: chrom- 8 321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\ 8 321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:01 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC2 8 5 First Level Revie w

er: bonnettj Date: 03-Nov-2011 10:21:43 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C 8

PF O A 421.0 > 375.9 4.431 4.433 -0.002 1.000 34203552 21.2

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.432 4.434 -0.002 197 8 1051 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.432 4.434 -0.002 197 8 1051 9.19 3 Ammonium Perfluorooctanoate ( APF O) 413.0 > 36 8 .9 4.433 4.439 -0.006 1.000 44171 8 76 21.7 0.70- 1.30 1.00 413.0 > 169.0 4.433 4.439 -0.006 1.000 8 332659 3.72- 6.92 5.30 1 Perfluorooctanoic acid 413.0 > 36 8 .9 4.433 4.439 -0.006 1.000 44171 8 76 20.9 0.70- 1.30 1.00 413.0 > 169.0 4.433 4.439 -0.006 1.000 8 332659 3.72- 6.92 5.30 $ 6 13C 8

PF O S 506.9 > 8

0.0 4.579 4.5 8 6 -0.007 1.000 9255367 20.2 2 Perfluorooctanoic Sulfonate 49 8 .9 > 79.9 4.5 8 0 4.5 8 6 -0.006 1.000 14223555 19. 8 0.70- 1.30 1.00 49 8 .9 > 9 8 .9 4.5 8 0 4.5 8 6 -0.006 1.000 7690600 1.30- 2.42 1. 8 5

* 5 13C4 PF O S ( IS ) 502.9 > 8

0.0 4.579 4.5 8 6 -0.007 501 8 364 9.56 $ 8 13C4 PF O S 502.9 > 8

0.0 4.579 4.5 8 6 -0.007 501 8 364 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 11 22 33 44 55 66 77 88Y(X100000) C511K02014 [ MS QQQ Chro ] :m /z 421.0 > 375.94.431 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 7 14 21 28 35 42 49Y(X100000) C511K02014 [ MS QQQ Chro ] :m /z 417.0 > 371.94.432 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 7 14 21 28 35 42 49Y(X100000) C511K02014 [ MS QQQ Chro ] :m /z 417.0 > 371.94.432



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 2 4 6 8 10 12Y(X1000000) C511K02014 [ MS QQQ Chro ] :m /z 413.0 > 368.94.433 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 3 6 9 12 15 18 21Y(X100000) C511K02014 [ MS QQQ Chro ] :m /z 413.0 > 169.04.433 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 2 4 6 8 10 12Y(X1000000) C511K02014 [ MS QQQ Chro ] :m /z 413.0 > 368.94.433



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 3 6 9 12 15 18 21Y(X100000) C511K02014 [ MS QQQ Chro ] :m /z 413.0 > 169.04.433 

### $ 6 13C8 PFOS

3 4 5

Min 0 4 8 12 16 20 24Y(X100000) C511K02014 [ MS QQQ Chro ] :m /z 506.9 > 80.04.579 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 5 10 15 20 25 30 35Y(X100000) C511K02014 [ MS QQQ Chro ] :m /z 498.9 > 79.94.580



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 3 6 9 12 15 18 21Y(X100000) C511K02014 [ MS QQQ Chro ] :m /z 498.9 > 98.94.580 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02014 [ MS QQQ Chro ] :m /z 502.9 > 80.04.579 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02014 [ MS QQQ Chro ] :m /z 502.9 > 80.04.579



### 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 V ol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 94589 Lims Sample ID: 9 Sublist: chrom-8321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:02 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC285 First Level Revie w

er: bonnettj Date: 03-Nov-2011 10:21:20 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C8 PF O A 421.0 > 375.9 4.422 4.433 -0.011 1.000 67015770 48.3

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.423 4.434 -0.011 17002248 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.423 4.434 -0.011 17002248 7.90 3 Ammonium Per

f luorooctanoate (

APF O) 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 Per f luorooctanoic 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 PF O S 506.9 > 80.0 4.570 4.586 -0.016 1.000 18393914 46.4 2 Per f luorooctanoic Sul f

onate 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 PF O S ( IS ) 502.9 > 80.0 4.571 4.586 -0.015 4350363 9.56 $ 8 13C4 PF O S 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 3 6 9 12 15Y(X1000000) C511K02015 [ MS QQQ Chro ] :m /z 421.0 > 375.94.422 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 6 12 18 24 30 36 42Y(X100000) C511K02015 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 6 12 18 24 30 36 42Y(X100000) C511K02015 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 3 6 9 12 15 18 21Y(X1000000) C511K02015 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 6 12 18 24 30 36 42Y(X100000) C511K02015 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 3 6 9 12 15 18 21Y(X1000000) C511K02015 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 6 12 18 24 30 36 42Y(X100000) C511K02015 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### $ 6 13C8 PFOS

3 4 5

Min 0 6 12 18 24 30 36 42Y(X100000) C511K02015 [ MS QQQ Chro ] :m /z 506.9 > 80.04.570 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 9 18 27 36 45 54 63 72Y(X100000) C511K02015 [ MS QQQ Chro ] :m /z 498.9 > 79.94.571



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 5 10 15 20 25 30 35 40Y(X100000) C511K02015 [ MS QQQ Chro ] :m /z 498.9 > 98.94.571 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10Y(X100000) C511K02015 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10Y(X100000) C511K02015 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571



### 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.: O perator: T W/ J B Instrument ID: LC_LCMS5 V ol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 945 8 9 Lims Sample ID: 10 Sublist: chrom- 8 321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\ 8 321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC2 8 5 First Level Revie w

er: bonnettj Date: 03-Nov-2011 10:23:45 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C 8

PF O A 421.0 > 375.9 4.422 4.433 -0.011 1.000 123902997 107.1

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.423 4.434 -0.011 14194691 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.423 4.434 -0.011 14194691 6.59 3 Ammonium Perfluorooctanoate ( APF O) 413.0 > 36 8 .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 > 36 8 .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 13C 8

PF O S 506.9 > 8

0.0 4.570 4.5 8 6 -0.016 1.000 32699964 104.5 2 Perfluorooctanoic Sulfonate 49 8 .9 > 79.9 4.571 4.5 8 6 -0.015 1.000 51 8 04971 105.3 0.70- 1.30 1.00 49 8 .9 > 9 8 .9 4.571 4.5 8 6 -0.015 1.000 2 8 2 8 204 8 1.30- 2.42 1. 8 3

* 5 13C4 PF O S ( IS ) 502.9 > 8

0.0 4.571 4.5 8 6 -0.015 343410 8 9.56 $ 8 13C4 PF O S 502.9 > 8

0.0 4.571 4.5 8 6 -0.015 343410 8 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 4 8 12 16 20 24 28Y(X1000000) C511K02016 [ MS QQQ Chro ] :m /z 421.0 > 375.94.422 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 4 8 12 16 20 24 28 32Y(X100000) C511K02016 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 4 8 12 16 20 24 28 32Y(X100000) C511K02016 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 5 10 15 20 25 30 35Y(X1000000) C511K02016 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 9 18 27 36 45 54 63Y(X100000) C511K02016 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 5 10 15 20 25 30 35Y(X1000000) C511K02016 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 9 18 27 36 45 54 63Y(X100000) C511K02016 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### $ 6 13C8 PFOS

3 4 5

Min 0 9 18 27 36 45 54 63 72Y(X100000) C511K02016 [ MS QQQ Chro ] :m /z 506.9 > 80.04.570 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 2 4 6 8 10 12Y(X1000000) C511K02016 [ MS QQQ Chro ] :m /z 498.9 > 79.94.571



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02016 [ MS QQQ Chro ] :m /z 498.9 > 98.94.571 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 4 14 24 34 44 54 64 74Y(X10000) C511K02016 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571 

### $ 8 13C4 PFOS

3 4 5

Min 4 14 24 34 44 54 64 74Y(X10000) C511K02016 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571



### 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:

Calib End Date: GC Column: ID: 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) 0.9264 1.79 2.08 -14.0 20.0 Lin1
Perfluorooctanoic acid (PFOA) 0.9640 1.72 2.00 -14.0 20.0 Lin1
Perfluorooctanoic Sulfonate 1.284 1.85 2.02 -8.4 20.0 Lin1 13C8 PFOA 0.8633 2.04 2.00 2.0 20.0 Lin1 13C4 PFOA 2253292 2153400 10.5 10.0 4.6 Ave 13C8 PFOS 0.8917 1.91 1.91 -0.1 20.0 Lin1 13C4 PFOS 570417 550386 9.91 9.56 3.6 Ave



### 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 Vol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 94589 Lims Sample ID: 12 Sublist: Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC285 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C8 PF O A 421.0 > 375.9 4.422 4.433 -0.011 1.000 3890502 2.04

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.423 4.434 -0.011 22532916 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.423 4.434 -0.011 22532916 10.5 3 Ammonium Per

f luorooctanoate (

APF O) 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 Per f luorooctanoic 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 PF O S 506.9 > 80.0 4.570 4.586 -0.016 1.000 972526 1.91 2 Per f luorooctanoic Sul f

onate 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 PF O S ( IS ) 502.9 > 80.0 4.571 4.586 -0.015 5453191 9.56 $ 8 13C4 PF O S 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 2 4 6 8 10Y(X100000) C511K02018 [ MS QQQ Chro ] :m /z 421.0 > 375.94.422 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02018 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02018 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 2 4 6 8 10 12Y(X100000) C511K02018 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 4 7 10 13 16 19 22 25Y(X10000) C511K02018 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 2 4 6 8 10 12Y(X100000) C511K02018 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 7 10 13 16 19 22 25Y(X10000) C511K02018 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### $ 6 13C8 PFOS

3 4 5

Min 4 8 12 16 20 24 28Y(X10000) C511K02018 [ MS QQQ Chro ] :m /z 506.9 > 80.04.570 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 8 12 16 20 24 28 32Y(X10000) C511K02018 [ MS QQQ Chro ] :m /z 498.9 > 79.94.563



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 6 8 10 12 14 16 18Y(X10000) C511K02018 [ MS QQQ Chro ] :m /z 498.9 > 98.94.571 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02018 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02018 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571



### 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:

Calib End Date: GC Column: ID: 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) 1.051 5.25 5.20 0.9 20.0 Lin1
Perfluorooctanoic acid (PFOA) 1.094 5.04 5.00 0.8 20.0 Lin1
Perfluorooctanoic Sulfonate 1.346 4.65 4.78 -2.7 20.0 Lin1 13C8 PFOA 0.8369 5.06 5.00 1.2 20.0 Lin1 13C4 PFOA 2121411 2153400 9.85 10.0 -1.5 Ave 13C8 PFOS 0.9000 4.89 4.78 2.3 20.0 Lin1 13C4 PFOS 528000 550386 9.17 9.56 -4.1 Ave



### 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 Vol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 945 8 9 Lims Sample ID: 20 Sublist: chrom- 8 321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\ 8 321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:12 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC2 8 5 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C 8

