Document QM3oj7JBQ4RgyQ76ko87DzGNv
AZzze.-z'fsS'
AXYS METHOD MLA-031 Rev 01
pfos_s i_D2
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Lab Name: AXYS ANALYTICAL SERVICES
Sample Collection:
Contract No.: Matrix: Sample Receipt Date:
4191 SERUM 03-Feb-2005
Lab Sample IP: Sample Size: Initial C alibration Oate:
Extraction Date:
l6-Feb-2005
Instrum ent ID:
Analysis Date:
17-Feb-2005
Time: 21:34:20
LC Column ID:
Extract Volume (mL): Injection Volume (pL):
2 30.0
Sample Datafile: Blank Data Filename:
Dilution Factor:
N/A
Cal. Ver. Data Filename:
Concentration Units : ng/mL
CLIENT ID:
02-Feb-2005
L7602-8RI 2.00 17-Feb-2005 LC-MS/MS C18( Zorbax XDB PFS5G_027S48 PFS5G,,027S40 PFS5G.027S37
COMPOUND
LAB F LA G 12
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U u u
0.344 17.1 2.91 1.21 0.415 0.152 u u 6.15 16.9
1.88 1.31 0.293 0.0777 0.101 0.0085 0.0049
0.0099 0.0087 0.0061 0.123 0.0340 0.0844
3.24 4.86 5.38 5.76 6,06 6.38
5.28 5.98
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLAG'
SPIKE CONC.
(nfl)
12.0 12.0
CONC. FOUND
(ng)
10.4 8.75
R (V.)1
RETENTION TIME
87.0 72.9
4.86 5.72
(1) U = not detected (2) R (%) = Percent recovery
151Q5PF01_1 xts, S10
Approved by:
QA/QC Chemist
11-05-2005 dd-rttfn-yyyy
O A X Y S / M M / av L V T 'I C 3 A . L S E R V I C E S L T D CO BOX22:9, M5 MILLSID. m \ SIDHT, It.. CANADAV 3SSTU (250) iSS-5800 FAX(250) 455-S811
3-7
AXYS METHOD MLA-031 Rev 01
pfos_s i_D2
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
CLIENT ID:
Lab Name: AXYS ANALYTICAL SERVICES
Sample Collection:
03-Feb-2005 18:00
Contract No.: M atrix: Sample Receipt Date: Extraction Date: Analysis Date: Extract Volume (mL): Injection Volume {pL): Dilution Factor: Concentration Units :
4191 SERUM 08-Feb-2005 16-Feb-2005 17-Feb-2005 2 30.0 WA ng/mL
Time: 17:01:37
Lab Sample ID: Sample Size: Initial Calibration Date: Instrum ent ID: LC Column ID: Sample Datafile: Blank Data Filename: Cal. Ver. Data Filename:
L7609-5R i 2.00 17-Feb-2005 LC MS/MS C18,2orbax XDB PFS5GJJ27S27 PFS5G_027S40 PFS5G_027S20
COMPOUND
LAB FLAG '
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U u u
0.097
9.12 2.06 0724
0.245 u u u
2.56 42.8
3.09 1.16 0.458 0.0352 0.0510 0.0084 0.0117 0.0031 0.0379 0.0041 0.164 0.0071 0.116
3.17 4.84 5.38 5.76 6.07
5.28 5,99
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB F LA G 12
SPIKE CONC.
(ng)
12.0 12.0
CONC. FOUND
(ng)
10.1 9.50
R (%)*
RETENTION TIME
83 8 79 2
4.82 5,76
(1) U = not detected (2) R (%) = Percent recovery
151Q5PfD1_1.xls, S15
Approved by:
QA/QC Chemist
11-05-2005 ddmm-yyyy
A X Y S A N A L Y T IC A L SER.VTCZES L T D P.0 BOX7719.7045 Mitts8.WfSl.SIDW,U , (MUMYBl 358Ttl (250)5S5-5B00 X(250)iH-5811
pArXoYsSsMi EsTaHOD MLA*031 Rev 01
Form 1A/2
PERFLUORiNATED SURFACTANT ANALYSIS REPORT
Sample CollecUon;
23-Mar-2005 17:52
U b Name: AXYS ANALYTICAL SERVICES
Contract No.:
191
Lab Sample ID:
L7714-3R
Matrix:
SERUM
Sample Size;
1.00 mL
Sample Receipt date; 29-Mar-2005
Initial Calibration Date:
BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID:
LC-MS/MS
Analysis Date:
22-Apr-2005
Time: 6:36:38
LC Column ID;
C18, ZwbaxXDB
Extract Volume (mL): 2
Sample Datatile:
PFS5GJ0S8S70
Injection Volume {pL}; 30 0
Blank Data Filename:
PFS5GJD58S026
Dilution Factor: Concentration Units :
m ng/mt
Multiple Cal. data Filenames;
PFS5G,,058S050 PFS5G 058S062 PFS5G_058S080 PFS5GJJ58SQ81
COMPOUND
LAB FLAG1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPaA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
0110 U U
2 83 0 716 0235 0059 0 014 U 4.77 14 B
0.0680 00632 0 0278 0 0239 0.0117 00117 00079 0 0174 0 0581 0.0307 0.0867
2 01
534 5 73 606 640 6 72
5 50 6 22
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAB1
SPIKE CONC.
(t>8)
120 120
CONC. FOUND
(ng)
10.1 120
R (%)3
RETENTION TIME
84 2 100
5.34 6 06
(1) U " not delected (2) R {%) - Percent recovery
15625PFD2J Id *. S17
Approved by
.QA/QC Oiemist
10-05-2005
dd-mm-yyyy
A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0 BOX1?. 701SMHIS10 WEST, S1DHET, IC . CAHAQAVit 358Tfl (7501 1555800 TAX(250) S5-58I1
AXYS METHOD M U -031 Rev 01
PF0 S_S1_D8
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
23-Mar-200517:50
Lab Nam*: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Samplo ID:
L7714-5R(A)
Matrix: Sample Receipt date:
SERUM 29-Mar-2005
Sample Size: Initial Calibration Date:
100 mL BRACKETING CAL
Extraction Date:
21-Apr-2005
instrument ID:
LOMS/MS
Analysis Date:
22-Apr-2005
Time: 6:48:31
LC Column ID:
018. ZorbaxXDB
Extract Volume {mL): 2
Sample Datafile;
PFS5GJ)58S071
Injection Volume (pL): 30 0
Blank Data Filename;
PFS5G_058S026
Dilution Faeton Concentration Units :
ti/A ng)mL
Multiple Cal. data Filenames:
PF55G 058S050
PFS5G_O50SO62 PFS5GJ358S0B0 PFS5G_058S081
COMPOUND
LAB FUG'
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
0066 U
0 073 387
1.10 0342 0151 0 033 U 7 07 15 8
0.266 0.0336 00904
0,0183 00181 0.0074 0 0105 00033 0 0500 00542 0250
1 91
3 97 5 38 577 610 644 6 81
5 54 6.25
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FUG*
SPIKE CONC.
(ng)
120 12 0
CONC. FOUND
(ng)
10.5 102
R t% )a
RETENTION TIME
87 2 852
538 6 10
(1) U = not detected (2) R (%) = Percent recovery
15B25FFD2_2 xd. sts
Approved by:
.QA/QC Chemist
10-05-2005
dd-mm-yyyy
)JK> A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0. sox 2719. 7045Mats to Wf5t, StDHPf, 11 , CANADAVBl 3SBTit (250) 5551100 FAX(250) 4SI 5811
PAXYS METHFOD M U -0O31 Rev 01 S
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
(DUPLICATE)
Sample Collection:
23-Mar-2005 17:50
Lab Nemo; AXYS ANALYTICAL SERVICES
Contract No.: Matrix:
4191 SERUM
Lab Sample ID: Sample Size:
WG15625-1Q4 (DUP L7714-6R (A)) 100 mL
Sample Receipt dele: 29-Mar-2005
Initial Calibration Date:
BRACKETING CAL
Extraction Date;
2t-Apr-2005
Instrument ID:
LC-MS/MS
Analysis Date:
22-Apr-20Q5
Time: 7:02:23
LC Column ID:
C18, Zorbax XDB
Extract Volume (mL): 2
Sample Datafile:
PFS5GJ158S072
Injection Volume (pL}; 30 0
Blank Data Filename:
PFS5G_058S02e
Dilution Factor: Concentration U n its :
N/A ng/mL
Multiple Cal. data Filenames:
PFS5GJ058S050 PFS56J058S062 PFSBG_058S060 PFS5G,,058S081
COMPOUND
LAB FUG1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
0 074 U
0 109 3,46 1.11 G356 0116 0021 u 734 14 8
0109 0 0279 0 0883 00260 0 0165 0.0207 0 0054 00171 0 0556 0122 0144
204
3 78 5.34 5 73 605 638 6 72
5 50 6.22
LABELED COMPOUND
13C-PFOA 13CPFDA
LAB FUG1
SPIKE CONC.
(B)
12 0 120
CONC. FOUND
(n0)
9.97 107
R (V.)*
RETENTION TIME
83.1 534 89 4 6 06
(1) U a not detected (2) R (%) - Percent recovery
isbispfoz^z us. sie
Approved by:.
QA/QC Chemist
1O-0M005
dd-mfTvyyyy
0)JP A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0 BOX221?. 2045 JUS(0 WEST. SiPMfYBC,MIO* m 3SBTU(250) 455-5800FAX(2501 45558! 1
AXYS METHOD MLA-031 Rev 01
PFOS_Si,,OB
Forni 1A12
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
23-Mar-2005 17:55
Lab Name: AXYS ANALYTICAL SERVICES
Contract No,:
4191
Lab Sample ID;
L7714-1R
Matrix:
SERUM
Sample Size:
100 mL
Samplo Receipt date: 2&*Mar-2005
Initial Calibration Date:
BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID:
LC-MS/MS
Analysts Date;
22-Apr-2005
Time: 6:23:45
LC Column ID:
C18, Zofbax XDB
Extract Volume (mL): 2
Sample Datafile:
PFS5G_058SQ69
Injection Volumo (pL); 30 0
Blank Data Filename:
PFS5G_05BS025
Dilution Factor Concentration Units :
N/A ng/ml
Multiple Cal. data Filenames:
PFS5GJ358S050 PFS5GJD5SS062 PFS5G,,058S060 PFS5G_O58SO01
COMPOUND
LAB FLAG1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
0102 U u
3.39 0 907 0 269 0159 0 030 u 207 14.9
0.182 00324 0.0624 D03B7 00244 0 0083 0.0037 0 0082 0 130 0 0509 0 0927
208
5 38 5 73 6 10 6.40 6.76
552 6 22
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG'
SPIKE CONC.
|ng)
12 0 120
CONC. FOUND
(ngj
9 73 138
R(%>*
RETENTION TIME
81 1 115
5 36 6 10
(1) U ~ not detect! (2) R (%) Percent recovery
i5625PF02j.*ii S16
Approved by.
P A /Q C Cliem tst
10-05-200S
dd-mm-yyyy
A X Y S A . M / \ L Y T T O A . L S E R V I C E S L T D ro 60X 2?t5. 2015 Mills M WIST. SIDKtT, BE., UKJtSAVil 3SBi l l (25D) iSSiSOOf (750) 555 501)
3Z
AXYS METHOD MLA-031 Rev 01
PFos s i _ds
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Lab Name; AXYS ANALYTICAL SERVICES
Sample Collection;
15-Mar-2005 12:05
Contract No.;
4191
Lab Sample ID:
L7685-4R
Matrix:
SERUM
Sample Size:
100 mL
Sample Receipt dale;
17-Mar-2005
Initial Calibration Date:
BRACKETING CAL
Extraction Date;
21-Apr-2005
Instrument ID:
LC-MS/MS
Analysis Date:
22-Apr-2005
Time: 6:45:06
LC Column ID;
C18, ZorbaxXDB
Extract Volume (mL): 2
Sample Datafile;
PFS5GJ058S066
(njectlon Volume (pL): 30 0
Blank Data Filename:
PFS5G_058S026
Dilution Factor; Concentration U n its:
N/A ng/mL
Multiple Cal- data Pilonamos;
PF55GJ058S050 PFS5GJJ58S062 PFS5GJW8S080 PFS5Gj058S081
COMPOUND
LAB FLAG1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPoA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
0 088 U U
2.40 0633 0 288 0118 0 033 U 2,34 120
0,165 0 0529 0.106 00406 00274 0 0153 0 0094 0 0044 0 0783 0.0919 0 157
\
2 04
5 34 5.73 6.08 638 6 76
5.49 622
LABELED COMPOUND
13C-PFA 13C-PFDA
LAB FLAG1
SPIKE CONC.
fog)
120 120
CONC. FOUND
fog)
11.0 122
R (%)'
RETENTION TIME
91 5 101
534 6 06
(1) U = not detected (2) R (%) = Percent recovery
15625PFD2J2 ids, si 3
Approved by;.
QA/QC Chemist
10-05-2005
tfd-mm-yyyy
)]{(<> A X Y S A x r x l / ^ L V T I O V L S E R V I C E S L T D PO BOX1219. J0 ttlUSSOWIST. SlflWY. BC. CMO*VAL3SII m SO) 5S-SBOOft SOI 45SS8II
3
AXYS METHOD MLA-031 Rev 01
FF0S_S1 DB
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
U b Name: AXYS ANALYTICAL SERVICES
Sample Collection:
15-Mar-2QQ5 12:10
Contract No-: Matrix: Sample Receipt dale: Extraction Date; Analysis Date; Extract Volume (mL):
4191 SERUM 17-Mar-2005 21-Apr-2005 22-Apr-20Q5 2
Time: 5:32:09
Lab Sample ID: Sample Star. Initial Calibration Date; Instrument ID: LC Column ID: Sample Datafile;
L7685-2R 100 mL BRACKETING CAL LC-MS/MS CIS, Zorbax XDB PFS5G,,058S065
Injection Volume (pL): 30 0
Blank Data Filename:
PFS5G,,058S026
Dilution Factor; Concentration U n its:
N/A ng/mL
Multiple Cal. data Filenames:
PFS5G_0S6S050 PFS5G,,058S062 PFS5G_058S080 PFS5GJ058SOB1
COMPOUND
LAB FLAG1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPaA PFHxA
PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
0 057 U
0,179 610 1.18 0501 0150 0047 U 2 28 43 7
0217 0.0741 0.0395 00486 0.0214 0 0088 0.0219 00024 0 0882 0.246 0 410
204
3B4 5 36 5.73 6 06 638 6.76
5 49 622
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG1
SPIKE CONC,
{fl)
120 120
CONC. FOUND
("0)
8.09 9,60
R (%>*
RETENTION TIME
674 5 36 800 6 06
(1) (J = not detected (2) R (%) = Percent recovery
1SMSPFD2_2 ms S12
Approved by;.
