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,^-s -^ ?y y""^. '< UNITED STATES ENVIRONMENTAL PROTECTION AGENCY 5 »/ iBKiii 1 ' HOUSTON BRANCH REGION VI eeoo HORNWOOD DRIVE HOUSTON TEXAS 77074 Ref. Case No. Site Name l^/^T^^ Date: /A^-77 Subject: CLP Data Review 7&^-^~- ^ From: Michael L. Daggett, Chief, Organic Lab Section, 6E-HL CD r^ To: Hank Thompson, 6E-SH "H T-l A review of the laboratory raw data for the reference site has been 0 completed by members of the Laboratory Section. Samples were: INORGANIC: ORGANIC: 3^o?/gLZ>3 The data was found: ( ) Acceptable (W Provisional; use of data requires caution. Problems are noted In Review Sumrnai ( ) Unacceptable; data should not be used. Problems are noted in Review Summary. Questions regarding the review can be addressed to me. Attachments cc: David Stockton, 6E-HL Duane Geuder, WH-548A

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,^-s -^?y

y"" .'< UNITED STATES ENVIRONMENTAL PROTECTION AGENCY5

»/iBKiii1' HOUSTON BRANCH

REGION VI

eeoo HORNWOOD DRIVEHOUSTON TEXAS 77074

Ref. Case No.

Site Name l^/^T^^

Date: /A^-77

Subject: CLP Data Review7&^-^~- ^From: Michael L. Daggett, Chief, Organic Lab Section, 6E-HL CD

r^To: Hank Thompson, 6E-SH "H

T-lA review of the laboratory raw data for the reference site has been 0completed by members of the Laboratory Section. Samples were:

INORGANIC:

ORGANIC: 3^o?/gLZ>3

The data was found:

( ) Acceptable(W Provisional; use of data requires caution. Problems are noted In Review Sumrnai( ) Unacceptable; data should not be used. Problems are noted in Review Summary.Questions regarding the review can be addressed to me.Attachmentscc: David Stockton, 6E-HL

Duane Geuder, WH-548A

^ .

ORGANIC QA CHECKLIST

Site Vertac____________ Contract No. 68-01-7390

Case No. 8019/04________ Contractor TMS Analytical

Reviewed By Melvin L. Ritter , , soi1_________

Date 11/13/87 & 11/16/87 Acct. # 8TFAJN38 SF TFAU04

Sanple No. DF0212-03 __________ ___________ _________

DF0212-18 ___ __________ ^

___ __________ T-IDF0213-04 through DF0213-12. ——— —————————— ^.0

OVERALL COMMENTS (.To Be Oanpleted By EPA PERSONNEL)

1. Holding Times2. Tun ing/Performance3. Calibrations4. Blanks5. Surrogates6. Matrix Spike/Dup7. OOBpound Identity8. Case Assessment

TOA Ei/H A fcst Other

__ _ __ __ A__ _ __ __ -A-

__ __ A

- ' _^

OOTOffiMTS OR CLARIFICATIONS (See Attached)

A - Acceptable - All items delivered; all criteria met.___________________

P - Provisional - Data usable; sane non-essential review items missing or criteria

were not met.___________________________________________

U - Unacceptable - Data unusable; essential review items missing or criteria not met.

/^ r>

COMMENTS/CLARIFICATIONSREGION VI CLP QA REVIEW

CASE 8019________ SITE Vertac_____________ LAB TMS

The following is a summary of sample qualifiers used by Region VI inreporting this CLP Case data:

No. Acceptable Provisional Unacceptable

VOA _________ ________ __________BNA —————————— ————————— ——————————— ^PEST ______ _____ _______ r-OTHER Dioxin____9 ____3 ___________ ^

— - — — — — — — — - — — — — —' — — — — • • — ' - — — " ^^

0COMMENTS:

Batch 04 for Case 8019 is considered as provisional. The sampleswere analyzed for 2,3,7,8-TCDD and problems noted by the lab forthese samples were reported in the narrative. The provisional ratingapplies because of the need for the lab to resubmit Form B-1S, theresults form. The lab listed samples -09, -10 and -11 as being positivehits for dioxin, when in fact, the results should have been listedas MFC, because of failure of the results to identify 2,3,7,8-TCDDas per the contract requirements. The lab has been requested toresubmit Form B-1S.Evaluation:

1. Calibrations- All contract requirements for initial and continuingcalibrations were met, including performance column checks. Allresponse factors and their calculations and subsequent use wereas per the contract.

2. Method Blank- Acceptable. Detection limit of 0.3 ppb; surrogatesignal/noise ratio good and internal standard recovery good.

3 . Internal standards and surrogate recoveries- Provisional.Lab reportedsevere problems with a number of samples due to recoveries and reransamples -09, -10 and -11. Supplemental data was Included In thereport to verify the problems. Results should have been reportedas MFC values, not as positive hits for these three samples; labrequested to resubmit resultstorm,B-iy.

4. Spike/Duplicate Results- Unacceptable high recovery was reportedby the lab for the native spike 1 ppb amount; the lab reported 3 . 5ppb,or 350% recovery; reruns confirmed this problem. Per David Anderson,FIT

ORGANIC CLP/QA REVIEWCONTINUATION PAGE

CASE NO. 8019__________ SITE vertac

COMMENTS:

this sample DF0213-11 used for the native spike (suppose to be cleanand used to demonstrate the lab ability to process and recover a_____'known amount of added TCDD) was Station 26 on the custody list and ^actually was a sample from an area that previously had shown an !>•amount of TCDD greater than 1 ppb. This native spike QC data Is ,_(thus useless. T-*—————————————————————————————————————————————————————— 0Duplicate results done by the lab for sample DF0213-12 showedgood agreement in that both sets of data had TCDD less than 1 ppb.

5. Performance Sample- Acceptable. The lab did DF0212-18 as the performanceevaluation sample and the result found of 6 . 7 5 ppb agrees with theknown result to within the 95% acceptance window. Data here was good.

6 . Compound Identity- Provisional due to need for resubrnlttal and dueto very poor internal standards and surrogate recoveries for thesesamples. Positive results reported for DF0213-06 ( 0.7ppb) and forDF0213-08 ( 2 ppb).

7. Case Assessment- Provisional. In addition to the required resubfor Batch 04 as noted earlier, three samples are being requestedfor re-extraction and reanalysisfrom earlier submissions fromthe lab In this Case 8019; samples DF0212-09 and DF0212-12 fromBatch 02 and DF0213-01 from Batch 03 were all reported by the labto have an MFC of greater than 1 ppb. By terms of the contract,Section C 2. 1 . 5 , page C-2, the samples showing >1 ppb MFC shall_____be reanalyzed.

^ ^

CONTRACT LABORATORY PROGRAMRAS RE-ANALYSIS REQUEST/APPROVAL RECORD

SECTION A

fl. Case No. 8019 SAS No.______ ff2. DPO or RSCC David Scockton

S3. Details of Re-Analysis Request:

o Laboratory Name: TMS Analytical_______________________

o Sample No(s). . Fraction(sfc DF0212-09, Batch 02 Dioxins———WOili-H. Batch 02———————————

DF62l^-01. Batch 03o Reason for Re-Analysis; Samples had a reported MFC > 1 ppb.

Contract, Section C2.1.5, requires rerun when MFC > 1.

o Procedure for Re-Analysis: Dioxin IFB for 2.3.7,8-TCDD.

i?4. Name of PO Contacted: __________________ Date / /

REQUEST; Approved __ Not Approved __RE-ANALYSIS; Billable __ Not Billable __

#5. Name of SMO Contact; __________________. Date / /

SECTION B (TO BE COMPLETED BY SMO)

)»1. Date of Laboratory Notification (Verbal) / /

f2. Re-Analysis Start Date / / f3. Data Due Date / /

SECTION C (PROJECT OFFICER CONCURRENCE)

Concurrence By ______________;______________ Date / /Project Officer Signature

Return intact form to:Sample Management Office

P.O. Box 812Alexandria, Virginia 22313

Distribution: (1) PO Copy (2) DPO/RSCC Copy (3) SMO File Copy (») Lab Copy

7/22/S6

TMS^ ^ ^^

TMS ANALYTICAL SERVICES, INC.TANDEM MASS SPECTROMETRY

6376 Morenc; TrailIndianapolis, Indiana 46268317-291-5697

October 1 5 , 1987

CLP Sample Management OfficeViar & Go.209 Madison S t . , Suite 200Alexandria, VA 22314To whom it may concern:Enclosed is the complete Sample Da-fca Package for the analysis ofsamples for 2 , 3 , 7 , 8 - T C D D according to the procedures specifiedunder CLP contract »7390.These samples were received as Case ?8019, Batch #4 on September23. Results were sent by overnight courier on October 16 forarrival on the October 1 8 , four days late of the October 1 4 , 1987due date.On 09/23/87, Tony Neskey from SMO called Dan Delinger from TMS tonotify the lab that Case #8910 Batch 4 should be Case #8019 Batch4 . Adjustments were made by Kelly E. Mills, Sample Custodian, on09/23/87.Problems were experienced with three of these samples. Samples#213-09, 10, and 11 are invalid regarding proper ion. ratios andsignal to noise requirements. TMS Analytical was conscious ofthis discrepancy and re-ran the samples several times (seesupplement). In all cases, recovery proved to be extremely low-We believe an interfering substance within the samples causesthis problem- This conclusion is based upon: ( 1 ) no problems ofthis nature were encountered with the other samples, ( 2 ) allthese samples were of the same type (sludge), and ( 3 ) in allthree samples a 320/322 ion pair is present without theconfirmation ion.If you should have any questions regarding these data or thisreport, please contact Dan Delinger at (3 1 7 ) 2 9 1 - 5 6 9 7 .

Very truly yours,<y^\ ' J <LL,A_>^»L^vfc», •3< --•'YZ^l*^

Dennis L . Hearing Ph. D.President

CC'USEPA EMSL/LV QA Division944 E . Harmon Ave.Executive Center, Rm 228Las Vegas, NV 89109

USEPA REGION VI LABORATORYMonterey Park Plaza - Bidg. C6608 Hornwood DriveHouston, TX 77074Attn: Melvin Ritter

October 7 , 1987

CLP Sample Management OfficeViar & Co.209 Madison S t . , Suite 200Alexandria, VA 22314To whom it may concern: UT5Please replace the existing B-3 Forms found in the Sample Data ^Package and the Sample Data Summary Package with these corrected ^*B-3 Forms. Our files have been updated and corrected by C. Tn

Krauss, Document Control Officer. 'If you should have any questions please feel free to contact meat (317)291-5697.