PF O A 421.0 > 375.9 4.431 4.433 -0.002 1.000 88 77243 5.06

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.432 4.434 -0.002 21214105 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.432 4.434 -0.002 21214105 9. 8 5 3 Ammonium Per

f luorooctanoate (

APF O) 413.0 > 36 8 .9 4.424 4.435 -0.011 0.99 8 116056 8 9 5.25 0.70- 1.30 1.00 413.0 > 169.0 4.424 4.435 -0.011 0.99 8 21 8 10 8 1 3.72- 6.92 5.32 1 Per f luorooctanoic acid 413.0 > 36 8 .9 4.424 4.435 -0.011 0.99 8 116056 8 9 5.04 0.70- 1.30 1.00 413.0 > 169.0 4.424 4.435 -0.011 0.99 8 21 8 10 8 1 3.72- 6.92 5.32 $ 6 13C 8

PF O S 506.9 > 8

0.0 4.570 4.5 8 6 -0.016 1.000 22714 8 4 4. 8 9 2 Per f luorooctanoic Sul f

onate 49 8 .9 > 79.9 4.571 4.5 8 6 -0.015 1.000 3395 88 1 4.65 0.70- 1.30 1.00 49 8 .9 > 9 8 .9 4.571 4.5 8 6 -0.015 1.000 19056 88 1.30- 2.42 1.7 8

* 5 13C4 PF O S ( IS ) 502.9 > 8

0.0 4.571 4.5 8 6 -0.015 504767 8 9.56 $ 8 13C4 PF O S 502.9 > 8

0.0 4.571 4.5 8 6 -0.015 504767 8 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 3 6 9 12 15 18 21 24Y(X100000) C511K02026 [ MS QQQ Chro ] :m /z 421.0 > 375.94.431 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02026 [ MS QQQ Chro ] :m /z 417.0 > 371.94.432 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02026 [ MS QQQ Chro ] :m /z 417.0 > 371.94.432



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 4 8 12 16 20 24 28 32Y(X100000) C511K02026 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 4 12 20 28 36 44 52 60Y(X10000) C511K02026 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 4 8 12 16 20 24 28 32Y(X100000) C511K02026 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 12 20 28 36 44 52 60Y(X10000) C511K02026 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### $ 6 13C8 PFOS

3 4 5

Min 4 13 22 31 40 49 58 67Y(X10000) C511K02026 [ MS QQQ Chro ] :m /z 506.9 > 80.04.570 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 16 28 40 52 64 76 88Y(X10000) C511K02026 [ MS QQQ Chro ] :m /z 498.9 > 79.94.571



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 11 18 25 32 39 46 53Y(X10000) C511K02026 [ MS QQQ Chro ] :m /z 498.9 > 98.94.571 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02026 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02026 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571



### 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:

Calib End Date: GC Column: ID: 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) 1.456 0.205 0.208 -1.7 30.0 Lin1
Perfluorooctanoic acid (PFOA) 1.499 0.193 0.200 -3.5 30.0 Lin1
Perfluorooctanoic Sulfonate 1.834 0.209 0.191 9.2 30.0 Lin1 13C8 PFOA 1.029 0.176 0.200 -11.8 30.0 Lin1 13C4 PFOA 2209935 2153400 10.3 10.0 2.6 Ave 13C8 PFOS 1.130 0.198 0.191 3.7 30.0 Lin1 13C4 PFOS 552973 550386 9.60 9.56 0.5 Ave



### 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 Vol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 94589 Lims Sample ID: 22 Sublist: chrom-8321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:13 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC285 First Level Revie w

er: bonnettj Date: 03-Nov-2011 10:27:30 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C8 PF O A 421.0 > 375.9 4.422 4.433 -0.011 1.000 454974 0.1764

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.423 4.434 -0.011 22099352 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.423 4.434 -0.011 22099352 10.3 3 Ammonium Per

f luorooctanoate (

APF O) 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 Per f luorooctanoic 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 PF O S 506.9 > 80.0 4.561 4.586 -0.025 0.998 119511 0.1982 2 Per f luorooctanoic Sul f

onate 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 PF O S ( IS ) 502.9 > 80.0 4.571 4.586 -0.015 5286424 9.56 $ 8 13C4 PF O S 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 Revie w 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 4 6 8 10 12 14 16Y(X10000) C511K02028 [ MS QQQ Chro ] :m /z 421.0 > 375.94.422 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02028 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02028 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423



### 3 Ammonium Per

f luorooctanoate (

APFO ) ( M

)

2.9 3.9 4.9

Min 4 7 10 13 16 19 22Y(X10000) C511K02028 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 41 46 51 56 61 66 71Y(X1000) C511K02028 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### 1 Per f luorooctanoic acid ( M

)

2.9 3.9 4.9

Min 4 7 10 13 16 19 22Y(X10000) C511K02028 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 41 46 51 56 61 66 71Y(X1000) C511K02028 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### $ 6 13C8 PFOS

3 4 5

Min 41 46 51 56 61 66 71Y(X1000) C511K02028 [ MS QQQ Chro ] :m /z 506.9 > 80.04.561 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 41 47 53 59 65 71 77 83Y(X1000) C511K02028 [ MS QQQ Chro ] :m /z 498.9 > 79.94.563



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 41 45 49 53 57 61 65 69Y(X1000) C511K02028 [ MS QQQ Chro ] :m /z 498.9 > 98.94.563 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02028 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02028 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571



### 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 - PF O A DuPont Client ID: Instrument ID: LC_LCMS5 Lims B atch ID: 94589 Lims Sample ID: 22 O perator ID: TW /J B Injection V ol: 20.00 ul 3 Ammonium Per

f luorooctanoate (

APF O), Signal: 1 , m/ z : 413.0 > 368.9 Ty pe: q uant , R T : 4.44 Processing Integration Results R T : 4.42 Response: 604504 Amount: 0.175797

4.02 Min 4 6 8 10 12 14 16 18 20 22 24Y(X10000) C511K02028 [ MS QQQ Chro ] :m/ z 413.0 > 368.94.424



### Manual Integration Results R T : 4.42 Response: 669691 Amount: 0.204588

4.04 Min 4 6 8 10 12 14 16 18 20 22 24Y(X10000) C511K02028 [ MS QQQ Chro ] :m/ z 413.0 > 368.94.424



### Revie w er: bonnettj , 03-Nov-2011 10:27:30 Audit Action: Manuall y

Integrated Audit Reason: B aseline

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 - PF O A DuPont Client ID: Instrument ID: LC_LCMS5 Lims B atch ID: 94589 Lims Sample ID: 22 O perator ID: TW /J B Injection V ol: 20.00 ul 1 Per f luorooctanoic acid , Signal: 1 , m/ z : 413.0 > 368.9 Ty pe: q uant , R T : 4.44 Processing Integration Results R T : 4.42 Response: 604504 Amount: 0.168424

4.02 Min 4 6 8 10 12 14 16 18 20 22 24Y(X10000) C511K02028 [ MS QQQ Chro ] :m/ z 413.0 > 368.94.424



### Manual Integration Results R T : 4.42 Response: 662476 Amount: 0.193029

4.04 Min 4 6 8 10 12 14 16 18 20 22 24Y(X10000) C511K02028 [ MS QQQ Chro ] :m/ z 413.0 > 368.94.424



### Revie w er: bonnettj , 03-Nov-2011 10:27:30 Audit Action: Manuall y

Integrated Audit Reason: B aseline

Page 96 of 272

### FORM VII

Lab Name: Job No.:
SDG No.:

Instrument ID: Calibration Date: Calib Start Date: Lab Sample ID:

Calib End Date: GC Column: ID: 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) 1.224 0.530 0.520 1.9 30.0 Lin1
Perfluorooctanoic acid (PFOA) 1.273 0.509 0.500 1.8 30.0 Lin1
Perfluorooctanoic Sulfonate 1.470 0.466 0.478 -2.5 30.0 Lin1 13C8 PFOA 0.9244 0.491 0.500 -1.8 30.0 Lin1 13C4 PFOA 2172383 2153400 10.1 10.0 0.9 Ave 13C8 PFOS 1.025 0.513 0.478 7.2 30.0 Lin1 13C4 PFOS 542774 550386 9.43 9.56 -1.4 Ave



### 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 Vol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 945 8 9 Lims Sample ID: 23 Sublist: chrom- 8 321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\ 8 321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:14 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC2 8 5 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C 8

PF O A 421.0 > 375.9 4.422 4.433 -0.011 1.000 10040 8 6 0.4912

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.423 4.434 -0.011 21723 8 29 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.423 4.434 -0.011 21723 8 29 10.1 3 Ammonium Per

f luorooctanoate (

APF O) 413.0 > 36 8 .9 4.424 4.435 -0.011 1.000 13 8 317 8 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. 8 7 1 Per f luorooctanoic acid 413.0 > 36 8 .9 4.424 4.435 -0.011 1.000 13 8 317 8 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. 8 7 $ 6 13C 8

PF O S 506.9 > 8

0.0 4.561 4.5 8 6 -0.025 1.000 265950 0.5126 2 Per f luorooctanoic Sul f

onate 49 8 .9 > 79.9 4.563 4.5 8 6 -0.024 1.000 3 8 1316 0.4659 0.70- 1.30 1.00 49 8 .9 > 9 8 .9 4.563 4.5 8 6 -0.024 1.000 214039 1.30- 2.42 1.7 8

* 5 13C4 PF O S ( IS ) 502.9 > 8

0.0 4.562 4.5 8 6 -0.024 51 88 919 9.56 $ 8 13C4 PF O S 502.9 > 8

0.0 4.562 4.5 8 6 -0.024 51 88 919 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 4 8 12 16 20 24 28Y(X10000) C511K02029 [ MS QQQ Chro ] :m /z 421.0 > 375.94.422 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02029 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02029 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 4 9 14 19 24 29 34 39 44Y(X10000) C511K02029 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 41 50 59 68 77 86 95 104Y(X1000) C511K02029 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 9 14 19 24 29 34 39 44Y(X10000) C511K02029 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 41 50 59 68 77 86 95 104Y(X1000) C511K02029 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### $ 6 13C8 PFOS

3 4 5

Min 41 51 61 71 81 91 101 111Y(X1000) C511K02029 [ MS QQQ Chro ] :m /z 506.9 > 80.04.561 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 6 8 10 12 14Y(X10000) C511K02029 [ MS QQQ Chro ] :m /z 498.9 > 79.94.563



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 41 49 57 65 73 81 89 97Y(X1000) C511K02029 [ MS QQQ Chro ] :m /z 498.9 > 98.94.563 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02029 [ MS QQQ Chro ] :m /z 502.9 > 80.04.562 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02029 [ MS QQQ Chro ] :m /z 502.9 > 80.04.562



### 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:

Calib End Date: GC Column: ID: 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) 1.121 1.05 1.04 0.9 30.0 Lin1
Perfluorooctanoic acid (PFOA) 1.166 1.01 1.00 1.0 30.0 Lin1
Perfluorooctanoic Sulfonate 1.468 0.978 0.956 2.3 30.0 Lin1 13C8 PFOA 0.8922 1.02 1.00 2.0 30.0 Lin1 13C4 PFOA 2223136 2153400 10.3 10.0 3.2 Ave 13C8 PFOS 0.9528 1.00 0.956 4.6 30.0 Lin1 13C4 PFOS 560829 550386 9.74 9.56 1.9 Ave



