# Fish Sampling and Analysis for PFOS in Largemouth Bass from the Tennessee River in the Vicinity of the 3M Decatur Facility

3M Company Decatur, Alabama

May 2012

11P-0094-7 

# 3M Company St. Paul, Minnesota

®

## FISH SAMPLING AND ANALYSIS FOR PFOS IN LARGEMOUTH BASS FROM THE TENNESSEE RIVER IN THE VICINITY OF THE 3M DECATUR FACILITY, DECATUR, ALABAMA

May 2012

Prepared for 3M Company St. Paul, MN

by
WESTON SOLUTIONS, INC.

West Chester, PA 19380

W.O. No. 02181.129.122\\Weston\natacc\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\Fish sampling PFOS 2012\2012 Fish Sampling Report.doc 

## i 

# TABLE OF CONTENTS

Section Page

1. INTRODUCTION.......................................................................................................... 1-1
2. MATERIALS AND METHODS .................................................................................. 2-1
3. RESULTS ....................................................................................................................... 3-1
4. REFERENCES ............................................................................................................... 4-1



# APPENDICES

APPENDIX A 3M ENVIROMENTAL LABORATORY ANALYTICAL DATA PACKAGES

APPENDIX B AXYS LABORATORY ANALYTICAL DATA PACKAGE\\Weston\natacc\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\Fish sampling PFOS 2012\2012 Fish Sampling Report.doc 

## ii 

# LIST OF TABLES

Section Page

Table 3-1 Fish Sampling Summary and Catch Per Unit Effort ............................................ 3-8

Table 3-2 Fish Morphometrics and PFO S Concentrations .................................................. 3-9

Table 3-3 Largemouth Bass Filet PFOS Concentration Summary Statistics ..................... 3-10

Table 3-4 Surface Water PFOS Concentrations-April 2012 .............................................. 3-11\\Weston\natacc\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\Fish sampling PFOS 2012\2012 Fish Sampling Report.doc 

## iii 

# LIST OF FIGURES

Section Page

Figure 2-1 Fish and Surface Water Sampling Locations-April 2012 .................................... 2-4

Figure 3-1 Largemouth Bass Filet PFOS C oncentrations-April 2012................................... 3-4

Figure 3-2 Largemouth Bass Filet PFOS Concentration Box and Dot Plots ........................ 3-5

Figure 3-3 Largemouth Bass Filet PFOS Concentrations vs. Length ................................... 3-6

Figure 3-4 Surface Water PFOS Concentrations-April 2012 ................................................ 3-7\\Weston\natacc\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\Fish sampling PFOS 2012\2012 Fish Sampling Report.doc 

## 1-1 

# 1. INTRODUCTION

Fish sampling was performed at three adjoin ing reaches spanning a distance of 2.5 miles in the Tennessee River in the vicinity of the 3M facility in Decatur, Alabama from April 3 through 6, 2012 to characterize current concentrations of perfluorooctanesulfonate (PFOS) in filet samples from largemouth bass ( Micropterus salmoides ). The largemouth bass was selected for sampling for the following reasons:

• Correspondence with the fish samples colle cted in earlier sampling performed by 3M in 2004 and 2006 and subsequent collect ions by the Alabama Department of Environmental Management (ADEM) in 2007, 2008 and 2009;

• Predator species representing the highest trophic level; and

• Recommended target species (EPA, 1993; EPA 2000).
In addition to collecting fish samples, su rface water samples were collected from each fish sampling reach for PFOS analysis. Prior to sampling, a draft Work Plan for Fish Sampling and Analysis for PFOS in Largemouth Bass in the Tennessee River in the Vicinity of the 3M Decatur Facility (draft Work Plan ) was prepared for review by the Alabama Department of Environmental Management (ADEM) and the Alabama Department of Public Health (ADPH). The Work Plan was subsequently revised to reflect comments received (WESTON, 2012) . The following sections describe the sampling activities and provide the analytical results for PFOS concentrations in filet tissue and water samples.\\Weston\natacc\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\Fish sampling PFOS 2012\2012 Fish Sampling Report.doc 

## 2-1 

# 2. MATERIALS AND METHODS

A scientific collection permit (SCP) was obt ained from the Alabama Department of Conservation and Natural Resources (DCNR) for fish collection. All collection efforts were performed in accordance with the SC P requirements including providing advance notification of pending field collection activities to the appropriate DCNR regional fisheries management/enforcement personnel. ADEM personnel were also notified and observed virtually the entire sample collection process. Electrofishing was conducted using a boat-mounted, generator-powered Smith-R oot VI-A electrofisher fitted with two bow-mounted anodes and a single trailing cathode.

Sampling reaches were shorelin e lengths of approximately 0. 75 miles. The upper reach was
the southern shoreline of th e Tennessee River above the co nfluence of Bakers Creek and
extended to the east. The central reach was the shore line within the mout h of Bakers Creek and the lower reach extended along the southern shoreline of the Te nnessee River adjacent to the 3M property. The mouth of Bakers Creek and lower sampling reaches correspond respectively with the DBC an d DOU collection locations in the 2004 and 2006 fish sampling activities perf ormed by 3M (Weston 2008). The three fish sampling reaches are shown in Figure 2-1. Electrofishing focused on shoreline areas where sufficient structure exists to attract and hold largemouth bass. Based on input from the ADEM, the target size range for largemouth ba ss to be collected was 13-18 inches in length in an attempt to coincide with the size range of fish collected previously by ADEM. The target sample size of largemouth bass from each of the three fish sa mpling reaches was 10 fish for a total target of 30 fish specimens. Fish collection was performed under oversight by personnel from ADEM who were present in a se parate boat. These individuals also observed sample preparation and other procedur al aspects of the study.

Surface water samples were coll ected using a peristaltic pum p from each of the three sampling reaches during fish collection activities for PFOS analyses. Samp ling depth was determined on the basis of total water depth. Because the surface water sampling locations
were less than 10 feet deep, samples were collected at the 0.6 depth (six-tenths of the total depth of water measured from the surface). In addition to collecting surface water samples\\Weston\natacc\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\Fish sampling PFOS 2012\2012 Fish Sampling Report.doc 

## 2-2 for laboratory analysis of PF OS concentrations, routine water quality data including the parameters of temperature, sp ecific conductance, dissolved oxygen, pH and turbidity were also collected at the sampling locations.

In order to collect data suitable for assessing the range of variability in fish tissue PFOS concentrations and for consistency with pa st 3M and ADEM collections, samples were prepared from individual fish specimens for an alysis rather than composite samples from multiple specimens. Sample IDs were assigned in the sequence of sample collection and did not contain information on the sampling locations. Each fish retained for tissue analysis was weighed and the total length was measured. Per input received from ADEM, skin-off filet tissue samples were prepared in the field from the right side filets of the fish specimens. In addition to the primary sa mples, field duplicate samples and quality assurance/quality control (QA/QC) sample s were prepared. Fi eld QA/QC samples included the collection of three equipment rins eate blanks to document the adequacy of decontamination of knives used to prepare th e fish filet samples. Filet tissue samples were shipped frozen to the Michigan Stat e University Wildlife Toxicology Laboratory (MSU WFL) for preparation of tissue homogenates. As inst ructed by the Study Director, MSU WTL forwarded the homogenized sample s to the appropriate laboratories for analysis. The 3M Environmental Laboratory in St. Paul, Minnesota served as the primary laboratory for this study. Th e AXYS Analytical Services , Ltd. (AXYS) laboratory in Sidney, British Columbia, Canada, provided va lidation results in this study design.

Field duplicate samples were prepared in the fiel d from the left side filets of the chosen fish specimens. The left side filet was remove d after the right side filet had been removed and was prepared as a skin-off filet tissue sample. Six left side skin-off fillets were
chosen at random and sent as field duplicate samples to MSU WTL for preparation of tissue homogenates. Three of these duplicates were provided to the 3M Environmental Laboratory and the other three were sent to AXYS. The source of the blind field duplicates was not rev ealed to either laboratory. The b lind field duplicates had unique sample identification numbers on the Chain of Custody form sent to the laboratory such that the laboratory could not determine its sour ce. Additional left side filets collected and\\Weston\natacc\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\Fish sampling PFOS 2012\2012 Fish Sampling Report.doc 

## 2-3 not required for QA/QC analysis were prepared as skin-on filets, frozen and transferred to the 3M Environmental Laboratory to be retained indefinitely.

Additionally, process control fish samples were se nt by the 3M Environmental Laboratory to the MSU WTL to be analyzed before, during and after the processing of the field samples to confirm adequate d econtamination of homogenization equipment between preparation of indivi dual study samples and the abse nce of other contamination vectors associated with the preparati on of the tissue homogenates. Following homogenization, these samples were returned to the 3M Environmental Laboratory for analysis.

Finally, a standard reference material (S RM) fish tissue sample obtained from the
National Institute of Standards and Technol ogy (NIST) was sent to MSU WTL to be repackaged into two aliquots. One aliquot wa s forwarded to AXYS for analysis and the other aliquot was sent to the 3M E nvironmental Laboratory for analysis.

The 3M Environmental Laboratory analyzed each tissue homogenate sample and a laboratory duplicate for PFOS. As noted above , three split samples prepared from skinoff left side filets (representing 10% of the target sample number collected) were also analyzed for PFOS by AXYS. Surface water sa mples were analyzed for PFOS by the 3M Environmental Laboratory.

## Tennesee River

3M Decatur Lower Reach



### Middle Reach Upper Reach 

## LOC001

LOC002

LOC003 Flow



# Bakers Creek 0 1,000 500 Feet 

### Legend:

3M Decatur, AL Facility 

## Figure 2-1 Fish and Surface Water

Sampling Locations April 2012

Bakers Creek and Tennessee River

File: Y:\3MDec\MXD\Fish_SW_Sampling_Locs.mxd, 5/1/2012 12:09:12 PM, ricksc 

### Imagery Source: ESRI Bing Mapping Service 2011 Fish Sampling Location

Surface Water Sampling Locations\\Weston\natacc\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\Fish sampling PFOS 2012\2012 Fish Sampling Report.doc 

## 3-1 

# 3. RESULTS

A total of 26 largemouth bass were collected between the three sampling reaches during the week of April 2, 2012. Ten fish each we re collected in the upper reach above the
mouth of Bakers Creek and the middle reach at the mouth of Bakers Creek and six fish
were collected from the lower reach below th e mouth of Bakers Creek. A summary of the individual electrofishing runs including the overall elap sed times, the timer seconds recorded during which a potential was applie d by the electrofishing unit, the number of bass captured and the catch per un it effort (CPUE) is provided in Table 3-1. Total time of collection varied by reach with the upper reach requiring approximately two hours and the middle reach requiring approximately 3.5 hour s to obtain the target number of 10 fish specimens each. In contrast, a total of over 10 hours were expended to obtain the six fish specimens from the lower reach. On April 6, 2012, the last sche duled day for fish collection, efforts to collect additional specimens from the lower reach were suspended when winds of over 20 miles per hour from the north northeast prevented safe vessel operation along the lee shore.

Fish lengths, weights and skin-off filet PFO S concentrations are tabulated by sampling reach in Table 3-2 and analytical results ar e shown in Figure 3-1. The analytical data packages for analyses performed by the 3M Environmental Laborat ory are provided in Appendix A and the analytical data package fo r analyses of split samples performed by the AXYS laboratory is provided in Appendix B. While the majority of the fish were within ADEM’s target length range of 13 to 18 inches, one specimen from the middle reach slightly exceeded the ta rget range (MSF13; 18.5 inches total length). One fish in the upper reach (MSF03; 12 inches total lengt h) and three fish from the lower reach (MSF01, MSF16 and MSF22; 10.75, 12.5 and 11.25 inches total length, respectively) were below ADEM’s target range but above th e 8 inch minimum length established in the original draft Work Plan

.
Comparisons of primary sample and fiel d duplicate sample PFOS concentrations obtained from analysis by the 3M E nvironmental Laboratory indicated good correspondence with relative pe rcent difference (RPD) values ranging from 2 to 9% for\\Weston\natacc\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\Fish sampling PFOS 2012\2012 Fish Sampling Report.doc 

## 3-2 the study fish. Comparisons of split sample PFOS concentrations obtained by the AXYS laboratory of left hand filets with the re sults from the 3M Environmental Laboratory analyses of the corresponding right hand filets i ndicated less, but acceptable, agreement with RPDs ranging from 21 to 33%. The AXYS PFOS concentrations were higher than the respective 3M Environmental Laboratory PF OS concentrations for the split samples. The AXYS analyses did not include analysis of PFOS laboratory matrix spike (LMS) sample(s) at sufficiently high concentrations relative to endogenous concentrations of
PFOS for use in the evaluation of met hod performance. The 3M Environmental Laboratory analyzed PFOS LMS samples at relevant concentrations for each of the specimens and LMS recoveries ranged from 77% to 125%. (overall mean recovery ± standard deviation of 99% ± 10%).

The overall comparison of PFOS concentrations measured in all fish samples indicated good agreement between laboratories. In ge neral, PFOS concentrations reported by AXYS were greater than those from 3M for the samples. There was a systematic difference in the reported PFOS concentrations between both laboratori es, but this is not unexpected given the potential difference in analytical methodologies used at each laboratory (Lindström et al. 2009). For instance, the use of linear isomer PFOS
calibration with a 499 to 80 MS /MS transition for data acqu isition by AXYS but not by the 3M Environmental Laboratory can bi as high the quantification of mixed branched/linear PFOS in environmental sample s by 8% (Riddell et al. 2009). Given what is known about the variability in the quantific ation of PFOS in biol ogical tissues, results from this interlaboratory comparison reinfor ce the validity of the results of this study.

