Document omZ77v9r8nKr33p2EO4RYJLzo

................................................. J~ C lllffb C 3 A n a lytica l San/ices" P-1 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Project Data File Result Table Instrument Name Ewan's Projects\PFCs 021710\SamplesShort.wiff 021710short.rdb API 5000 Sample Name Acquisition Date Acquisition Method Injection Vial KQ1000664-03 2/18/2010 5:39:30 AM PFCkinetexShort.dam 47 Injection Volume Sample Type Dilution Factor Weight to Volume 5 Unknown 1.00 0.00 Results Summary Analyte Peak Name IS Name PFBA 1 13C-PFBA PFPeA 1 13C-PFHxA PFBS 1 180-PFHS PFHxA 1 13C-PFHxA PFHpA 1 13C-PFHxA PFHxS 1 180-PFHS SJ80-PFHS 13C-PFDA SJ3C-PFDA 13C-PFDA IS Area 5469400 6199200 3800700 6199200 6199200 3800700 4384200 4384200 Analyte RT (Exp RT ) 1.24 (1.27) 3.53 (3.60) 4.19 (4.26) 5.23 (5.31) 6.13 (6.23) 6.22 (6.32) 6.21 (6.31) 7.50 (7.65) Analyte Area 11064000 12889000 22525000 14747000 5449800 28400000 3800700 4384200 Calc. Cone (ng/mL) 19.30 21.90 18.30 24.40 25.00 26.00 1.07 1.00 Modified? No No No No No No No No 0 -a ' Page 137 of 169 222 Created with AnalysPf&porter Printed: 18/02/2010 4:02:00 PM IRC Summary Analyte Peak Name PFBA2 PFPeA2 PFBS2 PFHxA 2 PFHpA2 PFHxS2 SJ3C-PFBA S_13C-PFHxA RT (Exp RT ) 1.24(1.27) 3.53(3.60) 4.19(4.26) 5.23(5.31) 6.13(6.22) 6.22 (6.32) 1.24(1.26) 5.22(5.30) Area 11064000 12889000 9505500 1470200 15250000 12629000 5469400 6199200 M od ifie d ? No Calc (Exp) MRM Ratio 1.00(1.00) Ratio C onfirm s ID YES No 1.00(1.00) YES No 0.42 (0.40) YES No 0.10(0.10) YES No 2.80(2.90) YES No 0.44(0.40) YES No 0.49(13.20) No No 0.42(13.71) No Page 138 of 169 223 P-3 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Quantitative Peak Review KQ1000664-03 'fee 3 ^ 1; B lChrt S0s5 L a.s Lte ,,B t6e*S5 I! 3.S -5_ io \9C; 05 I 10 IS 3 15.6 2 10*6 5CMS 20 00*0 30 25 40 2gt 8'G9.r6t 60.5 40*5 20*5 .5 5.^ PFBA 7 13C-PFBA PFPe/Tl 213.0/169.0 Da Baseline Missed 217.0/172.0 Da q Baseline Missed 263.0/219.0 Da a Baseline Missed 4.6 n Wrnn4n.1P9 eak X- _____ n Wrnnn Peak_____ n Wrnnn Peak 6 . 2 1 30.S 5.23 25*. 1 Jtei 7i% 2*6 21 i*S* 1*6 __iS_____40I __45____SO__ lei 55 it) 65 70 "f* 16et S0*5 4S `o ;s PFBS 180-PFHS PFHxAl *c 299.0/80.0 Da 403.0/103.0 Da 313.0/269.0 Da Baseline d Missed o Baseline Missed Baseline Missed n Wrnnn Peak 6 .1 3 r Wrnnn Peak 14.C 1:* 5 .^ n Wrnnn Peak 6*6 6 . ^ 5e 6 i 3 '.a1, * 80*5 = t-te* 4te5 5 ** 6" 2 2*6 20*6 ________ 1 __________ 55 f.D 66 ?t) <5 6E 55 00 l6 SS 60 6S 70 13C-PFHxA 315.0/270.0 Da c Baseline c Missed 1fi I2* n Wrnnn Peak 5.^ 1tee * tel i1 60*5 S 405 20*5 OteO 45 St Si. 60 13C-PFHxA 315.0/270.0 Da c Baseline Missed n Wrnnn Peak 3*5 t.S ?s - US 6 .^ 1 * W5 l 4.5 5 j*S SS 6.0 55 ?a PFHpA i 363.0/169.0 Da Baseline Missed _____________ n Wronn Peak_____ <>s E. teS 1 H i 2 JeS 2*5 1*5- I a I $! 60 $5 T*m nw S 180-PFHS .' 0 403.0/103.0 Da BnasWerlinnnen Missed Peak_____ 13C-PFHxA 315.0/270.0 Da Baseline Missed n Wrnnn Peak IIoe a o.5 S0.5 - 4 0.s ?o.s i J 70 '5 SO 85 1 3C-PFDA 515.0/470.0 Da Baseline Missed - J 7 i W rnnn Peak_____ PFHxSI 399.0/80.0 Da Baseline Missed p Wrnnn Peak 1CM6 60.6 4CMS 1 i :o * s ' 70 75 SO 6 5 S 13C-PFDA 515.0/470.0 Da Baseline Missed n Wrnnn Peak_____ 180-PFHS 403.0/103.0 Da Baseline Missed n Wrnnn Peak -tee 7 .5 0 Ite S 5W 40.5 20*5 70 75 80 Ton mtn 35 13C-PFDA 515.0/470.0 Da BnasWerlinnnen Missed Peak Before A fter Page 139 of 169 224 / Y C o lu m b ia A n a lytica l Services" Created with AnalysPFffeporter Printed: 18/02/2010 4:02:00 PM Ion Ratio Confirmation ' 1.24 .......... .... [ 05 10 '5 .S4 :o6 5 ,5 .t | 1ttef 50*5 ... 3.53.......... 30 IS 40 45 PFBA2 213.0/169.0 Da Baseline c Missed Wrong Peak PFPeA2 263.0/219.0 Da Baseline Missed Wrong Peak 1 KQ1000664-03 4*6 a* 3*6 i3 2?6 16 PFBS2 299.0/99.0 Da Q Baseline Miss< Wrong Peak to*. 80*5 40ei/ :o*6 2 S*i a 20*6 -< f3 1.5*61 CM 5 0*5 00*0 1 PFHxA 2 313.0/119.0 Da Baseline c Missed o Wrong Peak femageisrioM afe PFHpA2 363.0/319.0 Da Baseline c Missed Wrong Peak PFHxS2 399.0/99.0 Da Baseline Missed c Wrong Peak S_13C-PFDA 515.0/470.0 Da Baseline Missed Wrong Peak NB. PFBA and PFPeA do not have qualifying ion transitions. Before A fter N/A Baseline Missed Wrong Peak Page 140 of 169 225 f t C o lu m b ia WvJ Analytical Services" Created with Analyst Reporter Printed: 18/02/2010 3:24:00 PM Project Data File Result Table Instrument Name Ewan's Projects\PFCs 021710\Samplesl_ong.wiff 021710long.rdb API 5000 Sample Name Acquisition Date Acquisition Method Injection Vial KQ1000664-04 2/17/2010 11:02:27 PM PFCkinetexLong.dam 48 Injection Volume Sample Type Dilution Factor Weight to Volume 5 Unknown 1.00 0.00 Results Summary Analyte Peak Name IS Name PFOA 1 13C-PFOA PFNA 1 13C-PFNA PFOS 1 13C-PFOS PFDA 1 13C-PFDA PFUnA 1 13C-PFUnA PFDS 1 13C-PFOS PFDoA 1 13C-PFD0A PFTrA 1 13C-PFDOA PFTeA 1 13C-PFDOA IS Area 3454200 2401200 8029900 2491600 115010 8029900 163280 163280 163280 Analyte RT (Exp RT ) 1.26 (1.36) 2.08 (2.06) 2.13 (2.09) 3.15 (3.06) 3.94 (4.06) 3.94 (3.87) 4.57 (4.55) 5.13 (5.06) 5.57 (5.51) Analyte Area 4642500 11713000 39909000 4568100 2760000 8762300 1688100 882130 741830 Calc. Cone (ng/mL) 26.500 44.900 46.500 17.800 22.900 9.570 17.100 15.900 17.900 Modified? No No No No No No No No No Page 142 of 170 226 Created with Analys\jRporter Printed: 18/02/2010 3:24:00 PM IRC Summary I Analyte Peak Name PFOA2 S_13C_PFOA PFNA2 S_13C_PFNA PFOS2 SJ3C-PFOS PFDA2 SJ3C-PFDA PFUnA2 S_13C-PFUnA PFDS2 PFDoA2 S_13C-PFDoA PFTrA 2 PFTeA2 RT (Exp RT ) 1.27(1.36) 1.28(1.36) 2.09(2.08) 0.00 (2.44) 2.14(2.12) 2.14(2.00) 3.14 (3.06) 3.15(3.04) 3.94 (3.88) 3.94 (3.88) 3.94(3.87) 4.57 (4.53) 4.58 (4.64) 5.11 (5.13) 5.57(5.56) Area 10345000 3454200 3928000 0 13519000 8029900 670560 2491600 483140 115010 2773700 413810 163280 335960 228710 M od ifie d ? No Calc (Exp) MRM Ratio 2.23(2.16) Ratio C onfirm s ID YES No 0.74 (43.19) No No 0.34(0.34) YES No 0.00 (0.00) No No 0.34(0.32) YES No 0.20 (21.71) No No 0.15(0.14) YES No 0.55(17.53) No No 0.18(0.19) YES No 0.04(1.60) No NO 0.32 (0.32) YES No 0.25(0.28) YES No 0.10(3.71) No No 0.38(0.34) YES No 0.31 (0.29) YES Page 143 of 170 227 Createci with Analyst' Reporter Printed: 18/02/2010 3:24:00 PM Quantitative Peak Review PFOA 1 413.0/169.0 Da BnasWerlinnnenPMeaisksed 13C-PFOA 417.0/372.0 Da Baseline c Missed Wrnnn Peak KQ1000664-04 l2.08 PFNA 1 463.0/419.0 Da d Baseline Missed p Wrnnn Ppak 3^ 13C-PFNA 468.0/423.0 Da Baseline Missed n Wrnnn Peak PFOS 1 499.0/80.0 Da Baseline Missed i i Wrnnn Ppak 13C-PFOS 503.0/80.0 Da o Baseline Missed Wrnnn Ppak PFDA 1 513.0/469.0 Da Baseline Missed r. W rnnn Ppak 13C-PFDA 515.0/470.0 Da c BpasWerlinnnenPMpails<sed PFUnA 1 563.0/519.0 Da Baseline a Missed n Wrnnn Peak 13C-PFUnA 565.0/270.0 Da BnasWerlinnnenPMeaisksed PFDS 1 599.0/80.0 Da g Baseline c Missed Wrnnn Peak 13C-PFOS 503.0/80.0 Da c Baseline Missed n Wrnnn Peak PFDoA 1 613.0/569.0 Da Baseline Missed p Wrnnn Ppak 13C-PFD0A 615.0/169.0 Da Baseline Missed Wrnnn Ppak PFTrA 1 663.0/619.0 Da BpasWerlinnnenoPMeaisksed 13C-PFDOA 615.0/169.0 Da Baseline Missed ___ r W rnnn P aak___ PFTeA 1 713.0/669.0 Da c Baseline Missed ___n Wrnnn Peak 13C-PFDoA 615.0/169.0 Da Baseline Missed ___ p W rnnn Peak___ Before After 228 Page 144 of 170 Created with AnalysfeRfeporter Printed: 18/02/2010 3:24:00 PM Ion Ratio Confirmation PFOA2 413.0/369.0 Da c Baseline Missed c Wrong Peak PFNA2 463.0/219.0 Da Baseline c Missed d Wrong Peak KQ1000664-04 ft i J,i | 3 14 ^ ....... PFOS2 499.0/99.0 Da Baseline Missed a Wrong Peak PFDA2 513.0/269.0 Da Baseline Missed Wrong Peak PFUnA 2 563.0/269.0 Da o Baseline o Missed Wrong Peak 1 ''1 . 5 7 ..... Mi_ _ i ...... Mi PFTeA2 713.0/169.0 Da d Baseline c Missed Wrong Peak PFDS2 599.0/99.0 Da Baseline c Missed c Wrong Peak Before A fter PFDoA2 613.0/169.0 Da Baseline Missed Wrong Peak PFTrA 2 663.0/169.0 Da Baseline Missed Wrong Peak Page 145 of 170 229 p. 9 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Project Data File Result Table Instrument Name Ewan's Projects\PFCs 021710\SamplesShort.wiff 021710short.rdb API 5000 Sample Name Acquisition Date Acquisition Method Injection Vial KQ1000664-04 2/18/2010 5:49:03 AM PFCkinetexShort.dam 48 Injection Volume Sample Type Dilution Factor Weight to Volume 5 Unknown 1.00 0.00 Results Summary Analyte Peak Name IS Name PFBA 1 13C-PFBA PFPeA 1 13C-PFHxA PFBS 1 180-PFHS PFHxA 1 13C-PFHXA PFHpA 1 13C-PFHxA PFHxS 1 180-PFHS SJ80-PFHS 13C-PFDA SJ3C-PFDA 13C-PFDA IS Area 4898600 6091700 3527300 6091700 6091700 3527300 4128300 4128300 Analyte RT (Exp RT ) 1.25 (1.27) 3.54 (3.60) 4.19 (4.26) 5.22 (5.31) 6.12 (6.23) 6.20 (6.32) 6.20 (6.31) 7.50 (7.65) Analyte Area 10065000 11921000 21238000 14167000 4878500 27983000 3527300 4128300 Calc. Cone (ng/mL) 19.60 20.60 18.60 23.90 22.70 27.90 1.06 1.00 Modified? No No No No No No No No -V , i i ,o Page 141 of 169 230 f i Columbia O Analytical Services* Created with AnalysPR&^orter Printed: 18/02/2010 4:02:00 PM IRC Summary Analyte Peak Name PFBA2 PFPeA2 PFBS2 PFHxA 2 PFHpA2 PFHxS2 S_13C-PFBA S_13C-PFHxA RT (Exp RT) 1.25(1.27) 3.54 (3.60) 4.19(4.26) 5.22(5.31) 6.12(6.22) 6.20 (6.32) 1.24(1.26) 5.22(5.30) Area 10065000 11921000 8681100 1337900 14085000 12197000 4898600 6091700 Modified? No Calc (Exp) MRM Ratio 1.00(1.00) Ratio Confirms ID YES No 1.00(1.00) YES No 0.41 (0.40) YES No 0.09(0.10) YES No 2.89(2.90) YES No 0.44(0.40) YES No 0.49(13.20) No No 0.43(13.71) No Page 142 o f 169 231 ............................................... Columbia Analytical Services" p. 11 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Quantitative Peak Review KQ1000664-04 15ft sS?' lI3s 5 60*0 05 10i 15 6(5 51.*55 f ie$ 10 05 I 10 '5 7(M & ,5rt 31 '0* 60*5 :D I 30 }5 4a 'M 3 50.5 45 45 5.^ 50 55 60 PFBA* ? 213.0/169.0 Da Baseline c Missed n Wrnnn Peak 4.19 s" 1i '6 -I)TlTM9f4 5 50 PFBS 1 299.0/80.0 Da Baseline a Missed n Wrnnn Peak 6^2 S%2 80*6 6 3 0*i :r5 55 60 65 71) 13C-PFBA PFPeA"l 217.0/172.0 Da 263.0/219.0 Da Baseline c Missed Baseline c Missed I95_______________________ n .. 6'.*55 Wrnnn Peak_____ :s*i 5. t&rt n Wrnnn Peak 5.^ I 4.5 :s *I 1,50r.6t 60.5 55 61 65 70 46 50 55 60 180-PFHS 403.0/103.0 Da Baseline c Missed r Wrnnn Peak 5.^ &S1 1<t*i 50.5 15 50 55 60 PFHxAl 313.0/269.0 Da Baseline Missed n Wrnnn Peak b*i M 6.^> i| M i6 55 $0 65 70 13C-PFHxA 315.0/270.0 Da c Baseline Missed n Wrnnn Peak 5.^ m '1*6 3i 51*6 Tm.nvir 13C-PFHxA 315.0/270.0 Da Baseline Missed 6*65 r Wrnnn Peak 6.^) - 6.6 | 3 3.6 1.6 55 6.0 65 70 PFHpAI 13C-PFHxA PFHxi"l 180-PFHS 363.0/169.0 Da 315.0/270.0 Da 399.0/80.0 Da 403.0/103.0 Da D Baseline Missed Baseline Missed Baseline Missed Baseline Missed n Wrnnn Peak fc*S 1l ^4*6 Ii*i 55 60 65 70 n Wrnnn Peak 10.6 7.^0 00.5 | 40e5 70s 70 75 *0 n Wrnnn Peak 7.50 00.5 |$& 60(5 40e5 70S 15 78 775m*non 1.0 n Wrnnn Peak >0.6 80.5 ! * | 40e5 85 7(J i J5Tm,mm 30 65 S_180-PFHS 13C-PFDA S 13C-PFDA 13C-PFDA 403.0/103.0 Da 515.0/470.0 Da 515.0/470.0 Da 515.0/470.0 Da Baseline Missed Baseline a Missed Baseline Missed Baseline Missed n Wrnnn Peak_____ n Wrnnn Peak_____ n Wrnnn Peak_____ n Wrnnn Peak Before A fter Page 143 o f 169 232 Jf" CofurnlbfSl cL3 Analytical Services" Ion Ratio Confirmation Created with AnalysPR^orter Printed; 18/02/2010 4:02:00 PM KQ1000664-04 PFBA2 213.0/169.0 Da o Baseline c Missed Wrong Peak 6.12 PFPeA2 263.0/219.0 Da Baseline c Missed Wrong Peak 6. PFBS2 299.0/99.0 Da d Baseline Missed Wrong Peak -A PFHpA2 363.0/319.0 Da Baseline g Missed g Wrong Peak PFHxS2 399.0/99.0 Da Baseline c Missed Wrong Peak S_13C-PFDA 515.0/470.0 Da Baseline c Missed c Wrong Peak NB. PFBA and PFPeA do not have qualifying ion transitions. Before A fter PFHxA 2 313.0/119.0 Da Baseline Missed c Wrong Peak N/A Baseline c Missed Wrong Peak Page 144 o f 169 233 Created witn Anaiyqi>.rtSporter Printed: 18/02/2010 3:24:00 PM Project Data File Result Table Instrument Name Ewan's Projects\PFCs 021710\SamplesLong.wiff 021710long.rdb API 5000 lUot? Sample Name KQ1000664-01 Acquisition Date 2/17/2010 10:39:49 PM Acquisition Method PFCkinetexLong.dam Injection Vial 45 Injection Volume Sample Type Dilution Factor Weight to Volume 5 Unknown 1.00 0.00 Results Summary Analyte Peak Name IS Name PFOA 1 13C-PFOA PFNA 1 13C-PFNA PFOS 1 13C-PFOS PFDA 1 13C-PFDA PFUnA 1 13C-PFUnA PFDS 1 13C-PFOS PFDoA 1 13C-PFDOA PFTrA 1 13C-PFDOA PFTeA 1 13C-PFD0A IS Area 4454200 2968000 8870700 2634600 125850 8870700 198400 198400 198400 Analyte RT (Exp RT ) 1.24 (1.36) 2.07 (2.06) 2.11 (2.09) 3.13 (3.06) 3.91 (4.06) 3.92 (3.87) 4.57 (4.55) 5.11 (5.06) 5.57 (5.51) Analyte Area 4210800 6745900 17683000 5626900 3426100 11102000 2308700 1158100 921160 Calc. Cone (ng/mL) 18.700 20.900 18.700 20.700 26.000 11.000 19.300 17.200 18.300 Modified? No No No No No No No No No 4 (o Page 130 of 170 . 234 Created with Analy^b-flelporter Printed: 18/02/2010 3:24:00 PM IRC Summary Analyte Peak Name PFOA2 S_13C_PFOA PFNA2 S_13C_PFNA PFOS2 S_13C-PFOS PFDA2 S_13C-PFDA PFUnA2 S_13C-PFUnA PFDS2 PFDoA2 S_13C-PFDoA PFTrA 2 PFTeA2 RT (Exp R T ) 1.26(1.36) 1.26(1.36) 2.07 (2.08) 0.00 (2.44) 2.11 (2.12) 2.10(2.00) 3.10(3.06) 3.13(3.04) 3.92(3.88) 3.92(3.88) 3.92(3.87) 4.56 (4.53) 4.57 (4.64) 5.11 (5.13) 5.57 (5.56) Area 8964800 4454200 2212300 0 5762500 8870700 736140 2634600 717300 125850 3592700 578860 ' 198400 413010 274850 M o d ifie d ? No Calc (Exp) MRM Ratio 2.13(2.16) Ratio C onfirm s ID YES No 1.06 (43.19) No No 0.33(0.34) YES No 0.00(0.00) No No 0.33(0.32) YES No 0.50 (21.71) No No 0.13(0.14) YES No 0.47(17.53) No No 0.21 (0.19) YES No 0.04(1.60) No No 0.32(0.32) YES No 0.25(0.28) YES No 0.09 (3.71) No No 0.36(0.34) YES No 0.30(0.29) YES Page 131 of 170 235 Created with A n a lyft ^ p o rte r Printed: 18/02/2010 3:24:00 PM Quantitative Peak Review JL_ 1.26 PFOA 1 413.0/169.0 Da l Baseline Missed r- W rnnn Peak 13C-PFOA 417.0/372.0 Da Baseline Missed ___n Wrnnn Peak 2.10 KQ1000664-01 2.06 PFNA 1 463.0/419.0 Da Baseline Missed n Wrnnn Peak 3.13 13C-PFNA 468.0/423.0 Da Baseline c Missed r Wrnnn Peak 3.13 PFOS 1 499.0/80.0 Da Baseline Missed r Wrnnn Peak I3.91 t\ :c 13C-PFOS 503.0/80.0 Da Baseline Missed n Wrnnn Pnak rsooo 3.92 - ir-ooo i imo 5600 PFDA 1 513.0/469.0 Da Baseline c Missed n Wrnnn Peak 13C-PFDA 515.0/470.0 Da g Baseline Missed Wrnnn Peak PFUnA 1 563.0/519.0 Da d Baseline g Missed -----r Wrong Peak -- 4.57 140 To4w6IMA SO PFDoA 1 613.0/569.0 Da BnasWerlinnnen Missed Peak 5.57 i i 13C-PFUnA PFDS 1 13C-PFOS 565.0/270.0 Da BnasWerlinnnenaPMeaisksed 4.57 599.0/80.0 Da Baseline a Missed n Wrnnn Peak !IW 1 s&:o*s 1 itS lOeS 5PH i I<0 <5 SO SS 5 Sd $5 00 13C-PFDOA 615.0/169.0 Da PFTrA 1 663.0/619.0 Da 503.0/80.0 Da c Baseline Missed n Wrnnn Peak 4*4 *e s so 13C-PFDOA 615.0/169.0 Da s$ BnasWerlninnen Missed Ppak D Baseline Missed .n Wrong Peak Baseline Misse n Wrnnn Peak PFTeA 1 713.0/669.0 Da Baseline Missed ____n Wrnnn Peak___ 13C-PFDoA 615.0/169.0 Da _a__BnasWerlinnnen Missed Peak Before After 236 Page 132 of 170  Ion Ratio Confirmation Created with A nalysU ^gorter Printed: 18/02/2010 3:24:00 PM KQ1000664-01 PFOA2 413.0/369.0 Da d Baseline Missed Wrong Peak PFNA2 463.0/219.0 Da c Baseline c Missed o Wrong Peak 5*', 1 ** |& i Mi 3 C*S 1 ............. - ....... - 3 . 