GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

GLP10-01-02: Interim Report 19 - Analysis of PFBS. PFHS. and PFOS in Groundwater 

Samples Collected at the Off-Site BP Property in Decatur. AL in July 2011 

Study Title 

Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and 

Perfluorobutane Sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 

Site-Related Monitoring Program 

Data Requirement 

EPA TSCA Good Laboratory Practice Standards 40 CFR Part 792 

Study Director 

Jaisimha Kesari P.E., DEE 

Weston Solutions, Inc. 

1400 Weston Way 

Westchester, PA 19380 

Phone:610-701-3761 

Author 

Susan Wolf 

3M Environmental Laboratory 

Interim Report Completion Date 

Date of signing 

Performing Laboratory 

3M Environmental Health and Safety Operations 

Environmental Laboratory 

3M Center, BIdg 260-05-N-17 

St. Paul, MN 55144 

Project Identification 

GLP10-01-02-19 

Total Number of Pages 

70 

^•^ 1 ^^ ^ The testing reported herein meet the requirements of ISO/IEC 17025-2005 "General Requirements for the 

'^^ 1 ^^1^.- . Competence of Testing and Calibration Laboratories", in accordance with the A2LA Certificate #2052.01. 

lACCREpiTEPj Testing that complies with this Intemational Standard also operate in accordance with ISO 9001:2000. 

Testing Cert #2052.01 

Page 1 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

This page has been reserved for specific country requirements. 

Page 2 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

GLP COMPLIANCE STATEMENT 

Report Title: Interim Report 19 Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Collected at the Off-Site BP Property in Decatur, AL in July 2011 

Study: Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and 

Perfluorobutane Sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 

Site-Related Monitoring Program. 

This analytical phase was conducted in compliance with Toxic Substances Control Act (TSCA) Good 

Laboratory Practice (GLP) Standards, 40 CFR 792, with the exceptions listed below: 

• These are environmental samples where there is no specific test substance, no specific test 

system and no dosing of a test system. 

• The reference substances have not been characterized under the GLPs and the stability under 

storage conditions at the test site have not been determined under GLPs. 

\ 

Gary HoHenstein/Sponsor Representative Date 

Jaisimha Kesari, P.E., DEE, Study Director Date 

Page 3 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

QUALITY ASSURANCE STATEMENT 

Report Title: Interim Report 19 Analysis of PFBS, PFHS, and PFOS in Groundwater Samples 

Collected at the Off-Site BP Property in Decatur, AL in July 2011 

Study: Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and 

Perfluorobutane Sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur Phase 3 

Site-Related Monitoring Program. 

This analytical phase was audited by the 3M Environmental Laboratory Quality Assurance Unit (QAU), 

as indicated in the following table. The findings were reported to the principal investigator (P.I.), 

laboratory management and study director. 

Inspection Dates 

8/12/11,8/15/11 

L^^viX^.^ 

Phase 

Data / Report 

Date Reported to 

Testing Facility 

Management 

8/23/11 

Study Director 

8/23/11 

. //.r^^C y ^^XS'k 

QAU RepresentdKive Date 

Page 4 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

TABLE OF CONTENTS 

GLP Compliance statement 3 

Quality Assurance Statement 4 

Table of Contents 5 

List of Tables 6 

1 Study Information 7 

2 Summary 8 

3 Introduction 9 

4 Test & Control Substances 9 

5 Reference Substances 10 

6 Test System 11 

7 Method Summary 11 

7.1 Methods 11 

7.2 Sample Collection 12 

7.3 Sample Preparation 12 

7.4 Analysis 12 

8 Analytical Results 13 

8.1 Calibration 13 

8.2 System Suitability 13 

8.3 Limit of Quantitation (LOQ) 13 

8.4 Continuing Calibration 14 

8.5 Blanks 14 

8.6 Lab Control Spikes (LCSs) 14 

8.7 Analytical Method Uncertainty 17 

8.9 Field Matrix Spikes (FMS) 17 

Page 5 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

9 Data Summary and Discussion 17 

10 Conclusion 20 

11 Data/Sample Retention 20 

12 Attachments 20 

13 Signatures 21 

LIST OF TABLES 

Table 1. Summarized PFBS, PFHS, and PFOS Results (BP Groundwater, July 2011) 9 

Table 2. Sample Description Key Code 11 

Table 3. Instmment Parameters 12 

Table 4. Liquid Chromatography Conditions 12 

Table 5. Mass Transitions 13 

Table 6. Limit of Quantitation (LOQ) 14 

Table 7. Laboratory Control Spike Recovery 15 

Table 7 continued. Laboratory Control Spike Recovery 16 

Table 8. Analytical Uncertainty 17 

Table 9. Field Matrix Spike Levels 17 

Table 10. DALGWBPMW47 110713 18 

Table 11. DALGWBPMW121 110713 18 

Table 12. Trip Blank 19 

Table 13. Rinseate Blank 19 

Page 6 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

\1 Study Information 

Sponsor 

3M Company 

Sponsor Representative 

Gary Hohenstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

Study Director 

Jaisimha Kesari, P.E., DEE 

Weston Solutions, Inc. 

Westchester, PA 19380 

Phone:(610)701-3761 

Fax:(610)701-7401 

j.kesari@westonsolutions.com 

Study Location 

Testing Facility 

3M EHS Operations 

3M Environmental Laboratory 

Building 260-5N-17 

St. Paul, MN 55144 

Study Personnel 

William K. Reagen, Ph.D., 3M Laboratory Manager 

Cleston Lange, Ph.D., Principal Analytical Investigator, (clange(a?mmm.com): phone (651)-733-9860 

Susan Wolf, 3M Analyst 

Chelsie Grochow, Analyst 

Kevin Eich, Analyst 

Kelly Ukes, Analyst 

Jonathan Steege, Analyst 

Study Dates 

Study Initiation: March 8,2010 

Interim 19 Experimental Termination: August 3, 2010 

Interim Report Completion: Date of Interim Report Signing 

Location of Archives 

All original raw data and the analytical report have been archived at the 3M Environmental 

Laboratory according to 40 CFR Part 792. The test substance and analytical reference standard 

reserve samples are archived at the 3M Environmental Laboratory according to 40 CFR Part 792 

Page 7 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

\2 Summary 

The 3M Environmental Laboratory received groundwater samples from two different wells located at 

the Off-Site BP Property in Decatur, AL. A total of thirteen sample bottles were received at the 3M 

Environmental Laboratory for perfluorooctane sulfonate (PFOS), perfluorohexane sulfonate (PFHS) 

and perfluorobutane sulfonate (PFBS), and included duplicate groundwater samples from each 

sampling location. Samples also included two field matrix spike (FMS) samples for each location, one 

trip blank set containing Milli-QTM water and appropriate trip blank spikes, and one equipment rinseate 

blank. The equipment rinseate blank did not have a FMS sample prepared for determination of PFBS, 

PFHS, and PFOS recovery. 

The groundwater samples, trip blanks and equipment rinseate blank associated with GLP10-01-02-19 

were received from Weston personnel on July 18,2011. All of the samples were prepared and 

analyzed for PFBS, PFHS, and PFOS following 3M Environmental Laboratory Method ETS-8-044.0 

and conducted under 3M project GLP-10-01-02-19. The average measured PFBS, PFHS, and PFOS 

concentrations are summarized in Table 1. The equipment rinseate and the trip blank sample were 

below the lower limit of quantitation (LLOQ), indicating adequate control of sample contamination 

during shipping and sample collections. The analytical method uncertainties associated with the 

reported results are: PFBS + 10%, PFHS + 11% and PFOS + 29%. 

Page 8 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

Table 1. Summarized PFBS, PFHS, and PFOS Results (BP Groundwater, July 2011). 

Sampling Location 

DAL GWBPMW47 110713 

DALGWBPMW121 110713 

Trip Blanks (Milli-QTM Water) 

GLP10-01-02-19 Equipment rinseate blank: 

DALGWBPMW121 

PFBS 

Avg. Cone. 

(ng/mL) ± RPD 

0.188 ±2.7% 

<0.0250 

<0.0250 

<0.0250 

PFHS 

Avg. Cone. 

(ng/mL) ± RPD 

0.138 ±2.2% 

<0.0250 

<0.0250 

<0.0250 

PFOS 

Avg. Cone. 

(ng/mL) ± RPD 

0.210 ±3.8% 

<0.0400 

<0,0400 

<0.0400 

The analytical method uncertainties associated with the reported results are: PFBS ± 10%, PFHS ± 11 %, and 

PFOS ±29%. 

This analytical study was conducted as part of the Phase 3 Environmental Monitoring and Assessment 

Program for the 3M facility located in Decatur, Alabama. The objective of the overall program is to gain 

information regarding concentrations of perfluorooctane sulfonate (PFOS), perfluorohexane sulfonate 

(PFHS) and perfluorobutane sulfonate (PFBS), in various environmental media such as groundwater, 

soils and sediments that are associated with and near the Decatur facility. This analytical study was 

conducted to analyze groundwater samples collected from two wells located at the off-site BP property 

in Decatur, AL for PFBS, PFHS, and PFOS in an effort to characterize regional groundwater conditions. 

The 3M Environmental Laboratory prepared sample containers (250 mL high-density polyethylene 

bottles) which were shipped to Decatur, AL Weston personnel prior to field sampling. Sample 

containers for each sampling location included a field sample, field sample duplicate, and two field 

matrix spike samples. Each empty container was marked with a "fill to here" line to produce a final 

sample volume of 200 mL. Containers designated for field matrix samples were fortified with an 

appropriate matrix spike solution containing PFBS (linear), PFHS (linear), and PFOS (linear) prior to 

being sent to the field for sample collection. All sample bottles included the addition of ^^02-PFBS, 

^^Ca-PFHS, and ^^Ca-PFOS (internal standard) at a nominal concentration of 1 ng/mL. See section 8.8 

of the report for field matrix spike levels. 

Samples were prepared and analyzed according to the procedure defined in 3M Environmental 

Laboratory method ETS-8-044.0 "Determination of Perfluorinated Compounds In Water by High 

Performance Liquid Chromatography/Mass Spectrometry Direct injection Analysis". The use of internal 

standards was used to aid in the data quality objectives. 

Table 1 summarizes the average PFBS, PFHS, and PFOS concentrations for the duplicate samples 

collected, the trip blank, and aqueous equipment rinseate blank. Tables 10-13 summarize the 

individual sample results and the associated field matrix spike recoveries. All results for the quality 

control samples prepared and analyzed with the samples are reported and discussed elsewhere in this 

report 

fX^ ^ 

A'MTest&JDontmlSubstanceM 

There was not a test substance or control substances in the classic sense of a GLP study. This study 

was purely analytical in nature. 

Page 9 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

5 Reference Substances 

Reference Substance 

Chemical Name 

Chemical Fomriula 

Identifier 

Use 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFHS 

(linear) 

Perfluorohexane sulfonate 

C6F13SO3" 

Sodium Salt 

Target Analyte Reference 

Standard 

Wellington 

04/02/2013 

Frozen 

LPFHXSAM08 

TCR08-0018 

Crystalline 

98% 

t'CJPFHS 

(linear) 

Sodium 

Perfluorohexanesulfonate 

'"Cs^'CsFiaSOaNa" 

CAS#MPFC-C-0511 

Intemal Standard 

Wellington 

05/25/2014 

Frozen 

092310 

TCR11-0016 

Liquid 

5Mg/mL<^' 

Reference Substance 

Chemical Name 

Chemical Fonmula 

Identifier 

Use 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFOS 

(linear) 

Perfluorooctane sulfonate 

CeFiySOa 

Potassium Salt 

CAS #2795-39-3 

Target Analyte Reference 

Standard 

Wellington 

10/18/2013 

Frozen 

LPFOSKBM06 

TCR08-0001 

Crystalline 

98% 

PFOS 

(linear + branclied) 

Perfluorooctane sulfonate 

C8F17SO3" 

Potassium Salt 

CAS #2795-39-3 

LCS Reference Standard 

3M 

12/14/2016 

Frozen 

171 

TCR-696 

White Powder 

86.4% 

r'C J PFOS 

(linear) 

Sodium 

Perfluorooctanesulfbnate 

"CsFiySOa-Na* 

CAS#MPFC-C-0511 

Intemal Standard 

Wellington 

05/25/2014 

Frozen 

092310 

TCR11-0016 

Liquid 

5|jg/mL<^' 

(1) Custom mixture of seven mass-latieled (^^0) periluoroallcylcarboxyllc adds, two mass labeled 

("C) perfluoroalkylsulfonates and one mass-labeled ("C) perfluoro-1-octanesulfonamlde. 

Page 10 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

Reference Substance 

Chemical Name 

Chemical Formula 

Identifier 

Use 

Source 

Expiration Date 

Storage Conditions 

Chemical Lot Number 

TCR Number 

Physical Description 

Purity 

PFBS 

(predominantly linear) 

Perfiuorobutane sulfonate 

C4F9SO3" 

Potassium Salt 

Target Analyte Reference 

Standard 

3M 

01/10/2017 

Frozen 

41-2600-8442-5 

TCR-121 

White Powder 

96.7% 

[1802] PFBS 

(linear) 

f^OJ-Ammonium 

Perfluorobutanesulfbnate 

C4F9S[^^02]0-NH4' 

NA 

Intemal Standaitl 

RTI Intemational 

03/09/2015 

Frozen 

11546-107-2 

TCR-1009, TCR-1031 

Liquid 

>99% 

6 Test System 

The test systems for this study are groundwater samples collected from wells located in Decatur, AL by 

Weston Solutions, Inc. personnel. Samples for this study are "real worid" samples, not dosed with a 

specific lot of test substance. 

Table 2. Sample Description Key Code. 

string Number 

Example 

1 

2 

3 

4 

5 

String Descriptor Example 

DAL GWBPMW470110713 

Sampling Location 

Well ID 

Sampling Point 

Sampling Date 

Sample Type 

DAL = Decatur, Alabama 

GW= Groundwater 

Example: BPMM/47 

110713-July 13,2011 

0=primary sample 

DB=duplicate sample 

LS = low spike 

MS = midspil(e 

HS = higlispil(e 

7 Method Summary 

7.1 Methods 

Analysis for all analytes was completed following 3M Environmental Laboratory method ETS-8-044.0 

"Detemnination of Perfluorinated Compounds In Water by High Perfomnance Liquid 

Chromatography/Mass Spectrometry Direct Injection Analysis". 

Page 11 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

7.2 Sample Collection 

Samples were collected in 250 mL NalgeneTM (high-density polyethylene) bottles prepared at the 3M 

Environmental Laboratory. Sample bottles associated with GLP10-01-02-19 were retumed to the 

laboratory at ambient conditions on July 18, 2011. Samples were stored refrigerated at the laboratory 

after receipt. A set of laboratory prepared Trip Blank and Trip Blank field matrix spikes were sent with 

each cooler of sample collection bottles. 

7.3 Sample Preparation 

Samples were prepared by removing an aliquot of the well mixed sample and placing it in an autovial for 

analysis. 

During the preparation of the laboratory control samples, an aliquot of a separate intemal standard 

spiking solution was added to the laboratory control samples (nominal concentration of 1 ng/mL). The 

samples bottles were spiked with an intemal standard mix at a nominal concentration of 1 ng/mL prior to 

being sent to the field for sample collection 

7.4 Analysi s 

All study samples and quality control samples were analyzed for PFBS, PFHS, and PFOS using high 

perfomnance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS). Detailed instrument 

parameters, the liquid chromatography gradient program, and the specific mass transitions analyzed are 

described in the raw data hard copies placed in the final data packet, and are briefly described below. 

Table 3. Instrument Parameters. 

Instrument Name 

Analytical Method Followed 

Analysis Data 

Liquid Chromatograph 

Guard column 

Analytical column 

Injection Volume 

Mass Spectrometer 

Ion Source 

Electrode 

Polarity 

Software 

ETSKirl( 

ETS-8-044.0 

7/29/11-PFBS and PFHS 

Agilent 1200 

Betasil 018 (4.6 mm X 100 mm), 5n 

Betasil 018 (4.6 mm X 100 mm), 5n 

25 nL 

Applied Biosystems API 5500 

Turtx) Spray 

Turtx) Ion electrode 

Negative 

Analyst 1.5.2 

EJSK\tk 

ETS-8-044.0 

8/2/11-PFOS 

Agilent 1200 

Betasil 018 (4.6 mm X 100 mm), 5n 

Betasil 018 (4.6 mm X 100 mm), 5n 

25 nL 

Applied Biosystems API 5500 

Turtx) Spray 

Turtxj Ion electrode 

Negative 

Analyst 1.5.2 

Table 4. Liquid Chromatography Conditions. 

Step 

Number 

Total Time 

(min) 

Flow Rate 

(ftUmin) 

Percent A 

(2 mM ammonium acetate) 

PercentS 

(Metl)anoO 

ETS-8-044.0 Analyzed 7/29/11 and 8/2/11 

0 

1 

2 

3 

4 

5 

0 

2.0 

14.5 

15.5 

16.5 

20.0 

750 

750 

750 

750 

750 

750 

97.0 

97.0 

5.0 

5.0 

97.0 

97.0 

3.0 

3.0 

95.0 

95.0 

3.0 

3.0 

Page 12 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

Table 5. Mass Transitions. 

Analyte 

PFBS 

PFHS 

PFOS 

Mass Transition 

Q1/Q3 

299/80 

299/99 

399/80 

399/99 

499/80 

499/99 

499/130 

Reference 

Material 

structure 

Linear 

Unear 

Linear 

Intemal Standard 

["O J PFBS 

t^CJPFHS 

["C^PFOS 

Mass Transition 

Q1/Q3 

303m 

402/80 

507/80 

Dwell time was 30 msec for each transition. The individual transitions were summed to produce a "total 

ion chromatogram" (TIC), which was used for quantitation. 

\8 Analytical Results 

BA Calibration 

Samples were analyzed using a stable isotope internal standard calibration curve. Calibration standards 

were prepared by spiking known amounts of the stock solution containing the target analytes into a 

laboratory-prepared synthetic groundwater containing calcium and magnesium. A separate intemal 

standard spiking solution was prepared and an aliquot was added at the same level to all calibration 

standards and laboratory control samples at a nominal concentration of 1 ng/mL. A calibration curve 

ranging from approximately 0.025 ng/mL to 100 ng/mL was prepared. Sample DAL GW BPMW47 was 

quantitated using extemal calibration due to inconsistent intemal standard area counts. 

A quadratic, 1/x weighted, calibration curve of the standard peak area/peak area ratios was used to fit 

the data for each analyte. The data were not forced through zero during the fitting process. Calculating 

the standard concentrations using the peak area/peak area ratios and the resultant calibration curve 

confirmed accuracy of each curve point. 

Each curve point was quantitated using the overall calibration curve and reviewed for accuracy. Method 

calibration accuracy requirements of 100±25% (100±30% for the lowest curve point) were met for all 

analytes. The correlation coefficient (r) was greater than 0.995 for PFBS, PFHS, and PFOS. 

8.2 System Suitability 

A calibration standard was analyzed four times at the beginning of each analytical sequence to 

demonstrate overall system suitability. The acceptance criteria of less than or equal to 5% relative 

standard deviation (RSD) for peak area and retention time criteria of less than or equal to 2% RSD was 

met for PFBS, PFHS, and PFOS. 

8.3 Limit of Quantitation (LOQ) 

The LOQ for this analysis is the lowest non-zero calibration standard in the curve that meets linearity 

and accuracy requirements and for which the area counts or area ratio are at least twice those of the 

appropriate blanks. The LOQ for all analytes can be found in Table 6. 

Page 13 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

Table 6. Limit of Quantitation (LOQ). 

Sampling location 

DAL GWBPMW47 110713 

DALGWBPMW121 110713 

PFBS 

LOQ, ng/mL 

0.0250 

0.0250 

PFHS 

LOQ, ng/mL 

0.0250 

0.0250 

PFOS 

LOQ, ng/mL 

0.100 

0.0400 

8.4 Continuing Calibration 

During the course of each analytical sequence, continuing calibration verification samples (CCVs) were 

analyzed to confirm that the instmment response and the initial calibration curve were still in control. All 

CCVs met method criteria of 100% ± 25% for PFBS, PFHS, and PFOS. 

8.5 Blanks 

Three types of blanks were prepared and analyzed with the samples: solvent blanks, trip blanks, and 

equipment rinseate blanks. Solvent blank results were reviewed and used to evaluate method 

perfomriance to detennine the LOQ for PFBS, PFHS, and PFOS. Trip blanks reflect the shipping and 

sample collection conditons the sample bottles and samples experience. Equipment rinseate blanks 

are aqueous samples that reflect the efficiency of equipment cleaning in the field between different 

sample collections and are proof of no cross contamination of samples from the equipment. 

8.6 Lab Control Spil<es (LCSs) 

Low, mid, and high-level lab control spikes were prepared and analyzed in triplicate with each 

preparation set. LCSs were prepared by spiking known amounts of the analyte into Milli Q water or 

synthetic groundwater to produce the desired concentration. The spiked water samples were then 

prepared and analyzed in the same manner as the samples. The method acceptance criteria, average 

of LCS at each level should be within 100% ± 20% with an RSD <20%. 

7/29/11 Analysis - internal standard calibration: All LCSs met acceptance criteria for PFBS and PFHS. 

7/29/11 Analysis - external standard calibration: All LCSs met acceptance criteria for PFBS and PFHS. 

8/2/11 Analysis - intemal standard calibration: All LCSs met acceptance criteria for PFOS. 

8/2/11 Analysis - extemal standard calibration: The low set of LCS samples for PFOS had an average 

recovery of 122%. The mid and high sets of LCS samples met acceptance criteria for PFOS. 