Thank You,

Cynthia J . KraussDocument Control Officer

CC:USEPA EMSL/LV QA Division944 E . Harmon Ave.Executive Center, Rm 226Las Vegas, NV 89109

USEPA REGION VI LABORATORYMonterey Park Plaza - Bidg. C6608 Hornwood DriveHouston, TX 77074Attn: Melvin Ritter

ENCLOSURES:

TMS, /-N 5t"/^-^/

TMS ANALYTICAL SERVICES, INC.

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FORM B-1S. TCDD SOIL DATA REPORT FORM Page 1 of 2

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FORM B-1S. TCDD SOIL DATA REPORT FORM Page 2 of 2

Lab; T/7fS ^^^^vnc.AL______ - Report Date; / ' ( ^ / / ( / / g ^

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TMS Analytical Services Inc.6376 MORENC1 TRAIL • TEL-1317) 291-5697 • INDIANAPOLIS. INDIANA 46268TANOEM MASS SPECTROMETRY

FORM B-1S. TCDD SOIL DATA REPORT FORM Page 1 of ;

Lab; ~~~ /g /-^J ^ y r-/r <-. • Report Dace; /'g//<//1y?

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ITMS "MS Analytical .Services Inc.TANDEM MASS SPECTnQMETRY 6376 MORENa TRAIL •TEL-SIT) 291.5697 • INDIANAPOLIS. INDIANA 46268

FORM B-1S. TCDD SOIL DATA REPORT FORM

Lab; ~~/~/ytS /J'O^/^T-A^/'K—

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Column; -S^ £> 3'3 /

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TANDEM MASS SPECTROM6TBY

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FORM B-2 . page 1 of 2

INITIAL CALIBRATIOtI SUMMARY

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FOR1-1 B-3

ROUTINE CALIBRATION SUMMARY

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TMS Analytical Services Inc.6376 MORENCI TRAIL • TEL. (317) 291.5697 • INDIANAPOLIS. INDIANA 46268

FOR11 B-3

ROUTINE CALIBRATION SM-iMAP.Y

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3tb-6./Z6-£TS.-'t'H:3itt3!6I08 3Sy3 !31dlWSsft ^uyseaiyJ ?ii1^ esseuss 28/sfl/oi

TS F.'RHJ.M MIW swwi.wom ssyi'i ain

011816

M I D NASS CHROMATOGRAnS OATH; IXT0213 Sl1Q/133-'87 2; 03 see CHLI; C,.U3325S7 if3SW1PLE: CASE 8019!BATCH4/'213-0?/9.91GCOHDS. i G0t'1 SP233l/ie0/ieO-208e25.'2@0-24ne4/'8RANGE: G17@4,185S LABEL; N 5, 2.5 OUHH! A 1, \.Q J 0 BASE; LI 29, 3

SCANS 1784 TO 1859

8T8TTOMID MASS CHROMATOGRAMS DATA; i:n;:Tu213 ftl SCANS 1704 TO 185@16/93/87 2s03s80 CALI; CALS32587 S3SAMPLE: CASE 8019:BATCH4/-213-@7/9.91GCONDS.: 69N SP2331.-''18e/l@@-2ea@25/209-240@4/SRANGE: G 1794,1356 LABEL; N 5, 2.5 QUAH; A 1. 1.6 J 0 BASE; U 20.. 3

17817476.71539. 7436.

332.699± 0.500

3S8S.

334.106± 8.509

SCANTIME

@3-'I-4 ••.•IQW

ZS8I £381 9T8T '-gQg-f-

I/3SZTs •B3 n sssya e r s't ••0 n ;|M-|Q u-t' ••e n siaayi esai't 'n^TO ;33nyas./t'est'z-£iee/e3ao0e-0ui/'0@'[/-T£e;ds HSS s 'saNoo

335 • 6/'S0-£ I S/t-HOiHg; G 108 3Sy:i •• 3"1dWS£tt ^ys-GR'il^ iIT'O WW-'i. ;8/£8/uT

6SST 01 t-O^I SH':'::i3 Vs 3^WW ^^W 3ia QII-1

011819

•!:;.£.[8S.1Is 'BE n !3sya u r eri • t 1.1 :n"l"li3 s's •s n ;"i3ay'i eesi't'o^ia ••^m

8/ra"{'£-603'£S30aS-a01.''00I/I££:£dS H09 "SQNOOrc3b•6./S^3-£:1^.'••^'H^i^g;6T98 3Sy:3 !3"ldNyS

£S ^SSieuTiJ srT'J 8u!8t'!£ 28/SS/OT1ft 91£OL::'ii i^.l.Ui] SUHdOOiyUCiaHO SS9N Gil.)B38I 01 t'SZT StiyOS

011820

3NI1 ZQW bF^b l J.-:-bt t - c - L l ! - . > • • . . , - . - . . •u t ...^•.;.lNyOS 0t'8l 0Z8T 008t Sy.'l S9/'l Ot'Zt SS^I

' ^^ /M^JV^^^^Vv-^

dSZIs 'es n !3SMa 9 r £fi • i " :N')rii-i e'2 •s n naa'.n ussT't-ozia =3:inyas/i'aflt-s-eos/sesiBas-flui/sBi/isseds NBS !'SC]NOJ

586 • e.-'SO-S I S./t-HOma •• b 108 3SH3 s 31dWSSft ^SP^Gn'T'-i STT^i e9!81?!£ .IS/eQ/M-i

0S3T 01 t-C^T SI!H:IS Itt STT'n.lJii :i-;.l.i'r.! SI.I".i)OO.lnHOaH::i SS"1.1 dIH

011821

gg8TTOMID HASS CHRiJmTOGRAMS DnTO; iJCTu21G Sl SCANS 1704 TO 1S5816/S3/S7' 3;48!@9 CKLI; C"L832537 tt3SAMPLE: CASE 8019; BATCH4./213-88/9.38i3COHDS.; 6611 SP2331/ie0/100-200625/2e9-24Ei@4/SRANGE: G1704.ia5Fi LABEL; H 5, 2.5 QIJAH; A 1, 1.9 J 6 BASE; LI 20, 3

17S65632.ssraa.

A 5632.

332.039± 0.500

1756724.6364.

17867123.687bb.1\ 7144.

334.100± 0.569

^ \7 . / \

172R 1740 17ei3 1730 1860 1S20 1840 SCAN,.-,.,.-, ,.-. r.— <".r-! ic,.""-. fq . - 'c 19;49 20;02 TIME

S88TTOMID RIC DATA; OCT6217 #116/03/87 4:10:00 CALI; CALE82587 #3SAMPLE: CASE 8019!BATCH4/213-S9/10.28GCONDS.! 6011 SP2331/100/'100-200e25/2ee-240(M/-8RANGE; G1794.1850 LABEL; H 0, 4.0 QUAN: A 8, 1.0 J

SCAMS 1704 TO 1859

0 BASE: U 20, 3

o o -nom u"i r~ M 3•• • rn N. n'"• " co 1/1ID -^ in—»(no

--3§°J(-n(«iS->®-0 (>-1 1-0 CT 1^s§ I

" M OiCT I

^"'5"'^^

0 03 0 0CT I 0 I> 3>CM 1~ —I3> 4». — 3>3: G> — —

-o. oo^ P30 Si

fr-k *^ ts^

" !»

^ s"OT3>in

SgSTTOSCANS 1704 TO 1850MID MASS CHROMATOGRAMS DATA: OCT0217 #1

10/83/87 4:10:60 CALI; CftL892587 #3SAMPLE: CASE 8019:8^1^4/213-09/19.282CONDS.; 60M SP2331/l00/10a-200e25/2S0-240e4/8RANGE: G1704/1850 LABEL; N 5. 2.5 QUAM; A 1, 1.0 J

1748

988TTOMID MASS CHROMATOGRAMS DATA; OCT0217 ttl SCANS 1704 TO 1850WQ3/87 4;10;00 CALI; CAL092587 #3SAMPLE; CASE Se^BATW-^-aS/ie.^GCONDS.: GBM SP2331/100/100-200(>25/200-240@4/8RANGE; G17B4/1850 LABEL; N 5, 2.5 QUAN: A I / 1.0 J 8 BASE: U 20; 3

17776488.64907.

1749500.4314.

G512.

332.099t 0.500

1747517.5222.

S128.

334.190± 0.590

1729 -1740 1766 1780 1800 1820 1840 SCANIRi-n IR.W 19; 1.0 iq-23 19;'3l; 19;49 20:02 TIME

MID RIC OATAs 0016508 #110/05.'87 7850:08 CALIi CAL692587 #3SAMPLE; CASE 8019:BATCH4/213-10/10.24GCONOS.: 6011 SP2331/100/'100-200e25/200-240@4/8RANGE: G17@4<1850 LABEL; H 0, 4.0 QUAN; A Q, 1.0 J

SCANS 1704 TO 1850

U 20, 3

1763

_1712 i723 1733 1741 1743

17201•^•.l•"i

174Q1'"' • '"c

1769) n. 1 n

17801 q .'-••?

180019;W

1S2019; 49

184320:02

8S8TTO

MID MASS CHROMATOGRAMS DATA: OCT0508 #1CAL632587 #3

SCANS 1704 TO 1850IQ.'Q5/87 7;50!00 CALI:SAMPLE; CASE 8019;BATCH4/'213-10/'10.24GCONDS.; CBM SP233l/l08/100-20Q@25/200-240@4/'8RANGE; G1794,1S50 LABEL; N 5. 2.5 QIJAN: ft

175987.414. ,

1. 1.0 J 0 BASE; U 20, 3

CO<M00

088TTOMID MASS CHROMATOGRftMS DATA: OCT0588 #1 SCANS 1704 TO 185010/05/87 7!50!@0 CALIs CAL692587 #3SAMPLE; CASE 8ei9;BATCH4/'213-10/10.24GCONDS. s 6011 SP2331/100/100-200@25/'200-24ee4/8RANGE; G1704,1859 LABEL; H 5, 2.5 QUAN; A 1 , 1.0 J 0 BASE; U 20, 31789

5856.54040.

1762154.

.-U12-

5856

332.09A 9.59

7000

334,101± 0.501

17G1218.1461, / v.—-—-^ // \_

1729 1740 1769 1780 1800 1820 1840 SCANIP-4-'! i".^- i q - i n iq.""' I'a.'sR 19;49 20;02 .TIME

61'=61ezsi

at'bi6081

Ul ^tu9;l

c,y6leszi

y sNyna e't- ••e H naayi as8T't'ezi3 saawa8./t'86t'2-0BZ/'fieBeez-e0i/00i/'iessds nag i'sano3

^^6•6/II-eI^-/t'H^iya^5I08 asro saidHre£» isszww ••nw Baiifrifi J.B.-'sa/ut

nt t'Bseicio syiw 3ia OIH@s8i 01 t?@zi snyos011831

3S8TTOHID MASS CHROtlATOGRAMS DATA; OCT9594 #1IQ/SS/S? 5;41;6@ CrtLI; CHL9925S7 #3SAMPLE; CASE 8619;BATCH4/213-11/9.95GCONDS.; 60n SP2331/'190/'10@-2ee@25/'200-240@4.'SRAHGE; G1704-1650 LABEL; N 5, 2.5 QUAH; A 1; 1.0 J 8 BASE; U 2Q, 3

SCANS 1794 TO 1850

109.