1 2 ......- ................- .. . Hi. 3 . ................................... | 5& .......: : ,, ............... __________________ , L -- - PFUnA 2 563.0/269.0 Da Baseline Missed |o Wrong Peak PFDS2 599.0/99.0 Da Baseline Missed d Wrong Peak - T ..~ PFTeA2 713.0/169.0 Da o Baseline d Missed Wrong Peak Before A fter PFOS2 499.0/99.0 Da Baseline Missed Wrong Peak .....4 PFDoA2 613.0/169.0 Da Baseline Missed Wrong Peak PFDA2 513.0/269.0 Da Baseline Missed Wrong Peak .......-...5. 1...- ......-.. SSOM0_________ , i________ PFTrA 2 663.0/169.0 Da Baseline Missed Wrong Peak Page 133 of 170 237 b l cal Services' Created with AnalyJ'f^eporter Printed: 18/02/2010 4:02:00 PM Project Data File Result Table Instrument Name Sample Name Acquisition Date Acquisition Method Injection Vial Ewan's Projects\PFCs 021710\SamplesShort.wiff 021710short.rdb API 5000 l O < P l - M $ KQ1000664-01 2/18/2010 5:20:25 AM PFCkinetexShort.dam 45 Injection Volume Sample Type Dilution Factor Weight to Volume 5 Unknown 1.00 0.00 Results Summary Analyte Peak Name IS Name PFBA 1 13C-PFBA PFPeA 1 13C-PFHxA PFBS 1 180-PFHS PFHxA 1 13C-PFHXA PFHpA 1 13C-PFHXA PFHxS 1 180-PFHS S_180-PFHS 13C-PFDA S_13C-PFDA 13C-PFDA IS Area 5833100 7119300 4033900 7119300 7119300 4033900 4426800 4426800 Analyte RT (Exp RT ) 1.24 (1.27) 3.53 (3.60) 4.19 (4.26) 5.24 (5.31) 6.15 (6.23) 6.23 (6.32) 6.23 (6.31) 7.54 (7.65) Analyte Area 12337000 13459000 22470000 14328000 5248100 21146000 4033900 4426800 Calc. Cone (ng/mL) 20.10 19.90 17.00 20.50 20.90 17.30 1.13 1.00 Modified? No No No No No No No No Page 129 of 169 238 Columbia A n alytical Created with Analyil'l4porter Printed: 18/02/2010 4:02:00 PM IRC Summary Analyte Peak Name PFBA2 PFPeA2 PFBS2 PFHxA 2 PFHpA2 PFHxS2 S_13C-PFBA S_13C-PFHxA RT (Exp R T ) 1.24(1.27) 3.53 (3.60) 4.19(4.26) 5.24(5.31) 6.14(6.22) 6.23 (6.32) 1.23(1.26) 5.23 (5.30) Area 12337000 13459000 9242600 1371800 14854000 8691100 5833100 7119300 M od ifie d ? No Calc (Exp) MRM Ratio 1.00(1.00) Ratio C onfirm s ID YES No 1.00(1.00) YES No 0.41 (0.40) YES No 0.10(0.10) YES No 2.83 (2.90) YES No 0.41 (0.40) YES No 0.47(13.20) No No 0.50(13.71) No Page 130 of 169 239 Columbia Analytical Services" Quantitative Peak Review PFBA 1 213.0/169.0 Da c Baseline c Missed r; W rnn4n.1P9 eak 13C-PFBA 217.0/172.0 Da c Baseline d Missed ___g.Wmnn Poflk___ p. 19 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM KQ1000664-01 >, \ &' ; j< * S0e5 ,L PFPeA 1 263.0/219.0 Da c Baseline a Missed h Wrnnn Peak 13C-PFHxA 315.0/270.0 Da c Baseline Missed __r Wr.tMLEfia)i__ PFBS 1 299.0/80.0 Da Baseline c Missed r W rnn6n.15Peak 180-PFHS 403.0/103.0 Da Baseline Missed n Wrnnn Peak PFHxA 1 313.0/269.0 Da c Baseline Missed r Wrnnn Peak 13C-PFHxA 315.0/270.0 Da c Baseline c Missed r Wrnnn Peak PFHpA 1 363.0/169.0 Da c Baseline Missed n W rnnn Peak 13C-PFHxA 315.0/270.0 Da Baseline Missed ___n Wrnnn Peak PFHxS1 399.0/80.0 Da Baseline Missed Wrnnn Peak 180-PFHS 403.0/103.0 Da Baseline g Missed ___n Wrnnn Peak___ S_180-PFHS 403.0/103.0 Da Baseline Missed ___n Wrnnn Peak 13C-PFDA 515.0/470.0 Da Baseline Missed ___ p W rnnn Peak S_13C-PFDA 515.0/470.0 Da Baseline Missed ____n W rnnn Peak Before After 13C-PFDA 515.0/470.0 Da g Baseline Missed i-- \ A/rnrto Dnl/ Page 131 of 169 240 Columbia Analytical Services*' Created with Analyil'f^eporter Printed: 18/02/2010 4:02:00 PM Ion Ratio Confirmation zn1.24 ' 3.53" PFBA2 213.0/169.0 Da c Baseline Missed Wrong Peak 6.U PFPeA2 263.0/219.0 Da Baseline Missed c Wrong Peak KQ1000664-01 ..4, 1 9 ... PFBS2 299.0/99.0 Da o Baseline Missed d Wrong Peak PFHxA 2 313.0/119.0 Da c Baseline o Missed Wrong Peak Tfe imageisroUva 60 PFHpA2 363.0/319.0 Da d Baseline Missed c Wrong Peak PFHxS2 399.0/99.0 Da Baseline Missed o Wrong Peak S_13C-PFDA 515.0/470.0 Da o Baseline Missed Wrong Peak NB. PFBA and PFPeA do not have qualifying ion transitions. Before A fter N/A Baseline Missed Wrong Peak Page 132 of 169 241 Created with Analy?'F^porter Printed: 18/02/2010 3:24:00 PM Project Data File Result Table Instrument Name Ewan's Projects\PFCs 021710\SamplesLong.wiff 021710long.rdb API 5000 Sample Name Acquisition Date Acquisition Method Injection Vial KQ1000664-02 2/17/2010 10:47:22 PM PFCkinetexLong.dam 46 Injection Volume Sample Type Dilution Factor Weight to Volume 5 Unknown 1.00 0.00 Results Summary Analyte Peak Name IS Name PFOA 1 13C-PFOA PFNA 1 13C-PFNA PFOS 1 13C-PFOS PFDA 1 13C-PFDA PFUnA 1 13C-PFUnA PFDS 1 13C-PFOS PFDoA 1 130-PFDoA PFTrA 1 13C-PFD0A PFTeA 1 13C-PFDOA IS Area 4400400 2963600 9009700 2867600 124700 9009700 183810 183810 183810 Analyte RT (Exp RT ) 1.26 (1.36) 2.07 (2.06) 2.10 (2.09) 3.11 (3.06) 3.93 (4.06) 3.94 (3.87) 4.58 (4.55) 5.12 (5.06) 5.58 (5.51) Analyte Area 4282700 6569300 18297000 5864400 3702300 11465000 1892500 1273900 997460 Calc. Cone (ng/mL) 19.200 20.400 19.000 19.800 28.400 11.200 17.000 20.400 21.300 M odified? No No No No No No No No No t " ^u ` Page 134 of 170 242 Created with Analyit- iporter Printed: 18/02/2010 3:24:00 PM IRC Summary Analyte Peak Name PFOA2 S_13C_PFOA PFNA2 S_13C_PFNA PFOS2 SJ3C-PFOS PFDA2 S_13C-PFDA PFUnA2 S_13C-PFUnA PFDS2 PFDoA2 S_13C-PFDoA PFTrA 2 PFTeA2 RT (Exp RT ) 1.23(1.36) 1.25(1.36) 2.07 (2.08) 0.00 (2.44) 2.12 (2.12) 2.12(2.00) 3.14 (3.06) 3.12(3.04) 3.94 (3.88) 3.92(3.88) 3.94(3.87) 4.59 (4.53) 4.59 (4.64) 5.12(5.13) 5.58(5.56) Area 9664100 4400400 2187500 0 5900400 9009700 750000 2867600 672360 124700 3651400 530830 183810 341800 293600 M o d ifie d ? No Calc (Exp) MRM Ratio 2.26 (2.16) Ratio C onfirm s ID YES No 1.03 (43.19) No No 0.33(0.34) YES No 0.00 (0.00) No No 0.32(0.32) YES No 0.49 (21.71) No No 0.13(0.14) YES No 0.49(17.53) No No 0.18(0.19) YES No 0.03 (1.60) No No 0.32(0.32) YES No 0.28 (0.28) YES No 0.10(3.71) No No 0.27(0.34) YES No 0.29(0.29) YES Page 135 of 170 243 Columbia Analytical Sonfices- Quantitative Peak Review _____ 1PFOA 1 413.0/169.0 Da BnasWerlinnnen c Missed Peak i 2.10 PFOS 1 499.0/80.0 Da Baseline a Missed r- Wrnnn Peak 13C-PFOA 417.0/372.0 Da Baseline Missed r Wrnnn Peak 2.12 i 13C-PFOS 503.0/80.0 Da Baseline Missed r Wrnnn Peak PFUnA 1 563.0/519.0 Da g Baseline Missed n Wrnnn Peak 13C-PFUnA 565.0/270.0 Da BnasWerlinnnen c Missed Peak Created with Analys|jRporter Printed: 18/02/2010 3:24:00 PM KQ1000664-02 JL L! 2.10 JLPFNA 1 463.0/419.0 Da Baseline Missed r Wrnnn Peak 13C-PFNA 468.0/423.0 Da Baseline c Missed ___n Wrnnn Peak___ i )D PFDA 1 513.0/469.0 Da BnasWerlinnnenPMnaisksed J(1 J L13C-PFDA 515.0/470.0 Da c BnasWerlinnnenPMeaisksed PFDS 1 599.0/80.0 Da Baseline Missed i Wrnnn Peak 13C-PFOS 503.0/80.0 Da Baseline q Missed ___n Wrnnn Peak___ PFDoA 1 613.0/569.0 Da BnasWerlinnnenPMeaisksed 13C-PFDOA 615.0/169.0 Da Baseline Missed Wrnnn Peak PFTrA 1 663.0/619.0 Da Baseline Missed n W rnnn Peak___ 13C-PFDOA 615.0/169.0 Da ___BnasWerlinnnen PMn aisks_e_d_ PFTeA 1 713.0/669.0 Da Baseline Missed ___ n W rnnn Peak 13C-PFD0A 615.0/169.0 Da ___BnasWerlinnnen PMe aisksed Before A fter 244 Page 136 o f 170 Ion Ratio Confirmation Created with Analyif-$$porter Printed: 18/02/2010 3:24:00 PM KQ1000664-02 PFOA 2 413.0/369.0 Da Baseline c Missed d Wrong Peak PFNA2 463.0/219.0 Da Baseline Missed c Wrong Peak PFOS2 499.0/99.0 Da Baseline c Missed Wrong Peak PFDA 2 513.0/269.0 Da c Baseline Missed Wrong Peak PFUnA2 563.0/269.0 Da Baseline o Missed c Wrong Peak PFDS 2 599.0/99.0 Da a Baseline Missed Wrong Peak PFDoA2 613.0/169.0 Da Baseline Missed Wrong Peak PFTrA 2 663.0/169.0 Da Baseline Missed Wrong Peak PFTeA2 713.0/169.0 Da Baseline Missed Wrong Peak Before A fter Page 137 of 170 245 leal Services- Created with A nalysf Reporter Printed: 18/02/2010 4:02:00 PM Project Data File Result Table Instrument Name Sample Name Acquisition Date Acquisition Method Injection Vial Ewan's ProjectsVPFCs 021710\SamplesShort.wiff 021710short.rdb API 5000 pojen - e p ^ y KQ1000664-02 2/18/2010 5:29:57 AM PFCkinetexShort.dam 46 Injection Volume Sample Type Dilution Factor Weight to Volume 5 Unknown 1.00 0.00 Results Summary Analyte Peak Name IS Name PFBA 1 13C-PFBA PFPeA 1 13C-PFHxA PFBS 1 180-PFHS PFHxA 1 13C-PFHxA PFHpA 1 13C-PFHxA PFHxS 1 180-PFHS SJ80-PFHS 13C-PFDA S_13C-PFDA 13C-PFDA IS Area 6053100 7357000 4044700 7357000 7357000 4044700 4520200 4520200 Analyte RT (Exp RT ) 1.24 (1.27) 3.54 (3.60) 4.19 (4.26) 5.24 (5.31) 6.13 (6.23) 6.23 (6.32) 6.23 (6.31) 7.51 (7.65) Analyte Area 12880000 14104000 23314000 14912000 5578000 21856000 4044700 4520200 Calc. Cone (ng/mL) 20.30 20.20 17.70 20.60 21.50 17.90 1.11 1.00 M odified? No No No No No No No No Page 133 of 169 246 p. 26 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM IRC Summary Analyte Peak Name PFBA2 PFPeA2 PFBS2 PFHxA 2 PFHpA2 PFHxS2 S_13C-PFBA S_13C-PFHxA RT (Exp R T ) 1.24(1.27) 3.54(3.60) 4.19(4.26) 5.24(5.31) 6.14(6.22) 6.23 (6.32) 1.25(1.26) 5.23 (5.30) Area 12880000 14104000 9604100 1400000 15070000 8832700 6053100 7357000 M o d ifie d ? Calc (Exp) MRM R a tio No 1.00(1.00) Ratio Confirm s ID YES No 1.00(1.00) YES No 0.41 (0.40) YES No 0.09(0.10) YES No 2.70 (2.90) YES No 0.40(0.40) YES No 0.47(13.20) No No 0.49(13.71) No Page 134 of 169 247 Quantitative Peak Review Createci with Analysffteporter Printed: 18/02/2010 4:02:00 PM KQ1000664-02 PFBA1 213.0/169.0 Da Baseline c Missed r W rnnn Peak 13C-PFBA 217.0/172.0 Da c Baseline Missed I- W rnnn Peak PFPeA 1 263.0/219.0 Da o Baseline Missed r W rnnn Peak 13C-PFHxA 315.0/270.0 Da BrasWerlinnnen c Missed Peak PFBS 1 299.0/80.0 Da c Baseline d Missed r. W rnnn Peak 180-PFHS 403.0/103.0 Da c Baseline c Missed h Wrnnn Peak PFHxA 1 313.0/269.0 Da a Baseline Missed n Wrnnn Peak 130-PFHxA 315.0/270.0 Da BnasWerlinnnen Missed Peak PFHpA 1 363.0/169.0 Da BnasWerlinnnen Missed Peak 67 SJ80-PFHS 403.0/103.0 Da Baseline Missed ___ ri W rnnn Peak___ si tr 13C-PFHXA 315.0/270.0 Da d Baseline Missed ___ p Wrnnn Peak___ I PFHxS 1 399.0/80.0 Da Baseline Missed n Wrnnn Peak 7^1 10* ,, eo*s s i 1 0*5 180-PFHS 403.0/103.0 Da a BnasWerlionnegcPMeaisks_e_d_ !C*fc u n ti COtS 1 'n ;s *n as 13C-PFDA 515.0/470.0 Da BnasWerlinnnenPMeaisks_e_d___ ' s ao *>me m i S 13C-PFDA a5 515.0/470.0 Da BnasWerlinnnenPMeaisks_e_d___ 13C-PFDA 515.0/470.0 Da D BnasWerlinnnenPMeaiskse Before A fter Page 135 of 169 248 p. 28 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Ion Ratio Confirmation 1.24 KQ1000664-02 PFBA2 213.0/169.0 Da c Baseline Missed Wrong Peak PFPeA2 263.0/219.0 Da Baseline Missed Wrong Peak I PFBS2 299.0/99.0 Da d Baseline Missed d Wrong Peak 6.14' B05 3-.. tbc* I JL liwS fiOri PFHpA2 363.0/319.0 Da Baseline c Missed Wrong Peak PFHxS2 399.0/99.0 Da Baseline Missed d Wrong Peak S_13C-PFDA 515.0/470.0 Da Baseline Missed d Wrong Peak NB. PFBA and PFPeA do not have qualifying ion transitions. Before A fter PFHxA 2 313.0/119.0 Da c Baseline Missed Wrong Peak ismageis N/A Baseline a Missed Wrong Peak Page 136 o f 169 249 f t Columbia O Analytical Services" Analyte Name: Internal Standard: PFOA 1 13C-PFOA Created with A n a l^ rt^ p o rte r Printed: 18/02/2010 3:24:00 PM Data File Acquisition Date Acquisition Method Project 021710\CalLong.wiff 2/17/2010 6:30:13 PM PFCkinetexLong.dam Ewan's Projects\PFCs Result Table Algorithm Used Instrument Name 021710long.rdb IntelliQuan API 5000 Regression Equation:_______ y = 0.0508 x + -0.00146 (r = Q.9989)7 Exp Cone (ng/mL) # o f Values Mean Calc Cone (ng/mL) 0.1 1 0.114 0.5 1 0.477 1 1 0.958 5 1 4.871 10 1 10.158 20 1 18.413 50 1 51.608 % Accuracy 114 95 96 97 102 92 103 J STD NaN NaN NaN NaN NaN NaN NaN %CV NaN NaN NaN NaN NaN NaN NaN '4 6 ? * * io " i3 h is it a 1B is :i :: n AneM* Cv. /ISCOK a * 7 it 33 34 n 37 m 5 S 7\ 7 71 7* * 47 * V" 7 / t9\l Page 1 of 170 250 JT C o itir o b ia A n alytical S -e rv te " Created with AnalysLRflporter Printed: 18/02/2010 3:24:00 PM Analyte Name: Internal Standard: PFNA 1 13C-PFNA Data File Acquisition Date Acquisition Method Project 021710\CalLong.wiff 2/17/2010 6:30:13 PM PFCkinetexLong.dam Ewan's Projects\PFCs Result Table Algorithm Used Instrument Name 021710long.rdb IntelliQuan API 5000 Regression Equation: Exp Cone (ng/mL) 0.1 0.5 1 5 10 20 50 y = 0,109 x + -0.00371 (r = 0,9976) ^ # of Values Mean Calc Cone (ng/mL) 1 0.107 1 0.463 1 1.096 1 4.964 1 9.849 1 17.699 1 52.422 % Accuracy 107 93 110 99 98 88 105 J STD NaN NaN NaN NaN NaN NaN NaN %CV NaN NaN NaN NaN NaN NaN NaN ,t,^ ________________________________ _ ____________________ ___________________ -___ ( J J 5 e j 6 V <0 II '2 13 I IS H 17 U H 20 21 22 23 24 25 2$ 27 28 28 30 31 32 33 34 K 3E 3> 36 39 40 41 42 43 45 46 47 48 48 Anoly* Cone VIS Cone (jy lb 1 Z1 Page 2 of 170 251 created witn Anaiypt importer Printed: 18/02/2010 3:24:00 PM Analyte Name: Internal Standard: PFOS 1 13C-PFOS Data File Acquisition Date Acquisition Method Project 021710\CalLong.wiff 2/17/2010 6:30:13 PM PFCkinetexLong.dam Ewan's Projects\PFCs Result Table Algorithm Used Instrument Name 021710long.rdb IntelliQuan API 5000 Regression Equation: Exp Cone (ng/mL) 0.1 0.5 1 5 10 20 50 y = 0.107 x + -0.0016 (r = 0.9989) ^ # o f Values Mean Calc Cone (ng/mL) 1 0.093 1 0.489 1 1.026 1 5.187 1 10.889 1 18.688 1 50.229 % Accuracy 93 98 103 104 109 93 100 l STD NaN NaN NaN NaN NaN NaN NaN %CV NaN NaN NaN NaN NaN NaN NaN J416 13 h K H I? in ii to :: J3*nB?M4Co"^C-y!SConi :7 252 31 u 13 34 is * v 43 44 4!, V "^7 gilO 'L J i Page 3 of 170 created witn AnaiysLR^Dorter Printed: 18/02/2010 354:00 PM Analyte Name: Internal Standard; PFDA 1 13C-PFDA Data File Acquisition Date Acquisition Method Project Regression Equation: Exp Cone (ng/mL) 0.1 0.5 1 5 10 20 50 021710\CalLong.wiff 2/17/2010 6:30:13 PM PFCkinetexLong.dam Ewan's Projects\PFCs Result Table Algorithm Used Instrument Name 021710long.rdb IntelliQuan API 5000 y = 0.103 x + 0.000852 (r = 0.9990) / # of Values Mean Calc Cone (ng/mL) 1 0.099 1 0.482 1 1.103 1 4.925 1 10.077 1 18.489 1 51.425 % Accuracy 99 96 110 99 101 92 103 STD NaN NaN NaN NaN NaN NaN NaN %CV NaN NaN NaN NaN NaN NaN NaN Lr"- S' Page 4 of 170 253 /* C o lu m b ia 3 Analytical Services- Created with Analyst importer Printed: 18/02/2010 3:24:00 PM Analyte Name: Internal Standard: PFUnA 1 13C-PFUnA Data File Acquisition Date Acquisition Method Project 021710\CalLong.wiff 2/17/2010 6:30:13 PM PFCkinetexLong.dam Ewan's Projects\PFCs Result Table Algorithm Used Instrument Name 021710long.rdb IntelliQuan API 5000 Regression Equation: Exp Cone (ng/mL) 0.1 0.5 1 5 10 20 50 y = 1.05 x + 0.0336 (r = 0.9994)/ # of Values Mean Calc Cone (ng/mL) 1 0.083 1 0.530 1 1.090 1 5.374 1 9.317 1 20.372 1 49.833 % Accuracy 83 106 109 107 93 102 100 J STD NaN NaN NaN NaN NaN NaN NaN %CV NaN NaN NaN NaN NaN NaN NaN Page 5 of 170 254 Created with Analy^bRjsporter Printed: 18/02/2010 3:24:00 PM Analyte Name: Internal Standard: PFDS 1 13C-PFOS Data File A cquisition Date Acquisition Method Project 021710\CalLong.wiff 2/17/2010 6:30:13 PM PFCkinetexLong.dam Ewan's ProjectsVPFCs Result Table Algorithm Used Instrument Name 021710long.rdb IntelfiQuan API 5000 Regression Equation: Exp Cone (ng/mL) 0.1 0.5 1 5 10 20 50 y = -0.000414 xA2 + 0.118 x + -0.00244 (r = 0.9991) ^ # o f Values Mean Calc Cone (ng/mL) % Accuracy 1 0.095 95 1 0.499 100 1 1.019 102 1 5.061 101 1 10.781 108 1 18.757 94 1 50.430 101 i STD NaN NaN NaN NaN NaN NaN NaN %CV NaN NaN NaN NaN NaN NaN NaN I J 9 9 io Ti 17 13 N 4 17 19 " ?i 27 23 24 25 77 28 29 30 51 33 34 35 3? 