3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 1 OF 23 

# Final Report

Analysis of PFOA, PFBS, PFHS, and PFOS in Aqueous Samples from

3M Decatur, Alabama : Groundwater Treatment Plant GAC System

– September 2013

Laboratory Request Number: ISO13

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Method Re quirement: 3M Method ETS

- 8

- 044.1

Report Date

– Date of Last Signature



## Testing Laboratory

3M EHS &S Operations 3M Environmental Laboratory Building 260

- 5N

- 17 Maplewood, MN 55144

- 1000

Requester

Gary Hohenstein 3M Building 224

- 5W

- 03 Saint Paul, MN 55144

- 1000 Phone: (651) 737

- 3570

The testing reported herein meet the requirements of ANSI/ISO/IEC 17025:2005 “General Requirements for the Competence of Testing and Calibration Laboratories”, in accordance with the A2LA Testing Certificate # 2052.01. Additionally, the laboratory’s quality system has been audited and was determined to be in conformance with the EPA GLPs (40 CFR 792) by an independent A2LA assessment.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 2 OF 23 

### 3M Envir onmental Laboratory

3M Environmental Laboratory Technical Director: William K. Reagen, Ph.D

. 3M Principal Analytical Investigator: Susan Wolf Report Author: Chelsie Grochow



## Analytical Report ISO13

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3M Decatur Groundwater Treatment Plant System; Sep tember 2013 Sampling

Report Date: Date of Last Signature



# 1 Introduction/Summary

The 3M Environmental Laboratory analyzed water samples from the groundwater treatment plant GAC system at the 3M Decatur, AL facility. Water samples were collected by Weston Solutions personnel

on September 30 , 2013

. Samples were returned to the 3M Environmental Laboratory for analysis of P erfluorooctanoate (PFOA) , Perfluorobutane sulfonate (PFBS), Perf luorohexane sulfonate (PFHS), Perfluorooctane sulfonate (PFOS) under la bo ratory project number ISO13

- 07

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. Analysis of the samples was completed as specified under 3M Environmental Laboratory General Project Outline (GPO) number GPO11

- 1006.

T he 3M Environmental Laboratory provided sample containers for seven sampling locatio ns; ACI, ACM2, ACE , WW8R, WW9R , WW10R, and WW11R . The sample set consisted of a field sample, field

sa mple duplicate and a field matrix spike. Each empty container was marked with a “fill to here” line that corresponded to a final volume of 200 mL. Cont ainers reserved for field matrix spikes were fortified with an appropriate matrix spike solution containing all analytes prior to being sent to the field for sample collection. S ample bottles for sampling locations ACM2 and ACE

, along with the Trip Blank sample and low spike

, were fortified with internal standards and surrogates prior to being sent to the field for sample collection.

Samples were prepared and analyzed by method ETS

- 8

- 044. 1 “ Method of Analysis for the Determination of Perfluorinated Comp ounds in Water by LC/MS/MS; Direct Injection Analysis ”. Select internal standards were used to aid in the data quality objectives.

Table 1 summarizes the sample results using the analytical method identified above. All results for quality control samp les prepared and analyzed with the samples will be reported and discussed elsewhere in this report.

The testing reported herein meet the requirements of ANSI/ISO/IEC 17025:2005 “General Requi rements for the Competence of Testing and Calibration Laboratories”, in accordance with the A2LA Testing Certificate # 2052.01. Additionally, the laboratory’s quality system has been audited and was determined to be in conformance with the EPA GLPs (40 CF R 792) by an independent A2LA assessment.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 3 OF 23 

### Table 1 . Sample Results Summary

3M LIMS ID Sample Description PFOA Concentration (ng/mL) PFBS Concentration (ng/mL) PFHS C oncentration (ng/mL) PFOS Concentration (ng/mL)

ISO13

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- 001 DAL

- GW

- ACI ; Sample 2280 349 1370 3170

ISO13

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- 002 DAL

- GW

- ACI ; Sample Dup 2350 363 1420 3310
Average 2320 (1) 356 (1) 1400 (1) 3240 (1)
%RPD Sample/Sample Dup 3.0 3.9 3.6 4.3

ISO13

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- 004 DAL

- GW

- ACM2; Sample 1210 468 1550 1.31

ISO13

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- 005 DAL

- GW

- ACM2 ; Sample Dup 1220 471 1570 1.29 Average 1220 (1) 470 (1) 1560 (1) 1.30 (2 )
%RPD Sample/Sample Dup 0.82 0. 64 1.3 1.5

ISO13

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- 007 DAL

- GW

- ACE; Sample 0.109 1920 0.157 0. 0419

ISO13

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- 008 DAL

- GW

- ACE ; Sample Dup 0.121 1980 0.154 0.0485 Average 0.115 (2 ) 1950 (1 ) 0.156 (2 ) 0.0452 (2 )
%RPD Sample/Sample Dup 10 3.1 1. 9 15

ISO13

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- 010 DAL

- GW

- WW8R; Sample 2890 309 1360 4110

ISO13

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- 011 DAL

- GW

- WW8R ; Sample Dup 2890 296 1370 4090 Average 2 890 (1) 303 (1) 1370 (1) 4100 (1)
%RPD Sample/Sample Dup 0.0 4.3 0.73 0.49

ISO13

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- 013 DAL

- GW

- WW9R; Sample 2740 252 1230 4130

ISO13

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- 014 DAL

- GW

- WW9R ; Sample Dup 2720 245 1210 4270 Average 2730 (1) 249 (1) 12 20 (1) 4200 (1)
%RPD Sample/Sample Dup 0.73 2.8 1. 6 3. 3

ISO13

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- 019 DAL

- GW

- WW10R; Sample 2040 244 1020 2760

ISO13

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- 020 DAL

- GW

- WW10R ; Sample Dup 2090 250 1040 2780 Average 2070 (1) 247 (1) 1030 (1) 2770 (1)
%RPD Sample/Sample Dup 2.4 2.4 1.9 0.72

ISO13

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- 022 DAL

- GW

- WW11R; Sample 1700 297 1010 2190

ISO13

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- 023 DAL

- GW

- WW11R ; Sample Dup 1730 301 993 2210 Average 1 720 (1) 299 (1) 1000 (1) 2200 (1)
%RPD Sample/Sample Dup 1.7 1. 3 1. 7 0.91