Summary statistics for the largemouth bass filet tissue PFOS concentrations obtained by the 3M Environmental Laboratory analysis of primary (right hand filet) samples are provided in Table 3-3. Median largemouth ba ss filet tissue PFOS concentrations were 624, 1930 and 979 ng/g for the upper, middle a nd lower reaches, respectively and 852 ng/g for the combined data set (all reaches). Fish filet concentrati on data for each of the reaches is depicted in box plots (Figure 3- 2). A scatter plot of PFOS and specimen length
indicates no correlation between conc entration and length (Figure 3-3).\\Weston\natacc\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\Fish sampling PFOS 2012\2012 Fish Sampling Report.doc 

## 3-3 Only one of three intended sets of water sa mples were collected. Collection of a second set was planned for April 6, 2012 but, as previo usly noted, unsafe c onditions on the river precluded this action. The in tended splitting of water samp les with the AXYS laboratory did not occur, in part due to the accelerat ed pace of this study. Surface water PFOS concentrations and routine water quality para meters are tabulated in Table 3-4 and shown in Figure 3-2.

## Tennesee River

3M Decatur Lower Reach



### Middle Reach Upper Reach 

## Flow



# Bakers Creek LOC001

LOC002

LOC003

0 1,000 500 Feet 

### Legend:

3M Decatur, AL Facility 

## Figure 3-1 Largemouth Bass Filet PFOS Concentrations April 2012

Bakers Creek and Tennessee River

File: Y:\3MDec\MXD\Largemouth_Bass_PFOS_April2012.mxd, 5/9/2012 9:56:43 AM, ricksc 

### Imagery Source: ESRI Bing Mapping Service 2011 Fish Sampling Location

Surface Water Sampling Locations

Note: PFOS concentrations are the average of primary and duplicate sample analytical results on a wet weight basis. 

### Middle Reach PFOS ( ng/g) MSF02 4240 MSF07 2920 MSF08 1360 MSF09 2020 MSF27 (MSF09D) 2120 MSF10 1840 MSF11 2940 MSF11D (AXYS) 3720 MSF11D (AXYS Dup) 3510 MSF12 526 MSF13 950 MSF14 3370 MSF15 754 

### Lower Reach PFOS ( ng/g) MSF01 4770 MSF16 1520 MSF17 165 MSF28 (MSF17D) 180 MSF24 437 MSF24D (AXYS) 537 MSF25 306 MSF26 2090 MSF29 (MSF26D) 2050

Upper Reach PFOS ( ng/g) MSF03 70.7 MSF04 576 MSF05 471 MSF05D (AXYS) 656 MSF06 156 MSF18 701 MSF19 675 MSF20 1180 MSF21 671 MSF22 4660 MSF23 52.5

## Figure 3-2 Largemouth Bass Filet PFOS Concentration Box Plots

0.0 1000.0 2000.0 3000.0 4000.0 5000.0

Combined Lower Middle Upper 

# ReachPFOS (ng/g)

Whiskers ( T ) denote the largest (and smallest) adjacent values within 1.5 times the interquartile range (IQR)

Red dot denotes an outlier greater than 1.5 times the IQR above the upper quartile (75 th percentile) value3000.04000.05000.0

PFOS (ng/g)Figure3‐3LargemouthBassPFOSConcentrationsvs.LengthUpperMiddle0.01000.02000.00.00 5.00 10.00 15.00 20.00Length(inches)Lower

### 3M Decatur Lower Reach



### Middle Reach Upper Reach 

## Tennesee River

Flow



# Bakers Creek 0 1,000 500 Feet 

### Legend:

3M Decatur, AL Facility 

## Figure 3-4 Surface Water PFOS Concentrations April 2012

Bakers Creek and Tennessee River

File: Y:\3MDec\MXD\Surface_Water_PFOS_April2012.mxd, 5/10/2012 10:45:30 AM, ricksc 

### Imagery Source: ESRI Bing Mapping Service 2011 Fish Sampling Location

Surface Water Sampling Locations

Note: PFOS concentrations are the average of primary and duplicate sample analytical results.



# Sample ID PFOS ( ng/mL) LOC001 0.450

Sample ID PFOS ( ng/mL) LOC002 0.691

Sample ID PFOS ( ng/mL) LOC003 0.0237Table 3-1Fish Sampling Summary and Catch Per Unit EffortDate Run Reach HoursTimer(seconds)Timer(hours)Bass(count)CPUE(bass/hour)CPUE(bass/timerhours)4/3/2012 1 Lower 1.00 1355 0.38 1 1.00 2.664/3/2012 2 Middle 1.00 1680 0.47 1 1.00 2.144/3/2012 3 Upper 1.00 1939 0.54 4 4.00 7.434/3/2012 4 Middle 1.08 1897 0.53 9 8.31 17.084/4/2012 1 & 2 Lower 2.00 3459 0.96 2 1.00 2.084/4/2012 3 Upper 1.25 2253 0.63 2 1.60 3.204/4/2012 4 Upper 1.20 1112 0.31 4 3.33 12.954/4/2012 5 Lower 1.00 1809 0.50 0 0.00 0.004/4/2012 6 Lower 1.00 1525 0.42 0 0.00 0.004/5/2012 1 Lower 1.17 2071 0.58 1 0.86 1.744/5/2012 2 Lower 1.25 2020 0.56 0 0.00 0.004/5/2012 3 Lower 2.00 2806 0.78 1 0.50 1.284/6/2012 1 Lower 0.67 1291 0.36 1 1.50 2.79SummaryTotal Total HoursTotalTimer(seconds)TotalTimer(hours)TotalBass(count)AverageCPUE(bass/hour)Average CPUE(bass/timerhours)Lower Reach9 10.08 16336 4.54 6 0.61 1.32Middle Reach2 2.08 3577 1 10 4.65 9.61Upper Reach3 3.45 5304 1.47 10 2.98 7.86Overall14 15.62 25217 7.00 26 1.78 4.10Notes:CPUE = Catch per unit effortTimer seconds record the number of seconds that the electrofisher potential was appliedTable 3-2Fish Morphometrics and PFOS ConcentrationsSample ID Date Analytical LaboratorySamplingReachLength(inches)Weight(pounds)PFOS Concentration(ng/g)MSF03 4/3/2012 3M Environmental Laboratory Upper 12.00 0.9 70.7MSF04 4/3/2012 3M Environmental Laboratory Upper 14.75 1.7 576MSF05 4/3/2012 3M Environmental Laboratory Upper 17.75 2.9 471MSF05D 4/3/2012 AXYS Laboratory Upper " " 656MSF06 4/3/2012 3M Environmental Laboratory Upper 14.00 1.5 156MSF18 4/4/2012 3M Environmental Laboratory Upper 15.75 2.5 701MSF19 4/4/2012 3M Environmental Laboratory Upper 14.75 1.8 675MSF20 4/4/2012 3M Environmental Laboratory Upper 14.25 1.0 1180MSF21 4/4/2012 3M Environmental Laboratory Upper 17.00 2.8 671MSF22 4/4/2012 3M Environmental Laboratory Upper 11.25 0.8 4660MSF23 4/4/2012 3M Environmental LaboratoryUpper17.50 3.1 52.5MSF02 4/3/2012 3M Environmental Laboratory Middle 14.50 1.8 4240MSF07 4/3/2012 3M Environmental Laboratory Middle 16.00 2.2 2920MSF08 4/3/2012 3M Environmental Laboratory Middle 13.50 1.3 1360MSF09 4/3/2012 3M Environmental Laboratory Middle 13.25 1.2 2020MSF09D (MSF27) 4/3/2012 3M Environmental Laboratory Middle " " 2120MSF10 4/3/2012 3M Environmental Laboratory Middle 14.00 1.7 1840MSF11 4/3/2012 3M Environmental Laboratory Middle 15.375 2.0 2940MSF11D 4/3/2012 AXYS Laboratory Middle " " 3720MSF11D (Duplicate) 4/3/2012 AXYS Laboratory Middle " " 3510MSF12 4/3/2012 3M Environmental Laboratory Middle 15.50 2.1 526MSF13 4/3/2012 3M Environmental Laboratory Middle 18.50 3.3 950MSF14 4/3/2012 3M Environmental Laboratory Middle 17.50 3.6 3370MSF15 4/3/2012 3M Environmental LaboratoryMiddle 17.50 3.3 754MSF01 4/3/2012 3M Environmental Laboratory Lower 10.75 0.5 4770MSF16 4/4/2012 3M Environmental Laboratory Lower 12.50 1.0 1520MSF17 4/4/2012 3M Environmental Laboratory Lower 13.75 1.2 165MSF17D (MSF28) 4/4/2012 3M Environmental Laboratory Lower " " 180MSF24 4/5/2012 3M Environmental Laboratory Lower 16.00 2.1 437MSF24D 4/5/2012 AXYS Laboratory Lower " " 537MSF25 4/5/2012 3M Environmental Laboratory Lower 16.50 2.1 306MSF26 4/5/2012 3M Environmental Laboratory Lower 15.00 1.7 2090MSF26D (MSF29) 4/5/2012 3M Environmental LaboratoryLower" " 2050Notes:PFOS concentrations are the average of the primary and duplicate analytical results expresssed in ng/g (ppb) on a wet weight basisSample IDs with a "D" suffix are field duplicates obtained from left side filet samplesTable 3-3Largemouth Bass PFOS Concentration Summary StatisticsParameterUpper Reach Middle Reach Lower Reach Combined ReachesMinimum 52.5 526 165 52.5Maximum 4660 4240 4770 4770Mean 921 2092 1548 1516Median 624 1930 979 852Geometric Mean 440 1725 833 863Standard Deviation 1358 1238 1753 1451Notes:PFOS concentrations in ng/g (wet weight).Summary statistics obtained from primary data (field duplicate / split sample data not included).Table 3-4Surface Water DataLower Reach Middle Reach Upper ReachSample Station ID LOC001 LOC002 LOC003Northing (Decimal degrees) 34.644 34.638 34.637Westing (Decimal degrees) 87.035 87.029 87.021Date 04/05/12 04/05/12 04/05/12Time 9:50 10:17 10:37Temperature (°C) 21.63 21.77 21.5Specific conductance (μs/cm) 189 187 193Dissolved oxygen (mg/L) 7.74 9.75 8.13pH (S.U.) 7.33 8.13 7.56Turbidity (NTU) 35.2 23.5 21.5Average PFOS (ng/mL) 0.450 0.691 0.0237Notes:Average PFOS concentration is the average of primary and duplicate analytical results in ng/mL (ppb)\\Weston\natacc\FOLDERS.0-9\3M-DECAT\Phase 3 Work Plan\Fish sampling PFOS 2012\2012 Fish Sampling Report.doc 

## 4-1 

# 4. REFERENCES

EPA. 2000. Guidance for Assessing Chemical C ontaminant Data for Use in Fish Advisories, Volume I, Fish Sampling and Analysis . Third Addition. EPA. Office of Water. Washington, District of Columbia.

EPA. 1993. Fish Field and Laboratory Methods for Evaluating the Biological Integrity of Surface Waters . EPA. Environmental Monitoring Sy stems Laboratory. Cincinnati, OH.

Reynolds. J.B. 1996. Electrofishing. Page s 221-254 in B.R. Murphy and D.W. Willis
editors. Fisheries Techniques
, Second Edition . American Fisheries Society. Bethesda,
MD.

WESTON 2008. Perfluorinated Sulfonates Data Repor t, 3M Decatur, Alabama Facility,
Site-Related Environm ental Monitoring Program , September 2008, Weston Solutions, Inc., West Chester, PA.

Lindström G., Karrman A., and van Bavel B. (2009). Accuracy and precision in the determination of perfluorinated chemicals in human blood verified by interlaboratory comparisons. J. Chromatogr. A 1216: 394-400.

Riddell N, Arsenault G., Chittim B., Martin JW., McAlees A., and McCrindle R. (2009). Branched perfluorooctane sulf onate isomer quantification and characterization in blood serum samples by HPLC/ESI-MS/(/MS). Environ. Sci. Technol. 43: 7902-7908.

WESTON. 2012. Amended Work Plan for Fish Samp ling and Analysis for PFOS in Largemouth Bass in the Tennessee River in the Vicinity of the 3M Decatur Facility

. Weston Solutions, Inc., West Chester, PA.

# APPENDIX A 3M ENVIRONMENTAL LABORATORY ANALYTICAL DATA PACKAGES

# APPENDIX B AXYS LABORATORY ANALYTICAL DATA PACKAGE2045 Mills Road West TEL 250-655-5800 FAX 250-655-5811 SIDNEY, BRITISH COLUMBIA, CANADA V8L 5X2 

### www.axysanalytical.com



# AXYS Client No.: 4673

Client Address: Cardno ENTRIX 4295 Okemos Road, Suite 101 Okemos, MI, US, 48864

The AXYS contact for these data is Kalai Pillay.