.QA/QC Chemist
10-05 2005
dd-mm-yyyy
^3(( A X Y S > X M / X L V T I C Z A , L S E R V I C E S L T D M 80XZI.OU 111$HO. WfST.SlDMt. BC anmV8l3S81fl (750) l-BOOFJtX I250H5S-SSII
3+
AXYS METHOD MLA-031 Rev Ot
PFOS_5l_D2
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
CLIENT ID:
Sample C ollection:
15-Feb-2005 13:40
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID:
L7620-5
Matrix:
SERUM
Sample Size:
2.00
Sample Receipt Date: Extraction Date: Analysis Date:
18-Feb-2005 18-Feb-2005 18-Feb-2005
Time: 22:31:49
Initial Calibration Date: Instrument ID: LC Column ID:
17-Feb-2005 LC-MS/MS C18, ZorbaxXDB
Extract Volume (mL):
2
Sample Datafile:
PFS5GJJ2BS27
Injection Volume (pL): 30.0
Blank Data Filename:
PFS5G_028S17
Dilution Factor:
N/A
Cal. Ver. Data Filename: PFS5G 028S14
Concentration Units : ng/mL
COMPOUND
LAB FLAG1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U U U
0.243 6.78 0.978 0.228 0.067 U U U 5.27 10,5
1.49 0.777 0.0791 0.0179 0.261 0.0031 0.0021 0.0029 0.0170 0.0041 0.0197 0,0050 0.0586
3.37 4.88 5.38 5.72 6.03
5.28 5,96
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLAG '
SPIKE CONC.
(ng)
12.0 12.0
CONC. FOUND
(ng)
10.2 9.71
R (%)J
RETENTION TIME
85.3 80.9
4.88 5.72
(1) U = not detected (2) R (%) - Percent recovery
i6032PFOt_2.xls, S4
Approved by:
QA/QC Chemist
11-05-2005
dd-fnm-yyyy
A X Y S A N A L Y T I C A L S E R V I C E S L T D PO. BOX 2015 MILLSto WEST, SIDNEY, BC, CANADAVBL 3S8TEL(250) 655-S800FAX(250) 45558] t
AXYS METHOD MLA-031 Rev 01
pfos_s i_D2
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
CLIENT ID:
Lab Name: AXYS ANALYTICAL SERVICES
Sample Collection:
01 -Feb-2005 10:00
Contract No.: Matrix; Sample Receipt Date: Extraction Date: Analysis Date: Extract Volume (mL): Injection Volume fpL): Dilution Factor: Concentration Units :
4191 SERUM 02-Feb-2005 16-Fet>-2005 17-Feb-2005 2 300 N/A ng/mL
Time: 20:42:48
Lab Sample ID: Sample Size: Initial Calibration Date: Instrum ent tO: LC Column ID; Sample Datafile: Blank Data Filename: Cal. Ver. Data Filename:
L7602-4R i 2.00 17-Feb-2005 LC-MS/MS C18, Zorbax XDB PFS5G_027S44 PFS5G027S40 PFS5GJJ27S37
COMPOUND
LAB F LA G 12
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U u u u
2.01 0.578 0.135 0.032 u u u 4.36 22.4
2.50 0.730 0.306 0,0252 0.0256 0.0057 0.0060 0.0022 0.0213 0.0035 0.0350 0,0257 0.0709
4.64 5.38 5.72 6.04
5,28 5.98
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLA G 1
SPIKE CONC.
(ng)
120 120
CONC. FOUND
(09)
10.0 8,28
R [% Y
RETENTION TIME
83.5 69.0
4.84 5 72
(1) U = not detected (2) R (%) = Percent recovery
15t05PFDI_1 ris. S6
Approved by:
QA/QC Chemist
11-05-2005
dd-mm-yyyy
$)][( A X Y S A N A L Y T I C A L S E R V I C E S L T D PO, OX21t, 7MS wttsRi. WIST, SiDKE, B.C., UNJUMVBt 3S8Til (250; i 55-5800FU (250) S5SB11
AXYS METHOD MLA-031 Rev 01
p F O S S t _D2
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Semple Collection:
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID:
M atrix:
SERUM
Sample Size:
Sample Receipt Date: 10-Feb-2005
Initial Calibration Date:
Extraction Date:
16-Feb-2005
Instrum ent ID:
Analysis Date:
17-Feb-2005
Time: 17:40:35
LC Column ID:
Extract Volume (mL):
2
Sample Datafile:
Injection Volume (pL): 30.0
Blank Data Filename:
Dilution Factor:
N/A
Cal. Ver. Data Filename:
Concentration Units : ng/mL
CLIENT ID:
05-Feb-2005 09:02
L7609-9R i 2.00 17-Feb-20Q5 LC-MS/MS C18, Zorbax XDS PFS5G_027S30 PFS5GJJ27S40 PFS5G_027S20
COMPOUND
LAB FLAG *
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U U U
0.111 6.13 1.04 0.244 0.061 U U U 1.68 13.5
2.15 0.800 0.536 0.0765 0.0466 0.0095 0.0047 0.0014 0.0053 0.0046 0.221 0.0151 0.0874
3.10 4.80 6.38 5.76 6.06
5.28 5.99
LABELED COMPOUND
C13*PFOA C13-PFDA
LAB FLAG 1
SPIKE CONC.
()
12.0 12.0
CONC. FOUND
(nflj
9.88 10.0
R(%)2
RETENTION TIME
82.3 83.7
4.80 5.76
(1) U = not detected (2) R {%} = Percent recovery
15105PFDi_1.xls, $18
Approved by;
QA/QC Chemist
11-05-2005
dd-fnm-yyyy
C[C A X Y S A N A L Y T I C A L S E R V I C I E S L T D M . BOX 2219, IMS WUS ID. WIST. K t . D.C.. (MUDA VBl 3SB1EI (7S0) A55-SSOO FAX (2S0) KS-SBH
37
AXYS METHOD MLA-031 Rev 01
PFOS_st_D2
Form 1A/2
PERFLUORINATEO SURFACTANT ANALYSIS REPORT
Lab Name: AXYS ANALYTICAL SERVICES
Sample Collection:
Contract No.:
4191
Lab Sample ID:
M atrix:
SERUM
Sample Size:
Sample Receipt Date: Oa-Feb-2005
Initial Calibration Date:
Extraction Date:
16-Feb-2005
Instrum ent ID:
Analysis Date:
17-Feb-2005
Time: 16:09:38
LC Column ID:
Extract Volume (mL):
2
Sample Datafile:
Injection Volume (pL): 30,0
Blank Data Filename:
Dilution Factor:
N/A
Cal. Ver. Data Filename:
Concentration U n its : ng/mL
CLIENT ID:
05-Feb-2005 09:05
L7609-2R t 2.00 17-Feb-2005 LC -M S /M S C18, Zorbax XDB PFS5G_027S23 PFS5G_027S40 PFS5G_027S20
COMPOUND
LAB FLAG'
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U U U
0.099 4.34 0.588 0.163 0.141 U U U 2.66 14.0
1.66 1.19 0.339 0.0588 0.0439 0.0108 0.0167
0.0028 0.0290 0,0083 0.0341 0.0180 0.119
3.08 4.68 5.35 5.72 6.04
5.22 5.96
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLAG'
SPIKE CONC.
(no)
12.0 12.0
CONC. FOUND
<ng)
10.7 7.50
R (% )i
RETENTION TIME
89.1 62.5
4.68 5.72
(1) U = not detected (2) R (%) = Percent recovery
i5 iQ 5 P F D ij.*is .s ii
Approved by:.
QA/QC Chemist
11-05-2005 dtJ-mm-yyyy
CilC A X Y S / X M / V L Y T I O A J L . S E R N / I C Z E S L T D FO FOXm i , 2M5 MIUS RD. WSJ, SIDNEYB.C.. CANADAV8L3S8Ttt (250) 655-5DOOfAX(250) 455-581)
AXYS METHOD MLA-031 Rev 01
PF0SS1 02
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample C ollection:
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID: ,
Matrix:
SERUM
Sample Size:
Sample Receipt Date: 1CFFeb-2005
Initial Calibration Date:
Extraction Date:
16-Feb-2005
Instrum ent ID:
Analysis Date:
17-Feb-2005
Time: 17:27:36
LC Column ID:
Extract Volume (mL):
2
Sample Datafile:
Injection Volume (pL): 30.0
Blank Data Filename:
Dilution Factor:
N/A
Cal. Ver. Data Filename:
Concentration Units : ng/mL
CLIENT 10:
08Feb-2005 07:55
L7609-8R 1 2.00 17-Feb-2005 LC-MS/MS C1S, Zorbax XDB PFS5G_027S29 PFS5G_02?S40 PFS5G_027S20
COMPOUND
LAB FLAG1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U u u
264 45.7 0.706 0.229 0.115 u u u 5.40 19.7
3.08 0.768 0.460 0.0360 0.251 0.0125 0.0256 0.0033 0.0190 0.0144 0 0363 0.0065 0 0663
3.19 4.66 5.36 5 76 6.07
5.28 599
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLAG1
SPIKE CONC.
<ns)
12.0 12.0
CONC. FOUND
(ng)
10.5 9.98
R{% )2
RETENTION T IM E
87.1 83.2
4.86 5.76
(1 ) U = not detected (2) R (%) = Percent recovery
15105PFD1_1.*ls, S17
Approved by:
QA/QC ChBmist
11-05-2005 Od-mm-yyyy
A X Y S A N A L Y T I ( _ A L S E R V I C E S L .T D P.0. BOX221?. 2045 MILLS3 WIST, SIDMT. 6C, CANADAV8L358 IL (250) 55-5800 FAX(250) 55-5611
AXYS METHOD MLA-031 Rev 01
PFOSsi oa
Form 1A/2
PERFLUORtNATED SURFACTANT ANALYSIS REPORT
Sample Collection;
01-Mar-2005 15:45
Lab Name: AXYS ANALYTICAL SERVICES
Contract No,;
4191
Lab Sample ID;
L7652-7R2
Matrix;
SERUM
Sample Size:
1 00 mL
Sample Receipt date: 03-Mar-2005
Initial Calibration Date;
BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID:
LC-M5/MS
Analysts Date;
21-Apr-20O5
Time: 22:46:26
LC Column ID:
CIS, Zorbax XDB
Extract Volume (mL): 2
Sample Datafile;
PFS5GJJ5BS34
Injection Volume {pL): 300
Blank Data Filename;
PFS5GJ3S8S026
Dilution Factor: Concentration U n its :
N/A ng/mL
Multiple Cal, data Filenames:
PFS5G_058S029 PFS5G_058S038 PFS5G,,058S050
COMPOUND
LAB FLAG *
conc
FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFNxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
U 0084 0 618 33 2 0 978 0 358 0166 0038
u 10 3 59 5
0207 0.0818 0.0627 0 0408 00181 00250 00121 0 0140 0185 00140 0 131
2.53 3,80 5 32 5 69 608 6 38 672
5.52 6.22
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG1
SPIKE CONC.
(ng)
12 0 120
CONC. FOUND
tngi
10.1 13 6
R (%)s
RETENTION T IM E
8 4 0 5 32 113 6 06
(1) U = not delected (2) R (%) = Percent recovery
1562SPFDi _2 *is. 5
Approved by;.
QA/QC Chemist
10-05-2005 dd-fnrn-yyyy
C][(A X V S A N A L Y T IC A L SERVICES L T D rotDX2219,2045Mills(0.WEST,SIDNEY.H .WHAMVSl358IH(750)S5SBODFAX(750)55SOM
AXYS METHOD MLA-031 Rev 01
ffos s i db
Form 1A/2
PERFLUORJNATED SURFACTANT ANALYSIS REPORT
Sample Collection;
01-Mar-2005 15:45
Lab Name; AXYS ANALYTICAL SERVICES
Contract No.:
4151
Lab Sample ID;
L7652-8R2
Matrix:
SERUM
Sample Size;
100 mL
Sample Receipt date: 03-Mar-2005
Initial Calibration Date:
BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID;
LC-MS/MS
Analysis Date;
21-Apr-2005
Timo: 22:59:19
LC Column ID:
CIS, ZorbaxXDB
Extract Volume (mLJ: 2
Sample Datafile:
PFS5GJJ585035
Injection Volume (pL): 300
Blank Data Filename:
PFS5GJJ58S026
Dilution Factor Concentration U n its :
N/A ng/mL
Multiple Cal. data Filenames:
PFS5G_058S029 PFS5GJJ58S038 PFS5G_058S050
COMPOUND
LAB FLAG*
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPaA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
U U
0.822 191 0 850 0 243 0075 0025 U 7 19 429
0. ISO 0.0471 0 0549 00402 00157 0 0108 00094 0,0095 00840 0.0834 0 0497
3.87 5 32 5.69 6.02 6 36 672
5.49 618
l a b e l e d COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG'
SPIKE CONC.
(nfl)
120 120
CONC. FOUND
(ng)
11 3 13,1
R ("/.)*
94.3 109
RETENTION TIME
5 32 BOB
(1) U = not detected (2) R (%) " Percent recovery
1562SPFQ1J2 >d*. S7
Approved by:
QA/QC Chemist
10-05-2005 rftl'fnm-yyyy
<>)][(& A X Y S A N A L Y T I C A L S E R V I C E S L T D M BOX7?t9 204SItti 10 WT SIDNEY, t . CANADAV8L3S TEI [250) 655-5800FAX(ISO) 655-5111
AXYS METHOD MLA-031 Rev 01
pfos_s \ db
Forni 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection*.
01-Mar-2005 15:45
Lab Name; AXYS ANALYTICAL SERVICES
Contract No.:
4181
Lab Sample ID:
L7652-10R2
Matrix:
SERUM
Sample Size:
100 mL
Sample Receipt date; 03-Mar-2005
Initial Calibration Date:
BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID:
LC-M5/MS
Analysis Date:
22-Apr-2005
Time: 0:07:21
LC Column ID:
C10, ZorbaxXDB
Extract Volume (mL); 2
Sample Datafile:
PFS5Gw05flS040
Injection Volume (pL): 30 0
Blank Data Filename:
PFS5GJ058S026
Dilution Factor. Concentration U n its :
N/A ng/mt
COMPOUND
LAB FLAG1
CONC FOUND
Multiple Cal. data Filenames:
DETECTION UMfT
PFS5Gj058S029 PFS5G_058S038 PFS5GJD58S050
RETENTION TIME
/
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
U U
0 356 446 1 36 0521 u 0045 u 8 12 604
0 287 00785 0.0646 0 0515 0 0107 0 0390 0891 0.0046 0 249 0 0475 0 195
3.83 5.49 5 89 622
8.90
5.66 636
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG'
SPIKE CONC.
ng)
12,0 12.0
CONC. FOUND
(n9
133 129
R (%)3
RETENTION TIME
111 549 106 622
(1) U = not detected (2) R (%) = Persemi recovery
i50Z5PFDi_2ids. S3
Approved by:.