(1) Reported results were prepared and anal yzed by ETS

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- 044. 1 using external standard calibration . The analytical method uncertainties associated with the reported results are as follows: PFOA ±14 %, PFBS ± 1 3 %, PFHS ±1 2 %, and PFOS ± 1 6 %. (2) Reported results were prepared and analyzed by ETS

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- 044.1 us ing internal standard calibration. The analytical method uncertainties associated with the reported results are as follows: PFOA ± 1 3 %, PFHS ± 1 4 %, and PFOS ± 15 %.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 4 OF 23 

# 2 Methods

- Analytical and Preparatory

2.1 Methods Analysis was completed using 3M Environmen tal Laboratory Method ETS

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- 044. 1 “ Method of Analysis for the Determination of Perfluorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis ”

.

Table 2 . Target Analytes

Target Analytes Acronym Reference Material Structu re Perfluorooctanoic Acid (C8 Acid) PFOA Linear + Branched Perfluorobutanesulfonate (C4 Sulfonate ) PFBS Linear Perfluorohexanesulfonate (C6 Sulfonate) PFHS Linear Perfluorooctanesulfonate (C8 Sulfonate) PFOS Linear + Branched



## 2.2 Sample Collection Sampl es were collected on September 30 , 201 3 in Nalgene TM 

### (high

- density polyethylene) bottles prepared at the 3M Environmental Laboratory. Prior to sample collection, bottles designated for field matrix spikes were spiked in the laboratory with a known volume of an appropriate matrix spiking solution containing PFOA, PFBS, PFHS, and PFOS

. Sample bottles for sampling locations ACM2 and ACE, along with the Tr ip Blank sample and low spike, were fortified with a mixture of mass

- labeled internal standards at a nom i nal concentration of 1 ng/mL and a mixture of surrogate recovery standards at a nominal concentration of 0.1 ng/mL

. Collected sample bottles were received by the laboratory at ambient conditions on October 9 , 201 3

. The sample bottles for locations ACI, A CM2, ACE, WW8R, WW9R and the Trip Blank samples were prepared on August 20, 2013 . Sample bottles for locations WW10R and WW11R were prepared on September 24, 2013 . All sample bottles were prepared with spiking solutions that expired on September 29, 2013 , just prior to sample collection on September 30, 2013. A deviation is included with the raw data.



## 2.3 Sample Preparation
All s ample s were diluted with methanol and analyzed for all analytes. Samples diluted 1:10 were prepared by removing a 1 mL aliquot of the well mixed sample and adding 8.9 mL of methanol and 0.1 mL of a surrogate spiking solution. The 1:100 dilutions were prepared by removing a 0.1 mL aliquot of the well mixed sample and adding 9.8 mL of methanol and 0.1 mL of a surrogate spiking solu tion. Prepared samples were analyzed by external standard calibration.

The ACE and ACM2 sample set s and the Trip Blank sample were prepared and analyzed for all analytes by transferring a n aliquot of the well mixed sample into an autovial. Prepared samples were analyzed by internal standard calibration.

During the preparation of the laboratory control samples for internal standard calibration , an aliquot of a separate internal standard spiking solution was added to the laboratory control samples ( nominal concentration of 1 ng/mL). The sample bottles for ACE, ACM2, and Trip Blank were spiked with an internal standard mix at a nominal concentration of 1 ng/mL prior to being sent to the field for sample collection. The laboratory control samples wer e analyzed in the same manner as the samples.



## 2.4 Analysis All samples and quality control samples were analyzed for f our target analytes using high per formance liquid chromatography/ tandem mass spectrometry (HPLC/MS/MS). Pertinent instrument parameters,
t he liquid chromatography gradient program, and the specific mass transitions analyzed are described in the tables below.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 5 OF 23 

### Due to the nature of the sample, the wide range of concentrations found in the sample, and the environmental occurrence of multiple iso mers of the laboratory’s analytes of interest, the software used for processing the analytical results is not able to consistently integrate the analytical peak, manual integration of the analytical peak is necessary. All manual integrations are performed following the procedures outlined in method ETS

- 12

- 010. The consistency of the laboratory’s integration is ensured through the training of laboratory personnel, the peer review process required for all manual integrations, the review of manual integratio ns by the QAU, and where necessary the review of manual integrations by laboratory management.

Table 3 . Instrument Parameters.

Instrument Name ETS Kirk

Analysis Dates 10/15 /13

– external standard calibration

10

/ 1 6 /13

– internal s tandard calibration Analytical Method ETS

- 8

- 044.1 Liquid Chromatograph Agilent 1260

Guard column Betasil C18 (4.6 mm X 100 mm), 5 μ Analytical column Betasil C18 (4.6 mm X 100 mm), 5 μ Injection Volume 5 or 20 μ L Mass Spectrometer Applied Biosystems TripleQuad 5500

Ion Source Turbo Spray Polarity Negative

Software Analyst 1.6.1



### Table 4 . Liquid Chromat ography Gradient Program.

Step Number Total Time (min) Flow Rate ( μ L/min) Percent A (2 mM ammonium acetate) Percent B (Methanol)

0 0.00 750 90.0 10.0

1 0.50 750 90.0 10.0

2 4.00 750 70.0 30.0

3 6.00 750 70.0 30.0

4 11.0 750 20.0 80.0

5 13.0 750 20.0 80.0

6 13.5 750 10.0 90.0

7 16.0 750 10.0 90.0

8 16.5 750 90.0 10.0

9 19.0 750 90.0 10.03M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 6 OF 23 

### Table 5 . Mass Transitions

.