### Batch ID: WG39768 Date:

Analysis Type: Matrix Type: Tissue

Contract: 4673 Blank: Samples: WG39768-101

L17838-1 Reference Tiss. TCR11-0039 L17838-2 MSF05D 120403 L17838-3 MSF11D 120403 L17838-4 MSF24D 120405
Reference or Spike: WG39768-102 WG39768-104 WG39768-105

Duplicate:

WG39768-103

Comments:

1. Data are not blank corrected.

FQA-006 Rev. 2. 18-Jul-1994 Copyright AXYS Analytical Services Ltd



# BATCH SUMMARY

February 1993 27-Apr-2012



# BATCH MAKEUP Perfluorinated Organic(1) Where applicable, custom lab flags have been used on this report.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_L17838

- 1_Form1A_FC2G_157S24_SJ1453688.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. Reference Tiss. TCR11-0039 Sample Collection: N/A Form 1A PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: L17838-1

Matrix: TISSUE Sample Size: 2.00 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 00:32:37 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 24

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng/g (wet weight basis)
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
COMPOUND LAB FLAG 1 CONC. FOUND REPORTING LIMIT (RL) 2 RETENTION TIME

PFOS 7.16 1.00 (L) 8:17



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-1_Form1A_FC2G_157S24_SJ1453688.html)(1) Where applicable, custom lab flags have been used on this report.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_L17838

- 1_Form2_FC2G_157S24_SJ1453688.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. Reference Tiss. TCR11-0039 Sample Collection: N/A Form 2 PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: L17838-1

Matrix: TISSUE Sample Size: 2.00 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 00:32:37 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 24

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng absolute
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
LABELED COMPOUND LAB FLAG 1 SPIKE

CONC. CONC.

FOUND R(%) 2 RETENTION TIME

13C4-PFOS 36.0 31.5 87.6 8:17

CLEANUP STANDARD

13C8-PFOA 12.0 10.6 88.5 7:04



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-1_Form2_FC2G_157S24_SJ1453688.html)(1) Where applicable, custom lab flags have been used on this report.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_L17838

- 2_Form1A_FC2G_157S28_SJ1453692.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. MSF05D 120403 Sample Collection: 03-Apr-2012 Form 1A PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: L17838-2 (A)

Matrix: TISSUE Sample Size: 2.11 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 01:39:33 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 28

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng/g (wet weight basis)
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
COMPOUND LAB FLAG 1 CONC. FOUND REPORTING LIMIT (RL) 2 RETENTION TIME

PFOS 656 0.948 (L) 8:17



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-2_Form1A_FC2G_157S28_SJ1453692.html)(1) Where applicable, custom lab flags have been used on this report.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_L17838

- 2_Form2_FC2G_157S28_SJ1453692.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. MSF05D 120403 Sample Collection: 03-Apr-2012 Form 2 PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: L17838-2 (A)

Matrix: TISSUE Sample Size: 2.11 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 01:39:33 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 28

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng absolute
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
LABELED COMPOUND LAB FLAG 1 SPIKE

CONC. CONC.

FOUND R(%) 2 RETENTION TIME

13C4-PFOS 36.0 28.4 79.0 8:17

CLEANUP STANDARD

13C8-PFOA 12.0 9.77 81.5 7:06



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-2_Form2_FC2G_157S28_SJ1453692.html)(1) Where applicable, custom lab flags have been used on this report; D = dilution data.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_L17838

- 3_Form1A_FC2G_158S8_SJ1453777.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. MSF11D 120403 Sample Collection: 03-Apr-2012 Form 1A PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: L17838-3 N (A)

Matrix: TISSUE Sample Size: 2.15 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 16:11:38 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_158 S: 8

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: 5 Cal. Ver. Data Filename: FC2G_158 S: 4

Concentration Units: ng/g (wet weight basis)
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
COMPOUND LAB FLAG 1 CONC. FOUND REPORTING LIMIT (RL) 2 RETENTION TIME

PFOS D 3720 4.65 (L) 8:21



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-3_Form1A_FC2G_158S8_SJ1453777.html)(1) Where applicable, custom lab flags have been used on this report; D = dilution data.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_L17838

- 3_Form2_FC2G_158S8_SJ1453777.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. MSF11D 120403 Sample Collection: 03-Apr-2012 Form 2 PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: L17838-3 N (A)

Matrix: TISSUE Sample Size: 2.15 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 16:11:38 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_158 S: 8

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: 5 Cal. Ver. Data Filename: FC2G_158 S: 4

Concentration Units: ng absolute
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
LABELED COMPOUND LAB FLAG 1 SPIKE

CONC. CONC.

FOUND R(%) 2 RETENTION TIME

13C4-PFOS D 36.0 20.4 56.5 8:21

CLEANUP STANDARD

13C8-PFOA D 12.0 8.90 74.2 7:06



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-3_Form2_FC2G_158S8_SJ1453777.html)(1) Where applicable, custom lab flags have been used on this report.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_L17838

- 4_Form1A_FC2G_157S27_SJ1453691.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. MSF24D 120405 Sample Collection: 05-Apr-2012 Form 1A PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: L17838-4

Matrix: TISSUE Sample Size: 2.05 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 01:22:47 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 27

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng/g (wet weight basis)
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
COMPOUND LAB FLAG 1 CONC. FOUND REPORTING LIMIT (RL) 2 RETENTION TIME

PFOS 537 0.976 (L) 8:17



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-4_Form1A_FC2G_157S27_SJ1453691.html)(1) Where applicable, custom lab flags have been used on this report.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_L17838

- 4_Form2_FC2G_157S27_SJ1453691.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. MSF24D 120405 Sample Collection: 05-Apr-2012 Form 2 PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: L17838-4

Matrix: TISSUE Sample Size: 2.05 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 01:22:47 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 27

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng absolute
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
LABELED COMPOUND LAB FLAG 1 SPIKE

CONC. CONC.

FOUND R(%) 2 RETENTION TIME

13C4-PFOS 36.0 27.3 75.9 8:17

CLEANUP STANDARD

13C8-PFOA 12.0 10.8 90.3 7:06



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_L17838-4_Form2_FC2G_157S27_SJ1453691.html)(1) Where applicable, custom lab flags have been used on this report; U = not detected at RL.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39768

- 101_Form1A_FC2G_157S22_SJ1453684.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. Lab Blank Sample Collection: N/A Form 1A PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. N/A
Contract No.: 4673 Lab Sample I.D.: WG39768-101

Matrix: TISSUE Sample Size: 2.00 g

Sample Receipt Date: N/A Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 24-Apr-2012 Time: 23:59:06 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 22

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng/g
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
COMPOUND LAB FLAG 1 CONC. FOUND REPORTING LIMIT (RL) 2 RETENTION TIME

PFOS U 1.00 (L)



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-101_Form1A_FC2G_157S22_SJ1453684.html)(1) Where applicable, custom lab flags have been used on this report.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39768

- 101_Form2_FC2G_157S22_SJ1453684.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. Lab Blank Sample Collection: N/A Form 2 PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. N/A
Contract No.: 4673 Lab Sample I.D.: WG39768-101

Matrix: TISSUE Sample Size: 2.00 g

Sample Receipt Date: N/A Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 24-Apr-2012 Time: 23:59:06 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 22

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng absolute
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
LABELED COMPOUND LAB FLAG 1 SPIKE

CONC. CONC.

FOUND R(%) 2 RETENTION TIME

13C4-PFOS 36.0 33.2 92.3 8:17

CLEANUP STANDARD

13C8-PFOA 12.0 11.2 93.7 7:04



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-101_Form2_FC2G_157S22_SJ1453684.html)(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________
These pages are part of a larger report that may contain information necessary for full data evaluation. Results reported relate only to the sample tested.

For Axys Internal Use Only [ XSL Template: FC-Form8A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39768

- 102_Form8A_SJ1453676.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 Form 8A PERFLUORINATED ORGANICS ONGOING PRECISION AND RECOVERY (OPR) AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Contract No.: 4673 Lab Sample I.D.: WG39768-102

Matrix: TISSUE Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS
Analysis Date: 24-Apr-2012 Time: 22:51:55 Column ID: C18MS Extract Volume (uL): 4000 OPR Data Filename: FC2G_157 S: 18 Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

ALL CONCENTRATIONS REPORTED ON THIS FORM ARE CONCENTRATIONS IN EXTRACT, BASED ON A 1 mL EXTRACT VOLUME.

COMPOUND LAB FLAG 1 SPIKE CONC. (ng/mL) CONC. FOUND (ng/mL) % RECOVERY RETENTION TIME

PFOS 80.0 87.1 109 8:17



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-102_Form8A_SJ1453676.html)(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________
These pages are part of a larger report that may contain information necessary for full data evaluation. Results reported relate only to the sample tested.

For Axys Internal Use Only [ XSL Template: FC-Form8B.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39768

- 102_Form8B_SJ1453676.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 Form 8B PERFLUORINATED ORGANICS ONGOING PRECISION AND RECOVERY (OPR) AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Contract No.: 4673 Lab Sample I.D.: WG39768-102
Matrix: TISSUE Initial Calibration Date: 24-Apr-2012
Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS Analysis Date: 24-Apr-2012 Time: 22:51:55 Column ID: C18MS Extract Volume (uL): 4000 OPR Data Filename: FC2G_157 S: 18 Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22
Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

ALL CONCENTRATIONS REPORTED ON THIS FORM ARE CONCENTRATIONS IN EXTRACT, BASED ON A 1 mL EXTRACT VOLUME.

LABELED COMPOUND LAB FLAG 1 SPIKE CONC. (ng/mL) CONC. FOUND (ng/mL) % RECOVERY RETENTION TIME

13C4-PFOS 36.0 29.0 80.5 8:17

CLEANUP STANDARD

13C8-PFOA 12.0 11.2 93.3 7:04



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-102_Form8B_SJ1453676.html)(1) Where applicable, custom lab flags have been used on this report; D = dilution data.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39768

- 103_Form1A_FC2G_158S9_SJ1453778.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. MSF11D 120403 (Duplicate) Sample Collection: 03-Apr-2012 Form 1A PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: WG39768-103 N (DUP L17838-3)

Matrix: TISSUE Sample Size: 2.07 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 16:28:24 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_158 S: 9

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: 5 Cal. Ver. Data Filename: FC2G_158 S: 4

Concentration Units: ng/g (wet weight basis)
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
COMPOUND LAB FLAG 1 CONC. FOUND REPORTING LIMIT (RL) 2 RETENTION TIME

PFOS D 3510 4.83 (L) 8:21



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-103_Form1A_FC2G_158S9_SJ1453778.html)(1) Where applicable, custom lab flags have been used on this report; D = dilution data.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39768

- 103_Form2_FC2G_158S9_SJ1453778.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. MSF11D 120403 (Duplicate) Sample Collection: 03-Apr-2012 Form 2 PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: WG39768-103 N (DUP L17838-3)

Matrix: TISSUE Sample Size: 2.07 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 16:28:24 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_158 S: 9

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: 5 Cal. Ver. Data Filename: FC2G_158 S: 4

Concentration Units: ng absolute
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
LABELED COMPOUND LAB FLAG 1 SPIKE

CONC. CONC.

FOUND R(%) 2 RETENTION TIME

13C4-PFOS D 36.0 25.9 72.0 8:21

CLEANUP STANDARD

13C8-PFOA D 12.0 10.7 89.2 7:06



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-103_Form2_FC2G_158S9_SJ1453778.html)(1) Where applicable, custom lab flags have been used on this report.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39768

- 104_Form1A_FC2G_157S29_SJ1453693.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. MSF05D 120403 (MS) Sample Collection: 03-Apr-2012 Form 1A PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: WG39768-104 (MS)

Matrix: TISSUE Sample Size: 2.01 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 01:56:19 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 29

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng/g (wet weight basis)
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
COMPOUND LAB FLAG 1 CONC. FOUND REPORTING LIMIT (RL) 2 RETENTION TIME

PFOS 670 0.995 (L) 8:17



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-104_Form1A_FC2G_157S29_SJ1453693.html)(1) Where applicable, custom lab flags have been used on this report.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39768

- 104_Form2_FC2G_157S29_SJ1453693.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. MSF05D 120403 (MS) Sample Collection: 03-Apr-2012 Form 2 PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: WG39768-104 (MS)

Matrix: TISSUE Sample Size: 2.01 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 01:56:19 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 29

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng absolute
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
LABELED COMPOUND LAB FLAG 1 SPIKE

CONC. CONC.

FOUND R(%) 2 RETENTION TIME

13C4-PFOS 36.0 35.4 98.2 8:17

CLEANUP STANDARD

13C8-PFOA 12.0 11.0 91.3 7:06



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-104_Form2_FC2G_157S29_SJ1453693.html)(1) Where applicable, custom lab flags have been used on this report.

(2) Reporting Limit (Code): S = sample detection limit; M = method detection limit; L = lowest calibration level equivalent; Q = contract defined limit.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39768

- 105_Form1A_FC2G_157S30_SJ1453694.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. MSF05D 120403 (MSD) Sample Collection: 03-Apr-2012 Form 1A PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: WG39768-105 (MSD)

Matrix: TISSUE Sample Size: 2.11 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 02:13:05 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 30

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng/g (wet weight basis)
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
COMPOUND LAB FLAG 1 CONC. FOUND REPORTING LIMIT (RL) 2 RETENTION TIME

PFOS 653 0.948 (L) 8:17



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-105_Form1A_FC2G_157S30_SJ1453694.html)(1) Where applicable, custom lab flags have been used on this report.

(2) R(%) = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39768

- 105_Form2_FC2G_157S30_SJ1453694.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. MSF05D 120403 (MSD) Sample Collection: 03-Apr-2012 Form 2 PERFLUORINATED ORGANICS ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: WG39768-105 (MSD)

Matrix: TISSUE Sample Size: 2.11 g (wet)

Sample Receipt Date: 19-Apr-2012 Initial Calibration Date: 24-Apr-2012

Extraction Date: 23-Apr-2012 Instrument ID: LC MS/MS

Analysis Date: 25-Apr-2012 Time: 02:13:05 Column ID: C18MS

Extract Volume (uL): 4000 Sample Data Filename: FC2G_157 S: 30

Injection Volume (uL): 15 Blank Data Filename: FC2G_157 S: 22

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_157 S: 15

Concentration Units: ng absolute
This page is part of a total report that contains information necessary for accreditation compliance. Results are compliant with NELAP accreditation described in the total report. Sample results relate only to the sample tested.
LABELED COMPOUND LAB FLAG 1 SPIKE

CONC. CONC.