259.877± 0.59S

37,

328.938± 0.500

1843 SCAN28:82 TIME

35' 0 CD- 0

iri 1/1 r~ cn 3— • m •\ xr" — 00 LO 'W

ID -.Jl/1 ~^•wo _ cr")

"-iaflo-00 |s) ® •ggtoS

'^So§§^

P^£— 0 -k.G) M

"MS

^£^1^0• ^ •i-nrJ i-oeg i_n"3>in(

*. 0 0^» ?3

(t>-M

0 -b

H-t«)i-o

ISM cn*-»M

9S8TTOMID MASS CHROMATOGRAMS DATA! GCTO506 ttlH3/@5..'S7 fi!47;9@ CALIi C(,t.ij925S7 tt3SAMPLE! CASE 8019: BATCH4/213-12/16. £iSr,COHDS.! 6@M SP2331/10i3/l@[email protected](.l-2-101^-1/8RANGE: G 1704..1850 LABEL: N 5, 2.5 QUA?!; ri 1 , 1 .9 J 9 BASE; U 2t3, 3

SCANS 1784 TO 1853

3Hll W°-Q6 St^bl afc-bl C G - b t " • • . ; l -i-r.-.l ...I .-.I

Hy::iS 0{-ST 03SI 088T @3.J.t 03.'? n^I "3<U

S^^^ f""^^^'j ' '. I 1

'i ,iees'a Tsee"zee

ess'8 T966'eZ£

' i^i•9K0321£: ''oe n sasya o r Q'I • i H ^"'rio e'z •s N naayi ossr't-u^io !33nya

8. Hii3t£-0e3/SSs)6S£-99I/89I/'I££3dS US3 s •SQHOO3y0 • u I .-'£ I -S t S./t-HOiya s 6 T 98 35^3 •• BIdUbS

ss zssssa'i'n snyJ oeizi'!9 zs/se/ei6S8i 01 wi SHHOS ift srisn.i.-J!:i ;H.!.|.!|] sHyyaoiyMoaH:! ssyi'i QIN

011837

SS8TTOHID MASS CHROMATOGRANS DiiTn; OCiese.S ftl10/05/S7 6!47!S6 Cnl-Is Cii;.&325S7 #3SAMPLE; CASE 8019;BATCH4/-213-12/10.08GCOHDS,: e:0M SP2331/ie0/130-250@25/20M-2'10@4-'SRANGE: G1704,1559 LABEL; N 5, 2.5 GUAHs n 1 . 1 .8 J

SCAtIS 1704 TO 1850

17532979.

2G5:-"& >A--.

6 BASE; LI 28,1787624S.57766.

/\ 624S.

332.093± 0.50S

17876499.64388./ 6512.

1728i •"•. .•-\ -•

17533S15.

33363.

f\

1740

{ '., 334,100i1 I ± 9.500

'' \-——i—-"f=——r—=—r-——T——r"^"—'39 1800 1828 1849 SCAH

•-, i.-!,--..- iq :dq 29; 02 TIME

6S8TTOMID RIC Dnln: UCTU5U7 #1 SCrtHS 1704 TO 1859ii3-'05-'s7 7!2e!ee CALI; i::h,Le925S7 tt3SfW'LE! CASE 8013SBRTCH4/213-12 DUP/9.9HGCOHDS.! 6en SP2331/160/109-290i]'25/2ee-24B@4/8RAtiGE; (,1704 ..1S50 LRBEL; H 0. 4.0 RI.-IHH; H H, 1.9 ..I S BRSE; LI 28, 3

179:3

1 f l - b

Ai1 i

,1 i

11872.

;_1713-._.-. ,. .-17i4 l743- ..-/ \\-^__1831 _ 1837

172i3 1749 176n 1788 1890 1826 1848 SCANi " - - - . !.-.-i— • ! • ' • • ! , : . • i-a. '•-•. ^''••'•i" IS:'!^ 21'';l32 TTHE

^? i. ,' l.Q —SSigo.-; o -o i;m 1.1-1i— c. _"• • m '-i ir— •• W i.riCI --j i.i-i

•£•--~ iTl 0-^ 0 B- 0S^S:-^

^g^g-1 W '-' Q —10 CA.I ^£i Ci 0

T^- l ;l .m r~i im '•s :

r-..-i IJ)fz ii-n CT >—- ro M

"g?^_ c? ir. c. c'.£" r';' 1.0 r" -i3; -ii. 135 —' l': r5 i7"J "• BB

13 cr'i-i:i eni-.-i o•:.n -.Jix'-.J =«=

3HI1WJS

ass'o TSSB'SSS

06s'e T960•8S£

011841

r"OK!".Ibt83 J. Ie •BS n !3sya e r e'i • i n wm s'e •s H snaay"! eesT't'ezi'i saoHw

8.'••i'^n^•^-^^^J^.••••e^3^^9^-0^^I/^3^I.''l££^dS Ma9 ! •50103OOG'S.-'dria SI-STS/l-HOlUgsGISS 3Sy3 !3'ldHHS

ss ^sszee-iro snTO ea'e;^ zs/-s@/eT0S8I 01 Wt SH93S TS ^OSOlOO !yina SHH::JOOiyHO;:IH:J SSHU QIH

ai-lii oi'to bp^i ;,-o, .,.•'-,, . , • . . . , ...., ...i . . i •.,.iNyos QW ezsi eesi es.'i o^t 0^1 Bezt

r-'-' '"•••...;

\ / \ i

\ l l /'ess's T 'i ,1 ''i ,.'eer-t'ss \ 1 ', ,-''\ / •^fc

/ -%5Sl 93^1

"r'1•^ -zJis•sszs£6ZI

\ / \ /SOS-Q-f \ ; 1 ,;eeB'zss ', \ ,••

'i ; S'f •-s^

1 j W-:W

\]'959*' •c' ,-,*.

011842

./V•63£0t-•^b^3^'S6ZIc '82 n sasya 0 r a'l ••T y inyri£i s's 's n siaayi esai't'e^TQ s33wa

8/1'8:i9t-S-083/SSB@OZ-0ei/-0ai/1£eSdS MBS i'SQHOOaub-e/dna si-sis/tHoiva'sies asyo :3idMys

Stt ^•3^^6^J"1L.J:3 !I'TO 9@S0Z^ Z8/S@/-8I8S81 01 WI SH93S Tft ZOS01JO SHIHO SHy:d301WOaH3 SSbH OIN

smioMID RIC: DATA; HCTH503 Sl Sr:AHS 1704 TO 185818/95/S7 5!l2!@0 CHLI; CALe92587 ?3SAMPLE! CASE 8013;BATL:H4/212-03/9.9(jGCOHDS.: G0M SP2331/'lSB/iea-260@25-' 2uo-24ni-4- SRANGE! G1704.1S59 LABEL; H 0, 4.n QUnH; n 0, 1.0 J C^BftSE; IJ 20; 3

108.0-1 ^^ 15168.

I

^ ^RIC_ ^ ^r\.i \ i .

_..1712__^ , _ 17;33 1741, _,.•• '-,,....—'' ''-———._1.8.14_^_„lp_30 1845

1729 1748 17en 1789 1800 1S20 1S40 SCANi . - , . < • - i , - , , . - , - i,-,-i,-, )r,,.-<, ,,:,,-,>- iq;49 26:82 TIME

^8TTOHID MASS CHROHftTOGRfiHS DATA: OCTffiUS! 91 SCANS 1784 TO 1856H3/S5/87 5sl2!8S CALIs CnLy33587 S3SAMPLE; CASE SEllSiBHTCW/^^-^/g.gaGCOUDS.; 6£iM SP2331.''10e/'10i3-2Eii3e25.'2e0-246@.! •£;RRNGE: G17@4,1859 LABEL: H 5, 2.5 QUAH; H 1 , l.Q .1 0 BASE; LI 29, 3

,1-j i 61.

• (,l,ltf •''lvJWk•Al\<--—^——L^——^——————^ —-^————————J————————————1———r^-^

17G41,'0.

l.fl-1 1521- 1^7.

^'a _ ''! 328.098

I ± 0.500|i,i I

A't^v^--- '• .. > r AAL———,——————^————,————————————r-(——_^.——._-,-__——^——i——,——————^——————^-1————^——————,——————^————|

1729 174U i7ey 1789 1888 1825 1840 SCANf.-.. I-, ,,-. . - i - : • . ,-,.-." I.-,.-,,- ig;4g 2n;fl9 TIME

SCANS 1704 TO 1858MID MASS CHRQt'lHTOGF;Hl'IS Di-iTu; OCTQ5B3 #119.'£i5/'87 5;12!@0 CHLIS CnL.632587 »3SftMPLE; CASE S019:BATCH4/212-63/9.30GCOHCS.: 6@M £P2331/10a/100-2t3e625/200-24ee4.-8RANGE: G1784.1850 LABEL: H 5, 2.5 QUnN; A 1 . 1 .9 J 0 BASE; U 2Q, 3

a i/o >• i-u

MID ?55 CHROHRTOOWIS DHTH: uCTu5u3 »1 SCANS 1794 TO 1859ie.'e5-"87 5; 12:00 CftLIi ?1892537 ft3SAMPLE; CftSE 8019:BATCH4/212-03/'9.90GCOHDS.: 60H SP2331/'ie0/lCi0-2e0e25/-2i3£i-24e@4.''8RflHGE; G1704,1858 LABEL; N 5. 2.5 BUflH: fl 1, l.S J 0 BASE; U 20, 3

17S85614.

73.

•"i ••;,-'>

nn.

3.34

3-,

9-

/

../'»'" "1" •r-"- T '-• r'"'

/y

1729 1748IF'.,''; I'"'.1--:'-

17612903.24324.

,'•.,/ \

' \

\

i7ee3911.!28bb.

'\',\

1768i--f. (1-1

52245.

A....... —r -T- •••'" —-T-" ••—+ • r" -17S87694.

65SG6.

