DEQ-CFW_00070494

FEB v 'j 2e08
Lower Cape Fear Water & Sewer Ad
FACSIMILE T1t7MMITTAL SHEET
DATE: ZI
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FAX NUMBER
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REFERENCE:
TOTAL NUMBER OF PAGES:
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Post Office Box 1673, Wilmington, North Carolina 28401 [phone] [phone] Fax
Office Location:1107 New Pointe Blvd, Suite 17, Leland, North Carolina 28451
e-mail: donC)dwasa.ore web page: www.)cfwasa.M
F El
1 'A 0991 '0N
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DEQ-CFW 00070494

ANALYTICAL WORT
PFOA Analysis
Lot #, D70190467
JeffMusselwhite
Smithfield Foodo
15855 Hwy 87
Tar Heel, NC 28392
TesLkmetloa Dmvcr
t
Q> ko�z
Qail DeRuzzo
Project Manager
Ausot, 2007
STL
STL Denver
4955 Yarrow Street
Arods, 00 W02
7sh $03 736 0100 Faxs $03 4317171
wWWA-Inacom
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DEQ-CFW 00070495

Table of Contents
Standard Deliverables
Report Contents
Standard Deliverables
The Cover l Wr and the Report Cover page are cowidered integral
parts of thk Standard ADelivetable package. This report is incomplete
unless all pages indicated to this Table of Contents are included.
s Table of Contents
e Case Narrative
e Executive Summary — Detection Highlights
a Methods Summary
a Method/Analyst Summary
• Lot Sample Summary
+ Analytical Results
e QC Data Association Summary
Chaim -of -Custody
Total Number
of Pages
0
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DEQ-CFW 00070496

Case Narrative
D7GI90467
The results included in this report have been reviewed for compliance with the Laboratory Quality
Manual. All results have been found to meet all requirements of ML`.AC and any exceptions are noted
below.
This report shall not be reproduced except in full, without the written approval of the laboratory or
sponsor. Dilution factors and footnotes have been provided on each datasheet to assist in the
interpretation of the results.
Sample Arrival and Receipt
The four water samples presented in this report was teeeived at the TeatAmerica Denver laboratory at a
temperature of 16.3°C on July 19, 2007, which is above the recommended receipt temperature of 4°C +/-
2°C. The client was notified.
t
Analytical standards were prepared using the acid form of the compound perfluorooctanoic acid (PFOA).
Pertluom-n-[1,2,3,4-'SCa300tsnoic acid was introduced at &a extraction step and was used as an internal
stanndard ;for quarntitation of PFOA.
Sample Extraction and Analysis
The samples presented in this report were analyzed for the target analytes by TestAmerica Denver's SOP
DEN-LC-0011
For water samples a 250 mL aliquot of tech sample is acidified with I mL of 6N HCI solution and it is
extracted using solid phase extraction technique with methanol conditio4ed C18 cartridges. Each sample
is spiked with the itternal standard, prior to extraction. After the sample is passed through the cartridge,
the analytes are eluted with 4 mL of methanol. The final volume is brought to 5 mL using methanol and
the extract is analyzed by LC/MS/MS.
Method OC Samulles
The Method Blank is processed reagent water spiked with surrogate and prepared with each batch of 20
samples of the same matrix. The method blanks were non -detect at the reporting limit for the target
analyte.
Each batch is prepared with Laboratory Control Samples (LCS). The LCS recoveries for both levels
were within established control limits for the target analyte.
An"gd Comments
T o internal standard recovery for 13C4 PFOA was below the control limit in the method blank
associated with QC batch 7208485. Because all other internal standard recoveries were in control, no
corrective action was necessary.
The internal standard recovery for 13C4 PFOA was above tbi control limit in sample "2" in QC batch
7201367• The sardple vvas re-extraoted nine days after collection and re -analyzed with the internal
standard recovery in control and with similar results. Only the re -extracted sample results are reported.
No other anomalies were noted.
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DEQ-CFW 00070497

D7=90467
i
REPORTIXQ
ANALYTICAL
PARWTER
RESULT
LIMIT
UNITS
METHOD
1
07/18/07 07:50
001.
PFOA
0.13
0.015
ug/L
DEN-LC-0012
2
07/18/07 07:55
002
l :—
PYOA
0.13
0.015
ug/L
DEN-LC-0012
3
07/18/07 07sS9
002
PFOA
0.13
0.015
ug/L
D8N-LC-0012
4
07/18/07 0003 03
' 004
PFOA
0.13
0.013
ug/II
D8N-LC-0012
4 a f1R41 'oil W�Il9 1, 5007 '91 'Uvr
DEQ-CFW 00070498