As the reference material used for quantitation of PFOS is predominantly linear, and the PFOS present 

in the water samples are comprised of both linear and branched isomers, additional LCS samples of 

PFOS (linear and branched) were prepared at three concentrations in triplicate to evaluate the potential 

for analytical bias. 

8/2/11 Analysis - intemal standard calibration: The low, mid, and high linear and branched LCSs had 

average recoveries of 129%, 122%, and 122%. 

8/2/11 Analysis - extemal standard calibration: The low linear and branched LCS set had an average 

recovery of 126%. The mid and high sets of LCS samples met acceptance criteria for PFOS. 

The following calculations were used to generate data in Table 7 for laboratory control spikes. 

Page 14 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

LCS Percent Recovery = 

Calculated Concentration „ 

Spike Concentration 

100% 

LCS% RSD = standard deviation LCS replicates . ^ Q^^^ 

average LCS recovery 

Table 7. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Intemal standard 

calibration 

Analyzed 7/29/11 

Lab ID 

LCS-110726-1 

LCS-110726-2 

LCS-110726-3 

Average ±%RSD 

LCS-110726-4 

LCS-110726-5 

LCS-110726-6 

Average ±%RSD 

LCS-110726-7 

LCS-110726-8 

LCS-110726-9 

Average ±%RSD 

Spiked 

Concentration 

(ng/mL) 

0.199 

0.199 

0.199 

PFBS 

Calculated 

Concentration 

(ng/mL) 

0.215 

0.212 

0.224 

VoRecovery 

108 

107 

113 

109±2.9% 

1.99 

1.99 

1.99 

2.14 

2.02 

2.13 

107 

101 

107 

105% ±3.3% 

19.9 

19.9 

19.9 

21.2 

21.6 

21.6 

106 

108 

108 

107% ±1.1% 

Spiked 

Concentration 

(ng/mL) 

0.199 

0.199 

0.199 

PFHS 

Calculated 

Concentration 

(ng/mL) 

0.217 

0.216 

0.224 

VoRecovery 

109 

108 

112 

110% ±1.9% 

1.99 

1.99 

1.99 

2.20 

2.11 

2.19 

111 

106 

110 

109% ±2.4% 

19.9 

19.9 

19.9 

21.3 

21.9 

21.8 

107 

110 

110 

109% ±1.6% 

ETS-8-044.0 

Extemal standard 

calibration 

Analyzed 7/29/11 

Lab ID 

LCS-110726-1 

LCS-110726-2 

LCS-110726-3 

Average ±%RSD 

LCS-110726-4 

LCS-110726-5 

LCS-110726-6 

Average ±%RSD 

LCS-110726-7 

LCS-110726-8 

LCS-110726-9 

Average ±%RSD 

PFBS 

Spiked 

Concerttration 

(ng/mL) 

0.199 

0.199 

0.199 

Calculated 

Concentration 

(ng/mL) 

0.205 

0.201 

0.218 

VoRecovery 

103 

101 

110 

105 ±4.5% 

1.99 

1.99 

1.99 

2.07 

1.99 

2.11 

104 

100 

106 

103% ±3.1% 

19.9 

19.9 

19.9 

19.8 

20.2 

20.6 

99.7 

101 

104 

102% ±2.2% 

PFHS 

Spiked 

Concerttration 

(ng/mL) 

0.199 

0.199 

0.199 

Calculated 

Concentration 

(ng/mL) 

0.213 

0.208 

0.221 

VoRecovery 

107 

105 

111 

108% ±2.8% 

1.99 

1.99 

1.99 

2.12 

2.02 

2.07 

107 

101 

104 

104% ±2.9% 

19.9 

19.9 

19.9 

21.0 

21.6 

21.8 

105 

109 

109 

108% ±2.1% 

Page 15 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Table 7 continued. Laboratory Control Spike Recovery. 

ETS-8-044.0 

Intemal standard 

calibration 

Analyzed 8/2/11 

Lab ID 

LCS-110726-1 

LCS-110726-2 

LCS-110726-3 

Average ±%RSD 

LCS-110726-4 

LCS-110726-5 

LCS-110726-6 

Average ±%RSD 

LCS-110726-7 

LCS-110726-8 

LCS-110726-9 

Average ±%RSD 

Spiked 

Concentration 

(ng/mL) 

0.199 

0.199 

0.199 

PFOS (linear) 

Calculated 

Concentration 

(ng/mL) 

0.219 

0.211 

0.226 

VoRecovery 

110 

106 

114 

110% ±3.6% 

1.99 

1.99 

1.99 

2.15 

2.04 

2.13 

108 

103 

107 

106% ±2.5% 

19.9 

19.9 

19.9 

21.1 

21.7 

21.4 

106 

109 

107 

107% ±1.4% 

Lab ID 

LCS-110726-10 

LCS-110726-11 

LCS-110726-12 

Average ±%RSD 

LCS-110726-13 

LCS-110726-14 

LCS-110726-15 

Average ±%RSD 

LCS-110726-16 

LCS-110726-17 

LCS-110726-18 

Average ±%RSD 

PFOS (linear+branched) 

Spiked 

Concentration 

(ng/mL) 

0.198 

0.198 

0.198 

Calculated 

Concentration 

(ng/mL) 

0.252 

0.254 

0.264 

VoRecovery 

127 

138 

133 

129% ±2.5%TM 

1.98 

1.98 

1.98 

2.29 

2.39 

2.53 

116 

121 

128 

122% ±5.0%*^' 

19.8 

19.8 

19.8 

23.0 

24.3 

25.3 

116 

123 

128 

122% ±4.9%'^' 

ETS-8-044.0 

Extemal standard 

calibration 

Analyzed 8/2/11 

Lab ID 

LCS-110726-1 

LCS-110726-2 

LCS-110726-3 

Average ±%RSD 

LCS-110726-4 

LCS-110726-5 

LCS-110726-6 

Average ± %RSD 

LCS-110726-7 

LCS-110726-8 

LCS-110726-9 

Average ±%RSD 

PFOS (lineal) 

Spiked 

Concentration 

(ng/mL) 

0.199 

0.199 

0.199 

Calculated 

Concentration 

(ng/mL) 

0.243 

0.241 

0.245 

VoRecovery 

122 

121 

123 

122% ±0.82%TM 

1.99 

1.99 

1.99 

1.99 

2.01 

2.09 

99.9 

101 

105 

102% ±2.6% 

19.9 

19.9 

19.9 

22.7 

21.8 

22.2 

114 

110 

111 

112% ±1.9% 

Lab ID 

LCS-110726-10 

LCS-110726-11 

LCS-110726-12 

Average ±%RSD 

LCS-110726-13 

LCS-110726-14 

LCS-110726-15 

Average ± %RSD 

LCS-110726-16 

LCS-110726-17 

LCS-110726-18 

Average ±%RSD 

PFOS (linear + branched) 

Spiked 

Concentration 

(ng/mL) 

0.198 

0.198 

0.198 

Calculated 

Concentration 

(ng/mL) 

0.246 

0.249 

0.251 

VoRecovery 

124 

126 

127 

126% ±1.2%TM 

1.98 

1.98 

1.98 

1.83 

1.69 

1.95 

92.2 

85.6 

98.4 

92.1% ±7.0% 

19.8 

19.8 

19.8 

17.8 

19.7 

18.2 

90.0 

99.6 

92.1 

93.9% ±54% 

(1) The average recovery did not meet method acceptance criteria of 100% ± 20%. 

Page 16 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

8.7 Analytical Method Uncertainty 

Analytical uncertainty is based on historical QC data that is control charted and used to evaluate 

method accuracy and precision. The method uncertainty is calculated following ETS-12-012.2. The 

standard deviation is calculated for the set of accuracy results (in %) obtained for the QC samples. The 

expanded uncertainty is calculated by multiplying the standard deviation by a factor of 2, which 

con-esponds to a confidence level of 95%. The most recent 50 data points were used to generate the 

method uncertainty values listed in Table 8. The method uncertainty ifor PFOS by ETS-12-012-2 was 

found to be ± 24%, however, since the highest recovery for the LCSs, the low set of branched and 

linear LCS, was 129%, the analytical uncertainty assigned to this study for PFOS will be ± 29%. 

Table 8. Analytical Uncertainty. 

Analyte 

PFBS 

PFHS 

PFOS 

Standard Deviation 

5.15 

5.33 

12.2 

lUettiod Uncertainty 

±10% 

±11% 

±29% 

8.8 Field IVIatrix Spikes (FMS) 

Low, mid, and high field matrix spikes (FMS) were collec:ted at each sampling point to verify that the 

analytical method is applicable to the collected matrix. Field matrix spikes were generated by adding a 

measured volume of field sample to a container spiked by the laboratory with PFBS (linear), PFHS 

(linear), and PFOS (linear) prior to shipping sample containers for sample collection. Field matrix spike 

recoveries within method acceptance criteria of 100±30% confinn that "unknown" components in the 

sample matrix do not significantly interfere with the extraction and analysis of the analytes of interest. 

Field matrix spike concentrations must be 50% of the sample concentration to be considered an 

appropriate field spike. Field matrix spikes are presented in section 9 of this report. 

Table 9. Field Matrix Spike Levels. 

Sampling Location 

MW47 

MW121 

Trip Blank 

Spike Level 

Low 

High 

Low 

High 

Low 

Mid 

Hiqh 

PFBS, ng/mL 

0.250 

1.00 

2.00 

20.0 

0.250 

1.00 

20.0 

PFHS, ng/mL 

0.250 

1.00 

2.00 

20.0 

0.250 

1.00 

20.0 

PFOS, ng/mL 

0.250 

1.00 

2.00 

20.0 

0.250 

1.00 

20.0 

- _ (Sample Concentration of FMS - Average Concentration: Field Sample & Field Sample Dup.) ^ 

Spike Concentraton 

9 Data Summar y and Discussion 

The tables below summarize the sample results and field matrix spike recoveries for the sampling 

locations as well as the Trip Blank and rinseate blank. Results and average values are rounded to 

three significant figures according to EPA rounding rules. Because of rounding, values may vary slightly 

from those listed in the raw data. Field matrix spike recoveries meeting the method acceptance criteria 

of ± 30%, demonstrate that the method was appropriate for the given matrix and their respective 

quantitative ranges. 

Page 17 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Table 10. DAL GW BPMW47 110713 (1) 

3MUMSID 

GLP1OO1-02-19-005 

GLP10-01-02-19-006 

GLP10-01-02-19-007 

GLP10-01-02-19-008 

Description 

DAL GW BPMW47 0 110713 

DAL GW BPMW47 DB 110713 

DAL GW BPMW47 LS 110713 

DAL GW BPMW47 HS 110713 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

0.190 

0.185 

0.435 

1.16 

VoRecovery 

NA 

NA 

99.0 

97.3 

0.188 ng/mL ±2.r/o 

PFHS 

Concentration 

(ng/mL) 

0.139 

0.136 

0.408 

1.13 

VoRecovery 

NA 

NA 

108 

99.3 

0.138 ng/mL±2.r/o 

PFOS 

Concentration 

(ng/mL) 

0.206 

0.214 

0.506 

1.36 

%Recovery 

NA 

NA 

118 

115 

0.210 ng/mL ±3.8% 

NA= Not Applicable 

(1) Results generated using extemal standard calibration. 

Table 11. DAL GW BPMW121 110713 (1) 

3MUMSID 

GLP10-01-02-19-010 

GLP10-01-02-19-011 

GLP10-01-02-19-012 

GLP10^1-02-19-013 

Description 

DALGWBPMW121 0 110713 

DALGWBPMW121 DB 110713 

DALGWBPMW121 LS 110713 

DALGWBPMW121 HS 110713 

Average Concentration (ng/mL) ± VoRPD 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

2.11 

21.7 

VoRecovery 

NA 

NA 

106 

109 

<0.0250 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

<0.0250 

2.22 

21.6 

VoRecovery 

NA 

NA 

111 

108 

<0.0250 

PFOS 

Concentration 

(ng/mL) 

<0.0400 

<0.0400 

2.15 

21.7 

VoRecovery 

NA 

NA 

108 

109 

O.0400 

NA = Not Applicable 

(1) Results generated using Intemal standard calibration. 

Page 18 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

Table 12. Trip Blank (1) 

3MUMSID 

GLP10-01-02-19-001 

GLP10-01-O2-19-002 

GLP1001-02-19-003 

GLP1CM)1-02-19-004 

Description 

DALGWTRIP1 0110713 

DALGWTRIP1 LS 110713 

DALGWTRIP1 MS 110713 

DALGWTRIP1 HS 110713 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

0.263 

1.02 

21.2 

%Recovery 

NA 

105 

102 

106 

PFHS 

Concentration 

(ng/mL) 

<0.0250 

0.268 

1.04 

21.5 

VoRecovery 

NA 

107 

104 

108 

PFOS 

Concentration 

(ng/mL) 

<0.0400 

0.255 

1.02 

20.9 

VoRecovery 

NA 

102 

102 

105 

NA = Not Applicable 

(1) Results generated using intemal standard calibration. 

Table 13. Rinseate Blank (1) 

3MUMSID 

GLP1CW)1-02-19-009 

Description 

DAL GW BPMW121 RS 110713 

PFBS 

Concentration 

(ng/mL) 

<0.0250 

VoRecovery 

NA 

PFHS 

Concerrtration 

(ng/mL) 

<0.0250 

VoRecovery 

NA 

PFOS 

Concentration 

(ng/mL) 

<0.0400 

VoRecovery 

NA 

NA = Not Applicable 

(1) Results generated using intemal standard calibration. 

Page 19 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

10 Conclusion 

Laboratory control spikes and field matrix spikes were used to determine the analytical method 

accuracy and precision for PFBS, PFHS, and PFOS. Analysis was successfully completed following 

3M Environmental Laboratory method ETS-8-044.0 described herein. 

11 Data/Sample Retention 

All remaining samples and associated project data (hardcopy and electronic) will be archived according 

to 3M Environmental Laboratory standard operating procedures. 

12 Attachments 

1 

Attachment A: Protocol Amendment 19 (General Project Outline) 

Attachment B: Representative Chromatograms and Calibration Curves 

Attachment C: Analytical Method 

Attachment D: Method Deviation 

Page 20 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

13 Signatures 

1 ^ 

Date 

2£l) Cleston Lange, Ph.D., 3M Principal Analytical Investigator 

M^^^^^-- ^ Q 'y/fy<!t^^<^oy/ 

William K. Reagen, Ph.D., 3M Environmental Laboratory Department Manager Date 

wiiStM 

\ 

11 

Gary Hohenstein, Sponsor Representative Date 

Jaisimha Kesari, Study Director Date 

Page 21 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

ATTACHMENT A: PROTOCOL AMENDMENT 

Page 22 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

Analytical Protocol: GLP10-01-02 

Amendment 19 

Study Title 

Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and 

Perfluorobutane sulfonate (PFBS) In Groundwater, Soil and Sediment for the 3M 

Decatur Phase 3 Site-Related Monitoring Program 

PROTOCOL AMENDMENT NO. 19 

Amendment Date: 

Julys, 2011 

Performing Laboratory 

3M Environmental, Health, and Safety Operations 

3M Environmental Laboratory 

Building 260-5N-17 

Maplewood, MN 55144-1000 

Laboratory Project Identification 

GLP10-01-02 

Sampling Event 

Decatur Phase 3; Off-Site BP Property 

Page 1 of 7 

Page 23 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

Analytical Protocol: GLPlb-01-02 

Amendment 19 

This amendment modifies the following portion of protocol: 

"Analysis of PFOS, PFHS and PFBS In Groundwater, Soil and Sediment for the 3M 

Decatur Phase 3 Site-Related Monitoring Program" 

PROTOCOL READS: 

No changes to the wording of the protocol are required. 

AMEND TO READ: 

No changes to the wording of the protocol are required. This amendment only addresses and documents 

the addition of the General Project Outline (GPO) for the collection and analysis of groundwater samples 

as part of the 3M Decatur Phase 3 Program for PFOS, PFHS and PFBS (GLP10-01-02). The anticipated 

sample collection will occur around the timeframe of the week of July 11, 2011. The groundwater 

samples for this sampling event will be entered into the 3M Environmental Laboratory LIMS as project 

GLP10-01-02-19 and reported as interim report GLP10-01-02-19, (reflecting study GLP10-01-02 and 

amendment-19), 

Reason; 

The reason for this amendment is to document the General Project Outline (GPO) which describes the 

anticipate groundwater sample collection event for two existing wells located at an off-site location on the 

BP Property. 

The GPO is four pages in length and included as attached to this amendment form. 

Page 2 of 7 

Page 24 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property.-July 2011 

Analytical Protocol: GLP1D-01-02 

Amendment 19 

Amendment Approval 

Gary Hohenstein, Sponsor Representative Date 

^jlZ.}z4l) 

Cleston C. Lange, Principal Analytical Investigator Date 

William Reagen, ErtS Opns Environmental Lab Management Date 

Jaisimha Kesari P.E., DEE, Study Director 

Page 3 of 7 

Page 25 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

Analytical Protocol: GLP10-01-02 

Amendment 19 

To: 

From: 

cc: 

Date: 

Subject: 

Environmental Health & Safety Operations, Environmental Laboratory 

General Project Outline 

Gary Hohenstein, 3M EHS&Opns 

Susan Wolf, 3M EHS&Opns; EnvinDnmental Lab 

William Reagen, 3M EHS&Opns; Environmental Lab 

Cleston Langey, 3M EHS&Opns; Environmental Lab 

Jai Kesari, Weston Solutions 

July 6,2011 

Analysis of Perfluorooctane Sulfonate (PFOS), Perfluorohexane Sulfonate (PFHS) and 

Perfluorobutane sulfonate (PFBS) in Groundwater, Soil and Sediment for the 3M Decatur 

Phase 3 Site-Related Monitoring Program; GLP Interim Report 19 - Decatur Phase 3; OffSite BP Property 

1 General Project Information 

Contacts 

Lab Request Number 

Six Digit Department Number 

Project Schedule/Test Dates 

3M Sponsor Representative 

Gary Hotienstein 

3M EHS Operations 

3M Building 224-5W-03 

Saint Paul, MN 55144-1000 

Phone:(651)737-3570 

aatiohensteinOmmm.com 

3M Environmental Laboratory Management 

William K. Reagen 

2M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9739 

wkreaaen®mmm.com 

Principal Analytical Investigator 

Cleston Lange 

3M EHS Opns, Environmental Laboratory 

260-5N-17 

651 733-9860 

ccl^nqetammm.com 

Sampling Coordinator 

Timothy Frtnak 

Weston Solutions 

Jimpthy.frlnaK(aM9tonsolutions,«im 

Phone: (334)-332-9123 

GLP10-01^2-19 

Dept #530711. Project #0022674449 

Sampling scheduled for the week of July 11, 2011 

All verbal and written correspondence will be directed to Gary Hohenstein. 

Page 4 of 7 

Page 26 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

Analytical Protocol: GLP10-01-02 

Amendment 19 

2 Background Information and Project Objective(s) 

The 3M EHS Operations Laboratory (3M Environmental Lab) will receive and analyze groundwater 

samples collected from two sampling locations for Perfiuorobutanesulfonate (PFBS), 

Perfluorohexanesulfonate (PFHS), and Perfiuorooctanesulfonate (PFOS) from existing wells located on 

the BP property. Analyses will be conducted under the GLP requirements of EPA TSCA Good Laboratory 

Practice Standards 40 CFR 792. 

Groundwater samples will be collected by Weston Solutions personnel the week of July 11, 2011. The 3M 

Environmental Laboratory will prepare the sample bottles with all required spikes to ensure that results for 

PFBS, PFHS, and PFOS are of a known precision and accuracy. The final report will be submitted to Gary 

Hohenstein and Jai Kesari upon completion under interim report GLP10-01-02-19. 

3 Project Schedule 

Sample collection bottles will be prepared by 3M Environmental Laboratory for sampling the week of July 11, 

2011. Sample bottles will be shipped in coolers ovemight to 3M Decatur for anival on Friday, July 8,2011. 

Sample bottles should be stored refrigerated on-site until sample collection. 

Martin Smith \ Weston Trailer 

3M Decatur Plant 

1400 State Docks Road 

Decatur, Alabama 35601 

4 Test Parameters 

The targeted limit of quantitation will be 0.025 ng/mL (ppb) for PFBS, PFHS, and PFOS. 

Two sampling locations have been specified. See attachment A for a list of the sampling locations that will be 

collected for this sampling event For each sampling location, a total of four sample bottles will be collected 

(sample, sample duplicate, low field matrix spike, and high field matrix spike). The "fill to here" line on each 250 

mL Nalgene tsottle will be 200 mL. One set of trip blanks consisting of reagent-grade water as well trip blank 

spikes will be prepared at the 3M Environmental Laboratory and sent to the sampling location with the other 

bottles. All sample bottles will include the addition of ^^Oa-PFBS, ''^OrPFHS. and "Ca-PFOS (intemal 

standard) at a nominal concentration of 1 ng/mL. All sample bottles will also include the addition of ^^C4-PF0S 

(surrogate spike) at a nominal concentration of 0.1 ng/mL One additional bottle will be prepared to be used for 

the preparation of the equipment rinseate blank. A SOOmL bottle of laboratory reagent water will be sent with 

the sample bottles to be used to generate the rinseate blank sample. The table below lists the matrix spike 

levels that will be prepared. 

Well No. 