### 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 Vol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 945 8 9 Lims Sample ID: 24 Sublist: chrom- 8 321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\ 8 321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:15 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC2 8 5 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C 8

PF O A 421.0 > 375.9 4.413 4.433 -0.020 1.000 19 8 3536 1.02

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.414 4.434 -0.020 22231363 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.414 4.434 -0.020 22231363 10.3 3 Ammonium Per

f luorooctanoate (

APF O) 413.0 > 36 8 .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 4 8 2610 3.72- 6.92 5.37 1 Per f luorooctanoic acid 413.0 > 36 8 .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 4 8 2610 3.72- 6.92 5.37 $ 6 13C 8

PF O S 506.9 > 8

0.0 4.561 4.5 8 6 -0.025 1.000 510 8 29 1.00 2 Per f luorooctanoic Sul f

onate 49 8 .9 > 79.9 4.563 4.5 8 6 -0.024 1.000 7 8 6956 0.9779 0.70- 1.30 1.00 49 8 .9 > 9 8 .9 4.563 4.5 8 6 -0.024 1.000 42631 8 1.30- 2.42 1. 8 5

* 5 13C4 PF O S ( IS ) 502.9 > 8

0.0 4.562 4.5 8 6 -0.024 5361524 9.56 $ 8 13C4 PF O S 502.9 > 8

0.0 4.562 4.5 8 6 -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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 4 11 18 25 32 39 46 53 60Y(X10000) C511K02030 [ MS QQQ Chro ] :m /z 421.0 > 375.94.413 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02030 [ MS QQQ Chro ] :m /z 417.0 > 371.94.414 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02030 [ MS QQQ Chro ] :m /z 417.0 > 371.94.414



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 4 13 22 31 40 49 58 67 76Y(X10000) C511K02030 [ MS QQQ Chro ] :m /z 413.0 > 368.94.415 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 4 6 8 10 12 14 16 18Y(X10000) C511K02030 [ MS QQQ Chro ] :m /z 413.0 > 169.04.415 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 13 22 31 40 49 58 67 76Y(X10000) C511K02030 [ MS QQQ Chro ] :m /z 413.0 > 368.94.415



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 6 8 10 12 14 16 18Y(X10000) C511K02030 [ MS QQQ Chro ] :m /z 413.0 > 169.04.415 

### $ 6 13C8 PFOS

3 4 5

Min 4 6 8 10 12 14 16 18Y(X10000) C511K02030 [ MS QQQ Chro ] :m /z 506.9 > 80.04.561 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 7 10 13 16 19 22 25Y(X10000) C511K02030 [ MS QQQ Chro ] :m /z 498.9 > 79.94.563



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 6 8 10 12 14 16Y(X10000) C511K02030 [ MS QQQ Chro ] :m /z 498.9 > 98.94.563 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02030 [ MS QQQ Chro ] :m /z 502.9 > 80.04.562 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02030 [ MS QQQ Chro ] :m /z 502.9 > 80.04.562



### 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:

Calib End Date: GC Column: ID: 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) 1.054 2.05 2.08 -1.5 30.0 Lin1
Perfluorooctanoic acid (PFOA) 1.097 1.97 2.00 -1.5 30.0 Lin1
Perfluorooctanoic Sulfonate 1.272 1.73 1.91 -9.5 30.0 Lin1 13C8 PFOA 0.8616 2.04 2.00 2.0 30.0 Lin1 13C4 PFOA 2221836 2153400 10.3 10.0 3.2 Ave 13C8 PFOS 0.8984 1.92 1.91 0.4 30.0 Lin1 13C4 PFOS 567461 550386 9.86 9.56 3.1 Ave



### 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 Vol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 945 8 9 Lims Sample ID: 25 Sublist: chrom- 8 321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\ 8 321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:16 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC2 8 5 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C 8

PF O A 421.0 > 375.9 4.422 4.433 -0.011 1.000 3 8 2 8 522 2.04

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.423 4.434 -0.011 2221 8 360 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.423 4.434 -0.011 2221 8 360 10.3 3 Ammonium Per

f luorooctanoate (

APF O) 413.0 > 36 8 .9 4.424 4.435 -0.011 1.000 4 8 72 8 9 8 2.05 0.70- 1.30 1.00 413.0 > 169.0 4.415 4.435 -0.020 0.99 8 937631 3.72- 6.92 5.20 1 Per f luorooctanoic acid 413.0 > 36 8 .9 4.424 4.435 -0.011 1.000 4 8 72 8 9 8 1.97 0.70- 1.30 1.00 413.0 > 169.0 4.415 4.435 -0.020 0.99 8 937631 3.72- 6.92 5.20 $ 6 13C 8

PF O S 506.9 > 8

0.0 4.561 4.5 8 6 -0.025 1.000 974794 1.92 2 Per f luorooctanoic Sul f

onate 49 8 .9 > 79.9 4.563 4.5 8 6 -0.024 1.000 13 8 0417 1.73 0.70- 1.30 1.00 49 8 .9 > 9 8 .9 4.563 4.5 8 6 -0.024 1.000 77203 8 1.30- 2.42 1.79

* 5 13C4 PF O S ( IS ) 502.9 > 8

0.0 4.562 4.5 8 6 -0.024 5424923 9.56 $ 8 13C4 PF O S 502.9 > 8

0.0 4.562 4.5 8 6 -0.024 5424923 9. 8 6

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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 2 4 6 8 10Y(X100000) C511K02031 [ MS QQQ Chro ] :m /z 421.0 > 375.94.422 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02031 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02031 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02031 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 4 8 12 16 20 24 28Y(X10000) C511K02031 [ MS QQQ Chro ] :m /z 413.0 > 169.04.415 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02031 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 8 12 16 20 24 28Y(X10000) C511K02031 [ MS QQQ Chro ] :m /z 413.0 > 169.04.415 

### $ 6 13C8 PFOS

3 4 5

Min 4 8 12 16 20 24 28 32Y(X10000) C511K02031 [ MS QQQ Chro ] :m /z 506.9 > 80.04.561 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 9 14 19 24 29 34 39Y(X10000) C511K02031 [ MS QQQ Chro ] :m /z 498.9 > 79.94.563



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 7 10 13 16 19 22 25Y(X10000) C511K02031 [ MS QQQ Chro ] :m /z 498.9 > 98.94.563 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 3 6 9 12 15Y(X100000) C511K02031 [ MS QQQ Chro ] :m /z 502.9 > 80.04.562 

### $ 8 13C4 PFOS

3 4 5

Min 0 3 6 9 12 15Y(X100000) C511K02031 [ MS QQQ Chro ] :m /z 502.9 > 80.04.562



### 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:

Calib End Date: GC Column: ID: 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) 1.055 5.27 5.20 1.3 20.0 Lin1
Perfluorooctanoic acid (PFOA) 1.098 5.06 5.00 1.2 20.0 Lin1
Perfluorooctanoic Sulfonate 1.338 4.62 4.78 -3.3 20.0 Lin1 13C8 PFOA 0.8606 5.21 5.00 4.2 20.0 Lin1 13C4 PFOA 2159755 2153400 10.0 10.0 0.3 Ave 13C8 PFOS 0.9171 4.98 4.78 4.2 20.0 Lin1 13C4 PFOS 556188 550386 9.66 9.56 1.1 Ave



### 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 Vol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 945 8 9 Lims Sample ID: 26 Sublist: chrom- 8 321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\ 8 321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:17 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC2 8 5 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C 8

PF O A 421.0 > 375.9 4.413 4.433 -0.020 1.000 9293452 5.21

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.414 4.434 -0.020 21597553 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.414 4.434 -0.020 21597553 10.0 3 Ammonium Per

f luorooctanoate (

APF O) 413.0 > 36 8 .9 4.415 4.435 -0.020 1.000 11 8 5249 8 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 Per f luorooctanoic acid 413.0 > 36 8 .9 4.415 4.435 -0.020 1.000 11 8 5249 8 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 13C 8

PF O S 506.9 > 8

0.0 4.561 4.5 8 6 -0.025 1.000 243 8 267 4.9 8 2 Per f luorooctanoic Sul f

onate 49 8 .9 > 79.9 4.554 4.5 8 6 -0.032 0.99 8 3556163 4.62 0.70- 1.30 1.00 49 8 .9 > 9 8 .9 4.563 4.5 8 6 -0.024 1.000 1937204 1.30- 2.42 1. 8 4

* 5 13C4 PF O S ( IS ) 502.9 > 8

0.0 4.562 4.5 8 6 -0.024 5317161 9.56 $ 8 13C4 PF O S 502.9 > 8

0.0 4.562 4.5 8 6 -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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 4 8 12 16 20 24Y(X100000) C511K02032 [ MS QQQ Chro ] :m /z 421.0 > 375.94.413 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02032 [ MS QQQ Chro ] :m /z 417.0 > 371.94.414 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02032 [ MS QQQ Chro ] :m /z 417.0 > 371.94.414



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 4 8 12 16 20 24 28 32Y(X100000) C511K02032 [ MS QQQ Chro ] :m /z 413.0 > 368.94.415 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 4 12 20 28 36 44 52 60Y(X10000) C511K02032 [ MS QQQ Chro ] :m /z 413.0 > 169.04.415 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 4 8 12 16 20 24 28 32Y(X100000) C511K02032 [ MS QQQ Chro ] :m /z 413.0 > 368.94.415



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 12 20 28 36 44 52 60Y(X10000) C511K02032 [ MS QQQ Chro ] :m /z 413.0 > 169.04.415 

### $ 6 13C8 PFOS

3 4 5

Min 4 13 22 31 40 49 58 67Y(X10000) C511K02032 [ MS QQQ Chro ] :m /z 506.9 > 80.04.561 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 17 30 43 56 69 82 95Y(X10000) C511K02032 [ MS QQQ Chro ] :m /z 498.9 > 79.94.554



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 11 18 25 32 39 46 53Y(X10000) C511K02032 [ MS QQQ Chro ] :m /z 498.9 > 98.94.563 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02032 [ MS QQQ Chro ] :m /z 502.9 > 80.04.562 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02032 [ MS QQQ Chro ] :m /z 502.9 > 80.04.562



### 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:

Calib End Date: GC Column: ID: 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) 1.018 10.3 10.4 -1.0 30.0 Lin1
Perfluorooctanoic acid (PFOA) 1.060 9.85 10.0 -1.5 30.0 Lin1
Perfluorooctanoic Sulfonate 1.321 9.18 9.56 -4.0 30.0 Lin1 13C8 PFOA 0.8391 10.2 10.0 2.0 30.0 Lin1 13C4 PFOA 2201775 2153400 10.2 10.0 2.2 Ave 13C4 PFOS 571245 550386 9.92 9.56 3.8 Ave 13C8 PFOS 0.8929 9.75 9.56 2.0 30.0 Lin1



### 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 Vol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 94589 Lims Sample ID: 27 Sublist: chrom-8321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:18 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC285 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C8 PF O A 421.0 > 375.9 4.413 4.433 -0.020 1.000 18474100 10.2