36 19 40 41 42 43 44 47 49 4 Cene ! IS Cone V* z^<* u Page 6 of 170 Created with AnalypL Bfiporter Printed: 18/02/2010 3:24:00 PM Analyte Name: Internal Standard: PFDoA 1 13C-PFDoA Data File Acquisition Date Acquisition Method Project 021710\CalLong.wiff 2/17/2010 6:30:13 PM PFCkinetexLong.dam Ewan's Projects\PFCs Result Table Algorithm Used Instrument Name 021710long.rdb IntelliQuan API 5000 Regression Equation: Exp Cone (ng/mL) 0.1 0.5 1 5 10 20 50 y = 0.605 x + -0.00456 (r = 0.9959) ^ # of Values Mean Calc Cone (ng/mL) 1 0.089 1 0.563 1 0.825 1 5.565 1 9.667 1 22.817 1 47.074 % Accuracy 89 113 83 111 97 114 94 / STD NaN NaN NaN NaN NaN NaN NaN %CV NaN NaN NaN NaN NaN NaN NaN 3 s > e io n i: n u is n ia is io zi z: :i Aneh*a Cozn%e /ISCone z i zb b 31 iz u x ]? n n c -o 44 v , . 47 s <i Page 7 of 170 256 ureatea witn Anaiyspj-OEfporter Printed: 18/02/2010 3:24:00 PM K Analyte Name: Internal Standard: PFTrA 1 13C-PFDoA Data File Acquisition Date Acquisition Method Project 021710\CalLong.wiff 2/17/2010 6:30:13 PM PFCkinetexLong.dam Ewan's Projects\PFCs Result Table Algorithm Used Instrument Name 021710long.rdb IntelliQuan API 5000 Regression Equation: Exp Cone (ng/mL) 0.5 1 5 10 20 50 y = 0.336 x + 0.0691 (r = 0.9959) 7 # of Values Mean Calc Cone (ng/mL) 1 0.456 1 0.800 1 5.804 1 11.171 1 21.489 1 46.780 % Accuracy 91 80 116 112 107 94 7 STD NaN NaN NaN NaN NaN NaN %CV NaN NaN NaN NaN NaN NaN 1 4naK4 Cone tISClone^ ~ 4 i i u i? 16 T JO 7t J ? 23 24 25 27 28 31 32 53 34 K 3C 3 7 36 M 41 42 4 3 44 45 46 47 4 44 * ( i iUO 'Z ' Page 8 of 170 257 iytkal Sendees'' created witn Anaiyp. apporter Printed: 18/02/2010 3:24:00 PM Analyte Name: Internal Standard: PFTeA 1 13C-PFDoA Data File Acquisition Date Acquisition Method Project 021710\CalLong.wiff 2/17/2010 6:30:13 PM PFCkinetexLong.dam Ewan's Projects\PFCs Result Table Algorithm Used Instrument Name 021710long.rdb IntelliQuan API 5000 Regression Equation:_______ y = 0.000351 xA2 + 0.246 x + 0.0269 (r = 0.9993) " Exp Cone (ng/mL) # of Values Mean Calc Cone (ng/mL) % Accuracy 0.5 1 0.490 98 1 1 0.931 93 5 1 5.574 111 10 1 10.100 101 20 1 19.165 96 50 1 50.241 100 y STD NaN NaN NaN NaN NaN NaN %CV NaN NaN NaN NaN NaN NaN 5 6 8 TO II 1? 13 1 15 16 17 t# 1 20 21 22 23 Ana!tra Co2n5e 'ISC26one 26 l M 31 32 ]) i f K 3i 3' 3 ^, ? < Q> < Page 9 of 170 258 Created with Analyqk.Rifiporter t Printed: 18/02/2010 3:24:00 PM 1 Project Data File Result Table Instrument Name Ewan's ProjectsVPFCs 021710\CalLong.wiff 021710long.rdb API 5000 Sample Name Acquisition Date Acquisition Method Injection Vial IB 2/17/2010 6:30:13 PM PFCkinetexLong.dam 1 Injection Volume Sample Type Dilution Factor Weight to Volume 5 Unknown 1.00 0.00 Results Summary Analyte Peak Name IS Name PFOA 1 13C-PFOA PFNA 1 13C-PFNA PFOS 1 13C-PFOS PFDA 1 13C-PFDA PFUnA 1 13C-PFUnA PFDS 1 13C-PFOS PFDoA 1 13C-PFDOA PFTrA 1 13C-PFD0A PFTeA 1 13C-PFDOA IS Area 186 185 1700 451 33 1700 174 174 174 Analyte RT {Exp RT ) 1.57 (1.36) 0.00 (2.06) 2.10 (2.09) 0.00(3.06) 0.00 (4.06) 3.94 (3.87) 0.00 (4.55) 5.09 (5.06) 5.42 (5.51) Analyte Area 2795 0 458 0 0 1475 0 4776 4625 Calc. Cone (ng/mL) 296.000 N/A 2.530 N/A N/A 7.550 N/A 81.200 94.900 Modified? No No No No No No No No No (iO Page 10 of 170 259 Created with Analyst- Importer Printed: 18/02/2010 3:24:00 PM IRC Summary Analyte Peak Name PFOA2 S_13C_PFOA PFNA2 S_13C_PFNA PFOS2 S_13C-PFOS PFDA2 S_13C-PFDA PFUnA2 S_13C-PFUnA PFDS2 PFDoA2 S_13C-PFDoA PFTrA 2 PFTeA2 RT (Exp R T ) 0.00(1.36) 1.37 (1.36) 1.90 (2.08) 2.52 (2.44) 2.21 (2.12) 2.20 (2.00) 3.23 (3.06) 3.10 (3.04) 0.00 (3.88) 4.01 (3.88) 0.00(3.87) 0.00 (4.53) 4.70 (4.64) 5.09 (5.13) 5.52 (5.56) Area 0 186 366 276 155 1700 349 451 0 33 0 0 174 426 179 M o d ifie d ? No Calc (Exp) MRM Ratio 0.00 (2.16) Ratio C onfirm s ID No No 0.07 (43.19) No No 0.00(0.34) No No 0.00(0.00) No No 0.34(0.32) YES No 3.71 (21.71) No No 0.00 (0.14) No No 0.00 (17.53) No No 0.00 (0.19) No No 0.00(1.60) No No 0.00(0.32) No No 0.00 (0.28) No No 0.00(3.71) No No 0.09(0.34) No No 0.04 (0.29) No Page 11 of 170 260 Created with AnalysP-F^orter Printed: 18/02/2010 3:24:00 PM Quantitative Peak Review IB too e 0 3 0 100 1 .5 7 ,a / V '. r ' ,, , J4 gHm n / A ,, S PFOA 1 413.0/169.0 Da BnasWerlinnnenPMfiaisksed 2.10 /V/'W'W'-' 50 1 . 3 7 SO ii 10 i19 n y W , lii! I 25 13C-PFOA 417.0/372.0 Da d BnasWerlionnegPMeaisksed PFNA? 463.0/419.0 Da BnasWerlinnnenPMeaisksed ISM g. 1000 M M ii MW c 2.20 *i 500 JO 13C-PFNA 468.0/423.0 Da BnasWerlinnnenPMeaisksed 200 '50 10C I 0 PFOS 1 499.0/80.0 Da BnasWerlinnnen Missed Ppak 13C-PFOS 503.0/80.0 Da BnasWerlinnnenPMpaisksed PFDA 1 513.0/469.0 Da BnasWerlinnnenPMpaisksed 13C-PFDA 515.0/470.0 Da Baseline c Missed r Wrnnn Ppak PFUnA 1 563.0/519.0 Da c BnasWerlinnnenPMeaisksed 13C-PFUnA 565.0/270.0 Da Baseline Missed Wronn Peak PFDS 1 599.0/80.0 Da BnasWerlinnnenPMeaisksed 13C-PFOS 503.0/80.0 Da BnasWerlinnnen Missed Peak PFDoA 1 Tune, mm 13C-PFDOA 613.0/569.0 Da 615.0/169.0 Da Baseline Missed Wrnnn Peak BnasWerlinnnenPMeaisksed 15M 6 lOOO 3 MO 5.42 , . !U u f j |! j! ' J l / I V sJ1t 1M 50 4.7 f . 0 '*i-r V 'n vwj-{ 45 5B 55 SO PFTrAI 663.0/619.0 Da _d__BnasWerlinnnenPMeaisks_e_d___ PFTeA 1 713.0/669.0 Da d Baseline Missed ___n Wrnnn Peak___ 13C-PFDOA 615.0/169.0 Da BnasWerlninnen Missed Peak___ Before After 130-PFDoA 615.0/169.0 Da o BnasWerlinnnen Missed Pnak Page 12 of 170 261 Ion Ratio Confirmation Created with AnalyslPR^borter Printed: 18/02/2010 3:24:00 PM IB Before A fter Page 13 of 170 262 Createci with AnalJ^t^eporter Printed: 18/02/2010 3:24:00 PM Project Data File Acquisition Method Ewan's Projects\PFCs 021710\CalLong.wiff PFCkinetexLong.dam Sample Name A cquisition Date Acquisition Method Sample ID Sample Comment PFC 0.10ppb 2/17/2010 6:52:57 PM PFCkinetexLong.dam LCMS2-85A Results Summary Analyte Name Analyte RT (Expected) PFOA1 1.23(1.36) PFNA1 2.06(2.06) PFOS 1 2.10(2.09) PFDA 1 3.10(3.06) PFUnA 1 3.92 (4.06) PFDS 1 3.91 (3.87) PFDoA 1 4.54 (4.55) PFTrA 1 5.07 (5.06) PFTeA 1 5.56 (5.51) IS Name 13C-PFOA 13C-PFNA 13C-PFOS 13C-PFDA 13C-PFUnA 13C-PFOS 13C-PFDOA 13C-PFDOA 13C-PFDOA IS Area 3289300 2669800 7592300 2504200 222150 7592300 305390 305390 305390 Result Table Algorithm Used Instrument Name Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 021710long.rdb IntelliQuan API 5000 2 5 Standard 1.00 0.00 Analyte Area 14318 21049 63477 27648 26665 66470 14964 10486 6622 Exp Cone (ng/mL) 0.100 0.100 0.100 0.100 0.100 0.100 0.100 0.100 0.100 Calc. Cone (ng7mL) 0.114 Accuracy (%) 114 0.107 107 0.093 93 0.099 99 0.083 83 0.095 95 0.089 89 N/A N/A N/A N/A Mod? No No No No No No No No No 2- ( Page 14 o f 170 263 IRC Summary Analyte Peak Name PFOA 2 S_13C_PFOA PFNA 2 S_13C_PFNA PFOS 2 S_13C-PFOS PFDA2 S J3 C -P F D A PFUnA 2 S_13C-PFUnA PFDS 2 PFDoA2 S_13C-PFDoA PFTrA 2 PFTeA 2 Created with AnalystpRporter Printed: 18/02/2010 3:24:00 PM RT (Expected) 1.25(1.36) 1.24(1.36) 2.08 (2.08) 0.00 (2.44) 2.07(2.12) 2.11 (2.00) 3.12(3.06) 3.12(3.04) 3.89(3.88) 3.92(3.88) 3.91 (3.87) 4.54 (4.53) 4.54 (4.64) 5.11 (5.13) 5.57 (5.56) Area 19544 3289300 8617 0 19074 7592300 3350 2504200 3604 222150 22732 4509 305390 2650 413 M o d ifie d ? No No NO No No No No No No No No No No No No C a lc u la te d Ion Ratio (Expected Value) 1.36 229.73 0.41 0.00 0.30 119.61 0.12 90.57 0.14 8.33 0.34 0.30 20.41 0.25 0.06 Page 15 of 170 264 Created with Anal^fet^eporter Printed: 18/02/2010 3:24:00 PM Quantitative Peak Review 1.23 PFOA 1 413.0/169.0 Da BnasWerlinnnencPMeaisksed 13 C -P F O A 417.0/372.0 Da q Baseline o Missed n Wrnnn Peak PFOS 1 499.0/80.0 Da Baseline Missed Pftak 13C-PFOS 503.0/80.0 Da d BnasWerlinnnen c Missed Peak PFC O.IOppb ;VW PFNA 1 463.0/419.0 Da o BnasWerlinnnen3.P1M0eaisksed 13C-PFNA 468.0/423.0 Da BnasWerlinnnen Missed Peak '{/A,. n ik `w'\/V PFDA 1 513.0/469.0 Da Baseline Missed Wrnnn Peak 13C-PFDA 515.0/470.0 Da o BnasWerlinnnen d Missed Peak V'VU PFUnA 1 563.0/519.0 Da d Baseline Missed n Wrnnn Peak 13C-PFUnA 565.0/270.0 Da Baseline Missed n Wrnnn Peak nn PFDS 1 599.0/80.0 Da Baseline Missed ___ n Wrnnn Peak___ 13C-PFOS 503.0/80.0 Da BnasWerlinnnen Missed Peak PFDoA 1 613.0/569.0 Da c Baseline Missed n Wrnnn Peak 13C-PFDOA 615.0/169.0 Da BnasWerlinnnen Missed Peak 663.0/619.0 Da Baseline Missed n Wrnnn Peak *h SO 13C-PFDOA 615.0/169.0 Da Baseline Missed n Wrnnn Peak PFTeA 1 713.0/669.0 Da Baseline Missed n Wrnnn Peak 13C-PFDoA 615.0/169.0 Da _c__BnasWerlinnnen Missed P e a k ___ Before After 265 Page 16 of 170 Created with Analyst|fRd|5orter Printed: 18/02/2010 3:24:00 PM Ion Ratio Confirmation PFC O.IOppb , lOOtw i 5cn" \ 1.25 n ..................K T ........ PFOA2 413.0/369.0 Da Baseline Missed Wrong Peak ..."735 ..I tit77774"5.... "77 PFUnA2 563.0/269.0 Da Baseline Missed Wrong Peak PFNA2 463.0/219.0 Da Baseline c Missed Wrong Peak iToeo 10000 ww 25 w"> 00 2000 10 135 I *0: ...<.5.... PFDS2 599.0/99.0 Da Baseline Missed Wrong Peak PFOS2 499.0/99.0 Da Baseline Missed Wrong Peak 10000 |a 000 btwo I 00 2006 4.k4 40 45 50 PFDoA2 613.0/169.0 Da Baseline Missed Wrong Peak PFDA2 513.0/269.0 Da Baseline c Missed Wrong Peak 10i4 25*4. 15 20*4 2$ 104 50*3 PFTrA 2 663.0/169.0 Da G Baseline Misse Wrong Peak PFTeA2 713.0/169.0 Da Baseline Missed o Wrong Peak Before A fter Page 17 of 170 266 Created with A nalfst^eporter Printed: 18/02/2010 3:24:00 PM Project Data File Acquisition Method Ewan's Projects\PFCs 021710\CalLong.wiff PFCk.inetexLong.dam Sample Name A cquisition Date Acquisition Method Sample ID Sample Comment PFC 0.5ppb 2/17/2010 7:00:32 PM PFCkinetexLong.dam LCMS2-85B Results Summary Analyte Name Analyte RT (Expected) PFOA 1 1.27(1.36) PFNA1 2.06 (2.06) PFOS 1 2.09(2.09) PFDA 1 3.10(3.06) PFUnA 1 3.89 (4.06) PFDS 1 3.90 (3.87) PFDoA 1 4.54 (4.55) PFTrA 1 5.07 (5.06) PFTeA 1 5.53 (5.51) IS Name 13C-PFOA 13C-PFNA 13C-PFOS 13C-PFDA 13C-PFUnA 13C-PFOS 13C-PFDoA 13C-PFDOA 13C-PFDOA IS Area 3385400 2759300 7581500 2783700 204480 7581500 275140 275140 275140 Result Table Algorithm Used Instrument Name Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 021710long.rdb InteltiQuan API 5000 3 5 Standard 1.00 0.00 Analyte Area 77019 128820 383910 140780 120250 428430 92483 61214 40588 Exp Cone (ng/mL) 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 0.500 Calc. Cone (ng/mL) 0.477 Accuracy (%) 95 0.463 93 0.489 98 0.482 96 0.530 106 0.499 100 0.563 113 0.456 91 0.490 98 Mod? No No No No No No No No No Page 18 of 170 267 IRC Summary Analyte Peak Name PFOA2 S_13C_PFOA PFNA2 S_13C_PFNA PFOS 2 S_13C-PFOS PFDA2 S_13C-PFDA PFUnA 2 S_13C-PFUnA PFDS 2 PFDoA2 S_13C-PFDoA PFTrA 2 PFTeA 2 Created with AnalysPRf^porter Printed: 18/02/2010 3:24:00 PM RT (Expected) 1.28(1.36) 1.27(1.36) 2.08 (2.08) 0.00 (2.44) 2.13 (2.12) 2.10(2.00) 3.10(3.06) 3.08 (3.04) 3.90 (3.88) 3.92(3.88) 3.90(3.87) 4.55 (4.53) 4.53 (4.64) 5.08 (5.13) 5.52 (5.56) Area 173300 3385400 42381 0 121730 7581500 18842 2783700 26323 204480 128520 22676 275140 21930 12493 M od ifie d ? No No No No No No No No No No No No No No No C a lc u la te d Ion Ratio (Expected Value) 2.25 43.96 0.33 0.00 0.32 19.75 0.13 19.77 0.22 1.70 0.30 0.25 2.98 0.36 0.31 Page 19 of 170 268 / ? Columbia Analytical Services* Created with Analypt Importer Printed: 18/02/2010 3:24:00 PM Quantitative Peak Review PFC 0.5ppb |iS rsJ161oo0000o000wf0p0t os i | jHgBpHMg"H"1S bbb**kN j> ,f io is 3*5 1I ,V ifSl :o os to1 is *&g 11254620000000000000000000 :o 25*5 20*5 |& l 5*5 10*5 50*4 15 20 25 Hi 15 I2C 25 PFOA 1 13C-PFOA PFNA1 13C-PFNA 413.0/169.0 Da 417.0/372.0 Da 463.0/419.0 Da 468.0/423.0 Da Baseline Missed ______ n Wrong Peak_____ .5*4 i ,c,,4 * 510(**41 15 1?0 25 1fg 36 pfosT 499.0/80.0 Da _ _ _ 2_00_00_ _BnasWerlinn3nen^ Missed Peak_ _ _ _ _ _ _ 15000 | 10CIU SOW i51 Ic :54U1*****S55s55 BnasWerlinnnen Missed Peak 15 2T0un* mm 25 30 fs8g 20000 BnasWerlinnnen3 Missed P1 0eak 15000 10000 sooo fI,,& 25 ---- - -3-0- - - - - - - - 3-5- - - - - - - - -4-0- 13C-PFOS PFDA? 503.0/80.0 Da 4*4 BnasWerlinnn3en^ 2PMeaisksed 4 513.0/469.0 Da 1&m 21543l?0*******44444444 BnasWerlinnnen Missed Peak 1f c 46 BnasWerlinnnen3o.P0M8eaisksed 3*5 w US i 13C-PFDA ' 515.0/470.0 Da 6524U3*****S65555 BnasWerlinnnenc Missed Peak 35 40 4S 50 35 43 45 50 PFUnXi 13C-PFUnA 563.0/519.0 Da 565.0/270.0 Da __I?& .-now BnasWerlinnnencPMeaisksed imn TO <0 45 ...5.0............. 1Ji8' 24U85*****444444i Bna4sW.0erlinnne4n4.i55o3PMeais5k0sed 5S PFDoA"l 613.0/569.0 Da i|.& C.3)'0055****4444 JBnasWerlinnnen Missed Peak I! 5.53 50) \ ......S.O. L55 . . - 58 . . . 1*v 13C-PFDOA 615.0/169.0 Da 65**44 BnasWerlinnne4n.5 3PMeaisksed 42j***444 40 45 50 55 Ills 4rtu*wi . 