2045 Mills Road West TEL 250-655-5800 FAX 250-655-5811 SIDNEY, BRITISH COLUMBIA, CANADA V8L 5X2 

### www.axysanalytical.com



# AXYS Client No.: 4380
Client Address: DuPont CRG - URS Corp. 4051 Ogletown Road, Suite 300 Newark, DE, USA, 19713

The AXYS contact for these data is Kalai Pillay.

# PERFLUORINATED ORGANIC ANALYSIS

TISSUE SAMPLES

PROJECT NAME: WWO – Phase III

Contract: 4380 Data Package Identification: DPWG39837 Analysis WG39723



# 27 April 2012

### DUPONT CORPORATE REMEDIATION GROUP TISSUE SAMPLES

PROJECT: WWO PHASE III

NARRATIVE PERFLUORINATED ORGANICS ANALYSIS AXYS METHOD: MLA-043



### 4380: L 17643-1

03 May 2012



### This narrative describes the analysis of one hay sample for the determination of perfluorooctanoate (PFOA) using high performance liquid chromatography/tandem mass spectrometry (HPLC/MS-MS).

SAMPLE RECEIPT, STORAGE AND DESCRIPTION


### The sample was received at AXYS on the 8 th 

### of March 2012. Details of sample conditions on receipt are provided on the Sample Receiving Record form included in the Sample Receiving Documentation section of this data package. The sample was stored at -20°C prior to sample preparation and analysis.

SAMPLE PREPARATION AND ANALYSIS


### The sample and QC samples (a procedural blank, a lab-generated reference sample known as the Ongoing Precision and Recovery (OPR), a duplicate and three matrix spikes: low-level, mid-level and high-level) were analyzed in a single analysis batch named WG39723. The composition of the batch is shown on the Correlation Table and Batch List forms included in this Data Package.

Sample preparation, instrumental analysis and analyte quantification procedures were in accordance with AXYS Method MLA-043: "Analytical Procedure for the Analysis of Perfluorinated Organics Compounds in Tissue Samples by 

### LC/MS-MS". A method summary (MSU-043) ofAXYS Method MLA-043 is included in the data package.

Approximately 19 (wet) of each sample was accurately weighed, spiked with labeled quantification standards and extracted in basic methanol. After extraction, the raw extract was gravimetrically split into two equal portions: a 1/2 portion for cleanup and a 1/2 portion for backup as per Option B. The portion of extract for cleanup was spiked with labeled cleanup standards and then cleaned up using SPE cartridge. The extracts were then spiked with labeled recovery (internal) standards, and analyzed using liquid chromatography/mass spectrometry (LC-MS/MS). Analyte concentrations were determined by isotope dilution/internal standard method, comparing the area of the quantification ion to that of the 13C-labelled standard and correcting for response factors. Linear regression equations with 1/X2 weighting fit were determined from a multi-point calibration series prepared alongside the samples. Final results are calculated in terms of the whole sample extracted.

CALCULATIONS 

### Target compounds were quantified using isotope dilution/internal standard method, comparing the area of the quantification ion to that of the 13C-labelled standard and correcting for response factors. Linear quantification equations were determined from a multi-point calibration series with 1/X2 weighting fit and expressed as below:

### Y 

## = slope x 

### X 

### + intercept

Where: Y = 

### response ratio = 

## x conc. of Surr (ng/sample ) . (area of Target )
area of Surr

X 

## = concentration of target (ng/sample)

The slope and intercept were used to convert raw peak areas in sample chromatograms to final concentrations as follows:

Sample Conc. 

# = x 

## weight of Surr(ng/samplfj-mtercept x -- x . 

## ( area of Target

. .) ( 

## 1 ) [ 1 

# J

area of Surr slope sampleslze(g)

where 

## Surr is the surrogate standard

The recovery of the surrogate standard was calculated and monitored as an indication of overall data quality. Final target concentrations were recovery corrected by this method of quantification.

The standard concentrations and quantification equation can be found in the summary reports for the initial calibration in the Analysis Chromatography/Instrument QC section of this data package.

The lower reporting limit (R.L.) was defined as the concentration equivalent to the lowest calibration standard analyzed (LMCL) or the sample specific detection limits (SOL), whichever was greater.
LMCL 

# = [Lowest calibration standard concentration (ng/sample) x dilution factor or extract split factorj/sample size (g)



## SDL 

# = 

# (3

x

# Hei~ht of noise x 

## weight of Surr (ng/sample)

_ intercept) x 

# (_1_) x ( 

# 1 . ) Height 

## of Surr slope samp/eslze(L)

Three times noise height was used to calculate SOL in the same way as calculation of analyte concentration using the above formula.

The information for the final volume, quantification standard amounts, dilution factor and sample size can be found on the report forms in Analysis Reports/Sample Data section and/or the raw data in the Analysis Chromatography/Sample Data section of this data package.

The method summary (MSU-043) ofAXYS Method MLA-043 provides QC specifications for Ongoing Precision and Recovery (OPR) test sample. Recovery acceptance criteria for this work are 70-130% for the reported compound.

### For analyte concentrations greater than 10 times the reporting limits, RPD acceptance criteria for duplicates are 40 except for PFOA which is 20.

A calibration point in a calibration series is excluded if the analyte recovery is not within the method acceptance criteria for initial calibration (Table 7 ofAXYS Method MLA-043) and/or the resulting correlation coefficient of the calibration curve is less than 0.95.

REPORTING CONVENTIONS


### The AXYS contract number assigned for internal tracking was 4380. Individual samples were assigned a unique laboratory identifier of the form LXXXXX-X, where X is numeral. All data reports reference these unique AXYS IDs plus the client's sample identifier. To assist with locating data, a table correlating AXYS ID with the client sample number is included in this data package. Any extra work required and performed after the initial instrumental analysis of the sample's extract is given an extra "test suffix" code. The single letter code per extra work performed is added to the AXYS sample ID as a suffix, and is combined with any other applicable test suffix codes. The extra work codes used to report data in this package include: (A) 

## = the parent sample for a duplicate pair

The following laboratory qualifier flags are used in this data package:

U 

## = identifies a compound that was not detected
Results are reported in concentration units of nanograms per gram (ng/g). Concentration and detection limits are provided to two significant figures. Analysis results for each sample are provided on Analysis Report Form 

## 1A12.

QA/QC 

### NOTES 

### Samples and QC samples analyzed in each analysis batch were carried intact through the entire analytical process. The sample data were reviewed and evaluated in relation to the batch QC samples.

• Sample analyte concentrations are not blank corrected. The data should be evaluated with consideration to the procedural blank results.

• By virtue of the isotope dilution/internal standard quantification procedures, data are recovery corrected for possible losses during extraction and cleanup.

• All linearity, CALNER, OPR, Lab Blank, Matrix Spike, duplicate and labeled compound recovery specifications were met with the following exception:

The native spiking concentration of the low-level Matrix Spike (AXYS ID: WG39723-104) was very small relative to the concentration of the client sample WWO-X-OH-11 (HAY) (AXYS ID: L 17643-1). Consequently, this MS test cannot be used for quantification of spike recovery.

The Signal/Noise (S/N) ratios were measured as '0' for some compounds in the QC samples and sample data. This has been determined to be a limitation of the software and would not affect the data.

## ANALYTICAL DISCUSSION

WG39723


### The initial extraction was attempted using a 2g sample size but was unsuccessful, consequently the sample size for the analysis batch was reduced to 19.

A 30 minute sonication of the samples was employed during the extraction procedure. Further, it was observed that approximately 5g out of the 10mL of extraction solvent was recovered after the centrifuge step. The labeled compound recovery specifications of the method were met and overall data are deemed not to be significantly impacted by this variance.



## DATA PACKAGE
This data package was assigned a unique identifier, DPWG39837, shown on the cover page of the data package. Included in the data package after this narrative are the following documents:

• Method Summary
• Sample 'Correlation Table'
• Sample Receiving Documentation
• Sample Homogenization Records
• Laboratory Extraction Workup sheets for each sample
• Sample data reports (in order ofAXYS Sample ID)
• Laboratory QC data reports
• Instrumental QC data reports (organized by analysis date)
• Sample raw data (in order ofAXYS Sample ID)
• Laboratory QC raw data
• Instrumental QC raw data (organized by analysis date)



## I certify that this data package is in compliance with the terms and conditions of the contract, both technically and for completeness, except for the conditions detailed above. In addition, I certify, that to the best of my knowledge and belief, the data as reported are true and accurate. The following signature, on behalf of AXYS Analytical Services Ltd, authorizes the release of the data contained in this data package.


# tJ3 fY} 

# 12
Date tttned

## AXYS Analytical Services Ltd.

MSU-043 Rev 06, 17-Oct-2011 Summary of AXYS Me thod MLA-043 Rev 08 Ver 02 Page 1 of 6 

# Summary of AXYS Method MLA-043 Rev 08 Ver 02: Analytical Procedure for the Analysis of Perfluorinated Organic Compounds in Tissue Samples by LC-MS/MS

AXYS method MLA-043 describes the analysis of perfluorinated organic compounds (PFC) in tissue samples. Typical detection limits are in the range of 0.5 – 1 ng/g for 2 g samples.

Target Analytes Perfluorobutanoate (PFBA) Perfluorobutanesulfonate (PFBS) Perfluoropentanoate (PFPeA) Perfluorohexanesulfonate (PFHxS) Perfluorohexanoate (PFHxA) Perfluorooctanesulfonate (PFOS) Perfluoroheptanoate (PFHpA) Perfluorooctane sulfonamide (PFOSA) Perfluorooctanoate (PFOA) Perfluorononanoate (PFNA) Perfluorodecanoate (PFDA) Perfluoroundecanoate (PFUnA) Perfluorododecanoate (PFDoA)



## EXTRACTION The default sample size is 2 g (wet weight). Surrogate standards are added and the sample is extracted by shaking with methanolic potassium hydroxide solution.



## COLUMN CHROMATOGRAPHY CLEANUP After centrifugation a suitable aliquot of the supernatant is diluted with water and cleaned up by solid phase extraction (SPE) us ing disposable cartridges containing a weak anion exchange sorbent. Optional cleanup may be performed with ultra pure carbon powder. The eluate is spiked with recovery standards and analyzed by LC-MS/MS. Calibration solutions are processed through the same SPE procedure.



## INSTRUMENTAL ANALYSIS Analysis of sample extracts for perfluorinat ed organics by LC-MS/MS is performed on a high performance liquid chromatograph coupled to a triple quadrupole mass spectrometer. The MS is run at unit mass resolution in the Mult iple Reaction Monitoring (MRM) mode.

## AXYS Analytical Services Ltd.

MSU-043 Rev 06, 17-Oct-2011 Summary of AXYS Me thod MLA-043 Rev 08 Ver 02 Page 2 of 6 

## Analytes, Ions, and Quantification References

Target Analyte Typical Retention Time (minutes) Parent Ion Mass Daughter Ion Mass Quantified Against

Perfluorobutanoate (PFBA) 5.0 213 169 13 

### C 4 

### -PFBA 

## Perfluoropentanoate (PFPeA) 5.8 263 219 13 

### C 2 

### -PFHxA 

## Perfluorohexanoate (PFHxA) 6.2 313 269 13 

### C 2 

### -PFHxA 

## Perfluoroheptanoate (PFHpA) 6.6 363 319 13 

### C 2 

### -PFHxA 

## Perfluorooctanoate (PFOA) 7.0 413 369 (169) 1 13 

### C 2 

### -PFOA 

## Perfluorononanoate (PFNA) 7.4 463 419 13 

### C 5 

### -PFNA 

## Perfluorodecanoate (PFDA) 7.9 513 469 13 

### C 2 

### -PFDA 

## Perfluoroundecanoate (PFUnA) 8.5 563 519 13 

### C 2 

### -PFDA 

## Perfluorododecanoate (PFDoA) 9.0 613 569 13 

### C 2 

### -PFDoA 

## Perfluorobutane sulfonate (PFBS) 6.3 299 80 (99) 1 18 

### O 2 

### -PFHxS


## Perfluorohexane sulphonate (PFHxS) 7.2 399 80 (99/119) 1 18 

### O 2 

### -PFHxS


## Perfluorooctane sulfonate (PFOS) 8.2 499 80 (99) 1 13 

### C 4 

### -PFOS 

## Perfluorooctane sulfonamide (PFOSA) 9.9 498 78 13 

### C 8 

### -PFOSA 

## Surrogate Standard
13 

## C 4 

## -Perfluorobutanoic acid ( 13 

## C 4 

## -PFBA) 5.0 217 172 13 

## C 4 

## -PFOA
13 

## C 2 

## -Perfluorohexanoic acid ( 13 

## C 2 

## -PFHxA) 6.2 315 270 13 

## C 4 

## -PFOA
13 

## C 2 

## -Perfluorooctanoic acid ( 13 

## C 2 

## -PFOA) 7.0 415 370 13 

## C 4 

## -PFOA
13 

## C 5 

## -Perfluorononanoic acid ( 13 

## C 5 

## -PFNA) 7.4 468 423 13 

## C 4 

## -PFOA
13 

## C 2 

## -Perfluorodecanoic acid ( 13 

## C 2 

## -PFDA) 7.9 515 470 13 

## C 4 

## -PFOA
13 

## C 2 

## -Perfluorododecanoic acid ( 13 

## C 2 

## -PFDoA) 9.0 615 570 13 

## C 4 

## -PFOA

18 

## O 2 

## –Perfluorohexanesulfonate ( 18 

## O 2 

## -PFHxS) 7.2 403 84 (103) 1 13 

## C 4 

## -PFOA

13 

## C 4 

## –Perfluorooctanesulfonate ( 13 

## C 4 

## -PFOS) 8.2 503 80 (99) 1 13 

## C 4 

## -PFOA

13 

## C 8 

## –Perfluorooctane sulfonamide ( 13 

## C 8 

## -PFOSA) 9.9 506 78 13 

## C 4 

## -PFOA Clean-up Standard
13 

## C 8 

## -Perfluorooctanoic acid ( 13 

## C 8 

## -PFOA) 7.0 421 376 13 

## C 4 

## -PFOA Recovery Standard 13 

## C 2 

## -2H-Perfluoro-2-decenoic acid ( 13 

## C 2 

## -PFOUEA) 7.3 459 394 -

13 

## C 4 

## -Perfluorooctanoic acid ( 13 

## C 4 

## -PFOA) 6.9 417 372 -

1 

### Alternate transition within brackets, may be used if necessary to avoid interference.

## AXYS Analytical Services Ltd.

MSU-043 Rev 06, 17-Oct-2011 Summary of AXYS Me thod MLA-043 Rev 08 Ver 02 Page 3 of 6 

## CALIBRATION A series of at least six calibration solutions prepared in a clean reference tissue matrix similar in composition to the sample extract is used to establish initial multi-level calibration. The calibration solutions contain the analytes of interest covering the working range of the instrument together with labelled surrogate and recovery standards. A mid-level calibration solution is analyzed at least after every 20th sample to demonstrate calibration stability. All calibration solutions are processed through SPE cleanup. The concentration of the lowest level calibration standard used for quantification must exceed the method detection limit (MDL).
Nominal Final Concentrations of Calibration Solutions (ng/mL)
CAL A CAL B CAL C CAL D CAL E CAL F CAL G CAL H PFBA 0.125 0.312 1.25 5 25 50 125 312.5 

### PFPeA 0.125 0.312 1.25 5 25 50 125 312.5 

### PFHxA 0.125 0.312 1.25 5 25 50 125 312.5 

### PFHpA 0.125 0.312 1.25 5 25 50 125 312.5 

### PFOA 0.125 0.312 1.25 5 25 50 125 312.5 

### PFNA 0.125 0.312 1.25 5 25 50 125 312.5 

### PFDA 0.125 0.312 1.25 5 25 50 125 312.5 

### PFUnA 0.125 0.312 1.25 5 25 50 125 312.5 

### PFDoA 0.125 0.312 1.25 5 25 50 125 312.5 

### PFBS 0.25 0.625 2.5 10 50 100 250 625 

### PFHxS 0.25 0.625 2.5 10 50 100 250 625 

### PFOS 0.25 0.625 2.5 10 50 100 250 625 

### PFOSA 0.125 0.312 1.25 5 25 50 50 50 13 

### C 4 

### -PFBA 3 3 3 3 3 3 3 3 13 

### C 2 

### -PFHxA 3 3 3 3 3 3 3 3 13 

### C 2 

### -PFOA 9 9 9 9 9 9 9 9 13 

### C 5 

### -PFNA 3 3 3 3 3 3 3 3 13 

### C 2 

### -PFDA 3 3 3 3 3 3 3 3 13 

### C 2 

### -PFDoA 3 3 3 3 3 3 3 3 18 

### O 2 

### -PFHxS 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 13 

### C 4 

### -PFOS 4.5 4.5 4.5 4.5 4.5 4.5 4.5 4.5 13 

### C 8 

### -PFOSA 3 3 3 3 3 3 3 3 13 

### C 2 

### -PFOUEA 2.5 2.5 2.5 2.5 2.5 2.5 2.5 2.5 13 

### C 4 

### -PFOA 3 3 3 3 3 3 3 3

1 

### Concentrations shown are based on the amount added to ca libration standards, with appropriate split portion (1/10,

1/2 or entire extract) cleaned up on SPE and calculated in terms of a 4 mL extract volume.

## AXYS Analytical Services Ltd.

MSU-043 Rev 06, 17-Oct-2011 Summary of AXYS Me thod MLA-043 Rev 08 Ver 02 Page 4 of 6 

## ANALYTE IDENTIFICATION Positive identification of target PFC, surrogate standard and recovery standards require:

• ≥ 3:1 S:N for parent ion to daughter ion transition.

• Compound retention time falls within 0.4 minutes of the predicted retention times from the mean determined from the Initial Calibration. Natives with labeled surrogate standards must elute within 0.1 minutes of the associated labeled surrogates.



