3M ENVIRONMENTAL LAB ORATORY

REPORT NO. ISO14

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PAGE 1 OF 24 

# Final Report

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

3M Decatur, Alabama : Groundwater Treatment Plant GAC System

– February 2014

Laboratory Request Number: ISO14

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- 02

Method Re quirement: 3M Method ETS

- 8

- 044.1

Report Date

– Date of Last Signature



## Testing Laboratory

3M EHS 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

“Gener al 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 GLP s (40 CFR 792) by an independent A2LA assessment.3M ENVIRONMENTAL LAB ORATORY

REPORT NO. ISO14

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PAGE 2 OF 24 

### 3M Envir onmental Laboratory

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

. 3M Principal Analytical Investigator: Susan Wolf Report Author: Susanna Emond



## Analytical Report ISO14

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3M Decatur Groundwater Treatment Plant System; Febru ary 2014 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 So lutions personnel

on February 27

, 2014 . 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 laborato ry project number ISO14

- 07

- 02

. Analysis of the samples was completed as specified under 3M Environmental Laboratory General Project Outline (GPO) number GPO1 3

- 1 289

.

T he 3M Environmental Laboratory provided sample containers for seven sampling locations; 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. Containe rs 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

samp le and low spike

, were fortified with i nternal standards and surrogate recovery standard 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 Perfl uorinated Compounds in Water by LC/MS/MS; Direct Injection Analysis ”. I nternal

standards were used for select samples to aid in the data quality objectives.

Table 1 summarizes the sample results using the analytical method identified above. All result s for quality control samples 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 Requirements for the Competence of Testing and Calibration Laboratories”, in accordance with the A2LA Testing Certificate # 2052.01. Ad ditionally, 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

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PAGE 3 OF 24 

### Table 1 . Sample Results Summary (1)

3M LIMS ID Sample Description PFOA

Concentration (ng/mL) PFB S

Concentration (ng/mL) PFHS

Concentration (ng/mL) PFOS

Concentration (ng/mL)

ISO14

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- 02

- 001 DAL

- GW

- ACI

- 0

- 140227 1860 1470 722 1830

ISO14

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- 02

- 002 DAL

- GW

- ACI

- DB

- 140227 1880 1470 751 1760

Average 1870 1470 737 1 800

%RPD Sample/Sample Dup 1.1 0.0 3.9 3.9

ISO14

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- 02

- 004 DAL

- GW

- ACM2

- 0

- 140227 0.182 1250 0.0835 0.676

ISO14

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- 02

- 005 DAL

- GW

- ACM2

- DB

- 140227 0.173 1150 0.0821 0.709

Average 0.178 (2) 1200 0.0828 (2) 0.693 (2)

%RPD Sample/Sample Dup 5.1 8.3 1.7 4.8

ISO14

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- 007 DAL

- GW

- ACE

- 0

- (100x) 0.129 0.0342 0.0637 0.0970

ISO14

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- 008 DAL

- GW

- ACE

- DB

- (100x) 0.147 0.0377 0.0774 0.0962

Average 0.138 (2) 0.0360 (2) 0.0706 (2) 0.0966 (2)

%RPD Sample/Sample Dup 13 10 19 0.83

ISO14

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- 010 DAL

- GW

- WW8R

- 0

- 140227 2540 326 1350 4130

ISO1 4

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- 011 DAL

- GW

- WW8R

- DB

- 140227 2580 336 1380 4210

Average 2560 331 1370 4170

%RPD Sample/Sample Dup 1.6 3.0 2.2 1.9

ISO14

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- 013 DAL

- GW

- WW9R

- 0

- 140227 2640 265 1390 4580

ISO14

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- 014 DAL

- GW

- WW9R

- DB

- 140227 2620 274 1340 4730

Average 26 30 270 1370 4 660

%RPD Sample/Sample Dup 0.76 3.3 3.7 3.2

ISO14

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- 016 DAL

- GW

- WW10R

- 0

- 140227 1820 264 919 2840

ISO14

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- 017 DAL

- GW

- WW10R

- 140227 1740 256 950 2880

Average 1780 260 935 2860

%RPD Sample/Sample Dup 4.5 3.1 3.3 1.4

ISO14

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- 019 DAL

- GW

- WW11R

- 0

- 140227 1220 251 683 1850

ISO14

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- 020 DAL

- GW

- WW11R

- DB

- 140227 1370 272 709 2340

Average 1300 262 696 2100

%RPD Sample/Sample Dup 12 8.0 3.7 23 (3)

NA = Not Applicable (1) Reported results were prepared and analyzed by ETS

- 8

- 044

. 1 using external standard calibration . The analytical method uncertainties associated with the reported results are as follows: PFOA ±1 5 %, PFBS ± 1 0 %, PFHS ±1 4 %, and PFOS ± 14 %. (2) Reported results were prepared and analyzed by ETS

- 8

- 044.1 using internal stan dard calibration. The analytical method uncertainties associated with the reported results are as follows: PFOA ± 1 5 %, PFBS ± 9 .5 %, PFHS ± 9 .9 %, and PFOS ± 1 2 %. (3) Sample set did not meet sample / sample duplicate RPD acceptance criteria of ≤ 20%.3M ENVIRONMENTAL LAB ORATORY