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.414 4.434 -0.020 22017750 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.414 4.434 -0.020 22017750 10.2 3 Ammonium Per

f luorooctanoate (

APF O) 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 Per f luorooctanoic 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 PF O S 506.9 > 80.0 4.561 4.586 -0.025 1.002 4876213 9.75 2 Per f luorooctanoic Sul f

onate 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 PF O S ( IS ) 502.9 > 80.0 4.553 4.586 -0.033 5461101 9.56 $ 8 13C4 PF O S 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 7 14 21 28 35 42 49Y(X100000) C511K02033 [ MS QQQ Chro ] :m /z 421.0 > 375.94.413 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02033 [ MS QQQ Chro ] :m /z 417.0 > 371.94.414 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02033 [ MS QQQ Chro ] :m /z 417.0 > 371.94.414



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02033 [ MS QQQ Chro ] :m /z 413.0 > 368.94.415 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 2 4 6 8 10 12Y(X100000) C511K02033 [ MS QQQ Chro ] :m /z 413.0 > 169.04.415 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02033 [ MS QQQ Chro ] :m /z 413.0 > 368.94.415



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 2 4 6 8 10 12Y(X100000) C511K02033 [ MS QQQ Chro ] :m /z 413.0 > 169.04.415 

### $ 6 13C8 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02033 [ MS QQQ Chro ] :m /z 506.9 > 80.04.561 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 3 6 9 12 15 18 21Y(X100000) C511K02033 [ MS QQQ Chro ] :m /z 498.9 > 79.94.554



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 2 4 6 8 10 12Y(X100000) C511K02033 [ MS QQQ Chro ] :m /z 498.9 > 98.94.554 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02033 [ MS QQQ Chro ] :m /z 502.9 > 80.04.553 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02033 [ MS QQQ Chro ] :m /z 502.9 > 80.04.553



### 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:

Calib End Date: GC Column: ID: 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) 1.074 21.7 20.8 4.3 20.0 Lin1
Perfluorooctanoic acid (PFOA) 1.118 20.9 20.0 4.5 20.0 Lin1
Perfluorooctanoic Sulfonate 1.356 18.9 19.1 -1.2 20.0 Lin1 13C8 PFOA 0.8668 21.2 20.0 6.0 20.0 Lin1 13C4 PFOA 1922920 2153400 8.93 10.0 -10.7 Ave 13C8 PFOS 0.9005 19.7 19.1 3.0 20.0 Lin1 13C4 PFOS 522306 550386 9.07 9.56 -5.1 Ave



### 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 Vol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 945 8 9 Lims Sample ID: 2 8 Sublist: chrom- 8 321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\ 8 321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:1 8 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC2 8 5 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C 8

PF O A 421.0 > 375.9 4.413 4.433 -0.020 1.000 33334469 21.2

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.414 4.434 -0.020 19229199 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.414 4.434 -0.020 19229199 8 .93 3 Ammonium Per

f luorooctanoate (

APF O) 413.0 > 36 8 .9 4.415 4.435 -0.020 1.000 429 8 0700 21.7 0.70- 1.30 1.00 413.0 > 169.0 4.415 4.435 -0.020 1.000 8 30 8 9 8 9 3.72- 6.92 5.17 1 Per f luorooctanoic acid 413.0 > 36 8 .9 4.415 4.435 -0.020 1.000 429 8 0700 20.9 0.70- 1.30 1.00 413.0 > 169.0 4.415 4.435 -0.020 1.000 8 30 8 9 8 9 3.72- 6.92 5.17 $ 6 13C 8

PF O S 506.9 > 8

0.0 4.561 4.5 8 6 -0.025 1.000 8 993257 19.7 2 Per f luorooctanoic Sul f

onate 49 8 .9 > 79.9 4.554 4.5 8 6 -0.032 0.99 8 13544 8 04 1 8 .9 0.70- 1.30 1.00 49 8 .9 > 9 8 .9 4.554 4.5 8 6 -0.032 0.99 8 7463107 1.30- 2.42 1. 8 1

* 5 13C4 PF O S ( IS ) 502.9 > 8

0.0 4.562 4.5 8 6 -0.024 499324 8 9.56 $ 8 13C4 PF O S 502.9 > 8

0.0 4.562 4.5 8 6 -0.024 499324 8 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 11 22 33 44 55 66 77 88Y(X100000) C511K02034 [ MS QQQ Chro ] :m /z 421.0 > 375.94.413 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 7 14 21 28 35 42 49Y(X100000) C511K02034 [ MS QQQ Chro ] :m /z 417.0 > 371.94.414 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 7 14 21 28 35 42 49Y(X100000) C511K02034 [ MS QQQ Chro ] :m /z 417.0 > 371.94.414



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 2 4 6 8 10 12Y(X1000000) C511K02034 [ MS QQQ Chro ] :m /z 413.0 > 368.94.415 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 3 6 9 12 15 18 21Y(X100000) C511K02034 [ MS QQQ Chro ] :m /z 413.0 > 169.04.415 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 2 4 6 8 10 12Y(X1000000) C511K02034 [ MS QQQ Chro ] :m /z 413.0 > 368.94.415



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 3 6 9 12 15 18 21Y(X100000) C511K02034 [ MS QQQ Chro ] :m /z 413.0 > 169.04.415 

### $ 6 13C8 PFOS

3 4 5

Min 0 4 8 12 16 20 24Y(X100000) C511K02034 [ MS QQQ Chro ] :m /z 506.9 > 80.04.561 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 5 10 15 20 25 30 35Y(X100000) C511K02034 [ MS QQQ Chro ] :m /z 498.9 > 79.94.554



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 3 6 9 12 15 18 21Y(X100000) C511K02034 [ MS QQQ Chro ] :m /z 498.9 > 98.94.554 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02034 [ MS QQQ Chro ] :m /z 502.9 > 80.04.562 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02034 [ MS QQQ Chro ] :m /z 502.9 > 80.04.562



### 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:

Calib End Date: GC Column: ID: 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) 1.016 51.5 52.0 -1.0 30.0 Lin1
Perfluorooctanoic acid (PFOA) 1.058 49.5 50.0 -1.0 30.0 Lin1
Perfluorooctanoic Sulfonate 1.347 47.0 47.8 -1.7 30.0 Lin1 13C8 PFOA 0.7935 48.6 50.0 -2.8 30.0 Lin1 13C4 PFOA 1744580 2153400 8.10 10.0 -19.0 Ave 13C8 PFOS 0.8515 46.7 47.8 -2.3 30.0 Lin1 13C4 PFOS 453885 550386 7.88 9.56 -17.5 Ave



### 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 Vol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 94589 Lims Sample ID: 29 Sublist: chrom-8321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:19 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC285 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C8 PF O A 421.0 > 375.9 4.413 4.433 -0.020 1.000 69216654 48.6

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.414 4.434 -0.020 17445801 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.414 4.434 -0.020 17445801 8.10 3 Ammonium Per

f luorooctanoate (

APF O) 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 Per f luorooctanoic 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 PF O S 506.9 > 80.0 4.552 4.586 -0.034 1.000 18474613 46.7 2 Per f luorooctanoic Sul f

onate 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 PF O S ( IS ) 502.9 > 80.0 4.553 4.586 -0.033 4339142 9.56 $ 8 13C4 PF O S 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 3 6 9 12 15 18Y(X1000000) C511K02035 [ MS QQQ Chro ] :m /z 421.0 > 375.94.413 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 6 12 18 24 30 36 42Y(X100000) C511K02035 [ MS QQQ Chro ] :m /z 417.0 > 371.94.414 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 6 12 18 24 30 36 42Y(X100000) C511K02035 [ MS QQQ Chro ] :m /z 417.0 > 371.94.414



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 3 6 9 12 15 18 21Y(X1000000) C511K02035 [ MS QQQ Chro ] :m /z 413.0 > 368.94.415 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 6 12 18 24 30 36 42Y(X100000) C511K02035 [ MS QQQ Chro ] :m /z 413.0 > 169.04.415 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 3 6 9 12 15 18 21Y(X1000000) C511K02035 [ MS QQQ Chro ] :m /z 413.0 > 368.94.415



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 6 12 18 24 30 36 42Y(X100000) C511K02035 [ MS QQQ Chro ] :m /z 413.0 > 169.04.415 

### $ 6 13C8 PFOS

3 4 5

Min 0 6 12 18 24 30 36 42Y(X100000) C511K02035 [ MS QQQ Chro ] :m /z 506.9 > 80.04.552 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 10 20 30 40 50 60 70Y(X100000) C511K02035 [ MS QQQ Chro ] :m /z 498.9 > 79.94.554



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 6 12 18 24 30 36Y(X100000) C511K02035 [ MS QQQ Chro ] :m /z 498.9 > 98.94.554 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12Y(X100000) C511K02035 [ MS QQQ Chro ] :m /z 502.9 > 80.04.553 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12Y(X100000) C511K02035 [ MS QQQ Chro ] :m /z 502.9 > 80.04.553



### 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:

Calib End Date: GC Column: ID: 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) 0.8797 112 130 -14.2 30.0 Lin1
Perfluorooctanoic acid (PFOA) 0.9154 107 125 -14.2 30.0 Lin1
Perfluorooctanoic Sulfonate 1.178 103 120 -14.0 30.0 Lin1 13C8 PFOA 0.7055 108 125 -13.4 30.0 Lin1 13C4 PFOA 1426912 2153400 6.63 10.0 -33.7 Ave 13C8 PFOS 0.7564 104 120 -13.2 30.0 Lin1 13C4 PFOS 367327 550386 6.38 9.56 -33.3 Ave



### 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 Vol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 945 8 9 Lims Sample ID: 30 Sublist: chrom- 8 321_PF O A_S_Dupont * sub1 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\ 8 321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:20 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC2 8 5 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C 8

PF O A 421.0 > 375.9 4.413 4.433 -0.020 1.000 125 8 303 88 10 8 .2

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.414 4.434 -0.020 14269120 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.414 4.434 -0.020 14269120 6.63 3 Ammonium Per

f luorooctanoate (

APF O) E 413.0 > 36 8 .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 0.99 8 31020574 3.72- 6.92 5.26 1 Per f luorooctanoic acid E 413.0 > 36 8 .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 0.99 8 31020574 3.72- 6.92 5.26 $ 6 13C 8

PF O S 506.9 > 8

0.0 4.552 4.5 8 6 -0.034 1.000 33201962 103.7 2 Per f luorooctanoic Sul f

onate E 49 8 .9 > 79.9 4.554 4.5 8 6 -0.032 1.000 51703144 102. 8 0.70- 1.30 1.00 E 49 8 .9 > 9 8 .9 4.554 4.5 8 6 -0.032 1.000 2 8 344659 1.30- 2.42 1. 8 2

* 5 13C4 PF O S ( IS ) 502.9 > 8

0.0 4.553 4.5 8 6 -0.033 3511649 9.56 $ 8 13C4 PF O S 502.9 > 8

0.0 4.553 4.5 8 6 -0.033 3511649 6.3 8 QC Flag Legend Processing Flags E - Ex ceeded Ma x imum 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 4 8 12 16 20 24 28Y(X1000000) C511K02036 [ MS QQQ Chro ] :m /z 421.0 > 375.94.413 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 4 8 12 16 20 24 28 32Y(X100000) C511K02036 [ MS QQQ Chro ] :m /z 417.0 > 371.94.414 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 4 8 12 16 20 24 28 32Y(X100000) C511K02036 [ MS QQQ Chro ] :m /z 417.0 > 371.94.414