## QUANTIFICATION Target compounds are quantified using the internal standard method, comparing the area of the quantification ion to that of the 13 

## C-labelled standard and correcting for response factors. Linear quantification equations are determined from a multi-point calibration series with 1/X 2 

## weighting fit and expressed as below:
Y = slope × X + intercept

Where: Y = 

## ⎟ ⎠ ⎞ ⎜ ⎝ ⎛ × = (ng) Surr of weight Surr of area Target of area ratio response , and X = weight of target (ng) The slope and intercept are used to convert raw peak areas in sample chromatograms to final concentrations as follows:

Sample Conc. = 

## ⎟ ⎟ ⎠ ⎞ ⎜ ⎜ ⎝ ⎛ ⎟ ⎟ ⎠ ⎞ ⎜ ⎜ ⎝ ⎛ ⎟ ⎠ ⎞ ⎜ ⎝ ⎛ × (g) size sample 1 x slope 1 x intercept- (ng) Surr of weight Surr of area Target of area

where Surr is the surrogate standard

The recovery of the surrogate standard is calculated (by internal standard quantification against the recovery standard using an average RRF) and monitored as an indication of overall data quality. Final target concentrations are recovery corrected by this method of quantification.



## REPORTING LIMITS Concentrations and detection limits for the target analytes are reported. Typical reporting units for all data are ng/g on a wet weight basis. The following are commonly requested reporting limits: Method Detection Limit (MDL) - determined as specified by EPA Fed. Reg. 40 CFR Part 136 Appendix B (no iteration option). The 99% confidence level MDL is determined based on analysis of a minimum of 7 replicate matrix spik es fortified at 1-5 times the estimated detection limit. MDL is determined as required based on accreditation, contract and workload requirements.

## AXYS Analytical Services Ltd.

MSU-043 Rev 06, 17-Oct-2011 Summary of AXYS Me thod MLA-043 Rev 08 Ver 02 Page 5 of 6 

## Lower Method Calibration Limit (LMCL) - determined by prorating the concentration of the lowest calibration limit for sample size and extract volume. The following equation is used. LMCL = ((lowest level cal conc.) x (extract volume))/sample size. Typical extract volume for PFCs in tissues is 4 mL. For the analysis of PFCs it is AXYS standard to report sample concentrations using the LMCL as the lower reporting limit. In cases where the SDL is higher than the LMCL, the SDL will be used as the lower reporting limit. The SDL is defined as follows: Sample Specific Detection Limit or Sample Detection Limit (SDL) – determined individually for every sample analysis run by converting the area equivalent of 3.0 times (2.5 times for EPA 1600 series methods) the estimated chromatographic noise height to a concentration in the same manner that target peak responses are converted to final concentrations. The SDL accounts for any effect of matrix on the detection system and for recovery achieved through the analytical work-up.



## QUALITY ASSURANCE / QUALITY CONTROL All samples are analyzed in batches. The composition of a batch is detailed on a batch sheet. Each batch has the following composition:

• Batch Size - Each batch consists of test samples and additional QC samples.

• Blanks – 5% of the samples within a batch are procedural blanks.

• Duplicates – 5% of the samples within a batch are analyzed in duplicate.

• Matrix Spike/Matrix Spike Duplicate - may be analyzed upon client request.

• Reference Samples - 5% of the samples within a batch are spiked reference samples.
QC Specification Table: Procedural Blank Levels and OPR Recoveries

Analyte Procedural Blank Level ng/g 1 

## Acceptable Matrix Spike (% Recovery) 2


## Perfluorobutanoate (PFBA) < 0.5 70 – 130 Perfluoropentanoate (PFPeA) < 0.5 70 – 130 Perfluorohexanoate (PFHxA) < 0.5 70 – 130 Perfluoroheptanoate (PFHpA) < 0.5 70 – 130 Perfluorooctanoate (PFOA) < 0.5 70 – 130 Perfluorononanoate (PFNA) < 0.5 70 – 130 Perfluorodecanoate (PFDA) < 0.5 70 – 130 Perfluoroundecanoate (PFUnA) < 0.5 70 – 130 Perfluorododecanoate (PFDoA) < 0.5 70 – 130 Perfluorobutanesulfonate (PFBS) < 1 70 – 130 Perfluorohexanesulfonate (PFHxS) < 1 70 – 130 Perfluorooctanesulfonate (PFOS) < 1 70 – 130 Perfluorooctane sulfonamide (PFOSA) < 0.5 70 – 130

1 

### Based on the default Option B extraction procedure a (2 gram sample sizesplit 2X). Procedural blank limits must be

prorated accordingly for Option A or C. 2 

### Marginal exceedance allowance – recovery for one compound may be 60 – 140%.

## AXYS Analytical Services Ltd.

MSU-043 Rev 06, 17-Oct-2011 Summary of AXYS Me thod MLA-043 Rev 08 Ver 02 Page 6 of 6 

## QC Specification Table: Surrogate Standard Recoveries, Calibration and Samples

Surrogate Standard Recovery Range 1

13 

## C 4 

## -Perfluorobutyric acid ( 13 

## C 4 

## -PFBA) 20 - 150%
13 

## C 2 

## -Perfluorocaproic acid ( 13 

## C 2 

## -PFHxA) 40 - 150%
13 

## C 2 

## -Perfluorooctanoic acid ( 13 

## C 2 

## -PFOA) 40 - 150%
13 

## C 5 

## -Perfluorononanoic acid ( 13 

## C 5 

## -PFNA) 40 - 150%
13 

## C 2 

## -Perfluorodecanoic acid ( 13 

## C 2 

## -PFDA) 40 - 150%
13 

## C 2 

## -Perfluorododecanoic acid ( 13 

## C 2 

## -PFDoA) 40 - 150%
18 

## O 2 

## -Perfluorohexanesulfonate ( 18 

## O 2 

## -PFHxS) 40 - 150%
13 

## C 4 

## -Perfluorooctanesulfonate ( 13 

## C 4 

## -PFOS) 40 - 150%
13 

## C 8 

## -Perfluorooctane sulfonamide ( 13 

## C 8 

## -PFOSA) 20 – 130% Clean-up Standard
13 

## C 8 

## -Perfluorooctanoic acid ( 13 

## C 8 

## -PFOA) 40 - 150%

1 

### Lower surrogate recoveries may be reported for individual samples where dilution analysis or spiked sample results

demonstrate acceptable accuracy.


## QC Specification Table: Other Parameters
QC Parameter Specification Instrument Sensitivity Daily, S:N ≥ 3:1 for all analytes for lowest calibration standard. Initial Calibration (native compounds) - Daily, (1/x 2 

## ) weighed linear regression. - For the calculated concentrations, a maximum of 1 point per

calibration solution with a maximum of 3 points for all thecalibration solutions may fall within 60-140% of the actual concentration provided all remaining points, including those for PFOA, PFOS, and PFDA, fall within 70-130% of actual concentration. - Internal guideline - correlation coefficient >0.95. Calibration

curves with lower correlation coefficient values meeting all above criteria may be accepted based on batch specific QC results and professional judgement. - Surrogate recoveries must fall within the same limits as for the

samples in the table above. Continuing Calibration Verification (native compounds) Every 20 samples, determined concentrations must be within 30% of actual concentrations. Surrogate recoveries must fall within the same limits as for the samples in the table above. Instrumental Carryover and Instrument Background Every Initial Calibration, Cal/Ver, or SPM: < 0.3% carryover and area response of analytes in instrument blank < 800 judged following two previous methanol blank injections.

## Lab Name: AXYS Analytical Services Ltd. Project Manager: Kalai Pillay Project Number: N/A Contract No: 4380 Project Name: WWO – Phase III AXYS Method: MLA-043 Data Package Identification: DPWG39837 Program: Tissue Samples
Client Sample No. Lab Sample ID

LAB BLANK WG39723-101 OPR WG39723-102 MATRIX SPIKE WG39723-104 MATRIX SPIKE WG39723-105 MATRIX SPIKE WG39723-106

WWO-X-OH-11 (HAY) L17643-1 WG39723-103 DUPLICATE PERFLUORINATED ORGANIC ANALYSIS CORRELATION TABLE 

# DUPONT CORPORATE REMEDIATION GROUP

# ~)(~AXYS 

# I

2045 Mills Road West TEL: (250) 655-5800 Axys Analytical Services Ltd



### Sidney, British Columbia, Canada V8l5X2 FAX: (250) 655-5811

REPORT TO: INVOICE TO: Company 

# A OQIi'A 

# A-v**Se(~~ff's.** 

# 1}l6rr-- Company

Address 

# n"P o 

## ",1' [(If:':' 

# iSlde.. 14 

# Ret:, N'\ 

## 111.\ Address

'6;:;( 

# klJ 

# 1\1\\' \ 

# 'f i 

# c:":c.



# w: \.tn' 'l\c..J(;,('\ 

## \)€

## t~RD~ Contact 

# m\ 

# ke. J 

# kvttl\"" Contact

Phone 

## -'S 01.. 

# -:r 9 \ t:. 

## 9S ";f-"2., Phone



### FAX FAX
E-mail E-mail Project Name/Number: Sampler's Name: Signature: Sampling Sampling Container Client Sample Identification Matrix Date Time Type/No. 

## WWQ-**)(-()l~ ~\\**  

## (H 

## 1\-11 Itt'-'1 

# 2-H-I2- \ 4.20

Relinquished by (Signature} Date Time Received by (Signature) 

# \}.A 

# '')**~1** 

# 'r],1 

# \\oci) Date 

# Cf&-Mar-L1 Relinquished by (Signature) Date Time Received by (Signature)

Date Remarks 

# CHAIN OF CUSTODY
AXYS CLIENT #: 

# tj 3?£)

ANALYSIS REQUESTED



# 2
(>.- 

## <C



# ---

<t: 

# e p..

AXYS Lab Sample ID (Lab use only)



## t 

# i**''"=I~L.l.1\** = 

# I 'f..

" Courier Waybill No.

Time 

## i i 

# ,;7,0

Sample Receipt Time Cooler Temp °C Custody Seal 

### # Seal Intact YIN Sample Tags YIN

# ~® Express

NotaJi selVices and options are available to all destinations. 

### From

Company

Address

2 

### Your Internal R8terence

3 To

"A"'dd"-re"'s"'s_'-"-

______________ _

Recipient's Tax ID Number Required for Customs Purposes e.9., GST/RFC/VATfIN/EIN/ABN, Of as focally requiretl.
4 

### Shipment Information

Commodiw Description Ib_



# t uta! Declared VaJuefor·Carriage NoB13Arequired.**---------~-"-~-**
Bl3Afi1edelectrooica[J<r- 

## 0 Bl3ASummaryReporting. em

# "'~·'"~~I

i Sa ,?ixpress Package SelVice Packages up to 150tb. (68 kg)

### ~-**011J~dEx** International Priority 

## osC]**f!?,~f,!~;;,~~~J:~t~o~!First**

03 []

### fe~~!fnJ~!::~n~~~d~~~~k~~~omy notavalfab!e. 

### 5b Express Freight SelVice
700 FedEx International Priority Freight Pac,,!,ges over 150 Ib. (6ti kg)

86r-J FadEx International Economy Freight

6 

### Packaging "'These unique brown boxes with special pricing are provided by FedEx for FedEx IntI, Priority only.
060**F~Ex** Envelope

## 01~' Other_---'='· 020 FedEx Pak 03 0 FedEx 80x 040 FedExTube
15 

## 0 FadEx 10kg 80x· 25 

## 0 FedEx25kg 8ox' 7 

### Special Handling
01L!

### ~?y~,~~Fn~e~~?~;~iOn

8

9 

### Brokllr Selection Optional Notavailable with FedEx International FrrsL



### Payment CA L! Cargo Aircraft Only

Complete paymentuptlons for both transportation charges and duties and taxes. Bill transpollation charges 10: 

# ,- Enter fadEl! Acet No. or CreditCard No. below. 20 Recipient 3 

### [J Third Party 4 

## [J**Cred~** Card 5[] Cash/Cheque

Bill Customs charges to: All shipments may be subjectto Customs charges, which FedEx does not estimate prinfto clearance. 

### r--- Enter FedEx Aect:. No. below. 20 Recipient 30 Third Pany 5 [] Cash / Cheque



### 10 Required Signature Use of this Air Waybill constitutes your agreement to the Conditions of Contract ontha back ofthis Air Waybill. Certain international treatjes, including the Warsaw Convention, may apply to this shipment and limit our liability for damage, Joss, or delay, as described in the Conditions of Contract

Received above shipment in good order and condition. We agree to pay all charges, including Customs duties and taxes as applicable, and we agree to the Conditions of Contract as stated on the reverse side of the Recipient's Copy



# 8763 6479 

# [[lQ] PART 157683 

# 5 7 0 Rev,Date9/D9 ©lS94-2009 FedEx PRINTED IN U_SA RRDA 

# 5391 0426 

# - IDNo.Waybill : Date Shipped:

# ~NO**~MAR-12** AXYS Analytical Services Ltd SAMPLE RECEIVING RECORD Waybill #: 

### 876364795391 Date !Time Received: 

### 08-MAR-12 11 :30 

### AXYS Client & 

### Contract 

## # 4380;.DuPont Project Number: Receipt No: 

### WB12869 Login Number:
Received By: KPETTINGER Axys Sample ID's: 

# LJ**'~,LIJ** 

# .... I I Log in by:

Matrix Type: 

### 2 Tissues
Condition of Shipping Container:

# 'T~8ck Temperature upon Receipt: 

### ·19 Celcius Sample arrived frozen on dry ice.
Custody Seals: Shipping Containers

# yes~o**~)** Samples Yes INo )**-~**

Chain of Custody or Documents: SamplelD's Collection Location Date & Time Collection Collector's Name

Sample Tags Sample Labels Sample Labels Cross Referenced toCOC Sample Tags Cross Referenced to Sample Labels Sample Tags Cross Referenced to COC

Comments:

Action Taken: Intact Yes INo

Intact Yes INo

Yes

/'-.., 

# fff VNO 

# &INO

YeslNo
YeslNo Seal Numbers Yes INo

Seal Numbers Yes INo

Tracking Report IPacking List: Sample Tag Numbers Sample Type Preservative Added Preservation Requested yes.

# '~:**Y~I** 0 

## i

## ~s)~ Yes

### I~i) Yes 

# 'e)

Information Agrees Information Agrees Information Agrees Signature:

# .¥-:m-~'

Thermometer ID: 3093



# c9 NO

Yes INo Yes INa

# ~](($ AXYS

Axys ID versus AXYS Analytical Services Ltd. Login Chain of Custody Report (In01) 

### Apr. 

## 13, 2012 11:23 AM 

### Login Number: L 17643 

### Account: 4380 

### DuPont

Project:

Client Sample Identification
L 17643-1

WWO-X-OH-11 (HAY) 17-FEB-1214:20

Tissue Tissue EDataDeliv D.Package ANY FC043.HALF HOMOGEN IZA TlON PFC EDD PFOS DATA PKG SAMPLE RECEIPT Storage: WIF-4, 6A Received 08-MAR-12 

### Page: 1 of 1

Due PR

USD USD USD USD USD

### Sample Labeling Information: Batch 10: WG39726 Method: MLAxxx Sample ID Sample Type and Description AXYS Analytical Services Ltd 

### Date 

# I 

# &A P R-(**~** Analyst

# W~!YL" Contract,-,,#,,---: 

## _--"4",,38,,,-0_

Original Labeling 

# WD\6Nfl.-U

L 17643-1 

# zi olorK**hv.~** 

# t" \ \**~** 

## ",,-I lOlA 

# I Cirm' (bl't>wll 

# wWo- k()t-\-II**~** 

# [1-1AY'\ 

# dr, H&"lI 

### "'-
. 

### , 

# I

I

FWO-305 Rev 06, 22-Feb-2010 Reviewed 

### by 

# ;:'l':c.- date 

## II. -Ap 

## (-1'1- Page 

# -I- of 

# -+

' ,

## Sample Preparation
- Sample weights

WG: WG39726

on sample + container sample container (9) (9) 

### Sample ID (9)

L 

### 7643-1 ''IIQH

# Ij~;~~i 

# J:{.W/

Reviewed by: 

# )()L

FWO-342 Rev 03. 22-Feb-2010 Date:

water discarded (9) 

# L AXYS Analytical Services Ltd. 

# I C-A 

# PR-[l

After sample + container (9) (9)

# ~I' 81**~.:.:**


# .. '<::::?:



# ..**~**

. 

### / 

### Chemist: 

# W 

# Q/S!:?l/

on sample (gl**~ub** J3.Csize sample

# (m~) ;2on

# ~ :',2Si{? Contract: 4380**~** 

### wt (g)**~ub**

## Ja(;:~~e 

## wt (g) :O;ub

## ja(;:~~e wi (g) sample sample


# 1;b·17

, i 

### Page_of]

## Tissue Sample Preparation Record Sample 

### 10 Sample type L 17643-1 OW)lOle body 1 Ofillet

## >\?~

# ~ther 

# h"y
f / 

### Protocol Followed OTOC II'lPFOS 

### Sample 

### 10 Sample type
Owhole body 10filiet

Dother



### Protocol Followed OTOC 10PFOS 

### Sample 

### 10 Sample type
Owhole body 1 Ofillet



### Dother



### Protocol Followed OTOC 10PFOS 

### Sample 

### 10 Sample type
Dwhole body 

# I Dfillet
Dother



### Protocol Followed OTOC 10PFOS 

### Sample 

### 10 Sample type
Owhole body 1 Ofillet

Dother



### Protocol Followed OTOC 10PFOS 

### Sample 

### 10 Sample type

Dwhole body 

### I Dfillet
Dother



### Protocol Followed OTOC 10PFOS


### Reviewed by:

__ 

## S=·"'D=--G=--

__ _

FWO-104 Rev 07, 23-Sep-2009 AXYS Analytical Services Ltd.