REPORT NO. ISO14

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PAGE 4 OF 24 

# 2 Methods

- Analytical and Preparatory

2.1 Methods

Analysis was comple ted using 3M Environmental Laboratory Method ETS

- 8

- 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 Structure

Perfluorooctanoic Acid (C8 Acid) PFOA Linear + Branched

Perfluorobutanesulfonate (C4 Sulfonate ) PFBS Linear

Perfluorohexanesulfonate (C6 Sulfonate) PFHS Linear

Perfluor ooctanesulfonate (C8 Sulfonate) PFOS Linear + Branched



## 2.2 Sample Collection
Samples were collected on February 27

, 2014 in Nalgene TM 

### (high

- density polyethylene) bottles prepared at the 3M Environmental Laboratory. Prior to sample collection, bottles design ated 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 sp ike, were fortified with a mixture of mass

- labeled

internal standards at a nom inal concentration of 1 ng/mL and a mixture of surrogate recovery standards at a nominal concentration of 0.1 ng/mL prior to being sent to the field for sample collection

. Colle cted sample bottles were received by the laboratory at ambient conditions on March 5

, 2014

.



## 2.3 Sample Preparation

All s ample s were initially prepared by diluting with methanol (dilution factor of 100) and analyzing for all target analytes

. The 1:100 dilutio ns 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 solution (nominal concentration of 1 ng/mL)

. Prepared samples were analyzed by external standard calibration.

The ACE and ACM2 sample set s and the Trip Blank sample and low spike were subsequently prepared by removing a 0.4 mL aliquot of the well mixed sample and diluting it with 0.4 mL of methanol ( dilution factor of 2). Prepared samples were analyzed by internal stand ard 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 (nomi nal concentration of 1 ng/mL). Th e laboratory control samples were 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). Pe rtinent instrument parameters, the liquid chromatography gradient program, and the specific mass transitions analyzed are described

in the tables below.

Due to the nature of the sample, the wide range of concentrations found in the sample, and the

environ mental occurrence of multiple isomers 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

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REPORT NO. ISO14

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PAGE 5 OF 24 

### through the training of laboratory personnel, the peer review process required for all manual integrations , the review of manual integrations by the QAU, and where necessary the review of manual integrations by laboratory management.

Table 3 . Instrument Parameters.

Instrument Name ETS Buster ETS Kirk

Analysis Dates 3/06/14

– external standard calibration 3/13/14

– internal standard calibration

Analytical Method ETS

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- 044.1 ETS

- 8

- 044.1

Liquid Chromatograph Agilent 1100 Agilent 1260

Guard column Betasil C18 (4.6 mm X 100 mm), 5 μ Betasil C18 (4.6 mm X 100 mm), 5 μ
Analytical column B etasil C18 (4.6 mm X 100 mm), 5 μ Betasil C18 (4.6 mm X 100 mm), 5 μ
Injection Volume 10 μ L 10 μ L

Mass Spectrometer Applied Biosystems API 4000 Applied Biosystems API 5500

Ion Source Turbo Spray Turbo Spray

Polarity Negative Negative

Software Analyst 1.6.1 Analyst 1.6.1



### Table 4 . Liquid Chromatography 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 7 0.0 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

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PAGE 6 OF 24 

### Table 5 . Mass Transitions

.

Analyte Mass Transition

Q1/Q3 Interna l Standard (1) Mass Transition
Q1/Q3

PFOA 413/369

[ 13 C 8 ] PFOA 421/376 413/219

413/169

PFBS 299/80 [ 1 8 O 2 ]PFB S 303/84 299/99

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

PFOS 499/99

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

499/130

[ 13 C 4 ]PFOA surrogate 41 7/372 [ 13 C 8 ]PFOA 421/376

[ 13 C 4 ]PFOS surrogate 503/80 [ 13 C 8 ]PFOS 507/80

Dwell time was between 20 and 5 0 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 on 3/13 /14

. 

# 3 Data Analysis

3.1 Calibration
External Standard Calibration Analysis on 3/06 /14 : Samples were analyzed against an external

standard calibration curve. Calibration standards were prepared by spiking known amounts 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. 1 ng/mL to 1 50 ng/mL (nominal) were analyzed. The standards also contained the surrogates at concentrations ranging from 0. 1 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. Calc ulating the standard concentrations using the peak area counts and the resultant calibration curve confirmed accuracy of each curve point.

Internal Standard Calibration Analysis on 3/13 /14 : Samples were analyzed for all analytes against a

matrix

- matche d stable isotope internal standard calibration curve. Calibration standards were prepared by spiking known amounts of stock solutions into 50 mL of 50:50 methanol :laboratory reagent water.

The calibration standards contained an internal standard mix at a nominal concentration of 0.5 ng/mL.

A total of thirteen c alibration standards ranging from 0.0125 ng/mL to 5 0 ng/mL (nominal) were analyzed (0.0125 ng/mL to 10 ng/mL (nominal) for the SRSs). Low or high points may have been

disabled to meet method crite ria. 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. Calc ulating 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

standards consi sted 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 analyte s. The correlation coefficient r was greater than 0.995 for all analytes

.3M ENVIRONMENTAL LAB ORATORY

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PAGE 7 OF 24 

## 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 criteria for s ystem 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 with the exception of the peak

area count RSD for PF H S analyzed on 3/06/14 ( 10 %)

. A method deviation is included with the raw

data.