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 5 10 15 20 25 30 35Y(X1000000) C511K02036 [ MS QQQ Chro ] :m /z 413.0 > 368.94.415 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 9 18 27 36 45 54 63Y(X100000) C511K02036 [ MS QQQ Chro ] :m /z 413.0 > 169.04.406 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 5 10 15 20 25 30 35Y(X1000000) C511K02036 [ MS QQQ Chro ] :m /z 413.0 > 368.94.415



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 9 18 27 36 45 54 63Y(X100000) C511K02036 [ MS QQQ Chro ] :m /z 413.0 > 169.04.406 

### $ 6 13C8 PFOS

3 4 5

Min 0 9 18 27 36 45 54 63 72Y(X100000) C511K02036 [ MS QQQ Chro ] :m /z 506.9 > 80.04.552 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 2 4 6 8 10 12Y(X1000000) C511K02036 [ MS QQQ Chro ] :m /z 498.9 > 79.94.554



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02036 [ MS QQQ Chro ] :m /z 498.9 > 98.94.554 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 4 14 24 34 44 54 64 74 84Y(X10000) C511K02036 [ MS QQQ Chro ] :m /z 502.9 > 80.04.553 

### $ 8 13C4 PFOS

3 4 5

Min 4 14 24 34 44 54 64 74 84Y(X10000) C511K02036 [ MS QQQ Chro ] :m /z 502.9 > 80.04.553



### 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 Form 1 LCMS ORGANICS ANALYSIS DATA SHEET

Client Sample ID: Lab Name: Job No.:
SDG No.: 280-21985-1

Lab Sample ID: MB 280-94046/1-A Matrix: PC511K02020.d Lab File ID:
Date Collected: DV-LC-0012 Analysis Method: 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: ID: Gemini-NX
N Analysis Batch No.: 94589 ug/Kg Units:

CAS NO. COMPOUND NAME RESULT Q MDL RL

2.5 0.50 3825-26-1 Ammonium Perfluorooctanoate (APFO) ND 2.5 0.50 335-67-1 Perfluorooctanoic acid (PFOA) ND



### SURROGATE %REC CAS NO. LIMITS Q

92 50-200 STL00990 13C4 PFOA



### 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 T y pe: MB Sample ID: mb 280-94046/1-a , Sample Misc. In f o.: O perator: T W /JB Instrument ID: LC_LCMS5 V ol. Injected: 20.0000 ALS Bottle # : 0 Lims Batch ID: 94589 Lims Sample ID: 14 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal/ Ex ternal Standard Quant B y : Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC285 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug/L Ratio Range Ratio Flags $ 9 13C8 PF O A 421.0 > 375.9 4.449 4.433 0.016 1.000 17429442 10.7

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.450 4.434 0.016 19825404 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.450 4.434 0.016 19825404 9.21 3 Ammonium Per

f luorooctanoate (

APF O) 1 413.0 > 368.9 4.435 413.0 > 169.0 4.435 1 Per f luorooctanoic acid 1 413.0 > 368.9 4.435 413.0 > 169.0 4.435 $ 6 13C8 PF O S 506.9 > 80.0 4.596 4.586 0.010 1.000 4540517 9.76 2 Per f luorooctanoic Sul f

onate 498.9 > 79.9 4.586 498.9 > 98.9 4.586

* 5 13C4 PF O S ( IS ) 502.9 > 80.0 4.597 4.586 0.011 5078600 9.56 $ 8 13C4 PF O S 502.9 > 80.0 4.597 4.586 0.011 5078600 9.23 QC Flag Legend Processing Flags 1 - Missing Pea k s

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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 6 12 18 24 30 36 42Y(X100000) C511K02020 [ MS QQQ Chro ] :m /z 421.0 > 375.94.449 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 7 14 21 28 35 42 49Y(X100000) C511K02020 [ MS QQQ Chro ] :m /z 417.0 > 371.94.450 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 7 14 21 28 35 42 49Y(X100000) C511K02020 [ MS QQQ Chro ] :m /z 417.0 > 371.94.450



### 3 Ammonium Per

f luorooctanoate (

APFO ) ( ND )

2.9 3.9 4.9

Min 41 44 47 50 53 56 59 62Y(X1000) C511K02020 [ MS QQQ Chro ] :m /z 413.0 > 368.9 

### 3 Ammonium Per f luorooctanoate (

APFO ) ( ND )

2.9 3.9 4.9

Min 413 419 425 431 437 443 449 455Y(X100) C511K02020 [ MS QQQ Chro ] :m /z 413.0 > 169.0 

### 1 Per f luorooctanoic acid ( ND )

2.9 3.9 4.9

Min 41 44 47 50 53 56 59 62Y(X1000) C511K02020 [ MS QQQ Chro ] :m /z 413.0 > 368.9



### 1 Per f luorooctanoic acid ( ND )

2.9 3.9 4.9

Min 413 419 425 431 437 443 449 455Y(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 14Y(X100000) C511K02020 [ MS QQQ Chro ] :m /z 506.9 > 80.04.596 

### 2 Per f luorooctanoic Sul f

onate ( ND )

3 4 5

Min 413 416 419 422 425 428 431Y(X100) C511K02020 [ MS QQQ Chro ] :m /z 498.9 > 79.9



### 2 Per f luorooctanoic Sul f

onate ( ND )

3 4 5

Min 413 415 417 419 421 423Y(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 14Y(X100000) C511K02020 [ MS QQQ Chro ] :m /z 502.9 > 80.04.597 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02020 [ MS QQQ Chro ] :m /z 502.9 > 80.04.597



### 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 Form 1 LCMS ORGANICS ANALYSIS DATA SHEET

Client Sample ID: Lab Name: Job No.:
SDG No.: 280-21985-1

Lab Sample ID: CCB 280-94589/11 Matrix: PC511K02017.d Lab File ID:
Date Collected: DV-LC-0012 Analysis Method: 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: ID: Gemini-NX
N Analysis Batch No.: 94589 ug/L Units:

CAS NO. COMPOUND NAME RESULT Q MDL RL

0.50 0.052 3825-26-1 Ammonium Perfluorooctanoate (APFO) ND 0.50 0.052 335-67-1 Perfluorooctanoic acid (PFOA) ND



### SURROGATE %REC CAS NO. LIMITS Q

100 50-200 STL00990 13C4 PFOA



### 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. In f o.: O perator: T W/ JB Instrument ID: LC_LCMS5 V ol. Injected: 20.0000 ALS Bottle # : 0 Lims Batch ID: 945 8 9 Lims Sample ID: 11 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\ 8 321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant By: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC2 8 5 First Level Revie w

er: bonnettj Date: 03-Nov-2011 10:23:51 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C 8

PF O A 421.0 > 375.9 4.433

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.423 4.434 -0.011 2156 8 424 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.423 4.434 -0.011 2156 8 424 10.0 3 Ammonium Per

f luorooctanoate (

APF O) 1 413.0 > 36 8 .9 4.435 413.0 > 169.0 4.435 1 Per f luorooctanoic acid 1 413.0 > 36 8 .9 4.435 413.0 > 169.0 4.435 $ 6 13C 8

PF O S 506.9 > 8

0.0 4.5 8 6 2 Per f luorooctanoic Sul f

onate 1 49 8 .9 > 79.9 4.5 8 6 49 8 .9 > 9 8 .9 4.5 8 6

* 5 13C4 PF O S ( IS ) 502.9 > 8

0.0 4.571 4.5 8 6 -0.015 5205 8 20 9.56 $ 8 13C4 PF O S 502.9 > 8

0.0 4.571 4.5 8 6 -0.015 5205 8 20 9.46 QC Flag Legend Processing Flags 1 - Missing Pea k s

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 V ol: 20.00 ul $ 9 13C8 PFOA ( ND )

2.9 3.9 4.9

Min 410 416 422 428 434 440 446 452Y(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 56Y(X100000) C511K02017 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02017 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423



### 3 Ammonium Per

f luorooctanoate (

APFO ) ( ND )

2.9 3.9 4.9

Min 42 46 50 54 58 62 66 70Y(X1000) C511K02017 [ MS QQQ Chro ] :m /z 413.0 > 368.9 

### 3 Ammonium Per f luorooctanoate (

APFO ) ( ND )

2.9 3.9 4.9

Min 410 418 426 434 442 450 458 466Y(X100) C511K02017 [ MS QQQ Chro ] :m /z 413.0 > 169.0 

### 1 Per f luorooctanoic acid ( ND )

2.9 3.9 4.9

Min 42 46 50 54 58 62 66 70Y(X1000) C511K02017 [ MS QQQ Chro ] :m /z 413.0 > 368.9



### 1 Per f luorooctanoic acid ( ND )

2.9 3.9 4.9

Min 410 418 426 434 442 450 458 466Y(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 466Y(X100) C511K02017 [ MS QQQ Chro ] :m /z 506.9 > 80.0 

### 2 Per f luorooctanoic Sul f

onate ( ND )

3 4 5

Min 411 418 425 432 439 446 453 460Y(X100) C511K02017 [ MS QQQ Chro ] :m /z 498.9 > 79.9



### 2 Per f luorooctanoic Sul f

onate ( ND )

3 4 5

Min 411 415 419 423 427 431 435Y(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 14Y(X100000) C511K02017 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02017 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571



### 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 Form 1 LCMS ORGANICS ANALYSIS DATA SHEET

Client Sample ID: Lab Name: Job No.:
SDG No.: 280-21985-1

Lab Sample ID: CCB 280-94589/21 Matrix: PC511K02027.d Lab File ID:
Date Collected: DV-LC-0012 Analysis Method: 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: ID: Gemini-NX
N Analysis Batch No.: 94589 ug/L Units:

CAS NO. COMPOUND NAME RESULT Q MDL RL

0.50 0.052 3825-26-1 Ammonium Perfluorooctanoate (APFO) ND 0.50 0.052 335-67-1 Perfluorooctanoic acid (PFOA) ND



### SURROGATE %REC CAS NO. LIMITS Q

98 50-200 STL00990 13C4 PFOA



### 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. In f o.: O perator: T W/ JB Instrument ID: LC_LCMS5 V ol. Injected: 20.0000 ALS Bottle # : 0 Lims Batch ID: 945 8 9 Lims Sample ID: 21 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\ 8 321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:12 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant By: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC2 8 5 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C 8

PF O A 421.0 > 375.9 4.433

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.423 4.434 -0.011 21131544 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.423 4.434 -0.011 21131544 9. 8 1 3 Ammonium Per

f luorooctanoate (

APF O) 1 413.0 > 36 8 .9 4.435 413.0 > 169.0 4.435 1 Per f luorooctanoic acid 1 413.0 > 36 8 .9 4.435 413.0 > 169.0 4.435 $ 6 13C 8