WG· WG39726 Discard excess tissue Grinder / OG0110G03 OG0410G05 

### Dyes**~no** 

### Filleted/Djssected Virtis Blender Dyes 

## EJ"no 

# o large 

# I 0 stator OB0610B07 DMetals Droutine organics 

## & ",b" 

# 11 'If Discard excess tissue Grinder Dyes Ono OG0110G03 OG0410G05 

### Filleted/Dissected Virtis Blender Dyes Ono Dlarge 

# I Dstator OB0610B07 DMetals Droutine organics 

### Discard excess tissue Grinder Dyes Ono OG0110G03 OG0410G05 

### Filleted/Dissected Virtis Blender Dyes Ono Dlarge 

# I Dstator OB0610B07 

# o Metals Droutine organics 

### Discard excess tissue Grinder Dyes Ono OG0110G03 OG0410G05 

### Filleted/Dissected Virtis Blender Dyes Ono Dlarge 

# I Dstator OB0610B07 DMetals D routine organics 

### Discard excess tissue Grinder Dyes Ono OG0110G03 OG0410G05 

### Filleted/Dissected Virtis Blender Dyes Ono Dlarge 

# I Dstator OB0610B07 OMetals Droutine organics 

### Discard excess tissue Grinder Dyes Ono OG0110G03 OG0410G05 

### Filleted/Dissected Virtis Blender Dyes Ono Dlarge 

# I Dstator OB0610B07 

# o Metals 

# o routine organics 

### Contract· Equipment used: Os),atula I

# ~cissors Dforceps 

# 10spoon Dshears Dknife
Dstainless steel bowl 

### Dother 

# - Equipment used: Dspatula 

### Dscissors Dforceps Dspoon 

### Dshears Dknife
Dslainless steel bowl Dother 

### Equipment used: Dspatula 

### Dscissors 

# o forceps 

### Dspoon Dshears 

# o knife
Dstainiess steel bowl 

### Dother 

### Equipment used: Dspatula 

### Dscissors Dforceps Dspoon Dshears 

# o knife
Dstainless steel bowl Dother 

### Equipment used: Dspatula Dscissors Dforceps Dspoon Dshears Dknife
Dstainless steel bow!
Dother 

### Equipment used: Dspatula Dscissors Dforceps Dspoon Dshears Dknife
Dstainless steel bowl Dother 

# ,

Dscalpel

Dscalpel

Dscalpel

Dscalpel

Dscalpel

Dscalpel



### Page of 

# 4 \AXYS Analytical Services Ltd 

## Notes: 

## Batch ID: 

# WG39726 Method: MLAxxx



## Date: Analyst Fraction Notes:

I



### 1/ ! ,"" Reviewed 

### by date,

__**iQn,---,-!1'f.f-~,,-i _~** **~I/~_** I Page 

# L-t 

# ofl FWO-314 Rev 04, 13-May-2008BATCH LIST PART ONE AXYS Analytical Services Ltd Samples, Batch Surrogate. Recovery Spiking details 

## BATCH ID: WG39723

Method 10: MLA·043 R8.02 Comments: Contract 

### # 

# I Sample 

## Iwt Contract 

### # Sample 

## Iwt

-- -- 

### Method 10: 4380 l17643-1 

## ;( 

# ''3 <I.) 

# f"'r**~~6._** 

### Method ID: MtO'QAMt 

# o l,

- -- - -- - 

### Analyst:

- 

# li it

....**!~** - 

### Start Date: 

### I

---- Batch List Author:

--------------- --- 

### __ :**~TH.~_l:** 

### i::R

----- -----**--~---** -**g~~~~~_l3y:_** Project**Mana~er:** Kalai 

### 3 MS required: Low Level Spike: (Cal B level): 200uL of FC039C·AUTI §.Iass",,,,e.!},fl e : N/A

------- 

### Medium Level Spike: (Cal 0 levell OPR level): 320uL of

- 

### Glassware Treatment: 

### N/A FC039B-AUTI

- ----- - ----- -- - ----- 

### Rotovap Type: N/A High Level Spike: (Cal G level): 20uL of FC128A·STKI

---- 

### Matrix: Tissue

- --- -- 

### SalllJJle 

## 15i2:E!: 2 9 

### Moistures required? NO

- 

### Lipids required? NO

------------- Extraction Solvent: SPE 

## I SAR is spiked with 1/2 of the SUR used in the samples. This

--- - --------------- --- - 

### should be clearly stated on the first page of the batch list FMSProgra_m: NIA Save FMS discards? 

### NIA
Biohazard Type: i 

### None previous WG's associated with samples:

S ikin

Before Extraction: After Extraction: Product Samples required: Surrogate Cleanup Surrogate Recovery F. V.
L17643-1. WG39723-101, 102 

### 6\\'1 (%Itz. 

### fJbc**~3**

### ~F-,C",O,,4,,-3.,-He:A:=L,-F _______ 103, 104, 105, 106, '40uL FC021A.SUR/O 

## :tt;r 

## P '20uL FC022A·SURIO {fIN (D )2- 50ul

### FC008A-~C/olt1 4000 ul
FC043_HALF

FSA·004 Rev 16, 16-Feb-2010 

### __**}Ql!~_£'<:.!l?!~_~~_~~Ql_~_itf_** 20uL FC022A·SUR/ 

# 6\" 50ul FC008A-RECI 4000 uL 1-

________ -.-- 

### I

--

----- ..

- - -- ----

-----------

-,--
- - - - ----- --j

- -- -- --

- -

...

- ---

._ ..... _.-

- - ----- -----

--

-- -- - - --- ..
:

U-vial Instructions and Comments:

PPROP SNAP WI SAR T.**spjk.~** wTth 112 of the SUR ws.d in the s.mplos_ CHECK THAT LI PVCD SAR ALSO USES 112 SUR

PPROP SNAP WI PVCD

Page 1

### of~BATCH LIST PART TWO

BATCH ID- WG39723

QC Samples

WG39723-101 BLANK

WG39723-102 SPM

WG39723-103 DUP Type and Weight Analysis QC

i required for:

'FC043 HALF

1G CANADIAN SPRINGS WATER

OPT. A: lG SC520S LSOO· : 30 (1ST-REF). OPT. B&C: 1G: SC5211 (12T- ' REF) FC043,HALF

FC043 HALF

USE L17643-1 ,-------

FC043 HALF

WG39723-104 200ULOF MS FC039C-AUTI

.

WG39723-105 MS 320UL OF FC039B-AUT! FC043,HALF

FSA-004 Rev 16, 16-Feb-2010 Authentic spiking: Comments:

320uLFC039B-AUTI()! -# 10 

# illoj ......_;;\1"

...

.

......

• 200UL 

### C?F FC039C-AUTJ <5\ 

### 14 I; 

# ""'

.

.....•. Low Level Spike

320uL FC039B-AUTJ

....

- Medium Level Spike AXYS Analytical Services Ltd

QC Samples Type and Weight

WG39723-106 20UL OF MS FC128A-STKJ

WG39723-107 SAR SAR •

i

;

, Analysis QC required for:

FC043,HALF

FC043_HALF OC samples, Authentic Spiking and Comments

Authentic spiking: Comments:

20UL OF FC128A-STKllH 11- 

## 3 81z2. 

### HP

High Level Spike

.......

: 160ul FC0398-AUTI

. ..

...

## Page2of~

## ~)1[(1io Work Group: WG39723 4380 FC tissue Department: 5 

### PAH,LC,

... Lab AXYS 

### Operator: Path ofWG: S 8 9 10 12 20 30 

### Sample & 

### Account Product Matrix
L17643-1 4380 FC043.HALF T WG39723-101 BLANK FC043.HALF T 

### Created: 13-APR-2012 Due:

Deadline [PrJ Status Location & 

### Comments
24-MAY-12 

### [-I WG STORAGE" WJF-4, 6A.

..



### - [-I WG COMMENTS'" 1G CANADIAN SPRINGS WATER

.. 

### AXYS Analytical Services Ltd. Work Group Report (wk02) 13-APR-2012 

### 11 :07 AM 

### Page 1 

### of 1

WG39723-102 SPM FC043.HALF T



### - [-I WG COMMENTS = OPT. A: 1G SC5205 LSOO-30**(15T~REF).** OPT. B&C: 1G SC5211 (12T-REF)

... WG39723-103DUP FC043.HALF T



### - [-I WG COMMENTS'" USE l17643-1 ,., WG39723-104 MS FC043.HALF T -[-] WG COMMENTS = 2QOUL OF FC039C·AUTI

... WG39723-10S MS FC043.HALF T



### - [-I WG COMMENTS'" 320UL OF FC039B-AUTf

.. , WG39723-106 MS FC043.HALF T



### - [-I WG COMMENTS'" 20UL OF FC128A-STKJ

.. WG39723-107 SAR FC043.HALF T



### - [-I WG COMMENTS = SAR

.. 

### Axys ID versus Client ID Information L 17643-1 WWO-X-OH-11 (HAY) {(pname WWO PHASE III) (collect 17-FEB-12 14:20:00) 

# «» «» (rec.date 08-MAR-12)} 

### QC Samples: WG39723-101 BLANK IG CANADIAN SPRINGS WATER WG39723-102 SPM OPT. A: IG SCS20S LSOO-30 (1ST-REF). OPT. B&C: IG SCS211 (12T-REF) WG39723-103DUP (LI7643-1) USE L17643-1 WG39723-104 MS 200UL OF FC039C-AUT/ WG39723-10S MS 320UL OF FC039B-AUT/ WG39723-106 MS 20UL OF FCI28A-STKI WG39723-107 SAR SAR 

### Surrogate, Recovery, and Calibration Standards, and Workgroup Comments:

Moisture, TSS, Lipid Workgroups Associated with these Samples:

### Sample Labeling Information: Batch 

## 10: WG39723 Method: MLA-043 R8.02 AXYS Analytical Services Ltd 

### Date 17 

## 6ff?J:>- Analyst: 

# '1 

# -&

Sample 10 Sample Type and Description


## L17643-1 

# Vl-J d 

## vr'f WG39723-103 (OUP) 

# If

, 

### - - FWO 305 Rev 06, 22 Feb 2010 f

1'. 

# v 

# D J"M-€ 

## "vf LI7hl.f?-1 

## I 

# I

c \' 'r\ \**Ll-~r** i ReViewed by 2;. 

### \l date: 

# 'h. ,. L



# , Contract>.2#",:

__ 

## ",4""38,,,0,,-

Original Labeling 

## WWO X-Ol-\-II (liAr)


# WWO-'X DH-ll(i'WO

I

I**~~** 

# ,,- ;. 

## c, " Page**~** ot _,_ 

## n leI 

# 7

### Sample Labeling Information: Batch 10: WG39723 Method· MLA-043 R8.02 AXYS Analytical Services Ltd 

### Date: I 

# 7 AfjR I 

### 2. Analyst

## '1~
Sample ID Sample Type and Description


### WG39723-104 (MS) 

# Wof n. -h

### ~ } 

# rvl5: eJ-**t-\164-~ ~l**  

## (/ V J 

# Ur-j,f A



## - 

## M <; 

# O,\-**Ln6'1-~-1** 

### WG39723-105 (MS) 

## if iI



### WG39723-106 (MS) 

# tAN C!AfYJ., 

## VS 

# MS 

# Dr 1--11104-(-1 

# t 0 !



### FWO-305 Rev 06, 22-Feb-201 0 Reviewed by

## 9~ date \ 

# 'b fll/ 

# \1... Contract'" #",-: 

### _--,N.:cO""N""E=-

Original Labeling 

# wwO X-o\-\ \\(I-IA'O


# ItJWO -X-O\-\ II (HAl)


# Wwo -x-n\-\-I\ 

# lHAn**Page~** 

# oflAXYS Analytical Services Ltd 

### Sample Labeling Information: Batch ID: 

## WG39723 Method MLA-043 R8 02 Sample ID Sample Type and Description


### WG39723-101 (BLANK) C 

# le<:>..'t eotoY"\{OSS 1,'1) \A 

## i 

# cl. V Analyst: 

# Ij-fa

- (7t-o(pd 

## cA-Y"M 

# «,\ "'-VI 

## k

WG39723-102 (SPM) Ii 

## ",llow V"\ 

### 0 

## i 

## S h"V'P**-\::\s~",e** 

## - 

## Sp'\<.ecl 

# li"ta:h-, )(

WG39723-107 (SAR) r. h (\ 

## :'.1-'1_1<...

FWO-305 Rev 06. 22-Feb-2010 

# -! \ date

## ~ 

## I**~A~'** 

## lZ Reviewed 

### by ';;:)**~** 

# SN- "Ar'" Contracotl:**#~:** 

### __**N!:!.O~N-,=-E**


### Original Labeling 

## c::i:lACtd1<t¥l 5ihv-tAa< 

## wa;te.V' ;j:\: 

# 3'3 Lt 

# " L 

# '500-1 too 

## '5 '2-T- RSj:: 

## 1\'26 

# -- ;--**pag~ofl**

## I 

## Sample 

## Wt & Moistures: Batch ID: 

# WG39723 Method: MLA-043 R8.02


## Sample ID Tare (a)
L 17643-1 WG39723-101 (BLANK)

WG39723-102 (SPM)
WG39723-103 (DUP)

. 

## WG39723-104 (MS) WG39723-105 (MS)
WG39723-106 (MS) WG39723-107 (SAR)



# I AXYS Analytical Services Ltd



## Date:'"' 

# AP !\12..Analyst:

# ~ Balance

# O~;:if1~ :2.022..

Moisture (SLA-015) (all weights in grams) Tare 

## + Wet Tare 

## + dry Tare (b) Tare 

## + wet Tare 

## + dry

1.8 171l;Pfl l2



## Moistures into oven: Date:

____ Time:

____ Analyst:

___ Out of Oven: Date:

____ Time:

___ _ 

## Extraction Information: Soxhlet: Dean Stark: Steam Distillation: Base Digest:

__ Sample 

## Backup WI or Vol 

### (9) (SLA-OSS) 

# (9 or mL) 

# 0.<17 N20
{.O( 

# e-fft/. o 

# 3 

# O.qq 0.'(1 

# o.en 1. 00 I



### I



## Analyst:

__ _ Vol: mL ----' 

## Drying: Drying Time: mins Analyst: Reagent:

______ _ Extraction Solvent used: Volume:

____ mL Begin: Date: Time:

____ Analyst:

____ End: Date:

____ Time:

____ Analyst:

__

FWO-306 

### Rev 08. 02-Jan-2011 Reviewed 

### by**_~,---_date** ---'-"-'-''l'-'--'--= 

### I Page

__ of 

## ----1--AXYS Analytical Services Ltd 

## Spiking Sheet: Batch 

## 10,---: 

## -'-W-'--G=.o:3-=:9-=-7=2""3

____ _ Method: MLA-043 R8.02 SLA-017 Witness name/ initials: 

# 9,", (;(fl.N:m/5Cr Before extraction Before extraction Cleanup Std. Cleanup Std. Recovery Recovery Surr. 10: 

### ((.Q;;2tA- 5uljQI Surr. 10:

### H:;.O::lIA-5i}~i 

### Surr.:**fCOU.A-~~liO** 

# I Surr.: Surr.: 

## KOOl5ti- 

# rz£cjC I Surr.: 

### Sample 

## 10 Date: 

### r1 Arc 

### \2 Date: 

## i1= A?(**I~** 

### Date: \'{ 

# Apr \2 Date: o t . 

## 'K r! 

### ·'7 Date: a e. ! 

## tiP; j- 

### Vol.: 

### ':JQ**~L** 

### Vol.: ::10**~L** 

### Vol.: ,"-0**~L** 

### VoL:**~L** 

### Vol.: 

### 50**~L** 

### Vol.:**~L** 

### Syringe#: 

## ll"iJl::J Syringe#: 

### SII::! Syringe#: gilL Syringe#: F.V.: 

## 4cCO uL F.v.:**~L** 

### Ampoule: 

# 1 Ampoule: 

# *' Ampoule: 

## '3 Ampoule: Syringe#: 

## Ii: I q Syringe#:

__

Analyst 

# 'J# Analyst**Ampoule:~** 

### Ampoule:

__ Start time: 

## IDS 6 Starl time:

-- 

### Start time: 

## 1:'J4S Start time: Fin. lime: 

## 1055 Fin. lime: 

## I-::EO 

# -- Fin. time: Fin. time: Time Witness 

### Time Witness 

### Analyst: 

# Sf\! Analyst: Analyst: 

# srJ Analyst: L 17643-1 ;\··:;(Lf 

# Sr-< 

# " / 

# V. \/ WG39723-101 (BLANK) \ f 

### '.::;z Lf 

# g,U 

# " / \I 

# J

WG39723-102 (SPM) \\ ',::24 

## c,r..,( 

# "- / 

# .J .J WG39723-103 (DUP) 1\ : ;1.4 

## C;u 

# '\ 

# V \( WG39723-104 (MS) 

# , , '. de; 

# seC / 

# "- V .1 

# • WG39723-105 (MS) 

# 1".-:1;:; 5(.£ 

# / 

# "- V

. • J WG39723-106 (MS) \ I 

# ;;is C;u 

# / 

# "- .J. -J f 

### WG39723-107 (SAR)


# - -- \ 1· 

# ;;L!?**~.(-<** 

# J ,)

Authentic SId: 

## tCO-S'H)-AVT/OI Authentic Std: 

## F(itJ913-Avl/OI Authentic Std: 

## rCor'lC -Aur:/O( Date: 

# i+ ."?(\@ Date: l-:f.**A~(** j':J 

### Date: 

## Ii-**8~(i;)** 

### Sample 

### 10 VoL: 3-;;20**~L** 

### VoL: 

# tbL2**~L** 

### VoL: ;;?(':{')**~L** 

### Syringe#: 

# 8:0:3 Syringe#: 

## 81C2::i Syringe#: 

## '6 \ 0'], 

### Ampoule#: \0 

### Ampoule#: 

### \0 Ampoule#: 

### (, Analyst: 

## '1tc- Analyst: 

## VI..kI--. Analyst:**~** 

### Time Witness Time Witness Time Witness 

# c:.JG.1LJ -:; ;;21

- ! ()? 