METHODS Summm '
D7O190467
ANALYTICAL PREPARATION
PEER METSOD ME HOD
LC/MS/MS, PFOA
RefeZ ewes
DEN-LC-0012
DEN Severn Trent Laboratores, Deaver, lFacility Standard
Operating Procedure.
9 'd 0991 'IN
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DEQ-CFW 00070499

METHOD /.ANALYST SUMMARY
D70190467
ANAL'YTXCM ANALYST
Ms'1 OD ANALTOT ID
DEN-LC-0012 Jaqueline So=ett 003601.
Raforoncee:
bEw Bove= Treat Laborarorae, aenwar, Facility standard
Qperat:ing Procedure.
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DEQ-CFW 00070500

"
SAMPLE SUMMARY
1)7421.904'67
=OLED SAMP
WO #
SAMPLE
CLIMT SAMPLE ID
DATE _
6T27V4
001
1
07/18/07 07150
,727V9
002
2
07/3.8/07 07t5$
727WD
003
3
07/18/07 07r59
L721WE
004
4
07/10/07 08:03
Nms
. The eoalydmd mutts of die mtpla Wad stave as prnented OR the follcab>p Psoeo.
• All celculadons ere performed berore robMing to evold rpuad-otrerroly In CRICVI gal 10111 ,
- R4Wtr aoW Iu "ND" ww not defeated N or dare The fitted Hold.
- Brit report mutt not be mprodu m, except In lu, without the wtmm spprovd of the idardory.
AaWN for due fbilowing pu metw ere over mporaW on s dry woipht buds: War, wmlvlty, datuhy, Atlshpobtt, I$nitsbOlty, Isyers, odor.
PAW filter sm, ON, porosity pressure, mashy, redox potential, epecim vWry, spot reds, solid., eolubillty, temperelurs, vbmlty, sad welOt.
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DEQ-CFW 00070501

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Smithfield Packing Company
Client Sample IDc 2
Lot-SaWle #... :
D70190467-002 Pork Order #...:
a27VOUA Matrix.........: WATER
Deus Gaugled...:
07/18/07
071SS Date Received..:
07/19/07
Prep Date......c
07/27/07
Analysis Date..:
07/28/07
Prep Hatch #...
7208489
Analysis Time—:
22.43
Dilution Factor:
1
Method......., .
DEN-LC-0012
REPORTING
PARAMklTP�R
RESULT
LIMIT__ ____ WITS
p1rok
0.13
0.015 ug/L 0.0026
PERCENT
RECOVERY
O(}A
RECOVERY
LIMNS
13C4 PFOA
167
(50 - 200)
0l 'A OR9l 'ON
Ad I S: Z 800Z '91 "r
DEQ-CFW 00070503

Smithfield packing Company
Client Stemple ID: 3
Lot -Sample #... !
D70190467-003
Work Order #... :
,727WD1AA Matr:Lx.I....... I WATER
Date Sampled....
07/18/07 07.59 Date Received, - -%
07/19/07
Prep Date......:
07/20/07
AnAaysis Date..:
01/26/07
Prey Batch #... i
7201367
AnaIySis Time..:
19:16
Dilution Factor:
1
Method ......... :'DEN
-LC-0012
• ��oRxz�
PATER P,9=T LIMIT , T UNITS MDL
PPOA 0.13 0.015 utg/L 0.0031
PERCENT RECOVERY
St7 ROGATX RECOVRRY LINXTS
i 13C4 PFOA 118 (SO - 200)
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DEQ-CFW 00070504

smit tiold Packing Company
Client sample ID: S
Lot-5atinple #...s
RIM
D7a190467-004 Work Ordex I
T27WRIM Matrix.........: WATU.
Date Sampl*d... s
07/19/07
o8a03 Date Reaeived..s
07/19/01
Prep Date......:
07/20/07
Analysis Date..:
07/20/07
prep Batch #... s
7201367
Analysis Time..:
19:48
Dilution Facto:
1
Method.....,...
DEN-W-0012
PARAMETER
REgULT
LIMIT UNITS l�L
PFOA
0.13
0.015 ng/L 0.0031
MIMCENT
RSCOVIRY
SMOC;ATR
RECOVE1tX
LIMITS —.
13C4 PYOA
11.9
(so - 300)
71 'A OPQ I 'Oki
N [l :7 9007 '91 "Pr
DEQ-CFW 00070505

QC DATA ASSOCIATION SUMMARY
p70190467
Sample Preparation and Analysis Control Numbers
ANALYTICAL LHACH
SAMPLE
MIST&IX
METHOD.. ---- AATCg_. i
001
WATER
DEN-LC-0012
002
WATER
DEN-LC-0012
003
WATER
DEN-LC-0012
004
WATER
PEN-LC-0012
PRIM?
rCH
7201367
7208409
7201367
7201367
Ms RUN
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DEQ-CFW 00070506