130 35 40 45 PFDS 1 599.0/80.0 Da BnasWerlinnnena Missed Peak 5.07 I15 2C 25 30 13C-PFOS 503.0/80.0 Da BnasWerlinnnen Missed Peak *& 654***444 1 '1l*4i 45 50 65 60 4.0 45 50 55 PFTrA 1 663.0/619.0 Da BnasWerlinnneno Missed Peak_____ 13C-PFDOA B6na1sW5e.0rlin/n1ne6n9 P.0MeaDiskased PFTeA 1 G B7na1sW3e.0rlinn/6ne6n9 P.0MeaDiskas_e_d___ 13C-PFDOA B6na1sW5e.0rlin/n1ne6n9 P.0MeaDiskas_e_d___ Before After Page 20 of 170 269 Ion Ratio Confirmation Created with AnalysPR4?)orter Printed: 18/02/2010 3:24:00 PM PFC 0.5ppb Before A fter Page 21 o f 170 270 ST CAonlaulymtibciaal Services- Created with Analyst importer Printed: 18/02/2010 3:24:00 PM Project Data File Acquisition Method Ewan's Projects\PFCs 021710\CalLong.wiff PFCkinetexLong.dam Sample Name A cqu isition Date Acquisition Method Sample ID Sample Comment PFC 1.0ppb 2/17/2010 7:08:07 PM PFCkinetexLong.dam LCMS2-85C Results Summary Analyte Name Analyte RT (Expected) PFOA 1 1.23 (1.36) IS Name 13C-PFOA IS Area 3356000 PFNA 1 2.03 (2.06) 13C-PFNA 2574400 PFOS 1 2.08 (2.09) 13C-PFOS 7600400 PFDA 1 3.08 (3.06) 13C-PFDA 2542500 PFUnA 1 3.90 (4.06) 13C-PFUnA 209310 PFDS 1 3.89(3.87) 13C-PFOS 7600400 PFDoA 1 4.54 (4.55) 13C-PFDoA 290240 PFTrA 1 5.07 (5.06) 13C-PFDOA 290240 PFTeA 1 5.53 (5.51) 13C-PFDOA 290240 Result Table Algorithm Used Instrument Name Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 021710long.rdb IntelliQuan API 5000 4 5 Standard 1.00 0.00 Analyte Area 158340 297510 821270 291450 245580 893930 143490 98161 74342 Exp Cone (ng/mL) 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 Calc. Cone (ng/mL) 0.958 Accuracy (%) 96 1.100 110 1.030 103 1.100 110 1.090 109 1.020 102 0.825 83 0.800 80 0.931 93 Mod? No No No No No No No No No Page 22 o f 170 271 IRC Summary Analyte Peak Name PFOA2 S_13C_PFOA PFNA2 S_13C_PFNA PFOS 2 S_13C-PFOS PFDA2 S_13C-PFDA PFUnA2 S_13C-PFUnA PFDS 2 PFDoA 2 S_13C-PFDoA PFTrA 2 PFTeA2 Created with AnalysPRjborter Printed: 18/02/2010 3:24:00 PM RT (Expected) 1.26(1.36) 1.25 (1.36) 2.02 (2.08) 0.00 (2.44) 2.07(2.12) 2.08 (2.00) 3.10 (3.06) 3.05 (3.04) 3.90 (3.88) 3.89(3.88) 3.89(3.87) 4.53 (4.53) 4.54 (4.64) 5.07(5.13) 5.52(5.56) Area 372000 3356000 93995 0 262120 7600400 36921 2542500 48498 209310 271790 43135 290240 34820 20771 M o d ifie d ? No No No No No No No No No No No No No No No C a lc u la te d Ion Ratio (Expected Value) 2.35 21.19 0.32 0.00 0.32 9.25 0.13 8.72 0.20 0.85 0.30 0.30 2.02 0.35 0.28 Page 23 of 170 272 Quantitative Peak Review Created with Analyst importer Printed: 18/02/2010 3:24:00 PM PFC 1.0ppb PFOA 1 413.0/169.0 Da Baseline Missed p Wrnnn Ppak I______ ^ _____ Li13C-PFOA 417.0/372.0 Da Baseline Missed _____ n Wrnnn Peak___ PFOS 1 499.0/80.0 Da Baseline Missed n Wrnnn Ppak 13C-PFOS 503.0/80.0 Da Baseline Missed n Wrnnn Peak PFNA 1 463.0/419.0 Da o Baseline Missed n Wrnnn Peak la PFDA 1 513.0/469.0 Da Baseline Missed n W rnnn Pp.ak 13C-PFNA 468.0/423.0 Da Baseline Missed i Wrnnn Peak 13C-PFDA 515.0/470.0 Da Baseline a Missed n Wrnnn Peak IPFUnA 1 563.0/519.0 Da Baseline c Missed ___ r Wrnnn Peak PFDoA 1 613.0/569.0 Da Baseline Missed n Wrnnn Peak Tun, nun 13C-PFUnA 565.0/270.0 Da Baseline Missed W rnnn Peak 13C-PFDoA 615.0/169.0 Da Baseline Missed n Wrnnn Peak JO J5 PFDS 1 599.0/80.0 Da Baseline Missed Wrnnn Peak PFTrA 1 663.0/619.0 Da Baseline Missed r. W rnnn Peak 13C-PFOS 503.0/80.0 Da Baseline Missed Wrnnn Peak 13C-PFDOA 615.0/169.0 Da Baseline Missed n Wrnnn Peak PFTeA 1 713.0/669.0 Da Baseline Missed ___ n W rnnn Peak___ 13C-PFDOA 615.0/169.0 Da Baseline Missed ___n Wrong Peak___ Before After 273 Page 24 o f 170 Ion Ratio Confirmation Created with AnalysPF&f)orter Printed: 18/02/2010 3:24:00 PM PFC 1.0ppb Before A fter Page 25 of 170 274 Created with Analyst importer Printed: 18/02/2010 3:24:00 PM Project Data File Acquisition Method Ewan's Projects\PFCs 021710\CalLong.wiff PFCkinetexLong.dam Result Table Algorithm Used Instrument Name 021710long.rdb IntelliQuan API 5000 Sample Name A cquisition Date Acquisition Method Sample ID Sample Comment PFC 5.0ppb 2/17/2010 7:15:39 PM PFCkinetexLong.dam LCMS2-85D Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 5 5 Standard 1.00 0.00 Results Summary Analyte Name Analyte RT (Expected) PFOA 1 1.20(1.36) PFNA1 1.98(2.06) PFOS 1 2.03(2.09) PFDA 1 3.06 (3.06) PFUnA 1 3.89 (4.06) PFDS 1 3.88 (3.87) PFDoA 1 4.52 (4.55) PFTrA 1 5.06 (5.06) PFTeA 1 5.51 (5.51) IS Name 13C-PFOA 13C-PFNA 13C-PFOS 13C-PFDA 13C-PFUnA 13C-PFOS 13C-PFDOA 13C-PFDOA 13C-PFDOA IS Area 3384000 2759300 7552200 2677400 210740 7552200 243760 243760 243760 Analyte Area 831690 1480000 4176000 1362800 1190900 4421900 819010 492610 343170 Exp Cone (ng/mL) 5.000 5.000 5.000 5.000 5.000 5.000 5.000 5.000 5.000 Calc. Cone (ng/mL) 4.870 Accuracy (%) 97 4.960 99 5.190 104 4.930 99 5.370 107 5.060 101 5.560 111 5.800 116 5.570 111 Mod? NO No No No No No No No No I/O Page 26 of 170 275 IRC Summary Analyte Peak Name PFOA2 S_13C_PFOA PFNA2 S_13C_PFNA PFOS 2 S_13C-PFOS PFDA2 S_13C-PFDA PFUnA2 S_13C-PFUnA PFDS 2 PFDoA2 S_13C-PFDoA PFTrA 2 PFTeA2 Created with AnalysP'RS^orter Printed: 18/02/2010 3:24:00 PM RT (Expected) 1.21 (1.36) 1.19(1.36) 1.97(2.08) 0.00 (2.44) 2.03(2.12) 2.01 (2.00) 3.03 (3.06) 3.06 (3.04) 3.86(3.88) 3.88 (3.88) 3.87(3.87) 4.53 (4.53) 4.55 (4.64) 5.05(5.13) 5.51 (5.56) Area 1906300 3384000 478680 0 1325400 7552200 184660 2677400 248160 210740 1386100 232560 243760 160530 126530 M o d ifie d ? No No No No No No No No No No No No No No No C a lc u la te d Ion Ratio (Expected Value) 2.29 4.07 0.32 0.00 0.32 1.81 0.14 1.96 0.21 0.18 0.31 0.28 0.30 0.33 0.37 Page 27 of 170 276 Created with A n a l^ t Reporter Printed: 18/02/2010 3:24:00 PM Quantitative Peak Review PFC 5.0ppb 1.20 12*5 1.98 10*5 \ 3*4 1 '4 * 2 0*S | .5*5 l0*5 5 "* 5 0*4 S 40.4 20*4 05 n i is ru I05 10 15 20 L 15 20 25 Tim* min pfo aT 13C-PFOA PFNA 1 413.0/169.0 Da a Baseline Missed 417.0/372.0 Da C Baseline Missed 463.0/419.0 Da C Baseline Missed ______ 0*5 a. 'GaS i, ' I 10*5 00*0 n Wrnnn Peak_____ ' 1 I is ;u :s jn SeS 5 J*5 2.5 *S n Wrnnn Peak 15 20 25 T*n* mm l 5*5 1 !i 5 0*4 30 n Wrnnn Peak 3.06 m 2S 16 35 Turn* nun PFOS 1 13C-PFOS PFDA 1 499.0/80.0 Da 503.0/80.0 Da 513.0/469.0 Da a Baseline Missed n Wrnnn Peak Baseline Missed n Wrnnn Peak BnasWerlinnnenPMeaisksed 15*5 3^3 35 0 4S PFUnATM1 1*4 I '** 3^ 50 !5 40 4 5 Ten* mm 13C-PFUnA 7*5 6*5 .M iI w"s 2*5 1*5 50 10 I 735 40 PFDS 45 563.0/519.0 Da 565.0/270.0 Da 599.0/80.0 Da Baseline Missed n Wrnnn Peak Baseline a Missed n Wrnnn Peak BnasWerlinnnenPMeaisksed i 5*5 fc 10*5 " 50*4 ilI 3 `0 45 50 PFDoAl 613.0/569.0 Da D Baseline Missed n Wrnnn Peak 6M- 5.51 4*4 L.3i 1*4 I 2*4 I l4.0 4S SO Ton*, mm 13C-PFDOA 5.5 615.0/169.0 Da Baseline Missed n Wrnnn Peak 4|5 It 4 10*5 80*4 ^ *0e4 |! 40*4 20*4- I 45 50 $S PFTrA"l 663.0/619.0 Da BnasWerlinnnen Missed Peak 1*4 2 0*5 3i|& l 11*5 50*4 Id I<5 20 25 13C-PFNA 468.0/423.0 Da c Baseline Missed n Wrnnn Peak 3 0*5 3.06 2 5*5 4&g :os >5.5 5 40 1 0*5 5 0*4 i25 30 35 13C-PFDA 515.0/470.0 Da o Baseline Missed n Wrnnn Peak SeS 2.01 4*5 |" 1TM 1.5 15 20 5 Jfl 13C-PFOS 503.0/80.0 Da q BnasWerlionnenPMeaisksed 1& ltA 2 60 46 45 SD 56 13C-PFDOA 615.0/169.0 Da Baseline q Missed n Wrnnn Peak_____ SO 55 60 40 45 SO 55 PFTeA 1 713.0/669.0 Da a Baseline Missed _____ n Wrnnn Peak_____ 13C-PFDOA 615.0/169.0 Da BnasWerlinnnen Missed Peak_____ Before After Page 28 of 170 277 Created with A nalysP F^orter Printed: 18/02/2010 3:24:00 PM Ion Ratio Confirmation PFC 5.0ppb ........ ;............... i D 18 : Tin nm : <s PFOA2 413.0/369.0 Da Baseline Missed Wrong Peak l SeS ~ IObS y 1 I 3 T r TM . . . 45 PFUnA2 563.0/269.0 Da Baseline c Missed Wrong Peak 1C 60*4 1 -------- 1-------------- :o4 ....... is t :ok : ......... : s jo I n Me PFNA2 463.0/219.0 Da Baseline Missed Wrong Peak 7e$ . 6*5 H S*S 4ei Jl 1 J*S 1 w ..........................................- i f .............- ............................. 1*5 J0 m 55 40 *5 PFDS 2 599.0/99.0 Da Baseline Missed Wrong Peak <5*s :os f1 ,1i04.SC J\ 50*4 .......... .................... IS JC ?S JO PFOS2 499.0/99.0 Da Baseline Missed Wrong Peak 15*5 | ji ____ i I s0*4 E3______ " -- It " 40 5 50 PFDoA2 613.0/169.0 Da Baseline Missed Wrong Peak ! S*S 2 10tl S 50*4 _3/0 ...............tM X:............. PFDA2 513.0/269.0 Da Baseline Misse Wrong Peak 6*4 S 6*4 t|f 4*4 ............. 5. 5... ......... 2*4 & 45 SC 55 Tuan min PFTrA 2 663.0/169.0 Da Baseline Missed Wrong Peak PFTeA2 713.0/169.0 Da Baseline o Missed d Wrong Peak Before A fter Page 29 of 170 278 Created with Anali&tReporter Printed: 18/02/2010 3:24:00 PM Project Data File Acquisition Method Ewan's Projects\PFCs Q21710\CalLong.wiff PFCkinetexLong.dam Result Table Algorithm Used Instrument Name 021710long.rdb IntelliQuan API 5000 Sample Name A cquisition Date Acquisition Method Sample ID Sample Comment PFC 10ppb 2/17/2010 7:23:15 PM PFCkinetexLong.dam LCMS2-85E Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 6 5 Standard 1.00 0.00 Results Summary Analyte Name A nalyte RT (Expected) PFOA 1 1.27(1.36) PFNA1 2.03(2.06) PFOS 1 2.09 (2.09) PFDA1 3.08(3.06) PFUnA 1 3.88 (4.06) PFDS 1 3.90 (3.87) PFDoA 1 4.55 (4.55) PFTrA 1 5.06 (5.06) PFTeA 1 5.53(5.51) IS Name 13C-PFOA 13C-PFNA 13C-PFOS 13C-PFDA 13C-PFUnA 13C-PFOS 13C-PFDOA 13C-PFDoA 13C-PFDOA IS Area 3499200 2760800 7587400 2754900 239570 7587400 291580 291580 291580 Analyte Area 1798800 2948100 8820800 2866500 2341000 9289900 1702900 1115500 742120 Exp Cone (ng/mL) 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 10.000 Calc. Cone (ng/mL) 10.200 Accuracy (%) 102 9.850 99 10.900 109 10.100 101 9.320 93 10.800 108 9.670 97 11.200 112 10.100 101 Mod? No No No No No No No No No ^\v Page 30 of 170 279 iiimbia IRC Summary Analyte Peak Name PFOA 2 S_13C_PFOA PFNA2 S_13C_PFNA PFOS 2 S_13C-PFOS PFDA2 S_13C-PFDA PFUnA2 S_13C-PFUnA PFDS 2 PFDoA2 S_13C-PFDoA PFTrA 2 PFTeA2 Created with Analyjfr Importer Printed: 18/02/2010 3:24:00 PM RT (Expected) 1.28(1.36) 1.25(1.36) 2.03 (2.08) 0.00 (2.44) 2.09 (2.12) 2.09 (2.00) 3.10(3.06) 3.09 (3.04) 3.88(3.88) 3.89 (3.88) 3.89 (3.87) 4.53 (4.53) 4.55 (4.64) 5.06 (5.13) 5.52 (5.56) Area 4114400 3499200 959540 0 2823500 7587400 423110 2754900 498530 239570 3009400 513210 291580 355810 262660 M o d ifie d ? No No No No No No No No No No No No No No No C a lc u la te d Ion Ratio (Expected Value) 2.29 1.95 0.33 0.00 0.32 0.86 0.15 0.96 0.21 0.10 0.32 0.30 0.17 0.32 0.35 Page 31 of 170 280 Created with Analy^.Fporter Printed: 18/02/2010 3:24:00 PM Quantitative Peak Review " 1Cr6 S.4 3U*5 25eS & 2 0*5 1 is.5 s i oes i SCJ i 0 `. ID >5 2 If Tifna mm os io is PFOA 1 13C-PFOA :o 25*5 20.5 8 15*5 i g | lOeS 50J i2 .0 3 IS 20 25 PFNA 7 PFC 10ppb ; us :u*s & ' US I i c5 SOeJ 30 2 .0 4 L 15 20 T m t mm 13C-PFNA 25 413.0/169.0 Da 417.0/372.0 Da 463.0/419.0 Da 468.0/423.0 Da Baseline Missed n Wrnnn Peak c Baseline c Missed n Wrnnn Peak c Baseline Missed n Wrnnn Peak c Baseline Missed n Wrnnn Peak V, Ml 1 S.5 ? i 4eS iS us SeS 8 Mi | 3.5 3 2.5 'e5 Mi SfA 8 1i M 1*5 3 .0 8 i *sS US & | 2.6 S 1 PFOS T is :o :5 Tun mm 13C-PFOS io 2.5 30 Tw .m n PFDA 1 3S 0 25 30 IS 13C-PFDA 499.0/80.0 Da 503.0/80.0 Da 513.0/469.0 Da 515.0/470.0 Da o Baseline a Missed _____________n Wrnnn Peak_____ 3 1*5 it', 'ii I jo PFUnAi j r. t ( so c Baseline Missed n Wrnnn Peak 3^ -< i.J 35 0 J 5 13C-PFUnA Baseline Missed n Wrnnn Peak 1 | I06 I 5 SOeS SO 30 I 35 40 T*i min PFDS 1 45 Baseline Missed _____ n Wrnnn Peak_____ US 5.5 8 *tS 1 .s 15 20 26 13C-PFOS 10 563.0/519.0 Da 565.0/270.0 Da 599.0/80.0 Da 503.0/80.0 Da D Baseline Missed n Wrnnn Peak 1.'- . [ Ir is 0 JS PFDoaI so Baseline Missed n Wrnnn Peak 6.J 4.55 6.4 8 4.J " Baseline Missed n Wrnnn Peak 5[ 2.5.5 8 2D.5 1 15e5 10.5 l JO J5 50 TW. mm 13C-PFDOA 5D.J ' $5 JS 50 55 PFTrA 1 Baseline Missed n Wrnnn Peak UJ 5.J & . -4 *M 00 4.0 45 50 65 13C-PFDoA 613.0/569.0 Da 615.0/169.0 Da 663.0/619.0 Da 615.0/169.0 Da Baseline Missed n Wrnnn Peak 5.53 Q Baseline Missed n Wrnnn Peak 6.J 4^5 Baseline Missed Baseline o Missed n Wrnnn Peak_____ _____________ n Wrnnn Peak_____ ' S*S 5*4 | J#J 1 5 -.'.J 3S 2.J 1 SO 55 60 J.B JS SO 55 PFTeATM1 713.0/669.0 Da Baseline Missed r Wrong Peak_____ 13C-PFDoA 615.0/169.0 Da c Baseline Missed n Wrnnn Peak_____ Before After Page 32 o f 170 281 Ion Ratio Confirmation Created with Analyst- importer Printed: 18/02/2010 3:24:00 PM PFC 10ppb PFOA2 413.0/369.0 Da Baseline d Missed Wrong Peak & 2S 3 . s i - ..........~ " " W : <0 T .bs rttt -- *5 PFUnA2 563.0/269.0 Da Baseline Missed Wrong Peak PFNA2 463.0/219.0 Da a Baseline Missed q Wrong Peak 15*G 11 & 10*i I i 5 50e5 -3 # - . M JO 35 0 <5 Tim r m PFDS2 599.0/99.0 Da Baseline Missed Wrong Peak PFOS2 499.0/99.0 Da Baseline Missed Wrong Peak i0S 25*5 & 00*4 f 15.5 * lOeS SOM 3 ________ <0 5 so PFDoA2 613.0/169.0 Da Baseline Missed Wrong Peak PFDA2 513.0/269.0 Da d Baseline Missed Wrong Peak ' 5S iOeS | 10*5 50e< PFTrA 2 663.0/169.0 Da Baseline Missed Wrong Peak PFTeA 2 713.0/169.0 Da Baseline Missed Wrong Peak Before A fter Page 33 of 170 282 fc$' Created with Analyqt>.RE>orter Printed: 18/02/2010 3:24:00 PM Project Data File Acquisition Method Ewan's Projects\PFCs 021710\CalLong.wiff PFCkinetexLong.dam Result Table Algorithm Used Instrum ent Name 021710long.rdb IntelliQuan API 5000 Sample Name A cqu isition Date Acquisition Method Sample ID Sample Comment PFC 20ppb 2/17/2010 7:30:49 PM PFCkinetexLong.dam LCMS2-85F Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 7 5 Standard 1.00 0.00 Results Summary Analyte Name Analyte RT (Expected) PFOA1 1.23 (1.36) PFNA 1 2.00 (2.06) PFOS 1 2.06(2.09) PFDA 1 3.05 (3.06) PFUnA 1 3.88 (4.06) PFDS 1 3.88 (3.87) PFDoA 1 4.53 (4.55) PFTrA 1 5.07 (5.06) PFTeA 1 5.52 (5.51) IS Name 13C-PFOA 13C-PFNA 13C-PFOS 13C-PFDA 13C-PFUnA 13C-PFOS 13C-PFDOA 13C-PFDOA 13C-PFDOA IS Area 3368000 2744800 7774400 2957800 209900 7774400 265160 265160 265160 Analyte Area 3142500 5275000 15521000 5644600 4476600 16094000 3656900 1934500 1290400 Exp Cone (ng/mL) 20.000 20.000 20.000 20.000 20.000 20.000 20.000 20.000 20.000 Calc. Cone (ng/mL) 18.400 Accuracy (%) 92 17.700 89 18.700 93 18.500 92 20.400 102 18.800 94 22.800 114 21.500 107 19.200 96 Mod? No No No No No No No No No v Page 34 of 170 283 IRC Summary Analyte Peak Name PFOA2 S_13C_PFOA PFNA2 S_13C_PFIMA PFOS 2 S_13C-PFOS PFDA2 S_13C-PFDA PFUnA2 S_13C-PFUnA PFDS 2 PFDoA2 S_13C-PFDoA PFTrA 2 PFTeA2 Created with Analyst- importer Printed: 18/02/2010 3:24:00 PM RT (Expected) 1.24(1.36) 1.21 (1.36) 2.00 (2.08) 0.00 (2.44) 2.03 (2.12) 2.05 (2.00) 3.06 (3.06) 3.08 (3.04) 3.89 (3.88) 3.88 (3.88) 3.88 (3.87) 4.52 (4.53) 4.53 (4.64) 5.06 (5.13) 5.52(5.56) Area 7082100 3368000 1812800 0 4981100 7774400 817940 2957800 828080 209900 5244600 895480 265160 608580 427830 M o d ifie d ? No No No No No No No No No No No No No No No C a lc u la te d Ion Ratio (Expected Value) 2.25 1.07 0.34 0.00 0.32 0.50 0.14 0.52 0.18 0.05 0.33 0.24 0.07 0.31 0.33 Page 35 o f 170 284 lu m b l Created with Analy^Ffeporter Printed: 18/02/2010 3:24:00 PM Quantitative Peak Review Ji PFOA 1 413.0/169.0 Da BnasWerlinnnenPMeaisksed 13C-PFOA 417.0/372.0 Da BnasWerlinnnenPMeaisks_e_d_ ______ 2 ^ ^ PFC 20ppb ^n*5 1.|99 15 2Q f 1- AB sm JHHk 00.0------ ----- /B^ ^ -------- PFNA 1 463.0/419.0 Da Baseline Missed n Wrnnn Peak. 13C-PFNA 468.0/423.0 Da o Baseline Missed ___r Wrnnn Peak___ PFOS 1 499.0/80.0 Da BnasWerlinnnenPMeaisksed 13C-PFOS 503.0/80.0 Da BnasWerlinnnenPMeaisksed PFDA 1 513.0/469.0 Da BnasWerlinnnenPMeaisksed 13C-PFDA 515.0/470.0 Da Baseline Missed n Wrnnn Peak PFUnA 1 563.0/519.0 Da Baseline Missed Wrnnn Peak 13C-PFUnA 565.0/270.0 Da Baseline Missed Wrnnn Peak PFDS 1 599.0/80.0 Da BnasWerlinnnenPMeaisksed 13C-PFOS 503.0/80.0 Da Baseline Missed n Wrnnn Peak PFDoA 1 613.0/569.0 Da o BnasWerlinnnenPMaaisksed 3.v50**55 :j 13C-PFD0A 615.0/169.0 Da BnasWerlinnnenPMeaisksed PFTrA 1 663.0/619.0 Da o BnasWerlinnnen Missed Paak 13C-PFDOA 615.0/169.0 Da BnasWerlinnnenPMeaisksed 50 55 SO PFTeA 1 713.0/669.0 Da _d__BnasWerlinnnendPMeaisks_e_d_ 13C-PFDoA 615.0/169.0 Da o BnasWerlinnnen d Missed Peak___ Before After Page 36 of 170 285 Created with Analyfl- dporter Printed: 18/02/2010 3:24:00 PM Ion Ratio Confirmation 1.24' TsS 8 1! M A .............................. 1$ 20 25 50 PFOA2 413.0/369.0 Da a Baseline d Missed o Wrong Peak PFNA 2 463.0/219.0 Da Baseline Missed Wrong Peak Isw toes MM 20e5 kPFC 20ppb S*5 A 9 si ,| 3 06 15 :d 25 30 ......2.5.....A33 .