# S!'M 1\·)\ 

# C;u-



# ------- IJGt-1i.( -:l;;lj

- itl'1 

# M<;


# - 

# - il>' C;Cc
I 

# JGt -:91. t;;13

- lOt) 

# Me...**:\.~,.,** \\. 0\. 

# y--, [A)Gt"1"'p;;r-S

- \ 0 

## -:J**~A\:** 

# - - ! I. 

# '1 ::2 

# S:G(

FWO-310 Rev 08, 16-Feb-2010 Reviewed

## by_r~J'l.t\l'i.\ __ date

## '\~) 

# AVe \1, Page of 

# 1

# I

I 

# I


# I

: 

# I Spiking Sheet: Batch 

## ID,--: --'-W-=--=G:..:3:..:9'-'7c.:2=-=3"----

___ _ SLA 017



# - AXYS Analytical Services Ltd


### Method: MLA-043 R8,02 Witness name/ initials'

## ~(.,Q tMA 

### ..-<" 

## Before extraction Before extraction Cleanup Std. 

# I Cleanup Std. Recovery Surr, ID: Surf. ID: Surr,: , Surr,: Surr.: 

### Sample 

## ID Date: Date: Date: 

## I Date: Date: VoL: uL VoL:**~L** 

### VoL:**~L** 

# I Vol.**~L** 

### VoL:**~L** 

### Syringe#: Syringe#: Syringe#: ' Syringe#: F,V,:**~L** 

### Ampoule: Ampoule: Syringe#:

__ Ampoule: Ampoule: Analyst: Analyst: 

### Ampoule:

__ Start time:

-- 

### Start time:

-- 

### Start time: i 

### Fin, time: Fin, time: -- 

## I : 

### , Fin, time: 

# I Time 

### Witness 

# I Time 

# , Witness Analyst: I 

### Analyst: 

# I Analyst: L 17643-1 

# : I ! 

# i WG39723-101 (BLANK) i 

# :

WG39723-102 (SPM) I 

### WG39723-103 (DUP) 

## I WG39723-104 (MS) I 

# I WG39723-105 (MS) 

# : : 

### : 

### WG39723-106 (MS) 

# I I WG39723-107 (SAR) i 

# I : I 

# I ! 

# : : 

# I :
I



### i 

## I : :

: 

# I
Authentic Std: FCI?l5'k 

## STK/tli Authentic Std: 

# I Authentic Std:

# ~~le. 11: 

# ;:;/;§c I@

# ~L Date: Date: Sample 

## 10 VoL:**~L** 

### : VoL: Syringe#: 

## \St;;t;;) Syringe#: 

# I Syringe#: Ampoule#: 

## -S 

# I Ampoule#: Ampoule#: Analyst:**~** I 

### Analyst: Analyst: Time Witness 

# ! Time 

# ! Witness Time 

# I CJ0t'l'1:;Z ;:2"1

- : 0(, 

## 1"\, " \ \ ',-3'1 I 

# SJA' 

# : I I 

# I I 

# ! 

# I

FWO-310 Rev 08, 16-Feb-2010 

## \ 't. (\ \") Reviewed**u,_~--,----** 

### __ date \ OMy( I L/ 

## Recovery Surr.: 

### Date: VoL:**~L** 

### F,V,:**~L** 

### Syringe#:

__ 

# I Ampoule:

__ Start time:

--



### , Fin, time:

Analyst:



# I
I



# I I 

# :**~L**

Witness



### Page 

# I

I

I 

### I



# !



# , of....L...AXYS Analytical Services Ltd



### Extract Splitting Sheet: Batch 10: 

# WG39723 Method' MLA 043 R8 02 

### Balance 

## #:

# ~\ 

# D4 Analyst:

# -=S,,-,~J,--_ Date \ 

# g Apr 

# )1 Time

# ~",-,-D_

- ! 

### Weight (g: Sample ID C-tube + 

### Total Portion + 

### Portion: Portion: Portion: Portion: Portion: C-tube total extract Extract c-tube 

# '/L bi\tv 

# r (column a)

## (fpl~rrr b)

## (~a)9~ (column c) (c-a) (direct wt) 

### (direct wt) 

### (direct wt) 

### (direct wt) L 

## 17643-1 

## I 

## (',Ii:) 

# \ 

# 2S0 I WG39723-101 

## I 

# ",2; .,1>1 H 1'1")2-

1 

# I I 

# 43.£ I (BLANK)**g~u** 

# i ISLi'1 I



### . I I 

## I WG39723-102 i 

# I I 

# I I 

# 3q-, : 

### (SPM) I ( 

### -, 

## () 

# 14 

# '0

, a () 

# I ! I 

# , " ' I I , . I 

## WG39723-103 

# I {;(,g , I 

# SO I 

# 5**I~** 

# I 

# 55 I 

# I (OUP) " .IL I I 

# , WG39723-104 (MS) I 

# ('.1'1. 12.65 

# 5,,'3 I 

# 2££ I 

### I 

## WG39723-105 (MS) 

## I 

## ( 17 

# II 

# ilq I 

# 5i1 

# i 257 I t)" i I 

## WG39723-106 (MS)**~** 

# II 

# " -16 50 L \ 

## 2C,2. 

## WG39723-107



# - i I (SAR) 

# I I i 

# I I 

# I I I I 

### i 

# I I 

# i I i I I 

# I

I 

## I

I 

### i

FWO-311 Rev 06. 1-0ct-2010 Reviewed 

### by**---"'~_** Date -'-'-'-'-'f'---""--- 

### \ \ 

### ---, Page _"'_ of _,_

### AXYS Analytical Services Ltd



## LC Methods Cleanup Worksheet Workgroup' WG39723 Method' MLA 043 R8 02 

# - SPE Pre-Elution! Conditioning: Date:

## \~**J~r\L** Analyst:**~** 

### SPE type: \ffiMO 

### WA\( Lot#: 

# en.; Reagent Lot Vol. Time 

### # mL
0.1 M Formic acid 

# 11.'-\ 

# S \\\ S
0.3% NH 4 

### 0HI 99%

### l~S 

# 5 

# \\\**~** MeOH 1: MeOH

2: MeOH Reagent water type: Acidified water H 2 0 Type

___ (with Hel) pH OCM

2:30:68 Formic acid: Acetonitrile:MtBE

2% NH 4 0H in water H 2 0 Type

Hexane

1: Acetonitrile (CH,CN)

2: Acetonitrile (CH,CN)

0.1 M HCII 5% MeOH
MtBE 10:20:70 NH,OH: MeOH: MtBE

O.SM Sodium Acetate Buffer pH 4
1: 1 Acetonitrile: Acetone 

### Wash: / Load Sample:

__

Reagent
Reagent water type: 50% 0.1 M formic acid/50% MeOH 

### Lot 

### #


# \

'\. \

0.1 M formic acid 

# 1'-4
0.3%) basic (NH,OH)I 99% 

### CS water

20% MeOH/80% 0.1 M formic acid

Acidified water H 2 0Type (with HCI>'" pfH-;--
0.1 M HCII 5% MeOH

Acetonitrile (CH 3 CN)

5%MeOHI 95% water H,O Type 2% NH 4 0H in water. H 2 0 Type

MtBE
OCM

5% acetonitrile in water H,O Type
MeOH 

# 5\ Vol. mL



## c:;



# - 5
L Elution:

Time 

### Reagent Lot 

### #
MeOH 

# l3o.b 0.3% NH 4 OH/99% 

# /M,c'6S MeOH 

# \1.51 Carbon (optional)


## \ 'b2..D 1:1 acetone:MeOH
2 % formic acid in MeOH

Acetonitrile (CH 3 CN)

Hexane
2:30:68 formic acid: acetonitrile: MtBE

OCM

10:20:70 NH,OH: MeOH:MtBE

1:1 OCM:MeOH

3:1 MtBE: MeOH

Ethy! acetate

9:1 MtBE: MeOH

1 : 1 Acetonitrile: Acetone 

## Fraction: Analyst· 

# SN

Reconstitute for J.lvial:

Date: Analyst:

Vol. Time 

### Reagent Lot Vol. Time mL 

### # mL 0.1 % formic acid buffer
1 : MeOH iI

# ~ .-,
2: MeOH 0.3% NH 4 OH/99% MeOH 70:30 MeOH: water H,O Type
..•..

1:1 MeOH: 

### 0.1% acetate buffer

1:1 CH,CN: ammonium acetate, acetic acid buffer 1:1 0.1% Acetic acid in CH 3 CN:Water H,O Type 1: 1 0.2% Acetic acid in CH 3 CN:Water H20 Type 

## I I I Reagent water type:

___ 

# I

MeOH= Methanol; MtBE= Methyl-t-butyl ether; OCM= Dichloromethane; MeCN= CH 3 CN= Acetonitrile; NH 4 0H= Ammonium hydroxide (30% aqueous unless otherwise spec.); CS= Canadian Springs

FWO-334 Rev 02, 19-May-2011 Reviewed by:**--~".LL~------** Date: ....J'-U...Llj'-'--'-"'--

__ Page 

# ofl

### LC Methods Worksheet Workgroup: WG39723 Sample Preparation and Extraction' Analyst-

## '\~;:**~ll** ! '-J V 

### Reagent Lot# Vol. Time Vol. Time mL mL

50% formic acid 

# 1..\\ 

# N\ d"p 

## \DIIO
0,05 M KOH in MeOH 

# 31 to 

## 12:1;0

3% acetic acid 0.3% (NH 4 0H)! 99% MeOH Reagent water type: 

### CS 

# f?":lll \DD 

# \DOO

Carbon (50 mg )

acetonitrile (CH 3 CN)
Formic acid cone.
NH 4 0H cone.
EDTA
0.14 M Na z HP0 4 buffer pH 2 Hel cone. ammonium acetate buffer 1 M, pH 5.0 ammonium acetate buffer 1 M, pH 6.5 ammonium acetate buffer 1 M, pH 4,0 Phosphate buffer 1 M, pH 6,0 enzyme**~-** glucoronidase!sulfalase enzyme 11- glucoronidase 5% NH 4 0H in water H 2 0 type 5% borate buffer pH 9
0.012 g/mL FMOC-CI Acidified water with Hel (pH 

### J
3:1 MtBE:MeOH Sodium acetate buffer a.SM, oH 4 10% acetate buffer pH 4 EDC.HCI
140mM KOH in 80:20 MeOH:Water MeOH

FWO-333 Rev 04, 26-0ct-2011 

### AXYS Analytical Services Ltd
Method: MLA-043 R8.02
Date" 

## V: /' f'( 0" r·,; 

# , Vol. Time mL 

### Sonication

Analyst: 

# ':If'tl
Date: 

## 11 Afl'tl 2
Time: 

### IS: '30 #times: 

### IX**~MI'I\.** 

### :So 

### ':11<

Shak

Date: 

## nAf!?l2.
Time: 

# Is ,,;90 

### #times: 

### l 

# x: I/Ohi".

Oerivatization Analyst:
Date:
Start time:

End time:



### Millipore: Analyst:
Date: Time:



### Filtration: Analyst: Date: Time: 

### Fraction:

Extract pH check/adjust
1. pH 

# '" £.5
Date: 

# \'{, Ao,I2 Time: 

## \oL\D Analyst: 

# SN 2.pH

Date: Time: Analyst: 3.pH Date:
Time:
Analyst:



### Incubation:
Analyst: Date: Start time:
End time:

Reviewed by:

__ '-"'-'-

_______ Date: --'-"LL"i''--'---- 

### Manifold 

### # p':';, Analvst 

# "oN Date: 

## \is hoc 

# no.· Sample 10

L 17643-1 WG39723-101 (BLANK)
WG39723-102 (SPM)

WG39723-103 (DUP)

WG39723-104 (MS) WG39723-105 (MS) WG39723-106 (MS) WG39723-107 (SAR) Position

I 

## L 

## ? 

# 4 

# 5 (;

-, I**~**



# ,**Page~** #filter units

I I



# IAXYS Analytical Services Ltd 

## Notes: Batch 10: 

# WG39723 Method: MLA-043 R8.02



## Date: Analyst Fraction Notes: ". r>Afe·f/.

::. J.\?R 20lZ 

## viP 

## 1s"""oIp !..I 

### -too 

## \",\..--I and.

## ~ i2,. 

### '? (.., 

### I \

## ~ 

## tI"'- IS" '" 

## I -tube. 

## 'e,\l<ol-l--.c 6 B 1".\"<.. 

## <t**,,~J.** 

### 1<1 uJ 

## ".d.**~**
I 

### eircu 10.f"'l UJ n 

# += y
.... 

## d. V< "'- 

### -\-I-e... 3 "- 

## ,n!'" s,'?-e. 

# +0 \ 

# "**d.,-,~ -+~** 

### ~**_"I*o~** 

### '\ VH l+a-tl ""'1'1 

# ,**~**

### I"lAf~ 

### 12 

# 'HlA (V 

# \r.., I Q 

### 6"-\,,,,", waA. 

### '>D V\ " 

# u..:t 

# u -I'M :<l Co '" '''" 0--:< 

## per- Mcvr 

## tl1 

# a
. 

# P

, I Z 

# ADe**'~L** 

# sI'J Arlee**ct~.t\i{"I\;n"** 

# hr. <;aty",nl, s Wt'rt. 

# cttcuo,t, l 

# and Iv 

# 4**~** 

# or -I: 

# xhacl-**w"~** 

# obf";n-rc.**T~csc** S!!."'nirs \!\It.fC. 

### DfrbSCd v 

### An.,," j 

## wi-t\-, 0. 

# sDutul1j 5q 

### UCCL,nu 

# thc sill \'Cd 

### 00+ 

# of fh( heUJ 

# ad**((()iri~J~cd :M~\(**  , 

## i\:c\'\'n' \ 

# or <\66\t\&I\"\**l~xb1+** 

# .**~** v I\j \ c\ J J J -.J**~**

Reviewed by 

# SN dale 

# 15Apr 

# 12

FWO-314 Rev 04. 13-May-2008 Page

# Of~(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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_L17643

- 1_Form1A_FC2G_150S25_SJ1451385.html; Workgroup: WG39723; Design ID: 1817 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. WWO-X-OH-11 (HAY) Sample Collection: 17-Feb-2012 14:20 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. WWO PHASE III
Contract No.: 4380 Lab Sample I.D.: L17643-1 (A)

Matrix: TISSUE Sample Size: 0.970 g (wet)
Sample Receipt Date: 08-Mar-2012 Initial Calibration Date: 18-Apr-2012

Extraction Date: 17-Apr-2012 Instrument ID: LC MS/MS
Analysis Date: 19-Apr-2012 Time: 03:16:54 Column ID: C18MS
Extract Volume (uL): 4000 Sample Data Filename: FC2G_150 S: 25
Injection Volume (uL): 15 Blank Data Filename: FC2G_150 S: 23

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_150 S: 16

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

PFOA 71 1.0 (L) 7:06



## Page 1 of 1 (WG39723 - PFC_FC_LC_PFOA_L17643-1_Form1A_FC2G_150S25_SJ1451385.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_L17643

- 1_Form2_FC2G_150S25_SJ1451385.html; Workgroup: WG39723; Design ID: 1817 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. WWO-X-OH-11 (HAY) Sample Collection: 17-Feb-2012 14:20 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. WWO PHASE III
Contract No.: 4380 Lab Sample I.D.: L17643-1 (A)

Matrix: TISSUE Sample Size: 0.970 g (wet)
Sample Receipt Date: 08-Mar-2012 Initial Calibration Date: 18-Apr-2012

Extraction Date: 17-Apr-2012 Instrument ID: LC MS/MS
Analysis Date: 19-Apr-2012 Time: 03:16:54 Column ID: C18MS
Extract Volume (uL): 4000 Sample Data Filename: FC2G_150 S: 25
Injection Volume (uL): 15 Blank Data Filename: FC2G_150 S: 23

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_150 S: 16

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

13C2-PFOA 72 41 57 7:06

CLEANUP STANDARD

13C8-PFOA 12 11 93 7:06



## Page 1 of 1 (WG39723 - PFC_FC_LC_PFOA_L17643-1_Form2_FC2G_150S25_SJ1451385.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39723

- 103_Form1A_FC2G_150S26_SJ1451386.html; Workgroup: WG39723; Design ID: 1817 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. WWO-X-OH-11 (HAY) (Duplicate) Sample Collection: 17-Feb-2012 14:20 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. WWO PHASE III
Contract No.: 4380 Lab Sample I.D.: WG39723-103 (DUP L17643-1)

Matrix: TISSUE Sample Size: 0.990 g (wet)
Sample Receipt Date: 08-Mar-2012 Initial Calibration Date: 18-Apr-2012

Extraction Date: 17-Apr-2012 Instrument ID: LC MS/MS
Analysis Date: 19-Apr-2012 Time: 03:33:47 Column ID: C18MS
Extract Volume (uL): 4000 Sample Data Filename: FC2G_150 S: 26
Injection Volume (uL): 15 Blank Data Filename: FC2G_150 S: 23

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_150 S: 16

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

PFOA 61 1.1 (S) 7:06



## Page 1 of 1 (WG39723 - PFC_FC_LC_PFOA_WG39723-103_Form1A_FC2G_150S26_SJ1451386.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39723

- 103_Form2_FC2G_150S26_SJ1451386.html; Workgroup: WG39723; Design ID: 1817 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. WWO-X-OH-11 (HAY) (Duplicate) Sample Collection: 17-Feb-2012 14:20 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. WWO PHASE III
Contract No.: 4380 Lab Sample I.D.: WG39723-103 (DUP L17643-1)

Matrix: TISSUE Sample Size: 0.990 g (wet)
Sample Receipt Date: 08-Mar-2012 Initial Calibration Date: 18-Apr-2012

Extraction Date: 17-Apr-2012 Instrument ID: LC MS/MS
Analysis Date: 19-Apr-2012 Time: 03:33:47 Column ID: C18MS
Extract Volume (uL): 4000 Sample Data Filename: FC2G_150 S: 26
Injection Volume (uL): 15 Blank Data Filename: FC2G_150 S: 23

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_150 S: 16

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

13C2-PFOA 72 50 69 7:06

CLEANUP STANDARD

13C8-PFOA 12 13 100 7:06



## Page 1 of 1 (WG39723 - PFC_FC_LC_PFOA_WG39723-103_Form2_FC2G_150S26_SJ1451386.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: ___________ 

## Jenny Pape

___________ 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 13:08:41; Application: XMLTransformer-1.12.13; Report Filename: RPD_FC_LC_PFOA

- RPD_WG39723

- 103_L17643

- 1_.html; Workgroup: WG39723; Design ID: 1817 ] 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. WWO PHASE III
Contract No.: 4380 Client ID: WWO-X-OH-11 (HAY) Concentration Units: ng/g (wet weight basis)
L17643-1 (A) WG39723-103 COMPOUND LAB FLAG 1 CONC.

FOUND LAB

FLAG 1 CONC.