PF O S 506.9 > 8

0.0 4.5 8 6 2 Per f luorooctanoic Sul f

onate 49 8 .9 > 79.9 4.5 8 6 49 8 .9 > 9 8 .9 4.5 8 6

* 5 13C4 PF O S ( IS ) 502.9 > 8

0.0 4.571 4.5 8 6 -0.015 51 8 1337 9.56 $ 8 13C4 PF O S 502.9 > 8

0.0 4.571 4.5 8 6 -0.015 51 8 1337 9.41 QC Flag Legend Processing Flags 1 - Missing Pea k s

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 V ol: 20.00 ul $ 9 13C8 PFOA ( ND )

2.9 3.9 4.9

Min 413 416 419 422 425 428 431 434Y(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 56Y(X100000) C511K02027 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02027 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423



### 3 Ammonium Per

f luorooctanoate (

APFO ) ( ND )

2.9 3.9 4.9

Min 41 45 49 53 57 61 65Y(X1000) C511K02027 [ MS QQQ Chro ] :m /z 413.0 > 368.9 

### 3 Ammonium Per f luorooctanoate (

APFO ) ( ND )

2.9 3.9 4.9

Min 413 419 425 431 437 443 449Y(X100) C511K02027 [ MS QQQ Chro ] :m /z 413.0 > 169.0 

### 1 Per f luorooctanoic acid ( ND )

2.9 3.9 4.9

Min 41 45 49 53 57 61 65Y(X1000) C511K02027 [ MS QQQ Chro ] :m /z 413.0 > 368.9



### 1 Per f luorooctanoic acid ( ND )

2.9 3.9 4.9

Min 413 419 425 431 437 443 449Y(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 443Y(X100) C511K02027 [ MS QQQ Chro ] :m /z 506.9 > 80.0 

### 2 Per f luorooctanoic Sul f

onate ( ND )

3 4 5

Min 413 417 421 425 429 433 437 441 445Y(X100) C511K02027 [ MS QQQ Chro ] :m /z 498.9 > 79.9



### 2 Per f luorooctanoic Sul f

onate ( ND )

3 4 5

Min 413 416 419 422 425 428 431Y(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 16Y(X100000) C511K02027 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02027 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571



### 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 Form 1 LCMS ORGANICS ANALYSIS DATA SHEET

Client Sample ID: Lab Name: Job No.:
SDG No.: 280-21985-1

Lab Sample ID: LCS 280-94046/2-A Matrix: PC511K02021.d Lab File ID:
Date Collected: DV-LC-0012 Analysis Method: 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: ID: Gemini-NX
N Analysis Batch No.: 94589 ug/Kg Units:

CAS NO. COMPOUND NAME RESULT Q MDL RL

2.5 0.50 3825-26-1 Ammonium Perfluorooctanoate (APFO) 58.0 2.5 0.50 335-67-1 Perfluorooctanoic acid (PFOA) 55.5



### SURROGATE %REC CAS NO. LIMITS Q

91 50-200 STL00990 13C4 PFOA



### 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. In f o.: O perator: T W /J B Instrument ID: LC_LCMS5 V ol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 94589 Lims Sample ID: 15 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal/ Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC285 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug/L Ratio Range Ratio Flags $ 9 13C8 PF O A 421.0 > 375.9 4.449 4.433 0.016 1.000 17187234 10.7

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.450 4.434 0.016 19510836 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.450 4.434 0.016 19510836 9.06 3 Ammonium Per

f luorooctanoate (

APF O) 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 Per f luorooctanoic 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 PF O S 506.9 > 80.0 4.596 4.586 0.010 1.000 4654243 9.75 2 Per f luorooctanoic Sul f

onate 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 PF O S ( IS ) 502.9 > 80.0 4.597 4.586 0.011 5213188 9.56 $ 8 13C4 PF O S 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 6 12 18 24 30 36 42Y(X100000) C511K02021 [ MS QQQ Chro ] :m /z 421.0 > 375.94.449 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 7 14 21 28 35 42 49Y(X100000) C511K02021 [ MS QQQ Chro ] :m /z 417.0 > 371.94.450 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 7 14 21 28 35 42 49Y(X100000) C511K02021 [ MS QQQ Chro ] :m /z 417.0 > 371.94.450



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02021 [ MS QQQ Chro ] :m /z 413.0 > 368.94.451 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 0 2 4 6 8 10 12Y(X100000) C511K02021 [ MS QQQ Chro ] :m /z 413.0 > 169.04.451 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02021 [ MS QQQ Chro ] :m /z 413.0 > 368.94.451



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 2 4 6 8 10 12Y(X100000) C511K02021 [ MS QQQ Chro ] :m /z 413.0 > 169.04.451 

### $ 6 13C8 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02021 [ MS QQQ Chro ] :m /z 506.9 > 80.04.596 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 3 6 9 12 15 18 21Y(X100000) C511K02021 [ MS QQQ Chro ] :m /z 498.9 > 79.94.598



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 0 2 4 6 8 10 12Y(X100000) C511K02021 [ MS QQQ Chro ] :m /z 498.9 > 98.94.598 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02021 [ MS QQQ Chro ] :m /z 502.9 > 80.04.597 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14 16Y(X100000) C511K02021 [ MS QQQ Chro ] :m /z 502.9 > 80.04.597



### 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 Form 1 LCMS ORGANICS ANALYSIS DATA SHEET

Client Sample ID: Lab Name: Job No.:
SDG No.: 280-21985-1

Lab Sample ID: LLCS 280-94046/3-A Matrix: PC511K02022.d Lab File ID:
Date Collected: DV-LC-0012 Analysis Method: 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: ID: Gemini-NX
N Analysis Batch No.: 94589 ug/Kg Units:

CAS NO. COMPOUND NAME RESULT Q MDL RL

2.5 0.49 3825-26-1 Ammonium Perfluorooctanoate (APFO) 5.73 2.5 0.49 335-67-1 Perfluorooctanoic acid (PFOA) 5.48



### SURROGATE %REC CAS NO. LIMITS Q

95 50-200 STL00990 13C4 PFOA



### 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. In f o.: O perator: T W /J B Instrument ID: LC_LCMS5 V ol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 94589 Lims Sample ID: 16 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal/ Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC285 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug/L Ratio Range Ratio Flags $ 9 13C8 PF O A 421.0 > 375.9 4.458 4.433 0.025 1.000 17944069 10.7

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.459 4.434 0.025 20508155 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.459 4.434 0.025 20508155 9.52 3 Ammonium Per

f luorooctanoate (

APF O) 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 Per f luorooctanoic 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 PF O S 506.9 > 80.0 4.605 4.586 0.019 1.000 4641355 9.65 2 Per f luorooctanoic Sul f

onate 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 PF O S ( IS ) 502.9 > 80.0 4.606 4.586 0.020 5251794 9.56 $ 8 13C4 PF O S 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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 0 6 12 18 24 30 36 42 48Y(X100000) C511K02022 [ MS QQQ Chro ] :m /z 421.0 > 375.94.458 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 7 14 21 28 35 42 49Y(X100000) C511K02022 [ MS QQQ Chro ] :m /z 417.0 > 371.94.459 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 7 14 21 28 35 42 49Y(X100000) C511K02022 [ MS QQQ Chro ] :m /z 417.0 > 371.94.459



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 4 13 22 31 40 49 58 67Y(X10000) C511K02022 [ MS QQQ Chro ] :m /z 413.0 > 368.94.460 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 4 6 8 10 12 14 16 18Y(X10000) C511K02022 [ MS QQQ Chro ] :m /z 413.0 > 169.04.451 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 13 22 31 40 49 58 67Y(X10000) C511K02022 [ MS QQQ Chro ] :m /z 413.0 > 368.94.460



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 6 8 10 12 14 16 18Y(X10000) C511K02022 [ MS QQQ Chro ] :m /z 413.0 > 169.04.451 

### $ 6 13C8 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02022 [ MS QQQ Chro ] :m /z 506.9 > 80.04.605 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 7 10 13 16 19 22 25Y(X10000) C511K02022 [ MS QQQ Chro ] :m /z 498.9 > 79.94.598



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 6 8 10 12 14 16Y(X10000) C511K02022 [ MS QQQ Chro ] :m /z 498.9 > 98.94.607 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02022 [ MS QQQ Chro ] :m /z 502.9 > 80.04.606 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02022 [ MS QQQ Chro ] :m /z 502.9 > 80.04.606



### 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 Form 1 LCMS ORGANICS ANALYSIS DATA SHEET

Client Sample ID: Lab Name: Job No.:
SDG No.: 280-21985-1

Lab Sample ID: DLCK 280-94589/13 Matrix: PC511K02019.d Lab File ID:
Date Collected: DV-LC-0012 Analysis Method: 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: ID: Gemini-NX
N Analysis Batch No.: 94589 ug/L Units:

CAS NO. COMPOUND NAME RESULT Q MDL RL

0.50 0.052 J 3825-26-1 Ammonium Perfluorooctanoate (APFO) 0.488 0.50 0.052 J 335-67-1 Perfluorooctanoic acid (PFOA) 0.468



### SURROGATE %REC CAS NO. LIMITS Q

101 50-200 STL00990 13C4 PFOA



### 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. In f o.: O perator: T W/ J B Instrument ID: LC_LCMS5 V ol. Injected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 945 8 9 Lims Sample ID: 13 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\ 8 321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y: Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC2 8 5 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C 8

PF O A 421.0 > 375.9 4.422 4.433 -0.011 1.000 1013527 0.4953

* 4 13C4 PF O A ( IS ) 417.0 > 371.9 4.423 4.434 -0.011 21770259 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.423 4.434 -0.011 21770259 10.1 3 Ammonium Per

f luorooctanoate (

APF O) 413.0 > 36 8 .9 4.424 4.435 -0.011 1.000 12914 8 0 0.4 8 7 8 0.70- 1.30 1.00 413.0 > 169.0 4.415 4.435 -0.020 0.99 8 2319 88 3.72- 6.92 5.57 1 Per f luorooctanoic acid 413.0 > 36 8 .9 4.424 4.435 -0.011 1.000 12914 8 0 0.46 8 3 0.70- 1.30 1.00 413.0 > 169.0 4.415 4.435 -0.020 0.99 8 2319 88 3.72- 6.92 5.57 $ 6 13C 8

PF O S 506.9 > 8

0.0 4.570 4.5 8 6 -0.016 1.000 233919 0.4391 2 Per f luorooctanoic Sul f

onate 49 8 .9 > 79.9 4.571 4.5 8 6 -0.015 1.000 405313 0.491 8 0.70- 1.30 1.00 49 8 .9 > 9 8 .9 4.571 4.5 8 6 -0.015 1.000 210969 1.30- 2.42 1.92

* 5 13C4 PF O S ( IS ) 502.9 > 8

0.0 4.571 4.5 8 6 -0.015 5249734 9.56 $ 8 13C4 PF O S 502.9 > 8

0.0 4.571 4.5 8 6 -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 V ol: 20.00 ul $ 9 13C8 PFOA

2.9 3.9 4.9

Min 4 8 12 16 20 24 28 32Y(X10000) C511K02019 [ MS QQQ Chro ] :m /z 421.0 > 375.94.422 

### * 4 13C4 PFOA ( IS )

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02019 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 8 16 24 32 40 48 56Y(X100000) C511K02019 [ MS QQQ Chro ] :m /z 417.0 > 371.94.423