Client Lot #•••= D1O190461
N2 Lot -Sample #. R7O200000-367
A=ayaia Date..: 07/28/07
Diluti= Factor: 1
PARAMETER
PPOA
MET13M OW" RZPMT
Emw
Work Order #...: A'3ART)IAA,
prop Date......: 07/20/07
PzW Batch #...: 7301367
Matrix ........... WATIA
Analysis Tioe..: 17156
REPORTING
RESULT LIMTT WITS META
ND 0.015 ug/L PIN-LC-0012
PERCEW RECOVERY
SURROGATE RECOVERY LIMITS
13C4 PFOA 93 (50 - 200)
IAOTH (9)
CdwXdow are pe N mW hafm rowdlna to avaW m=d-off wmr# In a oulaNd :aultt,
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DEQ-CFW 00070507

HPLC
Client rot: #...: >57b] 90467 work order $...: ;73044LM mastrix......... I WATZR
US Lot-Saaple #s R70210000-499
pry Date...... s 07/27/07 AnaOYO:La Time.. 12a:40
Analysis Date..: 07/20/07 Prep Batch #...: 7208489
Dilution Factor: l
REPORTXNC;
PARAMETZR INSULT LIMIT UVITS METHOD
PFOA - Nil 0.015 ug/L DEN-LC-0012
PERCENT RECOVERY
SURROGATE RECOVERY LIMITS
13C4 I3VOA 31 * {5i? - 200)
A°WO(5) :
CslealRdow sm pmlbmd bskm rouadlnf to svold round -off emu Is adc AW =fts.
• 8urr6si: rto0vary Is audid. kowd 0autm i I► N.
S l d OW 'IN Wdzs: z 800Z 9l "PC
DEQ-CFW 00070508

;l, HoJATMT CCeTROL SAML» ZVALUATICU RAP=
HFnC
Client Lot #...- D70190467 Work Oxdlox #...: J3AMIAC Matrix.........: WATER
LCS Lot -Samples R70200000-367
Prep Date......: 07/20/07 Analyai,e Date..: 07/28/07
PM Batch #...a 7201367 Analymis Time..: 19s12
Dilution Pictorr 1
PRRCm RECOVERY
RECOVERY I.zM1T8 METHOD
PARAM&TSR �_
PPOA log (70 - 3,30) wi-LC-OQLZ
PERCENT RECOVERY
9U00A,T3 RECOVERY LIMITS
I$M PFO,A, 95 (50 - 200)
>i m (a) r
Calauledom aro "Mid hetbro roundins to avoid round-otr ermn In m1ml and m MM,
Bald print danatee =Ual plmm*n
t
I
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DEQ-CFW 00070509

L&BORLTORX COmi'=L SA1t1= DATA REPORT
Client Lot #...r D7G190467 Work Ord= #...: O'3AEDIAC
Y.CB Lot -Samples R70200000-347
pep Date ...... % 07/20/07 Analysis Date..: 07/28/07
Prep Batch #... % 7201357 Analysis Time..; 10:12
Dilution Factor; 1
PARAMETER
PFOA
0M OGATS
13C4 PPOA
SPIKE MEASURED
AMO'f jNT AMOUNT
0.200 0.217
PERCENT
ER C0MY
95
C mlidex ere psoomwd before roandho to avoid imww-oK error% 19 a wtsted rWIAL
DOW print denotes pontmi pmamtsm
Matrix.......... WATIM
PERCENT
UNITS RECOVERY METHOD
mg/L- __- 109 mw .-LC-0012
RECOVERY
LIMITS —
(50 - 200)
W 7,,�:l, 9007, '91 'upf
DEQ-CFW 00070510

LAPORATOU' t CODrML SANKA S'VA'C. %=ON REPORT
HPLC
client Lot 0/0190467 Work Ostler J3=31M ......... ; WATER
YACS Lot-Sample#s R7,3200000-367
Prep Date......: 07/20/07 Azmayois Date..s 07/28/07
pM Batch #...; 7201367 analysis Time..: l8s28
Dilution Factors 1
P91CMIT 19COV'E1d'Y'
PARAMETER RECOVERY LIMITfi ____. METHOD
Ppm 119 (70 - 130) DELP-LC-0012
PERCENT RECOVERY
SURROGATE RECOVERY LIMITS
13C4 P80A 93 (50 - 200)
u4wAdesu Am performed bra m roundha to Vold mud -off emu M alatw saula,
DON prw davotes contra► parnm m"
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DEQ-CFW 00070511