FOUND MEAN RELATIVE PERCENT DIFFERENCE PFOA 71 61 66 16



## Page 1 of 1 (WG39723 - RPD_FC_LC_PFOA-RPD_WG39723-103_L17643 -1_.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39723

- 101_Form1A_FC2G_150S23_SJ1451381.html; Workgroup: WG39723; Design ID: 1817 ] 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.: 4380 Lab Sample I.D.: WG39723-101

Matrix: AQUEOUS (TISSUE METHOD) Sample Size: 1.00 g
Sample Receipt Date: N/A Initial Calibration Date: 18-Apr-2012

Extraction Date: 17-Apr-2012 Instrument ID: LC MS/MS
Analysis Date: 19-Apr-2012 Time: 02:43:22 Column ID: C18MS
Extract Volume (uL): 4000 Sample Data Filename: FC2G_150 S: 23
Injection Volume (uL): 15 Blank Data Filename: FC2G_150 S: 23

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_150 S: 16

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

PFOA U 1.0 (L)



## Page 1 of 1 (WG39723 - PFC_FC_LC_PFOA_WG39723-101_Form1A_FC2G_150S23_SJ1451381.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39723

- 101_Form2_FC2G_150S23_SJ1451381.html; Workgroup: WG39723; Design ID: 1817 ] 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.: 4380 Lab Sample I.D.: WG39723-101

Matrix: AQUEOUS (TISSUE METHOD) Sample Size: 1.00 g
Sample Receipt Date: N/A Initial Calibration Date: 18-Apr-2012

Extraction Date: 17-Apr-2012 Instrument ID: LC MS/MS
Analysis Date: 19-Apr-2012 Time: 02:43:22 Column ID: C18MS
Extract Volume (uL): 4000 Sample Data Filename: FC2G_150 S: 23
Injection Volume (uL): 15 Blank Data Filename: FC2G_150 S: 23

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_150 S: 16

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

13C2-PFOA 72 80 110 7:06

CLEANUP STANDARD

13C8-PFOA 12 12 100 7:06



## Page 1 of 1 (WG39723 - PFC_FC_LC_PFOA_WG39723-101_Form2_FC2G_150S23_SJ1451381.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: ___________ 

## Jenny Pape

___________ 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 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39723

- 102_Form8A_SJ1451375.html; Workgroup: WG39723; Design ID: 1817 ] 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.: 4380 Lab Sample I.D.: WG39723-102
Matrix: TISSUE Initial Calibration Date: 18-Apr-2012
Extraction Date: 17-Apr-2012 Instrument ID: LC MS/MS Analysis Date: 19-Apr-2012 Time: 01:36:19 Column ID: C18MS Extract Volume (uL): 4000 OPR Data Filename: FC2G_150 S: 19 Injection Volume (uL): 15 Blank Data Filename: FC2G_150 S: 23
Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_150 S: 16

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

PFOA 40 43 110 7:06



## Page 1 of 1 (WG39723 - PFC_FC_LC_PFOA_WG39723-102_Form8A_SJ1451375.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: ___________ 

## Jenny Pape

___________ 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 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39723

- 102_Form8B_SJ1451375.html; Workgroup: WG39723; Design ID: 1817 ] 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.: 4380 Lab Sample I.D.: WG39723-102
Matrix: TISSUE Initial Calibration Date: 18-Apr-2012
Extraction Date: 17-Apr-2012 Instrument ID: LC MS/MS Analysis Date: 19-Apr-2012 Time: 01:36:19 Column ID: C18MS Extract Volume (uL): 4000 OPR Data Filename: FC2G_150 S: 19 Injection Volume (uL): 15 Blank Data Filename: FC2G_150 S: 23
Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_150 S: 16

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

13C2-PFOA 72 71 98 7:06

CLEANUP STANDARD

13C8-PFOA 12 12 99 7:06



## Page 1 of 1 (WG39723 - PFC_FC_LC_PFOA_WG39723-102_Form8B_SJ1451375.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39723

- 104_Form1A_FC2G_150S27_SJ1451387.html; Workgroup: WG39723; Design ID: 1817 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. WWO-X-OH-11 (HAY) (MS) Sample Collection: 17-Feb-2012 14:20 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. WWO PHASE III
Contract No.: 4380 Lab Sample I.D.: WG39723-104 (MS)

Matrix: TISSUE Sample Size: 0.970 g (wet)
Sample Receipt Date: 08-Mar-2012 Initial Calibration Date: 18-Apr-2012

Extraction Date: 17-Apr-2012 Instrument ID: LC MS/MS
Analysis Date: 19-Apr-2012 Time: 03:50:25 Column ID: C18MS
Extract Volume (uL): 4000 Sample Data Filename: FC2G_150 S: 27
Injection Volume (uL): 15 Blank Data Filename: FC2G_150 S: 23

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_150 S: 16

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

PFOA 63 1.0 (L) 7:06



## Page 1 of 1 (WG39723 - PFC_FC_LC_PFOA_WG39723-104_Form1A_FC2G_150S27_SJ1451387.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39723

- 104_Form2_FC2G_150S27_SJ1451387.html; Workgroup: WG39723; Design ID: 1817 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. WWO-X-OH-11 (HAY) (MS) Sample Collection: 17-Feb-2012 14:20 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. WWO PHASE III
Contract No.: 4380 Lab Sample I.D.: WG39723-104 (MS)

Matrix: TISSUE Sample Size: 0.970 g (wet)
Sample Receipt Date: 08-Mar-2012 Initial Calibration Date: 18-Apr-2012

Extraction Date: 17-Apr-2012 Instrument ID: LC MS/MS
Analysis Date: 19-Apr-2012 Time: 03:50:25 Column ID: C18MS
Extract Volume (uL): 4000 Sample Data Filename: FC2G_150 S: 27
Injection Volume (uL): 15 Blank Data Filename: FC2G_150 S: 23

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_150 S: 16

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

13C2-PFOA 72 55 76 7:06

CLEANUP STANDARD

13C8-PFOA 12 12 100 7:06



## Page 1 of 1 (WG39723 - PFC_FC_LC_PFOA_WG39723-104_Form2_FC2G_150S27_SJ1451387.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: ___________ 

## Jenny Pape

___________ 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 13:08:32; Application: XMLTransformer-1.12.13; Report Filename: MS_FC_LC_PFOA

- MS

- MSD_WG39723

- 104_L17643

- 1_Form8C.html; Workgroup: WG39723; Design ID: 1817 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. WWO-X-OH-11 (HAY) (MS) Sample Collection: 17-Feb-2012 14:20 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. WWO PHASE III Contract No.: 4380 Lab Sample I.D.: WG39723-104 (MS) Matrix: TISSUE Sample Size: 0.970 g (wet) Extraction Date: 17-Apr-2012 Initial Calibration Date: 18-Apr-2012 Analysis Date: 19-Apr-2012 Time: 03:50:25 Instrument ID: LC MS/MS Extract Volume (uL): 4000 Column ID: C18MS Injection Volume (uL): 15 MS Data Filename: FC2G_150 S: 27 Dilution Factor: N/A Blank Data Filename: FC2G_150 S: 23 Cal. Ver. Data Filename: FC2G_150 S: 16
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

PFOA N/A 2.6 71 63 N/A



## Page 1 of 1 (WG39723 - MS_FC_LC_PFOA-MS-MSD_WG39723-104_L17643 -1_Form8C.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39723

- 105_Form1A_FC2G_150S28_SJ1451388.html; Workgroup: WG39723; Design ID: 1817 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. WWO-X-OH-11 (HAY) (MS) Sample Collection: 17-Feb-2012 14:20 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. WWO PHASE III
Contract No.: 4380 Lab Sample I.D.: WG39723-105 (MS)

Matrix: TISSUE Sample Size: 0.970 g (wet)
Sample Receipt Date: 08-Mar-2012 Initial Calibration Date: 18-Apr-2012

Extraction Date: 17-Apr-2012 Instrument ID: LC MS/MS
Analysis Date: 19-Apr-2012 Time: 04:07:11 Column ID: C18MS
Extract Volume (uL): 4000 Sample Data Filename: FC2G_150 S: 28
Injection Volume (uL): 15 Blank Data Filename: FC2G_150 S: 23

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_150 S: 16

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

PFOA 110 1.0 (L) 7:06



## Page 1 of 1 (WG39723 - PFC_FC_LC_PFOA_WG39723-105_Form1A_FC2G_150S28_SJ1451388.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39723

- 105_Form2_FC2G_150S28_SJ1451388.html; Workgroup: WG39723; Design ID: 1817 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. WWO-X-OH-11 (HAY) (MS) Sample Collection: 17-Feb-2012 14:20 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. WWO PHASE III
Contract No.: 4380 Lab Sample I.D.: WG39723-105 (MS)

Matrix: TISSUE Sample Size: 0.970 g (wet)
Sample Receipt Date: 08-Mar-2012 Initial Calibration Date: 18-Apr-2012

Extraction Date: 17-Apr-2012 Instrument ID: LC MS/MS
Analysis Date: 19-Apr-2012 Time: 04:07:11 Column ID: C18MS
Extract Volume (uL): 4000 Sample Data Filename: FC2G_150 S: 28
Injection Volume (uL): 15 Blank Data Filename: FC2G_150 S: 23

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_150 S: 16

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

13C2-PFOA 72 52 72 7:06

CLEANUP STANDARD

13C8-PFOA 12 12 100 7:06



## Page 1 of 1 (WG39723 - PFC_FC_LC_PFOA_WG39723-105_Form2_FC2G_150S28_SJ1451388.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: ___________ 

## Jenny Pape

___________ 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 13:08:32; Application: XMLTransformer-1.12.13; Report Filename: MS_FC_LC_PFOA

- MS

- MSD_WG39723

- 105_L17643

- 1_Form8C.html; Workgroup: WG39723; Design ID: 1817 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. WWO-X-OH-11 (HAY) (MS) Sample Collection: 17-Feb-2012 14:20 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. WWO PHASE III Contract No.: 4380 Lab Sample I.D.: WG39723-105 (MS) Matrix: TISSUE Sample Size: 0.970 g (wet) Extraction Date: 17-Apr-2012 Initial Calibration Date: 18-Apr-2012 Analysis Date: 19-Apr-2012 Time: 04:07:11 Instrument ID: LC MS/MS Extract Volume (uL): 4000 Column ID: C18MS Injection Volume (uL): 15 MS Data Filename: FC2G_150 S: 28 Dilution Factor: N/A Blank Data Filename: FC2G_150 S: 23 Cal. Ver. Data Filename: FC2G_150 S: 16
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

PFOA N/A 41 71 110 91 N/A



## Page 1 of 1 (WG39723 - MS_FC_LC_PFOA-MS-MSD_WG39723-105_L17643 -1_Form8C.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form1A.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39723

- 106_Form1A_FC2G_150S29_SJ1451389.html; Workgroup: WG39723; Design ID: 1817 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. WWO-X-OH-11 (HAY) (MS) Sample Collection: 17-Feb-2012 14:20 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. WWO PHASE III
Contract No.: 4380 Lab Sample I.D.: WG39723-106 (MS)

Matrix: TISSUE Sample Size: 1.00 g (wet)
Sample Receipt Date: 08-Mar-2012 Initial Calibration Date: 18-Apr-2012

Extraction Date: 17-Apr-2012 Instrument ID: LC MS/MS
Analysis Date: 19-Apr-2012 Time: 04:23:57 Column ID: C18MS
Extract Volume (uL): 4000 Sample Data Filename: FC2G_150 S: 29
Injection Volume (uL): 15 Blank Data Filename: FC2G_150 S: 23

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_150 S: 16

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

PFOA 1000 1.0 (L) 7:06



## Page 1 of 1 (WG39723 - PFC_FC_LC_PFOA_WG39723-106_Form1A_FC2G_150S29_SJ1451389.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form2.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFC_FC_LC_PFOA_WG39723

- 106_Form2_FC2G_150S29_SJ1451389.html; Workgroup: WG39723; Design ID: 1817 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. WWO-X-OH-11 (HAY) (MS) Sample Collection: 17-Feb-2012 14:20 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. WWO PHASE III
Contract No.: 4380 Lab Sample I.D.: WG39723-106 (MS)

Matrix: TISSUE Sample Size: 1.00 g (wet)
Sample Receipt Date: 08-Mar-2012 Initial Calibration Date: 18-Apr-2012

Extraction Date: 17-Apr-2012 Instrument ID: LC MS/MS
Analysis Date: 19-Apr-2012 Time: 04:23:57 Column ID: C18MS
Extract Volume (uL): 4000 Sample Data Filename: FC2G_150 S: 29
Injection Volume (uL): 15 Blank Data Filename: FC2G_150 S: 23

Dilution Factor: N/A Cal. Ver. Data Filename: FC2G_150 S: 16

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

13C2-PFOA 72 52 73 7:06

CLEANUP STANDARD

13C8-PFOA 12 12 96 7:06



## Page 1 of 1 (WG39723 - PFC_FC_LC_PFOA_WG39723-106_Form2_FC2G_150S29_SJ1451389.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: ___________ 

## Jenny Pape

___________ 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 13:08:32; Application: XMLTransformer-1.12.13; Report Filename: MS_FC_LC_PFOA

- MS

- MSD_WG39723

- 106_L17643

- 1_Form8C.html; Workgroup: WG39723; Design ID: 1817 ] AXYS METHOD MLA-043 Rev 8 CLIENT SAMPLE NO. WWO-X-OH-11 (HAY) (MS) Sample Collection: 17-Feb-2012 14:20 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. WWO PHASE III Contract No.: 4380 Lab Sample I.D.: WG39723-106 (MS) Matrix: TISSUE Sample Size: 1.00 g (wet) Extraction Date: 17-Apr-2012 Initial Calibration Date: 18-Apr-2012 Analysis Date: 19-Apr-2012 Time: 04:23:57 Instrument ID: LC MS/MS Extract Volume (uL): 4000 Column ID: C18MS Injection Volume (uL): 15 MS Data Filename: FC2G_150 S: 29 Dilution Factor: N/A Blank Data Filename: FC2G_150 S: 23 Cal. Ver. Data Filename: FC2G_150 S: 16
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

PFOA N/A 1000 71 1000 97 N/A



## Page 1 of 1 (WG39723 - MS_FC_LC_PFOA-MS-MSD_WG39723-106_L17643 -1_Form8C.html)

## ________ 4:_- 

# 2:,_t5_0

__ f(-_8_A_-

. 

# 6/r.k(. 'i

# ts~\'<....e.-S . MassLynx 4.1 SCN627 Sample List Report Sample List: G:\Masslynx\lnst_ G'LMaster.PRO\SampleDB\FC2G_150.SPL Page 1 of 1 Last Modified: Wednesday, April 18, 2012 15:12:44 Pacific Daylight Time Printed: Wednesday, April 18, 2012 15:15:13 Pacific Daylight Time Page Position (1, 1)

File Name Sample 10 File Text Bottle Signln SignOut Inj VoL

1 FC2G 150S001 MeOH" 1,,15uL 1:8,A 

# wt 

# 'w 15.0 2 FC2G -150S002 MeOH" 1,,15uL 1:8,A 

## -- 15.0 3 FC2G-150S003 FC-L1N-39725T-A" 

### 1/2 1,,15uL 2:1,A 15.0 4 FC2G-150S004 FC-L1 N-39725T -A" 1 

### 12 1,,15uL 2:1,A 

# 15(

5 FC2G -150S005 FC-L1N-39725T-B" 

### 1/2 1" 15uL 2:1,8

. 15.0

_ 6 FC2G-150S006 FC-L1N-39725T-C" 1 

### 12 1,,15uL 2:1,C 15.0 7 FC2G:::: 150S007 FC-L1N-39725T-D" 

### 1/2 1,,15uL 2:1,0 15.0 8 F C2G _150S008 FC-L1N-39725T-E" 

### 1/2 1,,15uL 2:1,E 

### 15.0 

# !**~** .J'C1J 9 FC2G_150S009 FC-L1N-39725T-F" 

### 1/2 1,,15uL 2:1,F 15.0 10 FC2G 150S010 FC-L1N-39725T-G" 

### 1/2 1,,15uL 2:2,A 15.0 11 FC2G-150S011 FC-LlN-39725T-H" 

### 1/2 1,,15uL 2:2,8 

### 15.a. 12 FC2G-150S012 MeOH" 1,,15uL 1:8,A 15.0 13 FC2G::::150S013 MeOH" 1,,15uL 1:8,A 15.0 14 FC2G 150S014 FC-39725T-SAR2" 1,,15uL 2:2,C 15.0 15 FC2G-150S015 F C-39725T -SAR" 1" 15uL 2:2,0 

# T 15.0 16 FC2G-150S016 FC-L1N-39725T-0" 

### 1/2 1" 15uL 2:1,0 15.0 17 FC2G-150S017 FC-L1N-39725T-& 

### 1/2 1,,15uL 2:1,0



# - 

# - 15.0 18 FC2G-150S018

### WG39723-1-Ga~~ R

### ~~G39723, 15/4000uL 2:2,E 

# T 15.0 19 FC2G-150S019 WG39723-102"SPM ,G39723, 

### 15/4000uL 2:2,F 15.0 20 FC2G-150S020 WG39723-102,i,SPM 1 ,WG39723, 

### 15/4000uL 2:2,F 15.0 21 FC2G::::150S021 MeOH" 1,,15uL 1:8,A 15.0 22 FC2G 150S022 MeOH" 1" 15uL 1:8,A 15.0 

## U) 23 FC2G-150S023 WG39723-1 01 "BLK 1 ,WG39723, 15/4000uL 2:3,A 15.0**'\(:}-~\** 

### .- \ '<;<!..- i) 24 FC2G-150S024 WG39723-1 01 ,i,BLK 1 ,WG39723, 

### 15/4000uL 2:3,A 15.0 25 FC2G-150S025 L 17643-1" 1 , WG39723, 

### 15/4000uL 2:3,8 15.0 26 F C2G -150S026 WG39723-103"OUP 1 ,WG39723, 

### 15/4000uL 2:3,C 15.0 27 FC2G -1508027 WG39723-104"M8 1 ,WG39723, 

### 15/4000uL 2:3,0 15.0 28 FC2G -1508028 WG39723-105"MS 1 ,WG39723, 

### 15/4000uL 2:3,E 15.0 29 FC2G-1508029 WG39723-106"M8 1 ,WG39723, 

### 15/4000uL 2:3,F 15.0 30 FC2G-1508030 MeOH" 1;,15uL 1:8,A 15.0 31 FC2G-1508031 FC-L1N-39725T-D" 

### 1/2 1" 15uL 2:1,0 15.0" 32 FC2G-1508032 FC-L1N-39725T-D" 

### 1/2 1" 15uL 2:1,0 15.0 33 FC2G -150S033 MeOH" 1,,15uL 1:8,A 15.0 34 FC2G:::: 1508034 MeOH" 1,,15uL 1:8,A 15.0(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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form3A.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_18