FOUND R(%) 2 RETENTION TIME

13C4-PFOS 36.0 37.1 103 8:17

CLEANUP STANDARD

13C8-PFOA 12.0 10.9 91.1 7:04



## Page 1 of 1 (WG39768 - PFC_FC_LC_PFOA_WG39768-105_Form2_FC2G_157S30_SJ1453694.html)(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Kristina Coleman

___________

For Axys Internal Use Only [ XSL Template: FC-Form3A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_24

- Apr

- 2012_FC2G__Form3A_GS45507.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 Form 3A PERFLUORINATED ORGANICS INITIAL CALIBRATION PERCENT RECOVERIES

AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 CS0 Data Filename: FC2G_157 S: 4
Initial Calibration Date: 24-Apr-2012 CS1 Data Filename: FC2G_157 S: 5

Instrument ID: LC MS/MS CS2 Data Filename: FC2G_157 S: 6

LC Column ID: C18MS CS3 Data Filename: FC2G_157 S: 7

CS4 Data Filename: FC2G_157 S: 8

CS5 Data Filename: FC2G_157 S: 9

CS6 Data Filename: FC2G_157 S: 10

CS7 Data Filename: FC2G_157 S: 11

CS8 Data Filename: N/A

PERCENT RECOVERY (%) CS0 CS1 CS2 CS3 CS4 CS5 CS6 CS7 CS8 COMPOUND LAB FLAG 1

PFOS 104 91.9 86.4 105 99.5 112 101 99.7



## Page 1 of 1 (WG39768 - PFOA_FC_LC_24-Apr-2012_FC2G__Form3A_GS45507.html)(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Kristina Coleman

___________

For Axys Internal Use Only [ XSL Template: FC-Form3B.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_24

- Apr

- 2012_FC2G__Form3B_GS45507.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 Form 3B PERFLUORINATED ORGANICS INITIAL CALIBRATION PERCENT RECOVERIES

AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 CS0 Data Filename: FC2G_157 S: 4
Initial Calibration Date: 24-Apr-2012 CS1 Data Filename: FC2G_157 S: 5

Instrument ID: LC MS/MS CS2 Data Filename: FC2G_157 S: 6

LC Column ID: C18MS CS3 Data Filename: FC2G_157 S: 7

CS4 Data Filename: FC2G_157 S: 8

CS5 Data Filename: FC2G_157 S: 9

CS6 Data Filename: FC2G_157 S: 10

CS7 Data Filename: FC2G_157 S: 11

CS8 Data Filename: N/A

PERCENT RECOVERIES (%) CS0 CS1 CS2 CS3 CS4 CS5 CS6 CS7 CS8 LABELED COMPOUND LAB FLAG 1

13C4-PFOS 103 82.4 92.7 86.9 104 103 111 117

CLEAN-UP STANDARD

13C8-PFOA 101 99.6 94.3 98.3 101 98.9 103 104



## Page 1 of 1 (WG39768 - PFOA_FC_LC_24-Apr-2012_FC2G__Form3B_GS45507.html)(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Kristina Coleman

___________

For Axys Internal Use Only [ XSL Template: FC-Form3C.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_24

- Apr

- 2012_FC2G__Form3C_GS45507.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 Form 3C PERFLUORINATED ORGANICS INITIAL CALIBRATION RETENTION TIMES

AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 CS0 Data Filename: FC2G_157 S: 4
Initial Calibration Date: 24-Apr-2012 CS1 Data Filename: FC2G_157 S: 5

Instrument ID: LC MS/MS CS2 Data Filename: FC2G_157 S: 6

LC Column ID: C18MS CS3 Data Filename: FC2G_157 S: 7

CS4 Data Filename: FC2G_157 S: 8

CS5 Data Filename: FC2G_157 S: 9

CS6 Data Filename: FC2G_157 S: 10

CS7 Data Filename: FC2G_157 S: 11

CS8 Data Filename: N/A

RETENTION TIMES CS0 CS1 CS2 CS3 CS4 CS5 CS6 CS7 CS8 MEAN RT COMPOUND LAB FLAG 1

PFOS 8:17 8:17 8:17 8:17 8:17 8:17 8:17 8:17 8:17



## Page 1 of 1 (WG39768 - PFOA_FC_LC_24-Apr-2012_FC2G__Form3C_GS45507.html)(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Kristina Coleman

___________

For Axys Internal Use Only [ XSL Template: FC-Form3D.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_24

- Apr

- 2012_FC2G__Form3D_GS45507.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 Form 3D PERFLUORINATED ORGANICS INITIAL CALIBRATION RETENTION TIMES

AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 CS0 Data Filename: FC2G_157 S: 4
Initial Calibration Date: 24-Apr-2012 CS1 Data Filename: FC2G_157 S: 5

Instrument ID: LC MS/MS CS2 Data Filename: FC2G_157 S: 6

LC Column ID: C18MS CS3 Data Filename: FC2G_157 S: 7

CS4 Data Filename: FC2G_157 S: 8

CS5 Data Filename: FC2G_157 S: 9

CS6 Data Filename: FC2G_157 S: 10

CS7 Data Filename: FC2G_157 S: 11

CS8 Data Filename: N/A

RETENTION TIMES CS0 CS1 CS2 CS3 CS4 CS5 CS6 CS7 CS8 MEAN RT LABELED COMPOUND LAB FLAG 1

13C4-PFOS 8:17 8:17 8:17 8:17 8:21 8:17 8:17 8:17 8:18

CLEAN-UP STANDARD

13C8-PFOA 7:04 7:04 7:04 7:04 7:04 7:04 7:04 7:04 7:04



## Page 1 of 1 (WG39768 - PFOA_FC_LC_24-Apr-2012_FC2G__Form3D_GS45507.html)(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form4A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_FC2G_157S15__Form4A_SJ1453671.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 Form 4A PERFLUORINATED ORGANICS CALIBRATION VERIFICATION AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Initial Calibration Date: 24-Apr-2012 VER Data Filename: FC2G_157 S: 15

Instrument ID: LC MS/MS Analysis Date: 24-Apr-2012

LC Column ID: C18MS Analysis Time: 22:01:37

COMPOUND LAB FLAG 1 RETENTION TIME EXPECTED CONC. (ng) CONC. FOUND (ng) RECOVERY (%)

PFOS 8:17 80.0 86.8 108



## Page 1 of 1 (WG39768 - PFOA_FC_LC_FC2G_157S15__Form4A_SJ1453671.html)(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form4B.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_FC2G_157S15__Form4B_SJ1453671.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 Form 4B PERFLUORINATED ORGANICS CALIBRATION VERIFICATION AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Initial Calibration Date: 24-Apr-2012 VER Data Filename: FC2G_157 S: 15

Instrument ID: LC MS/MS Analysis Date: 24-Apr-2012

LC Column ID: C18MS Analysis Time: 22:01:37

LABELED COMPOUND LAB FLAG 1 RETENTION TIME EXPECTED CONC. (ng) CONC. FOUND (ng) RECOVERY (%)

13C4-PFOS 8:17 36.0 36.0 100

CLEANUP STANDARD

13C8-PFOA 7:06 12.0 12.1 101



## Page 1 of 1 (WG39768 - PFOA_FC_LC_FC2G_157S15__Form4B_SJ1453671.html)(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form4A.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_FC2G_158S4__Form4A_SJ1453773.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 Form 4A PERFLUORINATED ORGANICS CALIBRATION VERIFICATION AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Initial Calibration Date: 24-Apr-2012 VER Data Filename: FC2G_158 S: 4

Instrument ID: LC MS/MS Analysis Date: 25-Apr-2012

LC Column ID: C18MS Analysis Time: 15:04:34

COMPOUND LAB FLAG 1 RETENTION TIME EXPECTED CONC. (ng) CONC. FOUND (ng) RECOVERY (%)

PFOS 8:17 80.0 81.1 101



## Page 1 of 1 (WG39768 - PFOA_FC_LC_FC2G_158S4__Form4A_SJ1453773.html)(1) Where applicable, custom lab flags have been used on this report.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________

For Axys Internal Use Only [ XSL Template: FC-Form4B.xsl; Created: 27-Apr-2012 14:59:50; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_FC2G_158S4__Form4B_SJ1453773.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 Form 4B PERFLUORINATED ORGANICS CALIBRATION VERIFICATION AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811

Initial Calibration Date: 24-Apr-2012 VER Data Filename: FC2G_158 S: 4

Instrument ID: LC MS/MS Analysis Date: 25-Apr-2012

LC Column ID: C18MS Analysis Time: 15:04:34

LABELED COMPOUND LAB FLAG 1 RETENTION TIME EXPECTED CONC. (ng) CONC. FOUND (ng) RECOVERY (%)

13C4-PFOS 8:21 36.0 28.3 78.6

CLEANUP STANDARD

13C8-PFOA 7:06 12.0 11.8 98.3



## Page 1 of 1 (WG39768 - PFOA_FC_LC_FC2G_158S4__Form4B_SJ1453773.html)(1) Where applicable, custom lab flags have been used on this report; D = dilution data.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________
These pages are part of a larger report that may contain information necessary for full data evaluation. Results reported relate only to the sample tested.

For Axys Internal Use Only [ XSL Template: RPD.xsl; Created: 27-Apr-2012 15:00:24; Application: XMLTransformer-1.12.13; Report Filename: RPD_FC_LC_PFOA

- RPD_WG39768

- 103_L17838

- 3_.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 PERFLUORINATED ORGANICS ANALYSIS REPORT RELATIVE PERCENT DIFFERENCE AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Client ID: MSF11D 120403 Concentration Units: ng/g (wet weight basis)
L17838-3 (A) WG39768-103 COMPOUND LAB FLAG 1 CONC.

FOUND LAB

FLAG 1 CONC.

FOUND MEAN RELATIVE PERCENT DIFFERENCE PFOS D 3720 D 3510 3620 5.77



## Page 1 of 1 (WG39768 - RPD_FC_LC_PFOA-RPD_WG39768-103_L17838 -3_.html)(1) Where applicable, custom lab flags have been used on this report.

(2) R% = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________
These pages are part of a larger report that may contain information necessary for full data evaluation. Results reported relate only to the sample tested.

For Axys Internal Use Only [ XSL Template: MS.xsl; Created: 27-Apr-2012 15:00:16; Application: XMLTransformer-1.12.13; Report Filename: MS_FC_LC_PFOA

- MS

- MSD_WG39768

- 104_L17838

- 2_Form8C.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. MSF05D 120403 (MS) Sample Collection: 03-Apr-2012 Form 8C PERFLUORINATED ORGANICS MATRIX SPIKE (MS)

ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: WG39768-104 (MS)
Matrix: TISSUE Sample Size: 2.01 g (wet)
Extraction Date: 23-Apr-2012 Initial Calibration Date: 24-Apr-2012 Analysis Date: 25-Apr-2012 Time: 01:56:19 Instrument ID: LC MS/MS Extract Volume (uL): 4000 Column ID: C18MS Injection Volume (uL): 15 MS Data Filename: FC2G_157 S: 29
Dilution Factor: N/A Blank Data Filename: FC2G_157 S: 22
Cal. Ver. Data Filename: FC2G_157 S: 15

ALL CONCENTRATIONS REPORTED ON THIS FORM ARE CONCENTRATIONS ON SAMPLE SIZE BASIS

COMPOUND LAB FLAG 1 ION

ABUND. RATIO SPIKE

CONC (ng/g) SAMPLE

LAB FLAG 1 SAMPLE

CONC (ng/g) CONC.

FOUND (ng/g) MS

R% 2 REL

% DIFF

PFOS N/A 39.8 656 670 36.4



## Page 1 of 1 (WG39768 - MS_FC_LC_PFOA-MS-MSD_WG39768-104_L17838 -2_Form8C.html)(1) Where applicable, custom lab flags have been used on this report.

(2) R% = percent recovery.

These data are validated and reported as accurate and in accord with AXYS Analytical Services Ltd. ISO17025 compliant quality assurance processes. Signed: ___________ 

## Bryan Alonzo

___________
These pages are part of a larger report that may contain information necessary for full data evaluation. Results reported relate only to the sample tested.

For Axys Internal Use Only [ XSL Template: MS.xsl; Created: 27-Apr-2012 15:00:16; Application: XMLTransformer-1.12.13; Report Filename: MS_FC_LC_PFOA

- MS

- MSD_WG39768

- 105_L17838

- 2_Form8E.html; Workgroup: WG39768; Design ID: 1722 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. MSF05D 120403 (MSD) Sample Collection: 03-Apr-2012 Form 8E PERFLUORINATED ORGANICS MATRIX SPIKE DUPLICATE (MSD) ANALYSIS REPORT AXYS ANALYTICAL SERVICES 2045 MILLS RD., SIDNEY, B.C., CANADA V8L 5X2 TEL (250) 655-5800 FAX (250) 655-5811 Project No. 3M - ALABAMA
Contract No.: 4673 Lab Sample I.D.: WG39768-105 (MSD)
Matrix: TISSUE Sample Size: 2.11 g (wet)
Extraction Date: 23-Apr-2012 Initial Calibration Date: 24-Apr-2012 Analysis Date: 25-Apr-2012 Time: 02:13:05 Instrument ID: LC MS/MS Extract Volume (uL): 4000 Column ID: C18MS Injection Volume (uL): 15 MSD Data Filename: FC2G_157 S: 30
Dilution Factor: N/A Blank Data Filename: FC2G_157 S: 22
Cal. Ver. Data Filename: FC2G_157 S: 15

ALL CONCENTRATIONS REPORTED ON THIS FORM ARE CONCENTRATIONS ON SAMPLE SIZE BASIS

COMPOUND LAB FLAG 1 ION

ABUND. RATIO SPIKE

CONC (ng/g) SAMPLE

LAB FLAG 1 SAMPLE

CONC (ng/g) CONC.