LABORATORY CcrtRox, gAmm DATA Ra po
BPLC
Client Lot #...: D70190467 Work Order #.... J3A=LU Matrix ......... & WATER
LCeS Lot-9ample#t R702000D0-367
prep Date ...... c 07/20/07 Analysis Date..: 07/28/07
Axep Bauch #... s 1201367 Analysis Time..e 18128
Dilution 8'aatoxc 1
SPIKE MEASURED PERCENT
PARAMETER AMOCtDPl' ,AMOmm =TS .RECOVERY MBTMOD
PF" 0.0200 0.093E ug/L 119 mw-XC-0019
P 3RC8NT RECOVERY
SURROGATE RECOVERY LIMITS
13C4 PFOA 83 (50 - 200)
mO'1'E (SI) l _
cawh tp l us pertbrmed baste tsunami eo mid round-ot'l uroN In 9AWL oed rums,
Bold prpudents00W pe WWWR
61 d H91 'ON 91 'uvp
DEQ-CFW 00070512

LABORATORY CONTROL SAMPLE BVALDATICK R,BBORT
ULC
Client Lot #..•= D70130467 work Order #...: L730441AC matrix. ........ I WATER
LCs Lot-Semle#: R70270000-489
PrV Tate......: 07/27/07 AaalySie Date..: 07/28/07
Piep Batoh 8...: 7208499 AWlysis Time..a 21c56
Dilution Factor: 1
PERCENT RECOVERY
PARAMETER RECOVERY UMIT8 MBT Ob
Py0A, 1.08 (70 - '130) 1=-LC-0019
PERCENT RECOVERY
StIRROOATS REC0'U'3!R'Y LIMITS
13C4 PFOA 73 (50 - 200)
NOTA(S) s ---
Calouledons an WthrmW batbm toundN= to avoid murkaff W&A la 941CW& ad raaulm
)Told Print deaom cawal puamwn
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DEQ-CFW 00070513

LABORATORY CO1TntOL SAWLB DAM RBBORT
XPLC
Cliont Lot #... s D70190467 Mork Ordar #... r J'3Q441AC Matx*ia¢......... s WATSR
J.M Lot-8mW3.e#s R70270000-489
" Data..:.... 07/27/07 Aala3.ya1e Datte..r 07/28/07
Prep Batch #... : 7208489 Analysis Time..; 21;56
Dilution Factor: 1
SPIKE MEABufJI= PERCENT
P.AWETFR MOM AMYET T UNITS RECOVERY METHOD
PFOA 0.200 0.216 Z7-L 108 =P -IBC-0012
PERCENT RECOVERY
SURROGATE RECOVERY LIMITS
13C4 PFCA 73 (50 - zoo)
NOTE (0) a
Ctieulmlom m perfomud before roundim to wld mundaff orron In oiWW#d raalu.
sold pdm doom Control pmmmm
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DEQ-CFW 00070514

LAEOR&TORY aRMWL SAMPLE BVALUA=09 RZMT
HPLC
Client Lot #...s D70190467 Work Qrdex ...: J3Q441AA matrix ......... s PLATER
LCO Lot-SaWle#; R70270000-489
Pzeep Date......: 07/27/07 AA&Iysis Date..s 07/28/07
Prep Hatch S...: 7208489 Analyffie Titme..s 22t13
Dilution PACtOrt 1
PERC= RECOVERY
pATiAMExER RECOVERY LIMITS MaTHOD
PFOA 114 (70 - 130) DBU-LC-0012
PERCENT RECOVERY
SURROG;ATS _ RE OVER LIMITS
13C4 PFOA 64 (90 - 200)
&kulufotu uv perlbrmed oefbre round ft to avoid round -off error In a1091AW ream.
Bold print denotercontrolpirarawts
WdES:z soot 91,,Vr
DEQ-CFW 00070515

LABORATORY CONT90L M*= ZATA REPORT
Client Lot #
D70190497
BPLC
Work Order #...: J30441AD
X*tx-jx........... WATIR
UX T,*t-SsaWle#t
R70270000-489
prep Data......:
07/2?/07
Aualysis Date..: 07/28/07
Prep Satrh #...:
7206409
Analysim Time..: 22t13
Dilution pactor:
7,
1
SPIRE MEASURED
PERCFfa1T
PARPMTER
MO NT AMOUNT
UNITS RSCOVE Y HE=
pI
0.0200 0.0227
ug/L 24 D8N-LC-0012
PBRCSNT
RECOVERY
SMOGATE
RECOVERY
LIMITS
13C4 PFOA
I
64
{50 - 200)
NO'.P8 (a) t
CdcuWam ua performed bm*m
taurdft m AV* MuM-aff a m 1n oafOaU M tauf s-
Hold pft dwam comol pammean
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DEQ-CFW 00070516

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