MW-47 

MW-121 

Trip Blank 

Sample Level 

Low 

Hiflh 

Low 

High 

Low 

Mid 

High 

Spike Cone. (ng/mL) 

0.25 

1.0 

2.0 

20 

0.25 

1.0 

20 

Page 5 of 7 

Page 27 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Slte BP Property.- July 2011 

Analytical Protocol: GLPlb-01-02 

Amendment 19 

Test Methods 

Samples will be prepared and analyzed by LC/MS/MS fblkjwing ETS-8-044.0 "Detemnination of Perfluorinated 

Compounds In Water by High Performance LK|uid Chromatography/Mass Spectrometry Direct Injection 

Analysis". Alternately, samples may b»e analyzed by ETS 8-154.3 "Detemnination of Perfluorinated Acids, 

Alcohols, Amides, and Sulfonates In Water By Solid Phase Extraction and High Perfomnance Liquid 

Chromatography/Mass Spectrometry". 

The data quality objectives for these studies are quantitative results for the target analytes with an analytical 

accuracy of 100±30%. Field matrix spikes not yielding recoveries vinthin 100±30% will be addressed in the 

report and the final accuracy statement may be adjusted accordingly. 

Where applicable, samples will be analyzed against an intemal standard calibration curve. Each curve point will 

contain isotopically-labeled perfluorocarboxylic ackis and perfluorosulfonic acids at a nominal concentration of 1 

ng/mL. The calibration curve will be generated by taking the ratio of the standard peak area counts over ttie 

intemal standard peak area counts to fit the data for each analyte. 

6 Reporting Requirements 

For each sampling location, the report will contain the results for the sample, sample duplicate, and the field 

matrix spikes. Trip blank and trip blank spikes will be reported for the sampling event as will any 

equipment/rinseate blanks prepared in the fieM. Latioratory control spikes of reagent water prepared at the time 

of sample extraction will also be reported and used to evaluate the overall method accuracy and preciston. 

Mettiod blanks of reagent water prepared at the time of sample extraction will be used to determine ttie mettiod 

detection limit. For tiiose sampling locations where ttie field matrix spike level was not appropriate, due to 

higher than expected analyte concentrations, a laboratory matrix spike may be prepared and will be included in 

the final report. 

Page 6 of 7 

Page 28 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-site BP Property - July 2011 

Analytical Protocol: GLP10-01-02 

Amendment 19 

Attachment A 

Bottle request - BP Well Sampling Week of 11 July 2011 Sulfonates levels 

Young, Charles T. 

to cbjacoby2@mmm.com, stwolf@mmm.com, clange@mmm.com 07/05/2011 01:43 PM 

Co „ Frinak, Timothy R.' 

Analyses of sulfonates in the BP well groundwater samples should also be performed under GLPlO-01-02. 

Previously detennined levels of the sulfonates in 601R (close to MW-47) and 601L (close to MW-121) were: 

Sample ID 

DAL-GW-601R-0-

060413 

DAL-GW-601R-0-

070920 

DAL-GW-601L-0-

060413 

DAL-GW-601L-0-

070920 

Sample Date PFBS PFHS PFOS 

13-Apr-06 NR 0.0254 ND 

20-Sep-07 0.0331 0.0585 0.0649 

13-Apr-06 NR 20.8 2.54 

20-Sep-07 2.91 17.4 2.83 

Thanks, 

Charlie 

Charles T. Young 

Technical Director 

Weston Solutions, Inc. 

1400 Weston Way (5-2) 

West Chester, PA 19380 

(610)701-3787 

Fax (610) 701-3401 

Page 7 of 7 

Page 29 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

ATTACHMENT B: REPRESENTATIVE SAMPLE CHROMATOGRAMS AND 

CALIBRATION CURVE(S) 

Page 30 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0729a.rdb 

Data printed by STW 

Printing Time: 9:39:20 AM 

Printing Date: Thursday, August 25, 2011 

Page 1 of 1 

Page 31 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0729a.rdb 

Data printed by STW 

Printing Time: 9:39:35 AM 

Printing Date: Thursday, August 25, 2011 

Page 1 of 1 

Page 32 of 70 
GLP10-01-02; Interim Repoil 19 

Analysis of PFBS. PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0729a.rdb 

I

Sample Name: 1(110729a016r Ssmph ID:'11 003-25-ff' File: 

PMk Name:-13C3PFHS0S)- MaM(e«):"402.000J80.000 DaComment '1.0 ns/mL FC Md In Synth. Wataf Anrwtatlon:" 

Sample Index : 16 

Sample Type: Standar d 

Concentration : 0.94 5 ng/mL 

Calculate d Cone: N/A 

Acq. Date : 7/29/201 1 

Acq. Time: 7:47:0 1 FM 

Hodlfied : No 

Proc . Algorithm: Specif y Pari 

PerceriCage: 50 

"k110729a,»«r 

eter s - MO II I 

Bast . V)in< 

•Split . I 

Report Largest Pe« 

Min, Peak Heigtit: 

Min. Peak Hidth : 

Smoothlr.q Hidth : 

RT Hindow: 

Dipecte d RT: 

: Relai ! RT: 

1 Time: 15-2 

23767 32 coi 

4.076+005 

15. 6 min 

3.4«S 

3.2e5' 

3.0e5' 

2.8*5 

2.6*5 

2.4*5' 

22* 5 

2.0*5 

1.Be5-

1.6*5-

1.4*5-

1.2*5-

1.0*5-

6.0*4 

4.0*4-

2.0*4 

I

SatTpleName:1c110729aO28" San^to ID;'LCS-110726.r Rte:Tc110729a.»«r 

PeakNaine;'13C3PFHS(IS)- Maw(e«):'402.OCXV80.000DaComment -0.2ppb LCS" Anrtotatton: ~ 

Sample Index : 28 

Sample Type : QC 

Concentration : 0,939 ng/mL 

I

Sample Name: "k11072ga02r Sampl* ID: 1 1 005« r Fie:-k110729a.wttT 

Peak Name: '13C3PFHS(IS)" MiM{et>: '4O2.00CVBaox Da' 

Commenl: 'Method BlanlT Annotation: -

Sample Index: 27 

Sample Typ«: Unknown 

Concentration : 0.94 5 nq/mL 4.2*5-

Calculate d Cone: N/A 

Acq. Date : 7/29/201 1 4.0*5-

Acq. Time: 11:39:0 0 PM 

3.8*5 

3.6*5-

3.4*5-

3.2a5-

3.0a5-

2.8*5-

2.6a5-

2.4eS< 

2.2*5 

2.0*5-

1.6*5-

1.6*5-

1.4*5-

1.2*5 

1.0*5-

8.0Me.0a4-

4.0*4-

2.0*4-

Modified : 

Proc . Algorithm: 

Hols e Percentag e 

Vas 

Specif y Pa 

SO 

Base . Sub. Hindov: 1.00 

Peak-Split . Fac t t : 2 

Report Largest Peak: Yes 

Min- Peak Heigh t 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time: 

Area : 26 

Height : 

Star t Time: 

End Time: 

0.00 

0.00 

0 

30. 0 

15.2 

Ho 

Valle y 

IS. 2 

5342 cou 

.25fc*005 

15.1 

15. 5 

Sample Nam*:'k110729a031" SamptelD:*LCS-11072&4- Fie:*V110T2a».wlfr 

Peak Name: *13C3PFHS(IS)- Ma(a(es): '402.000)^.000 Da' 

Comment: '2ppb LCS' Arvwtatkin:" 

Sampli 

- - Type: OC 

ng/mL 

Proc . Algorithm: Sp 

Nois e Percentage : 

Base . Sub. window: 

Peak-Split . Factor: 

Report Largest Peak 

Min. Peak Height : 

Min. Peak Width: 

Smoothing Width: 

RT Hindow: 

Expecte d RT: 

Use Relativ e RT: 

ecif y Pa 

50 

1.00 

2 

: Yes 

0.0 0 

0.00 

0 

30. 0 

15. 2 r 

No 

Int . Type: Valle y 

Retentio n Tims: 

Area : 24722 

Height : 3.E 

Star t Time: 

15. 2 n 

0 COU 

;e*oos 

15.1 n 

Sample Type : 

Concentr a 

Calculate c 

Acq. Date 

Acq. Time 

Modified : 

Proc . Algc 

Hoise Per 

Base . Sub 

Peak-SplI 

Rei>ort La 

Min. Peak 

Min. Peak 

Smoothing 

ion : 

rithm : 

Hindo 

. Fact 

OC 

0.93 8 

N/A 

7/30/201 1 

1:03:29 Wl 

No 

Specif y Pa 

SO 

': 1.00 

o r: 2 

gest Peak: Yes 

Height 

Width: 

rildth : 

Expected RT: 

Use RelatI 

Retentio n 

Area : 

Height : 

Star t Time 

End Time: 

ve RT: 

Time: 

0.00 

0.00 

0 

30. 0 a 

15.2 n 

Ho 

Valle y 

15.2 1 

2450596 cou 

.410*005 c 

1S,1 n 

15. 5 n 

Data printe d by STW 

Printing Time: 9:45:19 AM 

Printin g Date: Thursday, August 25, 

Page 1 of 8 

2011 

Page 33 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS. PFHS. and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0729a.rdb 

V SamplB Name:'V11072«s034" Sample ID:-LCS-110726-7' Fita: VII0729a. 

• Peak Name: "13C3PFHS(IS)- MaM(Ba):'402.00080.000 Da' 

I Comment'20ppbLCS' Annotation:' 

Sample Type : 

Concentration : 

Calculate d Cor 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Hois e Percentage : 

Base . Sub. Mlndot 

Peak-Split . Fact e 

Report Largest Pt 

Kin . Peak Height : 

Min. Peak Width: 

Smoothing Width: 

QC 

0.93( 

N/A 

7/30/2011 

2:06:48 AM 

Specify Par. 

SO 

-: 1.00 

ng/mL 

RT I 

J RT : 

i RT: 

Int . Type : Valle y 

Retentio n Time: 15.2 

Area : 2258109 ct 

Height ; 3.49e-t005 

Star t Time: 15.1 

End Time: 15. 6 

I

Sample Name: 1(110729a05r Sample ID:'OLP1l>O1-02-1&oar File: 

Peak Name: -13C3PFHS(IS)' Mm«(e»): '402.00080.000 DaComment "DALQVWTRIP1 LS 11071T Annotatkm: " 

Sampli 

• - Type: Unknown 

ng/mL 

Sampl* Name: 1(1107288055- S«n^lD:'OLP1M)1<02-1&O0gr Fie: 

PttakName:'13C3PFHS(IS)r Ma*s<««}:-402.00000.000 Da' 

Comm*nt:-DALGWBPMW121RS1107ir Amotatktn:' 

Sample lnde:<: 55 

Sample Type : Unknown 

Concentration : 0.94 5 iig/mL 

Calculate d Cone: H/A 

Acq. Date : 7/30/20 H 

Acq. Time: 9:30:1 2 AM 

Modified : 

Proc . Algorithm: 

Hois e Percentage : 

Base . Sub. Mindow 

Peak-Split . Fact o 

Report Largest Pe 

Min. Peak Height : 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Tine : 

No 

Specif y Pa 

50 

: 1.00 

r : 2 

a k : Ve5 

0.0 0 

0.0 0 

0 

30. 0 

15. 2 n 

No 

Va 1 le y 

15. 2 n 

Area : 2346754 cou 

Height : ; 

Star t Time: 

End Time: 

.96e+005 

15. 0 n 

15.4 Tl 

Sample Name: 1(1107293067 San ^ ID: *OLP1(KlU^ 

Peak Name:-13C3PFHS(tS)" MaM(*«):'402.00O80.0001 

Comment:-DALOWBPMW121D11071T Annotation:'" 

Sample Index : 69 

Sample Type : Unknown 

Concentration : 0.94 5 ng/ml. 

Calculate d Cone: N/A 

Acq. Date : 7/30/301 1 

Acq. Time: 3:25:5 6 PM 

Spiecify Parameter! 

Int . Type: Valle y 

Retentio n Tims: 15.2 

Area : 2191960 coi 

Height : 3.62e+O05 

Star t Time: 15.1 

End Time : 15. 5 

Sample Type : 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Hois6 Percentag * 

Unknown 

0.94 5 r 

N/A 

7/30/201 1 

10:12:2 7 AM 

No 

Specif y Para 

50 

Base . Sub. Window: 1.00 

Peak-Split . Factor: 2 

Report Largest Peak: Yes 

Min. Pe-k Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

0.00 

0.00 

0 

30. 0 se 

I S . 2 m 

Valle y 

15.2 a 

Area : 2589379 coun 

Height : 

Star t Time: 

.12et00 5 cf 

15. 1 mi 

Modi 

Proc 

Sas e 

Peak 

Kin. 

Min. 

led : 

Alg 

Sub 

SplI 

t La 

Peak 

Peak 

Smoothing 

RT Window 

r i t 

Hi Id 

. Fac 

qea 

Hel 

Width 

Wirt 

Expecte d RT: 

Use Rela t 

h 

ve RT 

Data printe d by STW 

Printing Time: 9:45:19 AM 

Printin g Date: Thursday, August 25, 2011 

Page 2 of 8 

Page 34 of 70 
GLP10-01-02: Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0729a.rdb 

I

San*4eName:1(110729aO16' Sampte I0:-1100^-25-ff' Rte:lc110729a. 

P*akNama:'1802PreS(e)" Ma«*<ea):-aos.OOOM.OOO Da' 

Commant-1.0 no/mL FC«U in Synth. VVal*r Amotatton:-

Sample IndeK: 16 

Sample Type: Standar d 

ncentration : 0.97 5 ng/mL 

Iculate d Cone: N/A 

Acq. Date 

Acq. Time 

Modified : 

Proc . Algorithm: 

Kois e Per 

Sase . Sub 

Peak-Spl l 

entag e 

Wlndo 

7/29/2 0 

7 : 47:0 1 

Yes 

Specif y 

. Factor: 

Report Largest Peal 

Mtn. Peak 

Min. Peak 

Smoothing 

RT Window 

Heigh t 

Width: 

Width: 

Elxpected RT: 

Use Rela t 

Int . Type 

Retentio n 

Area : 

Height : 

ve RT: 

Time: 

Ba 

50 

1.1 

2 

: Y0 

0 

30. 0 

13. 7 

No 

s e To 

IS.--

1752298 c 

Star t Time: 

End Timer 

.14e*005 

13. 6 

H . O 

1 

PM 

Pa 

00 

Ba< 

I

Sample Name: I d 10729a02ff' Sampla ID:-LCS-110726-1* i 

PttakName:-1802PFBS(IS)- Ma«»(*«): *303.000/M.000 Da' 

Comm*nt: "0.2ppb LCS' AnfMtatton: ~ 

Sample Index 

I

Sampl*Nam*: 1(1107293027- SamplelD:-1100S«9r- Fl*:1(110729a.wtfr 

P*ak Nam*: -1802PFBsasr Maaa{8a): '3O3,00ai«4.00O Da' 

Comnwnt:'liMhodBlanir Annotatk>n:-

Sample Index : 27 

» Type : Unknown 

ng/mL 

Sample Type : 

Concentration : 

Cal c 

Acq. 

late d Cone 

Date : 

Time: 

Modified ! 

Proc 

Nola 

&aBP 

feak 

Repo 

Min. 

Mtn . 

Algorithm 

Unknown 

0.97 5 

H/A 

7/29/201 1 

ll:39i0 0 P 

Ho 

Specif y Pa 

Percentage : 50 

Sub. Window: 1.00 

Split . Fac 

t Largest 

Peak Heigh 

Peak Hidt h 

hing Midth 

RT Window: 

Expe t a d RT: 

Use Relativ e RT 

Int . 

Rete 

Area 

Type : 

tlo n Time: 

o r : 2 

eak : Yes 

: 0.0 0 

0.0 0 

0 

30. 0 

13.7 

Ho 

Base To Ba 

13.8 

1784 040 cou 

Height : 

Sta r Time : 

End Time: 

2.79e+005 

13, 6 

14. 0 

I

Sanq)tekame:ic11072aa03r Sampla 10: XCS-110^26-4' FI*:'V110729a.wirr 

Peak Name:'1802PFBS(lsr Mata(e*):-3O3.00ar84.0O0 Da' 

Comnwnt: '2ppb LCS' Annotatkin:" 

Sample Type: OC 

Acq. Da Ce : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Nois e Percentag e 

Base . Sub. Wlndo 

Peak-Split . Fact 

7/30/201 1 

12:00:0 4 AM 

No 

Specif y Par 

: 1.00 

r : 2 

Report Largest Peak: Yes 

Hin . Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

L'se Relativ e RT: 

Int . Type: 

Retentio n Time: 

Area : l e 

Height : 

Star t Time: 

End Time: 

0.0 0 

0.0 0 

0 

30. 0 s 

13. 7 m 

No 

valle y 

13.-' m 

7846 coun 

.B3e*005 Cf 

13. 6 m 

13. 9 ml 

ntr a ion : 

Calculate d Cone: 

Acq. 

Acq. 

Modi 

Proc 

Hois 

Base 

Peak 

fie|» 

Min. 

Min. 

Date 

Time 

led : 

Algorithm: 

Percentag e 

Sub 

Spl l 

t La 

Peak 

Peak 

Smoothing 

RT W 

Expe 

ndow 

0.96 8 

H/A 

7/30/201 1 

1:03:29 AM 

Yes 

Specif y Pa 

SO 

Window: 1.00 

. Factor: 2 

gest Peak: Yea 

Heigh t 

width : 

Width: 

t e d RT: 

Use Rela t 

Int . 

Rete r 

Area 

Heig. 

Sta r 

End 1 

Type 

tlo n 

Tim 

ime : 

ve RT: 

Time: 

0.0 0 

0.0 0 

0 

30. 0 

13. 7 n 

No 

Base To Ba. 

13.7 n 

1682968 cour 

.93et00 5 c 

13. 6 1 

14. 1 n 

Data printe d by STW 

Printing Time: 9:45:19 AM 

Printin g Date: Thursday, August 25, 

Page 3 of 

Page 35 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

•ETS-Kirk Results Name: kll0729a.rdb 

r

Sanvh Name:-k11O729a034' SMn;4e ID:'LCS-11072e-7- FUe: I d 1072Sa.wirr 

PeakNaiiM:''ie02PFBS<1S)" HaM<0t):-303.QOCU84.000 Oa' 

ConTMnt 'TOpF^ LCS* Annotation:" 

Simpli • 

Sample Type: 

Concentration : 

Calculate d Cone: 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Nois e Percentag e 

Base . Sub. Wlndo 

Peak-Split . Fa d 

Report Urgss t 1 

Min. Peak Heighl 

Min. Peak Hidth : 

Smoothing Hidth : 

RT Window; 

Expected RT: 

Use Relativt, RT: 

QC 

H/A 

7/30/201 1 

2:06:4 8 AM 

Yes 

Specif y Pa 

: 50 

w: 1.00 

o r : 2 

6ak : Yes 

: 0.0 0 

0.0 0 

0 

30. 0 

13. 7 n 

No 

Int . Type: Base To Basi 

Retentio n Time: 13.7 m; 

Area : 1566717 couni 

Height : 2.47etb0 5 c] 

Star t Time: 13. 6 m: 

End Time: 14. 1 m: 

I

Sampla Name: TrtlOTTSsOSr S«mplB lD:"GlP1(M)l-02-1W)02'"~Rie: 

Peak Hame: 'ie02PFBS((S)" Mata(e«): -303.OOQflM.000 Da' 

Conmienl:-DALGWTRIPlLS1107ir Annotatfen:" 

Sample Index : 57 

Sample Type: Unknown 

L«tlon: 0.97 5 ng/mL 

:«d Cone: N/A 

I

Sample Name:'It110729a05ff' SamptelD:'QLP1<M)l-O2-1Ml0r Fle:1c110729«.wr 

Peak Name: -1802PFBS(IS)- MaM(e«): -303.000/84.000 Da' 

Commw*:"DALGWBPMW121 RS1107ir ArewtaOon:"" 

Sample Inde.x: 55 

Sampl"e TypeType:: Unknown 

Concentration ; 

Calculate d Cone 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm 

Hois e Percentag e 

Unknown 

0.97 5 

N/A 

7/30/201 1 

9:30:1 2 AM 

No 

Specif y Pa 

: 50 

Base . Sub. Mindow: 1.00 

Peak-Split . Fac 

Min. Peak Heigh 

Min. Peak Width 

Smoothing Width 

RT Window: 

Expecte d RT: 

Use Relativ e RT 

Int . Type: 

Retentio n Time: 

o r : 2 

eak : Tea 

: 0.0 0 

0.0 0 

0 

30. 0 

13.7 n 

Ho 

valle y 

13.7 n 

Area : 1623564 cou 

Height : 

Star t Time: 

End Time: 

2.eOet00 5 

13. 6 n 

14-0 n 

13.5 14.0 145 15.0 155 16.0 

SamplBName:-k110729a06?' Sample ID: ^3lJ>1(H)1•02-1»«1ff' Fie: 

PeakName:-1802PFBS(ISr Mata(e«):-303.00084.000 Da' 

Comment: 'DALGW BPMW121 0 lions ' Annotation: -

Sample Index: 69 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Nois e Percentag e 

Base . Sub. Wlndo 

Peak-Split . Fact 

7/30/201 1 

10:12:2 7 AM 

No 

Specif y Parama 

SO 

: 1.00 mi 

r : 2 

Report Largest Peak: Yes 

Min. Pe»k Heigh t 

Min. Peik Width: 

Smoothing Width: 

RT HindoH: 

Expected RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time: 

Area : 17 

Height : 

Star t Time: 

End Time: 

0.0 0 c 

0.0 0 s 

30. 0 se c 

13. 7 min 

Ho 

Base To Base 

13.7 min 

2956 counts 

.BOatOOS ops 

13. 6 min 

14.1 min 

Sample Type : Unknown 

Concentration : 0.97 5 

Calculate d Cone: N/A 

Acq. Date : 7/30/201 1 

Acq. Time: 2:25:5 6 PM 

Modified : Ho 

Proc , Algorithm: Specif y Par 

Nois e Percentage : 50 

Base . Sub. Hindow: 1.00 

Peak-Split . Factor: 2 

ReiMrt Largest Peak: Yes 

Min. Peak Height : 0.0 0 

Min. Peak Width: 0.0 0 

Smooching Width: 0 

RT Window: 30. 0 s 

Expected RT: 13. 7 m 

Use Relativ e RT: No 

ng/mL 

amete 

c p s 

po 

Ln 

Int . Type : Base To Base 

Retentio n Time: 13. 7 m 

Area : 1518689 coun 

Height : 2.49e+005 c 

In 

ps 

Star t Timt: 13. 6 min 

End Time: 14. 1 m In 

Data printe d by STW 

Printing Time: 9:45:19 AM 

Printin g Date : Thursday, August 25, 2011 

Page 4 of 8 

Page 36 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0729a.rdb 

¥^Sanpl8Name:"k110729a0ier Sampto ID:'11 OOMS ^ Fil8:-k110728a.v.ttr 

I Peak Name;'PFBS- M«M{ei):-299.000/80.000 Da.299.00a«9.000 Da' 

I Comment'1.0 nfl/mLFC«td In Synth. Water Arvwtatbn:" 

Sampl. 