QA/QC Chemist
10-05-2005 tJd-mm-yyyy
A X Y S A N A L Y T I C A L S E R V I C E S L T D CO BOX2I , 01S (USRD WEST, SIDNEY. BC,CANADAV813SBHI (2S0) 55-5BOOFAX1250) 555B11
AXYS METHOD MLA-031 Rev 01
pfos, s i_D2
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
CLIENT ID:
Lab Name: AXYS ANALYTICAL SERVICES
Sample Collection:
12-Feb-2005 10:15
Contract No.: M atrix:
4191 SERUM
Lab Sample ID: Sample Size:
L7620-2 i (A) 2.00
Sample Receipt Date: Extraction Date: Analysis Date; Extract Volume (mL): Injection Volume (pL): Dilution Factor:
15-Feb-2005 16-Feb-2005 17-Feb-2005 2 30.0 N/A
Time: 18:19:41
Initial Calibration Date: Instrum ent ID: LC Column ID: Sample Datafile: Blank Data Filename: Cal. Ver. Data Filename:
17-Feb-2005 LC-MS/MS C18, ZorbaxXDB PFS5G_027S33 PFS5G_027S40 PFS5G_027S20
Concentration Units : ng/mL
COMPOUND
LAB FLAG *
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U u u
0.282 23.1 0.913 0.288 0.081 u u u 7.72 17.0
2.16 0.916 0413 0.0365 0.151 0.0093 0.0078 0.0033 0.0260 0.0035 0.0987 0.0080 0.117
3.17 4.84 5.38 5.76 6.07
5.28 5.99
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB F LA G 12
SPIKE CONC.
(no)
12.0 12.0
CONC. FOUND
("9)
9.73 10.2
R {%)*
RETENTION TIME
81.0 85.2
4.84 5.76
(1) U=not detected
(2) R (%) = Percent recovery
15105PFDl_1.xls, S21
Approved by:
QA/QC Chemist
11-05-2005 rtd-mm-yyyy
A X Y S /M 'nI L Y T K W L S E R V IC E S L T D P.0 BOX2219.20ASMILLS(D,WEST.SIDNEY,B.(.,CANACAV8 3SBTil (2501 ASSHOOfAX(250)S5S-5BH
AXYS METHOD MLA-031 Rev 01
pfos_s i_d2
Farm 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
CLIENT ID:
Lab Name: AXYS ANALYTICAL SERVICES
Sample C ollection:
12-Feb-2005 10:15
Contract No.: Matrix: Sample Receipt Date: Extraction Date: Analysis Date: Extract Volume (mL): Injection Volume (pL): Dilution Factor: Concentration Units :
4191 SERUM 15-Feb-2005 16-Feb*2005 17-Feb-2005 2 30.0 N/A ng/mL
Time: 18:32:40
Lab Sample ID: Sample Size: Initial Calibration Date: Instrum ent ID: LC Column ID; Sample Datafile: Blank Data Filename: Cal. Ver. Data Filename:
WG15105-1051 2.00 17-Feb-2005 LC-MS/MS C18, Zorbax XDB PFS5G_027S34 PFS5G_027S40 PFS5G,,027S20
COMPOUND
LAB FLAG'
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U U U
0.304 24.0 0.965 0.310 0.104 U U U 8.18 17.1
2.81 1.41 0.336 0.0289 0.111 0.0076 0.0024 0.0203 0.0240 0.0033 0.214 0.0155 0.287
3.19 4.84 5.38 5.76 6.06
5.28 5.99
LABELED COMPOUND
C13-PFOA C13-PFDA12
LAB FLAG'
SPIKE CONC.
(nfl)
12.0 12.0
CONC. FOUND
(ng)
8.19 7.73
R (%>*
RETENTION TIME
68.3 64.4
4.84 5.76
(1) U = not detected (2) R (%) = Percent recovery
15105PFD1_i J(ts, S22
Approved by:
QA/QC Chemist
11-05-2005 dd-fnm-yyyy
C( A X Y S A N A L Y T IC A L S E R V IC E S L T D P.0. BOX 2219. 2WS MILLS ID.WEST, SIDNEY, B t.. U M M V 8 L 3S8TEL (2S0) A5-S6Q0 FAX (H W 4SS-SIU
AXYS METHOD M U -031 Rev 01
FF0SJS1 DB
Form ifiJ2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection;
01-Mar-200514:00
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lsb Sample ID;
L7652-9R2
Matrix:
SERUM
Sample Size;
100 mL
Sample Receipt date: 03-Mar-2005
Initial Calibration Date;
BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID:
LC-MS/MS
Analysis Dale:
21-Apr-2005
Time: 23:17:46
LC Column ID:
C l8, ZorbaxXDB
Extract Volume (mLJ:
2
Sample Datafllo:
PFS5GJI58S036
Injection Volume (pL): 30 0
Blank Data Filename:
PFS5G,,058S026
Dilution Factor: Concentration U n its :
N/A ng/mL
Multiple Cal. data Filenames:
PFS5G 058S029 PFS5GJJ5BS038 PFS5G_058S050
COMPOUND
LAB FLAG1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
U 0100 247 SB.7 0849 0 294 0120 0 043 0,267 10 1 617
0.148 0 0783 0.0404 00433 00089 0 0246 0 0096 Q0063 0203 0.0199 0192
2,64 4 10 5 41 5 77 6 10 6.40 6 76 304 5 58 625
LABELED COMPOUND
13CPFOA 13C-PFDA
LAB FLAG1
SPIKE CONC.
ing)
12,0 12 0
CONC. FOUND
(ng)
11 3 12 5
RW 3
RETENTION TIME
94 1 104
5.40 6.10
(1) U = not detected
(2) R (% ) * Percent recovery
i5B25PFDi^2tda, SB
Approved by:
GA/QG Chemist
10*05-2005 ddmnvyyyy
<&][( A X Y S / \ M / \ L V T I O \ L S E R V I C E S L T D ro 1017717 20 MILLSRD. W5T S1DHX BC. CAHAOAVBl 3SBI (2S0I 6SS SSOOFAX(20) S5-5BM
AXYS METHOD MLA-031 Rev 01 pfos_s i_D2
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
CLIENT ID:
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
M atrix:
SERUM
Sample Receipt Date: 03-Feb-2005
Extraction Date:
16-Feb-2005
Analysis Date:
17-Feb-2005
Time: 21:21:22
Extract Volume (mL):
2
Injection Volume (pL): 30.0
Dilution Factor:
N/A
Concentration U n its : ng/ml
Sample Collection:
02-Fsb-2005 11:15
Lab Sample ID: Sample Size: Initial Calibration Date: Instrum ent ID: LC Column ID: Sample Datafile: Blank Data Filename: Cal. Ver. Data Filename:
L7602-7R i 2.00 17-Feb-2005 LC-MS/MS C18. Zorbax XDB PFS5GJJ27S47 PFS5G_027S40 PFS5G_027S37
COMPOUND
LAB FLAG'
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U U U
0.179 4.97 0.934 0.285 0.217 U U U 2.19 16.3
2.00 0.968 0.439 0.0422 0.0657 0.0081 0.0047 0.0029 0.0270 0.0047
1.51 0.0141 0.0757
3.21 4.84 5.38 5.76 6.06
5.28 5.99
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB F LA G 12
SPIKE CONC.
(n fl)
12.0 12.0
CONC. FOUND
(nfl)
10.3 10.2
R (% )7
RETENTION T IM E
85.8 85.0
4.84 5.76
(1) U = not detected (2) R (%} =Percent recovery
1510SPFO1_l .xls. S9
Approved by:.
QA/QC Chemist
11-OS-2005
dO-mm-yyyy
< ][> A X V S A N A L Y T IC A L S E R V T C I I H S LTCD PC fiOX2219, 2045 MILSRD WS1, SIOKt, IC, CANADAVBt 3S8TIL (250) A5S58TAX(750) 55-S811
4C,
AXYS METHOD MLA-031 Rev 01
pfs s i Da
Forni 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
30-Mar-2005 09:25
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID:
L7714-18R
Matrix:
SERUM
Sample Size;
100 mL
Sample Receipt dato;
01-Apr-2005
Initial Calibration Date:
BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID;
LOMS/MS
Analysis Date:
22-Apr-2005
Time: 7:53,54
LC Column ID:
C18, ZorbaxXDB
Extract Volume (mL): 2
Sample Datatila:
PFS5GJ58S76
Injection Volume (pL): 30 0
Blank Data Filename:
PFS5G_585026
Dilution Factor: Concentration Units :
NIA ng/mL
Multiple Cal. data Filenames;
PFS5GJJ5SS05D PFS5GJQ58S062 PFS5G_058SOBO PFS5G~05flS081
COMPOUND
LAB FLAG'
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
0119 U
0,155 7.38 0.75B 0 221 0 104 0 024 u 25 2 325
0.192 0.0756 0.0379 0 0379 0.0268 00161 00124 0.0147 0 0733 0.0283 0314
204
397 5 38 5 73 6 10 640 6 76
5 54 622
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG1
SPIKE CONC.
(ns)
12.0 12 0
CONC. FOUND
(ns)
9 58 9.37
R|%)*
RETENTION TIME
79 6 538 781 6 10
(1) U = not detected (2) R {%) Percent recovery
15B25PFD2_2*)s S23
Approved by:
.QA/QC Chemist
10-05-2005 dd-mrrvyyyy
A X Y S / \ M / \ L Y T I O \ L S E R V I C E S L T D W BOX1, 30 MIS ID. Wf5T, M l iC. UMikVit K8 Iti (35M&S55000 rw (350) tSSSBl 1
^7
pAfXoYsSsMi EdTbHOD MLA-031 Rev 01
Form 1A12
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Samp) Collodion:
30-Mar-2005 09:30
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID:
L7714-28R
M atrix:
SERUM
Sample Size;
100 mL
Sample Receipt date: 01-Apr-2005
Initial Calibration Date:
BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID:
LC-MS/MS
Analysis Date:
22-Apr-2005
Time; 8:19:39
LC Column ID:
C18, ZortoaxXDB
Extract Volume (mL): 2
Sample Datafile:
PF55G...058S78
Injection Volume (pL): 300
Blank Data Filename:
PFS5GJ058S02B
Dilution Factor: Concentration Units :
N/A ng/mL
Multiple Cal. data Fllonames:
PFS5GJJ58S050 PFS5GJJ58S062 PFS5GJJ58S080 PFS5G_058S081
COMPOUND
LAB FLAG**
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFflS PFHxS PFS
U U
0 053 6.42 1.02 0 297 0 206 0039 U 4 78 32 5
0125 0 0348 0 0487 00388 0.0186 0 0109 00143 0 0278 0 0866 0 0429 0465
3 81 540 5 77 6 10 6.40 6.76
S 54 622
LABELED COMPOUND
13C-PFOA 13C-PF0A
LAB FLAG*
SPIKE CONC.
(ng)
120 120
CONC. FOUND
(ng)
9 75 9 59
R i%)2
RETENTION TIME
81.2 799
5 40 6 10
( t) U ~ not detected (2) R {%) = Percent recovery
15625PFD2_2 rit, S2S
Approved by;.
_QA/QC Chemist
HWt-2005
dd-mm-yyyy
A X Y S A N A L Y T I C A L S E R V I C E S L T D RO BOX7219.104$ KlUS W WISTSIOHCY. 8C, UHAVil 3S8III (2501 *55-58001 (ISO) *S55111
AXYS METHOD M U -031 Rev 01
pfos_s i _ob
Form 1A2
PERFLUOR1NATED SURFACTANT ANALYSIS REPORT
Sample Collection:
26'Mar-2005 10:20
Lab Name: AXYS ANALYTICAL SERVICES
Contract No,:
4191
Lab Sample ID:
L7714-7R
Matrix: Sample Receipt date:
2 29'Mar-2005
Sample Size: Initial Calibration Date:
100 mL BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID:
LC-MS/MS
Analysis Dato:
22-Apr*2005
Tima; 7:15:16
LC Column ID;
C18, Zorbax XDB
Extract Volume (mL); 2
Sample Datafile:
PFSSG,,05BS073
Injection Volume (pL); 30 0
Blank Data Fitoname;
PFS5GJD58S026
Dilution Factor: Concentration Units :
N/A ng/mL
Multiple C al data Filenames:
PFS5G_05BS050 PFS5GJ356S062 PFS5G--O58S0B0 PFS5G O58SO0I
COMPOUND
LAB FLAG-*
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
0 102 U u
197 2 75 0 582 0294 0 086 u 19 6 108
0 0973 0138 00207
00213 0 0127 0 0156 00100 0 0113
0 0862 0 0142 0.190
204
536 5 73 606 6,38 6 72
552 622
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FUG*
SPIKE CONC.
(ne)
120 120
CONC. FOUND
(no)
11.0 11 9
R <%)a
RETENTION TIME
920 99 5
5,36 6 06
(1) U " notdelected (2) R (%) = Percent recovery
i56Z5PFD2_2 S20
Approved by:.
QA/QC Chemist
10-05-2005 ddmm-yyyy
^J[i0A X Y S A N A L Y T IC A L SERVICES L T D f.OBO275?.2045MtUSJtDWIST.Sl6WUt.au*vatSSSIII SW(SS-SSOOfAXUSO)HS-Sill
AXYS METHOD MLA-031 Rev 01
p f o s _51_db
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Lab Name: AXYS ANALYTICAL SERVICES
Sample Collection:
26-Feb-200510;05
Contract No,: Matrix:
4191 SERUM
Lab Sample ID; Sample Size;
L7652-1R2 100
mL
Sample Receipt date: Extraction Date: Analysis Data:
02-Mar-2005 21Apr-2005 21-Apr-2005
Time: 22:07:20
Initial Calibration Date; Instrument ID; LC Column ID;
BRACKETING CAL LC -M S /M S C18. ZorbaxXOB
Extract Volume (mL); 2
Sample Datafile:
PFS5G_05BS031
Injection Volume (pL): 30 0
Blank Data Filename:
PFS5G,,05aS026
Dilution Factor: Concentration Units :
WA ng/mL
Multiple Cal. data Filenames:
PFS5G_058S029 PFS5G_058S03S PFS5G_05BS050
COMPOUND
LAB FLAG1
CONC FOUND
DETECTION UMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUftA PFDoA PFBS PFHxS PFOS
U u u
4 10 0 977 0.455 0 351 0066 u 2 87 17 3
0.215 0 0750 00435 00647 0 0382 0 0268 0 0043 00147
0 0775 00251 0.108
5.32 5,73 6.06 6 40 6.72
549 622
LABELED COMPOUND
13C-PFOA 13CAFDA
LAB FLAG'
SPIKE CONC.
(ng)
120 12.0
CONC. FOUND
{ng)
108 9 51
R (*)'
90 0 793
RETENTION TIME
5 32 6 08
{1) U = not detected (2) R (%) - Percent recovery
1SB25PF01_2 *ts. S3
Approved by:.