- Apr

- 2012_FC2G__Form3A_GS45435.html; Workgroup: WG39723; Design ID: 1817 ] 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_150 S: 4
Initial Calibration Date: 18-Apr-2012 CS1 Data Filename: FC2G_150 S: 5

Instrument ID: LC MS/MS CS2 Data Filename: FC2G_150 S: 6

LC Column ID: C18MS CS3 Data Filename: FC2G_150 S: 7

CS4 Data Filename: FC2G_150 S: 8

CS5 Data Filename: FC2G_150 S: 9

CS6 Data Filename: FC2G_150 S: 10

CS7 Data Filename: FC2G_150 S: 11

CS8 Data Filename: N/A

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

PFOA 92.1 119 100 108 97.4 104 94.3 84.0



## Page 1 of 1 (WG39723 - PFOA_FC_LC_18-Apr-2012_FC2G__Form3A_GS45435.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form3B.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_18

- Apr

- 2012_FC2G__Form3B_GS45435.html; Workgroup: WG39723; Design ID: 1817 ] 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_150 S: 4
Initial Calibration Date: 18-Apr-2012 CS1 Data Filename: FC2G_150 S: 5

Instrument ID: LC MS/MS CS2 Data Filename: FC2G_150 S: 6

LC Column ID: C18MS CS3 Data Filename: FC2G_150 S: 7

CS4 Data Filename: FC2G_150 S: 8

CS5 Data Filename: FC2G_150 S: 9

CS6 Data Filename: FC2G_150 S: 10

CS7 Data Filename: FC2G_150 S: 11

CS8 Data Filename: N/A

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

13C2-PFOA 96.3 98.1 98.7 96.5 101 103 98.8 108

CLEAN-UP STANDARD

13C8-PFOA 102 97.3 102 96.7 100 99.4 105 97.4



## Page 1 of 1 (WG39723 - PFOA_FC_LC_18-Apr-2012_FC2G__Form3B_GS45435.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form3C.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_18

- Apr

- 2012_FC2G__Form3C_GS45435.html; Workgroup: WG39723; Design ID: 1817 ] 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_150 S: 4
Initial Calibration Date: 18-Apr-2012 CS1 Data Filename: FC2G_150 S: 5

Instrument ID: LC MS/MS CS2 Data Filename: FC2G_150 S: 6

LC Column ID: C18MS CS3 Data Filename: FC2G_150 S: 7

CS4 Data Filename: FC2G_150 S: 8

CS5 Data Filename: FC2G_150 S: 9

CS6 Data Filename: FC2G_150 S: 10

CS7 Data Filename: FC2G_150 S: 11

CS8 Data Filename: N/A

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

PFOA 7:09 7:09 7:06 7:09 7:06 7:06 7:06 7:06 7:07



## Page 1 of 1 (WG39723 - PFOA_FC_LC_18-Apr-2012_FC2G__Form3C_GS45435.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form3D.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_18

- Apr

- 2012_FC2G__Form3D_GS45435.html; Workgroup: WG39723; Design ID: 1817 ] 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_150 S: 4
Initial Calibration Date: 18-Apr-2012 CS1 Data Filename: FC2G_150 S: 5

Instrument ID: LC MS/MS CS2 Data Filename: FC2G_150 S: 6

LC Column ID: C18MS CS3 Data Filename: FC2G_150 S: 7

CS4 Data Filename: FC2G_150 S: 8

CS5 Data Filename: FC2G_150 S: 9

CS6 Data Filename: FC2G_150 S: 10

CS7 Data Filename: FC2G_150 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

13C2-PFOA 7:09 7:09 7:06 7:06 7:06 7:06 7:06 7:06 7:07

CLEAN-UP STANDARD

13C8-PFOA 7:06 7:09 7:06 7:06 7:06 7:06 7:06 7:06 7:06



## Page 1 of 1 (WG39723 - PFOA_FC_LC_18-Apr-2012_FC2G__Form3D_GS45435.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form4A.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_FC2G_150S16__Form4A_SJ1451309.html; Workgroup: WG39723; Design ID: 1817 ] 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: 18-Apr-2012 VER Data Filename: FC2G_150 S: 16

Instrument ID: LC MS/MS Analysis Date: 19-Apr-2012

LC Column ID: C18MS Analysis Time: 00:46:01

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

PFOA 7:06 40.0 42.8 107



## Page 1 of 1 (WG39723 - PFOA_FC_LC_FC2G_150S16__Form4A_SJ1451309.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form4B.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_FC2G_150S16__Form4B_SJ1451309.html; Workgroup: WG39723; Design ID: 1817 ] 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: 18-Apr-2012 VER Data Filename: FC2G_150 S: 16

Instrument ID: LC MS/MS Analysis Date: 19-Apr-2012

LC Column ID: C18MS Analysis Time: 00:46:01

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

13C2-PFOA 7:06 72.0 66.5 92.4

CLEANUP STANDARD

13C8-PFOA 7:06 12.0 11.9 98.8



## Page 1 of 1 (WG39723 - PFOA_FC_LC_FC2G_150S16__Form4B_SJ1451309.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form4A.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_FC2G_150S31__Form4A_SJ1451328.html; Workgroup: WG39723; Design ID: 1817 ] 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: 18-Apr-2012 VER Data Filename: FC2G_150 S: 31

Instrument ID: LC MS/MS Analysis Date: 19-Apr-2012

LC Column ID: C18MS Analysis Time: 04:57:29

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

PFOA 7:06 40.0 42.8 107



## Page 1 of 1 (WG39723 - PFOA_FC_LC_FC2G_150S31__Form4A_SJ1451328.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: ___________ 

## Jenny Pape

___________
For Axys Internal Use Only [ XSL Template: FC-Form4B.xsl; Created: 27-Apr-2012 13:08:22; Application: XMLTransformer-1.12.13; Report Filename: PFOA_FC_LC_FC2G_150S31__Form4B_SJ1451328.html; Workgroup: WG39723; Design ID: 1817 ] 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: 18-Apr-2012 VER Data Filename: FC2G_150 S: 31

Instrument ID: LC MS/MS Analysis Date: 19-Apr-2012

LC Column ID: C18MS Analysis Time: 04:57:29

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

13C2-PFOA 7:06 72.0 71.2 98.9

CLEANUP STANDARD

13C8-PFOA 7:06 12.0 12.7 106



## Page 1 of 1 (WG39723 - PFOA_FC_LC_FC2G_150S31__Form4B_SJ1451328.html)Quantify Sample Report MassLynx 4.1 SCN627

Dataset: G:\Masslynx\lnst_ G\PFC.PRO\FC\FC2G _150-b.qld

Last Altered: Friday, April 27, 2012 11 :33:53 Pacific Daylight Time Printed: Friday, April 27, 201213:05:43 Pacific Daylight Time**-----------~~------------------------------------------------**

ID: L 17643·1" Name: FC2G_150S025 Description: 1 ,WG39723, 15/4000uL Date: 19-Apr·2012 Time: 03:16:54

PFOA·1 FC2G _1508025

I 7.11

7.13e4 .' 276730

min 7.00 8.00

1# 

### NSI\l& 1:71:: ..•.• 5 PFOA-1 6 PFOA-2 19 13C2-PFOA 20 13C8-PFOA 21 13C4-PFOA PFOA·2 FC2G _1508025 10

7.00 7.11 1.45e4 55133

" 8.00**·'.:'.I.~.,\.,,~~::** ,".' 19 412.97> 368.98 19 412.97> 168.80 21 414.97> 369

.... 21 420.97> 375

.... 416.97> 371.9 min 

# Rr

.. >: 7.11 7.11 7.11 7.11 7.11 13C2·PFOA FC2G_1508025 100

%

0 7.00

..**~~,:I·;<**

71271 14476 76943 45963 47055 7.11 7.69e4 308258

8.00**:':I~~~I;1·** 76943 76943 47055 47055 min



### :ljIg'<:: 71.234 62.738 42.203 11.456 9.832

PV by HH, SV by JP 27-Apr-12, NOTE: CALlVERlSPM Conen & LOD units 

### = ng abs. 13C8·PFOA FC2G _1508025

7.00 1i:;;LOD

0.6616 7.11 "4.60e4 182882

I 8.00**~,,~.**

56.9 92.6 79.5 min

:SlN;:: 0 0 194 0 0 13C4·PFOA FC2G 1508025 100

- 7.11 4.71e4 186060
%

0 min 7.00 8.00


### '·':NoiSe". 

### 'f;elQht ' "**I.S~I!jht** 0 276730 308258 0 55133 308258 1590 308258 186060 0 182882 186060 0 186060**,;~~~es~: Fsc:;I\1r,l/c:O~~ctiOn;;;**  0.9700 1.0 

### MM 0.9700 1.0 bb 0.9700 1.0 bb 0.9700 1.0 

### MM 0.9700 1.0 

### MMQuantify Sample Report MassLynx 4.1 SCN627

Dataset: G:\Masslynx\lnst_ G\PFC.PRo\FC\FC2G _150-b.qld
Last Altered: Friday, April 27, 2012 11:33:53 Pacific Daylight Time Printed: Friday, April 27, 2012 13:05:43 Pacific Daylight Time

10: WG39723·103"DUP Name: FC2G_150S026 Description: 1 ,WG39723,15/4000uL Date: 19·Apr-2012 Time: 03:33:47
PFOA·1 PFOA-2 FC2G _150S026 13C2·PFOA FC2G_150S026 100 7.11 1.57e4 61141 10 7.11 8.98e4 365752
%



### o 7.00 8.00 7.00 8.00

5 PFOA-1 19 412.97> 368.98 7.11 72452 89792 6 PFOA-2 19 412.97> 168.80 7.11 15695 89792 19 13C2-PFOA 21 414.97>369

.... 7.11 89792 45129 20 13C8-PFOA 21 420.97 > 375

.... 7.11 49612 45129 21 13C4-PFOA 416.97> 371.9 7.11 45129 60.787 57.044 50.315 12.633 9.239

PV by HH, SV by JP 27-Apr-12, NOTE: CALlVERlSPM Concn 

### & LOD units 

### = ng abs. 13C8-PFOA FC2G _150S026 100

%



### o

1.1148

0.1527 0.0399 7.11 4.96e4 201798

8.00**%~eC··**

69.2 104.2 76.2 min

.$11'4.></ 142 0 0 250 695 13C4·PFOA FC2G 1508026

- 7.11

. Npl$e
, 1939 0 0 808 262 4.51e4 182283**·~I!:!m** 275184 61141 365752 201798 182283 min**I$~!mt** ,\SS",fl!iJ siZe**;F$cI9~Qet~1<!~,,:** 365752 0.9900 1.0 

### MM 365752 0.9900 1.0 bb 182283 0.9900 1.0 bb 182283 0.9900 1.0 

### MM 0.9900 1.0 

### MMQuantify Sample Report MassLynx 4.1 SCN627

Dataset: G:\Masslynx\lnst_G\PFC.PRO\FC\FC2G_150-b.qld

Last Altered: Friday, April 27, 2012 11:33:53 Pacific Daylight Time Printed: Friday, April 27, 2012 13:05:43 Pacific Daylight Time



### 10: WG39723-101"BLK Name: FC2G_150S023 Description: 1, WG39723, 15/4000uL Date: 19-Apr-2012 Time: 02:43:22

PFOA-1 FC2G _1508023 100 

# 1/\

7.78

# :~m'o 7.00 8.00



### #. 5 6 PFOA-2 19 13C2-PFOA 20 13C8-PFOA 21 13C4-PFOA PFOA-2 FC2G _1508023

# 100L16'~'11 '\j 

# \,c '.20 

# : ., ':( m'o

7.00 8.00

19 412.97> 368.98 19 412.97> 168.80 13C2-PFOA FC2G _1508023 100

%



### o 7.11 1.96e5 789308

196286 196286 21 414.97> 369

.... 7.11 196286 61332 80.123 21 420.97>375

.... 7.11 64527 61332 11.969 416.97> 371.9 7.11 61332 12.431

PV by HH, SV by JP 27-Apr-12, NOTE: CALlVERlSPM Concn & LOD units 

### = ng abs. 13C8-PFOA FC2G _1508023 13C4-PFOA FC2G_1508023 100 7.11 6.45e4 257648
%

7.00 8.00**;;%~ecY;S/""<2;;;** 

### 'N{j/$\i;> 327 104 111.3 0 99.7 

## a 103.6 0 

### o o a 7.11 6.13e4 243292**;fi~ijli~rf**

789308 257648 243292 ISHlilightr**~{!r\~;siZe:** 

## .**f'llI~Oelf!clion,;.** 789308 1.0000 1.0 MM-I 789308 1.0000 1.0 243292 1.0000 1.0 MM 243292 1.0000 1.0 MM 1.0000 1.0 MMQuantify Sample Report MassLynx 4.1 SCN627

Dataset:

Last Altered: Printed: G:\Masslynx\lnst_ G\PFC.PRO\FC\FC2G _150-b.qld Friday, April 27, 201211:33:53 Pacific DaylightTime Friday, April 27, 2012 13:05:43 Pacific Daylight Time

ID: WG39723-102"SPM Name: FC2G_150S019 Description: 1,WG39723,15/4000uL Date: 19-Apr-2012 Time: 01:36:19

PFOA-1 PFOA-2 FC2G_1508019 FC2G_1508019 100

% 7.11 8.47e4 340427 100

% 7.11 2.03e4 80525 13C2-PFOA FC2G_150S019 100

% 7.11 1.48e5 605508



## o -4TPI"T'Frr'-' min 

## o o 'i9'i'"Fl-1,..,.-n min 7.00 8.00 7.00 8.00
.-IS 

### Altifa.-**~:rJtJ/;~** 

## • 5 19 412.97> 368.98 7.11 84691 148381 42.544 6 PFOA-2 19 412.97> 168.80 7.11 20261 148381 43.918 19 13C2-PFOA 21 414.97> 369

.... 7.11 148381 52535 70.711 20 13C8-PFOA 21 420.97> 375

.... 7.11 55059 52535 11.923 21 13C4-PFOA 416.97> 371.9 7.11 52535 10.648

PV by HH, SV by JP 27-Apr-12, NOTE: CAUVERlSPM Concn & LOD units 

### = ng abs. 13C8-PFOA FC2G _1508019 100

%



## o

0.1477 7.11 5.51e4 227324

106.4 109.8 98.2 99.4 88.7 543 383 0 0 0 13C4-PFOA FC2G_150S019 100

%



## o 7.00 7.11 5.25e4 207780

8.00 

### NQiSli**':IEiigh~ ··..\I~H,~i!ltit;~~p'e**  siZEI;**,.,ac!Qt2Del~tlO!i:;;** 626 340427 605508 1.0000 1.0 MM 210 

### o o o 80525 605508 1.0000 605508 207780 1.0000 227324 207780 1.0000

. 207780 1.0000 1.0 bb 1.0 MM 1.0 MM 1.0 MMQuantify Sample Report MassLynx 4.1 SCN627

Dataset: G:\Masslynx\lnst_ G\PFC.PRO\FC\FC2G _150-b.qld

Last Altered: Friday, April 27, 2012 11 :33:53 Pacific Daylight Time Printed: Friday, April 27, 2012 13:05:43 Pacific Daylight Time

ID: WG39723-104"MS Name: FC2G_150S027 Description: 1,WG39723,15/4000uL Date: 19-Apr-2012 Time: 03:50:25

PFOA-1 FC2G_150S027 7.11 7.70e4 297089

7.00

5 PFOA-1 6 PFOA-2 19 13C2-PFOA 20 13C8-PFOA 21 13C4-PFOA 8.00 PFOA-2 FC2G_150S027 13C2-PFOA FC2G _150S027 7.11 1.58e4 62539

19 412.97> 368.98 7.11 100

%



### o 7.00

1·9 412.97> 168.80 7.11 15791 21 414.97> 369

.... 7.11 93560 21 420.97> 375

.... 7.11 46797 416.97> 371.9 7.11 42847 7.11 9.36e4 379945

8.00

93560 63.299 93560 56.186 42847 56.357 42847 12.809 8.953

PV by HH, SV by JP 27-Apr-12, NOTE: CAUVERlSPM Concn & LaD units 

### = ng abs. 13C8-PFOA FC2G.:.150S027 7.11 4.68e4 189718

2456.0 0 2180.0 194 75.9 0 103.5 0 72.4 0**-----------~.~~**

13C4-PFOA

7.00 8.00



## o 297089 379945 322 

### o o 

## o 62539 379945 379945 169876 189718 169876 169876 S!l!l)lllllslZe.**Fa¢!~ip.I!I~~~i;** 0.9700 1.0 bb 0.9700 1.0 bb 0.9700 1.0 

### MM 0.9700 1.0 

### MM 0.9700 1.0 

### MMQuantify Sample Report MassLynx 4.1 SCN627

Dataset: G:\Masslynx\lnst_ G\PFC.PRO\FC\FC2G_150-b.qld

Last Altered: Friday, April 27, 2012 11 :33:53 Pacific Daylight Time Printed: Friday, April 27, 201213:05:43 Pacific Daylight Time

ID: WG39723-105"MS Name: FC2G_150S028 Description: 1 ,WG39723, 15/4000uL Date: 19-Apr-2012 Time: 04:07:11

PFOA-1

min



### 1#' "

.. N!!nte 5 PFOA-l 6 PFOA-2 19 13C2-PFOA 20 13C8-PFOA 21 13C4-PFOA PFOA-2 FC2G _150S028



### ....... 100

%



### a 7.11 2.71e4 109534

7.00 8.00
'1St/!**T~CI!.**

19 412.97> 368.98 19 412.97> 168.80 21 414.97> 369

.... 21 420.97 > 375

.... 416.97> 371.9 min

,Rr-;
7.11 7.11 7.11 7.11 7.11 13C2-PFOA FC2G _150S028



### At

.. a::;· " 123944 27053 87601 44188 42097 7.11 8.76e4 352574



### I\SMa'

. 87601 87601 42097 42097 min

nglg" 108.852 103.580 53.709 12.311 8.796 13C8-PFOA FC2G _150S028 100

%



### a 7.00

"