\...3.5......... PFOS2 499.0/99.0 Da Baseline Missed a Wrong Peak PFDA*2 513.0/269.0 Da Baseline c Missed Wrong Peak PFUnA2 563.0/269.0 Da Baseline Missed Wrong Peak PFDS2 599.0/99.0 Da Baseline Missed Wrong Peak PFDoA2 613.0/169.0 Da Baseline Missed g Wrong Peak PFTrA 2 663.0/169.0 Da Baseline c Missed Wrong Peak 5 PFTeA2 713.0/169.0 Da Baseline Missed Wrong Peak Before A fter Page 37 of 170 286 Created with AnalyqLFBSporler Printed: 18/02/2010 3:24:00 PM Project Data File Acquisition Method Ewan's Projects\PFCs 02171 OVCalLong.wiff PFCkinetexLong.dam Result Table Algorithm Used Instrument Name 021710long.rdb IntelliQuan API 5000 Sample Name A cqu isition Date Acquisition Method Sample ID Sample Comment PFC 50ppb 2/17/2010 7:38:21 PM PFCkinetexLong.dam LCMS2-85G Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 8 5 Standard 1.00 0.00 Results Summary Analyte Name Analyte RT (Expected) PFOA1 1.21 (1.36) PFNA1 2.03 (2.06) PFOS 1 2.02 (2.09) PFDA1 3.04 (3.06) PFUnA 1 3.87 (4.06) PFDS 1 3.87(3.87) PFDoA 1 4.51 (4.55) PFTrA 1 5.07 (5.06) PFTeA 1 5.52 (5.51) IS Name 13C-PFOA 13C-PFNA 13C-PFOS 13C-PFDA 13C-PFUnA 13C-PFOS 13C-PFDoA 13C-PFDOA 13C-PFDOA IS Area 3380100 2533800 7717500 2651100 204360 7717500 267090 267090 267090 Analyte Area 8848200 14442000 41433000 14068000 10651000 37888000 7600500 4220200 3542200 Exp Cone (ng/mL) 50.000 50.000 50.000 50.000 50.000 50.000 50.000 50.000 50.000 Calc. Cone (ng/mL) 51.600 Accuracy <%) 103 52.400 105 50.200 100 51.400 103 49.800 100 50.400 101 47.100 94 46.800 94 50.200 100 Mod? No No No No No No No No No Page 38 o f 170 287 IRC Summary Analyte Peak Name PFOA2 S_13C_PFOA PFNA2 S_13C_PFNA PFOS 2 S J3C -P F O S PFDA2 S_13C-PFDA PFUnA 2 S_13C-PFUnA PFDS 2 PFDoA2 S_13C-PFDoA PFTrA 2 PFTeA2 Created with Analyfi-im porter Printed: 18/02/2010 3:24:00 PM RT (Expected) 1.23(1.36) 1.23 (1.36) 1.99 (2.08) 0.00 (2.44) 2.03 (2.12) 2.05 (2.00) 3.10(3.06) 3.04 (3.04) 3.89(3.88) 3.90(3.88) 3.87 (3.87) 4.52 (4.53) 4.52 (4.64) 5.06 (5.13) 5.51 (5.56) Area 20502000 3380100 4847600 0 13702000 7717500 2112300 2651100 1929500 204360 13707000 2322100 267090 1870600 1057700 M od ifie d ? No No No No No No No No No No No No No No No C a lc u la te d ton R atio (Expected Value) 2.32 0.38 0.34 0.00 0.33 0.19 0.15 0.19 0.18 0.02 0.36 0.31 0.04 0.44 0.30 Page 39 of 170 288 1Quantitative Peak Review ' 5*5 ut ?o*5 i :1 "*5 50*4 L !2*i I 0*b 6 Qe$ f 3 60*5 40*5 7 0.5 Created with AnalydM#$porter Printed: 18/02/2010 3:24:00 PM PFC 50ppb L2.03 2:0*5 1 S5 f 10*6 I 60*4 L 06 u :d PFOA1 413.0/169.0 Da Baseline c Missed r Wronn Peak ,, 2o.. ; t6M 3 l 0*i 5 0*6 06 10 5 20 13C-PFOA 417.0/372.0 Da c 5*5 BnasWerlionne2n.o0P5Meaisksed 45 i& 1*5 | 2.5 1*5 15 20 25 10 15 20 25 1PFNA1 463.0/419.0 Da ______BnasWerlinnnen3.0P4Meaisks_e_d___ 15*6 | , sS 60*6 B * l 5 13C-PFNA 468.0/423.0 Da c Baseline Missed <06? n Wrnnn3.0P4eak Z5e5 2 [i5 1 6.5 10*5 50*4 <6 l ro ? s 30 15 20 25 30 T*n*.ir*n 25 30 35 T** nwi 40 25 30 35 pfosT 13C-PFOS PFDA 1 13C-PFDA 499.0/80.0 Da 503.0/80.0 Da 513.0/469.0 Da 515.0/470.0 Da BnasWerlinnnen Missed Peak 1$*i . 10*i 6 0*6 BnasWerlinnnen Missed Peak 3 0*4 :s.4 & 2n*4 . .* 1 5*4 ! 5 0*3 i 6*6 BnasWerlinnnen3g Missed ^Peak 3 M *! M 2*t 1*6' BnasWerlinnnen Missed Peak 6*5 54 5*5 T*n* nwi PFUnA 1 563.0/519.0 Da D BnasWerlionnenPMeaisksed 14*S 12*i 10*50*1 I<0*6 :o*6 40 45 50 Tmv* nwi PFDoA 1 613.0/569.0 Da 8*5 BnasWerlionnen5.^P2Meaisksed t7*C5 ft 5*6 |5. 4*5 "j*6 3.5 0 4.5 50 13C-PFUnA 565.0/270.0 Da 5*4 BnasWerlinnn4en.52PMeaisksed 4*4 !* 3.4 s 3*4 f$ 2 I4.0 4.5 SD T*n*. m>r 13C-PFDOA 55 615.0/169.0 Da _____BnasWerlinnnenPMeaisks_e_d___ 5*4 4.4 1 2** 30 15 40 Time, pm PFDS 1 46 599.0/80.0 Da Baseline Missed 8*6 n Wrnnn5^P7eak 3*5 8*5 5*5 4*5 HS 2*6 1*5 45 60 55 *8 I 60 PFTrA 1 663.0/619.0 Da Baseline Missed n Wrnnn Peak_____ I15 20 26 10 13C-PFOS 503.0/80.0 Da BnasWerlinnnenPMeaisksed 6*4 4*4 2*4 1*4 40 45 50 5? 13C-PFDOA 615.0/169.0 Da BnasWerlinnnen Missed Peak_____ 1*5 60 55 0 40 46 50 55 PFTeATM1 713.0/669.0 Da BnasWerlionnen Missed Peak_____ 13C-PFDOA 615.0/169.0 Da Bi a! sWerlionnen Missed Peak_____ Before After Page 40 of 170 289 Created with A nalystFR ^irter Printed: 18/02/2010 3:24:00 PM Ion Ratio Confirmation 1tier ecws : 1*5 A ................... f e " .......................... PFC 50ppb O ti 2 1 0 11| \(Mi ............... ................... :M`,0 * c. .......... : ......... f- 1 I PFOA2 413.0/369.0 Da d Baseline Missed Wrong Peak PFNA2 463.0/219.0 Da Baseline c Missed Wrong Peak PFOS2 499.0/99.0 Da Baseline c Missed o Wrong Peak PFDA2 513.0/269.0 Da Baseline c Missed Wrong Peak PFUnA2 563.0/269.0 Da Baseline Missed Wrong Peak Tiiri* nwi PFDS2 599.0/99.0 Da Baseline Missed Wrong Peak PFDoA2 613.0/169.0 Da o Baseline a Missed c Wrong Peak PFTrA 2 663.0/169.0 Da Baseline Missed Wrong Peak PFTeA2 713.0/169.0 Da Baseline Missed Wrong Peak Before A fter Page 41 of 170 290 Created with Anal^fkReporter Printed: 18/02/2010 3:24:00 PM Project Data File Acquisition Method Ewan's Projects\PFCs 021710\CalLong.wiff PFCkinetexLong.dam Result Table Algorithm Used Instrument Name 021710long.rdb IntelliQuan API 5000 Sample Name A cquisition Date Acquisition Method Sample ID Sample Comment PFC 20ppb ICV 2/17/2010 8:01:01 PM PFCkinetexLong.dam LCMS2-77J Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 9 5 Quality Control 1.00 0.00 Results Summary Analyte Name Analyte RT (Expected) PFOA 1 1.24 (1.36) PFNA 1 2.04 (2.06) PFOS 1 2.06 (2.09) PFDA 1 3.06(3.06) PFUnA 1 3.91 (4.06) PFDS 1 3.89 (3.87) PFDoA 1 4.53 (4.55) PFTrA 1 5.07 (5.06) PFTeA 1 5.52(5.51) IS Name 13C-PFOA 13C-PFNA 13C-PFOS 13C-PFDA 13C-PFUnA 13C-PFOS 13C-PFDOA 13C-PFDOA 13C-PFDOA IS Area 3324800 2583600 7449100 2664400 194040 7449100 299150 299150 299150 Analyte Area 3415400 5823700 16562000 5489500 4610900 16977000 3300600 2191400 1582400 Exp Cone (ng/mL) 20.000 20.000 20.000 20.000 20.000 20.000 20.000 20.000 20.000 Calc. Cone (ng/mL) 20.300 Accuracy (%) 101 20.800 104 20.800 104 20.000 100 22.700 114 20.800 104 18.300 91 21.600 108 20.800 104 1 Mod? No No No No No No No No No (<J Z ,tf* Page 46 of 170 291 IRC Summary Analyte Peak Name PFOA2 S_13C_PFOA PFNA2 S_13C_PFNA PFOS2 S_13C-PFOS PFDA2 SJ3C-PFDA PFUnA2 S_13C-PFUnA PFDS 2 PFDoA2 S_13C-PFDoA PFTrA 2 PFTeA2 Created with AnalystpRZflorter Printed: 18/02/2010 3:24:00 PM RT (Exp RT ) 1.23(1.36) 1.23(1.36) 2.01 (2.08) 0.00 (2.44) 2.05(2.12) 2.06 (2.00) 3.06(3.06) 3.10(3.04) 3.89(3.88) 3.90(3.88) 3.89(3.87) 4.53(4.53) 4.53 (4.64) 5.07 (5.13) 5.53 (5.56) Area 7771100 3324800 1833900 0 5388300 7449100 861070 2664400 1010200 194040 5658600 946530 299150 602970 585430 M o d ifie d ? No No No No No No No No No No No No No No No Ratio C onfirm s ID YES No YES No YES No YES No YES No YES YES No YES No Page 47 of 170 292 Quantitative Peak Review L1.23 PFOA 1 413.0/169.0 Da Baseline c Missed r Wrnnn Peak 13C-PFOA 417.0/372.0 Da Baseline c Missed ___p Wrnnn Peak *o*s | i(>S PFOS 1 499.0/80.0 Da Baseline Missed n W rnnn Peak 13C-PFOS 503.0/80.0 Da BnasWerlinnnenPMpaisksed created witn Anai^ft&porter Printed: 18/02/2010 3:24:00 PM PFC 20ppb ICV 12.01 PFNA 1 463.0/419.0 Da Baseline Missed n Wrnnn Pnak 113C-PFNA 468.0/423.0 Da Baseline Missed __ n Wrnnn Peak 3.10 PFDA 1 513.0/469.0 Da Baseline Missed n Wrnnn Ppak 13C-PFDA 515.0/470.0 Da BnasWerlinnnencPMeaisksed PFUnA 1 563.0/519.0 Da Baseline c Missed p Wrnnn Peak 13C-PFUnA 565.0/270.0 Da BnasWerlinnnenPMeaisksed PFDS 1 599.0/80.0 Da Baseline Missed Wrnnn Peak 13C-PFOS 503.0/80.0 Da Baseline Missed Wrnnn Peak PFDoA 1 613.0/569.0 Da BnasWerlinnnen Missed Paak 13C-PFD0A 615.0/169.0 Da Baseline Missed W rnnn Peak PFTrA 1 663.0/619.0 Da o Baseline Missed ____p W rnnn Peak___ 13C-PFD0A 615.0/169.0 Da Baseline Missed ______p W rnnn P e a k ___ PFTeA 1 713.0/669.0 Da Baseline Missed ___ p W rnnn Peak___ <0 so 13C-PFDOA 615.0/169.0 Da Baseline Missed ___ n W rnnn Peak___ Before After Page 48 of 170 293 iumbia Ion Ratio Confirmation Created with AnalystR?^orter Printed: 18/02/2010 3:24:00 PM PFC 20ppb ICV PFOA2 413.0/369.0 Da c Baseline Missed Wrong Peak PFUnA2 563.0/269.0 Da Baseline g Missed a Wrong Peak PFNA2 463.0/219.0 Da Baseline Missed Wrong Peak PFDS2 599.0/99.0 Da Baseline d Missed Wrong Peak PFOS2 499.0/99.0 Da Baseline c Missed Wrong Peak PFDA2 513.0/269.0 Da Baseline Missed d Wrong Peak 5s M ........... I 4.f H..... . L . -: _ PFDoA2 613.0/169.0 Da Baseline Missed o Wrong Peak ! | M= J 7 ............... ... D*v ..... | 55 PFTrA 2 663.0/169.0 Da Baseline g Missed d Wrong Peak PFTeA2 713.0/169.0 Da Baseline Missed Wrong Peak Before A fter Page 49 of 170 294 M Columbia Anaiyliol Services* Analyte Name: Internal Standard: PFBA 1 13C-PFBA p. 74 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Data File A cquisition Date Acquisition Method Project 021710\CalShort.wiff 2/18/2010 12:04:57 AM PFCkinetexShort.dam Ewan's Projects\PFCs Result Table Algorithm Used : Instrument Name 021710short.rdb IntelliQuan API 5000 Regression Equation: Exp Cone (ng/mL) 0.1 0.5 1 5 10 20 50 y = 0.105 x + 0.0066 (r = 0.9990) # of Values Mean Calc Cone (ng/mL) 1 0.09 1 0.48 1 1.06 1 5.23 1 10.96 1 18.90 1 49.87 % Accuracy 88 97 106 105 110 94 100 STD NaN NaN NaN NaN NaN NaN NaN %CV NaN NaN NaN NaN NaN NaN NaN 1? I* 59 22 23 2* Zi 26 V Zi 2S A/ioMe Cone /IS Co 34 K % 36 39 40 49 4? Page 1 of 169 295 Created with AnalystftJpbrter Printed: 18/02/2010 4:02:00 PM Analyte Name: Internal Standard: Data File A cqu isition Date Acquisition Method Project PFPeA 1 13C-PFHxA 021710\CalShort.wiff 2/18/2010 12:04:57 AM PFCkinetexShort.dam Ewan's ProjectsVPFCs Result Table Algorithm Used Instrument Name 021710short.rdb IntetliQuan API 5000 Exp Cone (ng/mL) 0.1 0.5 1 5 10 20 50 # o f Values 1 1 1 1 1 1 1 Mean Calc Cone (ng/mL) 0.08 0.51 1.08 5.39 11.23 18.75 49.57 % Accuracy 77 103 108 108 112 94 99 / STD NaN NaN NaN NaN NaN NaN NaN %CV NaN NaN NaN NaN NaN NaN NaN > l > 9 3 10 31 3 ]J 3 55 V 36 3 40 4 42 41 47 46 tJ Page 2 of 169 296 p. 76 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Analyte Name: Internal Standard: PFBS 1 180-PFHS Data File Acquisition Date Acquisition Method Project 021710\CalShort.wiff 2/18/2010 12:04:57 AM PFCkinetexShort.dam Ewan's Projects\PFCs Result Table Algorithm Used Instrument Name 021710short.rdb IntelliQuan API 5000 Regression Equation: Exp Cone (ng/mL) 0.1 0.5 1 5 10 20 50 y = -0,00191 xA2 + 0.36 x + -0.00745 (r = 0.9975) # of Values Mean Calc Cone (ng/mL) % Accuracy 1 0.09 92 1 0.49 98 1 1.04 104 1 5.07 101 1 11.28 113 1 17.94 90 1 50.92 102 STD NaN NaN NaN NaN NaN NaN NaN %CV NaN NaN NaN NaN NaN NaN NaN os 00 15 75 I I4? t-5 i f i ; h u i; i8 t i a :i a es a ?? 28 es jo 3i r 33 Anly<CCone /ISConc 35 36 i; le i : s *' Page 3 of 169 297 Created with AnalystRR^orter Printed: 18/02/2010 4:02:00 PM Analyte Name: Internal Standard: PFHxA 1 13C-PFHxA Data File Acquisition Date Acquisition Method Project 021710\CalShort.wiff 2/18/2010 12:04:57 AM PFCkinetexShort.dam Ewan's ProjectsVPFCs Result Table Algorithm Used Instrument Name 021710short.rdb IntelliQuan API 5000 Regression Equation: Exp Cone (ng/mL) 0.1 0.5 1 5 10 20 50 y = -0.000207 xA2 + 0.102 x + 0.00567 (r= 0.9993) # of Values Mean Calc Cone (ng/mL) % Accuracy 1 0.09 94 1 0.49 98 1 1.04 104 1 5.14 103 1 10.65 107 1 18.83 94 1 50.37 101 STD NaN NaN NaN NaN NaN NaN NaN %CV NaN NaN NaN NaN NaN NaN NaN i < ? t ? e s '6 n i; U M rs is i? m >t : s ; i .v :* Cone /IS Cone :e .'s jo ji a 3* js a c ) < * -7 CO Page 4 of 169 298 Services* p. 7o Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Analyte Name: Internal Standard: PFHpA 1 13C-PFHxA Data File Acquisition Date Acquisition Method Project 021710\CalShort.wiff 2/18/2010 12:04:57 AM PFCkinetexShort.dam Ewan's Projects\PFCs Result Table Algorithm Used Instrument Name 021710short.rdb IntelliQuan API 5000 Regression Equation: Exp Cone (ng/mL) 0.1 0.5 1 5 10 20 50 ,,i J y = -3.03e-005 xA2 + 0.0359 x + 0.00196 (r= 0.9988) # of Values Mean Calc Cone (ng/mL) % Accuracy 1 0.09 91 1 0.49 97 1 1.07 107 1 5.09 102 1 10.89 109 1 18.57 93 1 50.40 101 STD NaN NaN NaN NaN NaN NaN NaN %CV NaN NaN NaN NaN NaN NaN NaN )5 20 Ji 2' 23 24 2 26 27 2 2S M 31 32 33 J* K Jt V Si 40 J1 yn* Conc/ISConc r-fc\ Page 5 of 169 i(D 299 Services- p. 79 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Analyte Name: Internal Standard: PFHxS 1 180-PFHS Data File Acquisition Date Acquisition Method Project 021710\CalShort.wiff 2/18/2010 12:04:57 AM PFCkinetexShort.dam Ewan's Projects\PFCs Result Table Algorithm Used Instrument Name 021710short.rdb IntelliQuan API 5000 Regression Equation: Exp Cone (ng/ml_) 0.1 0.5 1 5 10 20 50 y = -0.00178 xA2 + 0.334 x + 0.00367 (r= 0.9981) # of Values Mean Calc Cone (ng/mL) % Accuracy 1 0.09 93 1 0.49 98 1 1.04 104 1 5.11 102 1 11.08 111 1 18.15 91 1 50.83 102 STD NaN NaN NaN NaN NaN NaN NaN %CV NaN NaN NaN NaN NaN NaN NaN 3 4 5 i ? 8 4 10 H I? 1 H IS I 1 1* l- 0 ; i Vi 2 Ji : 9 31 32 3J M JS S ? * Cone / IS Cone 41 4? 45 <5 v li6 Page 6 of 169 300 lylicgl Services" p. 80 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Project Data File Result Table Instrument Name Ewan's Projects\PFCs 021710\CalShort.wiff 021710short.rdb API 5000 Sample Name Acquisition Date Acquisition Method Injection Vial IB 2/18/2010 12:04:57 AM PFCkinetexShort.dam 1 Injection Volume Sample Type Dilution Factor Weight to Volume 5 Unknown 1.00 0.00 Results Summary Analyte Peak Name IS Name PFBA1 13C-PFBA PFPeA 1 130-PFHxA PFBS 1 180-PFHS PFHxA 1 130-PFHxA PFHpA 1 13C-PFHxA PFHxS 1 180-PFHS SJ80-PFHS 13C-PFDA SJ3C-PFDA 13C-PFDA IS Area 0 0 0 0 0 0 0 0 Analyte RT (Exp RT ) 1.22 (1.27) 3.48 (3.60) 0.00 (4.26) 5.32 (5.31) 6.17 (6.23) 6.26 (6.32) 0.00 (6.31) 0.00 (7.65) Analyte Area 2558 4863 0 37209 11679 3607 0 0 Calc. Cone (ng/mL) N/A N/A N/A N/A N/A N/A N/A N/A Modified? No No No No No No No No 4 J) Page 9 of 169 301 fumbia Created with A nalyst^Jorter Printed: 18/02/2010 4:02:00 PM IRC Summary Analyte Peak Name PFBA2 PFPeA2 PFBS2 PFHxA 2 PFHpA 2 PFHxS2 S_13C-PFBA S_13C-PFHxA RT (Exp RT ) 1.22(1.27) 3.48 (3.60) 0.00 (4.26) 0.00 (5.31) 6.18 (6.22) 0.00 (6.32) 0.00 (1.26) 0.00 (5.30) Area 2558 4863 0 0 38199 0 0 0 Modified? No Calc (Exp) MRM Ratio 1.00(1.00) Ratio C onfirm s ID YES No 1.00(1.00) YES No 0.00(0.40) No No 0.00 (0.10) No No 3.27 (2.90) YES No 0.00(0.40) No No 0.00 (13.20) No No 0.00(13.71) No Page 10 o f 169 302 p. 82 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Of Quantitative Peak Review | S 1 - A - V . vVv,g, v V \ is n :to :tw 150 1W 50 0 Ml!!Mi\ifmjy* fI:f:ItVil ii'Iiif'j1lITfiftMhwi jlt PFBA 1 213.0/169.0 Da d Baseline a Missed n Wrnnn Poak 13C-PFBA 217.0/172.0 Da o Baseline a Missed ___n Wrnnn Peak IB PFPeA 1 263.0/219.0 Da Baseline o Missed n Wrnnn Peak 13C-PFHXA 315.0/270.0 Da Baseline q Missed n Wrnnn Peak pfbsT 299.0/80.0 Da Baseline o Missed n Wrnnn Ppak PFHpA 1 363.0/169.0 Da o Baseline d Missed n Wrnnn Peak M h d l0 i 180-PFHS 403.0/103.0 Da Baseline Missed n Wrnnn Ppak Ii 13C-PFHxA 315.0/270.0 Da Baseline Missed ___n Wrnnn Peak wSi PFHxA 1 313.0/269.0 Da Baseline Missed n Wrnnn Ppak jL,6.26 Vv^vv^'^wA'V11 Time mm PFHxS 1 399.0/80.0 Da d BnasWerlinnnenPMeaisksed 13C-PFHxA 315.0/270.0 Da Baseline Missed n Wrnnn