CWQC Chemist
1O-05-2DO5
ddmtn-yyyy
A X Y S A N A L Y T IC A L SERVICES LT D P.0 MX221?. 2045MAISMLWIST. SIOKft,i C, UMADAYtl 3STH(2S0t H5-SSOOFIX(25016S5S1)
so
AXYS METHOD MLA-031 Rev 01
pfos_s i_d2
Form 1A*2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
CLIENT ID:
Lab Name: AXYS ANALYTICAL SERVICES
Sample Collection:
03-Feb-2005 18:05
Contract No.: Matrix: Sample Receipt Date: Extraction Date: Analysis Date: Extract Volume (mL): Injection Volume (pL): Dilution Factor: Concentration Units :
4191 SERUM 08-Feb-2005 16-Feb-2005 17-Feb-2005 2 30.0 N/A ng/fnL
Time: 17:14:36
Lab Sample ID: Sample Size: Initial Calibration Date: Instrum ent ID: LC Column ID: Sample Datafile: Blank Data Filename: Cal. Ver. Data Filename:
L7609-6R i
2.00
mL
17-Feb-2005
LC-MS/MS
C18, Zorbax XDB
PFS5GJI27S28
PFS5G_027S40
PFS5G_027S20
COMPOUND
LAB FLAG1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U U u u
3.36 1.0S 0.361 0.166 u u u 2.99 21.4
224
0.939 0.346 0.0388 0.0582 0.0186 0.0044 0.0036 0.0250 0.0045 0.0591 0.0256 0 137
4.84 5.38 5.76 6,06
5.28 599
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLAG1
SPIKE CONC.
(ng>
12,0 12.0
CONC. FOUND
(nfl)
10.4 11.0
R {% f
RETENTION TIME
86.6 91.3
4.82 5.76
(1) U = not detected (2) R {%) = Percent recovery
15105PFD1 i xis. Si6
Approved by:
QA/GC Chemist
11-05-2005 dd-mm-yyyy
A X Y S A N A L Y T K ^ A L SER VIC ES L T D POBOX22'9.0A5MILLS*0.WISlSIDHIY,B.i,CAHABAV3L3S8HI (50)45S-S800FAX(25D)A5S-SS11
5
AXYS METHOD MLA-031 Rv 01
pfos. s i_db
Fonti 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Lab Name: AXYS ANALYTICAL SERVICES
Sample Collection:
00-Mar-2005 13:40
Contract No.; Matrix:
4191 SERUM
Lab Sample ID: Sample Site:
L7657-7R2 1.00
mL
Sample Receipt date: Extraction Date: Analysis Date: Extract Volume {m l):
10-Mar-2005 21-Apr-2005 22-Apr-2005 2
Time: 3:34:47
Initial Calibration Data; Instrument ID: LC Column ID: Sample Datafile;
BRACKETING CAL LC-MS/MS C l 8, ZorbaxXDB PFS5G_058S056
Inaction Volume (pL): 30.0
Blank Data Filename;
PFS5Gj058S026
Dilution Factor: Concentration Units :
NIA ng/mL
Multiple Ca|. data Filenames:
PFS5G_058S050 PFS5GJD58S0S2 PFS5G_058S0S0 PFS5G_0S8S081
COMPOUND
LAB FLAG'
CONC FOUND
DETECTION UMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
0052 U
0 259 6.90 0731 0.263 0 126 0026 u
508 196
0 166 0.0372 0 0292 00447 00092 0 0136 0,0119 00041 0 0314 0 068B 0 144
2 09
3 87 534 5 73 606 6 36 6 72
5 50 6 18
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG1
SPIKE CONC.
{ns)
12 0 12 0
CONC FOUND
(ng)
10-7 124
R (%)'
RETENTION T IM E
89 0 104
534 6 06
(1) U = not delected (2) R (%) = Percent recovery
i5025PfD2_2)d. SB
Approved by:
QA/OC ChemlBt
10-05-2005 dd-mm-yyyy
0 )][( A X Y S A N A L Y T I C A L S E R V A I C E S L T O P.O. BOX I , 2045 MILLS 10 WEST, SIOfET. 8 C . m m vet 3SI TEL (S 01 S-SBOO f (ISO) 5 5 S 1 1
Sx
AXYS METHOD MLA-031 Rev 01
pfos s t os
Form 1A/2
PERPLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collodion;
OB-Mar-2005 11:00
Lab Name; AXYS ANALYTICAL SERVICES
Contrad No.:
4191
Lab Sample ID;
L7652-25R2
Matrix;
SERUM
Sample Size:
100 mL
Sample Receipt date;
10-Mar-2005
Initial Calibration Date:
BRACKETING CAL
Extraction Date;
21-Apr2005
Instrument ID:
LC-MS/MS
Analysts Date:
22-Apr-20G5
Time; 1:24:26
LC Column ID;
C18, Zorbax XDB
Extract Volume (mL);
2
Sample Datafile:
PFS5G_Q58S046
fnjedlon Volume (pL): 30 0
Blank Data Filename:
PFS5G_058S026
Dilution FactorConcentration Units ;
N/A ng/mL
Multiple Cal. data Filenames:
PF55GJJ5SSD29 PFS5GJJ58S038 PFS5G_058S050
COMPOUND
LAB FLAG '
CONC FOUND
DETECTION LIMfT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
U U
0117 69 3 1 12 0.288 0 115 U U 18 9 102
0.181 0.114 0.0734 0.0541 00129 0 0157 0.0159 00377 0.0519 0 0749 0 171
3 67 534 5.73 6 06 6 38
5 50 622
LABELED COMPOUND
13C-FFOA 13C-PFDA
LAB FLAG*
SPIKE CONC.
(ng)
120 12 0
CONC. FOUND
<ngl
8 69 11 7
R<V.)J
RETENTION TIME
83 2 534 97 0 806
(1) U = not detected (2) R (% ) Percent recovery
15625PFD1 2 ids. S IS
Approved by:
QA/QC Chemist
10-05-2005 dd-mro-yyyy
A X Y S / A . h s i / ^ L . V n r i C > \ L S E R V I C E S L T D P.0 BOX11.20 MlllS 10 WESTSIOHEXBC. CAHMVBL3S8Ut 1250) SS-SftOOMX(250) 4555811
S3
AXYS METHOD M LA-031 Rev 01
pfos_s i Da
Form 1A/2
PRFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
08-Mar-2005 11:00
U b Name: AXYS ANALYTICAL SERVICES
Contract No.:
191
Lab Sample 10:
L7652-27R2
Matrix:
SERUM
Sample Size;
1 00 mL
Sample Receipt date;
10-Mar-2005
Initial Calibration Data:
BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID;
LC-MS/MS
Analysis Date;
22-Apr-20Q5
Time: 1:37:18
LC Column ID;
C18, Zorbax XDB
Extract Volume (mL): 2
Sample Datafile:
PFS5G_058SQ47
Injection Volume (pL): 30 0
Blank Data Filename:
PFS5GJ358S026
Dilution Factor: Concentration Units :
N/A ng/mL
Multiple Cal. data Filenames:
Pr55G_058S029 PFS5GJ05QS03Q PFS5GJD58S050
COMPOUND
LAB FLAG '
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
U u
0 839 786 107 0 486 0 199 0044 0117 17.3
112
0 312 0.103 0 0608 0,0510 0 0417 00168 0 0079 00102 0.0588 0128 0 204
387 5 38 5 73 6 06 6.40 8 76 304 552 622
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG*
SPIKE CONC.
(88)
120 120
CONC. FOUND
(ng)
8.60 9 43
R (V*)1
RETENTION TIME
73 3 78 5
5 36 6 06
(1) U = riot detected (2) R (%) = Percent recovery
i5625PfDi_2 4, s ib
Approved by:.
QA/QC Chemist
10-05-2005 dd-fnn-yyy/
A X Y S > \ f ^ / X L V T I C > \ L S E R V I C E S L T D M (OX721?. 201MIU5 M ttf$1. SIDNEY.8C, OtAWV81S8Tit (750) 4S5SS00fM (150S4S5-5011
AXYS METHOD MLA-031 Rev 01
pfos_s i_D2
Form 1A/2
PERFLUORINATEO SURFACTANT ANALYSIS REPORT
Lab Name: AXYS ANALYTICAL SERVICES
Sample C ollection:
Contract No.: M atrix: Sample Receipt Date: Extraction Date: Analysis Date: Extract Volume (mL): Injection Volume (pL): Dilution Factor: Concentration U n its :
4191 SERUM 02-Feb-2005 16-Feb-2005 IT-Feb-2005 2 30.0 N/A ng/ml.
Time: 20:04:02
Lab Sample ID: Sample Size: Initial Calibration Date: Instrum ent ID: LC Column ID: Sample Datafile: Blank Data Filename: Cal. Ver. Data Filename;
CLIENT ID:
01-Feb-2005 13:45
L7602-1R i 2.00 17-Feb-2005 LC-MS/MS C1B, 2orbax XDB PFS5G_027S41 PFS5GJ327S40 PFS5G_027S37
COMPOUND
LAB F LA G 12
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U U U
0.143 15.7 0.545 0.175 0.061 U U u
1.7 9.27
2.64 0.764 0.431 0.0237 0.157 0.0158 0.0095 0.0076 0.0180 0.0064 0.158 0.0990 0.0759
3.24 4.86 5.38 5.76 6.07
5.28 5.99
LABELED COMPOUND
C13-PFO C13-PFDA
LAB FLAG *
SPIKE CONC.
("9)
120 12.0
CONC. FOUND
("0)
10.2 9.46
R (%)*
RETENTION TIME
85,2 78.8
4.84 5.76
(1) U = not detected (2) R (%) = Percent recovery
15105PFD1_ t .xls, S3
Approved by:
QA/QC Chemist
11-05-2005 dd-mnvyyyy
)l'CS A X Y S A N A L Y T IC A L SERN/KZES L T D W BOXl, 2045 MIU5 *0 WEST, SIDNfT. U . HAM VBi 3S8111I2S0J 65$5800 NX S0) 655-5811
AXYS METHOD M U -031 Rev 01
PFOS S i Dfl
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sampln Collodion:
03-Mar-2005 13:55
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID;
L7652-12R2
Matrix:
SERUM
Sample Size;
100 mL
Sample Receipt date: 09-Mar-2005
Initial Calibration Date:
BRACKETING CAL
Extraction Date;
21-Apr-2005
Instrument ID:
LC-MS/MS
Analysis Date:
22-Apr*2005
Time: 0:20:16
LC Column ID:
C1, ZorbaxXDB
Extract Volume (mL): 2
Sample Datafile:
PFS5GJ58S041
Injection Volume (pL): 30 0
Blank Data Filename;
PFS5GJD58S026
Dilution Factor: Concentration Units :
N/A ng/mL
Multiple Cal. data Filenames:
PFS5G_05BS029 PFS5G_058S03fl PFS5gI o58S050
COMPOUND
LAB FLAG'
CONO FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
U U
154 42 3 1 26 0 371 0132
0 032 u
109 49 5
0.259 0.0311 00874 0 0580 0 0259 00234 00051 0 0062 0152 00252 0 107
3.88 5 35 5 73 6 10 6.40 877
5 52 6 25
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FU G '
SPIKE CONC
(ng)
12 0 120
CONC. FOUND
(ng)
10,4 11 7
R (%)*
RETENTION T IM E
864 97.7
536 6 10
(1) U = not detected (2) R <%) Percent recovery
i5025PFDi_z *)#, Sid
Approved by:.
.QA/QC Chemist
10*05-2005 ddmnvyyyy
A X Y S A N A L Y T IC A L SERVICES LTD f.O BOX2219.3045 MIUS WIST. SIQHIY,I C. HAD*YBl SBTL (250) 4555*00fAX (250) iSSSBIl
AXYS METHOD MLA-031 Rev 01
PF0S_S1_D2
Form 1A12
PERFLUORINATED SURFACTANT ANALYSIS REPORT
CLIENT ID:
Sample C ollection:
03-Feb-2005 16:00
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID;
L7609-4R i
Matrix:
SERUM
Sample Size;
2.00
Sample Receipt Date: 08-Feb-2005
Initial Calibration Date:
17-Feb-2005
Extraction Date: Analysis Date:
16-Feb-2005 17-Feb-2005
Time: 16:48:46
Instrum ent ID: LC Column ID:
LC-MS/MS C18, Zorbax XDB
Extract Volume (mL): Injection Volume (pL):
2 30.0
Sample Datafile: Blank Data Filename:
PFS5G_027S26 PFS5G_027S40
Dilution Factor:
N/A
Cat- Ver. Data Filename: PFS5G_027S20
Concentration Units : ng/mL
COMPOUND
LAB F LA G 12
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U u u
0.494 16.4 1.40 0.285 0.179 u u u 3-57 22.1
3.35 0.919 0.443 0.0489 0.101 0.0114
0.0122 0.0082 0.0210 0.0112 0.0775 0.0090 0.0811
3.15 4.84 5.38 5.76 6.07
5.28 5.99
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLAG1
SPIKE CONC.
(ng)
12.0 12.0
CONC. FOUND
(ng)
9.18 7,94
R ('A)1
RETENTION TIME
76.5 66.1
4.84 5.76
(1) U=not detected
(2) R (%) = Percent recovery
1510SPFD1_1.xls. S U
Approved by:
QA/QCChemist
11-05-2005 dd-mm-yyyy
A X Y S /XXI LVT-ICVXL S E R V IC E S LTTO POSOX771, 7045 MIILS. ESI,SIDNEY.B.C.,CUUUVIL358 TEL(250)55-5800 FM(750)55-5811
57
AXYS METHOD MLA-031 Rev 01
pfos_s i _D0
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample C ollection:
11-Mar-2005 15:00
Lab Name: AXYS ANALYTICAL SERVICES
Contract No,;
4191
Lab Sample ID:
L7657-18R2
Matrix: Sample Receipt date:
SERUM 15-Mar-200S
Sample Size; Initial Calibration Date:
100 mL BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID:
LC-MS/MS
Analysis Date:
22-Apr-2Q05
Time: 4:13:44
LC Column ID;
CIS. ZorbaxXDB
Extract Volume (mL): 2
Sample Datafile;
PFS5GJJ58SB5B
Injection Volume (pL): 30 0
Blank Data Filename;
PFS5G_058S026
Dilution Factor; Concentration Units :
N/A ng/mL
Multiple Cat. data Filenames:
PFS5G_058S050 PFS5G,,05BS062 PFS5G~Q58S080 PFS5G~058S081
COMPOUND
LAB FLAG'
CONC FOUND
DETECTION LIMIT
RETENTION TIME
FFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
0009 0029 0 308 222 0.936 0.351 0 149 0043 U 4 69 46 1
0.158 0.0695 0150 00423 0 0239 00139 00037 0 0182 0 0700 0.0594 0 284
209 261 3.86 5.35 5 74 607 638 677
5 51 622
LABELED COMPOUND
ISC'PFOA 13C-PFDA
LAB F L A G ''
SPIKE CONC.
too)
120 12,0
CONC. FOUND
(ng)
8.40 928
R <%)*
RETENTION TIME
700 5 33 773 6 07
(1) U not detected (2) R {%) - Percent recovery
15G25Pfdz_2 xii. S9
Approved by:.