Analyte Mass Transition
Q1/Q3 Internal Standard (1) Mass Transition Q1/Q3

PFOA 413/369 [ 13 C 8 ] PF OA 421/376 413/219

413/169

PFBS 299/80 NA NA 299/99

PFHS 399/99 [ 13 C 3 ]PFHS 402/ 80 399/80

PFOS 499/99 [ 13 C 8 ]PFOS 507/80 499/80

499/130 [ 13 C 4 ]PFOA surrogate 417/372 [ 13 C 8 ]PFOA 421/376 [ 13 C 4 ]PFOS surrogate 503/80 [ 13 C 8 ]PFOS 507/80 NA=Not applicable

Dwell time was 20 msec for each transition. The individual transitions were summed to produce a “total ion chromatogram” (TIC) , which was u sed for quantitation. (1) Internal standard s were used for the analysis of sampling locations ACM2, ACE, and the Trip Blank sample on 10 / 1 6/ 13

. 

# 3 Data Analysis

3.1 Calibration External Standard Calibration Analysis on 10/15/13: Samples were analyzed against an external standard calibration curve. Calibration standards were prepared by spiking known a mounts of the stock solution containing the target analytes into 90:10 methanol: Milli

- Q laboratory water. A total of eleven spiked standards ranging from 0.02 ng/mL to 50 ng/mL (nominal) were analyzed. The standards also contained the surrogates at conc entrations ranging from 0.02 ng/mL to 25 ng/mL nominal. A quadratic, 1/x weighted, calibration curve of the standard peak area counts was used to fit the data for each analyte. The data were not forced through zero during the fitting process. Calculatin g the standard concentrations using the peak area counts and the resultant calibration curve confirmed accuracy of each curve point.

Internal Standard Calibration Analysis on 10 / 1 6 /13 : Samples were analyzed against a matrix

- matched stable isotope inter nal standard calibration curve. Calibration standards were prepared by spiking known amounts of stock solutions into laboratory prepared reagent water . The calibration standards contained an internal standard mix at a nominal concentration of 1 ng/mL. A total of thirteen calibra tion standards ranging from 0.0 25 ng/mL to 25 ng/mL (nominal) were analyzed with the prepared samples. Of these t hirteen calibration standards, eleven contained the surrogates at concentrations ranging from 0.0 25 ng/mL to 10 ng/mL nominal. A quadratic, 1/x weighted, calibration curve of the ratio of the standard peak area counts over the internal standard peak area counts was used to fit the data for each analyte. The data were not forced through zero during the fitting process. Calculating the standard concentrations using the peak area ratios and the resultant calibration curve confirmed accuracy of each curve point.

For each calibration curve, t he reference standards of PFOA and PFOS used to prepare the calibration standard s consisted of both linear and branched isomers. Each curve point was quantitated using the overall calibration curve and reviewed for accuracy. Method calibration accuracy requirements of 100±25% (100±30% for the lowest curve point) were met for all ana lytes. The correlation coefficient (r) was greater than 0.995 for all analytes

.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 7 OF 23 

## 3.2 System Suitability
A calibration standard was analyzed four times at the beginning of the analytical sequence to demonstrate overall system suitability. T he acceptance crite ria for system suitability samples is less than or equal to 5% relative standard deviation (RSD) for peak area /ratio and retention time criteria of less than or equal to 2% RSD

. These cri teria were met for all analytes

.


## 3.3 Limit of Quantitation (LOQ)
The LO Q as defined in method ETS

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- 044. 1 is the lowest non

- zero calibration standard in the curve that meets linearity and accuracy requirements and for which the area counts are at least twice those of the appropriate blanks. The LOQs associated with the sampl e analysis are listed in Table 6

.

T able 6 . LOQ

Analyte Calibration LOQ, ng/mL

PFOA Internal standard 0.0240

PFHS Internal standard 0.0 400

PFOS Internal standard 0.0232

PFOA External standard 0.0192 (1)

PFBS External standar d 0.0200 (1)

PFHS External standard 0.0200 (1)

PFOS External standard 0.0185 (1) (1) The dilution factor was not applied to the LOQ.



## 3.4 Continuing Calibration During the course of the analytical sequence, several continuing calibration verification samples (CCVs) were analyzed to confirm that the instrument response and the initial calibration curve were still in control. The method acceptance criteria of 100% ± 25% was met for all analytes

.


## 3.5 Blanks
Two types of blanks were prepared and analyzed w ith the sa mples: method blanks/solvent blanks and field/trip blanks . Each blank result wa s reviewed and used to evaluate method performance to determine the LOQ for each analyte.



## 3.6 Lab Control Spikes (LCSs) Low, mid, and high lab control spikes were prepared for th e target analytes and analyzed in triplicate, while only low and high lab control spikes were prepared for the surrogates . LCSs were prepared by spiking known amounts of the analytes into either 10 mL of laboratory

- prepared matrix matched water or 1 mL of Milli

- Q water to produce the desired concentration. When applicable, t he LCSs were then diluted with methanol in the same manner as the samples

. Method ETS

- 8

- 044.1 states that the average recovery of LCS s at each spiking level be within 80%

- 120% wi th a RSD ≤20%. All LCS sampl es met method accuracy criteri a

.
All LCSs were used in the determination of the analytical m ethod uncertainty in section 3.7

.

T he following calculations were used to generate data in Table 7

.

100% * ion Concentrat Spike ion Concentrat Calculated Recovery Percent LCS =

100% * recovery LCS average replicates LCS deviation standard RSD LCS% =3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 8 OF 23 

### Table 7 . Lab Control Spike Results.

ETS

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- 044.1

Ex

ternal Standard

Calibration Analyzed 10/15 / 13 PFOA (Linear + Branched ) PFOA surrogate

Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Rec overy Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery

LCS

- 131015

- 1 0.191 0.200 105 0.199 0.216 109
LCS

- 131015

- 2 0.191 0.207 109 0.199 0.219 110

LCS

- 131015

- 3 0.191 0.224 117 0.199 0.193 97.2 Average ± %RSD 110 % ± 5.6 % 1 05 % ± 6.8 %

LCS

- 131015

- 4 4.74 5.39 114 4.94 5.35 108

LCS

- 131015

- 5 4.74 5.36 113 4.94 5.37 109

LCS

- 131015

- 6 4.74 5.32 112 4.94 5.43 110 Average ± %RSD 1 13 % ± 0.88 % 109 % ± 0. 92 %

LCS

- 131015

- 7 38.2 40.8 107

LCS

- 131015

- 8 38.2 37.5 98 .2

LCS

- 131015

- 9 38.2 37.5 98.3 Average ± %RSD 1 0 1 % ± 5.0 %

ETS

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- 044.1
External Standard

Calibration Analyzed 10/15 /13 PFBS PFHS

Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery

LCS

- 131015

- 1 0.199 0.226 113 0.199 0.220 110
LCS

- 131015

- 2 0.199 0.223 112 0.199 0.218 109

LCS

- 131015

- 3 0.199 0.235 118 0.199 0.228 115 Average ± %RSD 114 % ± 2.8 % 1 11 % ± 2.9 %

LCS

- 131015

- 4 4.95 5.55 112 4.95 5.61 113

LCS

- 131015

- 5 4.95 5.61 113 4.95 5.56 112

LCS

- 131015

- 6 4.95 5.47 110 4.95 5.50 111 Average ± %RSD 112 % ± 1.4 % 1 12 % ± 0.89 %

LCS

- 131015

- 7 39.8 42.6 107 39.8 42.5 107

LCS

- 131015

- 8 39.8 38.7 97.2 39.8 39.4 99.1

LCS

- 131015

- 9 39.8 38.4 96.4 39.8 3 8.6 97.0 Average ± %RSD 10 0 % ± 5.9 % 101 % ± 5.2 %3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 9 OF 23 

### Table 7 continued. Lab Control Spike Results.

ETS

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- 044.1
External Standard

Calibration Analyzed 10/15 /13 PFOS (Linear + Branched) PFOS surrogate

Lab ID Spiked Concentration (ng/mL) Calculat ed Concentration (ng/mL) %Recovery Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery

LCS

- 131015

- 1 0.185 0.210 114 0.190 0.206 108
LCS

- 131015

- 2 0.185 0.213 115 0.190 0.213 112

LCS

- 131015

- 3 0.185 0.217 117 0.190 0.193 101

Aver age ± %RSD 1 15 % ± 1.3 % 107 % ± 5.2 %

LCS

- 131015

- 4 4.59 5.34 116 4.73 5.26 111

LCS

- 131015

- 5 4.59 5.28 115 4.73 5.23 111

LCS

- 131015

- 6 4.59 5.24 114 4.73 5.30 112 Average ± %RSD 1 15 % ± 0

. 87 % 111 % ± 0. 52 %

LCS

- 131015

- 7 36.9 40.3 109

LCS

- 131015

- 8 36.9 37.1 1 01

LCS

- 131015

- 9 36.9 36.4 98.6 Average ± %RSD 103 % ± 5.3 %

ETS

- 8

- 044.1

In ternal Standard

Calibration Analyzed 10 / 1 6 /13 PFOA (Linear + Branched) PFOA surrogate

Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery S piked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery

LCS

- 131016

- 1 0.190 0.187 98.5 0.198 0.185 93.6
LCS

- 131016

- 2 0.190 0.204 107 0.198 0.193 97.5

LCS

- 131016

- 3 0.190 0.194 102 0.198 0.195 98.5 Average ± %RSD 103 % ± 4.1 % 96.5 % ± 2.7 %

LCS

- 131016

- 4 1.90 2.07 109 1.98 2.11 106

LCS

- 131016

- 5 1.90 2.01 106 1.98 1.97 99.6

LCS

- 131016

- 6 1.90 1.98 104 1.98 1.97 99.6 Average ± %RSD 106 % ± 2.4 % 10 2 % ± 3.6 %

LCS

- 131016

- 7 19.0 19.7 104

LCS

- 131016

- 8 19.0 18.5 97.6

LCS

- 131016

- 9 19.0 19.1 100 Average ± %RSD 101 % ± 3. 2 %3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 10 OF 23 

### Table 7 continued. Lab Control Spike Results.

ETS

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- 044.1

In ternal Standard

Calibration Analyzed 10 / 1 6 /13 PFHS PFOS (Linear + Branched)

Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) % Recovery Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery

LCS

- 131016

- 1 0.198 0.200 101 0.184 0.195 106
LCS

- 131016

- 2 0.198 0.212 107 0.184 0.202 110

LCS

- 131016

- 3 0.198 0.193 97.6 0.184 0.185 100 Average ± %RSD 102 % ± 4 .7 % 105 % ± 4.8 %

LCS

- 131016

- 4 1.98 2.13 108 1.84 1.97 107

LCS

- 131016

- 5 1.98 2.09 106 1.84 1.93 105

LCS

- 131016

- 6 1.98 1.99 100 1.84 1.92 105 Average ± %RSD 105 % ± 4

. 0 % 1 06 % ± 1.1 %

LCS

- 131016

- 7 19.9 20.9 105 18.4 18.5 100

LCS

- 131016

- 8 19.9 19.2 96.6 18.4 17.8 9 6.7

LCS

- 131016

- 9 19.9 19.7 99.0 18.4 17.7 96.0 Average ± %RSD 100 % ± 4.3 % 97.6 % ± 2.2 %

ETS

- 8

- 044.1
Internal Standard

Calibration Analyzed 10/16 /13 PFOS surrogate

Lab ID Spiked Concentration (ng/mL) Calculated Concentration (ng/mL) %Recovery

LCS

- 131016

- 1 0.189 0.185 98.0
LCS

- 131016

- 2 0.189 0.194 103

LCS

- 131016

- 3 0.189 0.200 106 Average ± %RSD 102 % ± 4.0 %

LCS

- 131016

- 4 1.89 1.99 105

LCS

- 131016

- 5 1.89 1.83 96.9

LCS

- 131016

- 6 1.89 1.93 102 Average ± %RSD 101 % ± 4 .1 %3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 11 OF 23 

## 3.7 Analytical Meth od Uncertainty Analytical uncertainty is based on historical QC data that is control charted and used to evaluate method accuracy and precision. The method uncertainty is calculated following ETS

- 12

- 012.2. The standard deviation is calculated for the set of accuracy results (in %) obtained for the QC samples. The expanded uncertainty is calculated by multiplying the standard deviation by a factor of 2, which corresponds to a confidence level of 95%.

Table 8 . Analytical Method Un certainty.