Stanc ird 

1.00 

Sample Type : 

Concentr a tio r 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: Sp. 

Hois e Percentage : 

Base . Sub. Window: 

Peak-Split , Factor: 

Report Largest Peak 

Min. Peak Height : 

Min. Peak Width: 

Smoothing Width: 

RT Window: 30. 0 

Expecte d RT: 

Use Relativ e RT: Hi 

SO 

3,7 

Height : 

Star t Time: 

End Time: 

2431425 counts 

4.ne+00 5 cp s 

13. 6 min 

4.0e5 

3.Be5 

3.6e5-

3.4e5 

3J2e5 

3.0e5 

2.6e5 

2.6e5 

2.4e5-

2,2e5 

2.0e5-

1,Sa5-

1.4e5-

1.2e5-

1.0e5-

8.0e4-

6.0e4-

4.0e4-

2.0e4-

I

Sanv^Nsme:1c110729a02Sr Sanqile ID: t,CS-110726-r FUe:-V11072d>.wir 

Pttak Name: -PFBS' MaM<es): "299.000/80.000 Da,299.00Q/!99.DOO Da' 

Comment -0.2ppb LCS- Annotation:" 

Sample Index : 

T

Sampta Name:'V110729a02r Sampla ID:'11 00&«Sr Fie: 1(110729a.wffT 

Peak Name: "PFBS' MaM(e«): "299.000/80^0 Da.299.O0Qm.0O0 Da' 

Comment:'Method BtardT Annotation:-

Sample Inde!<: 27 

Sample Type : Unknown 

Concentration : N/A 1800-

Calculate d Cone: < 0 

Acq, Date : 7/29/2011 ^TQQ. 

Acq. Time: 11:39:0 0 PM 

fy E 

Modified : 1 

c . Algorithm: Spei 

s e Percentage : 90 

Base . Sub. Window: l.i 

Peak-Split . Factor: 2 

Report Largest PeaK: Y< 

Min. Peak Height : 0 

Min. Peak Width: 0 

lOChIng Width: 0 

RT Window: 30. 0 

Expected RT: 13.7 

telati i RT: 

Int . Type : 

Retentio n Time: 

Area : 

Height : 

Star t Time : 

End Time: 

Base To 

13.a 

1099S 

l.eOe'OO 

13.6 

13.9 

1600 

1S00 

1400 

1300 

1200 

1100-

1000 

I

Sam|ileN«me:*k110729aO3l- SaTi«>lelD:1.CS-11072&4- Fte:1c110729a.wir 

Peak Name: -PFBS' HaM(e«): '298.00ai80XXX) Da,299.000/99.000 DaComment *2ppb LCS- Annotation: ~ 

8.0e5' 

7.5e5 

7.0e5 

6.5eS 

6.0e5 

5,5e5 

5.0e5' 

4.5e5 

4.0e5 

3.Se5 

3.0eS' 

2.5e5-

2.0tt5 

1.5a5 

1.0e5' 

5.0e4-

155 16,0 

Sample Type; OC 

Concentration : 0.199 

Calculate d Cone: 0.21 5 

Acq, Date : 7/30/201 1 

Acq. Time: 12:00:0 4 AM 

Modified: No 

Proc . Algorithm: Specif y Par 

Nois e Percentage : 50 

Base . Sub. Window: 1.00 

Peak-Split . Factor: 2 

Report Largest Peak: Yes 

Min. Peak Height : 0.0 0 

Min. Peak Width: 0.0 0 

Smoothing Width: 0 

RT Window: 30. 0 s 

Expecte d RT: 13, 7 m 

Vsc Relativ e RT: Ko 

Int . Type: Base To Bas 

Retentio n Time: 13. 8 m 

Area : 493876 coun 

Height : 7,99o+004 o 

ng/mL 

ng/mL 

amete 

Bin 

n 

Star t Time: 13.6 min 

End Time: 14. 0 m in 

Concentration : 

Calculate d Cone: 

Acq, Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Hois e Percentage : 

Base , Sub. Windov 

1.99 

2.11 

7/30/201 1 

1:03:29 AM 

Vea 

Specif y Par 

SO 

1.00 

Peak-Split . Factor: 2 

Rejiort Largest Peak: Yes 

Min. Peak Height : 

Min. Peak Hidth : 

Smoothing Width: 

RT Window: 

Expecte d RT: 

L'se Relativ e RT: 

Int . Type : 

Retentio n Timt: 

0.0 0 

0.0 0 

0 

ng/mL 

ng/mL 

amete 

min 

30. 0 se c 

13.7 m 

No 

Manual 

13.7 m 

Area : 4732641 coun 

Height : fi 

Star t Time: 

End Time : 

53et005 c 

13.6 ra 

14. 0 m 

Ln 

Ln 

:s 

ps 

In 

in 

0.0-

15.5 16.0 

Data printe d by STW 

Printing Time: 9:45:19 AM 

Printin g Date: Thursday, August 25, 

Page 5 of 

Page 37 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS. PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0729a.rdb 

I

Sarrple Name:'V110729a034- Sample ID: "LCS-110726-r HIa:'Vt10729a.wi(r 

Peak Name:-pros' M«M(e«}:'299.000/BO.OOO Da.299.000im.000 Da' 

Convnai± "ZOppb LCS' Annotation:" 

Sample Index: 34 

Sample Type : 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Nois e Percentag e 

Base . Sub. Wlndo 

Peak-Split . Fact 

Report Largest P 

Min. Peak Heighl 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Inc . Type: 

Retentio n Time: 

QC 

19. 9 ng/mL 

21. 2 ng/mL 

7/30/201 1 

2:06:4 8 AM 

Yes 

Specif y Parameters - MQ II I 

: 50 

w: 1.00 min 

o r : 2 

0.0 0 cps 

0.0 0 se c 

0 points 

30. 0 se c 

13. 7 min 

No 

Manual 

13. 7 min 

Area : 41025637 counts 

Height : 

Star t Time: 

End Time: 

;.19et00 6 cps 

13. 6 min 

14. 1 min 

135 14.0 145 1^.0 1^.5 16.0 

I

Sample Name: •k110T29»05r Samfte ID:-GLP1Wl1,02-1frOOr ^E 7 

Peak Name:'PFBS' Maaa(e«):-299.OOCV80.000 Da,299,00(V99.00a Da' 

Cortwnent-DALGWTRIP1LS1107ir Annotatton:-" 

Sample Index : 57 

I.IOeS1.05e5 

1.00e5-

950e4-

9X0e4-

850e4-

8.0ae4-

750e4-

7.00e4-

6.50e4-

^ S.00e4-

I 55064-

I 

- 5.00M450e4-

4.00e4-

350»4-

3.00e4-

250e4-

2.00e4-

150e4-' 

1.00e4' 

5000.00 

0.00 

I

Sample Name: I d 10729a05?' SamplelO:-OLP1CKl1-02-1&O09' Fle:-k110729a.vi«r 

Peak Name: TFB5- MaM(ee): "299JXXV8DJOOO Da ,299.000^.000 Da' 

Coim)ent-DALGWE1PMWI21RS110713' Amototkm:-

Sample Type : 

Concentration : 

Calculate d Cone 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm 

Nois e Percentag . 

Unknown 

H/A 

< 0 

7/30/2011 

9:30:1 2 AM 

No 

Specif y Pa t 

: 50 

Base . Sub. Window: 1.00 

Peak-Split , Fac o r: 2 

Report Largest Peak: Yes 

Min. Peak Heigh 

Min. Peak Width 

Smooching Width 

RT Hindow: 

Expected RT: 

Use Relativ e RT 

Retentio n Time: 

Area : 

Height : 

Star t Time: 

End Time: 

O.OO 

0.00 

0 

30. 0 s 

13. 7 m 

No 

Ba3« To Bas 

13.7 m 

6969 coun 

1.60et003 c 

13.6 m 

13.9 m 

115 15.0 1^.5 16.0 

I

Sample Nan»:Tc110729a069^ Sampla ID: •OLP1O4J1.02-19O10^ F»a:-k110729a.««r 

Peak Name: -PFBS' Ma(a(ea): -299.00CV80X)00 Da.299,00ara9,000 Da" 

Comm©rt;"DALGWBPMW12101107ir Annotation: * 

Sample Index : 69 

Sample Type: 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Hois e Percentag e 

Unknown 

M/A 

0.2S3 

7/30/:01 1 

10:12:2 7 AM 

No 

Specif y Pa n 

SO 

Base . Sub. Window: 1.00 

Peak-Split . Fact i r : 2 

Report Largest Peak: Yes 

Min. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time: 

0.0 0 

0.0 0 

0 

30. 0 St 

13. 7 m 

No 

Valle y 

13. 7 m 

1.13e+005 cp s 

13. 6 min 

14. 0 min 

S..P1 . Typ.:: 

Concentr a 

Calculat e 

Acq. Dace 

Acq. Time 

Modified : 

Proc , Alg 

Nois e Pe r 

Base . Sub 

Peak-Spl l 

Cone 

rithm 

Unknown 

M/A 

0.0164 

7/30/2011 

2:25:5 6 PM 

Ho 

Specif y Pa 

entage : 50 

Wind w: 1.00 

. Factor: 2 

Reijort Largest Peak: Yes 

Min. Peak 

Min. Peak 

Smoothing 

RT Window 

Height : 0.0 0 

Width 

Width 

Expecte d RT: 

Use Rela t 

int . Type 

Retentio n 

Area : 

Height : 

ve RT 

Time: 

Star t Time: 

End Time: 

0.0 0 

0 

30. 0 

13, 7 

Ho 

Base To Ba 

13.8 

4 5575 cou 

7.67e.00 3 

13.6 

13.9 

1 

i 

7500 

7000 

6500 

6000 

5500 

5000 

4500 

4000 

3500 

3000 

2500 

1500 

1000 

500 

0 

11.47 

L 

1249 

1 to"mT 

.Wwif.Kk 195 16.0 

Data printe d by STW 

Printing Time: 9:45:19 AM 

Printing Date: Thursday, August 25, 

Page 6 of 8 

Page 38 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0729a.rdb 

I

SarrvleName:"k11072da016' Sample ID:'11 00»2&«- File:-k11D729a.wtir 

Peak Name: 'PFHS' Masa{ee): -399.000/99.000 Da.399.00(V80.000 Da' 

Comment "1.0 mini. FC etd In Synth. Watei" Amotatton: ~ 

Sample IndeK: 16 

Sample Type: Standar d 

Concentration : 1.00 ng/mL 

Calculate d Cone: 1.07 ng/mL 

Acq. Date : 7/29/201 1 

Acq, Time: 7:47:0 1 PM 

No 

Bafe 

Algorithm; Sj 

Sub. Window: 

Facte 

Report Largest Peal 

Min. Peak Height: 

Min. Peak Hidth: 

Smoothing Hidth: 

RT Window: 

Expected RT: 

Use Relal 

Height : 

Star t Time 

End Time: 

: RT: 

I

Sample Name:-Ic110729a027- Sample 10:'11 OO&e?' Fle:'K110729a.w»r 

Peak Nante: 'PFHS' Ma««(ea): -399,000/99.000 Da,399.000/80.000 Da' 

Comment: "Method Blanl^ Annotatkin: -

Sample Index: 27 

4^e4-

4.0e4 

3.Se4 

3.6e4-

3,4*4 

3.2e4' 

3,0e4 

2.8e4 

2.6e4 

. 2.4e4 

- 2.2e4 

2.0e4 

1.8e4 

1.6e4 

1.4e4 

1.2e4 

1.0 

8000.0' 

6000.0 

4000.0' 

2000.0 

Sample Type: 

Concentration: 

Calculated Cone: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Noise Percentage 

Base. Sub. Wlndo 

Peak-Split, Fact 

Unknown 

N/A 

< 0 

7/29/2011 

11:39:00 PM 

Yes 

Specify Par 

50 

1.00 

it: 1 

Report Largest Pea>:: Yes 

Min. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relative RT: 

Int. Tvpe: 

Retention Time: 

Area: 

Height: 

Start Time: 

End Time: 

0.00 

0.00 

a 30.0 s 

15.2 m 

No 

Manual 

15.2 m 

3197 coun 

.40et003 c 

15.2 m 

15.t B 

13.0 

i^iii.j,icrwh^iVitfl; tff\i .juAv JiUfOs^eff^j^iiSti^ J A 

SampleNan'«:-k110729a031" SamplelD:"LCS-11072&J- Fle:1c110729a.iMfr 

Peak Nanrte: -PFHS' MaM<e«): "399.000/99.000 Da ,399.000/80.000 Da' 

Comment: '2ppb LCS" Annotatton: "" 

Sample Index : 31 

LOSeeLOOeS9.50eS 

9.00e5' 

8.50eS 

6.00e5 

7.50e5-

7.00e5-

6.50e5 

6,0Oe5-

550eS5X0eS450eS4,00eS3.50eS3.00eS2.50e5-

2.00eS1.50e5-

LOOeS 

5.00e4' 

0.00-

I

Senile Name: •k110729a02ff' Sample ID: "LCS-110726-1- Flle:*k110729a.»«r 

Peak Name: 'PFHS' Maas(e«): -399.00099.000 Da,399.OOa'8aO0O Da' 

Comment "0:2ppb LCS" Annotatkin: "" 

Sample Index: 28 

Sample Type: QC 

Concentration : 0,199 ng/mL 

Calculate d Cone: 0.217 ng/mL 

Acq, Date : 7/30/:01 1 

Acq. Time: 12:00:0 4 AM 

Modified: No 

Proc, Algorithm 

Noise Percentage 

Base. Sub. Windo 

Peak-Split. Fact 

Report Largest 1 

Min. Peak Heigh 

Min. Peak Hidth 

Smoothing Hidth 

RT Window: 

Expected RT: 

Use Relative RT. 

Int. Type: 

Retention Time: 

Area: i 

Height: 

Start Time: 

End Time: 

Specify Pa 

: 50 

rf: 1.00 

or: 1 

eak: Yes 

: 0.00 

0.00 

0 

30.0 

15.2 n 

No 

Valley 

15.2 

15693 cou 

9.70e*004 

15.1 n 

15.4 n 

Sample Type: 

Concentration: 

Calculated Cone: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Noise Percentage 

QC 

1,99 

2.20 

7/30/2011 

ng/mL 

1:03:25 AM 

No 

Specify Paramete 

50 

Base. Sub. Window: 1.00 

Peak-Split. Fact 

Report Largest P 

Min. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Use Relative RT: 

Int. Type: 

Retention Time: 

Area: 60 

Height: 

End Time: 

jr: 1 

•ak: yes 

0.0 

0,0 

0 

30.0 

15.2 

No 

Valley 

15.2 

5595 CO 

.OBetOOo 

15.1 

15.6 

min 

po 

min 

min 

cps 

min 

min 

-^A 

Data printe d by STW 

Printing Time: 9:45:19 AM 

Printin g Date: Thursday, August 25, 2011 

Page 7 of 8 

Page 39 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0729a.rdb 

I

San ^ Nsmo: 1c11072S*034' Swnple 10:-LCS.110726-r Rto: I d lOTZga.wttT 

PMk Name:-f>FHS* Mnt<M): *399.00(y09.000 Oa,3a9.0O{V8OJlOO Da' 

Comnont'TOppt, LCS' 

Sample Index : 

Sample Type: 

Concentration : 

Calculate d Cone : 

Acq. Date : 

Acq. Time: 

Modified: 

Proc . Algorithm: 

Noise Percentag e 

34 

OC 

19. 9 

21, 3 

7/30/2011 

2:06:4 8 A^ 

Ho 

ng/mL 

ng/mL 

Specif y Paramet e 

50 

Base . Sub. Window: 1.00 

Peak-Split , Fac t 

Report Largest P 

Min. Peak Heigh t 

Min. Peak Width : 

Smoothing Width : 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time: 

Area : 4 9 

Height: 

Star t Time: 

End Time: 

r : 1 

a k : Yes 

min 

0.0 0 cp s 

0,0 0 se c 

0 

30. 0 

15.2 

No 

Valle y 

15.2 

47937 c 

.27e+006 

15.1 

15. 6 

po 

s e c 

min 

min 

unts 

c p s 

min 

min 

I

Sample Name;'VI10728a05r Sample 10:-GLP1IM]1.02-194X12" FUa:1 

Peak Name:'PFHS- Uata{e«): "399.00099.000 Oa,399.00(VBaO00 Da' 

Comment-DALOWTRIP1LS1107ir Amotatkm:"' 

Sample Index: 57 

I

SMi^Name:iniO729a0G5' San^le ID: "OLPI04)1-02-1 ^009" Fie:-k110729a.Mfr 

P*ak Name: -pFHS" Masses): -399.000^9.000 Da,399.00Q«0.000 Da' 

Commen(:-DALGWBPMW121RS110717- AmotaUon:-

Sample Index: SS 

Sample Type : 

Concentration : 

Calculate d Cone 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm 

Unknown 

N/A 

< 0 

7/30/2011 

9:30:1 2 AM 

No 

Specif y Pa 

Hoise Percentage : SO 

Base . Sub. Wind 

Peak-Split . Fac 

w: 1.00 

o r : I 

Report Largest Peak: Yes 

Min. Peak Heigh 

Min. Peak Width 

Smoothing Width 

RT Window: 

Expected RT: 

Use Relativ e RT 

int . Type: 

Retentio n Time: 

Area : 

Height : 

Star t Time: 

End Time: 

: 0.0 0 

0.0 0 

0 

30. 0 

15.2 n 

No 

Valle y 

1909 cou 

6.4ee<002 

15.2 n 

15.3 n 

1.2e4 

1.0e4 

8000.0-

G000.0' 

4000.0 

2000.0 

0.0- i.i^'iU'iPuMii^iiiMHiw'i^'wM*** j/\rf^ , _J 

Sample Type: 

ConcentratIon : 

Calculate d Cone: 

Acq. Time: 

Modified: 

Proc . Algorithm: 

Hoise Percentag e 

Unknown 

H/A 

0.268 

7/30/201 1 

10:12:2 7 AM 

Ho 

Specif y Para 

SO 

Base . Sub. Window: 1.00 

Peak-Split . Factor : 1 

Report Largest P 

Min. Peak Heigh t 

Min. Peak Width : 

Smoothing Width : 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time : 

a k : Yes 

0.0 0 

0.0 0 

0 

30. 0 St 

15.2 m 

No 

Valle y 

15.2 m 

Area : 786965 coun 

Height: 

Star t Time: 

End Time: 

.25et00 5 CF 

15. 1 m: 

15.4 ml 

1.25e5 

1.20e5 

1.15e5 

1.10a5 

^JC6»5 

1.00a5 

9.50e4 

9.00e4 

S.50e4 

8.00e4 

7J0e4 

• 7.00e4 

1 e.oo»4 

- 550*4 

5.00*4 

4.50e4 

4.00e4 

3.50e4 

3.00e4 

2.50a4 

2.00e4 

1.50e4 

1.00*4 

5000.00 

0.00 

15 22 

V.f ^ 

17.57 

1 1 

1

Sample Name: i(110729a069^ Sanv)lelb:S3LP1M)1-03-l&O10^ Fie: 

Peak Name: TFHS' MaM(ei):-399.00a«9.000Da,399.00aQO;000 DaComment: -OAL GW BPMW121 01107ir Annotatkin: "• 

Sample Index: 69 

Sample Type: Unknown 

Concentration: N/A 

Calculate d Cone: 0.0179 ng/mL 44e4-

Acq. Date : 7/30/2011 

Acq. Time: 3:25:5 6 PM 4.2*4-

4.0e4 

s - MQ II I 

3.8*4-

3.6*4-

3.2*4 

3.0e4 

Z8e4 

2.6e4 

2.4*4 

2 A 4 

2.0B4 

1.2e4' 

1.0e4' 

8000.0 

6000.0 

4000.0-

2000.0' 

Modified: 

Proc . Alg 

Nol»e Per 

Base . Sub 

Peak-Spli 

Yes 

rithm : Specif y 

Window: 

, Facto r 

Report Largest Pea 

Min. Peak 

Min. Peak 

Smoothing 

RT Window 

Height : 

Width : 

Width : 

Expected RT: 

Use Rela t 

Int . Type 

Rettntlo n 

Height : 

ve RT: 

Time : 

50 

Pa 

1.00 

3 

Y 

0 

0 

30. 0 

15-2 

No 

anua l 

15.2 

577 99 

7 . letOO 

00 

00 

0.0' 

15.21 

1. •jffi>iir*tf;f'rrf*it^r*jt^, 

Data printe d by STW 

Printin g Time: 9:45:20 AM 

Printin g Date : Thursday, August 25, 2011 

Page 8 of 8 

Page 40 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0729a ext.rdb 

kl 10729a ext.rdb (PFBS): "Quadratic" Regression ("1 / x" weighting): y = -1.33e+004 x'>2 •^ 2.33e•^006 x + 1.52e•^004 (r = 0.9998) 

25 30 35 40 45 50 55 

Concentration, ng/mL 

60 65 70 75 85 90 95 100 

Data printed by STW 

Printing Time: 9:41:39 AM 

Printing Date: Thursday, August 25, 2011 

Page 1 of 1 

Page 41 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0729a ext.rdb 

kl 10729a ext.rdb (PFHS): "Quadratic" Regression ("1 / x" weighting): y = -2.44e-^004 x*2 + 2.89e•^006 x + 3.35e-^003 (r = 0.9998) 

45 50 55 

Concentration, ng/mL 

Data printed by STW 

Printing Time: 9:41:55 AM 

Printing Date: Thursday, August 25, 2011 

Page 1 of 1 

Page 42 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0729a ext.rdb 

r

Sanv>leName:-k11O729a0ier Swnple ID: "11 003-2&«- FUs:'V110729a.wtr 

Peak Name: "PFBS- Mat«(ei): *299.000i'80.000 Da ,299.000/99.000 DaConwtMnt -1.0 ng/mL FC «d In Synth. Water Annotation: ~ 

SanpL " • 

'a Type: Standard 

ng/mL 

ng/mL 4.0e5. 