.QA/QC Chemist
ID 05-2005 dd-mnv-yyyy
(S][(0 A X Y S / \ N J > X L . V T 1 0 \ L S E R V I C E S L T D FO BOX2?IF. 20 MILLS10 WEST. SIDNEY, .C. CANADAV6t 3SBTtl (250) A5SSB0QF (250) 1555811
AXVS METHOD MLA-031 Rev 01
pfos_S1_db
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
28-Mar-2005 11;36
Lab Name: AXYS ANALYTICAL SERVICES
Contract No,;
4181
Lab Sample ID:
L7714-9R
Matrix: Sample Rocelpt date: Extraction Date;
SERUM 29*Mar-2005 21-Apr-2005
Sample Size: Initial Calibration Data; Instrument ID;
100 mL BRACKETING CAL LC-MS/MS
Analysts Date: Extract Volume (mL):
22-Apr-2D05 2
Time: 7:28:09
LC Column ID: Sample Datafile:
CIO, ZotbaxXDB PFS5GJJ58SD74
Injection Volume (pL): Dilution Factor: Concentration U n its :
300 N/A ng/mL
Blank Data Filename;
PFS5G_05BS026
Multiple Cal. data Filenames:
PFS5G_05BS050 PFS5gI058S062
PFS5GJ)58S080 PFS5GJ358S081
COMPOUND
LAB FUG'
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA
PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
U 0062 192 77 5 134 0421 0085 0 018 0165 18.6 784
0.254
00983 0 322 0 0371 0 0363 0.0305 0 0201 0 0057
0 291 0 0448 0.847
244 3 73 534 5 73 606 6 38 6 72 2 78 5 50 618
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG1
SPIKE CONC.
(ng)
120 120
CONC, FOUND
(ng)
9 72 116
R {%)'
RETENTION TIME
81 0 96 8
5 34 6,06
(1) U = not detected (2) R (%} = Percent recovery
is&25PF02^z is. S21
Approved by:.
,QA/QC Chemist
1O-0S-2005 dd-mrn-yyyy
A X Y S A N A L Y T IC A L SERVICES L T D fO BOX7219. 04S10$ ID WIST. SIDWT. B.C. CANADAVSI3S III (ISO) 55-5800FAX(2501 55$01)
sy
AXY5 METHOD M U -031 Rev 01
pfob s i d&
Form 1A/2
PERFLUOR1NATED SURFACTANT ANALYSIS REPORT
Sample Collection:
28-Mar-2005 11:40
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4181
Lab Sample ID;
L7714-11R
Matrix:
SERUM
Sample Size:
1.00 mL
Sample Receipt date: 29-Mer-2005
Initial Calibration Date:
BRACKETING CAL
Extraction Cato:
21*Apr-2005
Instrument ID:
LC-MS/MS
Analysis Date;
22-Apr-2005
Time: 7:41:01
LC Column !0;
C16, ZofbaxXDB
Extract Volume (mL):
2
Sample Datafile:
PFS5GJD58S075
Injection Volume (pL): 30 0
Blank Data Filename:
PFS5G_058S026
Dilution Factor: Concentration Units ;
N/A ng/mL
Multlplo Cal. data Filenames:
PFS5GJQ58S05Q PFS5G_05flS062 PFS5GJJ58S080 PFS5GJ35BS081
COMPOUND
LAB FUG1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
0122 0 053 188 121 1.04 0.457 0060 0011 U 33 4
109
0220 00825 0.0544 0 0542 0 0325 0 0108 0 0120 0 0207 0 115 0 0833 0 782
2 03 251 3 86 5.36 574 6 07 6 38 6 77
5.53 622
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FUG1
SPIKE CONC.
(ng)
120 12 0
CONC. FOUND
(ng)
9.25 9 31
R(%)J
RETENTION TIME
77 1 77 6
5 36 6 07
(1) U = not detected (2) R (%) = Percent recovery
SB75PFD2,,2 art, S22
ADDroved bv:
QA/QC Chemist
10-05-2005 dd-rtvTvyyyy
)][( A X Y S A N A L Y T I C A L S E R V I C E S L T D fO SO* 221?, 2045 MIUS RD WS1 SIDHfT. BC. CAKAMVBL358 Tft (750) (55 5600 FAX(750) (55 5811
AXYS METHOD MLA-031 Rev 01
pfos_s i_D2
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
CUENT ID:
Lab Name: AXYS ANALYTICAL SERVICES
Sample C ollection:
05-Feb-2005 10:50
Contract No.: Matrix: Sample Receipt Date: Extraction Date: Analysis Date: Extract Volume (mL): Injection Volume (pL): Dilution Factor: Concentration Units ;
4191 SERUM 08-Feb-2QQ5 16-Fet>-2Q05 17'Feb-2005 2 30.0 N/A ng/mL
Time: 16:22:51
Lab Sample ID: Sample Size: Initial C alibration Date: Instrum ent ID: LC Colum n ID: Sample Datafile: Blank Oata Filename: Cal. Ver. Data Filename:
L7609-3R i (A) 2.00 17-Feb-2005 LC-MS/MS C18, Zorbax XDB PFS5G_027S24 PFS5G_027S40 PFS5G__027S20
COMPOUND
LAB FLAG*
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA
PFBS PFHxS PFOS
U u u
0.284 4.68 1.03 0.372 0.148 u u u 2.20 12.0
2.97 0.799 0.552 0.0491 0.0382 0.0140 0.0066 0.0068 0.0330 0.0085 0.0480 0.0187 0.0387
3.21 4.84 5.38 5.76 6.07
5.28 5.99
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB F LA G 12
SPIKE CONC.
(nfl)
12.0 12.0
CONC. FOUND
(8)
10.7 10.0
R (%)*
RETENTION TIME
89.1 83.4
4.84 5.76
(1) U = not detected (2) R (%) = Percent recovery
1!i105PFD1_l xta, S12
A p p ro v e d by:
QA/QC Chemist
11-05-2005 dd-mm-yyyy
A X Y S /A -r^/K LY T IC ^X L S E R V IC E S LTTO P.0. SOX 221?, 2015 MILLS *0 WEST, SIDNEY, E C. CWUDA Vit SSE Tt 12SC> 4SS-S8O0 FIX (2S0) 6SS-S811
AXYS METHOD MLA-D31 Rev 01
pfos_Si _D2
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID:
Matrix:
SERUM
Sample Size:
Sample Receipt Date: 0B-Feb-2005
Initial Calibration Date:
Extraction Date:
16-Feb-2005
Instrum ent ID:
Analysis Date:
17-Feb-2005
Time: 16:35:46
LC Column ID:
Extract Volume {mL>: 2
Sample Datafile:
Injection Volume (pL): 30,0
Blank Data Filename:
Dilution Factor:
N/A
Cal. Ver. Data Filename:
Concentration Units ; ng/mL
CLIENT ID:
05-Feb-2005 10:50
WG15105-104 i 2.00 17-Feb-2005 LC-MS/MS C18. Zorbax XDB PFS5GJ27S25 PFS5G_027S40 PFS5G_027S20
COMPOUND
LAB FLAG'
CONC FOUND
DETECTION UMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U u u
0.325 4.68 0.944 0.368 0.145 u u u 2.72 11.5
2.54 0.764 0.348 0.0493 0.0428 0.0096 0.0064 0.0172 0.0200 0.0088 0.102 0.0166 0.142
3.17 4.78 5.35 5.72 6.04
5.24 5.98
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLAG1
SPIKE CONC.
(00)
12.0 12.0
CONC. FOUND
(ng)
10,3 8.93
R (%)J
RETENTION TIME
85.4 74.4
4.78 5.72
<1) U = not detected (2} R (%) = Percent recovery
1lO S P FD I^t xlS, S13
A pproved by:
b r * ? --- -
QA/QC Chemist
11-05-2005 dd-mm-yyyy
/ X X V S A N A L Y T K Z A L S E R X / I C f S L T O PO BOX 19. IMS Mills H>. WIST, SIDNEY, B C, UNtDAMl 35B TEI [2S0) S5-S600 FAX iZSO) 55-5811
AXYS METHOD MLA-031 Rev 01
pfos si_D2
Form 1A/2
PERFLUOR1NATED SURFACTANT ANALYSIS REPORT
Sample C ollection:
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID:
Matrix:
SERUM
Sample Size:
Sample Receipt Date: 10-Feb-2005
Initial Calibration Date:
Extraction Date:
16-Feb-2005
Instrum ent ID:
Analysis Date:
17-Feb-2005
Time: 17:53:55
LC Column ID:
Extract Volume (mL):
2
Sample Datafile:
Injection Volume (pL): 30.0
Blank Data Filename:
Dilution Factor:
N/A
Cal. Ver. Data Filename:
Concentration U n its : ng/mL
CLIENT ID:
05-Feb-2005 10:00
L7609-10R i 2.00 17-Feb-2005 LC-MS/MS C18, Zorbax XDB PFS5G_027S31 PFS5G_027S40 PFS5G 027S20
COMPOUND
LAB FLAG 12
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U U U
0.392 24.5 0.894 0.250 0.084 U U U 6.40 37.2
2.61 0.687 0.422 0.0315 0.170 0.0214 0.0039 0.0100 0.0170 0.0074 0.123 0.0137 0.0802
3.21 4.86 5.38 5.76 6.07
5.28 5.99
LABELED COMPOUND
C13-PFOA C13-PFDA
LA8 FLAG '
SPIKE CONC.
(9)
12.0 12.0
CONC. FOUND
(ng)
10.2 10.2
R (%)*
RETENTION TIME
84.9 84.7
4.84 5.76
(1) U = not detected (2) R (%) = Percent recovery
l5105P FD 1_l.xls, S19
Approved by:
_ /f e ****? * -
QA/QC Chemist
11-05-2005
dd-mm-yyyy
C ( A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0 80X221?. 2015 MltlS ID. WtSL SIDNEY. B.C, fMMM Y8L3S Ift f?SOI iSS-580ff FK (750) ASSSS1
AXYS METHOD MLA-031 Rev 01
pfos_s i_D2
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample C ollection:
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID:
Matrix:
SERUM
Sample Size:
Sample Receipt Date: 15-Feb-2005
Initial Calibration Date:
Extraction Date:
16-Feb-2005
Instrum ent ID:
Analysis Date:
17-Feb-2005
Time: 18:45:31
LC Column ID:
Extract Volume (mL):
2
Sample Datafile:
Injection Volume (pL): 30.0
Blank Data Filename:
Dilution Factor: Concentration Units :
NL'A nij/mL
Cal. Ver. Data Filename:
CLIENT ID:
11 Feb-2005 11:40
L7620-3 1
2.00
mL
17-Feb-2005
LC-MS/MS
C l 8, Zorbax XDB
PFS5GJJ27S35
PFS5GJJ27S40
PFS5G_027S20
COMPOUND
LAB FLAG `
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA
PFBS PFHxS PFOS
U U U
0.192 6.09 0.753 0.188 0.067 U U U 1.80 17.7
2.78 0.803 0.268 0.0418 0.0456 0.0074 0.0039 0.0097 0.0120 0.0120 0.0494 0.0096 0.0508
3.19 4.82 5.38 5.72 6.06
5.28 5.99
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLAG'
SPIKE CONC.
(ng)
12.0 12.0
CONC. FOUND
(n9)
9.81 9 47
R(% )12
RETENTION TIME
81.7 79.0
4.82 5.72
(1) U = not detected (2) R {% ) = Percent recovery
1S10SPF01_1 .Is, S23
A pproved by:.
-- ___1
QA/QC Chemist
1HJ5-200S dd-mm-yyyy
A X V S A . r - 'J A L Y T I C A L S E R V I C E S L T D P.D BOX2211. 2045 MILLSRD. ESI SIDMI, S.C.. CANAPAV8L 3SB111 (250! 65S-SS0& FAX(2S0) 455-SB11
AXYS METHOD MLA-031 Rev 01
PfOS s i db
Forni 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
15-Mer-2005 14:00
Lab Name; AXYS ANALYTICAL SERVICES
Contract No.:
41B1
Lab Sample ID;
L7685-7R
Matrix:
SERUM
Sample Size:
1.00 mL
Sample Receipt date:
17-Mar~2005
Initial Calibration Date:
BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID:
LC-MS/MS
Analysts Date:
22-Apr-2005
Tims: 5:57:59
LC Column ID:
C18. Zorbax XDB
Extract VolumB (mL): Injection Volume (pL):
2 30 0
Samplo Datafile: Blank Data Filename:
PFS5GJI58S087 PFS5GJD58S026
Dilution Factor; Concentration U nits:
N/A ng/ml.
Multiple Cat, data Filenames:
PFS5G 05BS050 PFS5GJ358S0B2 PFS5G__05BS030 PFS5g I058S0B1
COMPOUND
LAB FLAG1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
0.045 0085 1 71 749 0631 0.315 0 050 0 033 0 253 136 61 1
0102 0 171 0 0646 0 0354 0 0211 0 0135 0.0068 00140 0 0712 0.0617 0450
206 2 61 3 91 5 36 573 606 6 38 6.76 302 5 52 622
LABEUED COMPOUND
13C-PFOA 13C4PFDA
LAB FLAG1
SPIKE CONC.
(ng)
12 0 12.0
CONC. FOUND
(ng)
10 3 11 4
R(%)a
RETENTION TIME
856 536 953 6 06
(1) U = not delected (2) R (%) ~ Percent recovery
15625PFD2_2.rts. S u
Approved by:
QAIQC Chemist
10-05-2005 ddnvn-yyyy
A X Y S A N A L Y T I C A L S E R V I C E S L T D P.0 OXni. Q45 HUIS10. WEST, SUMY. 11, CANADAVSl S6TEI (KOI 55 S60OFAX(ISO) ISMBM
AXYS METHOD MLA-031 Rev 01
pfos S1 os
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection;
15-Mar-2005 14:00
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.;
4191
Lab Sample ID;
L76S5-9R
Matrix:
SERUM
Sample Sita;
100 mL
Sample Receipt date: Extraction Date: Analysis Date;
17-Mar-2005 21-Apr-2005 22-Apr-2005
Time: 6:10:52
Initial Calibration Date; Instrument ID; LC Column ID;
BRACKETING CAL LC-MS/MS C18, ZorbaxXDB
Extract Volume (mL): 2
Sample Datafile:
PFS5G_O5BS0GB
Injection Volume (yL): 300
Stank Data Filename:
PFS5G_058S026
Dilution Factor: Concentration Units ;
N/A ng/mL
Multiple Cal. data Filenames;
PFS5GJJ58S050 PFS5G_058S062 PFS5G_058SQ80 PFS5G~05flS081
COMPOUND
LAB FUG '
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFl/nA PFDoA PFBS PFHxS PFOS
0.061 0,070 0 779 388 0 805 0 355 0 064 0010 0144 761 47.6
00767 0 0302 0 0376 0 0161 00108 0 0277 0 0044 0.0121 0 0767 0 0440 0310
204 2 54 3 87 5 36 5 73 6 06 6 38 6 72 301 5.52 622
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FUG'
SPIKE CONC.