## 3.3 Limit of Quantitation (LOQ)

The LOQ as defined in method ETS

- 8

- 044. 1 is the lowest non

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

.

T able 6 . LOQ

Analyte LOQ, ng/mL

3/06 /14 Analysis (1) LOQ, ng/mL

3/13 /14 Analysis (2)

PFOA 9.58 0.0240

PFBS 10.0 0.0250

PFHS 10.0 0.0250

PFOS 9.27 0.0232
(1) The dilution factor of 100 was applied to the LOQ. (2) The dilution factor of 2 was applied to the LOQ.



## 3.4 Continuing Calibration
During the course of the analytical sequenc e, 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 samples: 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 the 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 o f 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 criteria with the following exception:

3/06/14 Analysis: Th e high level LCSs for PFOS

- Surrogate had an average recovery of 125%

. A

method deviation is included with the raw data.

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

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PAGE 8 OF 24 

### Table 7 . Lab Control Spike Results.

ETS

- 8

- 044. 1

Ex

ternal Standard Calibration

Analyzed 3/06 /14 PFOA (Linear + Branched ) 13 C 4 - PFO A surrogate

Lab ID Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) %Recovery Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) %Recovery

L CS

- 140306

- 1 0.958 0.926 96.6 0.998 1.06 106

LCS

- 140306

- 2 0.958 0.844 88.1 0.998 1.08 108

LCS

- 140306

- 3 0.958 0.880 91.8 0.998 1.08 108

Average ± %RSD 92.2 % ± 4.6 % 107 % ± 1.1 %

LCS

- 140306

- 4 9.58 10.10 106 9.98 11.3 113

LCS

- 140306

- 5 9.58 9.61 100 9.98 11. 8 118

LCS

- 140306

- 6 9.58 10.20 106 9.98 11.2 112

Average ± %RSD 104 % ± 3.3 % 114 % ± 2.8 %

LCS

- 140306

- 7 38.2 38.6 101

LCS

- 140306

- 8 38.2 38.5 101

LCS

- 140306

- 9 38.2 37.6 98.5

Average ± %RSD 100 % ± 1.4 %

ETS

- 8

- 044.1

External Standard Calibration

Analyzed 3/06 /14 PFBS PFHS

Lab ID Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) %Recovery Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) %Recovery

LCS

- 140306

- 1 1.00 1.05 105 1.00 1.06 106

LCS

- 140306

- 2 1.00 0.95 95. 0 1.00 1.05 105

LCS

- 140306

- 3 1.00 1.06 106 1.00 1.09 109

Average ± %RSD 102 % ± 6.0 % 107 % ± 2.0 %

LCS

- 140306

- 4 10.0 10.8 108 10.0 11.4 114

LCS

- 140306

- 5 10.0 11.2 112 10.0 11.2 112

LCS

- 140306

- 6 10.0 10.9 109 10.0 11.3 113

Average ± %RSD 110 % ± 1.9 % 113 % ± 0.88 %

LCS

- 140306

- 7 39.8 41.8 105 39.8 43.6 110

LCS

- 140306

- 8 39 .8 42.3 106 39.8 42.5 107

LCS

- 140306

- 9 39.8 40.9 103 39.8 42.5 107

Average ± %RSD 105 % ± 1.5 % 108 % ± 1.6 %

(1) LCS recovery did not meet acceptance criteria of 100 ± 20%.3M ENVIRONMENTAL LAB ORATORY

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PAGE 9 OF 24 

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

ETS

- 8

- 044.1

External Standard Calibration

Analyzed 3/06 /14 PFOS (Linear + Branched) 13 C 4 - PFO S surrogate

Lab ID Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) %Recovery Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) %Recovery

LCS

- 140306

- 1 0.927 0. 928 100 0.956 1.07 112

LCS

- 140306

- 2 0.927 0.942 102 0.956 1.07 112

LCS

- 140306

- 3 0.927 0.911 98.2 0.956 1.08 113

Average ± %RSD 100 % ± 1.9 % 112 % ± 0.51 %

LCS

- 140306

- 4 9.27 9.97 108 9.56 11.9 125

LCS

- 140306

- 5 9.27 9.71 105 9.56 12.0 126

LCS

- 140306

- 6 9.27 10.1 109 9.56 11.7 123

Average ± %RSD 107 % ± 1 .9% 125 % ± 1.2 % (1)

LCS

- 140306

- 7 36.9 38.2 103

LCS

- 140306

- 8 36.9 39.4 107

LCS

- 140306

- 9 36.9 38.1 103

Average ± %RSD 104 % ± 2 .2%

ETS

- 8

- 044.1

In ternal Standard Calibration

Analyzed 3/13 /14 PFOA (Linear + Branched) 13 C 4 - PFO A surrogate

Lab ID Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) %Recover y Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) %Recovery