### 3 Ammonium Per

f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 4 9 14 19 24 29 34 39Y(X10000) C511K02019 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424 

### 3 Ammonium Per f luorooctanoate (

APFO )

2.9 3.9 4.9

Min 41 50 59 68 77 86 95 104 113Y(X1000) C511K02019 [ MS QQQ Chro ] :m /z 413.0 > 169.04.415 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 9 14 19 24 29 34 39Y(X10000) C511K02019 [ MS QQQ Chro ] :m /z 413.0 > 368.94.424



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 41 50 59 68 77 86 95 104 113Y(X1000) C511K02019 [ MS QQQ Chro ] :m /z 413.0 > 169.04.415 

### $ 6 13C8 PFOS

3 4 5

Min 41 50 59 68 77 86 95 104 113Y(X1000) C511K02019 [ MS QQQ Chro ] :m /z 506.9 > 80.04.570 

### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 6 8 10 12 14 16Y(X10000) C511K02019 [ MS QQQ Chro ] :m /z 498.9 > 79.94.571



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 41 49 57 65 73 81 89 97 105Y(X1000) C511K02019 [ MS QQQ Chro ] :m /z 498.9 > 98.94.571 

### * 5 13C4 PFOS ( IS )

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02019 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571 

### $ 8 13C4 PFOS

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02019 [ MS QQQ Chro ] :m /z 502.9 > 80.04.571



### 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 Form 1 LCMS ORGANICS ANALYSIS DATA SHEET

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: PC511K02024.d Lab File ID:
Date Collected: DV-LC-0012 Analysis Method: 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: ID: Gemini-NX
N Analysis Batch No.: 94589 ug/Kg Units:

CAS NO. COMPOUND NAME RESULT Q MDL RL

3.4 0.69 3825-26-1 Ammonium Perfluorooctanoate (APFO) 77.9 3.4 0.69 335-67-1 Perfluorooctanoic acid (PFOA) 75.1



### SURROGATE %REC CAS NO. LIMITS Q

X 49 50-200 STL00990 13C4 PFOA



### 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 In j ect. Date: 02-Nov-2011 15:53:34 Dil. Factor: 1.0000 Sample T y pe: MS Sample ID: 280-21985-a-1-b ms , Sample Misc. In f o.: O perator: TW / JB Instrument ID: LC_LCMS5 V ol. In j ected: 20.0000 ALS Bottle # : 0 Lims Batch ID: 94589 Lims Sample ID: 18 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last U pdate: 03-Nov-2011 10:29:04 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant B y : Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC285 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C8 PF O A 421.0 > 375.9 4.431 4.433 -0.002 1.000 9280504 10.7

* 4 13C4 PF O A (IS ) 417.0 > 371.9 4.432 4.434 -0.002 10550504 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.432 4.434 -0.002 10550504 4.90 3 Ammonium Per

f luorooctanoate (APF O) 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 Per f luorooctanoic 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 PF O S 506.9 > 80.0 4.579 4.586 -0.007 1.000 2956142 10.1 2 Per f luorooctanoic Sul f

onate 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 PF O S (IS ) 502.9 > 80.0 4.579 4.586 -0.007 3198056 9.56 $ 8 13C4 PF O S 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: 945 8 9 Lims Sample ID: 1 8 Operator ID: T W / JB Injection V ol: 20.00 ul $ 9 13C 8

PFOA

2.9 3.9 4.9

Min 0 4 8 12 16 20 24Y(X100000) C511K02024 [ MS QQQ Chro ] :m /z 421.0 > 375.94.431 

### * 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min 0 4 8 12 16 20 24 2 8Y(X100000) C511K02024 [ MS QQQ Chro ] :m /z 417.0 > 371.94.432 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 4 8 12 16 20 24 2 8Y(X100000) C511K02024 [ MS QQQ Chro ] :m /z 417.0 > 371.94.432



### 3 Ammonium Per

f luorooctanoate (APFO)

2.9 3.9 4.9

Min 0 5 10 15 20 25 30Y(X100000) C511K02024 [ MS QQQ Chro ] :m /z 413.0 > 36 8 .94.433 

### 3 Ammonium Per f luorooctanoate (APFO)

2.9 3.9 4.9

Min 4 13 22 31 40 49 5 8 67Y(X10000) C511K02024 [ MS QQQ Chro ] :m /z 413.0 > 169.04.433 

### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 0 5 10 15 20 25 30Y(X100000) C511K02024 [ MS QQQ Chro ] :m /z 413.0 > 36 8 .94.433



### 1 Per f luorooctanoic acid

2.9 3.9 4.9

Min 4 13 22 31 40 49 5 8 67Y(X10000) C511K02024 [ MS QQQ Chro ] :m /z 413.0 > 169.04.433 

### $ 6 13C 8 PFOS

3 4 5

Min 4 15 26 37 4 8 59 70 8 1Y(X10000) C511K02024 [ MS QQQ Chro ] :m /z 506.9 > 8 0.04.579 

### 2 Per

f luorooctanoic Sul f

onate

3 4 5

Min 0 2 4 6 8 10 12 14Y(X100000) C511K02024 [ MS QQQ Chro ] :m /z 49 8 .9 > 79.94.571



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 4 13 22 31 40 49 5 8 67Y(X10000) C511K02024 [ MS QQQ Chro ] :m /z 49 8 .9 > 9 8 .94.571 

### * 5 13C4 PFOS (IS)

3 4 5

Min 4 15 26 37 4 8 59 70 8 1 92Y(X10000) C511K02024 [ MS QQQ Chro ] :m /z 502.9 > 8 0.04.579 

### $ 8 13C4 PFOS

3 4 5

Min 4 15 26 37 4 8 59 70 8 1 92Y(X10000) C511K02024 [ MS QQQ Chro ] :m /z 502.9 > 8 0.04.579



### 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 Form 1 LCMS ORGANICS ANALYSIS DATA SHEET

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: PC511K02025.d Lab File ID:
Date Collected: DV-LC-0012 Analysis Method: 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: ID: Gemini-NX
N Analysis Batch No.: 94589 ug/Kg Units:

CAS NO. COMPOUND NAME RESULT Q MDL RL

3.5 0.70 J 3825-26-1 Ammonium Perfluorooctanoate (APFO) 1.07 3.5 0.70 J 335-67-1 Perfluorooctanoic acid (PFOA) 0.983



### SURROGATE %REC CAS NO. LIMITS Q

51 50-200 STL00990 13C4 PFOA



### 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 ) -R E P In j ect. Date: 02-Nov-2011 16:01:19 Dil. Factor: 1.0000 Sample T y pe: DU Sample ID: 280-21985-a-1-c du , Sample Misc. In f o.: O perator: TW / J B Instrument ID: LC_LCMS5 V ol. In j ected: 20.0000 ALS B ottle # : 0 Lims B atch ID: 94589 Lims Sample ID: 19 Ra w Data: Smoothed Detector: MS QQQ Method: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\8321_PF O A_S_Dupont.m Last Update: 03-Nov-2011 14:45:19 Calib Date: 02-Nov-2011 14:51:42 Quant Method: Internal /Ex ternal Standard Quant By : Initial Calibration Last ICal File: \\Denchrom\chromdata\LC_LCMS5\20111103-2707.b\PC511K02016.d Limit G roup: LC - PF O A DuPont Integrator: Falcon Process H ost: D E NPC308 First Level Revie w

er: w illiamst Date: 03-Nov-2011 14:45:00 Signal RT ADJ RT DLT RT R E L RT Response O n-Col Amt ug / L Ratio Range Ratio Flags $ 9 13C8 PF O A 421.0 > 375.9 4.431 4.433 -0.002 1.000 9554896 10.6

* 4 13C4 PF O A (IS ) 417.0 > 371.9 4.432 4.434 -0.002 11017193 10.0 $ 7 13C4 PF O A 417.0 > 371.9 4.432 4.434 -0.002 11017193 5.12 3 Ammonium Per

f luorooctanoate (APF O) 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 Per f luorooctanoic 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 PF O S 506.9 > 80.0 4.570 4.586 -0.016 1.000 2947347 9.81 2 Per f luorooctanoic Sul f

onate 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 PF O S (IS ) 502.9 > 80.0 4.571 4.586 -0.015 3280529 9.56 $ 8 13C4 PF O S 502.9 > 80.0 4.571 4.586 -0.015 3280529 5.96 QC Flag Legend Revie w Flags M - Manuall y

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 B atch ID: 945 8 9 Lims Sample ID: 19 Operator ID: T W / J B Injection V ol: 20.00 ul $ 9 13C 8

PFOA

2.9 3.9 4.9

Min 0 4 8 12 16 20 24Y(X100000) C511K02025 [ MS QQQ Chro ] :m /z 421.0 > 375.94.431 

### * 4 13C4 PFOA (IS)

2.9 3.9 4.9

Min 0 4 8 12 16 20 24 2 8Y(X100000) C511K02025 [ MS QQQ Chro ] :m /z 417.0 > 371.94.432 

### $ 7 13C4 PFOA

2.9 3.9 4.9

Min 0 4 8 12 16 20 24 2 8Y(X100000) C511K02025 [ MS QQQ Chro ] :m /z 417.0 > 371.94.432



### 3 Ammonium Per

f luorooctanoate (APFO) (M)

2.9 3.9 4.9

Min 46 56 66 76 8 6 96 106 116 126Y(X1000) C511K02025 [ MS QQQ Chro ] :m /z 413.0 > 36 8 .94.433 

### 3 Ammonium Per f luorooctanoate (APFO) (M)

2.9 3.9 4.9

Min 41 43 45 47 49 51 53 55 57Y(X1000) C511K02025 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### 1 Per f luorooctanoic acid (M)

2.9 3.9 4.9

Min 46 56 66 76 8 6 96 106 116 126Y(X1000) C511K02025 [ MS QQQ Chro ] :m /z 413.0 > 36 8 .94.433



### 1 Per f luorooctanoic acid (M)

2.9 3.9 4.9

Min 41 43 45 47 49 51 53 55 57Y(X1000) C511K02025 [ MS QQQ Chro ] :m /z 413.0 > 169.04.424 

### $ 6 13C 8 PFOS

3 4 5

Min 4 15 26 37 4 8 59 70 8 1Y(X10000) C511K02025 [ MS QQQ Chro ] :m /z 506.9 > 8 0.04.570 

### 2 Per

f luorooctanoic Sul f

onate

3 4 5

Min 41 45 49 53 57 61 65 69Y(X1000) C511K02025 [ MS QQQ Chro ] :m /z 49 8 .9 > 79.94.571



### 2 Per f luorooctanoic Sul f

onate

3 4 5

Min 41 43 45 47 49 51 53 55Y(X1000) C511K02025 [ MS QQQ Chro ] :m /z 49 8 .9 > 9 8 .94.571 

### * 5 13C4 PFOS (IS)

3 4 5

Min 4 16 2 8 40 52 64 76 88Y(X10000) C511K02025 [ MS QQQ Chro ] :m /z 502.9 > 8 0.04.571 

### $ 8 13C4 PFOS

3 4 5

Min 4 16 2 8 40 52 64 76 88Y(X10000) C511K02025 [ MS QQQ Chro ] :m /z 502.9 > 8 0.04.571