A-T————'———^1——————————————————f———1789 1808 182S 1840f'^-•""'-! I ' ^ -^R 19; 43 20:02

5624

332.09± 0,50

7616

334.10(± 0.50(

SCHHTINE

M I D RIC Wf(\i i:ii::'!u5£i';i »119/05/37 6! 19; 0i3 Ci',1-^ ?1.632587 -S3SAMPLE: CfiSE 8019!BATCH4/212-18/9.99GCOHDS.; 60M SP2331/ia0/ieu-2eie@25/2UM-240a4.'3RANGE: 01704,1850 LABEL: H 0, 4.0 num); 9 i3, 1.0 J i3 BASE; U 2*3, 3

1 *' b I

SCA113 17S4 TO 1S50

17S9

••: /1743 .-• ^-.1888 1828 1:340

1749._.——^_--... .-..,-..-

1769 1780; .3, •-•':•

1809^•."'•K

1820 134019; 49 20; 02

SCAHS 1784 TO 1858MID MASS CHROMATOGRAtIS DnTu; OC.'fiKi35 11118/85/87 6s19;89 CALI; CfiLOS^K? ii3SAMPLE i CASE 8819:BATCH4/212-18/3.33GCOHDS.: GSM SP2331/le9/100-2eee25/•2e0-24G@4.'SRANGE; G 1784..1853 LABEL; H 5, 2,5 OLihH; n 1. 1.0 J 0 BASE; U 20. 3

1 ;-'b31431,

1568.

259,077± 9.5S0

1789212.1764./""'-"•-•,

.. .^ ''--"v.. ^ ^ ^ ^ . ^ ^ , ^ ^

338.

328.09S± 0.599

^^-^H}^•r" 1 i ' i ' i ' '-SO 1809 1828 1840 SCANi ; 1 ' " ' ' • I'-i.-'- !9;49 20;!32 TIMF

smioM I D MASS CHROIWTOGRAMS DOTH: OCT05u5 wl SCHHS 1764 TO 1858le/SS/S? 6!l3;@@ CnLI; Cr,L632587 #3SHHF'LE! CASE 8919: BATCH4/212-18/9.99GCOHDS.! GOM SP2331/109/lS0-20ue25/2He-24G6;-l.'SRHHGE; G 1704..1850 LftBEL: H 5, 2.5 QU9H; H 1, 1.0 J B BftSE; 1-1 20.. 3

1?.S3c- ^-17

OS8TTO

MID MASS CHROHATOGRANS DnTA: OCT(35e5 #1 SCANS 1704 TO 1S5810/05/87 6; 19:08 CnLI; C..L692587 #3SAMPLE; CASE S@19;BATCH4/-212-18/9.99GCOHDS. i 6HM £P2S31/10i3./10a-200@25/20a-24uiM/'SRANGE: G.1704..1853 LABEL; N 5.. 2.5 QUHN; n 1, 1.6 J @ BASE; LI 28, 3

17897513.G™ 7569.

1759 | 'i3951. | \32a(j2- / \ 332.099

A /1 \ ! \• '" i . . . . . . . . . . . . . . . . . . . . r | .,———.^ , „ , . , . , , , . , , „ . ,,.,.. ...... ,..,.. .,,,.. ....F..u,,.,,,.... . -^p. ,

17SS9616.82573, ^

{\1761 14717. ;

4nh7:'-i. | 334.1S8,1 'i ± 0.588

A / V.'z '•--.. ..•'' <1728 1749 l7£i:t 1788 1809 1820 1848 SCANi.-..^- f . - . . c ^ - f . . , i i , .q.-i ra-T- t9;43 2u;02 T T M F

T98TTOMID RIC DATA; OCT1583 ftl SCANS 1784 TO 185019/15/87 14;37;00 CALI; CflL@92587 1t3SAMPLE; CASE 8819;BHTCH4/213-89/9.93GCOHDS.: 68M SP2331/l@0-200@25/20e-240@4/HOLD 9RANGE: G17@4,1S59 LABEL; N 9, 4.6 Q U A N T A 0, 1.9 J 0 BASE; U 20, 3

103.0-1 lfrb4 22496.

'\

RIC_

JJ.33 / \

-IM-——172"^- ''' ''----— -J/ ' -----—^•^---—/J80! ^829^^—1^3 .-^^^^

1720 1740 1769 1780 1800 1820 1840 SCAN

?Q8TTOM I D MASS CHROMATOGRAMS DATA; OCT1563 #1 SCANS 1704 TO 1850le/lS-'S? 14; 37; 60 CALI; CAL092587 tt3SAMPLE; CASE 8019:BATCH4/213-09/9.93GCONDS.: 66(1 SP2331/100-200e25/200-249@4/HOLD 9RflNGE: G17@4,1850 LABEL; N 5, 2.5 QUAH; A 1; 1.6 J 0 BASE; U 20, 3

81'.9.0-1 ss2- A^ 95.

A -'-

yM^^U^—————————————————L-L-T————J———————'-.—————^———r——U——————————————U

7.4-i I 64.

-:JJA,ilq|Ayi//l^.-:=-'^1 l'f|;^|''lf^^|1720 174@ 1760 1789 1800 1828 1840 SCANffi .d-; )H.«=:C I ' -r in iq;^? l'?-'7^ 19;49 29:92 TIME

S98TTOM I D MASS CHROMATOGRANS DATA; OCT1593 ftl SCANS 1704 TO 185818/15/87 14!37;89 CALI; CAL092537 #3SAMPLE; CASE 8019;BATCH4/213-09/'9.93GCOHDS.; 60H SP2331/l@a-200@25/200-24e@4/HCiLD 9RANGE; G17@4,1850 LABEL; H 5; 2.5 QUAN; A 1, 1.6 J 8 BASE; U 29> 3

1738224. -. . > .

8S.3n r-21;4- ^ \P 242.

/ A \ . < - / \ \ 320 _ | v! \/ 320.696

I \ ' ± 9.508

f A /A^J^i/\/-—-^^AA /AA/^W^/yJi^vA/V/^^^ ^•—^———i——'——i———-7—1—r^——'———i———'——\———'———T———'———i •"'

1738 -/--"249.^ i

100.0-1 r T' '71 274.

c U__M-^322 ^ 322.896

\. " ± 0.500

/ \ i \

yVM .!-/——^nW^V^^ . ^ ^,1720 1740 1760 1780 1800 1S20 1840 SCAN1?.. ,-(•-, r--c,- f q . l F l iq.'i'? 19-3?; 19s49 20S02 TIME

^SSTTO

MID MASS CHROMATOGRAMS DATA; OCT1503 #1 SCANS 1794 TO 1850IQ/IS/S? 14;37;98 CALI; CAL092587 tt3SAMPLE; CASE 8019:BATCH4/213-09/9.93GCOHDS.; 60M SP2331/'100-2e0e25/2@0-246e4/HOLD 9RANGE: G1704,1850 LABEL; H 5, 2.5 QUAH: A 1. 1.0 J 0 BASE: LI 20, 3

17659285.

5.0-, s™ 9232.

32 _ I' ', 332.699l ' ± 0.509

173G / \312. / \2944. / \

176410864.

3.0-, wm- 10864.

/ \34 _ J \ 334.108

j \ ± S-500

, 1737 ?'385. ,' \

__3315. / \

1720 1740 17E.0 1789 18S0 1820 1840 SCAN1F;-4? IS-W l ^ - I O I?.?'? l9;3K i9;49 20!02 TI11E

398TTO

NID RIC DATA; OCT1584 #1CHL032587 S310/15/87 15;07;@8 CALI;SAMPLE: CASE 8@19;BATCH4/213-1@/[email protected]

COHDS.; 69M SP2331/ie0-2eee25/200-240@4/HOLD 9RANGE: G1704.1850 LABEL: N 6 , 4.@ QUAN; A 117b3

1735

SCANS 1784 TO 1S5@

1.9 J B BASE; U 20. 3

1710 1717 1805 1816 1792 1828 1840

17281 0 - ^

1743 1769l'"rlf>

17801 <?•'?•'<

1808^9•':'R

182019:49

184029:02

998TTOMID MASS CHRQMATOGRAMS DATA; OCT1584 #1

C.ftL992587 #3SCANS 1704 TO 1859

10/'15.'87 15;87;90 CAL1;SAMPLE; CASE 8919!BATCH4/'213-10/'10.17GCOHDS.: 68M SP2331•/^00-200@25/•2e0-240@4/HOLD 9RANGE: G1704,1850 LABEL: N 5, 2.5 QIJAH: ft 1..

17361.0 J 0 BASE; U 20; 3

77.939. 91.

259.877± 3.53B

70.

328.098± 0.500

SCANTIME

'1> g 3> S >—

?? 0 5 *-*m 1/11^ cn 3. .. CO LI

S^o-^®§S5iS^^'^sg—> -13 03 -•J 303 M (S " X>i-Jl (A.I "• i3 —IGl C«) ID •3> 0

' ro w— .. —r- >-> i> x»Ifl r"-1 -..IIS- 13—1 3£2^a?s w• • - [— M-t-

SM

= ^UI I

^5cs> '" I ©i-JIM-

4t -»IS) -J '-' 0

CT r® 0 I> 3>

^ ••>. 1-1 X'

^~ 0r- '"-• ono pc^i-o H'-l

3S8TTO

MID MASS CHROMATOGRAMS DATA: OCT1504 #1IS/IS-'S? 15:07:00 CALI; CAL0325S7 #3SAMPLE; CASE 8019!BATCH4/'213-10/10.17GCONDS.; G@M SP2331^100-200825/'200-246@4/'HOLD 9RANGE; 01704.1856 LABEL; H 5, 2.5 QUAN: A 1. 1.0 J 0

17£316512.99903.

SCANS 1704 TO 1850

BASE; LI 20, 3

1734183.1556.

176312672.123825.

/'"-•,

1735214.1456.

1728l;?!^

.1748I'"'' c'1"

17601C). 11-1

1780iq ••"•?!

1830^•W

132919; 49

184920:02

3^8TTOMID RIC DATA; OCT1507 #1 SCANS 1784 TO 165819/15/87 16;39iM CftLl! CAL8925S7 tt3SAMPLE: CASE 8919;BATCH4/'213-11 DL1P/10.07GCONDS.; GeM SP2331/'108-200@25./200-240@4/HULD 9RANGE; G1704/1S50 LABEL; H 8; 4.6 WM: A 8.. 1.0 J 0 BASE; U 20. 3

1765 18784.

1720 1748 1756 1780 1800 1820 1840 SCAHl.fl-'r"' r-'.^c i q - l ' - f l^.-'-s ^•"'K 19;49 2@!02 TIME

•0Z9•esi6SZI

H s~13ayi 0S8I't'0^I3 i33N9as '02 n sasya @ r 0-1 'i y !NynQ e'z 's6 aioH/t'80t'3-e0z/'seei00s-00i/ieezds Mes S'SONOOWQl/W II-£I3/t'H3i9a!6I08 3SW '3-ldUyS£# ^sssse'WJ snao aesessgi /s/si/'eint zesuoo ••yioa suya30iynoaH3 ssw oiu0S3I 01 W2I SHOTS

011860

It'21e '03 n ••3WQ Q r e'l 'i 9 SHOT s'z ••s H siaayi essrro^ia 'aaNya6 a"luH.-'t-S9K-eOZ/'S28903-00I/I££SdS M09 '•SON03329'ai/dno it-ets/wai.ya'6198 awo 'aidNre£# ^sseeeiaa ••nw W'GS:'-^ ^s/sT/'eiitt zefiiloo ••viw SMyaaomMoaHO ssyu QIN0S8i 01 frezi stwas

011861

MID MASS CHROMATOGRAMS DATA: OCT1587 #1 SCANS 1704 TO 185818/15/87 16s39;68 CALI! CAL032587 S3SAMPLE: CASE 8019:BATCH4/'213-11 DUP/10.67GCOHOS.: 60M SP2331/'100-200e25./200-240@4/HCiLD 9RANGE; 01704,1850 LABEL; N 5, 2.5 QUAN; A 1, 1.0 J 6 BASE; U 20, 3

17667024.