..**;J,,~p**

0.1353

0.0869 7.11 4.42e4 173025

" 'I

8.00
·.%Rec

264.0 251.2 72.4 99.5 71.1

PV by HH, SV by JP 27-Apr-12, NOTE: CALlVERlSPM Concn & LOD units 

# = ng abs. 13C4-PFOA

min 0 min 7.00 8.00**~/II!~** .. Noiss:";·::**H!ilig~t' \~ti~ighl**  Slimplesize fiat:!9i'2· PetectiOn

... 0 0 477539 352574 0.9700 1.0 

### MM 0 0 109534 352574 0.9700 1.0 bb 1219 289 352574 165594 0.9700 1.0 bb 0 0 173025 165594 0.9700 1.0 

### MM 303 546 165594 0.9700 1.0 

### MMQuantify Sample Report MassLynx 4;1 SCN627

Dataset: G:\Masslynx\lnst_ G\PFC.PRO\FC\FC2G_150-b.qld
Last Altered: Friday, April 27, 2012 11 :33:53 Pacific Daylight Time Printed: Friday, April 27, 2012 13:05:43 Pacific Daylight Time**----------.~~-----------------------------------------------------**

10: WG39723-106"MS Name: FC2G_150S029 Description: 1,WG39723,15/4000ul Date: 19·Apr·2012 Time: 04:23:57
PFOA·1 FC2G_150S029 100 7.11 9.86e5 3903333

7.00

5 PFOA-l 6 PFOA-2 19 13C2-PFOA 20 13C8-PFOA 21 13C4-PFOA 8.00 PFOA·2 FC2G _150S029 100 7.11 2.55e5 1049001

" 7.00 8.00 

### [S'"**'ria~ii** 19 412.97> 368.98 19 412.97> 168.80 21 414.97> 369

.... 21 420.97 > 375

.... 416.97> 371.9 min

7.11 7.11 7.11 7.11 7.11 13C2·PFOA FC2G _150S029

986435 255397 71088 34512 33981 7.11 7.11e4 288374



### ISl,Velf 71088 71088 33981 33981 min 13C8·PFOA FC2G_150S029 100

%

0 7.00 7.11 3.45e4 136866

8.00 

### "f19'Q{ · •.. ,LOO.

1036.274 1178.492 117.8 52.374 72.7 11.554 96.3 6.887 0.1033 57.4

PV by HH, SV by JP 27-Apr-12, NOTE: CALNERlSPM Concn & LOD units 

### = ng abs. min

0 0 0 0 200 13C4·PFOA FC2G 1508029 100 - 7.11 3.40e4 136817
%

0 7.00 8.00



### .•**l:lE!Igh,~**

3903333 0 1049001 0 288374 0 136866 684 136817 min



### IS,:!aiQh,!' Sal:llPle!llzB 288374 1.0000 288374 1.0000 136817 1.0000 136817 1.0000 1.0000 "f'aCfor20electiGn,;, 1.0 

### MM 1.0 bb 1.0 bb 1.0 

### MM 1.0 

### MMSample List Report 

# 4-;; g 0 

# ff-e1r**6:~** -1'

# (S~\,~S:**~_~~** _____

# ~_" __

# ~" MassLynx 4.1 SCN627 

### Sample List: G:\Masslynx\lnst_ G\_Master.PRO\SampleOB\FC2G_150.SPL Page 1 of 1 Last Modified: Wednesday, April 18, 2012 15:12:44 Pacific Daylight Time Printed: Wednesday, April 18, 2012 15:15:13 PacificOaylightTime Page Position (1, 1)

File Name Sample ID File Text Bottle Signln SignOut Inj VoL



### 1 FC2G 150S001 MeOH" 1,,15uL 1:8,A 

## ltft 

# 'w' 15.0 2 FC2G:::150S002 MeOH" 1 ,,15uL 1:8,A 15.0 3 FC2G 150S003 FC-LlN-39725T-A" 

### 1/2 1" 15uL 2:1,A 15.0 4 FC2G -150S004 FC-LlN-39725T-A" 

### 1/2 1" 15uL 2:1,A 15.0 5 FC2G:::150S005 FC-LlN-39725T-B" 

### 1/2 1" 15uL 2:1,8· 15.0 6 FC2G 150S006 FC-LlN-39725T-C" 

### 1/2 1,,15uL 2:1,C 15.0 7 FC2G-150S007 FC-LlN-39725T-D" 

### 1/2 1 ,,15uL 2:1,0 15.0 

## ';2(!;)t, .J 

## '<iJ 8 FC2G:::150S008 FC-LlN-39725T-E" 

### 1/2 1" 15uL 2:1,E 15.0 9 FC2G 150S009 FC-LlN-39725T-F" 

### 1/2 1 ,,15uL 2:1,F 15.0 10 FC2G:::150S010 FC-LlN-39725T-G" 

### 1/2 1" 15uL 2:2,A 15.0 11 FC2G 150S011 FC-LlN-39725T-H" 

### 1/2 1" 15uL 2:2,8 15.0· 12 FC2G:::150S012 MeOH" 1,,15uL 1:8,A 15.0 13 FC2G 150S013 MeOH" 1" 15uL 1:8,A 15.0 14 FC2G-150S014 FC-39725T-SAR2" 1" 15uL 2:2,C**15.0~** 

### 15 FC2G-150S015 FC-39725T-SAR" 1" 15uL 2:2,0 15.0 16 FC2G-150S016 FC-LlN-39725T-D" 

### 1/2 1,,15uL 2:1,0 15.0 17 FC2G -150S017**FC-LlN-39725T-~** 

### 1/2 1 ,,15uL 2:1,D 15.0 18 FC2G-150S018 WG39723-1.Q3::S R

### ~~G39723,15/4000UL 2:2,E 15.0 19 FC2G:::150S019 WG39723-102"SPM ,G39723, 15/4000uL 2:2,F 15.0 20 FC2G 150S020 WG39723-102,i,SPM 1,WG39723,15/4000uL 2:2,F 15.0 21 FC2G-150S021 MeOH" 1" 15uL 1 :8,A 15.0 22 F C2G::: 150S022 MeOH" 1" 15uL 1 :8,A 15.0

# r;t}~, ... " \ I:;<?"

# V~ 23 FC2G_150S023 WG39723-101 "BLK 1,WG39723,15/4000uL 2:3,A 15.0 24 FC2G_150S024 WG39723-101,i,BLK 1 ,WG39723,15/4000uL 2:3,A 15.0 25 FC2G 150S025 L 17643-1" 1,WG39723,15/4000uL 2:3,8 15.0 26 F C2G -150S026 WG39723-103"DUP 1,WG39723,15/4000uL 2:3,C 15.0 27 F C2G -150S027 WG39723-104"MS 1,wG39723,15/4000uL 2:3,0 15.0 28 FC2G:::150S028 WG39723-105"MS 1,wG39723,15/4000uL 2:3,E 15.0 29 FC2G 150S029 WG39723-106"MS 

### 1,wG39723,15/4000uL 2:3,F 15.0 30 FC2G-150S030 MeOH" 1;,15uL 1:8,A 15.0 31 FC2G-150S031 FC-LlN-39725T-D" 

### 1/2 1" 15uL 2:1,0 

### 15.0J 32 FC2G:::150S032 FC-LlN-39725T-D" 

### 1/2 1,,15uL 2:1,D 15.0 33 FC2G 150S033 MeOH" 1,,15uL 1 :8,A 15.0 34 FC2G:::150S034 MeOH" 1,,15uL 1:8,A



# -- 15.0Quantify Compound Summary ReportMassLynx 4.1 SCN627Dataset:G:\Masslynx\Inst_G\PFC.PRO\FC\FC2G_150-A1.qldLast Altered:Thursday, April 19, 2012 11:51:33 Pacific Daylight TimePrinted:Thursday, April 19, 2012 12:55:08 Pacific Daylight TimeMethod: G:\Masslynx\Master Methods\PFC\FC_043_08_02.mdb 08 Nov 2011 13:21:58Calibration: G:\Masslynx\Inst_G\PFC.PRO\CurveDB\FC2G_150-A1.cdb 19 Apr 2012 11:51:33Compound name: PFOA-1#12345678IDFC-LIN-39725T-A,,1/2FC-LIN-39725T-B,,1/2FC-LIN-39725T-C,,1/2FC-LIN-39725T-D,,1/2FC-LIN-39725T-E,,1/2FC-LIN-39725T-F,,1/2FC-LIN-39725T-G,,1/2FC-LIN-39725T-H,,1/2NameFC2G_150S004FC2G_150S005FC2G_150S006FC2G_150S007FC2G_150S008FC2G_150S009FC2G_150S010FC2G_150S011TypeStandardStandardStandardStandardStandardStandardStandardStandardRT7.157.157.117.157.117.117.117.11Area236881062755910118347612595803217311153196280IS Area175916197721203449173989182498171454137030113640Std. Conc1.0002.50010.00040.000200.000400.0001000.0002500.000ng/g0.9212.97810.03343.349194.766417.235943.4252100.550%Rec92.1119.1100.3108.497.4104.394.384.0S/N5825066700000Acq.Date18-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-12Acq.Time21:24:4621:41:3121:58:1622:15:0222:31:4822:48:3423:05:2023:22:06Detection...MMMMMMMMMMMMMMMMCompound name: PFOA-1Correlation coefficient: r = 0.993303, r^2 = 0.986650Calibration curve: 0.96404 * x + 0.0810483Response type: Internal Std ( Ref 19 ), Area * ( IS Conc. / IS Area )Curve type: Linear, Origin: Exclude, Weighting: 1/x^2, Axis trans: NoneConc0 500 1000 1500 2000 2500

Response0500100015002000PV by HH, Checked by JP 19-Apr-12, NOTE: CAL/VER Concn & LOD units = ng abs.Quantify Compound Summary ReportMassLynx 4.1 SCN627Dataset:G:\Masslynx\Inst_G\PFC.PRO\FC\FC2G_150-A1.qldLast Altered:Thursday, April 19, 2012 11:51:33 Pacific Daylight TimePrinted:Thursday, April 19, 2012 12:55:08 Pacific Daylight TimeCompound name: PFOA-2#12345678IDFC-LIN-39725T-A,,1/2FC-LIN-39725T-B,,1/2FC-LIN-39725T-C,,1/2FC-LIN-39725T-D,,1/2FC-LIN-39725T-E,,1/2FC-LIN-39725T-F,,1/2FC-LIN-39725T-G,,1/2FC-LIN-39725T-H,,1/2NameFC2G_150S004FC2G_150S005FC2G_150S006FC2G_150S007FC2G_150S008FC2G_150S009FC2G_150S010FC2G_150S011TypeStandardStandardStandardStandardStandardStandardStandardStandardRT7.157.157.117.157.117.117.117.11Area10731690659224314114395229684420193796965IS Area175916197721203449173989182498171454137030113640Std. Conc1.0002.50010.00040.000200.000400.0001000.0002500.000ng/g1.0951.8999.73044.968204.867438.8601005.7302301.323%Rec109.576.097.3112.4102.4109.7100.692.1S/N1417534990000Acq.Date18-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-12Acq.Time21:24:4621:41:3121:58:1622:15:0222:31:4822:48:3423:05:2023:22:06Detection...bbbbbbbbbbbbbbbbCompound name: PFOA-2Correlation coefficient: r = 0.991804, r^2 = 0.983675Calibration curve: 0.219327 * x + 0.198982Response type: Internal Std ( Ref 19 ), Area * ( IS Conc. / IS Area )Curve type: Linear, Origin: Exclude, Weighting: 1/x^2, Axis trans: NoneConc0 500 1000 1500 2000 2500

Response0200400PV by HH, Checked by JP 19-Apr-12, NOTE: CAL/VER Concn & LOD units = ng abs.Quantify Compound Summary ReportMassLynx 4.1 SCN627Dataset:G:\Masslynx\Inst_G\PFC.PRO\FC\FC2G_150-A1.qldLast Altered:Thursday, April 19, 2012 11:51:33 Pacific Daylight TimePrinted:Thursday, April 19, 2012 12:55:08 Pacific Daylight TimeCompound name: 13C2-PFOA#12345678IDFC-LIN-39725T-A,,1/2FC-LIN-39725T-B,,1/2FC-LIN-39725T-C,,1/2FC-LIN-39725T-D,,1/2FC-LIN-39725T-E,,1/2FC-LIN-39725T-F,,1/2FC-LIN-39725T-G,,1/2FC-LIN-39725T-H,,1/2NameFC2G_150S004FC2G_150S005FC2G_150S006FC2G_150S007FC2G_150S008FC2G_150S009FC2G_150S010FC2G_150S011TypeStandardStandardStandardStandardStandardStandardStandardStandardRT7.157.157.117.117.117.117.117.11Area175916197721203449173989182498171454137030113640IS Area6352170067717026268762790579584824636680Std. Conc72.00072.00072.00072.00072.00072.00072.00072.000ng/g69.33470.64871.03669.48672.76574.06171.10877.563%Rec96.398.198.796.5101.1102.998.8107.7S/N00000000Acq.Date18-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-12Acq.Time21:24:4621:41:3121:58:1622:15:0222:31:4822:48:3423:05:2023:22:06Detection...MMMMMMMMMMMMMMMMCompound name: 13C2-PFOAResponse Factor: 0.479319RRF SD: 0.0182766, % Relative SD: 3.81302Response type: Internal Std ( Ref 21 ), Area * ( IS Conc. / IS Area )Curve type: RFConc0.0 10.0 20.0 30.0 40.0 50.0 60.0 70.0

Response0.010.020.030.0PV by HH, Checked by JP 19-Apr-12, NOTE: CAL/VER Concn & LOD units = ng abs.Quantify Compound Summary ReportMassLynx 4.1 SCN627Dataset:G:\Masslynx\Inst_G\PFC.PRO\FC\FC2G_150-A1.qldLast Altered:Thursday, April 19, 2012 11:51:33 Pacific Daylight TimePrinted:Thursday, April 19, 2012 12:55:08 Pacific Daylight TimeCompound name: 13C8-PFOA#12345678IDFC-LIN-39725T-A,,1/2FC-LIN-39725T-B,,1/2FC-LIN-39725T-C,,1/2FC-LIN-39725T-D,,1/2FC-LIN-39725T-E,,1/2FC-LIN-39725T-F,,1/2FC-LIN-39725T-G,,1/2FC-LIN-39725T-H,,1/2NameFC2G_150S004FC2G_150S005FC2G_150S006FC2G_150S007FC2G_150S008FC2G_150S009FC2G_150S010FC2G_150S011TypeStandardStandardStandardStandardStandardStandardStandardStandardRT7.117.157.117.117.117.117.117.11Area6829171880774726395266374607485329137672IS Area6352170067717026268762790579584824636680Std. Conc12.00012.00012.00012.00012.00012.00012.00012.000ng/g12.23111.67112.29211.60612.02611.92412.56611.684%Rec101.997.3102.496.7100.299.4104.797.4S/N02473924187206127620Acq.Date18-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-12Acq.Time21:24:4621:41:3121:58:1622:15:0222:31:4822:48:3423:05:2023:22:06Detection...MMMMMMMMMMMMMMMMCompound name: 13C8-PFOAResponse Factor: 1.05481RRF SD: 0.0302495, % Relative SD: 2.86777Response type: Internal Std ( Ref 21 ), Area * ( IS Conc. / IS Area )Curve type: RFConc0.0 2.0 4.0 6.0 8.0 10.0 12.0

Response0.05.010.0PV by HH, Checked by JP 19-Apr-12, NOTE: CAL/VER Concn & LOD units = ng abs.Quantify Compound Summary ReportMassLynx 4.1 SCN627Dataset:G:\Masslynx\Inst_G\PFC.PRO\FC\FC2G_150-A1.qldLast Altered:Thursday, April 19, 2012 11:51:33 Pacific Daylight TimePrinted:Thursday, April 19, 2012 12:55:08 Pacific Daylight TimeCompound name: 13C4-PFOA#12345678IDFC-LIN-39725T-A,,1/2FC-LIN-39725T-B,,1/2FC-LIN-39725T-C,,1/2FC-LIN-39725T-D,,1/2FC-LIN-39725T-E,,1/2FC-LIN-39725T-F,,1/2FC-LIN-39725T-G,,1/2FC-LIN-39725T-H,,1/2NameFC2G_150S004FC2G_150S005FC2G_150S006FC2G_150S007FC2G_150S008FC2G_150S009FC2G_150S010FC2G_150S011TypeStandardStandardStandardStandardStandardStandardStandardStandardRT7.117.157.117.117.117.117.117.11Area6352170067717026268762790579584824636680IS AreaStd. Conc12.00012.00012.00012.00012.00012.00012.00012.000ng/g12.87414.20114.53312.70612.72611.7479.7787.434%Rec107.3118.3121.1105.9106.197.981.562.0S/N0297123299463405500Acq.Date18-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-1218-Apr-12Acq.Time21:24:4621:41:3121:58:1622:15:0222:31:4822:48:3423:05:2023:22:06Detection...MMMMMMMMMMMMMMMMCompound name: 13C4-PFOAResponse Factor: 4933.87RRF SD: 969.161, % Relative SD: 19.643Response type: External Std, AreaCurve type: RFConc0.0 2.0 4.0 6.0 8.0 10.0 12.0