Analyte Calibration Method Standard Deviation (%) Method Uncertainty

PF OA External Standard 6.87 ± 14 %

PFBS External Standard 6.72 ± 13 %

PFHS External Standard 5.90 ± 12 %

PFOS External Standard 8.04 ± 16 %

PFOA Internal Standard 6.43 ±13 %

PFHS Internal Standard 7.09 ± 14 %

PFOS Internal Standard 7.37 ± 15 %



## 3.8 Field Matrix Spikes (FMS) A field matrix spike w as collected at each sampling point to verify that the analytical method is applicable to the collected matrix. Field matrix spikes are genera ted by adding a measured volume of field sample to a container spiked by the laboratory with the target analytes prior to shipping sample containers for sample collection. Field matrix spike recoveries within method acceptance criteria of 100±30% confirm that “unknown” components in the sample matrix do not significantly interfere with the extraction and analysis of the analytes of interest. The standards used for the preparation of the field matrix spiking solutions contained reference materials comprise d of both linear and branched isomers for PFOA and PFOS. Field matrix spikes are presented in section 4 of this report.

100% *
on Concentrat Spike Dup.) Sample Field & Sample Field : ion Concentrat Average FMS of ion Concentrat (Sample Recovery FMS −

=



### Table 9 . Field Matrix Spike Concentrations

.

Final Concentration (ng/mL)

Locatio n Description PFOA PFBS PFHS PFOS

ACI Field Matrix Spike 2 000 201 0 200 0 1990

ACM2 Field Matrix Spike 5.00 5.00 5.00 5.00

ACE Field Matrix Spike 5.00 5.00 5.00 5.00

WW8R, WW9R Field Matrix Spike 2510 2510 2500 2490

Trip Blank Low Field Matrix Spike 5.0 0 5.00 5.00 5.00

High Field Matrix Spike 2510 2510 2500 24903M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 12 OF 23 

# 4 Data Summary and Discussion

The tables below summarize the sample results and field m atrix spike recoveries for the five locations as well as the Trip Blank. Each table provides the average concentration and the relative percent difference ( % RPD) of the sample and sample duplicate. Results and average values are rounded to three significant figures. Percent relative difference (%RPD) values are rounded to two significant figures. Because o f rounding, values may vary slightly from those listed in the raw data. Field matrix spikes meeting the method acceptance criteria of ± 30%, demonstrate that the method is appropriate for the given matrix.

All field matrix spike samples and surrogate re covery standards met method acceptance criteria except where noted below.

DAL

- GW

- ACM2 ; the FMS sample ( 5 ng/mL) was not appropriate for PFOA, PFBS, or PFHS ; however,
t he surrogate recovery standards 13 

### C 4 

### - PFOA and 13 

### C 4 

### - PFOS met method acceptance criteria. No additional QC samples were prepared.

DAL

- GW

- ACE ; the FMS sample (5 ng/mL) was not appropriate for PFBS; however, the surrogate recovery standard 13 

### C 4 

### - PFOS, met method acceptance criteria. No additional QC samples were prepared.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 13 OF 23 

### Table 10

. DAL GW ACI 130 930 (1)

PFOA PFBS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery

ISO13

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- 08

- 001 DAL

- GW

- ACI

- 0

- 13 0930 2280 NA 349 NA

ISO13

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- 08

- 002 DAL

- GW

- ACI

- DB

- 130930 2350 NA 363 NA

ISO13

- 0 7

- 08

- 003 DAL

- GW

- ACI

- FMS

- 130930 4230 95.5 2310 97.2 Average Concentration (ng/mL) ± %RPD 232 0 ng/mL ± 3.0 % 356 ng/mL ± 3.9 %

PFHS PFOS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery

ISO13

- 07

- 08

- 001 DAL

- GW

- ACI

- 0

- 130930 1370 NA 3170 NA

ISO13

- 07

- 08

- 002 DAL

- GW

- ACI

- DB

- 130930 1420 NA 3310 NA

ISO13

- 07

- 08

- 003 DAL

- GW

- ACI

- FMS

- 130930 3700 115 4850 80.9
Average Concentration (ng/mL) ± %RPD 1400 ng/mL ± 3.6 % 3240 ng/mL ± 4.3 %

13 C 4 - PFOA 13 C 4 - PFOS

3M LIMS ID Descript ion %Recovery %Recovery

ISO13

- 07

- 08

- 001 DAL

- GW

- ACI

- 0

- 130930 94.9 94.5

ISO13

- 07

- 08

- 002 DAL

- GW

- ACI

- DB

- 130930 99.5 97.9

ISO13

- 07

- 08

- 003 DAL

- GW

- ACI

- FMS

- 130930 92.2 95.7 Average Concentration (ng/mL) ± %RSD 95.5 % ± 3.9 % 96.0 % ± 1.8 %

NA = Not Applicable (1) S a mples were analyzed by external standard calibration

. The surrogate recovery standards 13 C 4 - PFOA and 13 C 4 - PFOS were added to the samples during sample preparation.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 14 OF 23 

### Table 11

. DAL GW ACM2 130 930

PFOA ( 1 ) PFBS ( 1 )

3M LI MS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery

ISO13

- 07

- 08

- 004 DAL

- GW

- ACM2

- 0

- 130 930 1210 NA 468 NA

ISO13

- 07

- 08

- 005 DAL

- GW

- ACM2

- DB

- 130930 1220 NA 471 NA

ISO13

- 07

- 08

- 006 DAL

- GW

- ACM2

- FMS

- 130930 1160 NC 442 NC Average C oncentration (ng/mL) ± %RPD 1220 ng/mL ± 0.82 % 470 ng/mL ± 0.64 %

PFHS (1 ) PFOS ( 2 )

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery

ISO13

- 07

- 08

- 004 DAL

- GW

- ACM2

- 0

- 130930 1550 NA 1.31 NA

ISO13

- 07

- 08

- 005 DAL

- GW

- A CM2

- DB

- 130930 1570 NA 1.29 NA

ISO13

- 07

- 08

- 006 DAL

- GW

- ACM2

- FMS

- 130930 1500 NC 6.39 102
Average Concentration (ng/mL) ± %RPD 1560 ng/mL ± 1.3 % 1.30 ng/mL ± 1.5 %

