3M ENVIRONMENTAL LABORATORY 

REPORTNO. IS013-07-07 

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

3M Decatur, Alabama.-Groundwater Treatment Plant GAC System — 

. July 2013 

I W *= TM I"k mm 

Repat Date — Date of Last Signawre 

3M EHS&S Operabons 

Building 260-5N-17 

Maplewood, MN 55144-1000 

~ 

Gary Hohenstein 

3M Building 224-51V-03 

Saint Paul, MN 55144-1 000 

Phone: (651) 737-3570 

ACCREDITED 

T-% - #205201 

The testing repoded erein meet the requirernerft of ANSUtSMEC 17025:2006 

"General Reqwrenienft for the Competence of Tesbng and Calibration Labomtories", in 

accordance wtth the A&A Tesbng Certrficate # 2062.01. Addifionally; the laboratmys 

quardy system has been audited and was determitned tD be in confonnance with the 

EPA GLPs (40 CFR 792) by an irKWperident A&A assessfnent 

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3M EWIRONMEIVTAL LABORATORY 

REPORTNO- IS013-071)7 

3M Environmental Labor-atory 

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

3M Principal Analyfical Invesfigator: Susan Wotf 

Report Author., Cheisie Grochow 

Anaiytical Repoi-t IS013-07-07 

3M Decatur Groundwater Treatrnent Plant System; July 2013 Sampling 

Report Date: Date of Last Signature 

1 Introduction/Summary 

system at the 3M Decatur, AL fac Water samples were collected • Weston Solufions personnel 

• July 23, 2013. Samples were retumed to the3M Environmental Laboratory for analysis • 

Perfluorooctmioate (PFOA), PerfluaDbutane suffonate (PFBS), Perfluorohexane sulfbnate (PFHS), 

Perfluaooctane sulfonate (PFOS), arvd the surrogate recovety standards ~PFOA and 13C4-PFOS 

under WxxatDry project number IS013-07-07. Analysis • the samples was completed as specified 

un•er 3M Environmental Labor-atory General Project Outline (GPO) num•er GPOI 1-100•. 

The 3M Environmental LaborattAV &AU,ided • I 

MM t R - - 

Samples were prepared and analyzed • method ETS-8-044.1 "Meffiod • Analysis f•r the 

Determination of Perfluorinated Compounds in Water by LCIMSIMS; Direct Injection Analysis7. Select 

hterml standards were use• t• aid in the •ata quality objecfives. 

Table I summarizes the sample resufts using te analyfical metiod kiengied above. AJI resufts lbr 

qualky control samples prepared and anaWed wkh the samples vvill be reported a'nd discussed 

elsewhere in ft report 

The tesfing reported herein meet the requirements of ANSMMEC 17025.,2005 "General 

Requirements for te Competence of Testirig and Calibration Labomtories", in 

accordance with the A21-A Testing Cerfiftate # 205Z0I. AdcNonalty, the WboratDr/s 

quoJKy system hm bftn audited md was detmTWirwd to be in confbnmnee with the EPA 

GLPs (40 CFR 792) by an independent A21-A assessnwvt 

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3M ENVIRONMEAfTAL LABORATORY 

REPORTNO- IS013-07-07 

Table 1. Sample Results Summary 

PFOA PFBS PFOS 

Concerftation Concentrabon 

:H 

Con 

ntL 

 on ConcenbaWri 

3M LMS ID Saffipie Description (ngI L) (nghnL) (ngfrnt.) (ng/mL) 

tS013,07-07-001 DAL-GW-ACI,- Sample 1650 1230 757 1700 

tS013-07-07-002 DAL-GW-AC, - Samp(e Dup 1610 1230 741 1600 

Average 1630 (l) 1230 749 ti) 16800, 

•RPD SainpWSample Dup 2.5 0.0 2.1 2.4 

IS013-07-07-004 DAL-GW-ACM27 Smple 875 1210 601 1-35 

IS013-07-07-005 DAL-GW74QW Sam le Dup 844 1210 585 127 

Average 8m (1) 1210 593 (l) 1.31 10 

%RPD &vnple/Sample Dup 3.6 0.0 2.7 6.1 

(S013-07-07-007 DAL-GW-ACE, Sample 0-0663 1970 0.0784 0.0267 

Ls013-07-07M8 DAL-GWACE; Sample Dup 0-0619 1950 0-0771 0-02137 

Avwage 0.0641 12) 1960 "1 0.0778 0 0.0277 r4 

•RPD SmVte/Swnple Dup 6.9 1.0 1.7 7.2 

IS013-07-07-010 DAL-GW-WW8R Sample 2530 258 1210 3850 

L9013-07-07-011 DAL-GW-WW8R; Sampte Dup 2750 268 1300 3970 

Avemp 2640 (1) 263 (l) 1260 3910 0) 