Ppak Tim, mm 180-PFHS 403.0/103.0 Da o Baseline Missed n Wronn Peak S_180-PFHS 403.0/103.0 Da o Baseline Missed n W rnnn Ppak___ ?5 30 13C-PFDA 515.0/470.0 Da Baseline o Missed n Wrnnn Ppak SJ3C-PFDA 515.0/470.0 Da Baseline Missed ______n W rn nn Ppak Before After 13C-PFDA 515.0/470.0 Da Baseline Missed n Wrnnn Ppak Page 11 of 169 303 iumbla p. 83 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Ion Ratio Confirmation wmfl sew 4 1.22 3.48 , , PFBA2 213.0/169.0 Da Baseline Missed o Wrong Peak PFPeA2 263.0/219.0 Da Baseline Missed Wrong Peak IB PFBS2 299.0/99.0 Da Baseline Missed Wrong Peak PFHxA 2 313.0/119.0 Da Baseline Missed Wrong Peak 6 .1 8 PFHpA2 363.0/319.0 Da Baseline Missed Wrong Peak Tin* * PFHxS2 399.0/99.0 Da d Baseline Missed Wrong Peak S_13C-PFDA 515.0/470.0 Da o Baseline Missed Wrong Peak NB. PFBA and PFPeA do not have qualifying ion transitions. Before A fter N/A Baseline o Missed Wrong Peak Page 12 of 169 304 lymba Created with A n a ly s P l^ o rte r Printed: 18/02/2010 4:02:00 PM Project Data File Acquisition Method Ewan's ProjectsVPFCs 021710\CalShort.wiff PFCkinetexShort.dam Result Table Algorithm Used Instrument Name 021710short.rdb IntelliQuan API 5000 Sample Name Acquisition Date Acquisition Method Sample ID Sample Comment PFC 0.10ppb 2/18/2010 12:33:38 AM PFCkinetexShort.dam LCMS2-85A Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 2 5 Standard 1.00 0.00 Results Summary Analyte Name Analyte RT (Expected) PFBA 1 1.24(1.27) PFPeA 1 3.52 (3.60) PFBS 1 4.20 (4.26) PFHxA 1 5.25 (5.31) PFHpA 1 6.15(6.23) PFHxS 1 S 180PFHS S 13CPFDA 6.25 (6.32) 6.25 (6.31) 7.55 (7.65) IS Name 13C-PFBA 13C-PFHXA 180-PFHS 13C-PFHxA 13C-PFHxA 180-PFHS 13C-PFDA 13C-PFDA IS Area 4436400 5263100 2854500 5263100 5263100 2854500 3476200 3476200 Analyte Area 70291 43417 73640 80401 27535 98784 2854500 3476200 Exp Cone (ng/mL) 0.10 0.10 0.10 0.10 0.10 0.10 1.00 1.00 Calc. Cone (ng/mL) 0.09 Accuracy <%) 88 0.08 77 0.09 92 0.09 94 0.09 91 0.09 93 1.02 102 1.00 100 Mod? No No No No No No No No Page 13 o f 169 305 IRC Summary Analyte Peak Name PFBA2 PFPeA2 PFBS 2 PFHxA2 PFHpA2 PFHxS2 S_13C-PFBA S_13C-PFHxA p. 85 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM RT (Expected) 1.24(1.27) 3.52(3.60) 4.19(4.26) 5.26 (5.31) 6.15(6.22) 6.24(6.32) 1.23(1.26) 5.24 (5.30) Area 70291 43417 27839 9322 84235 38137 4436400 5263100 Modified? No No No No No No No No Calculated Ion Ratio (Expected Value) 1.00 1.00 0.38 0.12 3.06 0.39 63.11 65.46 Page 14 of 169 306 Createci with AnalysPF&^orter Printed: 18/02/2010 4:02:00 PM Quantitative Peak Review PFC O.IOppb lCOOO irjfjwi ma 3 KW I^ - ' w * i--' J R M K r V ' 705 H PFBA ti JO 213.0/169.0 Da Baseline Missed n \A/rnnn Peak >5 1 .2 3 5*5 5*5 v 4*5 51 3*5 M 1H5 05 10 15 Tm* imn 13C-PFBA 20 217.0/172.0 Da C Baseline c Missed n Wronn Peak teM 0 iftMuJ 3 W80 4 ^0 5*5 & j5 l 3*5 S 2*5 >5 6 .^ 5 )5 40 45 50 55 BO B5 70 PFBS 7 299.0/80.0 Da Baseline Missed n Wrnnn Peak 6'.006 .^ JOWl " lOUU 4 | Cui WjWl 180-PFHS 403.0/103.0 Da Baseline Missed n Wrnnn Peak 12.5 10.6 a(w5 K*5 3i 40*5 :o5 5^ 45 50 55 CO PFHpAI 363.0/169.0 Da Baseline Missed n Wrnnn Peak 13C-PFHXA 315.0/270.0 Da Baseline c Missed n Wrnnn Peak K.S 5ir5 & i 4" r' S 3*5 3 C.S Hi 55 7 50 55 S 180-PFHS :(> 8.5 Hi ,, 5*5 - 56 ^ 2 3.5 2.5 H5 7 .^ 5 70 75 80 Tjnn "IT 13C-PFDA 35 403.0/103.0 Da 515.0/470.0 Da G Baseline Missed n Wrnnn Peak_____ BnasWerlinnnen Missed Peak 3 ,5 2 B00D 1CM 5000 21 4000 2009 111 15 Tnu> mi PFPeA 1 6 S0.5 &05 3i 40.6 20.6 45 I 45 50 55 13C-PFHXA 0 263.0/219.0 Da 315.0/270.0 Da Baseline c Missed n Wrnnn Peak 12000 5 . 2 5 10000 9 woo ! 6000 S 0 200(1 1............................ 45 50 5S 60 C Baseline Missed n Wrnnn Peak 1}*6 11M 0 8W &&eS i * 40*5 20.5 I 5 50 55 60 PFHxAl 313.0/269.0 Da Baseline Missed n Wrnnn Peak 25000 20000 & 15000 | 1000Q SOTiO 55 I 60 65 78 PFHx'sl 399.0/80.0 Da Baseline Missed n Wrnnn Peak 8*5 7*5- | 8 4.5 I 3H 2.5 le5- I 70 75 8.0 8 5 & ^ S 3 v l i 3 13C-PFHXA 315.0/270.0 Da C Baseline c Missed n Wrnnn Peak 6 .2 5 t*6 5e5 4tS 1.5 2*5 IH5 55 68 65 Tr* mm 180-PFHS 70 403.0/103.0 Da a Baseline Missed n Wrnnn Peak 8*5 7 .^ 7.5 8.5 " 1.5 2.5 1*5 70 75 80 05 S 13C-PFDA 515.0/470.0 Da BnasWerlinnnen Missed Peak 13C-PFDA 515.0/470.0 Da BnasWerlinnnen Missed Peak_____ Before A fter Page 15 of 169 307 S e rv ic e s ' Ion Ratio Confirmation p. 87 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM PFC 0.10ppb PFBA2 213.0/169.0 Da Baseline Missed Wrong Peak 6.15 PFPeA2 263.0/219.0 Da o Baseline Missed Wrong Peak ": 4-- PFBS2 299.0/99.0 Da Baseline Missed Wrong Peak PFHxA 2 313.0/119.0 Da a Baseline Missed d Wrong Peak Thisinage is not amiable PFHpA2 363.0/319.0 Da Baseline Missed Wrong Peak PFHxS2 399.0/99.0 Da Baseline c Missed d Wrong Peak S_13C-PFDA 515.0/470.0 Da o Baseline Missed Wrong Peak NB. PFBA and PFPeA do not have qualifying ion transitions. Before A fter N/A Baseline Missed Wrong Peak Page 16 of 169 308 Created with AnalysPT^porter Printed: 18/02/2010 4:02:00 PM Project Data File Acquisition Method Ewan's Projects\PFCs 021710\CalShort.wiff PFCkinetexShort.dam Result Table Algorithm Used Instrument Name 021710short.rdb IntelliQuan API 5000 Sample Name A cquisition Date Acquisition Method Sample ID Sample Comment PFC 0.5ppb 2/18/2010 12:43:13 AM PFCkinetexShort.dam LCMS2-85B Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 3 5 Standard 1.00 0.00 Results Summary Analyte Name Analyte RT (Expected) PFBA1 1.24 (1.27) PFPeA 1 3.53 (3.60) PFBS 1 4.19(4.26) PFHxA 1 5.24 (5.31) PFHpA 1 6.15(6.23) PFHxS 1 S 180PFHS S 13CPFDA 6.23 (6.32) 6.23 (6.31) 7.53(7.65) IS Name 13C-PFBA 13C-PFHxA 180-PFHS 13C-PFHxA 13C-PFHxA 180-PFHS 13C-PFDA 13C-PFDA IS Area 4415300 5327700 2817900 5327700 5327700 2817900 3642700 3642700 Analyte Area 253180 265090 474530 296040 103320 471260 2817900 3642700 Exp Cone (ng/mL) 0.50 0.50 0.50 0.50 0.50 0.50 1.00 1.00 Calc. Cone (ng/mL) 0.49 Accuracy (%) 97 0.51 103 0.49 98 0.49 98 0.49 97 0.49 98 0.96 96 1.00 100 Mod? No No No No No No No No tA Page 17 o f 169 309 IRC Summary Analyte Peak Name PFBA2 PFPeA2 PFBS 2 PFHxA2 PFHpA2 PFHxS2 S_13C-PFBA S_13C-PFHxA Created with Analyii'F^eporter Printed: 18/02/2010 4:02:00 PM RT (Expected) 1.24(1.27) 3.53 (3.60) 4.19(4.26) 5.24(5.31) 6.15(6.22) 6.24(6.32) 1.23(1.26) 5.24 (5.30) Area 253180 265090 184090 26023 302150 177290 4415300 5327700 Modified? No No No No No No No No Calculated Ion Ratio (Expected Value) 1.00 1.00 0.39 0.09 2.92 0.38 17.44 18.00 Page 18 of 169 310 Quantitative Peak Review Created with Ana lyit'ffeporter Printed: 18/02/2010 4:02:00 PM PFC 0.5ppb PFBA1 213.0/169.0 Da Baseline Missed Wrnnn Peak PFBS 1 299.0/80.0 Da Baseline Missed i Wrnnn Paak 13C-PFBA 217.0/172.0 Da BnasWerlinnnenPMeaisksed PFPeA 1 263.0/219.0 Da BnasWerlinnnenPMeaisksed 6*4 5.24 5e4 & 4*4 3*4 3 1 1 13C-PFHXA 315.0/270.0 Da BnasWerlinnnenPMeaisksed 13*6 5 | 9b* i 60*S 5 40*5 J0*5 180-PFHS 403.0/103.0 Da d BnasWerlinnnenPMfifilsksed PFHxA 1 313.0/269.0 Da BnasWerlinnnenPMaaisksed 13C-PFHxA 315.0/270.0 Da BnasWerlinnnen cPMe aisksed PFHpA 1 363.0/169.0 Da a Baseline c Missed n Wrnnn Peak___ 13C-PFHxA 315.0/270.0 Da BnasWerlinnnenPMeaisksed PFHxS 1 399.0/80.0 Da BnasWerlinnnenPMeaisksed 180-PFHS 403.0/103.0 Da BnasWerlinnnenPMeaisksed SJ80-PFHS 403.0/103.0 Da Baseline o Missed n W rnnn Peak___ 13C-PFDA 515.0/470.0 Da BnasWerlinnnen Missed Peak S_13C-PFDA 515.0/470.0 Da BnasWerlinnnenPMeaisks_e_d_ Before After 13C-PFDA 515.0/470.0 Da BnasWerlinnnen Missed P eak___ Page 19 of 169 311 Ion Ratio Confirmation 1.24 p. 91 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM PFC 0.5ppb PFBA2 213.0/169.0 Da a Baseline Missed Wrong Peak .15 PFPeA2 263.0/219.0 Da Baseline a Missed Wrong Peak PFBS2 299.0/99.0 Da Baseline c Missed Wrong Peak f | 4th ?0.4 oo PFHpA 2 363.0/319.0 Da Baseline Missed Wrong Peak PFHxS2 399.0/99.0 Da Baseline g Missed Wrong Peak S_13C-PFDA 515.0/470.0 Da Baseline c Missed Wrong Peak NB. PFBA and PFPeA do not have qualifying ion transitions. Before A fter PFHxA 2 313.0/119.0 Da Baseline Missed Wrong Peak Ihisgeisriolav N/A Baseline Missed Wrong Peak Page 20 of 169 312 .................................................. / ? C o ly m b ia A nalytical Services- p. 92 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Project Data File Acquisition Method Ewan's Projects\PFCs 021710\CalShort.wiff PFCkinetexShort.dam Result Table Algorithm Used Instrum ent Name 021710short.rdb IntelliQuan API 5000 Sample Name A cquisition Date Acquisition Method Sample ID Sample Comment PFC 1.0ppb 2/18/2010 12:52:48 AM PFCkinetexShort.dam LCMS2-85C Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 4 5 Standard 1.00 0.00 Results Summary Analyte Name Analyte RT (Expected) PFBA 1 1.24 (1.27) IS Name 13C-PFBA IS Area 4470800 PFPeA 1 3.53 (3.60) 13C-PFHxA 5343600 PFBS 1 4.19(4.26) 180-PFHS 2828500 PFHxA 1 5.23(5.31) 13C-PFHxA 5343600 PFHpA 1 6.13(6.23) 13C-PFHxA 5343600 PFHxS 1 S 180PFHS S 13CPFDA 6.23(6.32) 6.23 (6.31) 7.54 (7.65) 180-PFHS 13C-PFDA 13C-PFDA 2828500 3377400 3377400 Analyte Area 527130 551510 1035500 597140 215490 984600 2828500 3377400 Exp Cone (ng/mL) 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.00 Calc. Cone (ng/mL) 1.06 Accuracy (%) 106 1.08 108 1.04 104 1.04 104 1.07 1.04 107 104 1.04 104 1.00 100 Mod? No No No No No No No No 4 { H0 Page 21 of 169 313 IRC Summary Analyte Peak Name PFBA2 PFPeA2 PFBS 2 PFHxA2 PFHpA2 PFHxS2 S_13C-PFBA S_13C-PFHxA p. 93 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM RT (Expected) 1.24(1.27) 3.53 (3.60) 4.19(4.26) 5.24(5.31) 6.15 (6.22) 6.23 (6.32) 1.23(1.26) 5.23 (5.30) Area 527130 551510 381740 55969 627980 370800 4470800 5343600 Modified? No No No No No No No No Calculated Ion Ratio (Expected Value) 1.00 1.00 0.37 0.09 2.91 0.38 8.48 8.95 Page 22 of 169 314 1Quantitative Peak Review PFBA 1 213.0/169.0 Da BnasWerlinnnenPMeaisksed 4.19 13C-PFBA 217.0/172.0 Da BnasWerlionnenPMeaisksed p. 94 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM PFC 1.0ppb PFPeA 1 263.0/219.0 Da BnasWerlinnnenPMeaisksed 13C-PFHxA 315.0/270.0 Da o BnasWerlionnenPMeaisksed PFBS 1 299.0/80.0 Da BnasWerlinnnenPMeaisksed 180-PFHS 403.0/103.0 Da d BnasWerlinnnenPMeaisksed PFHxA 1 313.0/269.0 Da BnasWerlinnnenPMeaisksed 13C-PFHXA 315.0/270.0 Da Baseline a Missed i Wrnnn Peak ti n PFHpA 1 363.0/169.0 Da BnasWerlinnnenPMeaisksed 13C-PFHXA 315.0/270.0 Da Baseline Missed Wrnnn Peak PFHxS1 399.0/80.0 Da o Bra, sWerlinnnenPMeaisksed 180-PFHS 403.0/103.0 Da Baseline a Missed Wrnnn Peak S_180-PFHS 403.0/103.0 Da BnasWerlinnnenPMnaisksed 13C-PFDA 515.0/470.0 Da BnasWerlinnnenPMeaisksed S_13C-PFDA 515.0/470.0 Da BnasWerlinnnenpPMeaisksed Before A fter 13C-PFDA 515.0/470.0 Da BnasWerlinnnenaPMeaisks_e_d_ Page 23 of 169 315 Services- 31Ion Ratio Confirmation '3.53- Created with Analyst Reporter Printed: 18/02/2010 4:62TTO PM PFC 1.0ppb PFBA2 213.0/169.0 Da c Baseline Missed Wrong Peak [\ U>e5 6 15................ PFPeA2 263.0/219.0 Da Baseline Missed Wrong Peak PFBS2 299.0/99.0 Da Baseline Missed Wrong Peak PFHxA 2 313.0/119.0 Da c Baseline Missed c Wrong Peak Ifemqeisfiolai'aiable Si si- ti ;o PFHpA 2 363.0/319.0 Da Baseline Missed Wrong Peak PFHxS2 399.0/99.0 Da Baseline Missed Wrong Peak S_13C-PFDA 515.0/470.0 Da d Baseline Missed Wrong Peak N/A Baseline Missed Wrong Peak NB. PFBA and PFPeA do not have qualifying ion transitions. Before A fter Page 24 o f 169 316 Created with Analyst Reporter Printed: 18/02/2010 A:D2'00 PM Project Data File Acquisition Method Sample Name A cquisition Date Acquisition Method Sample ID Sample Comment Ewan's Projects\PFCs 02171OVCalShort.wiff PFCkinetexShort.dam PFC 5.0ppb 2/18/2010 1:02:19 AM PFCkinetexShort.dam LCMS2-85D Result Table Algorithm Used Instrum ent Name Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 021710short.rdb InteiliQuan API 5000 5 5 Standard 1.00 0.00 Results Summary Analyte Name Analyte RT (Expected) PFBA1 1.24 (1.27) PFPeA 1 3.53 (3.60) PFBS 1 4.19(4.26) PFHxA 1 5.23(5.31) PFHpA 1 6.12(6.23) PFHxS 1 S 180PFHS S 13CPFDA 6.22 (6.32) 6.22 (6.31) 7.52 (7.65) IS Name 13C-PFBA 13C-PFHxA 180-PFHS 13C-PFHxA 13C-PFHxA 180-PFHS 13C-PFDA 13C-PFDA IS Area 4390500 5343100 2823000 5343100 5343100 2823000 3454400 3454400 Analyte Area 2433300 2737200 4985800 2809900 982050 4690700 2823000 3454400 Exp Cone (ng/mL) 5.00 5.00 5.00 5.00 5.00 5.00 1.00 1.00 Calc. Cone (ng/mL) 5.23 Accuracy (%) 105 5.39 5.07 5.14 5.09 5.11 108 101 103 102 102 1.01 101 1.00 100 Mod? No No No No No No No No Page 25 o f 169 317 Services* IRC Summary Analyte Peak Name PFBA2 PFPeA2 PFBS 2 PFHxA2 PFHpA2 PFHxS2 S 13C-PFBA S_13C-PFHxA RT (Expected) 1.24(1.27) 3.53 (3.60) 4.19(4.26) 5.22 (5.31) 6.13(6.22) 6.22(6.32) 1.24(1.26) 5.22 (5.30) p. 97 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Area 2433300 2737200 1932300 258300 2917500 1776200 4390500 5343100 M od ifie d ? No No No No No No No No Calculated Ion Ratio (Expected Value) 1.00 1.00 0.39 0.09 2.97 0.38 1.80 1.90 Page 26 o f 169 318 /" Columbia c L i Analytics! Services" Q u a n tita tiv e P e a k R e v ie w Created with AnalyJ?'F$fx>rter Printed: 18/02/2010 4:02:00 PM P F C 5.0p p b PFBA 1 213.0/169.0 Da c BnasWerlionne4n.1P9Meaisksed 7PFBS 299.0/80.0 Da ___BnaWserlninnen d Missed Peak 6.12 13C-PFBA 217.0/172.0 Da f -2eI,?-*w55s"-t--BnasWerlionne6g.11I2II2PMeaisks_e_d_ 15 7 180-PFHS 403.0/103.0 Da BnasWerlninnen Missed Peak PFPeA 1 263.0/219.0 Da =i| 144663******555555 BnasWerlinnne5n.82f1cP3Meaisksed I 1 PFHxA 1 313.0/269.0 Da BnasWerlinnnenPMeaisksed 13C-PFHxA 315.0/270.0 Da Baseline Missed g. 811200**65? n W rnnn Peak | 20#S 13C-PFHXA 315.0/270.0 Da o Baseline Missed Wrnnn Peak PFHpA 1 363.0/169.0 Da a Baseline Missed Wrnnn Peak S_180-PFHS 403.0/103.0 Da BnasWerlinnnenPMeaisksed 13C-PFHxA PFHxS 1 315.0/270.0 Da 399.0/80.0 Da Baseline Missed 10e6 n Wrnn7.n52Peak 80*5 t 60(5 f 2 De6 | ft I BnasWerlinnnenPMeaisks_e_d_ 10*5 60*5 8 60(5 ' 0*5 ?H 75 80 85 13C-PFDA 515.0/470.0 Da BnasWerlinnnenPMeaisks_e_d_ SJ3C-PFDA 515.0/470.0 Da BnasWerlinnnenPMeaisks_e_d_ Before A fter 180-PFHS 403.0/103.0 Da BnasWerlinnnenPMeaisksed 13C-PFDA 515.0/470.0 Da BnasWerlinnnenPMeaisksed Page 27 of 169 319 Mmbk Created with A n a lytf ^Iporter Printed: 18/02/2010 4:02:00 PM Ion Ratio Confirmation 1.24 ......... us ........ 3.53.......... i iSet is 3 J5 05 10 IS .' 0 30 )5 <0 T^r>fc non <S PFBA2 PFPeA 2 213.0/169.0 Da Baseline c Missed o Wrong Peak 263.0/219.0 Da Baseline Missed d Wrong Peak ' 6 . 1 3 ........................................... us h U5 5 -5 i: uit>*s ! 2 - ~ .............. 