13 C 4 - PFOA (1) 13 C 4 - PFOS ( 2 )

3M LIMS ID Description %Recovery %Recovery

ISO13

- 07

- 08

- 004 DA L

- GW

- ACM2

- 0

- 130930 104 114

ISO13

- 07

- 08

- 005 DAL

- GW

- ACM2

- DB

- 130930 100 106

ISO13

- 07

- 08

- 006 DAL

- GW

- ACM2

- FMS

- 130930 96.9 103 Average Concentration (ng/mL) ± % RSD 100 % ± 3.6 % 108 % ± 5.3 %

NA = Not Applicable NC = Not Calculated; Spike level was less than 0. 5x the endogenous sample concentration. (1) Samples were analyzed by external standard calibration. The surrogate recovery standards 13 C 4 - PFOA and 13 C 4 - PFOS were added to the samples during sample preparation. (2) Samples were analyzed by i nternal standard calibr ation

.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 15 OF 23 

### Table 12

. DAL GW ACE 130 930

PFOA (1) PFBS (2 )

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery

ISO13

- 07

- 08

- 007 DAL

- GW

- ACE

- 0

- 130 930 0.109 NA 1920 NA

ISO13

- 07

- 08

- 00 8 DAL

- GW

- ACE

- DB

- 130930 0.121 NA 1980 NA

ISO13

- 07

- 08

- 009 DAL

- GW

- ACE

- FMS

- 130930 4.95 96.7 1970 NC Average Concentration (ng/mL) ± %RPD 0.115 ng/mL ± 10 % 1950 ng/mL ± 3.1 %

PFHS (1) PFOS (1)

3M LIMS ID Description Concentration (ng/mL) %Recovery Concen tration (ng/mL) %Recovery

ISO13

- 07

- 08

- 007 DAL

- GW

- ACE

- 0

- 130930 0.157 NA 0.0419 NA

ISO13

- 07

- 08

- 008 DAL

- GW

- ACE

- DB

- 130930 0.154 NA 0.0485 NA

ISO13

- 07

- 08

- 009 DAL

- GW

- ACE

- FMS

- 130930 5.05 97.9 5.12 101
Average Concentration (ng/mL) ± %RPD 0.156 ng/mL ± 1.9 % 0 .0452 ng/mL ± 15 %

13 C 4 - PFOA (1) 13 C 4 - PFOS (1)

3M LIMS ID Description %Recovery %Recovery

ISO13

- 07

- 08

- 007 DAL

- GW

- ACE

- 0

- 130930 84.3 90.7

ISO13

- 07

- 08

- 008 DAL

- GW

- ACE

- DB

- 130930 94.4 99.5

ISO13

- 07

- 08

- 009 DAL

- GW

- ACE

- FMS

- 130930 95.9 105 Average Concentrat ion (ng/mL) ± %RSD 91.5 % ± 6.9 % 98.4 % ± 7.3 %

NA = Not Applicable NC = Not Calculated; Spike level was less than 0.5x the endogenous sample concentration. (1) Samples were analyzed by internal standard calibration

. (2) Samples were analyzed by external standard c alibration. The surrogate recovery standards 13 C 4 - PFOA and 13 C 4 - PFOS were added to the samples during sample preparation.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 16 OF 23 

### Table 13

. DAL GW WW8R 130 930 (1)

PFOA PFBS

3M LIMS ID Description Concentration (ng/mL) %Recovery Conce ntration (ng/mL) %Recovery

ISO13

- 07

- 08

- 010 DAL

- GW

- WW8R

- 0

- 130 930 2890 NA 309 NA

ISO13

- 07

- 08

- 011 DAL

- GW

- WW8R

- DB

- 130930 2890 NA 296 NA

ISO13

- 07

- 08

- 012 DAL

- GW

- WW8R

- FMS

- 130930 5380 99.2 2740 97.1 Average Concentration (ng/mL) ± %RPD 2890 ng/mL ± 0.0 % 303 n g/mL ± 4.3 %

PFHS PFOS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery

ISO13

- 07

- 08

- 010 DAL

- GW

- WW8R

- 0

- 130930 1360 NA 4110 NA

ISO13

- 07

- 08

- 011 DAL

- GW

- WW8R

- DB

- 130930 1370 NA 4090 NA

ISO13

- 07

- 08

- 012 DAL

- GW

- WW8R

- FM S

- 130930 3920 102 6830 110
Average Concentration (ng/mL) ± %RPD 1370 ng/mL ± 0.73 % 4100 ng/mL ± 0.49 %

13 C 4 - PFOA 13 C 4 - PFOS

3M LIMS ID Description %Recovery %Recovery

ISO13

- 07

- 08

- 010 DAL

- GW

- WW8R

- 0

- 130930 94.2 96.3

ISO13

- 07

- 08

- 011 DAL

- GW

- WW8R

- DB

- 13093 0 94.5 96.1

ISO13

- 07

- 08

- 012 DAL

- GW

- WW8R

- FMS

- 130930 94.9 91.7 Average Concentration (ng/mL) ± %RSD 94.5 % ± 0.37 % 94.7 % ± 2.7 %

NA = Not Applicable (1) Samples were analyzed by external standard calibration. The surrogate recovery standards 13 C 4 - PFOA and 13 C 4 - PFOS were added to the samples during sample preparation

.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 17 OF 23 

### Table 14

. DAL GW WW9R 130 930 (1)

PFOA PFBS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery

ISO13

- 07

- 08

- 013 DAL

- GW

- WW9 R

- 0

- 130930 2740 NA 252 NA

ISO13

- 07

- 08

- 014 DAL

- GW

- WW9R

- DB

- 130930 2720 NA 245 NA

ISO13

- 07

- 08

- 015 DAL

- GW

- WW9R

- FMS

- 130930 5410 107 2810 102 Average Concentration (ng/mL) ± %RPD 2730 ng/mL ± 0.73 % 2 49 ng/mL ± 2.8 %

PFHS PFOS

3M LIMS ID Description Concen tration (ng/mL) %Recovery Concentration (ng/mL) %Recovery