(nB)
12 0 12 0
CONC. FOUND
(no)
tl.O 11.5
R (%)3
RETENTION TIME
91 3 955
536 606
(1) U = not delected (2) R (%) - PercenI recovery
156Z5FFD2_2 id*. S15
Approved by:
QA/QC Chemist
10-05-20D5 dd-nwn-yyyy
)][> A X V S A N A L Y T I C A L S E R V I C E S L T D P.0 8DX2219.204SMILLSID WES!. SIDHFY. t C CANADAVBt KBTILSO] iSS5600 ftt50) iSSSBIl
AXYS METHOD MLA-031 Rev 01
pfos s i db
Form 1A/2
PERFLUORJNATED SURFACTANT ANALYSIS REPORT
Sample Collection:
M-Mar-2005 09:15
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID:
L7652-14R2
Matrix:
SERUM
Sample Size:
1-00 mL
Sample Receipt date: 09-Mar*2005
Initial Calibration Date;
BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID:
LC-MS/MS
Analysis Date:
22-Apr-2005
Time: 0:33:13
LC Column ID:
C18, Zorbax XDB
Extract Volume (mL): 2
Sample Datafile;
PFS5G_058S042
Injection Volume (pL): 300
Blank Data Filename:
PFS5GJJ58S026
Dilution Factor: Concentration U n its :
N/A ng/mL
Multiplo Cal. data Filenames:
PFS5GJ158S029 PFS5G 058S038 PFS5GJ158S050
COMPOUND
LAB F L A G "1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPoA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
U 0 099 1 80 59 9 1 61 0 392 0 259 0 048
U 10 5 710
0199 00786 0 0589 0-0342 00098 0 0126 00073 00049 0274 00540 0175
2 56 3 89 5 34 5 73 606 6 38 6 72
5 52 622
LABELED COMPOUND
13C-PFQA 13C-PFDA
LAB FLAG'
SPIKE CONC,
(ng)
12 0 12 0
CONC. FOUND
(ng)
9 73 11.2
R (%)3
RETENTION TIME
81 1 93 2
534 6 06
<1) U = not detected (2) R (%) = Percent recovery
15625PFD1.2 xls .S U
Approved by:.__
QA/QC Chemist
10-05-2005 dd'd im -yyyy
0))K A X Y S A N A L Y T I C A L S E R V I C E S L T D ?0 80* 2319, 01 MILLSID. WESTS1HET, BC. t i w m 3SBTIL (?501 55 5600 FAX(250) S55B11
7
AXYS METHOD M U -031 Rev 01
Pfos st os
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
04-Mar-2005 09:15
Lab Nam: AXYS ANALYTICAL SERVICES
Contract No.;
4191
Lab Sample ID:
L7652-16R2
Matrix;
SERUM
Sample Size:
100 m l
Sample Receipt date; 09-Mar*2005
Initial Calibration Date;
BRACKETING CAL
Extraction Date; Analysis Date:
21-Apr-2005 22-Apr-2005
Time: D:46:0S
Instrument ID: LC Column ID:
LC-MS/MS C18. ZortjaxXOB
Extract Volume (mL): 2
Sample Datafile;
PFS5G_058SD43
Injection Volume (pL): 30.0
Blank Data Filename;
PFS5GJD58S026
Dilution Factor: Concentration U n its;
N/A ng/mL
Multiple Cal. data Filenames:
PFS5GJ58S029 PFS5GJO50SO3B PFS5GJ058S050
COMPOUND
LAB FUG *
CONG FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA
PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
U u
0829 82.3 1,65 0 584 0 383 0 074 0 172 17.8 11B
0 148
0.0792 0 0594 00185 00093 00117 00121 00153 0 0726 00442 0126
3 91 5 38 5,74 6 07 6.38 6 72 2.96
5.53 622
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG1
SPIKE CONC.
(ne)
12.0 12 0
CONC. FOUND
(ng>
960 11.1
M%>*
80 0 92 2
RETENTION TIME
5 35 6 07
(1) U = not detected (2) R (%) - Percent recovery
1S025PFD1,,2 m, S12
Approved by:.
QA/QC Chemist
10-05-2005
dd-rrvn-yyyy
<3][C A X Y S / ^ v M / K L Y T I O K L S E R V I C E S L T D fO &0XHR, ItMS WUS M V/m, SIDNEY, at . UHWiVtt 3S6 m (150) 5 5SOOFAXt?50) 556I1
< ry
AXYS METHOD MLA-031 Rev 01
pros s i db
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
02-Mar-2005 09:30
Lab Name; AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID;
L7652-6R2
Matrix:
SERUM
Sample Size:
1.00 mL
Sample Receipt date: Oa-Mar-2005
Initial Calibration Date:
BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID:
LC-MS/MS
Analysis Date:
21-Apr-2005
Time: 22:33:33
LC Column ID:
C l 8, ZotbaxXOB
Extract Volume (mL): Injection Volume (pL):
2 30 0
Sample Datafile: Blank Data Filename:
PFS5G,,058S033 PFS5G_058S026
Dilution Factor: Concentration U n its;
N/A ng/ml
Multiple Cal. data Filenames:
PFS5G 058S029 PFS5G_C58S038 PFS5GJD58S050
COMPOUND
LAB FLAG1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
U U
0.101 6.96
1.15 0.169
0091 0,035 U 4 69 22.6
0.203 00831 00582 0 0195
0 0098 0.0227
0.0069 00041 0 0519 0150 00847
394 5.32 5.69 6.06 6.38 6.72
550 622
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG1
SPIKE CONC.
(ng)
12,0 12 0
CONC. FOUND
(ng)
108 127
R (%)*
RETENTION TIME
90.4 5 32 106 6 06
(1) U = not detected (2) R (%) = Percent recovery
1562$PF01_2x)s, S5
Approved by:_
.QA/QC Chemist
10-05-200$
dd-nvn-yyyy
)J[^ A X Y S A N A L Y T I C A L S E R V I C E S L T D HO BOX7119.20(5 MILLS*0 WEST, SIDKEt BC.UNJLDiVBl 3SBTil (2501 iSSBQOEM(250) 5SS811
AXYS METHOD MLA-031 Rov 01
PFOS S1J3B
Form 1A/2
PERFLUOR1NATEO SURFACTANT ANALYSIS REPORT
Samp! Collection:
10-Mar-2005 16:25
Lab Name; AXYS ANALYTICAL SERVICES
Contract No,;
4191
Lab Sample ID;
L7657-11R2
Matrix:
SERUM
Sample Site:
100 mL
Sample Receipt dBto:
15-Mar-2005
Initial Calibration Data;
BRACKETING CAL
Extraclio n Data;
21-Apr-2005
Instrumont ID:
LOMS/MS
Analysis Date: Extraci Volume (mL): Injection Volume (pL): Dilution Factor; Concentratlon U n its ;
22-Apr*2005 2 30.0 N/A ngfrnL
Time: 3:47:39
LC Column ID;
C18, ZcrbaxXDB
Sample Datafile:
PFS5G_058S057
Blank Data Filename;
PFS5G--58S026
Multiple Cat. data Filenames;
PFS5GJ358S050 PFS5GJ058SQ62 PFS5G_058S080 PFS5G~0B8S081
COMPOUND
LAB FUG '
CONO FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
U u
0 228 B 78 0950 0290 0 298 0 072
u 729 21 0
0 180 00340 0 0483 0 0385 0 0204 0 0079 0 0045 0 0057 0 0708 0 0466 0103
3 81 5 35 5 74 6 07 638 6 72
551 6 22
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG'
SPIKE CONC.
(nfl)
120 12 0
CONC. FOUND
(ng)
12 1 14 2
R
101 118
RETENTION TIME
5 35 607
(1) U = not detected (2) R (%) = Percent recovery
\ 5625PFD2_z jOs. S7
Approved by.
,,QA/QC Chemist
10-05-2005 dd-mm-yyyy
A X Y S A N A L Y T I C A L S E R N / I C T E S L T D M. BOX 221?. lots MUIS *0 M SI S10KE, B C. CAHWiVl 3SB1EL <7S01 55 5800 f*X (ISOI 455-5*11
7
AXYS METHOD MLA-031 Rev 01
PFOS ST_Da
Form 1A/2
PERFLUOR1NATED SURFACTANT ANALYSIS REPORT
Sample Collection:
Ofl.Mar-2005 18:10
Lab Name: AXYS ANALYTICAL SERVICES
Contract No*; Matrix: Sample Receipt date;
4181 SERUM 10-Mar-2005
Lab Sample ID: Sample Size: Initial Calibration Date;
17652-29R2 100 mL BRACKETING CAL,
Extraction Date;
21-Apr-2005
Instrument ID:
LC-MS/MS
Analysis Date:
22-Apr-2005
Timo: 1:50:11
LC Column ID:
C18, Zorbex XDB
Extract Volume (mL):
2
Sample Datafile:
PFS5GJQ58S048
Injection Volume (pL): 30 0
Blank Data Filename;
PFS5GJJ5BS026
Ollulton Factor: Concentration U n its ;
N/A ng/mL
Multiple Cal. data Filenames;
PFS5G_0S8S028 PPS5G_G5BS038 PFS5G_058S050
COMPOUND
LAB FLAG1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
U U
0 047 5,35 0 56B 0,180
0 051 0035 U 239 204
0 147 0 0599 00417 00424 0 0110 00087 0 0087 0.0100 0,0621 00142 0127
3 83 5 35 5 74 6 07 6 38 6 72
5-53 622
LABELED COMPOUND
13C-PFOA 13C-PFDA
UB FLAG1
SPIKE CONC.
(ne)
12 0 120
CONC. FOUND
(ng)
108 13 6
R (%)*
RETENTION TIME
90.4 5 35 114 6 07
(1) U = not delected (2) R (%) - Percent recovery
l5625PF01_2*fs. S17
Approved by:.
QA/QC Chemist
10-05*! DOS dd-mnvyyyy
iS[(0 A X V S A N A L Y T I C A L S E R V I C E S L T D M 0X121? 704& MILLStil WIST, SIDNEY, i C, UHMUVBL 3SBTEI (2SO) 55-5800 FAX(550) H5 5S11
AXYS METHOD MLA-031 Rev 01
pfos s i Da
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection;
10-Mar-2005 16:25
U b Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID:
L7657-13R2
Matrix:
SERUM
Sample Size;
1 00 mL
Sample Receipt date:
15-Msr-2005
Initial Calibration Date:
BRACKETING CAL
Extraction Data:
21 -Apr-2005
Instrument ID:
LC-MS/MS
Analysis Date;
22-Apr-2005
Time: 4:00:32
LC Column ID:
C18, Zorbax XDB
Extract Volume (m l):
2
Sample Datafile;
PFS5GJ358S058
Injection Volume (pL): 30 0
Blank Data Filename:
PF55G_058S028
Dilution Factor: Concentration U n its ;
WA ng/mL
Multiple Cal, data Filenames:
PFS5G_058S050 PFS5G_05BS062 PFS5G_O59SO0Q PPS5G_058S081
COMPOUND
LAB FLAG'
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA FFHxA FFHpA PFOA PFNA PFDA PFUnA PFOoA PFBS PFHxS PFOS
0 025 U
0.101 7.55 0 910 0.234 0117 0036 U 7 42 17,3
0 223 00645 0.0849 0.0302 00112 0 0330 00142
00137 0.0950 0.0B5B 0136
2-09
3 81 534 573 6.06 6 36 6 72
5.50 61B
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG'
SPIKE CONO.
(no)
12.0 120
CONC. FOUND
(ns)
11.4 13.1
R (%)*
RETENTION TIME
95,4 5 32 109 606
(1) U = not detected 12) R 1%) - Percent reccwery
156ZSPFD2,,2 xf*. s b
Approved by:
QA/QC Chemist
10-05-2005
dd-mm.yjryy
A X Y S A r v j A L Y T I C Z ^ U S E R V I C E S L T T O PO BOX2?17,70 Mills ID WEST 51DHE1, BC CBHBDB81 3SSTEI (ISO) SSSEDOFBX1250} 5 511
7^
AXYS METHOD MLA-031 Rev 01
PF0S_S1 DB
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection;
OB*Mar-2005 18:10
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.;
4191
Lab Sample ID;
L7652-23R2
Matrix:
SERUM
Sample Size;
100 mL
Sample Receipt date; 10-Mar-2005
Initial Calibration Date:
BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID;
LC-MS/MS
Analysis Date:
22-Apr-2005
Time; 1:11:35
LC Column ID:
C l8, ZorbaxXDB
Extract Volume (mL): 2
Sample Datafile:
PF55G_058S045
Injection Volume (pL); 30 0
Blank Data Filename:
PFS5GJJ58S026
Dilution Factor; Concentration U n its:
N/A ngfmL
Multiple Cat. data Filenames:
PFS5G_058S029 PFS5GJQ5BS038 PFS5GJI58S050
COMPOUND
LAB FLAG '
CONC FOUND
DETECTION UMfT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
U u u
3.14 0-427 0168 0 080 0 025 u 1 22 11.2
0169 0 0952 00358 0 0459 0 0164 00143 0.0 IBS
0 0194 0 0540 0.0525 0186
5 36 5 73 610 6.40 6 77
554 6 22
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG'
SPIKE CONC.
(nfl)
120 120
CONC. FOUND
<ng)
10 7 133
R (/.)*
RETENTION TIME
89 5 5 36 111 506
(1) U s not detected (2) R {%) = Percent recovery
1M25PFD1_2 ids. sia
Approved by;
.QA/QC Chemist
10-05*2005 cW-mm-yyyy
)][C A X Y S A N A L Y T IC A L SERN/ICIES L T D fo BOX119, 20 Wits ID WEST. StOWtT B( 1IMHVt 3S8 IR (2SQ) 4SS-5800 FAXIS0) 4SS5SU
?3
AXYS METHOD MLA-031 Rev 01
pfo s_s i- 02
F o rm 1 A /2
PERFLUOR1NATED SURFACTANT ANALYSIS REPORT
Sample Collection:
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID:
Matrix:
SERUM
Sample Size:
Sample Receipt Date: 02-Feb-2005
Initial Calibration Date:
Extraction Date:
16-Feb-2005
Instrum ent ID:
Analysis Date:
17-Feb-2005
Time: 20:16:57
LC Column ID:
Extract Volume {mL): Injection Volume (pL):
2 30.0
Sample Datafile: Blank Data Filename:
Dilution Factor:
N/A
Cal. Ver. Data Filename:
Concentration Units : ng/mL
CLIENT ID:
01-Feb-2005 13:15
L7602-2R i
2.00
mL
17-Feb-2005
LC-MS/MS
C18, Zorbax XDB
PFS5G 027S42
PFS5G_027S40
PFS5GJ)27S37
COMPOUND
LAB F LA G 12
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U
u u
0.369 12.1 0.431 0.142 0.133 u u u 1.93 9.78
2.31 0.879 0.415 0.0381 0.0930 0.0062 0.0161 0.0022 0.0150 0.0053 0.0612 0.0125 0.0358
3.22 4.84 5.38 5.76 6.07
5.28 5.99
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLAG1
SPIKE CONC.