FOUND (ng/g) MSD

R% 2 REL

% DIFF

PFOS N/A 37.9 656 653



## Page 1 of 1 (WG39768 - MS_FC_LC_PFOA-MS-MSD_WG39768-105_L17838 -2_Form8E.html)AXYS Analytical Services Ltd.ACC-101 Rev 06, 29-Jun-2011Page 1 of 18Table 1aNELAP Accreditation Held by AXYS Analytical Services Ltd.for Chlorinated Dioxins/Furans, Chlorinated Pesticides, PCBs and PAHsMatrix Codes for Table 1aNPW = Non-Potable WaterDrW = Drinking WaterS = SolidT = TissueAccreditation Method Codes and Explanation for Table 1CodeAccreditation CertificateApplicable AXYS Method and DescriptionNo.Method Reference1 EPA 1613B MLA-017,performance based implementation of EPA1613B (GC/HRMS)2 EPA 8290MLA-017, performance basedimplementation ofEPA 8290 (GC/HRMS)3 AXYS MLA-017 MLA-017, performance based implementationof EPA 1613B, 8290 (GC/HRMS)4 EPA 608MLA-007, performance basedimplementation ofEPA 608 (GC/ECD)5 EPA 8270C or 8270D MLA-007, performance basedmodificationof 8270C/D (GC/LRMS)6 EPA 8081A or 8081B MLA-007, performance basedimplementation of EPA 8081A/B (GC/ECD)7 EPA 1668AMLA-010, performance basedimplementation ofEPA 1668A (GC/HRMS)8 SM 6630BMLA-007, performance based implementation of SM 18-20 6630B (GC/ECD)9 EPA 1625BMLA-021, performance basedmodificationof EPA 1625B (GC/LRMS)11 EPA 625MLA-007, performance basedmodificationof EPA 625 (GC/LRMS)20 EPA 8270C or 8270D MLA-021, performance basedmodificationof EPA 8270C/D (GC/LRMS)New YorkStateDepartmentof HealthCaliforniaDepartmentof PublicHealthState of FloridaDepartmentof HealthState of New JerseyDepartment ofEnvironmentalProtectionLab ID11674NELAPPrimaryLab ID01138CANELAPSecondaryLab ID E871007NELAP PrimaryLab ID CANA005NELAP SecondaryTABLE 1NPWSNPWSDr.WNPWS TDr.WNPWS TPCDD/F - Polychlorinated Dioxins and FuransDioxins1Dioxins and Dibenzofurans21,2,3,4,6,7,8-HpCDD121, 2, 3 2, 3 2, 3 1 2 21,2,3,4,6,7,8-HpCDF121, 2, 3 2, 3 2, 3 1 2 21,2,3,4,7,8,9-HpCDF121, 2, 3 2, 3 2, 3 1 2 21,2,3,4,7,8-HxCDD121, 2, 3 2, 3 2, 3 1 2 21,2,3,4,7,8-HxCDF121, 2, 3 2, 3 2, 3 1 2 21,2,3,6,7,8-HxCDD121, 2, 3 2, 3 2, 3 1 2 2AXYS Analytical Services Ltd.ACC-101 Rev 06, 29-Jun-2011Page 2 of 18New YorkStateDepartmentof HealthCaliforniaDepartmentof PublicHealthState of FloridaDepartmentof HealthState of New JerseyDepartment ofEnvironmentalProtectionLab ID11674NELAPPrimaryLab ID01138CANELAPSecondaryLab ID E871007NELAP PrimaryLab ID CANA005NELAP SecondaryTABLE 1NPWSNPWSDr.WNPWS TDr.WNPWS T1,2,3,6,7,8-HxCDF121, 2, 3 2, 3 2, 3 1 2 21,2,3,7,8,9-HxCDD121, 2, 3 2, 3 2, 3 1 2 21,2,3,7,8,9-HxCDF121, 2, 3 2, 3 2, 3 1 2 21,2,3,7,8-PeCDD121, 2, 3 2, 3 2, 3 1 2 21,2,3,7,8-PeCDF121, 2, 3 2, 3 2, 3 1 2 22,3,4,6,7,8-HxCDF121, 2, 3 2, 3 2, 3 1 2 22,3,4,7,8-PeCDF121, 2, 3 2, 3 2, 3 1 2 22,3,7,8-TCDD 1121, 2, 3 2, 3 2, 3 1 2 22,3,7,8-TCDF121, 2, 3 2, 3 2, 3 1 2 2OCDD121, 2, 3 2, 3 2, 3 1 2 2OCDF121, 2, 3 2, 3 2, 3 1 2 2Total TCDD11, 2, 3 2, 3 2, 3 2 2Total TCDF11, 2, 3 2, 3 2, 3 2 2Total PeCDD11, 2, 3 2, 3 2, 3 2 2Total PeCDF11, 2, 3 2, 3 2, 3 2 2Total HxCDD11, 2, 3 2, 3 2, 3 2 2Total HxCDF11, 2, 3 2, 3 2, 3 2 2Total HpCDD11, 2, 3 2, 3 2, 3 2 2Total HpCDF11, 2, 3 2, 3 2, 3 2 2PCBs – Polychlorinated biphenylsPCB 1 2-Chlorobiphenyl7 7 7 7PCB 3 4-Chlorobiphenyl7 7 7 7PCB 4 2,2'-Dichlorobiphenyl7 7 7 7PCB 5 2,3-Dichlorobiphenyl7 7 7 7PCB 15 4,4'-Dichlorobiphenyl7 7 7 7PCB 18 2,2',5-Trichlorobiphenyl7 7 7 7PCB 19 2,2',6-Trichlorobiphenyl7 7 7 7PCB 31 2,4',5-Trichlorobiphenyl7 7 7 7PCB 37 3,4,4'-Trichlorobiphenyl7 7 7 7PCB 44 2,2',3,5'-Tetrachlorobiphenyl 7 7 7 7PCB 52 2,2',5,5'-Tetrachlorobiphenyl 7 7 7 7PCB 54 2,2',6,6'-Tetrachlorobiphenyl 7 7 7 7PCB 66 2,3',4,4'-Tetrachlorobiphenyl 7 7 7 7PCB 77 3,3',4,4'-Tetrachlorobiphenyl 7 7 7 7PCB 81 3,4,4',5-Tetrachlorobiphenyl 7 7 7 7PCB 87 2,2',3,4,5'-Pentachlorobiphenyl 7 7 7 7AXYS Analytical Services Ltd.ACC-101 Rev 06, 29-Jun-2011Page 3 of 18New YorkStateDepartmentof HealthCaliforniaDepartmentof PublicHealthState of FloridaDepartmentof HealthState of New JerseyDepartment ofEnvironmentalProtectionLab ID11674NELAPPrimaryLab ID01138CANELAPSecondaryLab ID E871007NELAP PrimaryLab ID CANA005NELAP SecondaryTABLE 1NPWSNPWSDr.WNPWS TDr.WNPWS TPCB 101 2,2',4,5,5'-Pentachlorobiphenyl 7 7 7 7PCB 104 2,2',4,6,6'-Pentachlorobiphenyl 7 7 7 7PCB 105 2,3,3',4,4'-Pentachlorobiphenyl 7 7 7 7PCB 109 2,3,3',4,6-Pentachlorobiphenyl 7 7 7 7PCB 114 2,3,4,4',5-Pentachlorobiphenyl 7 7 7 7PCB 118 2,3',4,4',5-Pentachlorobiphenyl 7 7 7 7PCB 123 2,3',4,4',5'-Pentachlorobiphenyl 7 7 7 7PCB 124 2,3',4',5,5'-Pentachlorobiphenyl 7 7PCB 126 3,3',4,4',5-Pentachlorobiphenyl 7 7 7 7PCB 138 2,2',3,4,4',5'-Hexachlorobiphenyl 7 7 7 7PCB 141 2,2',3,4,5,5'-Hexachlorobiphenyl 7 7 7 7PCB 151 2,2',3,5,5',6-Hexachlorobiphenyl 7 7 7 7PCB 153 2,2',4,4',5,5'-Hexachlorobiphenyl 7 7 7 7PCB 155 2,2',4,4',6,6'-Hexachlorobiphenyl 7 7 7 7PCB 156 2,3,3',4,4',5-Hexachlorobiphenyl 7 7PCB 157 2,3,3',4,4',5'-Hexachlorobiphenyl 7 7 7 7PCB 167 2,3',4,4',5,5'-Hexachlorobiphenyl 7 7 7 7PCB 169 3,3',4,4',5,5'-Hexachlorobiphenyl 7 7 7 7PCB 170 2,2',3,3',4,4',5-Heptachlorobiphenyl 7 7 7 7PCB 180 2,2',3,4,4',5,5'-Heptachlorobiphenyl 7 7 7 7PCB 183 2,2',3,4,4',5',6-Heptachlorobiphenyl 7 7 7 7PCB 187 2,2',3,4',5,5',6-Heptachlorobiphenyl 7 7 7 7PCB 188 2,2',3,4',5,6,6'-Heptachlorobiphenyl 7 7 7 7PCB 189 2,3,3',4,4',5,5'-Heptachlorobiphenyl 7 7 7 7PCB 202 2,2',3,3',5,5',6,6'-Octachlorobiphenyl 7 7 7 7PCB 205 2,3,3',4,4',5,5',6-Octachlorobiphenyl 7 7 7PCB 206 2,2',3,3',4,4',5,5',6-Nonachlorobiphenyl 7 7 7 7PCB 208 2,2',3,3',4,5,5',6,6'-Nonachlorobiphenyl 7 7 7 7PCB 209 Decachlorobiphenyl7 7 7 7Aroclor 12607, 11 5, 7 11 5Aroclor 12547, 11 5, 7 11 5Aroclor 12217, 11 5, 7 11 5Aroclor 12327, 11 5, 7 11 5Aroclor 12487, 11 5, 7 11 5Aroclor 10167, 11 5, 7 11 5Aroclor 12427, 11 5, 7 11 5AXYS Analytical Services Ltd.ACC-101 Rev 06, 29-Jun-2011Page 4 of 18New YorkStateDepartmentof HealthCaliforniaDepartmentof PublicHealthState of FloridaDepartmentof HealthState of New JerseyDepartment ofEnvironmentalProtectionLab ID11674NELAPPrimaryLab ID01138CANELAPSecondaryLab ID E871007NELAP PrimaryLab ID CANA005NELAP SecondaryTABLE 1NPWSNPWSDr.WNPWS TDr.WNPWS TPesticides4,4'-DDD11 5 11 54,4'-DDE11 5 11 54,4'-DDT11 5 11 5Aldrin11 5 11 5Alpha-HCH11 5 11 5Beta-HCH11 5 11 5cis-Chlordane (alpha-Chlordane)5 5Chlordane, technical5, 11 5 11 5Delta-HCH11 5 11 5Dieldrin4 6 4 6Endosulphan I4 6 4 6Endosulphan II4 6 4 6Endosulphan sulphate4 6 4 6Endrin4 6 4 6Endrin aldehyde4 6 4 6trans-Chlordane (gamma-Chlordane)5 5Gamma-HCH (Lindane)11 5 11 5Heptachlor11 5 11 5Heptachlor epoxide4 6 4 6Hexachlorobenzene9 5 9 5Methoxychlor4,8 6 8 6Mirex 5PAHAnthracene9 20 9 20Pyrene 9209 20Benzo[ghi]perylene 9209 20Indeno[1,2,3-cd]pyrene 9209 20Benzo[b]fluoranthene 9209 20Fluoranthene 9209 20Benzo[k]fluoranthene 9209 20Acenaphthylene 9209 20Chrysene 9209 20Benzo[a]pyrene 9209 20Dibenz[ah]anthracene 9209 20Benz[a]anthracene 9209 20AXYS Analytical Services Ltd.ACC-101 Rev 06, 29-Jun-2011Page 5 of 18New YorkStateDepartmentof HealthCaliforniaDepartmentof PublicHealthState of FloridaDepartmentof HealthState of New JerseyDepartment ofEnvironmentalProtectionLab ID11674NELAPPrimaryLab ID01138CANELAPSecondaryLab ID E871007NELAP PrimaryLab ID CANA005NELAP SecondaryTABLE 1NPWSNPWSDr.WNPWS TDr.WNPWS TAcenaphthene 9209 20Phenanthrene 9209 20Fluorene 9209 20Naphthalene 9209 20AXYS Analytical Services Ltd.ACC-101 Rev 06, 29-Jun-2011Page 6 of 18Table 1bNELAP Accreditation Held by AXYS Analytical Services Ltd.for Perfluorinated Organic CompoundsMatrix Codes for Table 1bNPW = Non-Potable WaterDrW = Drinking WaterS = SolidT = TissueAccreditation Method Codes and Explanation for Table 1bCodeAccreditation CertificateApplicable AXYS Method and DescriptionNo.Method Reference12 AXYS MLA-041 MLA-041, laboratory performance based method (LC/MS-MS)13 AXYS MLA-043 MLA-043, laboratory performance based method (LC/MS-MS)14 AXYS MLA-060 MLA-060, laboratory performance based method (LC/MS-MS)State of FloridaDepartmentof HealthMinnesota Departmentof HealthState of New JerseyDepartment ofEnvironmentalProtectionLab ID E871007NELAP PrimaryLab ID 232-999-430NELAP PrimaryLab ID CANA005NELAP SecondaryTABLE 1Dr.WNPWSTDr.WNPWSTDr.WNPWSTPFC – Perfluorinated Organic CompoundsPerfluorobutanoate (PFBA)Note14 14 12 13 14 14 12 13 14 14 12 13Perfluoropentanoate (PFPeA)Note14 14 12 13 14 14 12 13 14 14 12 13Perfluorohexanoate (PFHxA)Note14 14 12 13 14 14 12 13 14 14 12 13Perfluoroheptanoate (PFHpA)Note14 14 12 13 14 14 12 13 14 14 12 13Perfluorooctanoate (PFOA)Note14 14 12 13 14 14 12 13 14 14 12 13Perfluorononanoate (PFNA)Note14 14 12 13 14 14 12 13 14 14 12 13Perfluorodecanoate (PFDA)Note14 14 12 13 14 14 12 13 14 14 12 13Perfluoroundecanoate (PFUnA)Note14 14 12 13 14 14 12 13 14 14 12 13Perfluorododecanoate (PFDoA)Note14 14 12 13 14 14 12 13 14 14 12 13Perfluorobutanesulfonate (PFBS)14 14 12 13 14 14 12 13 14 14 12 13Perfluorohexanesulfonate (PFHxS)14 14 12 13 14 14 12 13 14 14 12 13Perfluorooctanesulfonate (PFOS)14 14 12 13 14 14 12 13 14 14 12 13Perfluorooctane sulfonamide (PFOSA) 14 14 12 13 14 14 12 13Note: Accreditations by Minnesota Department of Health and NewJersey Department of Environmental Protection are against the corresponding acid form of the anion shown.