8E371..A

1738383.4451.

7024.

332.899± 8.500

1838644.8888.

-1————r-17658544.

164835.

1738431.5181.

8544.

334.100± 0.500

1838540.7581.

—i -,——,—^—r-'——i——i—' [ - - -I-—--T——i——r~^—'——r^—'1728 -1740 17ee 1780 1800 1828 1840 SCAN1K;4''! 1"! f 9 - t 0 19-23 19!36 19:49 2@;@2 TIME

S98TTOMID RIC DATA; OCT1665 ttl10/16/87 16;36;88 , CftLI; CAL392587 »3SAMPLE: CASE 8919:BftTCH4/213-89/7.77GCONDS.: G0M SP2331/ie0-2e@@25/2e@-24S@4/HOLD 9RANGE: G1784-1850 LABEL; N 9, 4.8 QUAHs A 6, 1.9 J

1775

SCANS 1794 TO 1850

0 BASE; U 29. 3

1817 1S35 1844

1729!R;4->

1748ffi.^r

i7eef q - 10

1789iq-•"''"(

isee^•."st:, 182919; 49

184028^32

s 'as n 'asya o r e 'T 'i y iMWiia s'2 's H 'laayn Bssi't'ezio saoNbia6 oT3H/'t'a@t'z-ee3''fi2i)00S-eei/'i££Zds N09 s'soHoa

3ZZ-2/'60-£TS/t'H3iya!6T0S 3Sy3 '-3~}MfS£# <i.8SSb0193 !n93 0@S9£i3I ^8/'9I/8l

@s8i 01 MZI SNyos i# s09ii::io sylHO SMyaooiyHoaHO ssw QW

011864

S8S55-2- -g- —f ^ c3

m ui i— S 3— • m 's 3>— — is i/iID -4U1

>I»»^0;unmm " TO\ co o)03<n 3> o •• i» >— CT —t) IXi '3 0

£5^ro is om i a-r-ME" <s> \131 r\)

r-n '-. 0

:^g^§^i-n t-i -'J

-B. -•J1=1 ID 0 0o ra ]> i;-in -&. i— —<

33- ' l-l X1

2: n: "• ••— oI— 1-1 0» 0 E 1-1LD isi-n ui^

998TTOHID MASS CHROMATOGRAMS DATA: OCT1685 #110/16/87 IS;36;08 CALI; CAL9925S7 #3SAMPLE: CASE 8019;BATCH4/213-09/'7.77GCOHDS.: 60M SP2331/'100-2e0(»25/200-240@4/'HOLO 9RANGE: G1704..1850 LABEL! N 5, 2.5 6UAN: A 1, l.S J

1775

SCANS 1784 TO 1858

0 BASE: U 20, 3

1758158.1537.

7928.

332.899± 0,500

1747225.2143.

9792.

334.100± 0.500

1729l'-;.^

1746l'''.1^"

1769in . l l l

1780IQ.'.'i

180019;3K

182019; 49

164020;02

SCANTIME

MID RIC DATA; OCT160G ttl10-'16/87 17;08;S0 CALIi CAL032537 #3SAMPLE; CASE 8019!BATCH4/213-1@/'9.59GCONDS.! 60M SP2331''10e-200@25/20S-24@e4/HOLD 9RANGE; G17@4,1859 LABEL; N 0, 4.6 QUAH; A 0, 1.0 J 0 BASE: U 20.

SCANS 1784 TO 1859

A

1719 1747

1729IS: 4:''

1746i •"'."-'-

1769('"'• 1F)

1780iq.'>-!

1800iq-^R

182919; 49

184920; 92

S98TTOMID MASS CHROMATOGRAMS DATA: OCT1696 ftlW[^S7 17; 88; 00 CHLI; CAL692587 »3SAMPLE; CASE 8ei9;BATCH4/213-10/9.59GCONDS.; 60M SP2331/'109-290('25/203-240@4/HOLD 9RANGE; G1794,185@ LABEL; N 5; 2.5 QUAH; A 1, 1.0 J

SCANS 1704 TO 1850

0 BASE; U 20, 3

88.

259.077± 9.508

74.

328.098± 0.598

SCANTIME

698TTOSCANS 1704 TO 1850MID MASS CHROMATOGRAMS DATA; OCT1606 #1

18/16/S7 17;08;08 CftLl! CftL@92587 #3SAMPLE! CASE 8@19!BATCH4/213-ie/9.59GCOHDS.! 6aM SP2331/'100-2ae@25/200-24ee4/HOLD 9RANGE: 01784,1859 LABEL; H 5, 2.5 QIJAN: A 1, 1.0 J 0 BASE; U 20; 3

1747118.979. 133.

320.096± 3.586

139,

322.896± 0.500

SCANTIME

m m r- 013":..?.» 5So -slint-^ <n o-SJ Q 3»— 0IS131/1-%1 I^ m •• ^-%0.§§ayss,^Q &JLDOO

»—• •« 0

r^g 5

®K>01®§

WiZ

t~M •*»Q M

^SSUI I

(Jl \ '^ M QCS '».

f-l 'S LD01 S:'£5

GI CT 0 0§2 PSr' '"• " 2?^ o

U8TTOSCANS 1764 TO 1858N10 R I C

10/Q1/S7 13!S3;e@SflNPLE; CALIBRATION SOU I 1COHDS.; e.on £p233i/-ioo/'ieo-2oei.];.:5^'.:!\. :.;^., • ; ;RAHRE; G1704,1850 LnOEL: 11 0 ^ 4 . S I ' i i . i i ; , ; 6. 1.0 J 0 BASE: U 20, 3

! r"JU

i . . , i i i i ; i . . 1 . 1 1 1 ' ' i i i i

17£;U

1SS3 1815703 1717 1726 1S421829

172" 17'11-. i •: '

1800iq--"^

1S2019; 49

184920; 02

HID MASS aiROMHWRhtiS U,i!.,. "•lH/Hl/97 13; (•'3; I'll;! I;,:,! I- '::;

SAHPLE; CnLIBRATioN SOLU 1COHD5.: GOU CP233l/l?/1^u1-2fl^^:;•; 'L;-l.. -• !;„:!.RhIICF: G17H4.1S59 L.HbEl-; N 5, 2.L.l I.I.!,.|L ,,

Lil ;{! SCONS 1784 TO 1850

1 ; 1 .0 J 6 BASE: U 26, 3

^vv/^^^h^..,.„ .^±^.——;—————-^——————;——————^———

i- p ' 1 1 1 •i 1 ' • - '^vvNv_^_

379.

343.

328.B98± 0.506

;\ -.'•-'

1890iq.'-'R

1820IS; 49

1S43 SC.HN29;92 .TIME

^ g^ ^ ©g s^!-• ^j0 — c-Ls y?'^

'••;

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1<•-'

)L-l •]

':':; /; s,i

•r1" ^§ " s' '"U-1 0 •:

5 ^ <

<LU ^

'3 <?

" !© ':.

•< ;. o;-'

(1<;

<'..

.': ((..-••.(1 ...

^•Q"a^

'J'l'S' • -i:'J •"1:0 'T-i•r-* T-'

1—Gl 1"'.C:l .0:' 0"

-

0 Q C-Ji-n is •a:—' _J

r-'i ir'. '"•"I u"'•3: l-'i CO->3 3 "" •?; ';'1

C^ 5 CT S Si

CI •—' •:T S fl1_! IJJ .rt

i-':i r'- LS

|sSaa" ri S S 3S: -— 1.1-1 i—l Ct;

LLII:-:'u"'

iTl KiiSi 10'"••3 C?i:'"i(••"i

-H

®®caei••-' IJ~I

• " s-0c':'

-H

I'-j !;"-'

; r3^-

—i '•'. i-Jl l 0 i3 f^

•—' S -0 EI --i C'-i 0l— e:i l— ':••! u-'-l — -a: ':••< o:i= i--:i cs; 0- "'0 Q CL1 IJ'I -.S C"? 11 = Si_i »-< •3: e' r'-1-1 UJ -^i.i"i r- i_3L'-l (O ..S '•• l .

I ' -;— -»— -L-.' CT • r 1=' •:T^ - -1 '.'"I I—' 1J_

,»••

smioHid RIC DnTn; r ' ,; |u2ui til SCnHS 1704 TO 18501@/@2/S7 14i57;00 CHLI! C(iLa325S7 S3SfWLE: CftLIBRHTIOH SOLH 1COUDS.: 6811 SP2331/109/100-2e0@25/280-2-10e-t'-8RHHGE; Gl?e4,LS59 LABEL; N 0, 4.0 QUni!; H 0. 1 .0-1 8 BASE: U 29; 3

1737rt 9568.

1765

I 'i I •\

/ \ I \1715 ^ y •'„.. ^ _,,'•' •,,-.,__^ _ 1790 1808 1813 ^824 1834 _

17?fl 1746 17Gn i7S0 1803 1S20 1649 SCAN' •"- ' •"• 1 1 ' • : " ' { - - • • : " ' " ' ' " ' ' " • " - " ' !9!49 20;R2 TIME

M I D WiSS CHROMflTOGRHNS DAm: UCT6291 til SCHHS 1704 TO 1850li3-'i32/'87 14i57!£'@ Cr,LIi CiM-C325S7 S3SWI.E; CftLIBRATIOH SOLH 1COHDS.i 60n SP233l/lOel/l0£l-2^1ue25/20^-2-lHe.!.^!RnHGE; G 1704,1850 LABEL; H 5, 2.5 i3l..lftil! rt 1,. \.V J 0 EUSE; U 28.. 3

1738lv5.

(''..I \.

2S9.

'•••1f,f 259.077

± 6.588

^fY^-———^^^M/-^^V^V/V\^——t—-r"——'———i———ri———[-—-—,-——i———,———I—-———————IL-,

173S426.3294.

A453.