6 . __ I'iS zz, &?0s5 800 = PFC 5.0ppb 1o*t |& 10*5 <o*5tOeS -...... -....4. L .... . :os , 35 C *5 50 PFBS2 299.0/99.0 Da c Baseline Missed Wrong Peak 10** 5*5 1 ** TM 5 2e <5 Tnt> nin PFHxA 2 313.0/119.0 Da Baseline c Misse Wrong Peak & iM i s ir'5 PFHpA2 363.0/319.0 Da d Baseline Missed Wrong Peak PFHxS2 399.0/99.0 Da Baseline c Missed d Wrong Peak S_13C-PFDA 515.0/470.0 Da Baseline Missed o Wrong Peak NB. PFBA and PFPeA do not have qualifying ion transitions. N/A Baseline Missed Wrong Peak Before A fter Page 28 of 169 320 Created with A n a ly s P f^ftrte r Printed: 18/02/2010 4:02:00 PM t* Project Data File Acquisition Method Ewan's Projects\PFCs 021710\CalShort.wiff PFCkinetexShort.dam Result Table Algorithm Used Instrument Name 021710short.rdb IntelliQuan API 5000 Sample Name A cquisition Date A cquisition Method Sample ID Sample Comment PFC 10ppb 2/18/2010 1:11:52 AM PFCkinetexShort.dam LCMS2-85E Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 6 5 Standard 1.00 0.00 Results Summary Analyte Name Analyte RT (Expected) PFBA1 1.24 (1.27) IS Name 13C-PFBA PFPeA 1 3.53(3.60) 130-PFHxA PFBS 1 4.19(4.26) 180-PFHS PFHxA 1 5.23 (5.31) 13C-PFHxA PFHpA 1 6.14(6.23) 13C-PFHxA PFHxS 1 S 180PFHS S 13CPFDA 6.24 (6.32) 6.23 (6.31) 7.54 (7.65) 180-PFHS 13C-PFDA 13C-PFDA IS Area 4346800 5390500 2737500 5390500 5390500 2737500 3673100 3673100 Analyte Area 5019200 5746500 10422000 5773500 2097900 9531500 2737500 3673100 Exp Cone (ng/mL) 10.00 10.00 10.00 10.00 10.00 10.00 1.00 1.00 Calc. Cone (ng/mL) 11.00 Accuracy (%) 110 11.20 112 11.30 113 10.70 10.90 11.10 107 109 111 0.92 92 1.00 100 Mod? No No No No No No No No i (<5 Page 29 of 169 321 IRC Summary Analyte Peak Name PFBA2 PFPeA2 PFBS 2 PFHxA2 PFHpA2 PFHxS2 S_13C-PFBA S_13C-PFHxA p. 101 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM RT (Expected) 1.24(1.27) 3.53 (3.60) 4.19(4.26) 5.23 (5.31) 6.15(6.22) 6.23 (6.32) 1.24(1.26) 5.23 (5.30) Area 5019200 5746500 4023400 531220 6195500 3769100 4346800 5390500 Modified? No No No No No No No No Calculated Ion Ratio (Expected Value) 1.00 1.00 0.39 0.09 2.95 0.40 0.87 0.93 Page 30 of 169 322 ServkaHr Quantitative Peak Review Created with AnalysPRl^&rter Printed: 18/02/2010 4:02:00 PM PFC 10ppb PFBA 1 213.0/169.0 Da Baseline Missed p Wrnnn Peak 13C-PFBA 217.0/172.0 Da Baseline c Missed n Wrnnn Peak PFPeA 1 263.0/219.0 Da Baseline a Missed Wrnnn Peak 13C-PFHxA 315.0/270.0 Da Baseline c Missed r Wrnnn Peak PFBS 1 299.0/80.0 Da Baseline Missed n Wrnnn Peak PFHpA 1 363.0/169.0 Da BasVeYlimnenoPMfliaskse. d 180-PFHS 403.0/103.0 Da a Baseline Missed n Wrnnn Pnak `,5 60 PFHxA 1 313.0/269.0 Da Baseline c Missed n Wrnnn Peak 65 60 13C-PFHxA 315.0/270.0 Da Baseline c Missed ______n W rnnn Peak___ & 1W * 51*5 00*0 60 65 ?o PFHxil 399.0/80.0 Da Baseline c Missed n W rnnn Peak___ 13C-PFHxA 315.0/270.0 Da d Baseline c Missed n Wrnnn Pnak 6.0 6 5 180-PFHS 403.0/103.0 Da Baseline Missed ___ n W rnnn P eak___ S_180-PFHS 403.0/103.0 Da Baseline Missed n W rn nn Paak___ 13C-PFDA 515.0/470.0 Da Baseline Missed n W rnnn Peak___ SJ3C-PFDA 515.0/470.0 Da Baseline a Missed n Wrnnn Peak Before A fter 13C-PFDA 515.0/470.0 Da Baseline Missed n W rnnn P eak___ Page 31 of 169 323 Created with AnalydM0|3orter Printed: 18/02/2010 4:02:00 PM Ion Ratio Confirmation n z1.24" 3.53 ?o*t | PFC 10ppb PFBA2 213.0/169.0 Da Baseline Missed Wrong Peak PFPeA2 263.0/219.0 Da Baseline Missed Wrong Peak PFBS2 299.0/99.0 Da Baseline c Missed Wrong Peak .......... 5.15 ---------- 1...... - - ..... I t.( H 70 PFHpA 2 363.0/319.0 Da Baseline Missed Wrong Peak 12 0 * '5*4 | I0*( ....- - ..6.83-.... ..... . 5 0*5 55 a 45 70 PFHxS 2 399.0/99.0 Da o Baseline Missed Wrong Peak 1 4*5 S|' <*s 2e5 Of S_13C-PFDA 515.0/470.0 Da Baseline Misse Wrong Peak NB. PFBA and PFPeA do not have qualifying ion transitions. Before A fter PFHxA 2 313.0/119.0 Da Baseline Missed Wrong Peak N/A Baseline Missed Wrong Peak Page 32 of 169 324 Created with AnalysPRlij&rter Printed: 18/02/2010 4:02:00 PM Project Data File Acquisition Method Ewan's Projects\PFCs 021710\CalShort.wiff PFCkinetexShort.dam Result Table Algorithm Used Instrument Name 021710short.rdb IntelliQuan API 5000 Sample Name A cqu isition Date Acquisition Method Sample ID Sample Comment PFC 20ppb 2/18/2010 1:21:24 AM PFCkinetexShort.dam LCMS2-85F Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 7 5 Standard 1.00 0.00 Results Summary Analyte Name Analyte RT (Expected) PFBA 1 1.23 (1.27) PFPeA 1 3.53 (3.60) PFBS 1 4.19(4.26) PFHxA 1 5.24 (5.31) PFHpA 1 6.15(6.23) PFHxS 1 S 180PFHS S 13CPFDA 6.24 (6.32) 6.25 (6.31) 7.55 (7.65) IS Name 13C-PFBA 13C-PFHxA 180-PFHS 13C-PFHxA 13C-PFHXA 180-PFHS 13C-PFDA 13C-PFDA IS Area 4379000 5482400 2894400 5482400 5482400 2894400 3846100 3846100 Analyte Area 8692500 9756700 16878000 10177000 3605200 15842000 2894400 3846100 Exp Cone (ng/mL) 20.00 20.00 20.00 20.00 20.00 20.00 1.00 1.00 Calc. Cone (ng/mL) 18.90 Accuracy (%) 95 18.70 94 17.90 90 18.80 94 18.60 18.20 93 91 0.93 93 1.00 100 Mod? No No No No No No No No 1^ i ^ 10 Page 33 of 169 325 ................................................. OAsnlallllytutfiocaisl Services'' IRC Summary Analyte Peak Name PFBA2 PFPeA2 PFBS 2 PFHxA2 PFHpA2 PFHxS2 S_13C-PFBA S_13C-PFHxA RT (Expected) 1.23(1.27) 3.53 (3.60) 4.19 (4.26) 5.24(5.31) 6.15(6.22) 6.24(6.32) 1.23 (1.26) 5.24(5.30) p. 105 Created with Analyst Reporter Printed; 18/02/2010 4;02:00 PM Area 8692500 9756700 6910000 927140 10382000 6436200 4379000 5482400 Modified? No No No No No No No No Calculated Ion Ratio (Expected Value) 1.00 1.00 0.41 0.09 2.88 0.41 0.50 0.54 Page 34 of 169 326 C o ltllT iS 'is Analytical S erv icer Quantitative Peak Review >0*6 & t(ttl t *0*6 * *rj*i 1.23 ii i6 l is :o PFBA 7 213.0/169.0 Da BnasWerlinnnenPMeaisksed j*6 l? to Ii 1*6 )* 40 65 so PFBS 7 299.0/80.0 Da Baseline Missed n Wrnnn Peak 0*5 6.15 l 4*4 'A a fcu 55 7(l 6*5 5.5 1 *5 |' ?3e*5t 1*6 05 1.23 li l 15 20 13C-PFBA 217.0/172.0 Da c BnasWerlinnnenPMeaisksed 6^5 i S J^ei s 2*5 1*6 I56 60 Time,mm66 70 180-PFHS 403.0/103.0 Da O BnasWerlinnnenPMeaisksed I26 1.0*6 3 #1*6 J &0*5 3 .0*5 :-o*5 45 50 55 60 Created with AnalysPR1ejx>rter Printed: 18/02/20104:02:00PM 115*6 3i%1 ' 50*5 PFC 20ppb 3.53 12*6 5.^4 10*6 | 80*5 | . 3 40*5 2MS I I30 T1i6m*mifi 40 PFPeA 1 263.0/219.0 Da D BnasWerlinnnenPMeaisksed | 15*0 34i '0*0 S0e5 46 46 50 55 60 13C-PFHxA 315.0/270.0 Da c Baseline Missed n Wrnnn Peak 12.6 >0*6 & 00.5 SI 4"0"*55 20*5 45 60 Tim*mm65 60 PFHxA 1 313.0/269.0 Da BnasWerlinnnenPMeaisksed 6.^4 3*6 42- 2*6 1*6 55 60 65 70 45 60 Tot*mm55 60 13C-PFHXA 315.0/270.0 Da Baseline c Missed n Wrnnn Peak 7*5 6*5 -& 5*5 3iS 43e*5S 2*6 1*6 6.^5 55 60 65 70 PFHpAI 363.0/169.0 Da Baseline Missed r Wrnnn Peak M7y5 > 5*5 1 :*s 1*4 5S hOi 5 70 13C-PFHXA P F H xil 180-PFHS 315.0/270.0 Da 399.0/80.0 Da 403.0/103.0 Da Baseline Missed n Wrnnn Peak BnasWerlinnnendPMeaisksed BnasWerlinnnenPMeaisksed 10*6 7.55 10*6 7.55 10*6 7.^5 3.0*5 | CM S 80*5 60*5 80*5 | S0.5 | 40*5 } 40*6 | 40*5 20*5 I'0*5 26*5 70 75l SO 85 70 76l 8.0 85 70 75 80 85 S 180-PFHS 403.0/103.0 Da BnasWerlinnnenPMeaisks_e_d___ 13C-PFDA 515.0/470.0 Da D BnasWerlinnnenoPMeaisksed S 13C-PFDA 515.0/470.0 Da D BnasWerlinnnencPMeaisks_e_d___ 13C-PFDA 515.0/470.0 Da BnasWerlinnnenaPMeaisks_e_d___ Before A fter Page 35 of 169 327 p. 107 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Ion Ratio Confirmation PFC 20ppb 3.53 30*6 :s*t ? CW4 PFBA2 213.0/169.0 Da Baseline Missed c Wrong Peak 50*# 1 - ;&#6 6..15.. 5 ' '"5>h 1 PFPeA2 263.0/219.0 Da Baseline Missed c Wrong Peak sews 0*0 PFBS2 299.0/99.0 Da Baseline g Missed g Wrong Peak eo*s - 40S ____ 5. 1 ........... ............- f r - .. PFHxA 2 313.0/119.0 Da Baseline o Missed Wrong Peak This riaqe is not amiable t>D i > 70 PFHpA2 363.0/319.0 Da d Baseline Missed Wrong Peak PFHxS2 399.0/99.0 Da Baseline c Missed Wrong Peak SJ3C-PFDA 515.0/470.0 Da Baseline Missed Wrong Peak NB. PFBA and PFPeA do not have qualifying ion transitions. Before A fter N/A Baseline Missed c Wrong Peak Page 36 of 169 328 Analytical Services" p. 108 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM Project Data File Acquisition Method Ewan's Projects\PFCs 021710\CalShort.wiff PFCkinetexShort.dam Result Table Algorithm Used Instrum ent Name 021710short.rdb IntelliQuan API 5000 Sample Name A cquisition Date Acquisition Method Sample ID Sample Comment PFC 50ppb 2/18/2010 1:31:00 AM PFCkinetexShort.dam LCMS2-85G Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 8 5 Standard 1.00 0.00 Results Summary Analyte Name Analyte RT (Expected) PFBA1 1.23 (1.27) IS Name 13C-PFBA PFPeA 1 3.53 (3.60) 13C-PFHxA PFBS 1 4.20 (4.26) 180-PFHS PFHxA 1 5.25 (5.31) 13C-PFHxA PFHpA 1 6.17(6.23) 13C-PFHxA PFHxS 1 S 180PFHS S 13CPFDA 6.25 (6.32) 6.25 (6.31) 7.57 (7.65) 180-PFHS 13C-PFDA 13C-PFDA IS Area 4432300 5177700 2784400 5177700 5177700 2784400 3076700 3076700 Analyte Area 23176000 24352000 37182000 23962000 8973300 34427000 2784400 3076700 Exp Cone (ng/mL) 50.00 50.00 50.00 50.00 50.00 50.00 1.00 1.00 Calc. Cone (ng/mL) 49.90 Accuracy (%) 100 49.60 99 50.90 102 50.40 101 50.40 50.80 101 102 1.12 112 1.00 100 Mod? No No No No No No No No tA1,t< -6 I 1 Page 37 of 169 329 IRC Summary Analyte Peak Name PFBA2 PFPeA2 PFBS 2 PFHxA2 PFHpA2 PFHxS2 S_13C-PFBA S_13C-PFHxA p. 109 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM RT (Expected) 1.23(1.27) 3.53(3.60) 4.19(4.26) 5.25 (5.31) 6.15(6.22) 6.25 (6.32) 1.23 (1.26) 5.25 (5.30) Area 23176000 24352000 17542000 2624000 23596000 16420000 4432300 5177700 Modified? No No No No No No No No Calculated Ion Ratio (Expected Value) 1.00 1.00 0.47 0.11 2.63 0.48 0.19 0.22 Page 38 of 169 330 ' 9t Quantitative Peak Review 1.23 7*6 b*5 1^ 9 1*6 06 1 1 10 i i 7O PFBA 7 2 1 3 .0 /1 6 9 .0 Da B a s e lin e M is se d _______ n W r o n n P e a k _______ Mi 0*6 i tSf 1 5 3*5 .'*6 1*6 05 10 Tm*.mn 15 20 13C -P F B A 2 1 7 .0 /1 7 2 .0 D a nc B a s e lin e M is s e d W rnnn Peak 6*5 6 .^5 6*6 4*6 1*6 w IS 40i 40 SO PFBS T 2 9 9 .0 /8 0 .0 Da B a s e lin e M isse d h Wrnnn Peak 20*6 ^ l6*6 i 0Ci6 OS SOI 65 n1 55 64 65 70 T*b* mm 1 8 0 -P F H S 4 0 3 .0 /1 0 3 .0 D a B a s e lin e M isse d n W rnnn Peak 10*6 * 8.0*5 i- 0*6 1l 4ll*S o5 45 5.25 l 50 55 60 PFC 4*6 3*6 aI 2.6 1 1*6 3.53 10 A 35 40 45 ' PFPeAl 2 6 3 .0 /2 1 9 .0 Da B a s e lin e M isse d n Wrnnn Peak 5*f 4*4 3 3*6 * I i'th 1*6 45 50i T<n*moi65 60 PFHxA 1 3 1 3 .0 /2 6 9 .0 D a B a s e lin e M issed n W rnnn Paak 7*6 * Sf ` 1t M. 1*6 55 I 60 65 1 70 P FH pA l 3 6 3 .0 /1 6 9 .0 D a n B a s e lin e M is s e d W rnnn Peak i6 6.25 5*6 & <ei ** 1w 1*0 65 1 ih 65 70 13C -P F H xA P FH xsl 3 1 5 .0 /2 7 0 .0 D a no B a s e lin e o M is s e d W rnnn Peak M 7*5 6*5 9 5*6 i 4*5 1 1.5 7.^7 1*5 3 9 9 .0 /8 0 .0 Da d B a s e lin e M issed n W rnnn Peak 8.6 7*56*5 9 6*6 7 .^7 $ 4*5 | 3.5 2*5 1*5- 70 75 B0 as 70 75 6.0 B.5 S 18 0 -P F H S 4 0 3 .0 /1 0 3 .0 Da n B a s e lin e M is s e d W r n n n P e a k _______ 13C -P FD A 5 1 5 .0 /4 7 0 .0 D a n B a s e lin e M is s e d Wrnnn Peak S 13C -P FD A 5 1 5 .0 /4 7 0 .0 Da n B a s e lin e M is s e d W r n n n P e a k _______ Before A fter 1 with Analys?1^eporter 18/02/2010 4:02:00 PM 5.25 56 l 65 60 1-P FH xA 1/270.0 D a in e d M is s e d -nnn P e a k 5.25 1 60 55 60 A P FH xA 1/270.0 D a in e M is s e d nnn P e a k 6.25 1 10 65 70 3 -P F H S 1/103.0 D a in e M is s e d nnn Peak I 75 BO T un* mm 3 -P F D A 1/470.0 D a in e o M is s e d -nnn P e a k 05 ige 39 of 169 331 Ion Ratio Confirmation p. 111 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM PFC 50ppb PFBA2 213.0/169.0 Da Baseline Missed Wrong Peak 30 35 PFPeA2 263.0/219.0 Da Baseline Missed c Wrong Peak PFBS2 299.0/99.0 Da c Baseline c Missed Wrong Peak PFHxA 2 313.0/119.0 Da Baseline Missed Wrong Peak PFHpA2 363.0/319.0 Da a Baseline o Missed d Wrong Peak PFHxS2 399.0/99.0 Da c Baseline Missed o Wrong Peak S_13C-PFDA 515.0/470.0 Da Baseline Missed o Wrong Peak NB. PFBA and PFPeA do not have qualifying ion transitions. Before After N/A Baseline Missed o Wrong Peak Page 40 of 169 332 Created with A n a ly s tR ^ ^ rte r Printed: 18/02/2010 4:02:00 PM Project Data File Acquisition Method Ewan's ProjectsVPFCs 021710\CalShort.wiff PFCkinetexShort.dam Result Table Algorithm Used Instrum ent Name 021710short.rdb IntelliQuan API 5000 Sample Name A cqu isition Date Acquisition Method Sample ID Sample Comment PFC 20ppb ICV 2/18/2010 1:59:41 AM PFCkinetexShort.dam LCMS2-77J Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 9 5 Quality Control 1.00 0.00 Results Summary Analyte Name Analyte RT (Expected) PFBA1 1.23(1.27) PFPeA 1 3.53 (3.60) PFBS 1 4.20 (4.26) PFHxA 1 5.25 (5.31) PFHpA 1 6.16(6.23) PFHxS 1 S 180PFHS S 13CPFDA 6.26 (6.32) 6.26 (6.31) 7.58(7.65) IS Name 13C-PFBA 13C-PFHxA 180-PFHS 13C-PFHxA 13C-PFHXA 180-PFHS 13C-PFDA 13C-PFDA IS Area 4331600 5138300 2789400 5138300 5138300 2789400 3241000 3241000 Analyte Area 9351500 10309000 18218000 10783000 3866800 17097000 2789400 3241000 Exp Cone (ng/mL) 20.00 20.00 20.00 20.00 20.00 20.00 1.00 1.00 Calc. Cone (ng/mL) 20.60 Accuracy (%) 103 21.10 106 20.40 102 21.40 107 21.30 20.60 107 103 1.07 107 1.00 100 Mod? No No No No No No No No Jr -TJ Page 45 of 169 333 ervices" D. 113 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM IRC Summary Analyte Peak Name PFBA2 PFPeA2 PFBS2 PFHxA 2 PFHpA2 PFHxS2 S_13C-PFBA S_13C-PFHxA RT (Exp RT ) 1.23(1.27) 3.53(3.60) 4.20 (4.26) 5.25 (5.31) 6.16(6.22) 6.26 (6.32) 1.23(1.26) 5.25(5.30) Area 9351500 10309000 7496200 985770 11034000 6956800 4331600 5138300 M o d ifie d ? No No No No No No No No Ratio C onfirm s ID YES YES YES YES YES YES No No Page 46 of 169 334 Quantitative Peak Review 1o* f. 3 56*5 7,5 65 6*5 3I 3*5 05 Mli 15 :o 05 I :oE l5*6 |1 IU* I 60*5 li) 15 ?0 3^ 30 1-5 p. 114 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM PFC 20ppb ICV 1(i*C- i.&* 00*5 S0*5 I 40*S :<i5 5.^5 40 45 45 SC 55 o0 PFBA ? 13C-PFBA PFPeA~1 13C-PFHxA 213.0/169.0 Da 217.0/172.0 Da 263.0/219.0 Da 315.0/270.0 Da Baseline Missed c Baseline Missed O Baseline c Missed c Baseline a Missed n Wrnnn Peak n Wrnnn Peak n Wrnnn Peak n Wrnnn Peak 3e6 I :K' 4.20 l| *3*5S .7*5 6.^6 75*5 20*6 8 l5*6 | 50*6 5.25 10*6 *8i 00*5 0.6*5 1 40.5 :o*5 5.25 35 40i 45 50 PFBS 1 299.0/80.0 Da Baseline Missed n Wrnnn Peak flS 6.16 5 *5 C*5 55 60 66 7J 180-PFHS 403.0/103.0 Da Baseline c Missed n Wrnnn Peak 10*6 * 50*5 0*5 S 40*5 30*6 5.25 I45 :3 55 60 PFHx a I 313.0/269.0 Da P Baseline Missed 4*6 n Wrnnn Peak 3*6 9 2.6 45 50 S5 6(1 13C-PFHxA 315.0/270.0 Da d Baseline Missed ______n Wrnnn Peak_____ 6*5 6.26 3**6i 54**55 3*5 2*5 55 bCi I 6`, ?a 45 50 I 55 SO Si 0 65 70 55 60 l 65 70 PFHpAI 363.0/169.0 Da d Baseline Missed _____ n Wrnnn Peak_____ C*5 3a,,sg' 5*4 4*5 3*5 3*5 I I I\*i 55 50 Time,nun65 ft 3ll 70 I 13C-PFHXA 315.0/270.0 Da D Baseline Missed 467***566 n Wrnnn Peak 7.58 beS 4TM321**.*5565 70 75i Oil 3Jsi 85 PFHxS 1 399.0/80.0 Da Baseline c Missed 987***551 n Wrnnn Peak 236i41,*9***sS5555 70 75 SO | 1| 0.5 180-PFHS 403.0/103.0 Da Baseline Missed n Wrnnn Peak W7*5. 