<ng)
12.0 12.0
CONC. FOUND
(nfl)
10.0 9.14
R (%)*
RETENTION TIME
83.6 76 1
4.84 5.76
(1) U = not detected (2) R (%) = Percent recovery
15105PFP1_t.xls, S4
Approved by:
<2 '
QA/QC Chemist
11-OS-2005
dd-mm-yyyy
g][C A X Y S A l ^ i / U J Y T I t ^ L S E R V I C E S L T D P.0 BOX 2 2 tt, 2(H5 M lltS ED WEST. SIBNEIf. .C., tANAM V81 3S8 T ft (250) 455-5800 FAX (250) 655-5811
7/
AXYS METHOD MLA-031 Rev 01
pfos_s i_d2
Form 1A12
PERFLUORINATED SURFACTANT ANALYSIS REPORT
CLIENT ID:
Lab Name: AXYS ANALYTICAL SERVICES
Sample Collection:
01-Feb-2005 13:15
Contract No.: M atrix: Sample Receipt Date: Extraction Date: Analysis Date: Extract Volume (mL): Injection Volume (pL): Dilution Factor: Concentration U n its :
4191 SERUM 02-Feb-2005 16-Feb-2005 17-Feb-2005 2 30.0 N/A ng/mL
Time: 20:29:56
Lab Sample ID: Sample Size: Initial Calibration Date: Instrum ent ID: LC Column ID: Sample Datafile: Blank Data Filename: Cal. Ver. Data Filename:
L7602-3R i 2.00 17-Feb-2005 LC-MS/MS C18, Zorbax XDB PFS5G_027S4J PFS5G_027S40 PFS5G_027S37
COMPOUND
LAB FLAG 12
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U U U
0.206 14,3 0.549 0.149 0.067 U u u 2.10 6.90
1.94 1.41 0.387 0.0350 0.0761 0.0048 0.0034 0.0118 0.0164 0.0066 0.0780 0.0110 0,0321
3,24 4.86 5.38 5.76 6.06
5.28 6.01
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLAG 1
SPIKE CONC.
(rtg)
12.0 12.0
CONC. FOUND
(ng)
8.97 8.77
R {%)*
RETENTION TIME
74.8 73.1
4.86 5.76
(1) U = not delected (2) R (%) = Percent recovery
`5105PFD1_1.xJ5.S5
Approved by;
ez -
QA/QC Chemist
11-05-2005
(W-mm-yyyy
A X Y S / V - M / V L V X I C Z A L S E R A / I C T E S l _ X D P.a SOX221, 2045 MILLS IO. WST, SIOttiT, Si,, CANADA81358 TIL (250) 55-S8CQFAX(250) S5-S8M
75"
AXYS METHOD MLA-031 Rev 01
pfos_s 1jc >2
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample IQ:
M atrix:
SERUM
Sample Size:
Sample Receipt Date: 19-Feb-2005
Initial Calibration Date:
Extraction Date:
21-Feb-2005
Instrum ent ID:
Analysis Date:
21-Feb-2005
Time: 16:20:21
LC Column ID:
Extract Volume (mL):
2
Sample Datafile:
Injection Volum e (pL): 30.0
Blank Data Filename:
Dilution Factor:
N/A
Cal. Ver. Data Filename:
Concentration Units : ng/mL
CLIENT ID:
17-Feb-20Q5 18:30
L7620-7
2.00
mL
17-Feb-2005
LC-MS/MS
C18, Zorbax XDB
PFS5G_029S09
PFS5G 029S08
PFS5GJJ29S05
COMPOUND
LAB F LA G 12
CONC FOUND
DETECTION U M iT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U u u
0.070 3,54 1,22 0.311 0.158 0.026 u u 1.92 8,51
1.55 0.743 0.118 0.0219 0.193 0,0072 0.0042 0.0063 0.0114 0.0048 0.0564 0,0074 0.0399
3.41 4.92 5.38 5.76 6.06 6.41
5.31 5.99
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLAG1
SPIKE CONC.
("9)
12.0 12.0
CONC. FOUND
(n g )
10.9 11.2
R(%>'
RETENTION TIME
90.5 93.1
4,90 5.76
(1) U = not detected (2) R (%) = Percent recovery
15143PfD1_1.xls. S3
Approved by:
* QA/QC Chemist
11-06-2005 dd-mnvyyyy
C J lO A X Y S A N A L Y T IC A L SERN/ICTES L T D P.0. BOX l , 7045 MILLS O. S I , 9 H K , i t-, CANADA V0L SS TL (?50) 655 5800 FAX (S0> 4SS-S8U
AXYS METHOD M U -031 Rev 01
pfos Si D8
Form 1AJ2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
02-Mar-2005 15:30
Cab Name; AXYS ANALYTICAL SERVICES
Contract No.: Matrix; Sample Receipt date: Extraction dataa: Analysis dataa; Extract Volume (mL): Injection Volume (pL): Dilution Factor Concentration U n its;
4191 SERUM O4-Msr-2005 21-Apr-2005 22-Apr-2005 2 30.0 N/A ng/mL
Tima: 2:42:48
Lab Sample ID:
L7657-1R2
Sample Size:
1.00 mL
Initial Calibration Date:
BRACKETING CAL
Instrument ID:
LC-MS/MS
LC Column ID:
C18, ZarbaxXDB
Sample data Filename:
PFS5G_05BS0S2
Blank data Filename:
PFS5G_05BS026
Multiple Cal. data Filenames:
PFS5G_05B5D5Q PFS5G--058S062 PFS5GJJ58S080 PFS5G_05BS081
COMPOUND
LAB FUG"
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
0.055 U
1 29 44,1 1.42 0 302 0090 0.031 U 118 55 2
0.146 00450 00822 0 0685 0 0153 00139 00149 0.0099 0.149 0 0743 0.491
209
3 79 534 5.73 6 06 638 6 72
5.52 622
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG'
SPIKE CONC.
(00)
120 12 0
CONC. FOUND
(ng)
9.49 120
R (%)*
RETENTION TIME
79.1 99 9
534 606
(1) U - not detected (2) R (%) = Percent recovery
15625PFD2,,2jd>. 52
Approved by:.
QWQC Chemist
1(MS-2005 dd-mm-yyyy
)][(0 A X Y S /\tM /V L .Y T T C I> M _ S E R V I C E S L T D M BOX2219. 20 AUU5ftp. WEST. SIMM BC. NUDAVBl 3S8TEI (2S0) S55B00 FAX(250) 4SSS811
AXYS METHOD MLA-031 Rev 01
pfos s i ds
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection;
02-Mar-20D5 13:17
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4101
Lab Sample ID:
L7657-3R2
Matrix:
SERUM
Sample Size:
TOO
mL
Sample Receipt date; 04-Mar-2005
Initial Calibration Date:
BRACKETING CAL
Extraction Date:
21-Apr-2005
Instrument ID:
LC-MS/MS
Analysis Datm
22-Apr-2005
Time: 3:09:01
LC Column ID:
CtS.ZorbaxXDB
Extract VolumB (mL); 2
Sample Datafile:
PFS5G_0585054
Injection Volume (pL); 30,0
Blank Data Filename:
PFS5G,,058S026
Dilution Factor. Concentration Units :
N/A ng/mL
Multiple Cel. data Filenames;
PFS5G_058S050 PFS5GJJ58SQ62 PFS5GJ15S080 PFS5G_058S081
COMPOUND
LAB FLAG1
CONG FOUND
DETECTION LIMIT
RETENTION TIME
FFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
0029 0046 0 652 371 1 13 0453 0259 0 045 U 112 51 1
0 138 OO70S 00459 00394 00127 0 0154 0 0062 00106 00536 0 0490 0473
2 04 2 54 3 89 5-34 5 73 606 638 6 72
5 50 622
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG1
SPIKE CONO.
(ng)
12.0 120
CONC. FOUND
(ng)
116 12,1
R (%)3
RETENTION TIME
97 0 5,34 101 6 06
(1) U = not detected (2) R (%) = Percent recovery
15B2SPFD2J2as. sa
Approved by._
QAJQC Chemist
10-05-2005
dd-mmyyyy
A X V S A N A L Y T I C A L S E R N / H C E S L T D Mi BOX221? 304$ ttlus ( WESTS1BKT, SC. OHM VBl S EL(7501 55 58(10FAX(750) 455-58)1
AXYS METHOD MLA431 Rev 01
pros s i oa
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
02-Msr-2005 13:15
Lab Nemo; AXYS ANALYTICAL SERVICES
Contract No.:
4191
la b Sample ID:
L7657-2R2
Matrix:
SERUM
Sample Size:
1-00 mL
Sample Recoipt date: 04-Mar-2005
Initial Calibration Dale;
BRACKETING CAL
Extraction Date;
21-Apr-2005
Instrument ID:
LC-MSfMS
Analysis Date: Extract Volume (mL):
22-Apr-2005 2
Time: 2:56:05
LC Column ID; Sample Datafile:
C18. ZorbaxXDB PF55G_O5BS053
Injection Volume (pL): 30,0
Blank Data Filename:
PFS5GJ05SS026
Dilution Factor: Concentration U n its ;
N/A ng/mL
Multiple Cal, data Filenames:
PFS5GJJ5BSQ50 PFS5G_05flS062 PFS5G.058S080 PFS5GJJ58S061
COMPOUND
LAB FUG '
CONC FOUND
DETECTION LiM rr
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
0124 U
1.26 117 1 49 0 599 0.212 0030 0 226 27,3 918
0 ISO 0152 00439 0 0388 00139 00175 0,0057 0-0101 0 0716 0 0272 0 850
200
3 87 5 33 570 6.07 6 36 6 77 3 01 5 51 8 18
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FUG'
SPIKE CONO.
(ig )
120 12,0
CONC. FOUND
(00)
118 12 8
R t%)3
RETENTION TIME
982 5 33 109 607
(1) U - not detected (2) R (% ) Percent recovery
i56Z5PFD2,,2 S3
Approved by;
.QWQC Chemist
10-05-2005 (td-mm-yyyy
<9][(* A X Y S Arvl/VL-VTIOVL SERVICES L T D P.0BOX2219.2045M1USHDWEST.S10HEY.Bf .ODUMVBL35*III (350)6555BOOf*X(350)*55-5811
79
AXYS METHOD MtA-031 Rev 01
pfos s i os
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
03-Mar~2005 16:07
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4131
Lab Semple ID;
L7652-18R2
Matrix: Sample Receipt date: Extraction Date; Analysis Date: Extract Volume (mL): Injection Volume (pL);
SERUM 09*Mar-2005 21-Apr-2005 22*Apr-2005 2 30 0
Time: 0:38:56
Sample Slxe: Initial Calibration Date: Instrument ID: LC Column ID: Sample Datafile: Blank Data Filename:
100 mL BRACKETING CAL LC-MS/MS C18, Zorbax XD8 PFS56J15BS044 PF55G,,058S026
Dilution Factor: Concentration Unite :
N/A ng/mL
Multiple Cal. data Filenames:
PFS5G_058S029 PF55GJ358S038 PFS5GJ058SO5Q
COMPOUND
LAB FLAG'
CONO FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUrtA PFDoA PFBS PFHxS PFOS
U U
0 092 6 95 108 0.352 0160 0041 U 322 43,1
0 297 00911 00750 0 0770 00464 00060 0.0843 00237 0144 00650 0.129
3 76 545 5 81 610 6 51 685
562 6.34
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG '
SPIKE CONO.
(ng)
120 120
CONC. FOUND
ino)
128 138
R (%)a
RETENTION TIME
106 5 45 115 6 18
(1) U = not detected (2) R (%) = Percent recovery
1502SFFO1 2xis, S13
Approved by:_
QA/QC Chemist
10-05-2005 dd-mm-yyyy
))[(< A X Y S A N A L Y T I C A L S E R V I C E S L T D PO BOX1?. 1015 MILLSIO. WEST, SIDNEYI f OHM V S* Wl 1750) 4555(00 ftt (750) 455SB11
SO
AXYS METHOD M U -031 Rev 01
pfos s i os
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
26.Feb.2Q05 10:06
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.: Matrix: Sample Receipt date; Extraction Date; Analysts Date; Extract Volume (mL): Injection Volume (pL): Dilution Factor: Concentration Units :
4191 SERUM 02-Mar-2005 21-Apr-2005 21-Apr-2005 2 30 0 N/A ng/mi
Time: 22:20:36
Lab Sample ID;
L7652-3R2
Sample Site:
100 mL
Initial Calibration Date:
BRACKETING CAL
Instrument ID;
LC-MS/MS
LC Column ID;
C1S, ZorbaxXDB
Sample Datafile:
PFS5G_056S032
Blank Data Filename:
PFS5G_058S026
Multiple Cal. data Filenames:
PFS5G,,058S029 PFS5G_Q58S038 PFS5GJ35BS050
COMPOUND
LAB FUG'
CONO FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA
PFOA PFNA FFDA PFUnA PFDoA PFBS PFHxS PFOS
U U U
3 69 0 895 0 354 0.416 0082 U 300 21 2
0178 OOB18 0.0414 00280 0.0189 00131 0 0248 00147 0116 0.0466 00812
5,.34 573 6 06 6.3B 6 72
5 52 622
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FUG1
SPIKE CONC.
(ng)
120 120
CONC. FOUND
(ngj
1t 6 126
96 5 105
RETENTION TIME
534 6 06
(1} ifnot detected
(2) R (%) a Percent recovery
iS625PF0i_2)ds S4
Approved by:
QA/QC Chemist
10-05-2005 Od-mm-yyyy
S> A X Y S A N A L Y T IC A L SERVICES L T D POBOX2W. 2045MISIDWSISiMiUC.ONAM81358III (2501655-5800NX(250)655-iBlt
8/
AXYS METHOD MLA-031 Rev 01
PFOS_S1 D2
Forni 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
CLIENT ID:
Sample Collection:
31-Jan-2005 10:00
Lab Name: AXYS ANALYTICAL SERVICES12
Contract No.:
4191
Lab Sample ID:
L7602-5R i
Matrix:
SERUM
Sample Size:
2.00
Sample Receipt Date: Extraction Date:
02-Feb-2005 16-Feb-2005
Initial Calibration Date: Instrum ent ID:
17-Feb-2005 LC-MS/MS
Analysis Date:
17-Feb-2005
Time: 20:55:47
LC Colum n ID:
C18, 2orbax XDB
Extract Volume (mL):
2
Sample Datafile:
PFS5G.027S45
Injection Volume (pL): 300
Blank Data Filename:
PFS5G.027S4Q
Dilution Factor;
N/A
Cal. Ver. Data Filename: PFS5GJJ27S37
Concentration U n its : ng/mL
COMPOUND
LAB FLAG *
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA
PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U U U
0.883 58.3
0.946 0,419 0.195 0.039 U 0.167 25.9 68.1
2.09 1.35 0,345 0.0256 0.327 0.0044 0.0138 0.0114 0.0071 0.0145 0.0730 0.0169 0.205
3.22 4.88 5.38 5.76 6.06 6.41
2.86 5.31 5.99
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLAG'
SPIKE CONC.