## AXYS Analytical Services Ltd.

ACC-101 Rev 06, 29-Jun-2011 Page 7 of 18 

## Table 2: Canadian and US State Specific Accreditation Held by AXYS Analytical Services Ltd.

Matrix Codes for Table 2 

### NP W = Non-Potable Water Dr. W = Drinking Water W = Aqueous S = Solid T = Tissue
Accreditation Method Codes and Explanation for Table 2
Code Accreditation Certificate Applicable AXYS Method and Description No. Method Reference

1 EPA 1613 MLA-017 Performance based implementation of EPA 1613B (GC/HRMS) 3 AXYS MLA-017 MLA-017 Performance based implementation of EPA 1613B (GC/HRMS) 7 EPA 1668A MLA-010 Performance based implementation of EPA 1668A (GC/HRMS) 10 AXYS MLA-007 MLA-007, Performance based modification of EPA 8270C/D, 8081A/B (GC/LRMS and GC/ECD) 12 AXYS MLA-041 MLA-041 Laboratory performance based method (LC/MS-MS) 13 AXYS MLA-043 MLA-043 Laboratory performance based method (LC/MS-MS) 14 AXYS MLA-060 MLA-060 Laboratory performance based method (LC/MS-MS) 15 AXYS MLA-010 MLA-010 Performance ba sed implementation of EPA 1668A (GC/HRMS) 16 AXYS MLA-028 MLA-028 Laboratory performance based method (GC/HRMS) 17 AXYS MLA-033 MLA-033 Performance ba sed implementation of EPA 1614 (GC/HRMS) 18 AXYS MLA-021 MLA-021 Performance based modification of EPA 8270C/D (GC/LRMS) 19 AXYS MLA-075 MLA-075 Performance ba sed implementation of EPA 1694 (LC/MS-MS)



### Canadian Association for Laboratory Accreditation (CALA) Washington State Department of Ecology Accreditation No.: A 2637 Lab. ID: C404 TABLE 2

W S Pulp T NP W S PCDD/F - Polychlorinated Dioxins and Furans 1,2,3,4,6,7,8-Hp CDD 3 3 3 3 1 1 1,2,3,4,6,7,8-Hp CDF 3 3 3 3 1 1 1,2,3,4,7,8,9-Hp CDF 3 3 3 3 1 1 1,2,3,4,7,8-Hx CDD 3 3 3 3 1 1 1,2,3,4,7,8-HxCDF 3 3 3 3 1 1 1,2,3,6,7,8-Hx CDD 3 3 3 3 1 1 1,2,3,6,7,8-HxCDF 3 3 3 3 1 1 1,2,3,7,8,9-Hx CDD 3 3 3 3 1 1 1,2,3,7,8,9-HxCDF 3 3 3 3 1 1 1,2,3,7,8-PeCDD 3 3 3 3 1 1 1,2,3,7,8-PeCDF 3 3 3 3 1 1 2,3,4,6,7,8-HxCDF 3 3 3 3 1 1 2,3,4,7,8-PeCDF 3 3 3 3 1 1 2,3,7,8-TCDD 3 3 3 3 1 1 2,3,7,8-TCDF 3 3 3 3 1 1 OCDD 3 3 3 3 1 1 OCDF 3 3 3 3 1 1 Total TCDD 1 1 Total TCDF 1 1 Total PeCDD 1 1 Total PeCDF 1 1 Total HxCDD 1 1

## AXYS Analytical Services Ltd.

ACC-101 Rev 06, 29-Jun-2011 Page 8 of 18 Canadian Association for Laboratory Accreditation (CALA) Washington State Department of Ecology Accreditation No.: A 2637 Lab. ID: C404 TABLE 2

W S Pulp T NP W S
Total HxCDF 1 1 Total HpCDD 1 1 Total HpCDF 1 1 Total PCDD 1 1 Total PCDF 1 1 Total PCDD + PCDF 1 1
PCBs – Polychlorinated biphenyls PCB 1 2-Chlorobiphenyl 15 15 15 7 7 PCB 2 3-Chlorobiphenyl 15 15 15 7 7 PCB 3 4-Chlorobiphenyl 15 15 15 7 7 PCB 4 2,2'-Dichlorobiphenyl 15 15 15 7 7 PCB 5 2,3-Dichlorobiphenyl 15 15 15 7 7 PCB 6 2,3'-Dichlorobiphenyl 15 15 15 7 7 PCB 7 2,4-Dichlorobiphenyl 15 15 15 7 7 PCB 8 2,4'-Dichlorobiphenyl 15 15 15 7 7 PCB 8/5 10 10 10 PCB 9 2,5-Dichlorobiphenyl 15 15 15 7 7 PCB 10 2,6-Dichlorobiphenyl 15 15 15 7 7 PCB 11 3,3'-Dichlorobiphenyl 15 15 15 7 7 PCB 12 3,4-Dichlorobiphenyl 15 15 15 7 7 PCB 13 3,4'-Dichlorobiphenyl 15 15 15 7 7 PCB 14 3,5-Dichlorobiphenyl 15 15 15 7 7 PCB 15 4,4'-Dichlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 16 2,2',3-Trichlorobiphenyl 15 15 15 7 7 PCB 16/32 10 10 10 PCB 17 2,2',4-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 18 2,2',5-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 19 2,2',6-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 20 2,3,3'-Trichlorobiphenyl 15 15 15 7 7 PCB 21 2,3,4-Trichlorobiphenyl 15 15 15 7 7 PCB 22 2,3,4'-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 23 2,3,5-Trichlorobiphenyl 15 15 15 7 7 PCB 24 2,3,6-Trichlorobiphenyl 15 15 15 7 7 PCB 24/27 10 10 10 PCB 25 2,3',4-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 26 2,3',5-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 27 2,3',6-Trichlorobiphenyl 15 15 15 7 7 PCB 28 2,4,4'-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 29 2,4,5-Trichlorobiphenyl 15 15 15 7 7 PCB 30 2,4,6-Trichlorobiphenyl 15 15 15 7 7 PCB 31 2,4',5-Trichlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 32 2,4',6-Trichlorobiphenyl 15 15 15 7 7 PCB 33 2,3',4'-Trichlorobiphenyl 15 15 15 7 7 PCB 33/20/21 18 10 10 PCB 34 2,3',5'-Trichlorobiphenyl 15 15 15 7 7 PCB 35 3,3',4-Trichlorobiphenyl 15 15 15 7 7 PCB 36 3,3',5-Trichlorobiphenyl 15 15 15 7 7 PCB 37 3,4,4'-Trichlorobiphenyl 15 15 15 7 7 PCB 38 3,4,5-Trichlorobiphenyl 15 15 15 7 7 PCB 39 3,4',5-Trichlorobiphenyl 15 15 15 7 7 PCB 40 2,2',3,3'-Tetrachlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 41 2,2',3,4-Tetrachlorobiphenyl 15 15 15 7 7 PCB 41/71/64/68 10 10 10

## AXYS Analytical Services Ltd.

ACC-101 Rev 06, 29-Jun-2011 Page 9 of 18 Canadian Association for Laboratory Accreditation (CALA) Washington State Department of Ecology Accreditation No.: A 2637 Lab. ID: C404 TABLE 2

W S Pulp T NP W S PCB 42 2,2',3,4'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 42/59 10 10 10 PCB 43 2,2',3,5-Tetrachlorobiphenyl 15 15 15 7 7 PCB 44 2,2',3,5'-Tetrachlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 45 2,2',3,6-Tetrachlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 46 2,2',3,6'-Tetrachlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 47 2,2',4,4'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 47/48/75 10 10 10 PCB 48 2,2',4,5-Tetrachlorobiphenyl 15 15 15 7 7 PCB 49 2,2',4,5'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 49/43 10 10 10 PCB 50 2,2',4,6-Tetrachlorobiphenyl 15 15 15 7 7 PCB 51 2,2',4,6'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 52 2,2',5,5'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 52/73 10 10 10 PCB 53 2,2',5,6'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 54 2,2',6,6'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 55 2,3,3',4-Tetrachlorobiphenyl 15 15 15 7 7 PCB 56 2,3,3',4'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 56/60 10 10 10 PCB 57 2,3,3',5-Tetrachlorobiphenyl 15 15 15 7 7 PCB 58 2,3,3',5'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 59 2,3,3',6-Tetrachlorobiphenyl 15 15 15 7 7 PCB 60 2,3,4,4'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 61 2,3,4,5-Tetrachlorobiphenyl 15 15 15 7 7 PCB 62 2,3,4,6-Tetrachlorobiphenyl 15 15 15 7 7 PCB 63 2,3,4',5-Tetrachlorobiphenyl 15 15 15 7 7 PCB 64 2,3,4',6-Tetrachlorobiphenyl 15 15 15 7 7 PCB 65 2,3,5,6-Tetrachlorobiphenyl 15 15 15 7 7 PCB 66 2,3',4,4'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 66/80 10 10 10 PCB 67 2,3',4,5-Tetrachlorobiphenyl 15 15 15 7 7 PCB 68 2,3',4,5'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 69 2,3',4,6-Tetrachlorobiphenyl 15 15 15 7 7 PCB 70 2,3',4',5-Tetrachlorobiphenyl 15 15 15 7 7 PCB 70/76 10 10 10 PCB 71 2,3',4',6-Tetrachlorobiphenyl 15 15 15 7 7 PCB 72 2,3',5,5'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 73 2,3',5',6-Tetrachlorobiphenyl 15 15 15 7 7 PCB 74 2,4,4',5-Tetrachlorobiphenyl 15 15 15 7 7 PCB 74/61 10 10 10 PCB 75 2,4,4',6-Tetrachlorobiphenyl 15 15 15 7 7 PCB 76 2,3',4',5'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 77 3,3',4,4'-Tetrachlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 78 3,3',4,5-Tetrachlorobiphenyl 15 15 15 7 7 PCB 79 3,3',4,5'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 80 3,3',5,5'-Tetrachlorobiphenyl 15 15 15 7 7 PCB 81 3,4,4',5-Tetrachlorobiphenyl 15 15 15 7 7 PCB 82 2,2',3,3',4-Pentachlorobiphenyl 15 15 15 7 7 PCB 83 2,2',3,3',5-Pentachlorobiphenyl 15 15 15 7 7 PCB 83/108 10 10 10 PCB 84 2,2',3,3',6-Pentachlorobip henyl 10, 15 10, 15 10, 15 7 7 PCB 85 2,2',3,4,4'-Pentachlorobiphenyl 15 15 15 7 7 PCB 85/120 10 10 10

## AXYS Analytical Services Ltd.

ACC-101 Rev 06, 29-Jun-2011 Page 10 of 18 Canadian Association for Laboratory Accreditation (CALA) Washington State Department of Ecology Accreditation No.: A 2637 Lab. ID: C404 TABLE 2