### 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: WW K-S- WW M-1 ( 0-.2 ) -R E P Instrument ID: LC_LCMS5 Lims B atch ID: 945 8 9 Lims Sample ID: 19 Operator ID: TW /J B Injection V ol: 20.00 ul 3 Ammonium Per

f luorooctanoate (

APFO ), Signal: 1 , m/ z : 413.0 > 36 8 .9 Ty pe: q uant , R T : 4.44 Processing Integration Results R T : 4.43 Response: 251 8 10 Amount: 0.131 8 97

3.97 Min 51 56 61 66 71 76 8 1 8 6 91 96 101 106 111 116 121 126Y(X1000) C511K02025 [ MS QQQ Chro ] :m/ z 413.0 > 36 8 .94.433



### Manual Integration Results R T : 4.43 Response: 275 88 2 Amount: 0.153222

3.97 Min 51 56 61 66 71 76 8 1 8 6 91 96 101 106 111 116 121 126Y(X1000) C511K02025 [ MS QQQ Chro ] :m/ z 413.0 > 36 8 .94.433



### Revie w er: w illiamst , 03-Nov-2011 14:45:00 Audit Action: Manuall y

Integrated Audit Reason: B aseline

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: WW K-S- WW M-1 ( 0-.2 ) -R E P Instrument ID: LC_LCMS5 Lims B atch ID: 945 8 9 Lims Sample ID: 19 Operator ID: TW /J B Injection V ol: 20.00 ul 3 Ammonium Per

f luorooctanoate (

APFO ), Signal: 2 , m/ z : 413.0 > 169.0 Ty pe: q uali f ier , R T : 4.44 Processing Integration Results R T : 4.42 Response: 30674 Amount: 0

2. 8 3. 8 4. 8 Min 41 43 45 47 49 51 53 55 57Y(X1000) C511K02025 [ MS QQQ Chro ] :m/ z 413.0 > 169.04.424



### Manual Integration Results R T : 4.42 Response: 472 8

0 Amount: 0

2. 8 3. 8 4. 8 Min 41 43 45 47 49 51 53 55 57Y(X1000) C511K02025 [ MS QQQ Chro ] :m/ z 413.0 > 169.04.424



### Revie w er: w illiamst , 03-Nov-2011 14:45:00 Audit Action: Manuall y

Integrated Audit Reason: B aseline

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: WW K-S- WW M-1 ( 0-.2 ) -R E P Instrument ID: LC_LCMS5 Lims B atch ID: 945 8 9 Lims Sample ID: 19 Operator ID: TW /J B Injection V ol: 20.00 ul 1 Per f luorooctanoic acid , Signal: 1 , m/ z : 413.0 > 36 8 .9 Ty pe: q uant , R T : 4.44 Processing Integration Results R T : 4.43 Response: 251 8 10 Amount: 0.126234

3.97 Min 51 56 61 66 71 76 8 1 8 6 91 96 101 106 111 116 121 126Y(X1000) C511K02025 [ MS QQQ Chro ] :m/ z 413.0 > 36 8 .94.433



### Manual Integration Results R T : 4.43 Response: 26 8 207 Amount: 0.140194

3.97 Min 51 56 61 66 71 76 8 1 8 6 91 96 101 106 111 116 121 126Y(X1000) C511K02025 [ MS QQQ Chro ] :m/ z 413.0 > 36 8 .94.433



### Revie w er: w illiamst , 03-Nov-2011 14:45:00 Audit Action: Manuall y

Integrated Audit Reason: B aseline

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: WW K-S- WW M-1 ( 0-.2 ) -R E P Instrument ID: LC_LCMS5 Lims B atch ID: 945 8 9 Lims Sample ID: 19 Operator ID: TW /J B Injection V ol: 20.00 ul 1 Per f luorooctanoic acid , Signal: 2 , m/ z : 413.0 > 169.0 Ty pe: q uali f ier , R T : 4.44 Processing Integration Results R T : 4.42 Response: 30674 Amount: 0

2. 8 3. 8 4. 8 Min 41 43 45 47 49 51 53 55 57Y(X1000) C511K02025 [ MS QQQ Chro ] :m/ z 413.0 > 169.04.424



### Manual Integration Results R T : 4.42 Response: 45 8 17 Amount: 0

2. 8 3. 8 4. 8 Min 41 43 45 47 49 51 53 55 57Y(X1000) C511K02025 [ MS QQQ Chro ] :m/ z 413.0 > 169.04.424



### Revie w er: w illiamst , 03-Nov-2011 14:45:00 Audit Action: Manuall y

Integrated Audit Reason: B aseline

Page 181 of 272

### Lab Name: Job No.:
SDG No.:
Instrument ID: Analysis Batch Number: LCMS ANALYSIS RUN LOG

DILUTION FACTOR COLUMN ID DATE ANALYZED LAB SAMPLE ID CLIENT SAMPLE ID LAB FILE 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 Gemini-NX 1 11/02/2011 13:42 STD0002 280-94589/2 IC Gemini-NX 1 11/02/2011 13:49 PC511K02008.d STD0005 280-94589/3 IC Gemini-NX 1 11/02/2011 13:57 PC511K02009.d STD0010 280-94589/4 IC Gemini-NX 1 11/02/2011 14:05 PC511K02010.d STD0020 280-94589/5 IC Gemini-NX 1 11/02/2011 14:13 PC511K02011.d STD0050 280-94589/6 IC Gemini-NX 1 11/02/2011 14:20 PC511K02012.d STD0100 280-94589/7 IC Gemini-NX 1 11/02/2011 14:28 PC511K02013.d STD0200 280-94589/8 IC Gemini-NX 1 11/02/2011 14:36 PC511K02014.d STD0500 280-94589/9 IC Gemini-NX 1 11/02/2011 14:43 PC511K02015.d STD1250 280-94589/10 IC Gemini-NX 1 11/02/2011 14:51 PC511K02016.d CCB 280-94589/11 Gemini-NX 1 11/02/2011 14:59 PC511K02017.d ICV 280-94589/12 Gemini-NX 1 11/02/2011 15:07 PC511K02018.d DLCK 280-94589/13 Gemini-NX 1 11/02/2011 15:14 PC511K02019.d MB 280-94046/1-A Gemini-NX 1 11/02/2011 15:22 PC511K02020.d LCS 280-94046/2-A Gemini-NX 1 11/02/2011 15:30 PC511K02021.d LLCS 280-94046/3-A Gemini-NX 1 11/02/2011 15:38 PC511K02022.d 280-21985-1 WWK-S-WWM-1(0-.2) Gemini-NX 1 11/02/2011 15:45 PC511K02023.d 280-21985-1 MS WWK-S-WWM-1(0-.2) MS Gemini-NX 1 11/02/2011 15:53 PC511K02024.d 280-21985-1 DU WWK-S-WWM-1(0-.2) DU Gemini-NX 1 11/02/2011 16:01 PC511K02025.d CCV 280-94589/20 Gemini-NX 1 11/02/2011 16:09 PC511K02026.d CCB 280-94589/21 Gemini-NX 1 11/02/2011 16:16 PC511K02027.d CCVL 280-94589/22 Gemini-NX 1 11/02/2011 16:24 PC511K02028.d CCVL 280-94589/23 Gemini-NX 1 11/02/2011 16:32 PC511K02029.d CCVL 280-94589/24 Gemini-NX 1 11/02/2011 16:39 PC511K02030.d CCVL 280-94589/25 Gemini-NX 1 11/02/2011 16:47 PC511K02031.d CCV 280-94589/26 Gemini-NX 1 11/02/2011 16:55 PC511K02032.d CCVL 280-94589/27 Gemini-NX 1 11/02/2011 17:03 PC511K02033.d CCV 280-94589/28 Gemini-NX 1 11/02/2011 17:10 PC511K02034.d CCVL 280-94589/29 Gemini-NX 1 11/02/2011 17:18 PC511K02035.d CCVL 280-94589/30 Gemini-NX 1 11/02/2011 17:26 PC511K02036.d



### DV-LC-0012 

### Page 182 of 272

### Lab Name: Job No.:
SDG No.: LCMS BATCH WORKSHEET

280-21985-1

Batch Number: Batch Analyst: Batch Start Date: Batch End Date: Cokley, Cheyana D 11/02/11 10:15 10/31/11 14:40 94046
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 1 mL MB 280-94046/1 PFC leach, DV-LC-0012 10.00 g 50 mL CALC NOT SET TO RUN 1 mL 1 mL LCS 280-94046/2 PFC leach, DV-LC-0012 10.12 g 50 mL CALC NOT SET TO RUN 0.1 mL 1 mL LLCS 280-94046/3 PFC leach, DV-LC-0012 WWK-S-WWM-1(0-.2 ) 10.04 g 50 mL CALC NOT SET TO RUN 1 mL 280-21985-A-1 PFC leach, DV-LC-0012 T WWK-S-WWM-1(0-.2 ) 10.09 g 50 mL CALC NOT SET TO RUN 1 mL 1 mL 280-21985-A-1 MS PFC leach, DV-LC-0012 T WWK-S-WWM-1(0-.2 ) 10.06 g 50 mL CALC NOT SET TO RUN 1 mL 280-21985-A-1 DU PFC leach, DV-LC-0012 T



### Page 1 of 2 DV-LC-0012 

### Page 183 of 272

### Lab Name: Job No.:
SDG No.: LCMS BATCH WORKSHEET

280-21985-1

Batch Number: Batch Analyst: Batch Start Date: Batch End Date: Cokley, Cheyana D 11/02/11 10:15 10/31/11 14:40 94046
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



### Page 2 of 2 DV-LC-0012 

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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.: 280-21985-1 TestAmerica Denver

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

Comments:



### Page 250 of 272

### 9-IN

Instrument ID: NOEQUIP 280-21985-1 Job Number:

Solid Matrix: SDG Number: Lab Name: GENERAL CHEMISTRY

TestAmerica Denver DETECTION LIMITS

11/01/2009 00:00 Method: D 2216 RL Date:

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
07:15 ZZZZZZ 07:15 ZZZZZZ 07:15 ZZZZZZ 07:15 ZZZZZZ 07:15 ZZZZZZ 07:15 ZZZZZZ 1 07:15 X 280-21985-1 T 1 07:15 X 280-21985-1 DU T 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



### 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
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 ZZZZZZ



### 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
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

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 Analyst: Batch Start Date: Batch End Date: Berry III, Paul B 10/26/11 07:15 93110
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 ) 7 1.27 g 17.95 g 13.26 g 280-21985-B-1 D 2216 T WWK-S-WWM-1(0-.2 ) 8 1.27 g 17.95 g 13.09 g 280-21985-B-1 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



### Page 1 of 1 D 2216 

### 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

True Radioactivity either was not measured or, if measured, is at or below background True The cooler's custody seal, if present, is intact. True The cooler or samples do not appear to have been compromised or tampered with. True 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 the COC. True 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 MS/MSDs N/A VOA sample vials do not have headspace or bubble is <6mm (1/4") in diameter. True Multiphasic samples are not present. True Samples do not require splitting or compositing. N/A Residual Chlorine Checked.

TestAmerica Denver 

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