3.Se5-

amet«r, - MO i n ^.SeSmin 3'***" 

3,2e5-

sec 3-0e5-

polnts 

ec 2,8e5 

lin 

2,6eS2.4e5' 

25*5 

2.0e5' 

1.8e5 

1.6e5 

1/»e5-

1.2e5 

1.0e5 

8.De4' 

6.0e4 

4J>e4' 

2.0e4-

Sample Type: 

Concentration: 

Calculated Cone: 

Acq. Time: 

Hodilled: 

Proc. Algorithm: 

Noise Percer.tage 

Base. Sub. Windo' 

Ptafc-Split. Facte 

Report Larg-st P 

Min. Peak Height 

Min. Peak Hidth: 

Smoothing Hidth: 

RT Hindow: 

Expected RT; 

Use Relative RT: 

Int. Type: 

Retention Time: 

Standard 

1.00 

1.0^ 

7/29/2011 

7:*7:01 PM 

Yea 

Specify Pa 

50 

r: 2 

ak: yes 

0,00 

0.00 

0 

30.0 c 

13.7 n 

No 

Manual 

13.7 1 

Area: 2<31019 cour 

Height: 

Start Time: 

End Time: 

.ITe-tOOS c 

13.6 R 

H.O n 

I

Sample Name: •Ml0729a02r Sample ID: *LX»-110726-r Flle:T(1l072e».wtr 

Peak Name: "PFBS* MHa{ea): -29g.00a«ao00 Da.299.000/99.000 Da* 

CommenfOJIppbLCS" Annotation;-

Sample Index: ZS 

I

Sample Name: I d 10729a027" Sample ID: 1 1 OOS«sr Fie: Td 10729a.*wr 

Peak Name: *PFBS' Maaa{ea): -209.00(V80i>00 Da,299.000/99.000 Da' 

Comment:-Method Btantf Annotalkin:" 

ample Index: 27 

Sample Type: Unknown 

Concentration: N/A 

Calculated Cone: < 0 

Modified: No 

Proc. Algorithm: Specify Pari 

se Percentage: 50 

Mtn. Peak Hidth : 

othing Width: 

RT Window: 

Expected RT: 

Height: 

Start Time 

End Time: 

I

Sample Name: iri10729a031- Sample ID:-LCS-11072fr4- Ne:Sd1072da.wttr 

Peak Name: -PFBS' Maas(ee): "299.00080.000 Da.299.00CV99.000 DaComment: ''2ppb LCS- Annotatkin: ~ 

Sample Index 

Sample Type: 

Calculated Cone: 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Noise Percentage 

OC 

0.199 

0,205 

7/30/2011 

ng/mL 

ng/mL 

12:00:0* AM 

No 

Specify Pa 

50 

Base. Sub. Window: 1.00 

Peak-Split. Factor: 2 

Report Largest P 

Kin. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Hindow: 

Expected RT: 

ak: Yes 

0.00 

0.00 

0 

30.0 

13.7 

amete 

c p s 

po 

nln 

Sample Type: QC 

Use Relative RT: No 

Int . Type: Base To Bi 

Retention Time: 13.9 

Area: 0387 6 coi 

Height: 1.99e*0Qt 

Start Time: 13.6 

End Time: H. 0 

Concentration: 

Calculated Cone: 

Acq. Date: 

Acq. Time: 

Modified: 

Proc. Algorithm: 

Noise Percentage 

1.99 

2.07 

7/30/2011 

1:03:29 AM 

Yes 

Specify Pa 

50 

Base. Sub. Window: 1.00 

Peak-Split. Fact r: Z 

Report Largest Peak: Yes 

Min. Pe»k Height 

Min. Peak Width: 

Smoothing Width: 

RT Hindow: 

Expected RT: 

Use Relative RT: 

Retention Timt: 

0.00 

0.00 

0 

30.0 s 

ng/mL 

ng/mL 

amete 

mlr, 

po 

13.7 min 

No 

Manual 

13.7 n in 

8.53e.005 cp3 

Data printe d by STW 

Printin g Time: 9:43:13 AM 

Printin g Date : Thursday, August 25, 2011 

Page 1 of 3 

Page 43 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0729a ext.rd b 

I

Sample Name; 10)107298034^ Sample 10:-LCS-110726-r Flla: 1(1107293. 

Peak Name:'PFBS- Maa^ee):-299.00080,000 Da.299.000iS9.00O Da' 

Comment: "ZOppb LCS- Annotation:" 

Sample Index: 34 

Concentration : 

Calculate d Cone: 

Acq, Date : 

Acq. Time: 

Modified: 

Proc . Algorithm: 

Noise Percentag e 

Base . Sub. Windo 

19. 9 

19.8 

7/30/2011 

2:06:( 8 AM 

Yes 

Specify Pa 

50 

: 1.00 

Peak-Split . Factor : 2 

Report Largest Peak: Yes 

Min. Peak Heigh t 

Min. Peak Hidth : 

Smoothing Hidth : 

RT Window: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time: 

0.0 0 

30. 0 

13.7 

Ho 

Manual 

13.T 

Acta : <10301$0 co 

Height : 

ng/mL 

ng/mL 

min 

c p 3 

po 

nin 

niii 

.19e*006 cp s 

12.5 13.0 13.5 14.0 14.5 15.0 15.5 16.0 

I

Sample Name: 1(1107298061' SaR^ID:-GLi>1M)1-02-19O05- Fle:1c1l0728a.wHr 

Peak Name: -pfBSr Ma««(ea): •SasjOOOOOOOO Da.299.OOaiS9.000 Da' 

Comment: 'DAL GW BPMW47 011071T 

Sample Index: fil 

Sample Type 

ConcentraCI 

Unknown 

an: N/A 

Calculate d Cone: 0.190 

Acq. Date : 

Acq. Time : 

Modified : 

Proc . Algor 

Nois e Perc e 

Base . Sub. 

Peak-Split . 

7/30/20 1 

11:36:5 7 

No 

thm: Specif y 

tage : SO 

ng/mL 

AM 

Parameters 

Window: 1.00 min 

Factor : 2 

Report Largest PeaK: Ve 

Min. Peak K iqht : 0 . 0 CDS 

Min. Peak Width: 0.0 0 se c 

Smoothing Width! 0 

RT Window: 

Expected RT 

Use Rtlatl v 

Retentio n T 

Area : 

Height : 

Star t Time: 

30. 0 

13.7 

RT: Ho 

Valle y 

me: 13.7 

459055 c 

7,68e*004 

13, 5 

MQ II I 

min 

unts 

c p s 

min 

I

Sample Name: idlO729a01Cr Sample ID:-11 003-2&«' Flto:1ri10729a,wir 

Peak Name: 'PFHS' Uaaa{e«): -399.00(Vd9.000 Da.399.00(V80.000 Oa' 

Comment '1.0 ng/mL FC ctd in Synth. Water Annotatk>n: " 

Sample Index: 16 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified: 

Proc . Algorithm: 

Hols e Percentag e 

1.00 

7/:9/201 1 

7:47:0 1 PM 

No 

ng/mL 

ng/mL 

Specif y Paramet e 

50 

Base . Sub. Window: 1.00 

Peak-Split . Factor : 2 

Report Largest Peak: Yes 

Hin. Peak Heigh t 

Min. Peak Hidth : 

Smoothing Hidth : 

RT Hindow: 

Expected RT: 

lisc Relativ e RT: 

Int . Type: 

Retentio n Time: 

O.OC 

O.OC 

0 

30. 0 

15.2 

Ho 

Valle y 

15.2 

Area : 2829353 cou 

Height : 

Star t Time: 

End Time: 

.81e>005 

15.1 

15.5 

min 

po 

min 

cps 

lin 

Bin 

I

Sarrfile Name: 1t110729a02r Sample ID: "11 OOS-S 

Peak Name: TFHS- Mat«{es}:-399,000/99 JUO Da ,31 

Comment:-Method BtanK" AnnotaUon:'-

Sample Index; 27 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Hois e Percentag e 

H/A 

0.002 H ng/m 

7/29/201 1 

11:39:0 0 PM 

Ho 

Specif y Paramet 

50 

Base . Sub. Hindow: 1.00 min 

Peak-Split . Fact s r : 2 

Rei>ort Largest Peak: Yes 

Min. Peak Height 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

Area : 

Height : 

Star t Time : 

End Time: 

0.0 0 c p 

0.0 0 s e 

0 p, 

30. 0 se c 

15,2 min 

No 

Base To Base 

15.2 min 

9516 counts 

.lle+00 3 cps 

15.2 min 

15.1 min 

WJO 163 17.0 17.5 

Data printe d by STW 

Printin g Time: 9:43:13 AM 

Printin g Date: Thursday, August 25, 2011 

Page 2 of 3 

Page 44 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0729a ext.rd b 

I

Sanv>leName:1c110729a02e^ Sample ID:-LCS-11072S-r Rla:1c110729a.vrtrr 

Peak Name: -PFHS- Mae*<e»): -390.00099.000 Da,399.00a«0.000 DaComment -0.2ppb LCS" Annotatkm:" 

Sample Indei;: 26 

Sample Type: OC 

Concentration : 0.199 ng/mL 

Calculated Cone: 0.213 ng/mL 

Acq. Date: 7/30/2011 

Acq. Time: 1Z:00:0( AM 

Modified : 

Proc . Algor 

Noise Perce : 

thm: 

Base . Sub. Wlndo 

Peak-Split . Fac t 

Yes 

Specif y 

50 

P 

-; 1.00 

3r: 2 

Report Largest Peak: Yes 

Min. Peak H. 

Min. Peak H 

Smoothing H 

RT Window: 

Expected RT 

Use Relativ t 

Int . Type : 

Retentio n T 

Area : 

Height : 

Star t Time: 

End Time: 

Igh t 

dth : 

dth : 

HT: 

S 

0 

0 

0 

30.0 

15.2 

Ho 

Manual 

15.2 

6462 

9,70etOO 

15.1 

15.4 

aramet e 

00 cp s 

00 se e 

po 

min 

min 

n t s 

min 

min 

I

Sample Name: 1(110729a034- Sample ID:-LCS-110726-7- Rle:1(110729a.wtr 

Peak Name: "PFHS" MaM(ea): -399.00039.000 Oa,399.00080.000 DaComment -20ppb LCS' Annotatkin: " 

Sample Index: 34 

I

SampleName:1(110729a03r Sample ID:ICS-l 10726-r Fle:1c110729a.wtr 

Peak Name: TFHS' Maea<aa); -399.000/98.000 Da,399.00O80X00 Oa' 

Commenl: -2ppb LCS' Annotatkm; " 

Sample Index: 31 

Sample Type : QC 

Concentration ; 1.99 ng/mL 

Calculated Cone: 2.12 ng/mL 1.05e6' 

Acq. Date: 7/30/2011 

1.00e6' 

g.50e5 

» - MQ 111 

aooes 

8,S0e5 

8.00eS' 

I t s 7.50e5 

7.00e5' 

6,50e5 

j6.00e5 . 

i 530e5 

I 5X0e5 

4,50e5 

4,0OeS' 

3.50e5' 

3.00e5-

2.S0e5 

2.00e5-

150e5-

1.00e5-

5.00»4' 

0.00-

Acq, Time: 

Modified : 

Proc . Algorithm: 

Hois e Percentag e 

1:03:29 AM 

Yes 

Specif y Pa 

50 

Base . Sub. Window: 1.00 

Peak-Split . Factor: 2 

Report Largest Peak: Yes 

Min. Peak Heigh t 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

Area : 60 

Height ; 

Stai t Time: 

End Tiwe : 

0.0 0 

0.0 0 

0 

30. 0 

15.2 

Ho 

Manual 

15.2 1 

5B37 cou 

.08e+006 

15,1 n 

15. 5 n 

A 

Concentration : 

Calculate d Cone : 

Acq. Date : 

Acq. Time: 

Modified: 

Pioc . Algorithm: 

Noise Percentag e 

IS 

21 

7/30 / 

2:06 : 

Ye 

Spec i 

Base . Sub. Window: 

Peak-Split . Fac t r : 

Report Largest Peak: 

Min. Peak Heigh t 

Min. Peak Hidth : 

Smoothing Hidth : 

RT Hindow: 

Expected RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

30. 

15 

No 

Manu 

15 

Area : 49745601 

Height: 

Star t Time : 

End Time: 

.27e+ 

15 

15 

t>c 

9 

0 

ng/mL 

ng/mL 

-Oil 

a 

Y 

•.0 

? . 

0 

0 

0 

1 

2 

a l 

7 

0 

1 

6 

AM 

Paramet e 

00 cp s 

00 se c 

s e c 

min 

min 

min 

min 

I

San^Name:1c110729a061" Sartvi|elD:-OLPlCK)1-O2-1&O05' Fla:' 

Peak Name: TFHS' Mats{e(}: -399.00ar99.000 Da,399.000/80J>00 Oa' 

Comment:-DALGWBPMVM701107ir Annotatton:-

Sample Index: 61 

5.4e4-

5.2a4-

5.0*4-

4.Se4-

4.6*4-

4.4e4-

4.2e4-

4.0e4-

3.8e4-

3.6e4-

3.4e4-

3,2e4-

3.0e4-

Sample Type : 

Concentration : 

Calculate d Cone 

Acq, Date : 

Acq. Time: 

Modified : 

Proc . Algorithm 

Nois e Percentage 

Unknown 

H/A 

0.13 9 ng/mL 

7/30/201 1 

11:36:57 AM 

Yes 

Specif y Paramet e 

Base . Sub. Window: 1.00 min 

Peak-Split . Fac o r : 2 

Reiioct Largest Peak: Yes 

Min. Peak Heigh 

Min. Peak Width 

Smoothing Width 

RT Window: 

Expected RT: 

Use Relativ e RT 

Int . Type : 

Retentio n Time: 

Area : 

Height : 

Star t Time: 

End Time : 

: 0.0 0 cp s 

0.0 0 se c 

0 po 

30. 0 se c 

15,2 min 

No 

Manual 

15. 2 roln 

03161 counts 

5.52e*004 cp s 

15.0 min 

15.J min 

6000.0-

6000.0 

4000.0 

2000.0 

0.0 

15.1 K 

JL ryf^^-N^^^T*-:^^ 

Data printe d by STW 

Printing Time: 9:43:13 AM 

Printin g Date: Thursday, August 25, 2011 

Page 3 of 3 

Page 45 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0802a.rdb 

1 

CO 

1 

(0 

27 J 

26-

25-

24-

23-

22-

21 

20-

19-

18-

17-

16 

15-

14-

13-

12-

11-

10-

9-

8-

7-

6-

5-

4-

3-

2-

1-

0-

12 14 

Analyte Cone. / IS Gone. 

Data printed by STW 

Printing Time: 9:45:52 AM 

Printing Date: Thursday, August 25, 2011 

Page 1 of 1 

Page 46 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0802a.rdb 

I

San^Name:Tc110802«01F Simpto IDi'l l OOMWf Ffc: Tell 0802a. wtT 

PwikNanM:'13CBPFOS-IS0S)- MH(m):-507.000v80.000 Da' 

Coramsnt "I.OnB/mL F=C ttd In Synth. VWnr AmotaUon:" 

O.Se4 

9.0o4 

8,5e4 

8,064 

7,5e4 

Calculate d Cone: 

Acq. Date : 

Acq, Time: 

Modified : 

Proc , Algorithm: 

Min. Peak Heigh t 

Mtn. Peak Hidth : 

Smoothing Hidth : 

RT Window: 

tlxpecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

N/A 

8/2/201 1 

8:38:2 6 PM 

No 

IntelllOu a 

0.0 0 

0.0 0 

0 p< 

30. 0 

16. 2 

No 

Valle y 

16.2 1 

Area : 613900 cou 

Height : 

Star t Time: 

End Time: 

9,77e+004 

15.1 1 

16. 5 r 

7.0g 

4.5«4 

4.0e4' 

3.5»4' 

3.0M 

2.Se4' 

2.0*4 

1.5*4 

1.0»4 

16.0 1&S 

I

Sample Name:'k110B02«025- Sanqda IO:-LCS-110726>1- FUe:1(110802a.Mi«r 

pHkNarM:-13CSPFO&4S0S)' MaM(M):"507.OOtkfSO.OOODaComment-0,2ppb LCS* AnnotatlMi:-

Sample Index: 26 

I Svnpte Name: ncl 10802*024- Sample 10: "11 005-129- FUe:-k110802«. 

I Peak Name:'13CSPFOS4S{IS}- U«u(tta):-507.00080^)00 Da' 

I Comment:-Method Btanir Amotatkm:-

Sample Type : 

Concentration : 

Calculate d Cone 

Acq. Date : 

Acq, Time: 

Modified : 

Proc , Algorithm 

Min. Peak Heigh 

Min. Peak Width 

Smoothing Width 

RT Window: 

Expecte d RT: 

l'se Relativ e RT 

Int . Type : 

Retentio n Time: 

Unknown 

0.96 0 ng/mL 

N/A 

a/2/201 1 

11:27:1 4 PM 

r e s 

IntelllQua n - IQA 11 

: 0.0 0 cp s 

0 points 

30. 0 se c 

16. 2 min 

No 

Base To Base 

16.2 min 

Area : &55709 counts 

Height : 

Star t Time: 

End Time: 

].5<BtO05 cp s 

IS. l min 

16.1 min i 

f 

* 

1.4*5 

1.2*5 

1.1*5 

1.0e5 

a.0e4 

7.0*4 

6.0*4 

3,0e4 

2.0e4 

I

Sample Name: 1(110802*028- Sample ID:'LCS-11072&4' Fle:1 

Peak Name:-13C8PFOS-IS(IS)- M«««(e*):-507,0Oai'8O.00O DaComment •2ppb LCS- Annotatfan:-

Sample Index: 29 

1.15*5 

I.IOeS 

1.05e5 

I.OOeS' 

S.50e4 

9.00*4 

8.50*4 

8,00*4 

7.50*4 

7.00*4 

6.50e4' 

6.00*4 

S.SOM 

5.00*4 

4.50*4 

4.00*4 

3.50*4 • 

3.00*4' 

2.50*4-

2.00*4-

1.S0e4' 

Sample Type : 

Concentration : 

Acq. Date : 

Acq. Time: 

Modided : 

Proc . Algorithm 

Min. Feak Heigh 

Min. Peak Hidt h 

RT Hindow: 

Expected RT: 

Use Relativ e RT 

Int . Type : 

Retentio n Time: 

Area : 

Height : 

Star t Time: 

End Time; 

QC 

0.9S3 ng/mL 

N/A 

e/2/:oi i 

11:16:1 8 PM 

No 

IntelllQua n -

; 0,0 0 cps 

0.0 0 se c 

30. 0 se c 

16.2 min 

Valle y 

16. 2 min 

1.15e*00S cps 

16.4 min 

IQA II 

! 

1.15*5 

1.10*5 

1.05*5 

1J»*5 

8.50»t 

8.00*4 

7.50*4 

6.50*4 

6.00*4 

5.50M 

5.00*4 

4,50*4 

4,00*4 

3,50*4 

3J»*4 

2.50M 

2.00*4 

IJOM 

1.00*4 

5ooaoo 

0.00 J 

Sample Type: 

Concentration : 

Calculate d Cone 

Acq. Timer 

Modified : 

Proc , Algorithm 

Min. Peak Helghi 

Min. Peak Width 

Smoothing Width 

RT Window: 

E:tpected RT: 

Use Relativ e RT 

Int . Type: 

Retentio n Time: 

QC 

0.95 3 

N/A 

8/3/201 1 

12:51:1 6 

Ho 

AM 

IntelllQua n -

: 0.0 0 

0.0 0 

0 

30. 0 

No 

Valle y 

16.2 

cps 

poin 

min 

Acea : 712792 counts 

Height : 

Star t Time: 

End Time: 

i.ieetoos 

16.1 

16.4 

c p s 

min 

16.0 16.3 

1.00*4-

5000.00 

0.00 

16.0 16.5 

Tim*, mtn 

Data printe d by STW 

Printing Time: 9:47:29 AM 

Printin g Date: Thursday, August 25, 2011 

Page 1 of 6 

Page 47 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS. PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0802a.rdb 

I San<)le Name: 1(110802*031- S«mplelD:'LCS-110726-r Ro: Tel 10802a.w«r 

I PaakNama:-13C8PFOS-IS0S>- MaM(««): "507.000/80.000 Da' 

I Convnent '20ppb LCS' 

ntelllQua. 