ISO13

- 07

- 08

- 013 DAL

- GW

- WW9R

- 0

- 130930 1230 NA 4130 NA

ISO13

- 07

- 08

- 014 DAL

- GW

- WW9R

- DB

- 130930 1210 NA 4270 NA

ISO13

- 07

- 08

- 015 DAL

- GW

- WW9R

- FMS

- 130930 3930 108 7200 120
Average Concentration (ng/mL ) ± %RPD 1220 ng/mL ± 1.6 % 420 0 ng/mL ± 3.3 %

13 C 4 - PFOA 13 C 4 - PFOS

3M LIMS ID Description %Recovery %Recovery

ISO13

- 07

- 08

- 013 DAL

- GW

- WW9R

- 0

- 130930 94.7 94.6

ISO13

- 07

- 08

- 014 DAL

- GW

- WW9R

- DB

- 130930 94.9 98.2

ISO13

- 07

- 08

- 015 DAL

- GW

- WW9R

- FMS

- 130930 99.1 9 5.3 Average Concentration (ng/mL) ± %RSD 96.2 % ± 2 .6 % 96.0 % ± 2.0 %

NA = Not Applicable (1) Samples were analyzed by external standard calibration. The surrogate recovery standards 13 C 4 - PFOA and 13 C 4 - PFOS were added to the samples during sample preparation

.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 18 OF 23 

### Table 15

. DAL GW WW10R 130 930 (1)

PFOA PFBS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery

ISO13

- 07

- 08

- 019 DAL

- GW

- WW10R

- 0

- 130930 2040 NA 244 NA

ISO13

- 07

- 08

- 020 DAL

- GW

- WW10R

- DB

- 130930 2090 NA 250 NA

ISO13

- 07

- 08

- 021 DAL

- GW

- WW10R

- FMS

- 130930 4570 99.6 2670 96.5 Average Concentration (ng/mL) ± %RPD 2070 ng/mL ± 2.4 % 247 ng/mL ± 2.4 %

PFHS PFOS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery

ISO13

- 07

- 08

- 019 DAL

- GW

- WW10R

- 0

- 130930 1020 NA 2760 NA

ISO13

- 07

- 08

- 020 DAL

- GW

- WW10R

- DB

- 130930 1040 NA 2780 NA

ISO13

- 07

- 08

- 021 DAL

- GW

- WW10R

- FMS

- 130930 3550 101 5350 104
Average Concentration (ng/mL) ± %RPD 1030 ng/mL ± 1.9 % 2770 ng/mL ± 0.72 %

13 C 4 - PFOA 13 C 4 - PFOS

3M LIMS ID Description %Recovery %Recovery

ISO13

- 07

- 08

- 019 DAL

- GW

- WW10R

- 0

- 130930 96.5 99.8

ISO13

- 07

- 08

- 020 DAL

- GW

- WW10R

- DB

- 130930 101 107

ISO13

- 07

- 08

- 021 DAL

- GW

- WW10R

- FMS

- 130930 96.1 99.9 Average Concentration (ng/mL) ± %RSD 97.9 % ± 2.8 % 102 % ± 4.0 %

NA = Not Applicable (1) Samples were analyzed by external standard calibration. The surrogate recovery standards 13 C 4 - PFOA and 13 C 4 - PFOS were added to the samples during sample preparation.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 19 OF 23 

### Table 16

. DAL GW WW11R 130 930 (1)

PFOA PFBS

3M LI MS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery

ISO13

- 07

- 08

- 022 DAL

- GW

- WW11R

- 0

- 130930 1700 NA 297 NA

ISO13

- 07

- 08

- 023 DAL

- GW

- WW11R

- DB

- 130930 1730 NA 301 NA

ISO13

- 07

- 08

- 024 DAL

- GW

- WW11R

- FMS

- 130930 4160 97.2 2660 94.1

A

verage Concentration (ng/mL) ± %RPD 1720 ng/mL ± 1.7 % 299 ng/mL ± 1.3 %

PFHS PFOS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recovery

ISO13

- 07

- 08

- 022 DAL

- GW

- WW11R

- 0

- 130930 1010 NA 2190 NA

ISO13

- 07

- 08

- 023 DAL

- GW

- WW 11R

- DB

- 130930 993 NA 2210 NA

ISO13

- 07

- 08

- 024 DAL

- GW

- WW11R

- FMS

- 130930 3490 99.6 4610 96.8
Average Concentration (ng/mL) ± %RPD 1000 ng/mL ± 1.7 % 220 0 ng/mL ± 0.91 %

13 C 4 - PFOA 13 C 4 - PFOS

3M LIMS ID Description %Recovery %Recovery

ISO13

- 07

- 08

- 022 DAL

- GW

- WW11R

- 0

- 130930 100 104

ISO13

- 07

- 08

- 023 DAL

- GW

- WW11R

- DB

- 130930 101 104

ISO13

- 07

- 08

- 024 DAL

- GW

- WW11R

- FMS

- 130930 96.3 96.8 Average Concentration (ng/mL) ± %RSD 99.1 % ± 2.5 % 102 % ± 4 .1 %

NA = Not Applicable (1) Samples were analyzed by external standard calib ration. The surrogate recovery standards 13 C 4 - PFOA and 13 C 4 - PFOS were added to the samples during sample preparation.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 20 OF 23 

### Table 17 . Trip Blank Results

PFOA PFBS

3M LIMS ID Description Concentration (ng/mL) %Recovery Concentration (ng/mL) %Recov ery

ISO13

- 07

- 08

- 016 DAL

- GW

- TRIP01

- 0

- 130930 <0.0240 (1) NA <0.20 0 (2 ) NA

ISO13

- 07

- 08

- 017 DAL

- GW

- TRIP01

- LS

- 130930 5.04 (2 ) 101 5.06 (2 ) 101

ISO13

- 07

- 08

- 018 DAL

- GW

- TRIP01

- HS

- 130930 2870 (2) 114 2690 (2) 107

PFHS PFOS

3M LIMS ID Description Concentrati on (ng/mL) %Recovery Concentration (ng/mL) %Recovery