LCS

- 140313

- 1 0.190 0.202 106 0.198 0.204 103

LCS

- 140313

- 2 0.190 0.208 110 0.198 0.211 106

LCS

- 140313

- 3 0.190 0.208 109 0.198 0.230 116

Average ± %RSD 108 % ± 1.9 % 10 8 % ± 6.3 %

LCS

- 140313

- 4 9.50 10.5 110 1.98 2.21 111

LCS

- 140313

- 5 9.50 10.2 108 1.98 2.33 118

LCS

- 140313

- 6 9.50 10.8 113 1.98 2.50 126

Average ± %RSD 110 % ± 2.3 % 118 % ± 6.3 %

LCS

- 140313

- 7 38.0 45.0 118

LCS

- 140313

- 8 38.0 42.8 113

LCS

- 140313

- 9 38.0 44.8 118

Average ± %RSD 116 % ± 2.5 %

(1) LCS recovery did not meet acceptance criteria of 100 ± 20%.3M ENVIRONMENTAL LAB ORATORY

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PAGE 10 OF 24 

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

ETS

- 8

- 044.1

Internal Standard Calibration

Analyzed 3/13/14 PFBS PFHS

Lab ID Spiked

Concentration (ng/mL) Calcu lated

Concentration (ng/mL) %Recovery Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) %Recovery

LCS

- 140313

- 1 0.198 0.190 95.9 0.198 0.226 114

LCS

- 140313

- 2 0.198 0.199 101 0.198 0.220 111

LCS

- 140313

- 3 0.198 0.202 102 0.198 0.223 113

Average ± %RSD 99.6 % ± 3.3 % 113 % ± 1.4 %

LCS

- 140313

- 4 9.92 10.0 101 9.92 11.1 112

LCS

- 140313

- 5 9.92 10.3 104 9.92 10.9 110

LCS

- 140313

- 6 9.92 10.4 105 9.92 11.0 111

Average ± %RSD 10 3 % ± 2.0 % 111 % ± 0.90 %

LCS

- 140313

- 7 39.6 44.1 111 39.6 45.9 116

LCS

- 140313

- 8 3 9.6 41.4 105 39.6 43.1 109

LCS

- 140313

- 9 39.6 42.2 107 39.6 45.8 116

Average ± %RSD 108 % ± 2.8 % 114 % ± 3.6 %

ETS

- 8

- 044.1

Internal Standard Calibration

Analyzed 3/13/14 PFOS (Linear + Branched) 13 C 4 - PFO S surrogate

Lab ID Spiked

Concentration (ng/mL) Ca lculated

Concentration (ng/mL) %Recovery Spiked

Concentration (ng/mL) Calculated

Concentration (ng/mL) %Recovery

LCS

- 140313

- 1 0.184 0.197 107 0.189 0.184 97.5

LCS

- 140313

- 2 0.184 0.222 121 0.189 0.196 104

LCS

- 140313

- 3 0.184 0.221 120 0.189 0.206 10 9

Average ± %RSD 116 % ± 6.7 % 104 % ± 5.6 %

LCS

- 140313

- 4 9.20 9.87 107 1.90 2.10 110

LCS

- 140313

- 5 9.20 10.1 109 1.90 2.34 123

LCS

- 140313

- 6 9.20 10.1 110 1.90 2.32 122

Average ± %RSD 109 % ± 1.4 % 118 % ± 6.1 %

LCS

- 140313

- 7 36.7 43.2 118

LCS

- 140313

- 8 36.7 40.2 110

LCS

- 140313

- 9 36.7 41.6 113

Average ± %RSD 114 % ± 3.6 %

(1) LCS recovery did not meet acceptance criteria of 100 ± 20%.3M ENVIRONMENTAL LAB ORATORY

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PAGE 11 OF 24 

## 3.7 Analytical Method Uncertainty
Analytical uncertainty is based on historical QC data that is control charted and used to ev aluate 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 multipl ying the standard deviation by a factor of 2, which corresponds to a confidence level of 95%.

Table 8 . Analytical Method Uncertainty.

Analyte Calibration Method Standard Deviation (%) Method Uncertainty

PF OA External Standard 7 .73 ± 15 %

PFBS External Standard 5.0 7 ± 10 %

PFHS External Standard 7.04 ± 14 %

PFOS External Standard 6.88 ± 14 %

PFOA Internal Standard 7.42 ±1 5 %

PFBS Internal Standard 4.73 ± 9.5 %

PFHS Internal Standard 4.95 ± 9.9 %

PFOS Internal Standard 5.81 ± 12 %



## 3.8 Fiel d 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 generated 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 i nterfere 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 comprised of both linear and branched

isomers for PFOA and PFOS. Field matri x 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)

Location Description PFOA PFBS PFHS PFOS

ACI Field Matrix Spike 1980 2000 2 000 2000

ACM2 , ACE Field Matrix Spike 4.96 5.00 5.00 4.99

WW8R, WW9R Field Matrix Spike 2480 2500 2510 2500

WW10R, WW11R Field Matrix Spike 1980 2000 2000 2000

Trip Blank Low Field Matrix Spike 4.96 5.00 5.00 4.99

High Field Matrix Spike 2480 2500 25 10 25003M ENVIRONMENTAL LAB ORATORY

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PAGE 12 OF 24 

# 4 Data Summary and Discussion

The tables below summarize the sample results and field m atrix spike recoveries for the seven locations as well as the Trip Blank. Each table provides the average concentration and the relative percent difference ( % RP D) of the sample and sample duplicate. Results and average values are rounded to three significant figures. Relative percent difference (%RPD) values are rounded to two significant figures. Because of 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 sample s met method acceptance criteria except where noted below.