<"0)
12.0 12.0
CONC. FOUND
(na)
9.88 7.96
R(%)*
RETENTION TIME
82.4 66.3
4.86 5.76
(1) U - not detected (2) R (%} = Percent recovery
151fl5PFD1_1.xls, $7
Approved by;
QA/QC Chemist
11-05-2005 dd-mm-yyyy
A X VS A N A L Y T IC A L SERN/ICTES L T D PO.BOX7I9, 1045MUSID.WEST.SI0M.CCJUUMV8L358Kl I7S0)55SB0DFAX(2S0)655-5811
AXYS METHOD MLA-031 Rev 01
PF0$_S1_D2
Forni 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample C ollection:
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID:
M atrix:
SERUM
Sample Size:
Sample Receipt Date: 02-Feb-2005
Initial Calibration Date:
Extraction Date:
16-Feb-2005
Instrument ID:
Analysis Date:
17-Feb-20Q5
Time: 21:06:47
LC Column ID:
Extract Volume (mLj:
2
Sample Datafile:
Injection Volum e (pL): 30.0
Blank Data Filename:
Dilution Factor:
N/A
Cal. Ver. Data Filename:
Concentration U n its : ng/mL
CLIENT ID:
31-Jan-2005 10:00
L7602-6R i 2.00 17*Feb-2005 LC-MS/MS C18, Zorbax XDB PFS5C_027S46 PFS5G_027S40 PFSSG_027S37
COMPOUND
LAB F L A G 12
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U U U
0.746 39.8 0.902 0.368 0.160 U U 0.290 15.6 46.5
2.21 1.28 1.03 0.0443 2.36 0.0086 0.0070 0.0025
0.0210 0.0037 0.106 0.0091 0547
3.22 5.00 5.56 592 6.23
2.82 5.45 6.17
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLAG1
SPIKE CONC.
(ng)
12.0 12.0
CONC. FOUND
(ng)
9.16 8.04
R (%)*
RETENTION TIME
76.3 67.0
4.98 5.92
(1) U = not detected (2) R {%) = Percent recovery
15105PFDl_1.xls, S8
Approved by:_
QA/QC Chemist
11-05-2005 dd-mm-yyyy
CIS A X V S A N A L Y T K Z A L S E R V I C E S L T D PO BOX7219. 7C4SMILLSID. S1. SIDHT, I mm m 3S Ttt 1250) 55-5800 FAX(250) ASS-5811
83
AXYS METHOD M LA-031 Rsv 01
pfos s i oe
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection;
29-Mar-2005 09:15
Lab Name: AXYS ANALYTICAL SERVICES
Contract Ho.:
4191
Matrix:
SERUM
Sample Receipt data: 01-Apr-2005
Extraction Date:
21-Apr-2005
Analysis Date:
22-Apr-2005
Time: 8:08:47
Extract Volume (mL): 2
Injection Volume (pL): 30.0
Dilution Factor;
N/A
Concentration U n its : ng/mL
Lab Sample ID:
L7714-23R
Sample Size:
1.00 m l
Initial Calibration Date;
BRACKETING CAL
Instrument ID:
LC-MS/MS
LC Column ID;
C1Q, ZorbaxXDB
Sample Datafile:
PFS5G_058S077
Blank Data Filename:
PFS5G_05BS026
Multiple Cal. data Filenames:
PFS5G_05SS050 PFS5G 058S062 PFS5G..058S080 PFS5G_058S081
COMPOUND
LAB FLAG'
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS PFHxS PFOS
U u
0822 23.1 0 589 0 233 0 169 0.023 0,138 5,58 20 2
0.192 0 0301 0.0582 00631 00234 0.0077 0.0130 0 0025 0 0601 0785 0 255
3 89 5 36 5 73 610 6 40 6 76 284 5 52 622
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG'
SPIKE CONC.
(ng)
120 120
CONC. FOUND
101 124
R (V.)1
RETENTION TIME
841 536 104 6 10
(1) U ~ not detected (2) R {%) * Percent recovery
1562SPFDZJ! *js. SZ4
Approved by:.
QA/QC Chemist
10-05-2005 dd-mm-yyyy
C)][> A X Y S / V r v l / Y L Y T I O \ . L S E R V I C E S L T D f.O 60X22I. 2015 Mills RD WISESIDNEYSC, CWUBAVII 3SB111 (250) SSJSSOOFAX1250) A55SSI 1
sv
AXYS METHOD MLA-031 Rev 01
PFOS s i os
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection;
12-Mar-20G5 10:05
Lob Nome: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID;
L7657-20R2
Matrix: Sample Receipt date:
SERUM 15-Mar-2005
Sample Size: Initial Calibration Data:
100 m l BRACKETING CAL
Extraction Date:
21-Apr-2005
instrument ID:
LC-MS/MS
Analysis Date:
22-Apr-2005
Time: 4:26:41
LC Column ID:
C1S. Zorbax XDB
Extract Volume (mL): 2
Sample Datafile:
PFS5GJI5BS0B0
Injection Volume fpL): 30 0
Blank Data Filename;
PFS5G_058S026
Dilution Factor: Concentration U n its :
N/A ng/mL
Multiple Cat. data Filenames:
PFS5GJJ5BSQ50 PFS5GJJ58S062 PFS5G,,05BS080 PFS5G_058S081
COMPOUND
LAB FLAG1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA
PFOA PFNA PFDA PFUnA PFOoA PFBS PFHxS PFOS
0108 U
0 972 57 8 301 0346 0108 0 022 u 137 704
0 186 0 0454
00549 0.0365 0 0190 0 0141 0 008B 00051 0 0318 00405 0 339
2 01
3 92 536 573 6 06 6 36 6 72
5 52 622
LABELED COMPOUND
13C-PFOA 13C-FFDA
LAB FLAG*
SPIKE CONC.
(ng)
120 12 0
CONC. FOUND
(ng)
997 12 2
RI*/.)1
RETENTION TIME
83 1 102
5 3$ 6 06
(1} U s not detected (2) R (%) = Percent recovery
i S625pfoz,,Z i4 sio
Approved by:.
)i-- "
.QA/QC Chemist
10-05-2005 dd-mnt-yyyy
)][(A X Y S A N A L Y T IC A L SERVICES L T D MBOXW?. 2045MUISBDWEST,SIDH.BC.MMDVBl3SBtilCO)45S-SBOOFAX1250)4S5-SBIt
8S
AXYS METHOD MLA-031 Rev 01
PFOS S1 D8
Form 1A/2
PERFLUQRINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
12-Mar-2005 10:10
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.: Matrix: Sample Receipt date: Extraction Date:
4191 SERUM 15-Mar-2005 21-Apr-2005
Lab Sample ID: Sample Size: Initial Calibration Date: Instrument ID:
L7657-21R2 100 mL BRACKETING CAL LC-MS/MS
Analysts Date:
22Apr-2005
Time: 5:18:53
LC Column ID:
C18. ZorbaxXDB
Extract Volume (mL):
2
Sample Datafile:
PFS5GJJ5BS064
Injection Volume (pL): 30.0
Blank Data Filename:
PFS5GJ058S02S
Dilution Factor; Concentration U n its:
N/A ng/mL
Multiple CaK data Filenames:
PFS5G_058S050 PFS5G- 058S062 PFS5G O58S0BO PFS5GJJ5BS081
COMPOUND
LAB FLAG'
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA
PFHpA PFOA PFNA PFDA
PFUnA PFDoA PFBS PFHxS PFOS
0 053 U u
32.1 1,48 0290 0093 0032 u 11.7 57 6
0152 0.0295 00481 00521 00113 0 0054 0.0090 0 0054 00613 00206 0 528
204
5 38 5 77 6 10 640 6 76
554 6 22
LABELED COMPOUND
13C-PFOA 13C-PFDA
LAB FLAG1
SPIKE CONC.
(ns)
120 12 0
CONC, FOUND
(no)
11 1 113
R (%)*
RETENTION TIME
923 94 1
538 6 10
{1} U not detected (2) R {%) = Percent recovery
isez5FFDz_2 *)s. S11
Approved by:.
QA/QC Chemist
1005-200S dd-mm-yyyy
)I[( A X Y S A N A L Y T I C A L S E R Y / I C Z E S L T D f.O I 0X7719 lo ti MlttS ta tffSt, SIMfr. 8C WWM VI 3581EI (250) 455 5850 FAX(ISO) 455-5811
AXYS METHOD M U-031 Rev 01
PFOs s i oa
Form 1A/2
PERFLUOR1NATED SURFACTANT ANALYSIS REPORT
Sample Collection:
09-Mar-200514:30
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.;
4191
Lab Sampla ID;
L7657-5R2
M atrix:
SERUM
Sample Size:
100 rr
Sample Receipt date;
10-Mar-20Q5
Inltlat Calibration Date:
BRACKETING CAL
Extraction Date;
21-Apr-20Q5
Instrument ID;
LOMS/MS
Analysts Date;
22-Apr-2005
Time: 3:21:54
LC Column ID:
CIS, ZorbaxXDB
Extract Volume (mL):
2
Sample Datafile:
PFS5G,,05SS055
Injection Volume (pL); 30.0
Blank Data Filename;
PFS5GJJ58S026
Dilution Factor Concentration Units :
N/A ng/mL
Multiple Cat. data Filenames:
PFS5G_058S050 PFS5GJJ58SQ62 PFS5GJJ58S80 PFS5G.058S081
COMPOUND
LAB FLAG1
CONC FOUND
DETECTION LIMIT
RETENTION TIME
PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFBS
PFHxS PFOS
299 U
0 098 2 21 0 575 0193 0192 0027 u 4 10 7 88
0219 0.150 0 0495 0 0510 0 0103 0 0103 00182 00160 0125 0354 00917
1 87
3.92 5 36 573 6,06 6 38 6 72
5 52 622
U B E LE D COMPOUND
13C4PFOA 13C-PFDA
LAB FUG1
SPIKE CONC.
(ng)
12.0 120
CONC. FOUND
(ng)
11.1 12 3
R(%>*
RETENTION TIME
923 5 36 102 6 06
(1) U " not detected (2) R {%) = Percent recovery
15625PFD2_2 *is. S5
Approved by.
.QA/QC Chemist
10-05-2005 (KUnnvyyyy
li A X V S A N A L Y T I C A L S E R V I C E S L T D PO S0 321, 30 Mitts *0WIST. S im 81. WM Vt 358TEL13SO) 4555800Ft 1350) Si-5111
87
AXYS METHOD MLA-031 Rev 01
2pfos_s ij d
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection :
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ip :
M atrix:
BLOOD
Sample Size:
Sample Receipt Date: 18-Feb-2005
Initial C alibration Date:
Extraction Date:
02-Mar-2005
Instrum ent ID:
Analysis Date:
17-Mar-2005
Time: 5:10:26
LC Column ID:
Extract Volume (mL):
2
Sample Datafile:
Injection Volum e fpL): 30.0
Blank Data Filename:
Dilution Factor:
N/A
Cal. Ver. Data Filename:
Concentration U n its : ng/g (wet weight basis)
CLIENT ID:
15-Feb-2Q05 13:40
L7620-6 i2 2.00 17-Mar-2005 LC-MS/MS C l8, Zorbax XDB PFS5G_038S62 PFS5G_038S58 PFS5GJJ38S67
COMPOUND
LAB FLAG *
CONO FOUND
DETECTION LIMIT12
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
U u
4.22 0.538 u u u
u 4.14 7.95
0.879 0.578 0.445 0.233 0.234 0.132 0.0630
0.0750 0.335 0.148
4.94 5.45
5.38 6.11
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLAG'
SPIKE CONC.
(ng)
12.0 12.0
CONC. FOUND
(ng)
116 12.7
R <%)3
RETENTION TIME
96.8 106
4.94 5.79
(1) U = not detected (2) Detection limits are lab blank corrected (3) R (%) = Percent recovery
15215PFD1 2.xls, 54
Approved by:.
QA/QC Chemist
11-05-2005 dd-mm-yyyy
A X VS A N A L Y T K Z A L S E R V IC E S L T D ro BOX2719. ?04S MIUS to. WEST. SIDHfT, B.C.. CANADAV8L 3SBTil (250) 555800 FAX(250) 55-5811
89
AXYS METHOD MLA-031 Rev 01
pfos_s i_D2
Form 1A/2
PERFLUORINATED SURFACTANT ANALYSIS REPORT
Sample Collection:
Lab Name: AXYS ANALYTICAL SERVICES
Contract No.:
4191
Lab Sample ID:
M atrix:
BLOOD
Sample Size:
Sample Receipt Date: 19-Feb-2005
Initial Calibration Date:
Extraction Date:
02-Mar-2005
Instrum ent ID:
Analysis Date:
17-Mar-2005
Time: 5:23:26
LC Column ID:
Extract Volume (mL):
2
Sample Datafile:
Injection Volume (pL): 30.0
Blank Data Filename:
Dilution Factor:
N/A
Cal. Ver. Data Filename:
Concentration Units : ng/g (wet weight basis)
CLIENT ID;
17-Feb-2005 18:30
L7620-8 2 1.94 g (wet) 17-Mar-2005 LC-MS/MS C18, Zorbax XDB PFS5G_038S63 PFS5G_038S58 PFS5G_038S67
COMPOUND
LAB F LA G 12
CONC FOUND
DETECTION LIMIT*
RETENTION TIME
PFBA PFPeA PFHxA PFHpA PFOA PFNA PFDA PFUnA PFDoA PFTA PFBS PFHxS PFOS
1.28 0.760 2.98 0.779 0.275 0.139 U
0.443 2.43 8.30
0.906 0 595 0.416 0.240 0,241 0.136 0.0649
0.0773 0.345 0.118
2.51 3.43 4.96 5.45 5.80 6.14
3.02 5.38 6.12
LABELED COMPOUND
C13-PFOA C13-PFDA
LAB FLAG'
SPIKE CONC.
(ng)
12.0 12.0
CONC. FOUND
(ns)
11.5 10.5
R (% )3
RETENTION TIME
96.2 87.5
4.94 5.79
(1) U = not detected (2) Detection limits are lab blank corrected (3) R (%) = Percent recovery
15215PFD1_2.xls, S5
Approved by:
QA/QC Chemist
11-05-2005
dd-mm-yyyy
A X Y S / K r x l / K L V T ' I C Z > M _ S E R V I C F . S L T O PC. BOXI9 , 04S MIILS ID, WEST, SIDNEY, B.C., (AADAVil 3S8 Ut (250) 6S5-S8Q0 FAX(2S0) 455 5811