ISO13

- 07

- 08

- 016 DAL

- GW

- TRIP01

- 0

- 130930 <0.400 (1) NA <0.0232 (1) NA

ISO13

- 07

- 08

- 017 DAL

- GW

- TRIP01

- LS

- 130930 5.17 (2 ) 103 5.40 (2 ) 108

ISO13

- 07

- 08

- 018 DAL

- GW

- TRIP01

- HS

- 130930 2740 (2) 110 2900 (2) 116

13 C 4 - PFOA 13 C 4 - PFOS

3M LIMS ID Description %Recovery %Recovery

ISO13

- 07

- 08

- 016 DAL

- GW

- TRIP01

- 0

- 130930 94.2 (1) 105 (1)

ISO13

- 07

- 08

- 017 DAL

- GW

- TRIP01

- LS

- 130930 102 (2 ) 108 (2 )

ISO13

- 07

- 08

- 018 DAL

- GW

- TRIP01

- HS

- 130930 101 (2) 105 (2 )

NA = Not Ap plicable (1) Samples were analyzed by internal standard calibration. (2) Sample s w ere analyzed by exte rnal standard calibration

. The surrogate recovery standards 13 C 4 - PFOA and 13 C 4 - PFOS were added to the samples during sample preparation.3 M ENVIRONMENTA L LABORATOR Y REPOR T NO

. /S O ^

3-07-0 8



# 5 Conclusio n

Laborator y contro l spike s wer e use d t o determin e th e analytica l metho d accurac y an d precisio n fo r al l analytes

. Th e accurac

y an d precisio n wer e the n use d t o estimat e th e metho d uncertaint y fo r th e results

. Fiel d matri x spik e recoverie s demonstrate d tha t th e analytica l metho d wa s appropriat e fo r th e give n sampl e matrix

. Analysi s wa s complete d usin g 3 M Environmenta l Laborator y Metho d ETS-8

- 044. 1 "Metho d o f Analysi s fo r th e Determinatio n o f Periluorinate d Compound s i n Wate r b y LC/MS/MS ; Direc t Injectio n Analysis"

. Analytica l result s ar e reporte d i n Tabl e 1 an d 10-1 7 o f thi s report

.



# 6 Dat a /

Sampl e Retentio n

Al l remainin g sampl e an d associate d projec t dat a (hardcop y an d electronic ) wil l b e archive d accordin g t o 3 M Environmenta l Laborator y standar d operatin g procedures

.



# 7 Attachment s

Attachmen t A : Analyt e Tren d Dat a fo r selec t samplin g point s a t th e Decatu r Groun d Wate r Treatmen t Plan t (GWTP ) GA C System

.



# 8 Signature s



# llh/lS

Susa n T

. Wolf

, 3IV(P,cincipa l Analytica l Investigato r Dat e

Willia m K

. Reagen

, Ph.D.

, 3 M Environmenta l Laborator y Technica l Directo r Dat e

Th e 3 M Environmenta l Laboratory' s Quality Assuranc e Uni t ha s audite d th e dat a an d repor t fo r thi s project

.

Quality Assuranc e R^r^entativ e Dat e

This test report shall not be reproduced

except in full, without

written approval

of the 3M Environmental

Laboratory.

PAG E 2 1 O F 2 33M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

- 07

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PAGE 22 OF 23 

### Attachment A : Analyte Trend Data for select sampling points at the Decatur Ground Water Treatment Plant (GWTP) GAC System

ACI (Activated Carbon Influent)

- Sample Results in ng/mL

ACI 6/29/ 12 8 /28/ 12 12/14/ 12 1/17/ 13 2/13/ 13 3/27/ 13 4/29/ 13 5/31/ 13 6/27/ 13 7/23/ 13 9/30/13

PFOA 1650 1410 2580 1910 2300 2220 1480 1860 1480 1630 2320

PFBS 1410 1830 723 588 830 1060 1360 1040 708 1230 356

PFHS 1460 1390 1380 895 1580 1090 777 940 942 749 1400

PF OS 964 172 2810 1810 2940 2490 1670 2150 1590 1680 3240



### AC E (Activated Carbon Ef fluent)

- Sample Results in ng/mL

ACE 8/28/ 12 12/14/ 12 1/17/ 13 2/13/ 13 3/27/ 13 4/29/ 13 5/31/ 13 6/27/ 13 7/23/ 13 9/30/13

PFOA 0.387 0.102 <0.0240 0.124 0.0380 0.0422 0.072 5 0.0717 0.0643 0.115

PFBS 0.256 <0.0250 <0.0250 0.0360 <0.0250 0.392 24.8 111 1960 1950

PFHS 0.552 0.117 <0.0250 0.178 0.0477 0.057 0.105 0.118 0.0778 0.156

PFOS 0.103 0.0376 <0.0232 0.0329 <0.0232 <0.0232 <0.0232 <0.0232 0.0277 0.0452

The ACE locati on was not sampled on 6/29/12.3M ENVIRONMENTAL LAB ORATORY REPORT NO. ISO13

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PAGE 23 OF 23 

### Attachment A : Analyte Trend Data for select sampling points at the Decatur Ground Water Treatment Plant (GWTP) GAC System

WW8R

- Sample Results in ng/mL

WW8R 12/13/ 12 1/17/ 13 2/13/ 13 3/27/ 13 4/29/ 13 5/31/ 13 6/27/ 13 7/2 3/ 13 9/30/13

PFOA 3630 4350 3250 3640 3190 2760 2760 2640 2890

PFBS 441 410 354 385 364 289 282 263 303

PFHS 1740 1930 1900 1760 1610 1330 1340 1260 1370

PFOS 4920 5710 4850 5120 4830 4180 4110 3910 4100



### WW9R

- Sample Results in ng/mL

WW9R 12/13/ 12 1/17/ 13 2/13/13 3/27/ 13 4/29/ 13 5/31/ 13 6/27/ 13 7/23/ 13 9/30/13

PFOA 3360 2710 2850 3330 2650 2660 2630 2410 2730

PFBS 321 184 236 278 244 226 225 212 249

PFHS 1480 954 1400 1440 1200 1120 1140 1030 1220

PFOS 4080 3690 4100 4660 4340 4210 4150 3670 4200