DAL

- GW

- ACM2 : the FMS spik e level at 5 ng/mL was not appropriate for PFBS ; however, t he surrogate recovery standard 13 

### C 4 

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

DAL

- GW

- WW11R : sample / sample duplicate %RPD was 23% for PFOS

.3M ENVIRONMENTAL LAB ORATORY

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PAGE 13 OF 24 

### Table 10

. DAL GW ACI 140 227 (1)

PFOA PFBS

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

ISO14

- 07

- 02

- 001 DAL

- GW

- ACI

- 0

- 140227 1860 NA 1470 NA

ISO14

- 07

- 02

- 002 DAL

- GW

- ACI

- DB

- 140227 1880 NA 1470 NA

ISO14

- 07

- 02

- 003 DAL

- GW

- ACI

- FMS

- 140227 3610 87.7 3340 93.5

Average Concentration (ng/mL) ± %RPD 1870 ng/mL ± 1.1 % 1470 ng/mL ± 0.0 %

PFHS PFOS

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

ISO14

- 07

- 02

- 001 DAL

- GW

- ACI

- 0

- 140227 722 NA 1830 NA

ISO14

- 07

- 02

- 002 DAL

- GW

- ACI

- DB

- 140227 751 NA 1760 NA

ISO14

- 07

- 02

- 003 DAL

- GW

- ACI

- FMS

- 140227 2890 107 3780 99.4

Average Concentration (ng/mL) ± %RPD 737 ng/mL ± 3.9 % 1800 ng/mL ± 3 .9 %

13 C 4 - PFOA 13 C 4 - PFOS

3M LIMS ID Sample Description %Recovery %Recovery

ISO14

- 07

- 02

- 001 DAL

- GW

- ACI

- 0

- 140227 110 110

ISO14

- 07

- 02

- 002 DAL

- GW

- ACI

- DB

- 140227 97.6 112

ISO14

- 07

- 02

- 003 DAL

- GW

- ACI

- FMS

- 140227 102 105

Average Concentration (ng/mL) ± %RSD 103 % ± 6.2 % 109 % ± 3.5 %

NA = Not Applicable (1) S amples 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. ISO14

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PAGE 14 OF 24 

### Table 11

. DAL GW ACM2 14022 7

PFOA ( 1 ) PFBS ( 2 )

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

ISO14

- 07

- 02

- 004 DAL

- GW

- ACM2

- 0

- 140227 0.182 NA 1250 NA

ISO14

- 07

- 02

- 005 DAL

- GW

- ACM2

- DB

- 140227 0.173 NA 1150 NA

ISO14

- 07

- 02

- 006 DAL

- G W

- ACM2

- FMS

- 140227 5.84 114 1240 NC

Average Concentration (ng/mL) ± %RPD 0 .178 ng/mL ± 5.1 % 1200 ng/mL ± 8.3 %

PFHS (1 ) PFOS ( 1 )

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

ISO14

- 07

- 02

- 004 DAL

- GW

- A CM2

- 0

- 140227 0.0835 NA 0.676 NA

ISO14

- 07

- 02

- 005 DAL

- GW

- ACM2

- DB

- 140227 0.0821 NA 0.709 NA

ISO14

- 07

- 02

- 006 DAL

- GW

- ACM2

- FMS

- 140227 5.77 114 6.28 112

Average Concentration (ng/mL) ± %RPD 0.0828 ng/mL ± 1.7 % 0.693 ng/mL ± 4 .8 %

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

3M LIMS ID Sample Description %Recovery %Recovery %Recovery

ISO14

- 07

- 02

- 004 DAL

- GW

- ACM2

- 0

- 140227 98.5 100 115

ISO14

- 07

- 02

- 005 DAL

- GW

- ACM2

- DB

- 140227 93.3 98.5 113

ISO14

- 07

- 02

- 006 DAL

- GW

- ACM2

- FMS

- 140227 92.3 95.3 109

Average C oncentration (ng/mL) ± % RSD 94.7 % ± 3.5 % 98.0 % ± 2.5 % 112 % ± 2.8 %

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 b y external standard calibration. The surrogate recovery standard 13 C 4 - PFOS was added to the
samples during sample preparation.3M ENVIRONMENTAL LAB ORATORY