595 374**.555 7(3 75 BO 15 S 180-PFHS 13C-PFDA S 13C-PFDA 13C-PFDA 403.0/103.0 Da 515.0/470.0 Da 515.0/470.0 Da 515.0/470.0 Da Baseline Missed Baseline d Missed Baseline c Missed Baseline Missed _____ n Wrnnn Peak_____ n Wrnnn Peak_____ n Wrnnn Peak_____ n Wrnnn Peak Before After Page 47 of 169 335 Iiimfoia Sendees' Ion Ratio Confirmation 1.23 '3.53 p. 115 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM PFC 20ppb ICV PFBA2 213.0/169.0 Da Baseline c Missed q Wrong Peak PFPeA2 263.0/219.0 Da o Baseline o Missed o Wrong Peak PFBS2 299.0/99.0 Da Baseline Missed d Wrong Peak PFHxA 2 313.0/119.0 Da Baseline c Missed Wrong Peak 6.: 6 PFHpA2 363.0/319.0 Da Baseline Missed c Wrong Peak PFHxS2 399.0/99.0 Da g Baseline Missed Wrong Peak S_13C-PFDA 515.0/470.0 Da Baseline Missed c Wrong Peak NB. PFBA and PFPeA do not have qualifying ion transitions. Before A fter 1 N/A d Baseline Missed Wrong Peak Page 48 of 169 336 Created with Analy^.Ff@orter Printed: 18/02/2010 3:24:00 PM Project Data File Acquisition Method Ewan's Projects\PFCs 021710\CalLong.wiff PFCkinetexLong.dam Result Table Algorithm Used Instrum ent Name 021710long.rdb IntelliQuan API 5000 Sample Name A cqu isition Date Acquisition Method Sample ID Sample Comment PFC 20ppb CCV 2/17/2010 7:53:28 PM PFCkinetexLong.dam LCMS2-85F Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 7 5 Quality Control 1.00 0.00 Results Summary Analyte Name Analyte RT (Expected) PFOA 1 1.22(1.36) IS Name 13C-PFOA PFNA 1 2.01 (2.06) 13C-PFNA PFOS 1 2.04 (2.09) 13C-PFOS PFDA1 3.06 (3.06) 13C-PFDA PFUnA 1 3.88 (4.06) 13C-PFUnA PFDS 1 3.89 (3.87) 13C-PFOS PFDoA 1 4.53 (4.55) 13C-PFDOA PFTrA 1 5.07 (5.06) 13C-PFDOA PFTeA 1 5.54 (5.51) 13C-PFDOA IS Area 3408100 2728400 7860000 2907400 196180 7860000 245450 245450 245450 Analyte Area 3176200 5790100 15685000 5567500 4174000 16066000 2985300 1967200 1444400 Exp Cone (ng/mL) 20.000 20.000 20.000 20.000 20.000 20.000 20.000 20.000 20.000 Calc. Cone (ng/mL) 18.400 Accuracy (%) 92 19.500 98 18.700 93 18.600 93 20.300 102 18.500 93 20.100 101 23.600 118 23.100 115 t Mod? No No No No No No No No No Page 42 of 170 337 IRC Summary Analyte Peak Name PFOA2 S_13C_PFOA PFNA 2 S_13C_PFNA PFOS2 S_13C-PFOS PFDA2 S_13C-PFDA PFUnA2 S_13C-PFUnA PFDS2 PFDoA2 S_130-PFDoA PFTrA 2 PFTeA2 created witn AnaiyBt kro n e r Printed: 18/02/2010 3:24:00 PM RT (Exp R T ) 1.21 (1.36) 1.23(1.36) 2.02 (2.08) 0.00 (2.44) 2.05 (2.12) 2.05 (2.00) 3.07(3.06) 3.08 (3.04) 3.88(3.88) 3.88(3.88) 3.89(3.87) 4.53 (4.53) 4.54 (4.64) 5.07(5.13) 5.54 (5.56) Area 7525700 3408100 1780500 0 4989400 7860000 795190 2907400 815730 196180 5355000 852990 245450 577910 445770 M od ifie d ? No No No No No No No No No No No No No No No Ratio C onfirm s ID YES No YES No YES No YES No YES No YES YES No YES YES Page 43 of 170 338 ly m b ia ureaiea wun Anaiysk^pf^ruii Printed: 18/02/2010 3:24:00 PM Quantitative Peak Review i L1.23 1PFOA 1 413.0/169.0 Da BnasWerlinnnencPMpaisksed PFOS 1 499.0/80.0 Da Baseline Missed n Wrnnn Peak ,,i 13C-PFOA 417.0/372.0 Da Baseline c Missed ____n Wrnnn Peak___ 2.05 U 2C JC 13C-PFOS 503.0/80.0 Da Baseline Missed ___r...Wrong.Beak 1 10000 6060 PFC 20ppb CCV lJl_ i! 2.01 PFNA 1 463.0/419.0 Da BnasWerlinnnencPMeaisksed 13C-PFNA 468.0/423.0 Da Baseline Missed ____n W rnnn Peak___ PFDA 1 513.0/469.0 Da Baseline Missed p Wrnnn Peak LjL_13C-PFDA 515.0/470.0 Da c BnasWerlinnnenoPMnaisksed PFUnA 1 563.0/519.0 Da d Baseline c Missed n Wrnnn Peak 13C-PFUnA 565.0/270.0 Da Baseline c Missed n Wronn Peak PFDS 1 599.0/80.0 Da Baseline Missed Wrnnn Peak 13C-PFOS 503.0/80.0 Da Baseline Missed n Wrnnn Peak PFDoAl 613.0/569.0 Da BnasWerlinnnenPMeaisksed 13C-PFDOA 615.0/169.0 Da BnasWerlinnnen Missed PFTrA 1 663.0/619.0 Da BnasWerlinnnenPMeaisks_e_d_ 13C-PFDoA 615.0/169.0 Da Baseline Missed n Wrnnn Pnak PFTeXl 713.0/669.0 Da Baseline Missed ___ n W rnnn Pnak___ 13C-PFDOA 615.0/169.0 Da BnasWerlinnnenPMnaisksed Before After 339 Page 44 of 170 Ion Ratio Confirmation created witn AnaiyBt p o r t e r Printed: 18/02/2010 3:24:00 PM PFC 20ppb CCV PFOA2 413.0/369.0 Da Baseline c Missed Wrong Peak PFNA2 463.0/219.0 Da c Baseline o Missed a Wrong Peak PFOS2 499.0/99.0 Da Baseline a Missed Wrong Peak 3.1 PFUnA 2 563.0/269.0 Da Baseline Missed c Wrong Peak i..................3 =r 9.................... 0*5 00t> ____________ , ___________ PFDS2 599.0/99.0 Da Baseline Missed Wrong Peak PFDoA2 613.0/169.0 Da Baseline d Missed Wrong Peak PFDA2 513.0/269.0 Da c Baseline c Missed Wrong Peak .I 1 PFTrA 2 663.0/169.0 Da Baseline Missed c Wrong Peak 1 SCI*IJk ___ 5. 4.............. .................... PFTeA2 713.0/169.0 Da Baseline g Missed Wrong Peak Before A fter Page 45 of 170 340 Created with AnalysPR^ftirter Printed: 18/02/2010 4:02:00 PM Project Data File Acquisition Method Ewan's Projects\PFCs 021710\CalShort.wiff PFCkinetexShort.dam Result Table Algorithm Used Instrum ent Name 021710short.rdb IntelliQuan API 5000 Sample Name A cquisition Date Acquisition Method Sample ID Sample Comment PFC 20ppb CCV 2/18/2010 1:50:06 AM PFCkinetexShort.dam LCMS2-85F Injection Vial Injection Volume Sample Type Dilution Factor Weight to Volume 7 5 Quality Control 1.00 0.00 Results Summary I Analyte Name Analyte RT (Expected) PFBA1 1.23(1.27) PFPeA 1 3.54(3.60) PFBS 1 4.20 (4.26) PFHxA 1 5.25 (5.31) PFHpA 1 6.16(6.23) PFHxS 1 S 180PFHS S 13CPFDA 6.26 (6.32) 6.26 (6.31) 7.58 (7.65) IS Name 13C-PFBA 13C-PFHxA 180-PFHS 13C-PFHxA 13C-PFHxA 180-PFHS 13C-PFDA 13C-PFDA IS Area 4484300 5242000 2855500 5242000 5242000 2855500 3456700 3456700 Analyte Area 8750100 9788300 17232000 10101000 3667700 16046000 2855500 3456700 Exp Cone (ng/mL) 20.00 20.00 20.00 20.00 20.00 20.00 1.00 1.00 Calc. Cone (ng/mL) 18.60 Accuracy (%) 93 19.70 98 18.60 93 19.60 98 19.80 18.70 99 94 1.02 102 1.00 100 Mod? No No No No No No No No Page 41 of 169 341 lymbla IRC Summary Analyte Peak Name PFBA2 PFPeA2 PFBS2 PFHxA 2 PFHpA2 PFHxS2 S_13C-PFBA S_13C-PFHXA p. 121 Created with Analyst Reporter Printed: 18/02/2010 4:02:00 PM RT (Exp RT) 1.23(1.27) 3.54(3.60) 4.20 (4.26) 5.25(5.31) 6.16(6.22) 6.26 (6.32) 1.23(1.26) 5.25(5.30) Area 8750100 9788300 6939500 934080 10506000 6486200 4484300 5242000 M od ifie d ? No No No No No No No No Ratio C onfirm s ID YES YES YES YES YES YES No No Page 42 o f 169 342 Created with Analy$'f3l|3brter Printed: 18/02/2010 4:02:00 PM Quantitative Peak Review PFC 20ppb CCV 1 0*8 * 0*1 1,23 4 0*6 2u*4 06*0 as t '.o 15 to PFBA ? 213.0/169.0 Da D Baseline d Missed n Wrnnn Peak J*i 2*4 iti 4b uC s1 > 5 1^ 05 :o 15 to 13C-PFBA 217.0/172.0 Da C Baseline Missed n Wrnnn Peak l 1 M"i 2*1 1*5 3^4 1 5*4 I 2 * 6 5,25 1 0*6 8 v 1 0 e 6 3 S05 g 80*5 | 6W 3 4 0S 2 (1 * 6 l 10 35 40 45 45 50 55 60 PFPe/Ti 263.0/219.0 Da Baseline c Missed n Wrnnn Peak 5.^5 2 0*6 S '5 e 6 1 10*6 3 113C-PFHXA 315.0/270.0 Da C Baseline Missed n Wrnnn Peak 1 2 * 6 5.25 1 0*0 g 8 0*5 I 3 4 0*5 50*5 ;s* 5 s i 4U * 1 SO PFBS ? 299.0/80.0 Da D Baseline c Missed n Wrnnn Peak 6.16 7*1 S 15 Mi ,i 4 > .* 5 I51 6,0 65 T n t. m m 180-PFHS 70 403.0/103.0 Da Baseline Missed n Wrnnn Peak 1 .2 * 6 1 0*6 z 96S 3 0*5 2 0*5 45 50 55 60 p f h x a "i 313.0/269.0 Da Baseline Missed n Wrnnn Peak 6.26 3*6 4.3! Mi I45 10 55 60 130-PFHxA 315.0/270.0 Da BnasWerlinnnenPMeaisksed 7*5 tel ,, 5*5 l% 444 3*5 2*5 <*5 56 tO 55 PFHpAI 70 4 5 5 0 `. 5 13C-PFHXA 60 55 60 65 T im e m in PFHxS 1 70 5 5 6 .0 65 180-PFHS 70 363.0/169.0 Da Baseline Missed 315.0/270.0 Da d Baseline Missed 399.0/80.0 Da Baseline Missed 403.0/103.0 Da Baseline Missed nn Wrnnn Peak 7*5 6*1 * 6*5 i **1 I| J5 ________ n Wrnnn Peak_____ ________ n Wrnnn Peak_____ Mi 7.^8 4*5 3*56*5 ?*4 7 * 5 . % i S *M*5i | 4 . 5*5 J S 3*5 3 4*5 6*5 7*5 3*5 Wrnnn Peak I 2*1 2*5 2*5 2*6 i* 5 5$ i 40 55 ?0 :u 75 00 65 70 75 60 85 U5 7(1 7 5 8 U 8 5 T im e m * S 180-PFHS 13C-PFDA S 13C-PFDA 13C-PFDA 403.0/103.0 Da 515.0/470.0 Da 515.0/470.0 Da 515.0/470.0 Da u Baseline Missed n Wrnnn Peak_____ BnasWerlinnnenPMeaisks_e_d___ Baseline Missed n Wrnnn Peak_____ BnasWerlinnnenPMeaisksed Before A fter Page 43 of 169 343 Created with AnalyJt'Reporter Printed: 18/02/2010 4:02:00 PM Ion Ratio Confirmation 1.23 PFBA2 213.0/169.0 Da o Baseline Missed Wrong Peak -6.16.. PFPeA2 263.0/219.0 Da Baseline c Missed Wrong Peak PFC 20ppb CCV PFBS2 299.0/99.0 Da Baseline c Missed Wrong Peak iO*f sc*o .......... 5. k .......... PFHxA 2 313.0/119.0 Da Baseline Missed Wrong Peak PFHpA2 363.0/319.0 Da o Baseline Missed c Wrong Peak PFHxS2 399.0/99.0 Da Baseline Missed Wrong Peak S_13C-PFDA 515.0/470.0 Da Baseline c Missed Wrong Peak NB. PFBA and PFPeA do not have qualifying ion transitions. Before A fter N/A Baseline Missed Wrong Peak Page 44 of 169 344 p. 124 Acquisition Date Vial Position Sample Name 1 2/17/2010 18:30 2 2/17/2010 18:52 43 2/17/2010 19:00 2/17/2010 19:08 21 PIBFC 0 10ppb 3 PFC 0.5ppb 4 PFC 1.Oppb 5 2/17/2010 19:15 6 78 22//1177//22001100 1199::2330 2/17/2010 19:38 65 PPFFCC 510.Oppppbb 7 PFC 20ppb 8 PFC 50ppb 9 2/17/2010 19:53 7 PFC 20ppb CCV 10 2/17/2010 20:01 9 PFC 20ppbICV 11 2/17/2010 20:08 25 K1001011-001 12 2/17/2010 20:16 13 2/17/2010 20:23 26 K1001011-002 27 K1001011-003 14 2/17/2010 20:31 28 K1001011-004 15 2/17/2010 20:38 29 K1001011-005 16 2/17/2010 20:46 30 K1001011-006 17 2/17/2010 20:54 31 K1001011-007 18 2/17/2010 21:01 32 K1001011-008 19 20 2212 2/17/2010 21:09 2/17/2010 21:16 2/17/2010 21:24 2/17/2010 21:31 23 2245 22//1177//22001100 2211::3496 2/17/2010 21:54 33 K1001011-009 34 K1001011-010 35 K1001011-011 3367 KK11000011001111--001132 38 K1001011-014 39 K1001011 -015 26 2/17/2010 22:02 27 2289 22//1177//22001100 2222::1079 2/17/2010 22 24 4410 KK11000011001111--001176 42 K1001011-018 43 K1001011-019 30 2/17/2010 22:32 31 2/17/2010 22:39 32 2/17/2010 22:47 33 2/17/2010 22:54 34 2/17/2010 23:02 35 36 22//1177//22001100 2233::1170 37 38 39 22//1177//22001100 2233::2352 2/17/2010 23:40 40 2/17/2010 23:47 4454 KKQ1010010001616-40-2001 46 KQ1000664-02 47 KQ1000664-03 48 KQ1000664-04 49 KQ1000664-05 50 KQ1000664-06 2234 KKQQ11000000662200--0012 2212 KKQQ11000000662200--0056 APFcqCukiisnietiotenxLMoenthgo.ddam PFCkinetexLong.dam PPFFCCkkiinneetteexxLLoonngg..ddaamm PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam PFC kinetexLong. dam PPFFCCkkiinneetteexxLLoonngg..ddaamm PFCkinetexLong.dam PFCkinetexLong.dam PFC kinetexLong .dam PPFFCCkkiinneetteexxLLoonngg..ddaamm PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam PPFFCCkkiinneetteexxLLoonngg..ddaamm PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam PPFFCCkkiinneetteexxLLoonngg..ddaamm PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam PFCkinetexLong.dam 0F2ile17N1aOmVeCalLong.wiff 021710\CalLong.wiff 00221177110O\VCCaalLlLoonngg..wwiiffff 021710\CalLong.wiff 021710\CalLong.wiff 002211771100\\CCaaliLLoonngg..wwiiffff 0022117711O0\VCCaalLlLoonngg.wwiiffff 002211771100\\SSaammpplieessLLoonngg,.wwiiffff 021710\SamplesLong.wiff 02171 OVSamplesLong.wiff 021710\SampiesLong.wiff 021710\SampiesLong.wiff 021710\SampiesLong.wiff 02171 OtSamplesLong.wiff 021710\SamplesLong.wiff 0022117711O0\VSSaammpplleessLLoonngg..wwiiffff 021710\SamplesLong.wiff 021710\SampiesLong.wiff 021710\SampiesLong.wiff 021710\SampiesLong.wiff 021710\SampiesLong.wiff 00221177110O\VSSaammpplelessLLoonngg..wwiiffff 021710\SampiesLong.wiff 02171 OVSamplesLong.wiff 02171 OVSamplesLong.wiff 021710\SamplesLong.wiff 021710\SampiesLong.wiff 021710\SamplesLong.wiff 02171 OVSamplesLong.wiff 021710\SampiesLong.wiff 021710\SampiesLong.wiff 002211771100\\SSaammppiieessLLoonngg..wwiiffff 021710\SampiesLong.wiff IS Peak Area (counts) 25405402.0620 2783700 2542500 2677400 22975574890000 2651100 2907400 23626147440000 3083200 3489500 3542200 3322000 3135900 2890600 3090100 3320900 3007600 2911800 3291800 3060500 3300300 3145300 2786900 23915744310000 2900400 2939100 22683647660000 2693100 2491600 2954000 22794711720000 2881600 2873500 2808200 Z 345 p. 125 Acquisition Date 1 2/18/2010 0:04 2 2/18/2010 0:33 43 22//1188//22001100 00::4532 56 78 9 2/18/2010 1:02 22//1188//22001100 22//1188//22001100 111:-:231111 1:50 10 2/18/2010 1:59 11 2/18/2010 2:09 1123 22//1188//22001100 22::1288 1145 22//1188//22001100 22::3477 1167 22//1188//22001100 23::0567 1189 22//1188//22001100 33::1265 20 2212 2/18/2010 22//1188//22001100 333:::345544 2234 25 2276 28 2/18/2010 4:03 2/18/2010 4:13 22//1188//22001100 44::2332 22//1188//22001100 44::5412 233190 222///111888///222000111000 555:::012100 333423 35 22//1188//22001100 55::2399 22//1188//22001100 55::4598 36 37 2/18/2010 2/18/2010 66::1078 38 2/18/2010 6:27 4309 2/18/2010 2/18/2010 66::3466 Position Sample Name Acquisition Method 1 IB PFCkinetexShort dam 2 PFC O.IOppb 43 PPFFCC 0I..O5ppppbb 65 PPFFCC 51.00ppppbb 87 PPFFCC 2500ppppbb PPFFCCkkiinneetteexxSShhoorrtt..ddaamm PPFFCCkkiinneetteexxSShhoorrtt.ddaamm PPPFFFCCCkkkiiinnneeettteeexxxSSShhhooorrrttt...dddaaammm 7 PFC 20ppb CCV PFCkinetexShort.dam 9 PFC 20ppbICV PFCkinetexShort.dam 25 K1001011-001 2276 KK11000011001111--000032 PPFFCCkkiinneetteexxSShhoorrtt..ddaamm PFC kinetexShort. dam 2289 KK11000011001111--000054 PPFFCCkkiinneetteexxSShhoorrtt..ddaamm 3310 KK11000011001111--000067 PPFFCCkkiinneetteexxSShhoorrtt..ddaamm 3323 KK11000011001111--000089 PPFFCCkkiinneetteexxSShhoorrtt..ddaamm 333465 KKK111000000111000111111---000111120 PPPFFFCCCkkkiiinnneeettteeexxxSSShhhooorrrttt...dddaaammm 37 K1001011-013 PFCkinetexShort.dam 38 K1001011-014 39 K1001011-015 444120 KKK111000000111000111111---000111876 PPFFCCkkiinneetteexxSShhoorrtt..ddaamm PFCkinetexShort.dam PPFFCCkkiinneetteexxSShhoorrtt..ddaamm 4434 KK11000011001111--001290 PPFFCCkkiinneetteexxSShhoorrtt..ddaamm 444567 KKKQQQ111000000000666666444---000123 PPPFFFCCCkkkiiinnneeettteeexxxSSShhhooorrrttt...dddaaammm 48 KQ1000664-04 PFCkinetexShort.dam 4590 KKQQ11000000666644--0065 PPFFCCkkiinneetteexxSShhoorrtt..ddaamm 23 KQ1000620-01 PFCkinetexShort.dam 24 KQ1000620-02 PFCkinetexShort.dam 22 KQ1000620-05 PFCkinetexShort.dam 21 KQ1000620-06 PFCkinetexShort.dam File Name 021710\CalShort.wiff 00221177110O\VCCaalSlShhoorrtt..wwiiffff 002211771100\\CCaallSShhoorrtt..wwiiffff 000222111777111000\\\CCCaaalllSSShhhooorrrttt...wwwiiiffffff 021710\CalShort.wiff 021710\CalShort.wiff 00221177110O\VSSaammpplelessSShhoorrtt..wwiiffff 021710\SamplesShort.wiff 002211771100\\SSaammpplleessSShhoorrtt..wwiiffff 002211771100\\SSaammpplleessSShhoorrtt..wwiiffff 002211771100\\SSaammpplleessSShhoorrtt..wwiiffff 021710\SamplesShort.wiff 002211771100\\SSaammpplleessSShhoorrtt..wwiiffff 021710\SamplesShort.wiff 00221177110O\VSSaammpplleessSShhoorrtt..wwiiffff 021710\SamplesShort.wiff 002211771100\\SSaammpplleessSShhoorrtt..wwiiffff 002211771100\\SSaammpplleessSShhoorrtt..wwiiffff 021710\SamplesShort.wiff 021710\SamplesShort.wiff 002211771100\\SSaammpplleessSShhoorrtt..wwiiffff 002211771100\\SSaammpplleessSShhoorrtt..wwiiffff 021710\SamplesShort.wiff 021710\SamplesShort.wiff 021710\SamplesShort.wiff 021710\SamplesShort.wiff IS Peak Area (counts) 34762000 3642700 3377400 3454400 33687436110000 3076700 3456700 3241000 4111000 4153700 4256500 4818300 4391200 3952600 4103700 3991000 4326800 4282000 44462555050000 4287300 4585900 4950500 4323500 4924800 4471900 4112800 4811100 4426800 4520200 4384200 4128300 4759500 4447500 4839900 4436900 4213600 4507500 Z ,i ^ / io 346