Response0200004000060000PV by HH, Checked by JP 19-Apr-12, NOTE: CAL/VER Concn & LOD units = ng abs.Quantify Sample ReportMassLynx 4.1 SCN627Dataset:G:\Masslynx\Inst_G\PFC.PRO\FC\FC2G_150-A1.qldLast Altered:Thursday, April 19, 2012 11:51:33 Pacific Daylight TimePrinted:Thursday, April 19, 2012 12:55:08 Pacific Daylight TimeMethod: G:\Masslynx\Master Methods\PFC\FC_043_08_02.mdb 08 Nov 2011 13:21:58Calibration: G:\Masslynx\Inst_G\PFC.PRO\CurveDB\FC2G_150-A1.cdb 19 Apr 2012 11:51:33ID: FC-LIN-39725T-A,,1/2Name: FC2G_150S004Description: 1,,15uLDate: 18-Apr-2012Time: 21:24:46PFOA-1min7.00 8.00%0100FC2G_150S004PFOA-17.152.37e394757.78PFOA-2min7.00 8.00%0100FC2G_150S004PFOA-27.151.07e3370013C2-PFOAmin7.00 8.00%0100FC2G_150S00413C2-PFOA7.151.76e566114813C8-PFOAmin7.00 8.00%0100FC2G_150S00413C8-PFOA7.116.83e426886113C4-PFOAmin7.00 8.00%0100FC2G_150S00413C4-PFOA7.116.35e4249525#56192021NamePFOA-1PFOA-213C2-PFOA13C8-PFOA13C4-PFOAIS#19192121Trace412.97> 368.98412.97> 168.80414.97 > 369....420.97 > 375....416.97 > 371.9RT7.157.157.157.117.11Area236810731759166829163521IS Area1759161759166352163521ng/g0.9211.09569.33412.23112.874LOD%Rec92.1109.596.3101.9107.3S/N5814000Noise163257000Height94753700661148268861249525IS Height661148661148249525249525Sample size1.00001.00001.00001.00001.0000Factor21.01.01.01.01.0Detection...MMbbMMMMMMPV by HH, Checked by JP 19-Apr-12, NOTE: CAL/VER Concn & LOD units = ng abs.Quantify Sample ReportMassLynx 4.1 SCN627Dataset:G:\Masslynx\Inst_G\PFC.PRO\FC\FC2G_150-A1.qldLast Altered:Thursday, April 19, 2012 11:51:33 Pacific Daylight TimePrinted:Thursday, April 19, 2012 12:55:08 Pacific Daylight TimeID: FC-LIN-39725T-B,,1/2Name: FC2G_150S005Description: 1,,15uLDate: 18-Apr-2012Time: 21:41:31PFOA-1min7.00 8.00%0100FC2G_150S005PFOA-17.158.11e331540PFOA-2min7.00 8.00%0100FC2G_150S005PFOA-27.151.69e3690013C2-PFOAmin7.00 8.00%0100FC2G_150S00513C2-PFOA7.151.98e580200313C8-PFOAmin7.00 8.00%0100FC2G_150S00513C8-PFOA7.157.19e428391913C4-PFOAmin7.00 8.00%0100FC2G_150S00513C4-PFOA7.157.01e4279051#56192021NamePFOA-1PFOA-213C2-PFOA13C8-PFOA13C4-PFOAIS#19192121Trace412.97> 368.98412.97> 168.80414.97 > 369....420.97 > 375....416.97 > 371.9RT7.157.157.157.157.15Area810616901977217188070067IS Area1977211977217006770067ng/g2.9781.89970.64811.67114.201LOD0.01400.1436%Rec119.176.098.197.3118.3S/N2501702473297Noise1264000115940Height315406900802003283919279051IS Height802003802003279051279051Sample size1.00001.00001.00001.00001.0000Factor21.01.01.01.01.0Detection...MMbbMMMMMMPV by HH, Checked by JP 19-Apr-12, NOTE: CAL/VER Concn & LOD units = ng abs.Quantify Sample ReportMassLynx 4.1 SCN627Dataset:G:\Masslynx\Inst_G\PFC.PRO\FC\FC2G_150-A1.qldLast Altered:Thursday, April 19, 2012 11:51:33 Pacific Daylight TimePrinted:Thursday, April 19, 2012 12:55:08 Pacific Daylight TimeID: FC-LIN-39725T-C,,1/2Name: FC2G_150S006Description: 1,,15uLDate: 18-Apr-2012Time: 21:58:16PFOA-1min7.00 8.00%0100FC2G_150S006PFOA-17.112.76e4109260PFOA-2min7.00 8.00%0100FC2G_150S006PFOA-27.116.59e32490713C2-PFOAmin7.00 8.00%0100FC2G_150S00613C2-PFOA7.112.03e578927213C8-PFOAmin7.00 8.00%0100FC2G_150S00613C8-PFOA7.117.75e430842913C4-PFOAmin7.00 8.00%0100FC2G_150S00613C4-PFOA7.117.17e4275873#56192021NamePFOA-1PFOA-213C2-PFOA13C8-PFOA13C4-PFOAIS#19192121Trace412.97> 368.98412.97> 168.80414.97 > 369....420.97 > 375....416.97 > 371.9RT7.117.117.117.117.11Area2755965922034497747271702IS Area2034492034497170271702ng/g10.0339.73071.03612.29214.533LOD0.04130.0354%Rec100.397.398.7102.4121.1S/N6675309241232Noise1644670334224Height10926024907789272308429275873IS Height789272789272275873275873Sample size1.00001.00001.00001.00001.0000Factor21.01.01.01.01.0Detection...MMbbMMMMMMPV by HH, Checked by JP 19-Apr-12, NOTE: CAL/VER Concn & LOD units = ng abs.Quantify Sample ReportMassLynx 4.1 SCN627Dataset:G:\Masslynx\Inst_G\PFC.PRO\FC\FC2G_150-A1.qldLast Altered:Thursday, April 19, 2012 11:51:33 Pacific Daylight TimePrinted:Thursday, April 19, 2012 12:55:08 Pacific Daylight TimeID: FC-LIN-39725T-D,,1/2Name: FC2G_150S007Description: 1,,15uLDate: 18-Apr-2012Time: 22:15:02PFOA-1min7.00 8.00%0100FC2G_150S007PFOA-17.151.01e5393798PFOA-2min7.00 8.00%0100FC2G_150S007PFOA-27.152.43e49339013C2-PFOAmin7.00 8.00%0100FC2G_150S00713C2-PFOA7.111.74e567096913C8-PFOAmin7.00 8.00%0100FC2G_150S00713C8-PFOA7.116.40e425218713C4-PFOAmin7.00 8.00%0100FC2G_150S007#56192021NamePFOA-1PFOA-213C2-PFOA13C8-PFOA13C4-PFOAIS#19192121Trace412.97> 368.98412.97> 168.80414.97 > 369....420.97 > 375....416.97 > 371.9RT7.157.157.117.117.11Area101183243141739896395262687IS Area1739891739896268762687ng/g43.34944.96869.48611.60612.706LOD0.01930.0384%Rec108.4112.496.596.7105.9S/N049901872994Noise01870135239Height39379893390670969252187237761IS Height670969670969237761237761Sample size1.00001.00001.00001.00001.0000Factor21.01.01.01.01.0Detection...MMbbMMMMMMPV by HH, Checked by JP 19-Apr-12, NOTE: CAL/VER Concn & LOD units = ng abs.Quantify Sample ReportMassLynx 4.1 SCN627Dataset:G:\Masslynx\Inst_G\PFC.PRO\FC\FC2G_150-A1.qldLast Altered:Thursday, April 19, 2012 11:51:33 Pacific Daylight TimePrinted:Thursday, April 19, 2012 12:55:08 Pacific Daylight TimeID: FC-LIN-39725T-E,,1/2Name: FC2G_150S008Description: 1,,15uLDate: 18-Apr-2012Time: 22:31:48PFOA-1min7.00 8.00%0100FC2G_150S008PFOA-17.114.76e51953338PFOA-2min7.00 8.00%0100FC2G_150S008PFOA-27.111.14e546962713C2-PFOAmin7.00 8.00%0100FC2G_150S00813C2-PFOA7.111.82e574666013C8-PFOAmin7.00 8.00%0100FC2G_150S00813C8-PFOA7.116.64e427247313C4-PFOAmin7.00 8.00%0100FC2G_150S00813C4-PFOA7.116.28e4252845#56192021NamePFOA-1PFOA-213C2-PFOA13C8-PFOA13C4-PFOAIS#19192121Trace412.97> 368.98412.97> 168.80414.97 > 369....420.97 > 375....416.97 > 371.9RT7.117.117.117.117.11Area4761251143951824986637462790IS Area1824981824986279062790ng/g194.766204.86772.76512.02612.726LOD0.0603%Rec97.4102.4101.1100.2106.1S/N0000634Noise0000399Height1953338469627746660272473252845IS Height746660746660252845252845Sample size1.00001.00001.00001.00001.0000Factor21.01.01.01.01.0Detection...MMbbMMMMMMPV by HH, Checked by JP 19-Apr-12, NOTE: CAL/VER Concn & LOD units = ng abs.Quantify Sample ReportMassLynx 4.1 SCN627Dataset:G:\Masslynx\Inst_G\PFC.PRO\FC\FC2G_150-A1.qldLast Altered:Thursday, April 19, 2012 11:51:33 Pacific Daylight TimePrinted:Thursday, April 19, 2012 12:55:08 Pacific Daylight TimeID: FC-LIN-39725T-F,,1/2Name: FC2G_150S009Description: 1,,15uLDate: 18-Apr-2012Time: 22:48:34PFOA-1min7.00 8.00%0100FC2G_150S009PFOA-17.119.58e53865211PFOA-2min7.00 8.00%0100FC2G_150S009PFOA-27.112.30e593794413C2-PFOAmin7.00 8.00%0100FC2G_150S00913C2-PFOA7.111.71e570632413C8-PFOAmin7.00 8.00%0100FC2G_150S00913C8-PFOA7.116.07e424407013C4-PFOAmin7.00 8.00%0100FC2G_150S00913C4-PFOA7.115.80e4242971#56192021NamePFOA-1PFOA-213C2-PFOA13C8-PFOA13C4-PFOAIS#19192121Trace412.97> 368.98412.97> 168.80414.97 > 369....420.97 > 375....416.97 > 371.9RT7.117.117.117.117.11Area9580322296841714546074857958IS Area1714541714545795857958ng/g417.235438.86074.06111.92411.747LOD0.0560%Rec104.3109.7102.999.497.9S/N0006120Noise0003990Height3865211937944706324244070242971IS Height706324706324242971242971Sample size1.00001.00001.00001.00001.0000Factor21.01.01.01.01.0Detection...MMbbMMMMMMPV by HH, Checked by JP 19-Apr-12, NOTE: CAL/VER Concn & LOD units = ng abs.Quantify Sample ReportMassLynx 4.1 SCN627Dataset:G:\Masslynx\Inst_G\PFC.PRO\FC\FC2G_150-A1.qldLast Altered:Thursday, April 19, 2012 11:51:33 Pacific Daylight TimePrinted:Thursday, April 19, 2012 12:55:08 Pacific Daylight TimeID: FC-LIN-39725T-G,,1/2Name: FC2G_150S010Description: 1,,15uLDate: 18-Apr-2012Time: 23:05:20PFOA-1min7.00 8.00%0100FC2G_150S010PFOA-17.111.73e67293368PFOA-2min7.00 8.00%0100FC2G_150S010PFOA-27.114.20e5178747213C2-PFOAmin7.00 8.00%0100FC2G_150S01013C2-PFOA7.111.37e557530813C8-PFOAmin7.00 8.00%0100FC2G_150S01013C8-PFOA7.115.33e422385613C4-PFOAmin7.00 8.00%0100FC2G_150S01013C4-PFOA7.114.82e4201739#56192021NamePFOA-1PFOA-213C2-PFOA13C8-PFOA13C4-PFOAIS#19192121Trace412.97> 368.98412.97> 168.80414.97 > 369....420.97 > 375....416.97 > 371.9RT7.117.117.117.117.11Area17311154201931370305329148246IS Area1370301370304824648246ng/g943.4251005.73071.10812.5669.778LOD0.04970.0533%Rec94.3100.698.8104.781.5S/N000762550Noise000294367Height72933681787472575308223856201739IS Height575308575308201739201739Sample size1.00001.00001.00001.00001.0000Factor21.01.01.01.01.0Detection...MMbbMMMMMMPV by HH, Checked by JP 19-Apr-12, NOTE: CAL/VER Concn & LOD units = ng abs.Quantify Sample ReportMassLynx 4.1 SCN627Dataset:G:\Masslynx\Inst_G\PFC.PRO\FC\FC2G_150-A1.qldLast Altered:Thursday, April 19, 2012 11:51:33 Pacific Daylight TimePrinted:Thursday, April 19, 2012 12:55:08 Pacific Daylight TimeID: FC-LIN-39725T-H,,1/2Name: FC2G_150S011Description: 1,,15uLDate: 18-Apr-2012Time: 23:22:06PFOA-1min7.00 8.00%0100FC2G_150S011PFOA-17.113.20e612985217PFOA-2min7.00 8.00%0100FC2G_150S011PFOA-27.117.97e5327252113C2-PFOAmin7.00 8.00%0100FC2G_150S01113C2-PFOA7.111.14e546263413C8-PFOAmin7.00 8.00%0100FC2G_150S01113C8-PFOA7.113.77e415610413C4-PFOAmin7.00 8.00%0100FC2G_150S01113C4-PFOA7.113.67e4150361#56192021NamePFOA-1PFOA-213C2-PFOA13C8-PFOA13C4-PFOAIS#19192121Trace412.97> 368.98412.97> 168.80414.97 > 369....420.97 > 375....416.97 > 371.9RT7.117.117.117.117.11Area31962807969651136403767236680IS Area1136401136403668036680ng/g2100.5502301.32377.56311.6847.434LOD%Rec84.092.1107.797.462.0S/N00000Noise00000Height129852173272521462634156104150361IS Height462634462634150361150361Sample size1.00001.00001.00001.00001.0000Factor21.01.01.01.01.0Detection...MMbbMMMMMMPV by HH, Checked by JP 19-Apr-12, NOTE: CAL/VER Concn & LOD units = ng abs.

### ---'--'------------------------------------------------------------- Quantify Sample Report MassLynx 4.1 SCN627

Dataset:

Last Altered: Printed: G:\Masslynx\lnst_ G\PFC.PRO\FC\FC2G _150-b.qld Friday, April 27, 2012 11 :33:53 Pacific DaylightTime Friday, April 27, 201213,:05:43 Pacific Daylight Time

Method: G:\Masslynx\Master Methods\PFC\FC_043_08_02.mdb 08 Nov 2011 13:21 :58 Calibration: G:\Masslynx\lnsC G\PFC.PRO\CurveDB\FC2G_150-A1.cdb 19 Apr 2012 11 :51 :33

ID: FC-LlN-39725T -D" 1/2 Name: FC2G_150S016 Description: 1,,15uL Date: 19-Apr-2012 Time: 00:46:01

PFOA-1 FC2G_150S016 100 7.11 9.97e4 395087

" 7.00 8.00 , min PFOA-2 FC2G_150S016 100 7.11 2.47e4 100227
%



### o 7.00 8.00 13C2-PFOA FC2G_150S016 100 7.11

# '~8~~~~

%**>.,~ttl**



### o

, "" ,min 7.00 8.00 13C8-PFOA

7.00
" 8.00

# 

### ,'Area," -J$Arjfjil**'.~g;,** 

### ':',o/.Ree,' 5 PFOA-1 19 412.97> 368.98 7.11 99677 173449 42.836 107.1 6 PFOA-2 19 412.97> 168.80 7_11 24700 173449 45.842 114.6 19 13C2-PFOA 21 414.97 > 369

__ .. 7.11 173449 65286 66.513 0.0816 92.4 20 13C8-PFOA 21 420.97 > 375

.... 7.11 68008 65286 11.851 98.8 21 13C4-PFOA 416.97> 371.9 7.11 65286 13.232 110.3

PV by HH, SV by JP 27-Apr-12, NOTE: CALlVERlSPM Concn & LOD units = ng abs. 13C4-PFOA FC2G_150S016 100 7.11

%

min 0- min 7.00 8.00**,~lN·:.** 

### No!ile**H~igbt** . ",;1$ 11&lgl:lt '. Siilll'ij)Iesiz& :'!"actor;!OetectlOn;

.. 0 0 395087 681240 1.0000 1.0 

### MM 849 118 100227 681240 1.0000 1,0 bb 2373 287 681240 264379 1.0000 1.0 

### MM 0 0 270350 264379 1.0000 1.0 

### MM 0 0 264379 1.0000 1.0 

### MMQuantify Sample Report MassLynx 4.1 SCN627

Dataset: G:\Masslynx\lnst_ G\PFC.PRO\FC\FC2G _150-b.qld

Last Altered: Friday, April 27, 2012 11 :33:53 Pacific Daylight Time Printed: Friday, April 27, 2012 13:05:43 Pacific Daylight Time**------~~--------------------------------------------------------------------------**

10: FC-LlN·39725T ·0" 1/2 Name: FC2G_150S031 Description: 1,,15uL Date: 19-Apr·2012 Time: 04:57:29

PFOA-1**#~.** 

### ",elM:;; 5 PFOA-1 6 PFOA-2 19 13C2-PFOA 20 13C8-PFOA 21 13C4-PFOA PFOA·2 FC2G_150S031 100 7.11 2.50e4 100798
%



### o**~h-r-~** min 7.00 B.OO
"!$#**I~T~** 19 412.97>368.98 7.11 19 412.97> 168.80 7.11 21 414.97> 369

.... 7.11 21 420.97 > 375

.... 7.11 416.97> 371.9 7.11 13C2-PFOA FC2G _150S031 100

. 7.11

., 1.77e5 ; 738968
%



### o 7.00**~f"iT-rTl~** min 8.00

101726 177273 42.774 25025 177273 45.435 177273 62325 71.210 69626 62325 12.709 62325 12.632

PV by HH, SV by JP 27-Apr-12, NOTE: CALlVERlSPM Concn & LOD units 

### = ng abs. 13C8·PFOA FC2G_150S031 100 7.11

%

7.00 B.OO

0.0025 106.9 0.6496 113.6 98.9 0.0683 105.9 0.0291 105.3 1373 86 0 574 1304 13C4·PFOA FC2G_150S031 100 7.11 6.23e4 245393

'" , min 8.00 7.00**N~~:' '!'l~I!l~~**  

### .•. ISHeil/fit**i~mple!!iaeiF!ilCt()~::I)III!1ctlon,,;** 286 392055 738968 1.0000 1.0 MM 1168 

### o 491 188 100798 738968 1.0000 738968 245393 1.0000 281857 245393 1.0000 245393 1.0000 1.0 bb 1.0 MM 1.0 MM 1.0 MMAXYS 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