REPORT NO. ISO14

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PAGE 15 OF 24 

### Table 12 . DAL GW ACE 140227 (1)

PFOA PFBS

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

ISO14

- 07

- 02

- 007 DAL

- GW

- ACE

- 0

- 140227 0.129 NA 0.0342 NA

ISO14

- 07

- 02

- 008 DAL

- GW

- ACE

- DB

- 140227 0.147 NA 0.0377 NA

ISO14

- 07

- 02

- 009 DAL

- GW

- ACE

- FMS

- 140227 5.76 113 5.17 103

Average Concentration (ng/mL) ± %RPD 0. 138 ng/mL ± 13 % 0. 0360 ng/mL ± 9.7 %

PFHS PFOS

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

ISO14

- 07

- 02

- 007 DAL

- GW

- ACE

- 0

- 140227 0.0637 NA 0.0970 NA

ISO14

- 07

- 02

- 008 DAL

- GW

- ACE

- DB

- 140227 0.0774 NA 0.0962 NA

ISO14

- 07

- 02

- 009 DAL

- GW

- ACE

- FMS

- 140227 5.54 109 5.76 113

Average Concentration (ng/mL) ± %RPD 0.0706 ng/mL ± 19 % 0.0966 ng/mL ± 0.83 %

13 C 4 - PFOA 13 C 4 - PFOS

3M LIMS ID Sample Description %Recovery %Recovery

ISO14

- 07

- 02

- 007 DAL

- GW

- ACE

- 0

- 14 0227 95.1 96.2

ISO14

- 07

- 02

- 008 DAL

- GW

- ACE

- DB

- 140227 91.6 89.3

ISO14

- 07

- 02

- 009 DAL

- GW

- ACE

- FMS

- 140227 91.4 94.7

Average Concentration (ng/mL) ± %RSD 92.7 % ± 2.2 % 93.4 % ± 3.9 %

NA = Not Applicable (1) Samples were analyzed by internal standard calibration

.3M ENVIRONMENTAL LAB ORATORY

REPORT NO. ISO14

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PAGE 16 OF 24 

### Table 13

. DAL GW WW8R 140227 (1)

PFOA PFBS

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

ISO14

- 07

- 02

- 010 DAL

- GW

- WW8R

- 0

- 140227 2540 NA 326 NA

ISO14

- 07

- 02

- 011 DAL

- GW

- WW8R

- D B

- 140227 2580 NA 336 NA

ISO14

- 07

- 02

- 012 DAL

- GW

- WW8R

- FMS

- 140227 5000 98.4 2890 102

Average Concentration (ng/mL) ± %RPD 25 60 ng/mL ± 1.6 % 331 ng/mL ± 3.0 %

PFHS PFOS

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

ISO14

- 07

- 02

- 010 DAL

- GW

- WW8R

- 0

- 140227 1350 NA 4130 NA

ISO14

- 07

- 02

- 011 DAL

- GW

- WW8R

- DB

- 140227 1380 NA 4210 NA

ISO14

- 07

- 02

- 012 DAL

- GW

- WW8R

- FMS

- 140227 4060 108 6790 105

Average Concentration (ng/mL) ± %RPD 1370 ng/mL ± 2.2 % 4170 ng/mL ± 1.9 %

13 C 4 - PFOA 13 C 4 - PFOS

3M LIMS ID Sample Description %Recovery %Recovery

ISO14

- 07

- 02

- 010 DAL

- GW

- WW8R

- 0

- 140227 95.6 99.0

ISO14

- 07

- 02

- 011 DAL

- GW

- WW8R

- DB

- 140227 101 119

ISO14

- 07

- 02

- 012 DAL

- GW

- WW8R

- FMS

- 140227 94.7 108

Average Concentration (n g/mL) ± %RSD 97.2 % ± 3.6 % 10 9 % ± 9.4 %

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

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PAGE 17 OF 24 

### Table 14

. DAL GW WW9R 140227 (1)