W S Pulp T NP W S PCB 86 2,2',3,4,5-Pentachlorobiphenyl 15 15 15 7 7 PCB 87 2,2',3,4,5'-Pentachlorobiphenyl 15 15 15 7 7 PCB 87/115/116 10 10 10 PCB 88 2,2',3,4,6-Pentachlorobiphenyl 15 15 15 7 7 PCB 89 2,2',3,4,6'-Pentachlorobiphenyl 15 15 15 7 7 PCB 90 2,2',3,4',5-Pentachlorobiphenyl 15 15 15 7 7 PCB 91 2,2',3,4',6-Pentachlorobip henyl 10, 15 10, 15 10, 15 7 7 PCB 92 2,2',3,5,5'-Pentachlorobiphenyl 15 15 15 7 7 PCB 93 2,2',3,5,6-Pentachlorobiphenyl 15 15 15 7 7 PCB 94 2,2',3,5,6'-Pentachlorobiphenyl 15 15 15 7 7 PCB 95 2,2',3,5',6-Pentachlorobiphenyl 15 15 15 7 7 PCB 95/93 10 10 10 PCB 96 2,2',3,6,6'-Pentachlorobiphenyl 15 15 15 7 7 PCB 97 2,2',3,4',5'-Pentachlorobiphenyl 15 15 15 7 7 PCB 97/86 10 10 10 PCB 98 2,2',3,4',6'-Pentachlorobiphenyl 15 15 15 7 7 PCB 99 2,2',4,4',5-Pentachlorobip henyl 10, 15 10, 15 10, 15 7 7 PCB 100 2,2',4,4',6-Pentachlorobiphenyl 15 15 15 7 7 PCB 101 2,2',4,5,5'-Pentachlorobiphenyl 15 15 15 7 7 PCB 101/90/89 10 10 10 PCB 102 2,2',4,5,6'-Pentachlorobiphenyl 15 15 15 7 7 PCB 103 2,2',4,5',6-Pentachlorobiphenyl 15 15 15 7 7 PCB 104 2,2',4,6,6'-Pentachlorobiphenyl 15 15 15 7 7 PCB 105 2,3,3',4,4'-Pentachlorobiphenyl 15 15 15 7 7 PCB 105/127 10 10 10 PCB 106 2,3,3',4,5-Pentachlorobiphenyl 15 15 15 7 7 PCB 107 2,3,3',4',5-Pentachlorobiphenyl 15 15 15 7 7 PCB 107/109 10 10 10 PCB 108 2,3,3',4,5'-Pentachlorobiphenyl 15 15 15 7 7 PCB 109 2,3,3',4,6-Pentachlorobiphenyl 15 15 15 7 7 PCB 110 2,3,3',4',6-Pentachlorobip henyl 10, 15 10, 15 10, 15 7 7 PCB 111 2,3,3',5,5'-Pentachlorobiphenyl 15 15 15 7 7 PCB 112 2,3,3',5,6-Pentachlorobiphenyl 15 15 15 7 7 PCB 113 2,3,3',5',6-Pentachlorobiphenyl 15 15 15 7 7 PCB 114 2,3,4,4',5-Pentachlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 115 2,3,4,4',6-Pentachlorobiphenyl 15 15 15 7 7 PCB 116 2,3,4,5,6-Pentachl orobiphenyl 15 15 15 7 7 PCB 117 2,3,4',5,6-Pentachlorobiphenyl 15 15 15 7 7 PCB 118 2,3',4,4',5-Pentachlorobiphenyl 15 15 15 7 7 PCB 118/116 10 10 10 PCB 119 2,3',4,4',6-Pentachlorobiphenyl 15 15 15 7 7 PCB 120 2,3',4,5,5'-Pentachlorobiphenyl 15 15 15 7 7 PCB 121 2,3',4,5',6-Pentachlorobiphenyl 15 15 15 7 7 PCB 122 2,3,3',4',5'-Pentachlorobiphenyl 15 15 15 7 7 PCB 123 2,3',4,4',5'-Pentachlorobiphenyl 15 15 15 7 7 PCB 124 2,3',4',5,5'-Pentachlorobiphenyl 15 15 15 7 7 PCB 125 2,3',4',5',6-Pentachlorobiphenyl 15 15 15 7 7 PCB 126 3,3',4,4',5-Pentachlorobip henyl 10, 15 10, 15 10, 15 7 7 PCB 127 3,3',4,5,5'-Pentachlorobiphenyl 15 15 15 7 7 PCB 128 2,2',3,3',4,4'-Hexachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 129 2,2',3,3',4,5-Hexachlorobi phenyl 10, 15 10, 15 10, 15 7 7 PCB 130 2,2',3,3',4,5'-Hexachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 131 2,2',3,3',4,6-Hexachlorobiphenyl 15 15 15 7 7 PCB 131/142 10 10 10

## AXYS Analytical Services Ltd.

ACC-101 Rev 06, 29-Jun-2011 Page 11 of 18 Canadian Association for Laboratory Accreditation (CALA) Washington State Department of Ecology Accreditation No.: A 2637 Lab. ID: C404 TABLE 2

W S Pulp T NP W S PCB 132 2,2',3,3',4,6'-Hexachlorobiphenyl 15 15 15 7 7 PCB 133 2,2',3,3',5,5'-Hexachlorobiphenyl 15 15 15 7 7 PCB 134 2,2',3,3',5,6-Hexachlorobiphenyl 15 15 15 7 7 PCB 134/143 10 10 10 PCB 135 2,2',3,3',5,6'-Hexachlorobiphenyl 15 15 15 7 7 PCB 136 2,2',3,3',6,6'-Hexachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 137 2,2',3,4,4',5-Hexachlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 138 2,2',3,4,4',5'-Hexachlorobiphenyl 15 15 15 7 7 PCB 138/163/164 10 10 10 PCB 139 2,2',3,4,4',6-Hexachlorobiphenyl 15 15 15 7 7 PCB 140 2,2',3,4,4',6'-Hexachlorobiphenyl 15 15 15 7 7 PCB 141 2,2',3,4,5,5'-Hexachlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 142 2,2',3,4,5,6-Hexachlorobiphenyl 15 15 15 7 7 PCB 143 2,2',3,4,5,6'-Hexachlorobiphenyl 15 15 15 7 7 PCB 144 2,2',3,4,5',6-Hexachlorobiphenyl 15 15 15 7 7 PCB 144/135 10 10 10 PCB 145 2,2',3,4,6,6'-Hexachlorobiphenyl 15 15 15 7 7 PCB 146 2,2',3,4',5,5'-Hexachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 147 2,2',3,4',5,6-Hexachlorobiphenyl 15 15 15 7 7 PCB 148 2,2',3,4',5,6'-Hexachlorobiphenyl 15 15 15 7 7 PCB 149 2,2',3,4',5',6-Hexachlorobiphenyl 15 15 15 7 7 PCB 149/139 10 10 10 PCB 150 2,2',3,4',6,6'-Hexachlorobiphenyl 15 15 15 7 7 PCB 151 2,2',3,5,5',6-Hexachlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 152 2,2',3,5,6,6'-Hexachlorobiphenyl 15 15 15 7 7 PCB 153 2,2',4,4',5,5'-Hexachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 154 2,2',4,4',5,6'-Hexachlorobiphenyl 15 15 15 7 7 PCB 155 2,2',4,4',6,6'-Hexachlorobiphenyl 15 15 15 7 7 PCB 156 2,3,3',4,4',5-Hexachlorobi phenyl 10, 15 10, 15 10, 15 7 7 PCB 157 2,3,3',4,4',5'-Hexachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 158 2,3,3',4,4',6-Hexachlorobiphenyl 15 15 15 7 7 PCB 158/160 10 10 10 PCB 159 2,3,3',4,5,5'-Hexachlorobiphenyl 15 15 15 7 7 PCB 160 2,3,3',4,5,6-Hexachlorobiphenyl 15 15 15 7 7 PCB 161 2,3,3',4,5',6-Hexachlorobiphenyl 15 15 15 7 7 PCB 162 2,3,3',4',5,5'-Hexachlorobiphenyl 15 15 15 7 7 PCB 163 2,3,3',4',5,6-Hexachlorobiphenyl 15 15 15 7 7 PCB 164 2,3,3',4',5',6-Hexachlorobiphenyl 15 15 15 7 7 PCB 165 2,3,3',5,5',6-Hexachlorobiphenyl 15 15 15 7 7 PCB 166 2,3,4,4',5,6-Hexachlorobiphenyl 15 15 15 7 7 PCB 167 2,3',4,4',5,5'-Hexachlorobiphenyl 15 15 15 7 7 PCB 168 2,3',4,4',5',6-Hexachlorobiphenyl 15 15 15 7 7 PCB 169 3,3',4,4',5,5'-Hexachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 170 2,2',3,3',4,4',5-Heptachlorobiphenyl 15 15 15 7 7 PCB 170/190 10 10 10 PCB 171 2,2',3,3',4,4',6-Heptachlor obiphenyl 10, 15 10, 15 10, 15 7 7 PCB 172 2,2',3,3',4,5,5'-Heptachlorobiphenyl 15 15 15 7 7 PCB 172/192 10 10 10 PCB 173 2,2',3,3',4,5,6-Heptachlorobiphenyl 15 15 15 7 7 PCB 174 2,2',3,3',4,5,6'-Heptachlorobiphenyl 15 15 15 7 7 PCB 174/181 10 10 10 PCB 175 2,2',3,3',4,5',6-Heptachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 176 2,2',3,3',4,6,6'-Heptachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 177 2,2',3,3',4,5',6'-Heptachlor obiphenyl 10, 15 10, 15 10, 15 7 7

## AXYS Analytical Services Ltd.

ACC-101 Rev 06, 29-Jun-2011 Page 12 of 18 Canadian Association for Laboratory Accreditation (CALA) Washington State Department of Ecology Accreditation No.: A 2637 Lab. ID: C404 TABLE 2

W S Pulp T NP W S PCB 178 2,2',3,3',5,5',6-Heptachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 179 2,2',3,3',5,6,6'-Heptachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 180 2,2',3,4,4',5,5'-Heptachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 181 2,2',3,4,4',5,6-Heptachlorobiphenyl 15 15 15 7 7 PCB 182 2,2',3,4,4',5,6'-Heptachlorobiphenyl 15 15 15 7 7 PCB 183 2,2',3,4,4',5',6-Heptachlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 184 2,2',3,4,4',6,6'-Heptachlorobiphenyl 15 15 15 7 7 PCB 185 2,2',3,4,5,5',6-Heptachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 186 2,2',3,4,5,6,6'-Heptachlorobiphenyl 15 15 15 7 7 PCB 187 2,2',3,4',5,5',6-Heptachlorobiphenyl 15 15 15 7 7 PCB 187/182 10 10 10 PCB 188 2,2',3,4',5,6,6'-Heptachlorobiphenyl 15 15 15 7 7 PCB 189 2,3,3',4,4',5,5'-Heptachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 190 2,3,3',4,4',5,6-Heptachlorobiphenyl 15 15 15 7 7 PCB 191 2,3,3',4,4',5',6-Heptachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 192 2,3,3',4,5,5',6-Heptachlorobiphenyl 15 15 15 7 7 PCB 193 2,3,3',4',5,5',6-Heptachlorob iphenyl 10, 15 10, 15 10, 15 7 7 PCB 194 2,2',3,3',4,4',5,5'-Octachlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 195 2,2',3,3',4,4',5,6-Octachlor obiphenyl 10, 15 10, 15 10, 15 7 7 PCB 196 2,2',3,3',4,4',5,6'-Octachlorobiphenyl 15 15 15 7 7 PCB 196/203 10 10 10 PCB 197 2,2',3,3',4,4',6,6'-Octachlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 198 2,2',3,3',4,5,5',6-Octachlor obiphenyl 10, 15 10, 15 10, 15 7 7 PCB 199 2,2',3,3',4,5,5',6'-Octachlo robiphenyl 10, 15 10, 15 10, 15 7 7 PCB 200 2,2',3,3',4,5,6,6'-Oct achlorobiphenyl 15 15 15 7 7 PCB 201 2,2',3,3',4,5',6,6'-Octachlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 202 2,2',3,3',5,5',6,6'-Octachlorobiphenyl 15 15 15 7 7 PCB 203 2,2',3,4,4',5,5',6-Octachlorobiphenyl 15 15 15 7 7 PCB 204 2,2',3,4,4',5,6,6'-Oct achlorobiphenyl 15 15 15 7 7 PCB 205 2,3,3',4,4',5,5',6-Octachlor obiphenyl 10, 15 10, 15 10, 15 7 7 PCB 206 2,2',3,3',4,4',5,5',6-Nonachlo robiphenyl 10, 15 10, 15 10, 15 7 7 PCB 207 2,2',3,3',4,4',5,6,6'-Nonachlorobiphenyl 10, 15 10, 15 10, 15 7 7 PCB 208 2,2',3,3',4,5,5',6,6'-Nonachlo robiphenyl 10, 15 10, 15 10, 15 7 7 PCB 209 Decachlorobiphenyl 10, 15 10, 15 10, 15 7 7 Total Monochlorobiphenyls 15 15 15 Total Dichlorobiphenyls 10, 15 10, 15 10, 15 Total Trichlorobiphenyls 10, 15 10, 15 10, 15 Total Tetrachlorobiphenyls 10, 15 10, 15 10, 15 Total Pentachlorobiphenyls 10, 15 10, 15 10, 15 Total Hexachlorobiphenyls 10, 15 10, 15 10, 15 Total Heptachlorobiphenyls 10, 15 10, 15 10, 15 Total Octachlorobiphenyls 10, 15 10, 15 10, 15 Total Nonachlorobiphenyls 10, 15 10, 15 10, 15 Total Decachlorobiphenyls 10 10 10 Total Polychlorinated biphenyls 10 10 10 7

Aroclors Aroclor 1260 10 10 10 7 7 Aroclor 1254 10 10 10 7 7 Aroclor 1268 10 10 10 Aroclor 1221 10 10 10 7 7 Aroclor 1232 10 10 10 7 7 Aroclor 1248 10 10 10 7 7 Aroclor 1016 7 7