%RPD SaffvWSample DW 8.3 3.8 72 3.1 

IS01I3 07-07-013 DAL-GW-MgR Sample 2370 210 1020 3600 

[so DAL-GW-WW9R; Sample Dup 2440 214 1040 3740 

Avemp 2410 03 212 m 1030 11) 3670 "1 

%RPD Sw ldSample Dup 2.9 1.9 1.9 3.8 

NA = W AMknW 

(1) Reported resufts were prepmod aW analyzed by ErS-&W I using exWmal sbndard agWxabm The arklybcal ffwfflod 

urmtawb)s assomted wdh the mported resuts are as folDm: PFOA t14T., PFBS t 12%, PFHS t13%, and PFOS t 15%- 

(2) Reporbgd mmks were pepared aW mWgd by ETS-&W I usrg mtanal sWrKlmd cabbrabon- The midytcN rrw#W 

urcmtwbes associabBd wdh ft reported msults are as folows- PFOA t 10%, PFHS t 14%, and PFOS t 15% 

2 lllethods - Analytical and Preparatory 

2.1 Meth•ds 

Table 2. Target AnaMes 

~iW~~~~l-„1„~M ! Yi . [.. ~ \E M I II . 

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3M ENVIRONMENTAL LABOPA TOPY 

REPORTNO- IS013-07-07 

2.2 Sample Collection 

Samples were collected on July 23,2013 in NalgeneTm (high-density potyethylene) botfles prepared at 

the 3M Environmental Laboratory. Prior t• sample collecfion, botfies deskjrtated for fidd matrix spikes 

were slYiked in the laboratory wkh a known volume of an appropriate matrix spiking solufim contag 

PFOA, PFBS, PFHS, arvd PFOS. Sample bottles for sampling •locations ACM2 and ACE, along with 

-t-ie %ita riominal conoenlrabon • 1 ng/mL and a mkWre • surrogate recovery standards at a nominal 

concentrafion • 0.1 ng/mL. Collected sample bottles were received • ft Liboratory at ambient 

conditons • July 25, 2013. 

2.3 Sample Preparation 

AJI samples were diluted wfth methanol and analyze• fbr all anaVes. Samples diMed 1:10 were 

-Afr-~V2; e• t I"t of vil-fg 2 "NTL z i x -I 

mL of a surrogate spng sohAon. The 1:100 dflubons were prepared by ranoving a 0.1 mL aliquot of 

the well mixed sample an• adding 9.8 mL of methanol and 0.1 mL of a surrogate s•iking soiufion. 

Prepared samples were analyze• by extemal standard cahbrafion. 

The ACE an• ACM2 sample sets and the Trip Blank sample were prepared and armlyzed for all 

analytes by transferfing an aliquot • the well mixed sample into an autovial. Prepared samples were 

analyzed • intemaA standard calibration. 

D urinn-the-p re• an ib x m AI)P--L--4j xt-4 tvW. Nnif-c ?SW# ,jf 2 

separate intemal standard spiking solubon was added to the laboratory control samples (nominal 

concentration of 1 ngImL). The sample bottles fbr ACE, ACM2, and Trip Blank were spiked whh an 

intemal stMard mix at a nominal concentrabon of I ng/mL prior to being sent to the field fbr sam•le 

collecbon. The laboratory cordrol samples were anWyzed m the sam manner as the samples. 

2.4 Analysis 

AJI samples and qualfty control samples were -• for four tirget analytes using high perfbrmance 

liquid chromatographyttandem mass specb -ometry (HPLUIVISIMS). Pertrient instrumerit parameters, 

the liquid dwomatography gradient program, and the specific mass transibom analyzed are desctibed 

h thetables bdow. 

Due • ffie nature of the sample, the wide range of concentrations found in the sarnple, and the 

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