PFOA PFBS

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

ISO14

- 07

- 02

- 013 DAL

- GW

- WW9R

- 0

- 140227 2640 NA 265 NA

ISO14

- 07

- 02

- 014 DAL

- GW

- WW9R

- DB

- 140227 2620 NA 274 NA

ISO1 4

- 07

- 02

- 015 DAL

- GW

- WW9R

- FMS

- 140227 4830 88.7 2740 98.8

Average Concentration (ng/mL) ± %RPD 2 630 ng/mL ± 0.76 % 270 ng/mL ± 3.3 %

PFHS PFOS

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

ISO14

- 07

- 02

- 0 13 DAL

- GW

- WW9R

- 0

- 140227 1390 NA 4580 NA

ISO14

- 07

- 02

- 014 DAL

- GW

- WW9R

- DB

- 140227 1340 NA 4730 NA

ISO14

- 07

- 02

- 015 DAL

- GW

- WW9R

- FMS

- 140227 3840 98.8 6920 90.8

Average Concentration (ng/mL) ± %RPD 1370 ng/mL ± 3.7 % 4660 ng/mL ± 3.2 %

13 C 4 - PFOA 13 C 4 - PF OS

3M LIMS ID Sample Description %Recovery %Recovery

ISO14

- 07

- 02

- 013 DAL

- GW

- WW9R

- 0

- 140227 101 109

ISO14

- 07

- 02

- 014 DAL

- GW

- WW9R

- DB

- 140227 98.3 109

ISO14

- 07

- 02

- 015 DAL

- GW

- WW9R

- FMS

- 140227 97.6 107

Average Concentration (ng/mL) ± %RSD 99.0 % ± 1.9 % 10 8 % ± 1.1 %

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

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PAGE 18 OF 24 

### Table 15 . DAL GW WW10R 140227 (1)

PFOA PFBS

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

ISO14

- 07

- 02

- 016 DAL

- GW

- WW10R

- 0

- 140227 1820 NA 264 NA

ISO14

- 07

- 02

- 017 DAL

- GW

- WW10R

- DB

- 140227 1740 NA 256 NA

ISO14

- 07

- 02

- 018 DAL

- GW

- WW10R

- FMS

- 140227 3710 97.3 2130 93.5

Average Concentration (ng/mL) ± %RPD 1780 ng/mL ± 4.5 % 2 6 0 ng/mL ± 3.1 %

PFHS PFOS

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

ISO14

- 07

- 02

- 016 DAL

- GW

- WW10R

- 0

- 14022 7 919 NA 2840 NA

ISO14

- 07

- 02

- 017 DAL

- GW

- WW10R

- DB

- 140227 950 NA 2880 NA

ISO14

- 07

- 02

- 018 DAL

- GW

- WW10R

- FMS

- 140227 3220 114 4770 95.7

Average Concentration (ng/mL) ± %RPD 935 ng/mL ± 3.3 % 2860 ng/mL ± 1.4 %

13 C 4 - PFOA 13 C 4 - PFOS

3M LIMS ID Sample Desc ription %Recovery %Recovery

ISO14

- 07

- 02

- 016 DAL

- GW

- WW10R

- 0

- 140227 103 106

ISO14

- 07

- 02

- 017 DAL

- GW

- WW10R

- DB

- 140227 103 114

ISO14

- 07

- 02

- 018 DAL

- GW

- WW10R

- FMS

- 140227 96.8 106

Average Concentration (ng/mL) ± %RSD 101 % ± 3 .7 % 1 08 % ± 4.5 %

NA = Not Appl icable (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. ISO14

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PAGE 19 OF 24 

### Table 16 . DAL GW WW11R 140227 (1)

PFOA PFBS

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

ISO14

- 07

- 02

- 019 DAL

- GW

- WW11R

- 0

- 140227 1220 NA 251 NA

ISO14

- 07

- 02

- 020 DAL

- GW

- WW11R

- DB

- 140227 1370 NA 272 NA

ISO14

- 07

- 02

- 021 DAL

- GW

- WW11R

- FMS

- 140227 3090 90.5 24 30 108

Average Concentration (ng/mL) ± %RPD 1300 ng/mL ± 1 2 % 262 ng/mL ± 8 .0 %

PFHS PFOS

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

ISO14

- 07

- 02

- 019 DAL

- GW

- WW11R

- 0

- 140227 683 NA 1850 NA

ISO14

- 07

- 02

- 020 DAL

- GW

- WW11R

- DB

- 140227 709 NA 2340 NA

ISO14

- 07

- 02

- 021 DAL

- GW

- WW11R

- FMS

- 140227 2910 110 3790 84.9

Average Concentration (ng/mL) ± %RPD 696 ng/mL ± 3.7 % 2 100 ng/mL ± 23 % (2)

13 C 4 - PFOA 13 C 4 - PFOS

3M LIMS ID Sample Description %Recovery %Recov ery

ISO14

- 07

- 02

- 019 DAL

- GW

- WW11R

- 0

- 140227 102 113

ISO14

- 07

- 02

- 020 DAL

- GW

- WW11R

- DB

- 140227 111 111

ISO14

- 07

- 02

- 021 DAL

- GW

- WW11R

- FMS

- 140227 95.4 109

Average Concentration (ng/mL) ± %RSD 103 % ± 7.7 % 111 % ± 1.9 %

NA = Not Applicable (1) Samples were anal yzed 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) Sample RPD set did not meet acceptance criteria of ± 20%

.3M ENVIRONMENTAL LAB ORATORY

REPORT NO. ISO14

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PAGE 20 OF 24 

### Table 17 . Trip Blank R esults

PFOA PFBS

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

ISO14

- 07

- 02

- 022 DAL

- GW

- TRIP

- 0

- 140227 <0.0240 (1) NA <0.0250 (1) NA

ISO14

- 07

- 02

- 023 DAL

- GW

- TRIP

- LS

- 140227 5.46 (1) 110 5. 15 (1) 1 03

IS O14

- 07

- 02

- 024 DAL

- GW

- TRIP

- HS

- 140227 2390 (2) 96.4 2450 (2) 98.0

PFHS PFOS

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

ISO14

- 07

- 02

- 022 DAL

- GW

- TRIP

- 0

- 140227 <0.0250 (1) NA <0.0232 (1) NA

ISO14

- 07

- 02

- 023 DAL

- GW

- TRIP

- LS

- 140227 5.47 (1) 109 5.35 (1) 107

ISO14

- 07

- 02

- 024 DAL

- GW

- TRIP

- HS

- 140227 2630 (2) 105 266 0 (2) 107

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

3M LIMS ID Sample Description %Recovery %Recovery %Recovery %Recovery

ISO14

- 07

- 02

- 022 DAL

- GW

- TRIP

- 0

- 140227 86.9 95.8 108 99.2

ISO14

- 07

- 02

- 023 DAL

- GW

- TRIP

- LS

- 140227 93.5 93.7 103 103

ISO14

- 07

- 02

- 024 DAL

- GW

- TRIP

- HS

- 140227 NA NA 92.7 102

NA = Not Applicable (1) Samples were analyzed by internal standard calibration. (2) Samp le 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