328.038i 0.500

^A/y^'1-—^AA^^VV^A/^^^^1728 17^3 17h9 17S0 ISSS 1829 1S4@ SCANi".,i-. f .- . . '— •- , ;" -.•-i.'-- K-i.-.c 19S49 2Q;S2 TIME

3nll £8^6 KF^bt -^.-ot ....-.•i-'i »^ • , „-;•.;., . . . ,•. iN935 8t-8l 0£8t SaSI US;I S3.'I Ut'ZI BSZI

"^^V^/.^^^^ ' ^-^^^^v^^—---^:^^ '-"1———————37V,--VV" -•-7'

60S'6 T9bU"£3S

'££Z .,^r '-6'aul

8£:ri-i_________• , I____1____I . . . . -. i.-.__._J____L___J____L_^-J____L-

"A/Vvv'V^ _/^W^- /W \ '^--^^^- -V/^^—"——fV^^' '^

UUS'0 T966 •e3S

•S09

e 'ee n !3sya a r e'l 'i " snnri9 s's •s N •• "13991 £ifi8t't'e^rs saoHya8./t'S!:it'S-G8?..-'SS39u3-00t/U0I/I££'3dS N89 •• "SOH03

i n"ios noiiyagnyo s3idnnsss zseseeiyj snyo easzssN ^s/zu/ei

13SST 01 t-921 SNH::IS Itt I93i?J.::iO ii;ijm.1 SH9a3019UOaH3 SSW QIH

011877

^ 8^8TTO• W

M I D MASS'C1-IROMATUGRHN-'; LmTn: nr:T0201 ftl SCAISS 1764 TO 185010/@2---37 14;57;90 CftLI; ?1.892587 %3SAMPLE: CRLIBRATIOH SOLH 1COUDS.: F.m SP2331/-100/ie8-2nu@25/20Ci-2')0e4.'aRAHGE; G17134..1S50 LABEL: H 5. 2.5 QUfti); H 1, 1.0 J 6 BASE: U 28, 3

17362571.

A'11 \ ^

/ \ )373.\ 11^J• 332. S991 . ' \ ± 9.5^38

\ 1 \.^ \ 1 \

i ••-... J \, ^. . - - ^1736321S.2^9- 3244.

\\S.

,( 1 A 334.10S/ \ ± 5-566

' \ 1 \• ! \ 1 \/ '\ / '.---1720 1740 1769 178S 18S9 132Q 1848 SCAN10..I--. i . - , . r ' . - •I1-:,'!-! ; - i , ^ " i q - ^ ^ l'5-^^ 20!02 TIME

smioHID R I C ! . „ ( ; , ; ... 1 . 1 1 ' . l i i l SCfiHS 1764 TO 1S5019/81/87 13!i33!en - . , . 1 . 1 ; U-.j&;::;;7 i;3SAMPLE; CALIBRATION SOLiI 1COHUS.: 6(iH SP2331/lHu/ien-2R&6S ;'L!. .:;"•.-! .;RHHGE; G17U4,1S50 LRBEL: H 0^4.9 L'!!.!!; , , 6. 1.0 J 6 BASE; U 20. 3

100.S-i ''"' 19552.

i11 '!I"'

i

1 l^ I i;''™i ,•••,"

i I !\i i / \i1 .i 11,n n

/ ''. / \ ^)7p? .IZl^-AS6— - • _ . - • ' ' • '''—-—.^l8^-. l815-^ 182q 1S42- "0

(0

j c<)..,....-...-.., _ .—.„._,-..„. _...^--.„.-._..-.,.... ^ ,.....-....-^———,———^———,———^———,———^———,

172n 17.1M h , . i.'SG 1890 1B2Q 1S43 SCftH) - • ' • • • • • • • • . . i • . • • • " • - iq-";K IS; 49 20; 62 TIME

988TTOH I D HflSS CHROt'lHTOffihIiL; i : , i T . ; . " . . i . - i - . i i H I SCiiNS 1704 TO 1858iM/m/SF ISii- '^inil 1 , 1 ! ; : . . : , , [ ;-.. -,:;;7 ;?3SAMPLE: CHLIBRHTIOH SOLU 1CTIDS.: CTt'l ?P2331/ln•;i/100-2e!'^^;•v^-.l'', - ! - • • • I •::F'HllCr: 01704,1858 L.HC.EL: H 5, ^^J i . i ! . . . ! . , . 1. I." J 8 BASE: U 2S, 3

:;:!,. .:•- • ; ' ^ 1 " 378.! ''i 'i[ 1.

\

:-••:< I I 259.07;i •, ± s.5Bei1 i

/ r 1 ' 1

/',/-' w'^H---- • ' .''•V'-^A^^^AS^^^^^^-':;- - - l r ; -.--, •••---;--•--,- • i , • • • • --•r———••———-i———;———i———r'———]——^

175.-:I1 L.' ^. ' J

i i . ' ; . n - 7'•;,'';;- 943.i'

[-'I I

j ^3^ ; i 328.898

/ !, ± 0.509

:.. ^ Z .., r .':;,r: .zl... -.-.:-. .:.: • • . "• 1 • / f ^^-A^^-^A^^^/V^--^172n 17..!Q i . . . ' . . 1783 1890 1S2S 1840 SCAM,.-.•, i - . . - - • , ,——:. 1^.01; i9;49 29;e2 TIME

0"1 <3:io IT.ICD 0C'40 -H

cnc:iCi:l U-J

c-'! isC-.1(•:«

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i-''i c:i=: C-4

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!{

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0

00 § =;-00 o o i—i i"'".' o. , !— e:i i— i"'"; inf—^ -z •" a: r-j 1:0^ '"'"' cc. a. —io 's (Xi i-i-i -.i_..i—i -i-

: c'"i —] : •n._, ti o r--(_• i-:i -<1-1:1 r.- i_;

:£-<_] l-l-'l !d u-. Q 1-3

TlCJ.•"i—.u

S88TTOHID NHSS C.HRi:iNHTOffiHNS n ; i i i . ; i . . i . . i ' : i l i . i l Sl SCHUS 1794 TO 1850IS/Ol-'S? 1^;(13!@9 C-LIs f.,!.^.::^'^ i;3SANPLE; CALIBRATIOH Sul-H 1CHHDS.; tUH SF•2331/'loEl• /lC.e-2a£l@25.•20^•^•!l :.;! .:;RHHGE; G17H4-1S50 Lnia.; N 5;,J.5 ^li^! ' i 1. 1.0 •J 6 BftSE; U 28, 3

.1 .::;•;] a.

S88TTOSCANS 1794 TO 1850HID RIC DATA; QCT0215 #1

CALI; CAL092587 tt319/03/87 3;87;00SAtlPLE: CALIBRrtTION SOLH 1COHDS.: eeM SP233l/190/'100-2@0@25/'200-240@4/8RAHGE! G1704-1850 LABEL; H Q, 4.6 WM: A 6. 1,8 J 9 BASE; U 28,

1755

SCAHS 1794 TO 1850MID MASS CHROMATOGRAMS DATA; Ui;re215 ftlCftLIs CAL032587 #318--'e3/87 3;S7!06

SAMPLE: CALIBRATION SOLN 1COHDS.; 60M SP2331/10@/100-200625/200-240@4/8RANGE; G1704..1S50 LABEL: H 5, 2.5 G'I-IAH! A 1, 1.0 J 0 BASE; LI 20, 3

175£162.1527. ISO.

259.077± 0,590

454.

323.098± 0.500

SCANTIME

(,.. 13 L.-i -~JK"' 'a r.J "••-!t--1

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173 -J L'"l— cn o-•J 0 S. r-is:3 r. ' •- Ln co »s* o— -n TO -•.J 3

S^3§§"§ er-i-> i:.

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l3 iSI

988TTO

MID MASS CHROMATOGRAMS DATA; OCT@215 <tlli3-'@3,-S7 3!@7!8S CALI! CnL@32587 »3SAMPLE; CALIBRRTIOH SOLN 1COHDS.; GBM SP2331/lQ0/103-200@25/239-24e@4/8RANGE! G1784,1S59 LABEL; H 5, 2.5 QIJAN; ft 1, 1.8 J 0 BASE: U 20, 3

17542733.23568.

SCANS 1784 TO 1350

17281 •-•. 1 -

1749 1769l '"i • < a

1783i'"i. •••'••1889iq-'il"

1S2019:49

18492@;92

t-i C3 ~~J 0m Li'i r" 1-1; :"o•• • m '•. i~•• •• t'J'1 '~1

e"i -•ii— IT] 1—1•_s Q I.'

•- i-i'i ro is'i— "Ti 'X'

5;aSS c-0 ,3 QO

^^= 00

0~ r_i

CT ir'" te-ta. l-.r,

'=' I - ' '

''.CO

}13C.J 0

-I-t

l.£i CO•• M '-b- QLD \'Xi

i r'-''I w

—I l-i-l'-i 03 3;-m :r

COi.coCO

3NI1N9:iS

SHSMSOt'SI

hp-eiOTt-i T

'-•:' t 008 T

ees •e T2.18'6££

St-Z

011886

3Nil £U-n£ bfibi -..-•bt ^ ••.-.'.Ny3S 0t-8t 0381 6031 68,11

0QS-U T960'33£:

! t

i____!____i ,. ! ^ ;,y^r-v-— . - / \_^^^-~ \/-,

ees'a T963'0S£

s '03 n s3sya e r a ' i ••i '•' i t r . ' i i o &•; 's N i 'myi essi't's.'.i? sBsnuy'•; •i-"•!i-"-!.]n?'/c,??!nci^--npii./mi/is:i:7:d? Hn9 ^saHni

T trios itoimagriyo !3idNnsst' ^0'?,^^ i , ' J ^•"r-:! eBsgQst. .is/'se/ei0S3I 01 t'O^I £|jy;iS Itt I""'"'!;''' ""ri! SlliiaTO.LHI'ln.'lll.^ SSHH i]IN

01188S

068TTONID HnS£ CHRUHATOGRhMS liiiii.; rii.lu:;;n| i,l SCANS 1704 TO 1856l^'SS-S? 4;i33i03 1..1.1; r,.i^-L-7 1*3SfW'LE; CHLIERHTIOH SOLH 1CLillDS.; 6eM ;.P2331/10£i/16u-2eue25/2GO-2^^-l "RHHGE; G17H4.1S59 l-!'il3El.: N 5, 2.5 Ul'i'il.l. ,( 1 , 1 . 0 J 0 BftSE; U 25, 3

. . f . l - •ilJ:.,:" 4836.

j \

S \ 1730( ! \ 2313:3.v i !, 19H4;3.

:-.' i \ A 332.939I • / •-, ± 8.580n / \/ \ / \

5 ]::;£:..

lOu.S- ^ j i1 '1 5176,

/ \

C , / '';

I1 i 179nI1 i 2582.

334 i1 "• 23432. 334.109i \' /'\ ± 6.508

/ ' / \'• •• ,.' i,

1 1 1 / \! '• / ':.