0.00 I 

0.00 ! 

Acq, Time: 

Min Peak Height 

Min, Peak Width: 

Smoothing Hidth : 

Expected RT: 

Use Relative RT: 

Int , Type: 

14.0 14.5 

I

Sample Name: 1(1108028041- Sample ID: •LCS-110726-13" Rte: I d 10802a.wlfT 

Peak Nam*: -13CSPFOS-IS<IS>- Ma**{e*}: -SO7.00a'80.O0O Da' 

Conment-2ppb LCS ECP Annotation:" 

Sample Index: 42 

se: QC 

1^.5 16.0 165 

Time, min 

I

Sampl* Name: 1(110802a03ff' Sampl* ID: TCS-110726-10^ Rto: Icl 10802*.wMT 

Peak Name:'1X:8PFOS-IS(t5>- Ma««{es):-S07.00(V80M)0 DaComment:-0.2ppb LCS ECP AnooteUon:-

Sample Indent: 39 

Sample Type : QC 

Concentration : 0.95 3 ng/mL 

Calculate d Cone: H/A 

Acq. Date : 8/3/2011 

Acq, Time: 4:22:1 9 AM 

Modified : 

Proc . Algo r 

Min. Peak He 

Min. Peak W 

thm: 

ight : 

dth : 

Smoothing Width: 

RT Window: 

Expected RT 

L'se Relativ e 

Int . Type: 

Retentio n T 

Area : 

Height : 

Star t Time: 

End Time : 

RT: 

62 

9 

Yes 

ntelliOua n 

0.0 0 c 

0.0 0 s 

0 po 

30. 0 s 

16.2 m 

No 

Valle y 

16. 2 m 

360 coun 

66e*004 c 

16.1 m 

Swnple Name: 1c110802a044- Sample ID: 1.CS-110726-16" Fle:1<110802a.»«r 

Peak Name: '13C8PFOS-IS(IS)'' Ma*s(e*): -507.00Q'80.000 Da' 

Comment: "20ppb LCS ECP Annotation:-

Sample Index : 45 

1.10*5-

1.06*5-

1.00e5-

0.50e4-

9.00e4-

8,50e4' 

8.00*4' 

7.50e4 

7.00e4 

6.50e4 

\ 6.00*4 

I 5.50e4' 

= 5.00*4-

4.50*4-

4.00*4-

3.50*4' 

3.00*4 

2.50*4 

2.00*4-

1.50*4 

1.00e4 

5000.00' 

0.00 

Sample Type: 

Concentration : 

Acq. Time: 

Modified : 

Proc . Algorithm 

Min. Peak Heigh 

Min. Peak Hidth 

Smoothing Hidth 

Expecte d RT: 

Use Relativ e RT 

Int . Type: 

Retentio n Time: 

Area : s 

Height : 

Star t Time: 

End Time: 

QC 

0.954 

H/A 

e/3/201 1 

5:26:1 1 Af 

Yes 

IntelliQ u 

: 0,0 0 

0.0 0 

0 

30. 0 

16. 2 

No 

Valle y 

16, 2 

39628 CO 

1.08e+005 

15. 1 

16.4 

Sample Type : 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time : 

Modified : 

Proc . Algorithm: 

Min. Peak Heighr 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

QC 

0.953 ng 

H/A 

a/3/201 1 

6:29:3 0 AK 

Yes 

IntelllQua n -

: 0.00 cp s 

0.00 se c 

0 poi n 

30. 0 se c 

16.2 min 

Ho 

Ease To Base 

16.2 min 

15.5 16.0 16,5 16,0 185 

"nine, mtn 

Data printe d by STW 

Printing Time: 9:47:29 AM 

Printin g Date: Thursday, August 25, 

Page 2 of 6 

Page 48 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0802a.rdb 

1

Sampla Name: Ir110802a05r Sample ID:-GLP1 (Ml-02-1 »• 

Peak Name: *13C8PFOS-IS(lsr M*t^**): *507.00(V80.000 Da* 

Comm*nt:-DALGUVBPUVV121RS110713- AnnotBtton:-

Sample Inde>:: 53 

Sample Type: Unknown 

ng/mL 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified: 

Proc . Algorithm: 

Min. Peak Heigh t 

Min. Peak Midth: 

Smoothing Hidth : 

RT Hindow: 

Expected RT: 

Use Relativ e RT: 

N/A 

e/3/20 1 

9:18:2 5 AM 

Yes 

IntelllQua n -

0,0 0 cp s 

0 poin t 

30. 0 se c 

15. 2 min 

Ho 

Int . Type: Base To 

Retentio n Time: 16. 1 

Area : 1017368 c 

Height : 1.64e*005 

Star t Time: 16. 0 

End Time: 13.4 

Base 

min 

ounts 

cps 

min 

mill 

IQA II 

^ 

1 

1.6*5 

1.5*5 

1.4*5 

1.3*5 

1.2e5 

1.1*5 

1.0e5 

8.0e4 

8.0M 

7.0*4 

6.0*4 

5.0*4 

4.0M 

14.0 14.5 I 

^?J^ 

Sanple Name: Vt 10802*066:' Sampla ID:-OLP1&O1-02-1&«1ff' Fite:1c110802«.vi4r 

Peak Name:-13C8PFOS-IS(IS)- Ma««(e*):-507.00CV8aoaQ Da' 

CoiT¥nefll:'DALOVUBPMVV12101107ir Annotatkm:-

Sample Index: 67 

: lir.known 

ng/mL 

005 

I

Sanv4aName: 1(110802*054- SamplelD:'OLP1(M>1-02.1&O0r Fle:-V110802a.Mtir 

Peak Nam*:-13C8PFOS-IS(tS)" M«**(**):-507.00080.000 DaComment:-DAL GWTRIPI LS 110713" Annotation;-

Sample Index: 55 

Sample Type : Unknown 

Concentration : 0.960 ng/RiL 

Calculated Cone: N/A , 

Acq- Date: 8/3/2011 l.'eo-] 

Acq. Time: 10:00:39 AM 

1.6*5-

1.5*5-

1.4*5-

1.3*5 

1.2*5-

1.1*5-

1.0*5-

ao*4-

8.0*4-

7,0*4-

6.0*4-

5,0*4-

4.0*4-

3.0*4-

2.0*4 

1.0*4-

Kin . Peak Height : 

Min. Peak Width: 0 

Smoothing Width: 0 

RT Window: 30 

Expecte d RT: 1 

Use Relativ e RT: H 

Int . Type: Val 

Retentio n Time: I 

Area : 1144622 

Height : 1.77e 

Star t Time: 16. 0 

End Time: 16,J 

UJO 14,5 

Sample Type: 

Calculate d Cone 

Acq. Date : 

Acq. Time: 

Modified: 

Proc . Algorithm 

Min. Peak Heigh' 

Hin . Peak Hidth 

Smooching Width 

RT Window; 

Expected RT: 

Use Relativ e RT: 

Int . Type: 

Retentio n Time: 

Ur-known 

0.96 0 

H/A 

8/3/201 1 

2:14:0 9 PH 

Yes 

IntelllQu a 

: 0.0 0 

0.0 0 

30. 0 

lS- 2 n 

No 

Valle y 

16. 2 n 

Area : 450215 cour 

Height : 

Star t Time: 

End Time: 

7,93e't004 c 

la. l 1 

16,4 n 

I

&leName:1[110802aOier Sample ID: 1 1 00»-25'«- hle:Sc110802*!«tfr 

Peak Name: TFOS- Ma«*(es): -499.000i«9,000 Da,4a9.00aB0.0OO Oa,4S9.00CV130.000 Da' 

Comment:-l.OnB/mLFC«tdln5ynth.Water- Annotation:-

Sample Index: 17 

1.15e5-

1.10*5-

1.05e5-

1.00e5-

9.50e4' 

9.00e4 

8,50*4-

aXKM7,50*4-

7.00*4 

^ 6.00*4-

I 5.50*4-

5.00*4 

4.50*4-

4.00*4-

3.50*4-

3.00*4-

2.50*4-

2.00*4-

1.50*4-

1.00*4-

5000.00-

0.00-

Sample Type: 

Concentration : 

Calculate d Cone 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm 

Hois e Percentag e 

Base . Sub. Hindo 

Peak-Split , Fa c 

Reiiort Largest 1 

Kin. Peak Heigh' 

Min. Peak Width 

Smoothing Width 

RT Window: 

Expecte d RT: 

Use Relativ e RT 

Int . Type : 

Retentio n Time: 

Standar d 

1,00 r.g/mL 

1.09 ng/mL 

8/2/201 1 

8:38:2 6 PM 

Ho 

Specif y Paramet e 

: 50 

rf: 1.00 min 

o t : 2 

eak : Yea 

: 0.0 0 cp s 

0.0 0 se c 

0 po 

30. 0 se c 

16. 3 min 

No 

Valle y 

16.2 Bin 

Area : 779765 counts 

Height : 

Star t Time: 

End Tim? : 

l,ne»00 5 cp s 

16. 1 min 

16.) min 

Data printe d by STW 

Printing Time: 9:47:29 ftM 

Printin g Date: Thursday, August 25, 2011 

Page 3 of 6 

Page 49 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0802a.rdb 

I S«m|)le Nama:-k11D802a024- Sunpte ID:-11 005-129- Fie: I d 10902a.wW 

} PukNanw:-PFOS- MM*<M):-499.00Q/99.000Oa.499.000/8O.00ODa.499.0(NV13O.00OOaI Coimont-MethodBbnK- Annotation:-

Sample Type: 

Concentration : 

Calculate d Cone: 

Acq. Dste : 

Acq. Time: 

Modi Iled : 

Ptoc , Algorithm: 

Hois e percentag e 

Unknown 

N/A 

0.00540 

e/2/201 1 

11:27:1 4 

Yes 

Specif y 

ng/mL 

PM 

Paramet e 

Base . Sub. Window: 1.00 min 

Peak-Split . Fac t 

Report Largest P 

Min. Peak Heigh t 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

3 r: 2 

a k : Ye 

0. 

0. 

0 

30. 0 

16. 3 

Ho 

Manual 

16. 2 

Area : 22566 c 

Height : 

Star t Time: 

End Time: 

.30e*00 ' 

15. 0 

15. 3 

)0 cp s 

>0 se c 

min 

c p s 

min 

min 

I

SampleName:1<110802a(n8" Sample ID: "LCS-11072&4- File: 1(110802*.»*r 

P««k Name: -PFOS' Mas«<e«): '439.000^.000 Da,499.00a/80.000 Oa,499,00CV130.000 DaComment "2ppb LCS" Anrwtatlon: ~ 

Sample Index: 

I

Sample Name: 1(110802*025- Sample ID:-LCS-110726-r Fle:1c1100a2a.wHr 

Peak Nam*; -pFOS- Mat«(e*): *499.O0Q'g9.O0O Da .499.000/80.000 Da .499iXXV130.000 Da' 

Comment: *0.2ppb LCS- Annotabon: ~ 

Sample Type : 

Concentration : 

Calculate d Cone 

Acq- Date : 

Acq. Time: 

Modified : 

Pcoc . Algorithm 

QC 

0.199 ng/mL 

0.219 ng/mL 

8/2/201 1 

11:18:1 8 PM 

No 

Specif y Parameters - MQ II I 

Nolae Percentage : 50 

Base . Sub. Wind 

Peak-Split . Fac 

w: 1.00 min 

o t : 2 

Report Largest Peak: Yes 

Min. Peak Heigh 

Min. Peak Width 

Smoothing Width 

RT Window: 

Expected RT: 

Use Relativ e RT 

Int . Type : 

Retentio n Time : 

Area : 

Height : 

: 0.00 cp s 

0.00 se c 

0 points 

30. 0 se e 

16.3 iDin 

No 

Valle y 

16.2 min 

79532 counts 

2.93e-t004 cps 

ft 

P 

2.8*4 

2.6*4 

1.8*4 

4000.0 

2000.0 

I

Sample Name: 1(1108O2aO3r Sample ID: TCS-110726-r FB«:1c110e02a.wtfr 

Peak Name: -PFCS- Ma««(**): -498.000/98.000 08.499.000^0.000 Da,499.0oa'130.000 Da' 

Comment-20ppb LCS' Annotation: 

"e Type: QC 

.g/riL 

Sample Type: QC 

Concentration : 

Calculate d Cone: 

Acq, Date : 

Acq. Time: 

Modilled : 

Proc , Algorithm: 

Nois o Percentag e 

1.99 

2.1 5 

8/3/201 1 

12:51:4 5 

No 

Specif y P 

50 

Base . Sub. Window: l.OC 

Peak-Split . Fact r : 2 

Report Largest Peak: Yea 

Min. Peak Height 

Min. Peak Hidth : 

Smoothing Hidth : 

RT Hindow: 

Expecte d RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Tims: 

ng/mL 

ng/mL 

AM 

aramet e 

min 

0.0 0 cp s 

0.00 se c 

0 

30. 0 

16. 3 

No 

Valle y 

16.2 

Area : 1769247 CO 

Height : 

Star t Tine : 

End Time: 

.eOo-fOOS 

16,1 

15.4 

min 

unts 

c p s 

Bin 

min 

2.7*5 

2.Ge5 

23*5 

2.4*5 

2.3«5-

2J*5-

2.1*5-

2.0e5< 

1,9*5-

1Ae5-

1.7*5 

1,6*5-

15*5-

1.4*5-

1.3*5-

1.2*5-

1.1*5-

1.0*5-

9.0M8.0*4-

7.0*4-

6.0e4-

5.0*4-

4.0e4-

3.0*4-

2.0*4-

1.0*4-

Sample Type : 

Concentration : 

Calculate d Cone: 

Acq, Date : 

Acq, Time: 

Modified: 

Ptoc , Algorithm: 

Nois e Percentag e 

QC 

19.9 

21. 1 

8/3/201 1 

1:51:58 AM 

No 

Specif y Pa 

50 

Base . Sub. window: 1.00 

Peak-Split . Fac t 

Rejjort Largest P 

Min. Peak Heigh t 

Min. Peak Width: 

Smoisthing Width: 

Expected RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

a r: 2 

:ak: Yes 

0.00 

0.00 

0 

No 

Valle y 

16.2 1 

Area : 22570284 co 

Height : 

Star t Tine : 

End Time: 

.I9e-f005 c 

16.1 n 

IS. 5 E 

- MQ 111 

= 

t 

1 

3.4*6 

3.2*6 

3.0*6 

2.8*6 

2,6*6 

2.4*6 

2,2*6 

2.0*6 

1.8*6 

1.6*6 

1.4*6 

1.2*6 

1.0*6 

8.0*5 

6.0*5 

15.5 16.0 165 17.0 17,5 16.0 18J 

Data printed by STW 

Printing Time: 9:47:29 AM 

Printin g Date: Thursday, August 25, 

Page 4 of 6 

Page 50 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

*ETS-Kirk Results Name: kll0802a.rdb 

T Sampl* Name: 1<110802a038f Sample ID:-LCS-110726-10' Fl*: 1c110802a.v«flr 

I Peak Name:-PFOS- Ma*s(e«):-499.00(V99.000Da.499.00ai'BO.OOODa.499.000/13aooODaI Comment ^.2ppb LCS ECF AmotaUon: " 

Sample Inde>:: 39 

Sample Type: QC 

Concentration: 0.198 ng/mL 

Calculated Cone: 0,252 ng/mL 

Acq. Date: 8/3/2011 

Acq. Tlnre: 1:22:49 AM 

Proc . Algorithm: Specif y Parameters - MQ II I 

Hols e Percentage : 50 

Base, Sub. Hindow: 1.00 min 

Report Largest Peak: 

Min. Peak Height : 

Min. Peak VJidth: 

Smoothing Vlldth: 

RT Window: 30 

Expecte d RT: 1 

Vif, Relativ e RT: N 

Int . Type : Man 

Retentio n Time: 1 

Area : 184609 

Height : l,e6 e 

Yes 

0,0 0 

0,0 0 

0 

0 

, 3 

a l 

.2 

004 

I

Sample Name: 1(110802aO44- Sample ID:*LCS-110726-16^ Fl*:1(110e02«.viir 

P«ak Name: -PFOS' Mat«(e«): -4a9.00(V&9.000 Da,499.00af80.000 Da,499.000/130.000 DaComment-20ppb LCS ECP Annotatkm:'^ 

Sample Index : 15 

Sample Type : QC 

Concentration : 19. 8 ng/mL 

Calculate d Cone: 23. 0 ng/mL 

Acq. Date : 8/3/201 1 

Acq. Time : 6:29:3 0 AM 

I Sample Nam*: VI10802a041- Sample ID: 1.CS-110726-1 r Fie: 1(110802a.MMT 

Peek Name: TFOS- MM«(**):-499J10ai99.000Da.499.00aQaOOOD*,499.00a/130.000Da' 

I Commw* •2ppb LCS ECF- Annolatkxi:" 

1.5*5 

1.4*5 

1.3*5-

1,2*5-

1,1*5 

1.0*5-

9.0*4-

8.0*4-

7.0*4-

Sample Index : 12 

Sample Type : OC 

Concentration : 1.98 

Calculate d Cone: 2.29 

Acq. Date : 8/3/201 1 

Acq. Time : 5:26:1 1 AM 

Modified : Yes 

Proc . Algorithm: Specif y Pa r 

Nois e Percentage : 50 

Base . Sub. Window: 1.00 

Peak-Split . Factor: 2 

Report Largest Peak: Ves 

Min. Peak Height : 0.0 0 

Mtn. Peak Width: 0.0 0 

Smoothing Width: 0 

RT Window: 30. 0 s 

Expecte d RT: 16.3 m 

Use Relativ e RT: No 

Int . Type : Manual 

Retentio n Time: 16.2 m 

Area : 1620995 coun 

Height : 1.74e*005 c 

iq/mL 

ig/mL 

min 

c p s 

s e c 

po 

in 

in 

ps 

UJO us 15.5 16J) 16,5 1^0 175 18.0 18.5 

Modified : Yes 

Proc , Algorithm: Specif y Par; 

itags: 50 

Bast lindoh 

Peak-Spl i 

Report Largest Peak: 

Min. Peak Height : 

Min. Peak Hidth : 

Smoothing Hidth : 

RT Hindov : 30, 0 

Expecte d RT: 

L'se Relativ e RT: Ni 

Int . Type : Mam 

6. 3 

17355578 counts 

1.70e*0O6 cp s 

15, e min 

15. 5 min 

1.7*6 

1.6*6-

1,Se6 

1,4*6 

1.3*8-

1.2*6 

1.1*6-

1.0*6-

9.0*5-

8.0*5-

7.0*5-

6.0*5-

5.0*5-

4J)eS3.0e5-

2.0*5-

I

SarMiNamaTvTlMC ^ 

P«ak Nam*: -PFOS' MMs(es): -499.000/99.000 Da,499.00QnO.OOO Oa ,499.000^30.000 DaComment*DALOWBPIyIW121 RS1107ir Armotafion:" 

Sample Index : 53 

Sample Type : 

N/A 

Calculate d Cone: 

Acq. Date : 

Acq. Time: . 

Modified : 

Proc , Algorithm: 

Noise Percentag e 

Base . Sub . Windc 

Peak-Split . Fac t 

<- 0 

8/3/20 1 

9:18:2 5 

Yes 

Specif y 

50 

AM 

Parame t 

i: 1.00 min 

o r: 2 

Retort Largest Peak: Y 

Min. Peak Heigh t 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expecte d RT: 

Van Relativ e RT: 

Retentio n Time: 

Area : 

Height : 

Star t Time: 

End Time : 

0 

D 

0 

30. 0 

16. 3 

No 

Manual 

16.0 

7265 

l.66e*00 

15,9 

16.2 

00 cp 

00 s e 

P" 

s e c 

min 

min 

min 

min 

2800 

15.0 153 18.0 165 17.0 17.5 18.0 185 

Data printe d by STW 

Printing Time: 9:47:29 AM 

Printin g Date: Thursday, August 25, 2011 

Page 5 of 6 

Page 51 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0802a.rdb 

Name:1(110802a054" SwnplB ID:"QIP1(W)1-02-1W>02- File:! 