## AXYS Analytical Services Ltd.

ACC-101 Rev 06, 29-Jun-2011 Page 13 of 18 Canadian Association for Laboratory Accreditation (CALA) Washington State Department of Ecology Accreditation No.: A 2637 Lab. ID: C404 TABLE 2

W S Pulp T NP W S
Aroclor 1242 7 7 Aroclor 1242/1016 10 10 10

Pesticides 2,4'-DDD 10, 16 10, 16 10, 16 16 2,4'-DDE 10, 16 10, 16 10, 16 16 2,4'-DDT 10, 16 10, 16 10, 16 16 4,4'-DDD 10, 16 10, 16 10, 16 16 4,4'-DDE 10, 16 10, 16 10, 16 16 4,4'-DDT 10, 16 10, 16 10, 16 16 Aldrin 10, 16 10, 16 10, 16 16 Alpha-HCH 10, 16 10, 16 10, 16 16 Beta-HCH 10, 16 10, 16 10, 16 16 cis-Chlordane (alpha-Chlordane) 10, 16 10, 16 10, 16 16 cis-Nonachlor 10, 16 10, 16 10, 16 16 Delta-HCH 10, 16 10, 16 10, 16 16 Dieldrin 10, 16 10, 16 10, 16 16 Endosulphan I 10, 16 10, 16 10, 16 16 Endosulphan II 10, 16 10, 16 10, 16 16 Endosulphan sulphate 10, 16 10, 16 10, 16 16 Endrin 10, 16 10, 16 10, 16 16 Endrin aldehyde 10, 16 10, 16 16 16 Endrin ketone 10, 16 10, 16 10, 16 16 Gamma-HCH (Lindane) 10, 16 10, 16 10, 16 16 Heptachlor 10, 16 10, 16 10, 16 16 Heptachlor epoxide 10, 16 10, 16 10, 16 16 Hexachlorobenzene 10, 16 10, 16 10, 16 16 Hexachlorobutadiene 16 16 Methoxychlor 10, 16 10, 16 10, 16 16 Mirex 10, 16 10, 16 10, 16 16 Oxychlordane 10, 16 10, 16 10, 16 16 Toxaphene 10 10 10 trans-Chlordane (gamma-Chlordane) 10, 16 10, 16 10, 16 16 trans-Nonachlor 16 10, 16 10, 16 16
BDE - Brominated Diphenylethers BDE 7 2,4-dibromodiphenylether 17 17 17 BDE 8 2,4’-dibromodiphenylether 17 17 17 BDE 10 2,6-dibromodiphenylether 17 17 17 BDE 11 3,3’-dibromodiphenylether 17 17 17 BDE 12 3,4-dibromodiphenylether 17 17 17 BDE 13 3,4’-dibromodiphenylether 17 17 17 BDE 15 4,4’-dibromodiphenylether 17 17 17 BDE 17 2,2’,4-tribromodiphenylether 17 17 17 BDE 25 2,3’,4-tribromodiphenylether 17 17 17 BDE 28 2,4,4’-tribromodiphenylether 17 17 17 BDE 30 2,4,6-tribromodiphenylether 17 17 17 BDE-33 2’,3,4-tribromodiphenylether 17 17 17 BDE 35 3,3’,4-tribromodiphenylether 17 17 17 BDE 37 3,4,4’-tribromodiphenylether 17 17 17 BDE 47 2,2’,4,4’-tetrabromodiphenylether 17 17 17 BDE 49 2,2’,4,5’-tetrabromodiphenylether 17 17 17 BDE 66 2,3’,4,4’-tetrabromodiphenylether 17 17 17 BDE 75 2,4,4’,6-tetrabromodiphenylether 17 17 17

## AXYS Analytical Services Ltd.

ACC-101 Rev 06, 29-Jun-2011 Page 14 of 18 Canadian Association for Laboratory Accreditation (CALA) Washington State Department of Ecology Accreditation No.: A 2637 Lab. ID: C404 TABLE 2

W S Pulp T NP W S BDE 77 3,3’,4,4’-tetrabromodiphenylether 17 17 17 BDE 85 2,2’,3,4,4’-pentabromodiphenylether 17 17 17 BDE 99 2,2’,4,4’,5-pentabrom odiphenylether 17 17 17 BDE 100 2,2’,4,4’,6-pentabrom odiphenylether 17 17 17 BDE 105 2,3,3’,4,4’-pentabrom odiphenylether 17 17 17 BDE 116 2,3,4,5,6-pentabromo diphenylether 17 17 17 BDE 119 2,3’,4,4’,6-pentabrom odiphenylether 17 17 17 BDE 126 3,3’,4,4’,5-pentabrom odiphenylether 17 17 17 BDE 140 2,2’,3,4,4’,6’-hexabromodiphenylether 17 17 17 BDE 153 2,2’,4,4’,5,5’-hexabromodiphenylether 17 17 17 BDE 154 2,2’,4,4’,5’,6-hexabromodiphenylether 17 17 17 BDE 155 2,2’,4,4’,6,6’-hexabromodiphenylether 17 17 17 BDE 166 2,3,4,4’,5,6-hexabromodiphenylether 17 17 17 BDE 181 2,2’,3,4,4’,5,6-heptabromodiphenylether 17 17 17 BDE-183 2,2’,3,4,4’,5’,6-heptabromodiphenylether 17 17 17 BDE 190 2,3,3’,4,4’,5,6-heptabro modiphenylether 17 17 17 BDE 206 2,2’,3,3’,4,4’,5,5’,6-nonabromodiphenylether 17 17 17 BDE 207 2,2’,3,3’,4,4’,5,6,6’-nonabromodiphenylether 17 17 17 BDE 208 2,2’,3,3’,4,5,5’,6,6’-nonabromodiphenylether 17 17 17 BDE 209 Decabromodiphenylether 17 17 17
PFC – Perfluorinated Organic Compounds Perfluorobutanoate (PFBA) 14 12 13 Perfluoropentanoate (PFPeA) 14 12 13 Perfluorohexanoate (PFHxA) 14 12 13 Perfluoroheptanoate (PFHpA) 14 12 13 Perfluorooctanoate (PFOA) 14 12 13 Perfluorononanoate (PFNA) 14 12 13 Perfluorodecanoate (PFDA) 14 12 13 Perfluoroundecanoate (PFUnA) 14 12 13 Perfluorododecanoate (PFDoA) 14 12 13 Perfluorobutanesulfonate (PFBS) 14 12 13 Perfluorohexanesulfonate (PFHxS) 14 12 13 Perfluorooctanesulfonate (PFOS) 14 12 13 Perfluorooctane sulfonamide (PFOSA) 14 12 13

PAH Anthracene 18 18 Pyrene 18 18 Benzo[ghi]perylene 18 18 Benzo[e]pyrene 18 18 Indeno[1,2,3-cd]pyrene 18 18 Perylene 18 18 Benzo[b]fluoranthene 18 18 Fluoranthene 18 18 Benzo[k]fluoranthene 18 Acenaphthylene 18 18 Chrysene 18 18 Benzo[a]pyrene 18 18 Dibenz[ah]anthracene 18 18 Benz[a]anthracene 18 18 Acenaphthene 18 18 Phenanthrene 18 18 Fluorene 18 18

## AXYS Analytical Services Ltd.

ACC-101 Rev 06, 29-Jun-2011 Page 15 of 18 Canadian Association for Laboratory Accreditation (CALA) Washington State Department of Ecology Accreditation No.: A 2637 Lab. ID: C404 TABLE 2

W S Pulp T NP W S Naphthalene 18 18
PPCP (Pharmaceutical and Personal Care Products) Acetaminophen 19 19 Azithromycin 19 19 Caffeine 19 19 Carbadox 19 19 Carbamazepine 19 19 Cefotaxime 19 19 Ciprofloxacin 19 19 Clarithromycin 19 19 Clinafloxacin 19 19 Cloxacillin 19 19 Dehydronifedipine 19 19 Digoxigenin 19 19 Digoxin 19 19 Diltiazem 19 19 1,7-Dimethylxanthine 19 19 Diphenhydramine 19 19 Enrofloxacin 19 19 Erythromycin 19 19 Flumequine 19 19 Fluoxetine 19 19 Lincomycin 19 19 Lomefloxacin 19 19 Miconazole 19 19 Norfloxacin 19 19 Norgestimate 19 19 Ofloxacin 19 19 Ormetoprim 19 19 Oxacillin 19 19 Oxolinic acid 19 19 Penicillin G 19 19 Penicillin V 19 19 Roxithromycin 19 19 Sarafloxacin 19 19 Sulfachloropyridazine 19 19 Sulfadiazine 19 19 Sulfadimethoxine 19 19 Sulfamerazine 19 19 Sulfamethazine 19 19 Sulfamethizole 19 19 Sulfamethoxazole 19 19 Sulfanilamide 19 19 Sulfathiazole 19 19 Thiabendazole 19 19 Trimethoprim 19 19 Tylosin 19 19 Virginiamycin 19 19
Anhydrochlortetracycline (ACTC) 19 19 Anhydrotetracycline (ATC) 19 19 Chlortetracycline (CTC) 19 19 Demeclocycline 19 19

## AXYS Analytical Services Ltd.

ACC-101 Rev 06, 29-Jun-2011 Page 16 of 18 Canadian Association for Laboratory Accreditation (CALA) Washington State Department of Ecology Accreditation No.: A 2637 Lab. ID: C404 TABLE 2

W S Pulp T NP W S Doxycycline 19 19 4-Epianhydrochlortetracycline (EACTC) 19 19 4-Epianhydrotetracycline (EATC) 19 19 4-Epichlortetracycline (ECTC) 19 19 4-Epioxytetracycline (EOTC) 19 19 4-Epitetracycline (ETC) 19 19 Isochlortetracycline (ICTC) 19 19 Minocycline 19 19 Oxytetracycline (OTC) 19 19 Tetracycline (TC) 19 19
Bisphenol A 19 19 Furosemide 19 19 Gemfibrozil 19 19 Glipizide 19 19 Glyburide 19 19 Hydrochlorothiazide 19 19 2-hydroxy-ibuprofen 19 19 Ibuprofen 19 19 Naproxen 19 19 Triclocarban 19 19 Triclosan 19 19 Warfarin 19 19

Albuterol 19 19 Amphetamine 19 19 Atenolol 19 19 Atorvastatin 19 19 Cimetidine 19 19 Clonidine 19 19 Codeine 19 19 Cotinine 19 19 Enalapril 19 19 Hydrocodone 19 19 Metformin 19 19 Oxycodone 19 19 Ranitidine 19 19 Triamterene 19 19
Alprazolam 19 19 Amitriptyline 19 19 Amlodipine 19 19 Benzoylecgonine 19 19 Benztropine 19 19 Betamethasone 19 19 Cocaine 19 19 DEET (N,N-diethyl-m-toluamide) 19 19 Desmethyldiltiazem 19 19 Diazepam 19 19 Fluocinonide 19 19 Fluticasone propionate 19 19 Hydrocortisone 19 19 10-hydroxy-amitriptyline 19 19 Meprobamate 19 19

## AXYS Analytical Services Ltd.

ACC-101 Rev 06, 29-Jun-2011 Page 17 of 18 Canadian Association for Laboratory Accreditation (CALA) Washington State Department of Ecology Accreditation No.: A 2637 Lab. ID: C404 TABLE 2

W S Pulp T NP W S Methylprednisolone 19 19 Metoprolol 19 19 Norfluoxetine 19 19 Norverapamil 19 19 Paroxetine 19 19 Prednisolone 19 19 Prednisone 19 19 Promethazine 19 19 Propoxyphene 19 19 Propranolol 19 19 Sertraline 19 19 Simvastatin 19 19 Theophylline 19 19 Trenbolone 19 19 Trenbolone acetate 19 19 Valsartan 19 19 Verapamil 19 19



## Table 1 and Table 2 - Explanation of Terms Used :

• NELAP = National Environmental Laboratory Accreditation Program

• Non-potable water = water not fit for consumption without treatment as it may contain

pollutants, contaminants, minerals or infective agents. Surface water, ground water, rainwater, effluents as well as any other non-drinking water sources are included in this category.

• Solid = environmental solid sample. Soil, sediment, biosolids, hazardous waste, mixed phase

samples with significant solids content are included in this category.

• Performance based implementation = methodology follows that of the method reference but

modifications deemed by AXYS as minor 1 

## may apply, results meet method reference data quality standard.

• Performance based modification = modi fications deemed by AXYS as significant 2 

## have been

made to method reference protocol, results meet method reference accuracy standard. The suitability of the methodology for any method prescriptive applications should be assessed based on the modifications made and the specific work requirements.

• Performance based method = an in-house AXYS method, published method reference not

applicable.

• GC/LRMS = gas chromatography, low resolution mass spectrometry detection.

• GC/HRMS = gas chromatography, high resolution mass spectrometry detection.

• GC/ECD = gas chromatography, electron capture detection.

• LC/MS-MS = liquid chromatography, mass s pectrometry-mass spec trometry detection.

## AXYS Analytical Services Ltd.

ACC-101 Rev 06, 29-Jun-2011 Page 18 of 18 

## Note 1: Performance Based Implementation - Examples of Minor Modifications - use of additional isotopically labeled references - adjustment of calibration range - adjustment of clean-up technique - use of a different extraction of same general type (example soxhlet vs soxhlet Dean Stark) - addition of matrix type using same principles (example addition of tissue matrix using same

detection principle and similar extraction type)

Note 2: Performance Based Modification - Examples of Significant Modifications - different acquisition conditions using same detection principle (example MS SIM vs. full scan) - different internal control limits while meeting method reference accuracy standard