1720 17-i" 17^-. i7y8 1S00 1820 1840 SCANt ,-, ' -, < • , - — T : . • -.: -,-~. <,-i--i- <i"i. ^.-, •-ii-i - .•"<-~i "TTMr-

T68TTORIC DftTH: HPR2301 ttl SCANS 1 TO 29084/23/87 8;16!99 CALI; CftLS423S7 ft5SftMPLE; COLUMH PERFORMANCE m'f',CONDS.; ll-IL/SP2331/100-2e9e25/20Q-240@4/HOLD10RftNGE: G 1, 208 LABEL; H 5, 2.5 GUAH! n @ , l.e,J 0 BASE; LI 20, 3

i.o-j 11', 28832.

2,3,7,8TCDD

7G

ft") I ; 1. I

^ / \ 0/' ^59 \. . ' ^

.----_ __ - _ - . , . -_ . ^_--^, , ^ • ' \ _ . -,, .. „„ i ^ - i T - T r

5t3 l O i . 156 290 SCAHI;-*!"' • ".'• ?:@9 S;49 TIME

368TTOMASS CHROMATOGRAMS DHTH! HPR2301 iH SCANS 1 TO 20904•/23•/87 8; 16! 90 CftLI; Cft!-042SS7 it5SAMPLE! COLUMN PERFORMANCE MIXCONOS.! llJL/'SP2331/'109-20a@25/200-240@4/Hi:iLDl£iRANGE! G 1- 209 LABEL; H 5/ 2.5 Ql-lftH: 9 I . l.(3 .-I 9 BASE: U 26, 3

1BG1434.

.-„- ,. 77 10595.y6.9-i ^65. ; 1434-

3353. ,

^326 i l l 328.096I ;, ( t 8.5M

/ \,?& " \/A / i ; \

^.y_•^•.^_^,.^.-^_^/L-^-./ V __ v.-r^-^^-^ ,_ . . ^^--. -.. ^-. _^ — ^ - ^ ^77 1658.

189.0-, ^ [2fs• 1650.

c - r\' l\

322 p I 1 322.096| ,"i \ i 0.580

. , I /U• ^ 1 \ 1 \

^.•—__^.^^~~~-,f\I'•—^^r^-_^-••^..,llll,^.rll-.lf^ —•.ii.i—^--''"' —^ / ___ - \ ^\--—..^--. ., n i i ^ - .-.-—- -.-y -—'-. i^'--^--^ — -" ---", -

50 ibn 159 206 SCAHi - d H : : • • • . ' ! 5;5@ R;40 TIME

268TTOMASS CHROMATOGRAMS DHTn; fll f.:2;:Lil 1,1 SCANS 1 TO 28084/23/87 S;16!@B CfiLl! i::Hl..»3-r7387' 1*5SAMPLE; COLUMN PERFORMANCE MIKCOHDS.; lUL/SP2331/ie0-200@25/-206-240S4/HOL01@RANGE: G 1, 206 LABEL; N 5, 2.5 QWh A 1 , 1 .0 J 0 BASE: LI 20. 3

193S24S.

'9.4-, ^l76- 8256.

- \i32 .-;?9-;'4-: 332.099"-(Y"- i 1] ± 6.590

1\ i \J \. i V-——•I-'" ' ' 1 1 " 1 " ' 1 ' i 1 1 '.•.-•^•.••.:....^——-•—- --=p--~ —..J-—^-.-. . . . . , - . - , - i -i - •r......z, . ! : „ . , . ^ . . (

1631U377.

39.3-1 '''';^::•"^• 10488,

F6 I,5247. I

334 _. 37597. 334.180(" | ± 0.580

/ 1\ / '

_ , I '^1_V58 H;iu 150 299 SCAN

MID RIC DUTft; HPR2306 Itl04/23.'-87 11:11; 89 CALl! CAU3;23S7 {i5SftMPLE; CALIBRftTION SOLN ICONDS.! lUL/'SP2331/199-290e25/'29S-249e4/HOL010RANGE; 01794,1999 LABEL; N 6, 4.9 QUW: n 0.

17591.3 J 0 BASE; U 29, 3

17SG

SCAHS 1764 TO 1900

29680.

171F. 1811 i22 1336 1849 1871 1883

1759<fl-^7

1859-?»"!• Fr?

1996 SCAH29;35 TIME

iO0500•^•r-10

968TTO

SCANS 1704 TO 1900MID MASS CHROMATOGRftriS DHTH! API AII; ttlCftLl! CAL642337 S594/23/87 l l ; l l !@@

SAMPLE; CftLIBRATION SOLN ICONOS.! 1UL/'SP2331/109-200@25/'200-249@4/'HOLD18RAHGE; 01794,1900 LABEL: N 5, 2.5 QUAM: ft 1, 1.0-J 0 BftSE; LI 20, 3

17E02025.15257.

^•--—./ '\ ^^ -,/--'\. A /•v"- —-I-———-——I——————-I——————'f"'"——1-

.-- •.A .--•v -——A '\.—-\ .-V^"-' '"-r1S89 18501750

l"!^? ?P; e?

2072.

320,896± 0.580

2444.

322.036± 0.500

1900 SCAN29;35 TIME

MID MASS CHROMATOGRAMS DflTfti RPR23ub ttl04/23/S7 11 ill!00 CflLI; CftL@42337 »5SAMPLE; CALIBRATION SOLN ICOHDS.: lUL/SP2331/ie0-20a@25/29e-240e4/HOLDieRANGE; G1784;19e@ LABEL: H 5. 2.5 laiJfth'! 9 1, 1.0 J @ BASE; U 20, 3

17589761.74277.

SCANS 1794 TO 1908

3792.

332.699A 6.500

12832.

17S6654S.52816. 334.160

± 0.590

17591 «t",7

isee 1850M-S2

1309 SCAN23;35 TIME

368TTOMID RIC DATA: APR2307 ttl SCANS 1784 TO I96004/23-/S7 ll!40!00 CALI; CAL642387 S5SAMPLE! CALIBRATION SOLH ICOHDS.: 1UL/SP2331/100-200@25/200-240@4/HOLD10RANGE! G1704/1900 LABEL; H R, 4.0 BUAN; A 6, 1.6-1 0 BASE: U 29. 3

3-i ^F6 29440.

E'1784

!\: ; '^I •: l \

17.21 1733 • J '"--—•'' s—-.-.1.8137--. J-823- ,-1837- -SL ^ 1875 1891

'—i———i———i———i———[———i———i———,—-—-,--- - -j-——i———i———i———i———]———i———i———i———i———j1750 13013 1856 1930 SCANIR!^ i"!-1'' 26; ©2 29; 35 TIME

368TTOMID MASS CHROMATOGRAM3 DATA: APR23Q7 #1 SCANS 1704 TO 196004/23/87 11;48!@0 CALI; CAL642387 tt5SAMPLE! CALIBRATION SOLN ICONDS.! lUL/SP2331/'100-200e25/'200-240@4/HOLD10RANGE; G1704.1980 LABEL; H 5, 2.5 QUAHs A 1, 1.0 J B BASE; U 28.. 3

1759447.

2G.4-i 36!52- 453.

259 _ [, 259.077| I, ± 0.508

MAA^A/ ^^V^J^^MA^AAA^^u—;—i—i———i——IT———y-——,———i—L.—i———,——_^—i—^———i———i———,———^———,—i—i——L_,———i • • ^17571682.

08.0-1 ^i35- 171S.

•328 32S.098\ ± 8-560

/ \

•• ......•'••-- y f'V^ 'S. .J.,,' ''_____\ . ,, ._ - -.._ ,-, _ ,-—.,/•; . r ^^f"V^f^—^•^ / -V•' "• ' \ 1-A /S^^ /• /•• ' /'V--. ^

1750 lSt3@ 1858 1900 SCAN1R-"57 I-•'"-i 28; 82 20:35 TIME

006TTOSCANS 1704 TO 1990HID MASS CHROMATOGRAMS OATH; APR2307 ti-1

CALI; CAL042337 »5S4/23/87 11s49!SBSAMPLE; CALIBRATION SOLH ICOHOS.: 1UL/SP2331 /• 108-209@25/200-24©@4-- HOLD 1@RANGE; G1704,1989 LABEL; H 5; 2.5 QUAH; A 1 . 1 . 0 - 1 0 BASE; U 20, 31758

2046.15340.

•. • • -~ -- -<(~ - - - —••1859 1900 SCAN

28!35 TIME

2868.

320.096± 0,500

2548.

322.096± 0.500

106TTO

MID MASS CHROMATOGRAMS DATA: APR23U7 ttlCALR42387 ft5

SCANS 1764 TO 1998M/23/37 11;48;88 CALI:SAMPLE; CALIBRATION SOLN ICONDS. •• 1UL''SP2331/100-200@25/'200-24034/HOLD10RANGE! 01764,1960 LABEL: N 5. 2.5 QUAH: A I / 1.0 J 9 BASE: U 29; 3

17569623.73743.

1900 SCAN20;35 TIME

9632.

332.099± 0,588

1297G.

'334,103± 0.590

S06TTOMID RIC DATA: AFR2162 ttl94/23/87 9il0;00 CALIs CftL8423S7 #5SAMPLE; CALIBRATION SOLH. ICOHDS.: lUL/SP2331/'100-2@@@25/209-240@4/'HOLDieRANGE; G1794,1990 LABEL; H 0, 4.0 QUAH; ft 0, 1.0-1 0 BASE; U 20. 3

1760

SCANS 1704 TO 1900

1787A

27689.

1714 1734 1323 1836 1853 1866 1889 1891

1750IR-'V7

laudj '" i« •'•H

1350?fl:02

19S0 SCAN20;35 TIME

0

CO0pit

SCANS 1704 TO 1900MID MASS CHROMATOGRAMS DATA; APR21S2 #1CALI; CAL642387 #504/23.-87 9s 10; 08

SAMPLE; CALIBRATION SOLN. ICOHDS.; lUL/'SP2331/10e-2S9e25/280-240e4/HOLD10RANGE! 01704,1390 LABEL; H 5, 2.5 QIJAH; A 1.. 1.8 J 0 BASE; U 20, 3

17621919.14631.

rsooI'l-^

1950•?fl;02

1938.

320.096± 9.500

2316.

322.996± 0.500

1900 SCAN20;35 TIME

?06TTOMID MASS CHROMATOGRAMS DATA: APR2102 ttl SCANS 1784 TO 198904./23--87 9; IBi SB CALI; CAL0423S7 1(5SAMPLE; CALIBRATION SOLN. ICONDS.; 1UL/'SP2331/100-200@25/200-24@@4/HOLD10RANGE; G1704,1900 LABEL; N 5, 2.5 QUAH! A 1, 1.0 J 0 BASE: U 28, 3

17599193.70807.