P»ak Nam*: 'PFOS' hU«»(a«): '439.00099.000 Da,499.000fSO.OOO Da.4S 

Coimwnt-DALGWTRIPILS 110717 Arvwtalion: "" 

Sample Index: 55 

5.0*4-

4.8*4-

4.0*4-

4.4*4-

4.2*4-

4.0*4-

3.8*4-

3.6e4-

3.4*4-

3.2*4-

3.0*4-

2,8*4-

2,6*4-

2,4*4-

2.2*4-

2,0*4-

1J*4-

1,6*41 

Sample Type : 

Concentration : 

Calculate d Cone 

Acq. Date : 

Acq. Time: 

Modified: 

Proc . Algorithm 

Hois e Porcentagr 

Base . Sub. Hindo 

Peak-Split . Fa c 

Report Largest 1 

Min. Peak Heigh 

Min. Peak Hidt h 

Smoothing Width 

KT Window: 

Expected RT: 

Use Relativ e RT 

Int . Type: 

Retentio n Time: 

Unknown 

0.25 5 ng/mL 

8/3/201 1 

10:00:3 9 AM 

No 

Specif y Paramet e 

: 50 

><: 1.00 min 

o r: 2 

eak: Yes 

0.00 cps 

0.0 0 fe e 

0 po 

30. 0 se c 

IS. 3 min 

No 

Valle y 

15. 2 min 

Area : 339150 counts 

Height : 

Star t Time: 

End Time: 

5.13e-f004 cp s 

1&-1 min 

15. 3 min 

4000.0-

2000.0-

..-T««ilDMt 

Sample Name: 1(110e02a066r Sample ID: ^3LP1OO1-02-1&O10' n*:-k1108D2a.wifrr 

P*ak Name: TFOS' M«**(**); '499.00098.000 D«,499.000/BO.OOO D*.499.000/130.000 D*-

Commeot:*DALGVWBPUWt21 0110713^ Awiotatton:-

Sample Index : 67 

Sample Type : Unknown 

Concentration : N/A 

Calculate d Cone: 0.0237 ng/mL 

Acq. Date : 6/3/2011 

Acq. Time: 2:11:0 9 PM 

Percenta l 

;ub. Mint 

Nols. 50 

Base 

Peak-Split . Factor : 

Report Largest Peak 

Min. Peak Height : 

Min. Peak Hidth : 

Smoothing Width : 

RT Window: 30.0 

Expected RT: 16.3 

0.0 0 cp s 

0.0 0 se e 

; Relal 

Int . Tvpe : 

Retentio n 1 

. RT: No 

16.2 

19655 . 

2800 

2600 

2400-

2200 

2000 

1800 

I 1600-

f 

I 1400 

1200' 

14.0 14.5 15.0 II 

Data printe d by STW 

Printin g Time: 9:47:29 AM 

Printin g Date: Thursday, August 25, 2011 

Page 6 of 6 

Page 52 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0802a ext.rdb 

kl 10802a ext.rdb (PFOS): "Quadratic" Regression ("1 / x" weighting): y = 4.17e-H003 x^a -^ 9.02e-H005 x -K -4.02e-H004 (r = 0.9972) 

9.0 10.0 11.0 12.0 13.0 14.0 15.0 16.0 17.0 18.0 19.0 20.0 21.0 22.0 23.0 24.0 25.0 

Concentration, ng/mL 

Data printed by STW 

Printing Time: 9:48:23 AM 

Printing Date: Thursday, August 25, 2011 

Page 1 of 1 

Page 53 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

*ETS-Kirk Results Name: kll0802a ext.rd b 

I

Single Name: 1(110e02aOier Sample ID: "11 003^5 ^ FUe:*V110802a.<Mrr 

PMk Name: 'PFOS' Mna(et): "499.000/99.000 Da,499.00(VSO.OO0 Da,499.000^30.000 Da' 

Connent '1.0 ng/mL FC ttd In Synlh. VMaT Annotation: ~ 

Sample Index: 17 

Sample Type: Standard 

- ^^^^ 

1.10eS< 

1.05*5 

I " 1.00e5-

9.50M 

9.00M 

e.50M' 

8.00*4 

7.50M7.00*4-

I »^-

^ 6.00*4-

I 5.50*4-

5.00*4 

4.50*4< 

4.00*4 

3.5064-

3.00*4 

2.50M 

2.00M 

1J0*4 

1.00*4 

5000.00 

0.00 

Concftntration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time : 

Modified : 

Proc , Algorithm: 

Kois e Percentag e 

1.00 

0.906 

8/2/20 1 

8:38:2 6 

No 

Specif y 

SO 

ng/mL 

ng/mL 

PM 

Pacamete 

Base . Sub . Vllndow: 1.00 min 

Pealt~split . Tact-: 

Repott Largest P« 

Min. Peak Heigh t 

Min. Peak Hidth : 

Smoothing Hidth : 

RT Hindow: 

Expecte d RT: 

Use Relativ e RT: 

int . Type : 

Retentio n Time: 

i : 2 

a t : Ye 

0 

30. 0 

16.3 

No 

Valle y 

16. 2 

Area : 779765 c 

Height : 

Star t Time: 

End Time: 

.176*005 

16.1 

16.4 

00 cp s 

30 se c 

s e c 

min 

min 

min 

min 

14.0 145 

I

Sampte Name: 1(110802*024' S«mpto 10:11 005-129- File: TcllOaoaa.wtfr 

Peak H«me: TFOS" Ma*s(a«): -499.000/99.000 Da,499.000^0.000 Da,499.000/130.000 Da' 

Commenl:-Method Btamr Annotation:" 

Sample Index : 25 

Sample Type : Unknown 

Concentration : H/A 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified : 

Proc . Algorithm: 

Nois e Percentage : 

Base- Sub. Hindo* 

Peah-Spllt . Fact o 

0.0687 

i/2/20 1 

11:27: H 

Yes 

Specif y 

50 

PM 

Par 

1.00 

i : 2 

Report Largest Peak: Ye 

Min. Peak Height : 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

0 

0 

0 

30. 0 

16. 3 

No 

Manual 

16.2 

Area : 21851 c 

Height : 2 

Star t Time: 

End Time: 

286-^00: 

16.3 

JO 

• » ) 

m 

ig/mL 

meters 

mlr. 

e p s 

poin t 

n 

m 

n 

n 

I

S«npteName:T(110802B025" Sample ID: •LCS-110726-1- Ble:*V110802a.w«r 

Peak Name: -PFOS* Mns(e*]: '499.000/99.000 Da,499.CO0/8O.DO0 Da,499.000^30.000 Da* 

Commert T).2ppb LCS" Annotatk>n: ^ 

Sample Index : 26 

Sample Type : QC 

Concentration : 0.199 ng/mL 

Calculate d Cone: 0.213 ng/mL 

1/2/2011 2J*4-

I Sample Name:'V110802a028- Sample 10:-LCS-11072&4- Fle:>1108Caa.wtfr 

Peak Name:-PFOS- Ms**(e«):-499JXX)/99.000Da,499.00CV80.000Da,499.00(V130.000 0«-

I Comment:-2ppbLCS' Annotation:' 

ample Index : 29 

Acq. Timt ll:4B: U PM 

Modltled : 

Pioc . Algorithm: 

Nol.i« Percentag e 

Base . Sub. Windo 

Peak-Split , Fact 

Report Largest f 

Min. Peak Heigh t 

Min. Peak Hidth : 

Smoothing Hidth : 

RT Window: 

Expecte d RT: 

l>at> Relativ e RT: 

Int . Type : 

Retentio n Time: 

Are*: 1 

Height : 

Star t Time : 

No 

Specif y Pa 

50 

rf: 1.00 

3 r: 2 

a k : Yes 

0.0 0 

0 

30. 0 

15. 3 r 

Ho 

Valle y 

16.2 n 

9532 cou 

.93et004 

16,1 n 

1.2*4 

1.0e4' 

8000.0 

G000.D 

4000.0-

2000.0 

Sample Type : QC 

Concentration : 1,99 

Calculate d Cone: 1.99 

Acq. Date : 8/3/101 1 

Acq, Time : 12:51:1 5 Ah 

Modified : No 

Ptoc , Algorithm: Specif y Par 

Nolae Percentage : 50 

Base . Sub. Window: 1.00 

Peak-Split . Factor: 2 

Min. Peak Height : 0.0 0 

Min. Peah Width: 0.0 0 

Smoothing Width: 0 

RT Window: 30. 0 3 

Expected RT: 16.3 n 

Use Relativ e RT: No 

Int . Type : Valle y 

Retentio n Time: 16.2 m 

Area : 17692*7 coun 

Height : 2.e0e'0D5 e 

Star t Time: 16.] DD 

End Time : 16.1 n 

ng/mL 

ng/mL 

min 

poin t 

i n 

in 

ts 

ps 

in 

- MQ II I 

J 

2.7*5 

2.ae5 

2,5e5-

2.4*5-

2.3*5-

2.2e -

1.7»5-

1.6e5-

1.5e5-

1.4e5-

1,3*5-

1.2e5-

1,1*5-

1,0e5-

9.0e4-

8.0*4-

7.0*4 • 

6.0M5.0*4-

4.0*4-

3.0*4-

155 18.0 165 17.0 175 18.0 185 

Data printe d by STW 

Printing Time: 9:49:53 AM 

Printing Date: Thursday, August 25, 

Page 1 of 3 

Page 54 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS. PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

*ETS-Kirk Results Name: kll0802a ext.rd b 

I

S*nTteName:1<110802a031" Sample IO:"LCS-110726-7- FUe:Tc1108O2*.*tr 

Peak Name: -pFOS- Ma««<e«): -499.000^.000 Da,499.000.«0.000 Da,499.000/130.000 Da' 

Comment -20ppb LCS" Annotation:" 

Sample Indey : 32 

Sample Typie: QC 

Concentration: 19.9 ng/mL 

Calculated Cone: 22.7 ng/mL 

Acq. Date: 8/3/2011 

Acq. Time: 1:54:56 AM 

Peak-Split . Factor: 

Report Largest Peak! 

Min. Peak Height : 

Min. Peak tlidth : 

Smoothing tlidth : 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Valle y 

ie : 1J. 2 

2257028^ c 

I

SamplaNama:-k110802aD41- Sample ID:-LCS-110728-13- F1e:*k110S02a.wtr 

Peak Name: 'PFOS' MaM(e«): '499.000/99.000 Da,4g9.00CVBO.OOO Oa .499.000/130.000 Da' 

Comment '2ppb LCS ECP* Annotation: 

Sample Ii 

I

Sample Name: VI10d02a03ff' Sample 10:-LCS-110726-10^ Fle:1(110802a.wHr 

P*ak Name: -PfOS- Ma*a(e*): "499.000/99.000 Da,499.000/SO.OOD Oa.499.00Ck'130.000 Da' 

Comment: -0.2ppb LCS ECp Arvwtatbn: -

Sample Index: 39 

Sample Type: QC 

Concentration : 0.19 8 ng/mL 

Calculate d Cone: 0.2*6 ng/mL 

Acq. Date: 8/3/2011 '•"* ' 

Acq. Time: 4:22:4 9 AM 

1.7*4-

Modified : Yes 

Ptoc . Algorithm: Specif y Param 

Nois e Percentage : 50 

Base . Sub. Window: l.0 0 m 

Peak-Split , Factor : 2 

Report Largest Peak: Yes 

tet a 

Min. Peak Height : 0.0 0 cp s 

Min. Peak Width: 0.0 0 

Smoothing Vlldth: 0 

RT Mindow: 30. 0 se e 

Expected RT: 16.3 min 

Use Relativ e RT: He 

Int . Type: Manual 

Retentio n Time: 16.2 min 

Area : 181636 counts 

Height : l.e5e*00< eps 

Star t Time: IS. 8 min 

End Time: 16.3 min 

poin t 

MQ II I 

J 

f 

1 

1.8*4 

1.5*4 

1.3*4 

1.2*4 

1.1*4 

1.0*4 

9000J) 

8000,0 

7000.0 

6000.0 

5000.0 

4000.0 

3000.0 

2000.0 

1000.0 

I

Saiiq)leName:'V110802a044* Sample ID: 1.CS-110726-16r Fle:1(110a02a.wir 

Peak Name: -PFOS- li«aM(et): -49d.000[%.000 Oa ,499.00080.000 Da ,499.000^ 30.000 Da' 

Comment:-20ppb LCS ECP Amotatton:-

Sample Index : *5 

Sample Type: QC 

Concentration : 19.8 ng/mL 

Calculate d Cone: 17.8 ng/mL 

Acq. Date : B/3/2011 

Acq. Time: 6:29:3 0 AH 

Sample Type: OC 

Concentration : 

Calculate d Cone: 

Acq. Date : 

Acq. Time: 

Modified: 

Proc . Algorithm: 

Molae Percentag e 

1.98 

1.83 

e/3/201 1 

ng/mL 

ng/mL 

5:26:1 1 AM 

Yes 

Specif y Pa 

50 

Base . Sub. Window: 1.00 

Peak-Split , Factor: 2 

Repott Largest Peak: Yes 

Min. Peak Height 

Min. Peak Hidth : 

Smoothing Hidth : 

RT Hindow: 

Expected RT: 

L'se Relativ e RT: 

Int . Type: 

Retentio n Time: 

O.Oi 

O.Oi 

30. 0 

16. 3 

Ho 

Manual 

16.2 

Area : 1620758 cou 

Height : 

Star t Time: 

End Time: 

.740*005 

15,8 

16-4 

min 

eps 

po 

min 

•nin 

cps 

roln 

min 

Modified : Yes 

Proe . Algorithm: Specif y Parame 

Nois e Percentage : 

Base . Sub, Window 

Peak-Split . Fact o 

Report Largest Pe. 

Min. Peak Height : 

Min. Peak Width: 

Smoothing Width: 

RT Window: 

Expected RT: 

Use Relativ e RT: 

Int . Type : 

Retentio n Time: 

50 

1.00 mi 

: 2 

k: Yes 

0.00 c 

0.00 s 

0 

30. 0 se c 

16, 3 roln 

No 

Manual 

16.2 min 

Area : 17345070 counts 

Height : 1 

Star t Time: 

End Time: 

70e-.006 eps 

IS. 9 min 

16. 1 roln 

15.5 16.0 16.5 17.0 17.5 1SJ) 1S.5 15.0 15.5 16.0 185 17.0 17.5 18.0 185 

Data printe d by STW 

Printing Time: 9:49:53 AM 

Printin g Date: Thursday, August 25, 

Page 2 of 3 

Page 55 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS. and PFOS in Water Samples 

Off-Site BP Property - July 2011 

Results Name: kll0802a ext.-rdb 

• S«nvlaNeme:-lc110802aOSff' San^le ID:-QLP1001-02-19-005- File: 

I Peak Name:-PFOS- Ua«s(e*):-499.000i'99.000 Oa,499.00a«),O00 Da, 

• Cofwn*nt-DALGWBPMW470110713- Annolatton:~ 

Sample Index: 59 

Sampl Unknown e Type: 

alci 

mtratic H/A 

0,206 ng/mL 

B/3/2011 

11:25:10 AM 

Nol! Percentage 

uase. Sub. Hindow: 

Peak-Split. Factoi 

Report Largest Pea 

Min. Peak Height: 

Min. Peak Width: 

Smoothing Width: 

RT Hindow: 

Expected RT: 

Vs^ Relative RT: 

Specify Parameter: 

50 

1.00 min 

1.3*4 

13*4 

1.2*4 

1,2*4 

1.1*4 

1.1*4 

1.0*4 

9500.0 

9000.0 

8500.0 

8000.0 

7500.0 

7000.0 

6500.0 

6000.0 

5600.0 

5000.0 

4500.0 

3500.0 

3000.0 

2S0O.O 

2O0O.O 

1500.0 

1000.0 

500.1 

'WM* 

16 

16.0K 

15 

II 

-.- • 1M7 

1 i i H Jl ^•Jll6i» 15.7^ ^^m p ^ 

• f TY ^ 

JM^ ^ m,. lu 

P"!^TM ,^Vm 

17.41 

ILJ M 

w f P 

^17.77 

ilk '"» 

n,i ^inu '.WwWw 

Data printed by STW 

Printing Time: 9:49:53 AM 

Printing Date: Thursday, August 25, 2011 

Page 3 of 3 

Page 56 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

ATTACHMENT C: ANALYTICAL METHOD 

Page 57 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS In Water Samples 

Off-Site BP Property - July 2011 

Environmental Laboiafioffy 

Method 

Method of Analysis for the Determination of Perfluorinated Compounds in Water 

by LC/MS/MS; Direct Injection Analysis 

Method Number: ETS-8-044.0 

Adoption Date: Upon Signing 

Effective Date: Q <//(^ / o "7 

Approved By: 

^//^/o y 

William K. Reagen, Laboratory Manager Date 

ETS-8-044.0 Page 1 of 11 

Method of Analysis for tlie Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct 

Injection Analysis Page 58 of 70 
GLP10-01-02; Interim Report 19 

Analysis of PFBS, PFHS, and PFOS in Water Samples 

Off-Site BP Property - July 2011 

1 Scope and Application 

This method is to be used to quantify Perfiuorobutanoic Acid (PFBA), Perfluoropentanoic Acid (PFPeA), 

Perfiuorohexanoic Acid (PFHA), Perfluoroheptanoic Acid (PFHpA), Perfluorooctanoic Acid (PFOA), 

PerfluorononanoicAcid (PFNA), Perfluorodecanoic Acid (PFDA), PerfluoroundecanoicAcid (PFUnA), 

Perfluorododecanoic Acid (PFDoA), Perfiuorobutanesulfonate (PFBS), Perfluorohexanesulfonate (PFHS), 

and Perfiuorooctanesulfonate (PFOS) by High Perfomnance Liquid Chromatography coupled to a tandem 

Mass Spectrometric Detector (LC/MS/MS) in clean water samples. Water samples containing heavy 

particulate may require preparation by an alternate method such as ETS-8-154 "Determination of 

Perfluorinated Acids, Alcohols, Amides, and Sulfonates In Water By Solid Phase Extraction and High 

Performance Liquid Chromatography/Mass Spectrometry". 

This method is considered a performance-based method. Data is considered acceptable as long as the 

defined QC elements are satisfied. 

Sample collection is not covered under this analytical procedure. 

2 IVIethod Summar y 

Clean aqueous samples are analyzed by direct injection using LC/MS/MS. Samples containing heavy 

particulate may not be suitable for analysis by this method. Samples containing suspended particulate 

should be centrifuge prior to removing a sample aliquot, or filtered. 

This is a performance-based method. Method accuracy is determined for each sample set using multiple 

laboratory control spikes at multiple concentrations. This method also requires that the precision and 

accuracy for each sample be determined using field matrix spikes to verify that the method is applicable to 

each sample matrix. Sample results for spikes outside of 70% to 130%, may be flagged as such (with 

expanded accuracy statements), or will not be reported due to non-compliant quality control samples. 

Fortification levels for field matrix spikes and for laboratory matrix spikes should be at least 50% of the 

endogenous level and less than 10 times the endogenous level to be used to determine the statement of 

accuracy for analytical results. 

3 Definitions 

3.1 Calibration Standard 

A solution prepared by spiking a known volume of the Working Standard (WS) into a predetermined 

amount of ASTM Type i, HPLC grade water, or other suitable water, and analyzed according to this 

method. Calibration standards are used to calibrate the instrument response with respect to analyte 

concentration. 

3.2 Laboratory Duplicate Sample (LDS, or Lab Dup) 

A laboratory duplicate sample is a separate aliquot of a sample taken in the analytical laboratory that is 

analyzed separately with identical procedures. Analysis of LDSs compared to that of the first aliquot give 

a measure of the precision associated with laboratory procedures, but not with sample collection, 

preservation, or storage procedures. 

3.3 Field Blank (FB)/Trip Blank 

ASTM Type I, HPLC grade water, or other suitable water, placed in a sample container in the laboratory 

and treated as a sample in all respects, including exposure to sampling site conditions, storage, 

preservation and all analytical procedures. The purpose of the FB is to determine if test substances or 

other interferences are present in the field environment. This sample is also refen-ed to as a Trip Blank. 

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3.4 Field Duplicate Sample (FDS, Field Dup) 

A sample collected in duplicate at the same time from the same location as the sample. The FDS is 

handled under identical circumstances and treated exactly the same throughout field and laboratory 

procedures. Analysis of the FDS compared to that of the first sample gives a measure of the precision 

associated with sample collection, preservation and storage, as well as with laboratory procedures. 

3.5 Field Matrix Spike (FMS) 

A sample to which known quantities of the target analytes are added to the sample bottle in the laboratory 

before the bottles are sent to the field for collection of aqueous samples. A known, specific volume of 

sample must be added to the sample container without rinsing. This may be accomplished by making a 

"fill to this level" line on the outside of the sample container. The FMS should be spiked between 

approximately 50% and 10 times the expected analyte concentration in the sample. If the expected range 

of analyte concentrations is unknown, multiple spikes at varying levels may be prepared to increase the 

likelihood that a spike at an appropriate level is made. The FMS is analyzed to ascertain if any matrix 

effects, interferences, or stability issues may complicate the interpretation of the sample analysis. 

3.6 Trip Blank Spike (Field Spike Control Sample, FSCS) 

An aliquot of ASTM Type I, HPLC grade water, or other suitable water, to which known quantities of the 

target analytes are added in the laboratory prior to the shipment of the collection bottles. The FSCS is 

extracted and analyzed exactly like a study sample to help determine if the method is in control and 

whether a loss of analyte could be attributed to holding time, sample storage and/or shipment issues. A 

low and high FSCS are appropriate when expected sample concentrations are not known or may vary. At 

least one separate, un-spiked sample must be taken at the same time and place as each FMS. 

3.7 Laboratory Control Sample (LCS) 

An aliquot of control matrix to which known quantities of the target analytes are added in the laboratory at 

the time of sample extraction. At least two levels are included, one generally at the low end of the 

calibration curve and one near the mid to upper range of the curve. The LCSs are extracted and analyzed 

exactly like a laboratory sample to determine whether the method is in control. LCSs should be prepared 

each day samples are extracted. 

3.8 Laboratory Matrix Spike (LMS) 

A laboratory matrix spike is an aliquot of a sample to which known quantities of target analytes are added 

in the laboratory. The LMS is analyzed exactly like a laboratory sample to determine whether the sample 

matrix contributes bias to the analytical results. The endogenous concentrations of the analytes in the 

sample matrix must be detemnined in a separate aliquot and the measured values in the LMS con'ected 

for these concentrations. LMSs are optional for analysis of aqueous samples. 

3.9 Laboratory Sample 

A portion or aliquot of a sample received fi-om the field for testing. 