.3M ENVIRONMENTAL LAB ORATORY

REPORT NO. ISO14

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PAGE 21 OF 24 

# 5 Conclusion

Laboratory control spikes were used to determine the analytical method accuracy and precision for all analytes. The accuracy and precision were then used to estimate the method uncertainty for the results. Field matrix spike recoveries demonstrated that the analytical method was appropriate for the given sample matrix

. Analysis wa s completed using 3M Environmental Laboratory Method ETS

- 8

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

. Analytical results are reported in Table 1 and 10

- 1 7 of this report.



# 6 Data / Sample Retention

All remaining sample and associated project data (hardcopy and electronic) will be archived according to 3M Environmental Laboratory standard operating procedures.



# 7 Attachments

Attachment A : Analyte Trend Data for the Decatur Groun d Water Treatment Plant (GWTP) GAC System

.



# 8 Signatures

Susan T. Wolf, 3M Principal Analytical Investigator

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

The 3M Environmental Laboratory’s Quality Assurance Unit has audited the data and report for this project.

Quality Assurance Representative

This test report shall not be reproduced except in full, without written approval of the 3M Environmental Laboratory.3M ENVIRONMENTAL LAB ORATORY

REPORT NO. ISO14

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PAGE 22 OF 24 

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

ACI (Activated Carbon Influent)

- Sample Results in ng/mL

ACI 03/27/13 04/29/13 05/31/13 06/27/13 07/23/13 09/30/13 10/28/13 11/18/13 12/13/13 01/30/14 02/27/14

PFOA 2220 1480 1860 1480 1630 2320 1880 2190 1830 1580 1870

PFBS 1060 1360 1040 708 1230 356 1590 1100 1350 202 1470

PFHS 1090 777 940 942 749 1400 866 1330 695 845 737

PFOS 2490 1670 2150 1590 1680 3240 2100 2240 1970 2700 1800



### AC E (Activated Carbon Ef fluent)

- Sa mple Results in ng/mL

ACE 03/27/13 04/29/13 05/31/13 06/27/13 07/23/13 09/30/13 10/28/13 11/18/13 12/13/13 01/30/14 02/27/14

PFOA 0.0380 0.0422 0.0725 0.0717 0.0641 0.115 0.231 0.478 0.0798 0.490 0.138

PFBS <0.0250 0.392 24.8 111 1960 1950 0.379 0.59 2 0.0766 0.257 0.0360

PFHS 0.0477 0.057 0.105 0.118 0.0778 0.156 0.180 0.366 0.0648 0.219 0.0706

PFOS <0.0232 <0.0232 <0.0232 <0.0232 0.0277 0.0452 0.0785 0.0726 0.0303 0.209 0.09663M ENVIRONMENTAL LAB ORATORY

REPORT NO. ISO14

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PAGE 23 OF 24 

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

WW8R

- Sample Results in ng/mL

WW8R 03/27/13 04/29/13 05/31/13 06/27/13 07/23/13 09/30/13 10/28/13 11/18/13 12/13/13 01/30/14 02/27/14

PFOA 3640 3190 2760 2760 2640 2890 2830 3040 2720 2660 2560

PFBS 385 364 289 282 263 303 312 362 316 326 331

PFHS 1760 1610 1330 1340 1260 1370 1300 1440 1270 1460 1370

PFOS 5120 4830 4180 4110 3910 4100 4410 4750 4060 3990 4170



### WW9R

- Sample Results in ng/mL

WW9R 03/27/13 04/29/13 05/31/13 06/27/13 07/23/1 3 09/30/13 10/28/13 11/18/13 12/13/13 01/30/14 02/27/14

PFOA 3330 2650 2660 2630 2410 2730 2820 2950 2690 2900 2630

PFBS 278 244 226 225 212 249 286 305 259 317 270

PFHS 1440 1200 1120 1140 1030 1220 1280 1340 1170 1460 1370

PFOS 4660 4340 4210 4150 36 70 4200 4380 4540 4190 4800 46603M ENVIRONMENTAL LAB ORATORY

REPORT NO. ISO14

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PAGE 24 OF 24 

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

WW10R

- Sample Results in ng/mL

WW10R 9/30/2013 10/28/2013 11/18/2013 12/13/2013 1/30/2014 2/27/2014

PFOA 2070 2150 2400 1890 1330 1780

PFBS 247 264 303 239 250 260

PFHS 1030 1030 1120 885 757 935

PFOS 2770 3160 3890 2920 1570 2860



### WW11R

- Sample Results in ng/mL

WW11R 9/30/ 2014 10/28/ 2014 11/18/2014 12/13/2013 1/30/2014 2/27/2014

PF OA 1720 1100 1320 1060 814 1300

PFBS 299 240 287 198 168 262

PFHS 1000 511 680 512 362 696

PFOS 2200 1670 1850 1570 1540 2100