3.10 Limit of Quantitation (LOQ) 

The lower limit of quantitation (LLOQ) for a dataset is the lowest concentration that can be reliably 

quantitated within the specified limits of precision and accuracy during routine operating conditions. To 

simplify data reporting, the LLOQ is generally selected as the lowest non-zero standard in the calibration 

curve that meets method criteria. Sample LLOQs are matrix-dependent. 

The upper limit of quantitation (ULOQ) for a dataset is the highest concentration that can be reliably 

quantitated within the specified limits of precision and accuracy during routine operating conditions. The 

highest standard in the calibration curve that meets method criteria is defined as the ULOQ. 

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3.11 Method Blank 

An aliquot of control matrix that is treated exactly like a laboratory sample including exposure to all 

glassware, equipment, solvents, and reagents that are used with other laboratory samples. The method 

blank is used to determine if test substances or other interferences are present in the laboratory 

environment, the reagents, or the apparatus. 

3.12 Sample 

A sample is an aliquot removed fi-om a larger quantity of material intended to represent the original source 

material. 

3.13 Stock Standard Solution (SSS) 

A concentrated solution of a single-analyte prepared in the laboratory with an assayed reference 

compound. 

3.14 Surrogate 

A compound similar in chemical composition and behavior to the target analyte(s), but is not normally 

found in the sample(s). A sun-ogate compound is typically a target analyte with at least one atom 

containing an isotopically-labeled substitution. If used, surrogate(s) are added to all samples and quality 

control samples. Sun-ogate(s) are added to quantitatively evaluate the entire analytical procedure 

including sample collection, preparation, and analysis. Inclusion of a sun-ogate analyte is an optional 

quality control measure and is NOT required. 

3.15 Working Standard (WS) 

A solution of several analytes prepared in the laboratory from SSSs and diluted as needed to prepare 

calibration standards and other required analyte solutions. 

4 Warnings and Cautions 

4.1 Health and Safety 

The acute and chronic toxicity of the standards for this method have not been precisely determined; 

however, each should be treated as a potential health hazard. The analyst should wear gloves, a lab 

coat, and safety glasses to prevent exposure to chemicals that might be present. 

The laboratory is responsible for maintaining a safe wori< environment and a current awareness of local 

regulations regarding the handling of the chemicals used in this method. A reference file of material safety 

data sheets (MSDS) should be available to all personnel involved in these analyses. 

4.2 Cautions 

The analyst must be familiar with the laboratory equipment and potential hazards including, but not limited 

to, the use of solvents, pressurized gas and solvent lines, high voltage, and vacuum systems. Refer to the 

appropriate equipment procedure or operator manual for additional infomnation and cautions. 

5 Interferences 

During sample preparation and analysis, major potential contaminant sources are reagents and 

glassware. All materials used in the analyses shall be demonstrated to be free from interferences under 

conditions of analysis by mnning method blanks. 

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Parts and supplies that contain Tefion® should be avoided or minimized due to the possibility of 

interference and/or contamination. These may include, but are not limited to: wash bottles. Teflon® lined 

caps, autovial caps, HPLC parts, etc. 

The use of disposable micropipettes or pipettes to aliquot standard solutions is recommended to make 

calibration standards and matrix spikes. 

6 Instrumentation, Supplies, and Equipment 

6.1 Instrumentation and Equipment 

A high perfomnance liquid chromatograph capable of pumping up to two solvents and equipped with a 

variable volume injector capable of injecting 5-100 |JL connected to a tandem Mass Spectrometer 

(LC/MS/MS). I 

Analytical balance capable of reading to 0.0001 g 

A device to collect raw data for peak integration and quantitation 

15-mL and 50-mL disposable polypropylene centrifuge tubes. 

Gas tight syringes, 25IJL, 50|JL, IOOJJL, 250|JL, SOOpL, 1000|JL. 

1 mL plastic HPLC autovial. 

Disposable pipettes, polypropylene or glass as appropriate 

Centrifuge capable of spinning 15-mL and 50-mL polypropylene tubes at 3000 rpm. 

6.2 Chromatographi c System 

Guard Column: Prism RP, 4.6 mm x 50 mm, 5 |jm 

Analytical Column: Betasil CI 8,4.6 mm x 100 mm, 5 |jm 

Temperature: lO'C 

Mobile Phase (A): 2 mM Ammonium Acetate in Water 

Mobile Phase (B): Methanol 

Gradient Program: 

Time (min) 

0.0 

0.5 

11.0 

13.5 

13.6 

17.0 

%A 

97 

97 

5 

5 

97 

97 

%B 

3 

3 

95 

95 

3 

3 

Flow Rate 

(mL/min) 

1.0 

1.0 

1.0 

1.0 

1.0 

1.0 

Injection Volume: 100 |JL 

Quantitation: Peak Area - quadratic curve fit, 1/x weighted. 

Run Time: ~ 17 minutes. 

The previous information is intended as a guide; alternate conditions and equipment may be used 

provided that data quality objectives are met. 

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6.3 MS/MS System 

6.3.1 Mode: Electrospray Negative ion, MRM mode, monitoring the following transitions: 

Analyte 

PFBA 

PFPeA 

PFHA 

PFHpA 

PFOA 

PFNA 

PFDA 

PFUnA 

PFDoA 

PFBS 

PFHS 

PFOS 

Transition Monitored 

213^169 

263^219 

313 ^269 and 313 ^119 

363 ^ 319, 363 ^ 169 and 363 ^ 119 

413 -^ 369, 413 ^ 219 and 413 -->• 169 

463 ^ 419, 463 -^ 169 and 463 ^. 219 

513 ^ 469, 513 ^ 219 and 513 ^ 269 

563 ^ 519, 563 ^ 269 and 563 -» 219 

613 ^ 569, 613 ^ 169 and 613 -->• 319 

299 -^ 80 and 299 -^ 99 

399 -^ 80 and 399 ->• 99 

499 -^ 80, 499 -^ 99 and 499 -^ 130 

Multiple transitions for monitoring the analytes is an option, as summing multiple transitions may provide 

quantitation of isomers that more closely matches NMR data and may have the added benefit of 

increased sensitivity. The use of one daughter ion is acceptable if method sensitivity is achieved, 

provided that retention time criteria are met to assure adequate specificity. 

The previous information is intended as a guide, alternate instruments and equipment may be used. 

7 Reagents and Standards 

7.1 Chemicals 

Water - Milli-Q, HPLC grade, or other suitably appropriate sources 

Methanol - HPLC grade 

Ammonium Acetate -A.C.S. Reagent Grade 

7.2 Standards 

Perfiuorobutanoic Acid (PFBA - C4 acid); Oakwood Products, Inc 

Perfluoropentanoic Acid (PFPeA - C5 acid, also known as NFPA, nonafluoropentanoic acid); Alfa Aesar 

Perfiuorohexanoic Acid (PFHA- C6 acid); Oakwood Products, Inc 

Perfluoroheptanoic Acid (PFHpA - C7 acid, also known as TDHA, tridecafluoroheptanoic acid); Oakwood 

Products, Inc 

Perfluorooctanoic Acid (PF0A-C8 acid); 3M 

PerfluorononanoicAcid (PFNA-C9 acid); Oakwood Products, inc 

Perfluorodecanoic Acid (PFDA-CIO acid); Oakwood Products, Inc 

PerfluoroundecanoicAcid (PFUnA-C11 acid); Oakwood Products, Inc 

PerfluorododecanoicAcid (PFDoA-CI2 acid); Oakwood Products, Inc 

Perfiuorobutanesulfonate (PFBS - C4 sulfonate); 3M 

Perfiuorohexanesulfonate (PFHS - C6 sulfonate); 3M 

Perfiuorooctanesulfonate (PFOS - C8 sulfonate); 3M 

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The previous information is intended as a guide. Reagents and standards from alternate sources may be 

used. 

7.3 Reagent Preparation 

2 mM Ammonium acetate solution (Analysis)—Weigh 0.3 g of Ammonium acetate and dissolve in 2.0 L of reagent 

water. 

Note: Altemative volumes may be prepared as long as the ratios of the solvent to solute ratios are maintained. 

7.4 Stock Standard Solution (SSS) and Working Standard Solution Preparation 

The following standard preparation procedure serves as an example. Weighed amounts and final volumes may be 

changed to suit the needs of a particular study. For example, IJL volumes may be spiked into volumetric flasks 

when diluting stock solutions to appropriate levels. 

100 \iglm\- target analyte SSSs—Weigh out 10 mg of analytical standard (corrected for percent salt and 

purity) and dilute to 10OmL with methanol or other suitable solvent, in a 10OmL volumetric fiask. Transfer to a 

125mL LDPE bottle or other suitable container. Prepare a separate solution for each analyte. Expiration dates 

and storage conditions of stock solutions should be assigned in accordance with laboratory standard operating 

procedure. An example of purity and salt con-ection is given below for PFOS. 

,^ XX X molecular weight of anion 

salt correction factor = = 

moclecular weight of salt 

499 PFOS (K^ )salt correction factor = ^^ ^ = 0.9275 

538 

10 mg CsFiySOs'K" with purity 90% = 8.35mg C8F17SO3" (10 mg*0.90*0.9275=8.35 mg) 

5 (jg/mL (5000 ng/mL) mixed working standard-^dd 0.5mL each of the 100|jg/mL SSSs to a 10mL volumetric 

fiask and bring up to volume with solvent. 

250 ng/mL mixed worthing standard—Add 1.25mL of the 5 iig/mL -mixed wori<ing standard solution to a 25mL 

volumetric flask and bring up to volume with solvent. 

125 ng/mL mixed standard—Add 625|JL of the 5 |jg/mL-mixed woricing standard solution to a 25mL volumetric 

flask and bring up to volume with solvent. 

Storage Conditions—Store all SSSs and working standards in accordance with laboratory standard operating 

procedure or in a refrigerator at 4''±2°C for a maximum period of 6 months from the date of preparation. 

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7.5 Calibration Standards 

Using the worthing standards described above, prepare calibration solutions in ASTM Type I water, HPLC water, or 

other suitable water, using the following table as a guideline. Note: Volumes of water and wori<ing standards may 

be adjusted to meet the data quality objectives addressed in the general project outline. Calibration levels other 

than those listed below can be prepared as needed. 

Concentration 

of WS, ng/mL 

125 

125 

125 

125 

250 

250 

250 

250 

5000 

5000 

5000 

Volume of WS,fiL 

10 

15 

20 

30 

20 

50 

100 

200 

25 

50 

100 

Final Volume of 

Calibration Standard (mL 

of ASTM Type 1 Water, or 

other suitable water) 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

50 

Final Concentration of 

Calibration Standard, ng/mL 

(ppb) in AS77M Type 1 Water, 

or otiier suitable water 

0.025 

0.0375 

0.050 

0.075 

0.100 

0.250 

0.500 

1.00 

2.50 

5.00 

10.0 

8 Sample Handling 

8.1 Water Sample Preparation 

This method is applicable to clean water samples. Samples containing heavy particulate may not be suitable for 

analysis by this method. Samples containing suspended particulate should be centrifuge prior to removing a 

sample aliquot, or filtered. 

Thoroughly mix sample before removing an aliquot and placing in a labeled plastic autovial. Plastic is 

prefen-ed over the use of glass autovials, to prevent the possibly of fluorochemical sticking to the glass. 

Dilute sample, if necessary, with ASTM Type I, HPLC water, or other suitable water. 

Prepare method QC samples and multiple method blanks and aliquot into labeled plastic autovials. 

Prepare at least five method blanks. 

9 Sample Analysi s - LC/MS/MS 

Analyze the standard curve prior to each set of samples. The standard curve may be plotted using a linear fit, 

weighted 1/x or unweighted, or by quadratic fil (y = ax^ + bx + c), weighted 1/x or unweighted, using suitable 

software. The calibration curves may include but should not be forced through zero. The mathematical method 

used to calculate the calibration curve should be applied consistently throughout a study. Any change should be 

thoroughly documented in the raw data. 

High and/or low points may be excluded fi-om the calibration curves to provide a better fit over the range 

appropriate to the data or because they did not meet the pre-determined acceptance criteria. Low-level curve 

points should also be excluded if their area counts are not at least twice that of the method and/or solvent blanks. 

The coefficient of detemnination (r^) value for the calibration curve must be greater than or equal to 0.990. Each 

point in the curve must be within ±25% of the theoretical concentration with the exception of the LLOQ, which may 

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be within ±30%. Justification for exclusion of calibrafion curve points will be noted in the raw data. A minimum of 6 

points will be used to constmct the calibration curve. 

If the calibration curve does not meet acceptance criteria, perform roufine maintenance or prepare a new standard 

curve (if necessary) and reanalyze. 

Continuing calibration verifications (CCV) are analyzed to verify the accuracy of the calibration curve. Analyze a 

mid-range calibration standard, one of the same standards used to constmct the calibration curve, at a minimum 

after every tenth sample, not including solvent blanks, with a minimum of one per sample set. Calibration 

verification injections must be within +25% to be considered acceptable. The calibration curve and the last passing 

CCV will then bracket acceptable samples. Multiple CCV levels may be used. 

Samples containing analytes that are quantitated above the concentration of the highest standard in the 

curve should be further diluted and reanalyzed. 

10 Quality Control 

10.1 Data Quality Objectives 

This method and required quality control samples is designed to generate data accurate to ±30% with a targeted 

LOQ of 0.025 ng/mL. Any deviations from the quality control measures spelled out below will be documented in 

the raw data and footnoted in the final report. 

10.2 Method Blanks 

Method blanks must be prepared with each analysis batch. At least five method blanks must be prepared. 

Method blanks may be injected multiple times, but no more than 3 injections should be removed from a single 

method blank. At a minimum, method blanks are analyzed prior to instmment calibration, prior to the analysis of 

CCV samples, and at the end of the analytical mn. 

The mean area count for each analyte in the method blanks must be less than 50% of the area count of the LOQ 

standard. The standard deviation of the area counts of these method blanks should be calculated and reported. If 

the mean area counts of the method blanks exceed 50% of the LOQ standard, then the LOQ must be raised to the 

first standard level in the curve that meets criteria, or altematively, the method blanks must be evaluated 

statistically to detennine outliers, or technical justification to eliminate one or more results should be made. 

10.3 Sample Replicates 

Samples duplicates are collected in the field. The relative percent difference, RPD, should be reported. RPD 

results greater than 20% will be flagged in the report, but will not be excluded fi-om reporting. The requirement for 

replicates excludes field blanks. 

10.4 Surrogate Spikes 

Sun-ogate spikes are not required but may be used on project specific requirements. 

10.5 Lab Control Sample 

Triplicate lab control spikes at a minimum of two different concentrations are to be prepared with each preparation 

batch. Low lab control spikes should be prepared at concentrations in the range of five to ten times higher than the 

targeted LOQ and high lab control spikes should be prepared at concentrations near the mid-point of the curve. 

The relative standard deviation of the control spikes evaluated independently at each concentration level must be 

less than or equal to 20% and the average recovery must be 80-120%. If the above criteria are not met, the entire 

set of samples should be re-injected or re-prepared as appropriate. 

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10.6 Field Matrix Spikes / Lab Matrix Spikes 

Recoveries of field matrix spikes and laboratory matrix spikes are anticipated to be between 70% and 130% of the 

fortified levels. Sample results for spikes outside of 70% to 130%, may be fiagged as such (with expanded 

accuracy statements), or will not be reported due to non-compliant quality control samples. 

The targeted fortification levels should be at least 50% of the endogenous level and less than 10 times the 

endogenous level to be used without justification to detemnine the statement of accuracy for analytical results. 

The average of the sample and the field duplicate should be used to calculate the recovery. 

11 Data Analysis and Calculations 

Use the following equation to calculate the amount of analyte found (in ng/mL, based on peak area) using the 

standard curve (linear regression parameters) generated by an appropriate software program: 

Analyte found (ng/mL) = (Peak Area-Intercept) ^ ^ ^ 

Slope 

DF = factor by which the final volume was diluted, if necessary. 

For samples fortified with known amounts of analyte prior to extraction, use the following equation to calculate the 

percent recovery. 

P _ Total analyte found (ng/mL) - Average analyte found in sample (ng/mL) 

Analyte added (ng/mL) 

12 Method Performance 

Any method performance parameters that are not achieved must be considered in the evaluation of the data. 

Nonconfomnance to any specified parameters must be described and discussed if the Technical Manager (nonGLP study) or Study Director (GLP study) chooses to report the data. 

If criteria listed in this method perfomnance section are not met, maintenance may be perfomned on the system and 

samples reanalyzed, or other actions taken as appropriate. Document all actions in the raw data. 

If data are to be reported when perfomnance criteria have not been met, the data must be footnoted on tables and 

discussed in the text of the report. 

12.1 System Suitability 

System Suitability standards are not a required component of this method. If required by protocol or by the 

technical manager, a minimum of three system suitability samples are injected at the beginning of each analytical 

mn prior to the calibration curve. Typically these samples are at a concentration near the mid level of the 

calibration cun/e and are repeated injections from one autosampler vial. The system suitability injections must 

have area counts with an RSD of S5% and a retention time RSD of S2% to be compliant. 

12.2 Quantitation 

Calibration Curve: The coefficient of detemnination (r^) value for the calibration curve must be greater than or 

equal to 0.990. Each point in the curve must be within ±25% of the theoretical concentration with the exception of 

the LLOQ, which may be within ±30%. 

CCV Performance: The calibration standards that are interspersed throughout the analytical sequence are 

evaluated as continuing calibration verifications in addition to being part of the calibration curve. The accuracy of 

each curve point must be within 25% of the theoretical value (within 30% for lowest curve point). Samples that are 

bracketed by CCVs not meeting these criteria must be reanalyzed. 

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Demonstration of Specificity: Specificity is demonstrated by chromatographic retention time (within 4% of 

standard) and the mass spectral response of unique ions. 

12.3 Sensitivity 

The targeted limit of quantitation for all analytes is 0.025 ng/mL. The LOQ for any specific analyte may vary 

depending on the evaluation of appropriate blanks and the accuracy of the low-level calibration curve points. Refer 

to Section 10 for additional details. 

12.4 Accuracy 

This method and required quality control samples are designed to generate data that are accurate to +/-30%. 

Section 10 contains additional infomnation regarding the required accuracy of laboratory control spikes, field matrix 

spikes and laboratory matrix spikes. 

12.5 Precision 

Samples should be collected in duplicate in the field. The relative percent difference, RPD, should be reported. 

RPD results greater than 20% will be flagged in the report, but will not be excluded from reporting. The 

requirement for replicates excludes field blanks or rinse blanks. 

Section 10 contains additional infomnation regarding the required precision of laboratory control spikes. 

13 Pollution Prevention and Waste Management 

Waste generated when perfomning this method will be disposed of appropriately. The original samples will be 

archived at the 3M Environmental Laboratory in accordance with intemal procedures. 

14 Records 

Each data package generated for a study must include all supporting infomnation for reconstmction of the data. 

Infomnation for the data package must include, but is not limited to the following items: study or project number, 

sample and standard prep sheets/records, instmment mn log (instmment batch records, instmment acquisition 

method, summary pages), instmment results files, chromatograms, calibration curves, and data calculations. 

15 Affected Documents 

None. 

16 Revisions 

Revision 

Number Summary of Changes 

} 

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ATTACHMENT D: DEVIATION(S) 

Page 69 of 70 
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RECORD OF DEVIATION/NONCONFORMANCE 

/. Identification 

study / Project No. 

GLP10-01-02-19 

Deviation type 

(Check one) 

D 

D 

SOP 

Protocol 

Date(s) of Occurrence: 

j<110802a and k l 10802a ext 

D Equipment Procedure 

D GPO 

Document Number: 

ETS-8-044.0 

0 

D 

Method 

Other: 

//. Descriptio n (attach extra pages as needed) 

Method Requirements: 

1. LCS average recoveries within ±20% (section 10.5). 

Actual procedure/process: 

1. kl 10802a; internal standard calibration: The low, mid, and high PFOS ECF LCS samples had average 

recoveries of 129%, 122%, and 122%. k110802a ext; external standard calibration: The low PFOS (linear) 

LCS had an average recovery of 122%. The low PFOS (linear and branched) LCS had an average 

recovery of 126%. 

///. Actions Taken 

(such as amendment issued, SOP revision, etc.) 

Corrective Action (D Yes IZf No) Reference: 

Acceptability of the nonconforming work: 

1. The recoveries for the LCSs (linear + branched) outside method acceptance criteria will be flagged in the 

final report. All of the LCSs prepared with this study were evaluated by ETS-12-012 to determine the 

method analytical uncertainty. The analytical uncertainty when evaluated by ETS-12-012 was detennined 

to be ±24% for PFOS. However, the analytical uncertainty for this study will be set at ±29%, based on the 

recovery of the low set of linear + branched LCS from run kl 10802a. 

Actions: D Halting of Wori< D Client Notification D Work Recall D Withholding of Report 

13 Other: Deviations will be noted in final report. 

Project Lead/PAI Approval: ( 1 

study Director (if GLP): 

Sponsor Approval (for GLP protocol deviations): NA 

Date: KJM 

Date> 

Date 

LL 

WlL 

Technical Reviewer (optional): NA Date: NA 

Laboratory Departrpent Mans 

rgd ^ 

Approval: Date: 

IV. Authorization to Resume Work 

Where halting of work occurred, resumption of work must first be approved by Laboratory Management 

Laboratory Department Manager Approval: NA Date: NA 

Deviation No. 

(assigned by Study Director or Team Leader at the end of study or project) 

ETS-4-008.7 Page 1 of 1 

Documentation of Deviations and Control of Nonconforming Testing ^^®