1900 SCAN20!35 TIME

9216,

332.099± 0.588

12080.

334.108± 0.500

906TTOMID RIC94/23/87 12;99;00SAMPLE; CALIBRATION SOLN IICOHDS.; 1UL/SP2331/100-200@25/200-RANGE; G1704/1900 LABEL; H 0. 4,1759

DATA: APR230S ftlCALIi CAL042387 ?5

240@4/HOLDl00 aUAH; A 0. 1.8 J

SCANS 1704 TO 1900

0 BASE; U 20; 349920.

1785

1712 1724 1734 1883

1750m;^

1880r"-f;-";n

185828; 92

1900 SCAN20:35 TIME

106TTOMID MASS CHROMATOGRflMS DATA; APR2308 ttl SCANS 1704 TO 190094/23/87 12s89;TO CALI; CAL042387 #5SAMPLE; CALIBRATION SOLN IICONDS.; lLIL/SP2331/100-200e25/'200-240@4/HOLD10RANGE; G1704-1900 LABEL: N 5. 2.5 QUftN; A 1, 1.8 J 0 BASE; U 20, 3

17601798.

13G16. 1834.

259.077± 0.580

.A,'I''''''- .-'''..,.A.<''- ~^—^ /S^JV '\ Js/\/\ \,."l 1r ^'1————1————i—""1 ^ ' t"—-^——•-—t-———i——"-l-17593533.27172. 3568,

528.098± 0.500

•^^-^~\-^-'T—i11' ' • • \ "'~"\ iv.^-.i^^^^-——-..Y, -. -|V'- - — . -. <-i ^q-. ^F^y..y .f->i . --T>-T, -^

1750 180*3 1858 1900 SCAN!R!57 1S!-?H 29:02 20:35 TIME

306TTOHID MASS CHROMATOGRAMS DATA; APR2398 til SCANS 1704 TO 199904.-•23./87 12;e9:09 CALIi CftL042387 ti5SAMPLE! CALIBRATION SOLH IICOHDS.! 1UL/•SP2331./190-200@25.••'200-24^@4--•HOLD10RANGE! G1704>1909 LABEL; N 5, 2.5 QUAH! A 1, 1.8-1 6 BASE; U 26, 3

176010160.

76,7-j 79?87- 10160.

•••QQ ) \ 328.096,1 1 ± 0.590

_______________/ ^____ . ________________________________-^——^——i——i——r—'——•—"'——r-''"^ •""'——'—^"^—r^—i——r—' ——^——i176813248.

160.8-1 "F6- 13248.

•^22 I 322.896i' I ± 0.500-_u^_,___ •

17^ IWQ 1856 1980 SCANIR-P" 1 •'!•-"-! •?fi:ffi' 23;35 TIME

306TTO

MID MASS CHROMATOGRAMS DATA: APR2368 iti SCANS 1.704 TO 190004/23/87 12;09;OS CALl! CAL042387 ft5SAMPLE; CALIBRATION SOLN IICONDS.; lUL/SP2331/'100-200@25/290-240@4/HriLD10RANGE: G1704..1900 LABEL; N 5/ 2.5 QUAH; A 1, 1.8 J 0 BASE; U 20, 3

17589632.

75.1-, 75^59- 964S.'

/- ' ' \ 1785I 5316.

43127.332 _ r-. 332.B99

'i j \ i 8.500

\ , , kl\_____175712831.

0@,0-i "I96' 12848.

j' | 1786| [ 5907.| | CC:-~J-~f 1

334 | "T 334.100

' J A_^___/__^^^ _____________1750 ISO" 1850 1990 SCAN1.3; 57 la^n -?!3; @2 29; 35 TIME

OT6TTOMID RIC DATA; HPR2309 ttl94/23/87 12;37s TO CALI; CAL042387 tt5SftMPLE; CALIBRftTIOH 50LN IICONDS.; lLIL/SP2331/10e-209e25/200-24e@4/HOLD18RANGE; 61794,1900 LABEL; N 0; 4,0 6UAH; A 6.. 1.8 J 0 BASE; U 20, 3

1756

SCANS 1794 TO 1900

1733

50816.

1716 1832 1819

17561"-°^

-r——T"Iwi? 1960 SCAN

26;35 TIME

©

S <c

i^Sfr,": •• »-< ^ • -CM _1 -J ®i—«E3r-

i r'- 0 rt 3

3T6TTOMID MASS CHROMATOGRAfIS84/23/87 12;37s88SAMPLE: CALIBRATION SOLH IICOHDS.: 1UL/SP2331/108-2BB@25/200-RAHGE; G1784,1980 LABEL;.N . , 5 ; 2,

10369.78444.

DATA; AFT-:2399 ttlCALI; CftL@423S7 »5

•248@4/HOLD1@5 QLIAH: A 1, 1.0 J

SCANS 1704 TO 1968

0 BASE; U 28, 3

"T—• •~i*' "" r

19320.

320.836± 0.508

"^"• l•" i" >

13129.

322.896± 0.5B8

18QnI'-l.'W

1859-'O-Pl?

1908 SCAN20;35 TIME

HID MASS CHROIWTOGRAMS DATA; APR2369 til04/23/87 12; 37! 00 CALl! CAL942387 ft5SAMPLE; CALIBRATION SOLN IICOHDS.; lUL/SP2331/'100-2e0e25/200-240e4/HOLDlBRANGE; G1704;1900 LABEL: N 5, 2.5 QUAN; A 1 , 1.9 J 0 BASE; U 20, 31755

10112.78835.

SCANS 1764 TO 1900

10128.

332.099± 0.500

13184,

17837294.55519.

334.100± 0.500

1PU0 185020; 82

1980 SCAN20;35 TIME

MID RIC DATA: APR2184 ttlCALIs Cffl-042387 ft504/23/87 10;13;80

SAMPLE; CALIBRATION SOLN IICOHDS.; lUL/SP2331/ie0-20e825/2ee-24084/HOLDl@RANGE; G1704/IS00 LABEL: H 0, 4.0 QUAH; A @,1760

SCANS 1704 TO 1900

1.9 J 0 BASE: LI 20, 349216,

1713 1737

175S'"•";?

18UOi'"r'''i'i

185029; 02

1900 SCAN29; 35 TIME

3T6TTOSCANS 1704 TO 1980MID MASS CHROMATOGRAMS DATA; APR2164 #1

CflLIs CAL042387 #504/23.-S7 18;13;SSSflMPLE: CALIBRrtTIOH SOLH HCONDS. s lUL-'SP2331/'100-2eee25/'200-240@4/'HOLDieRflNGE: 01704,1900 LABEL; H^5 , 2.5 QUAH: ft 1, 1.0 J 0 BASE; LI 2B, 3

li'b!1812.14737.

i>/ - , /^^^A^-^/•S-\A/S^/^V '\^~-^>^^^/^^/-^-A-l————r i •

1836.

259.077± 8.500

3644.

328.098± 8.500

1758 1800i'"i.-'""i

18505P;Fr?

1909 SCAN23;35 TIME

3T6TTOMID MASS CNROMATOGRAMS DATA; APR2184 ttl SCANS 1794 TO 190864/23/87 10s13!09 CALI: CALS42337 #5SAMPLE; CALIBRATION SOLN IICONDS.! 1UL/'SP2331/'100-200@25/'200-249@4/HOLD10RANGE! G1704,1980 LABEL; N 5, 2.5 GUAM! A 1.. 1.0 J 0 BASE: U 28, 3

17619928.76781.

I n I '"'-""I"' 'I————I—————|—..->~T.|. . , . . n- i - j - . i i i i i i i , i f ill", i. ii ,11.

176012841.96919.

——1————'-—-T————'————'————I———1859 185819;-fl3 20:82

9928.

320.096i S.509

12896,

322.896± 0.508

1908 SCAN20:35 TIME

LT6TTOMID MASS CHROMATOGRAMS DATA; APR21S4 #1 SCANS 1704 TO 199904/23/37 1@;13:00 CALl! CAL9423S7 #5SAMPLE; CALIBRATION SOLN 11CONDS,; 1UL/SP2331/'100-200@25/-200-240@4/HOLD10RANGE: G1704,19@e LABEL; N 5, 2.5 QUAN; A 1 , 1,0 J 0 BASE; U 20, 31759

9494,72125.

175912656.96502.

' ^1 1—T———1———-T"

9552.

332.099± 0.500

12656.

334.108± 0.500

1750 1889IR-Fi? 19;W

185620:02

1909 SCAN20:35 TIME

£ev-i

s^

S£-r-(stts r~-

TOQC'-c»-« C^(Ta-IMC:!Q;—lQ- •a:•0:0

C?l^

gg

^ ( S — — — — — — — — — — — — — — — — - — — — — — — — — ~ ^ ~ ~

0 51—L 0^ ^CD o1-* g!Pm tSg

^& COpi!13c-

0 C& •"

SroSQ \1 53^0

i"SS•r

CO

a3

m

0

—i®

s,0»-iQ<ri

0 ••

P —*0 CS®•si-<M<S

1 •

s'- c^^z:"?d0 CQG& '^1-1

£2 ®Cf ©<M cn

^S"3wu3§ 8S

IS<sIS ,

ro03COi-t

f)''-!CO»-t

01s

i•s

»-<

i7>

TO

jCO ..'-"r-',

'")

-———————————————' ''t

K

•Tlg

y1

Ct-'\^

3T6HOMID MASS CHROMATOGRAMS DATA;

CALI;APR2319 ttlCAL042387 »594."23/87 13s 86; 0®

SAMPLE; CALIBRATION SOLH IIICOHDS. s lUL/SP2331/100-200e25/200-240(>4/HOLD10RANGE! G1704,1900 LABEL; N 5.. 2.5 QUAN; fl 1.

17599846.75242.

SCANS 1784 TO 1900

1.0 J 9 BASE; U 20, 3

9856.

259.077± 0.590

6594.

328,098± 0,500

1756("•'=;?

1899f~r'v

1850••^•ff?

1908 SCAN29:35 TIME

MID MASS CHROMATOGRAHS84/23/87 13!86;08SAMPLE; CALIBRATION SOLN IIICONDS.: lUL•/SP2331/'100-200e25/'20e-240e4-/HOLD10RANGE; 01704,1990 LABEL: N 5, 2.5 QUAH; A 1 .1759

DATA: APR2319 #1CALI; CAL942387 #5

54592.417441.

SCANS 1704 TO 1900

1.9 J 0 BASE; U 20, 3

54592.

320.096± 0.500

78528.

322.096± 0.500

1866l?;^

185020; 92

1900 SCAN20:35 TIME

IS6TTO

SCANS 1784 TO 1900MID RIC DATA: APR2305 #1CALI; CAL042387 #5B4--23/-S7 18; 42; 06

SAMPLE; CALIBRATION SOLN IIICONDS.; lUL/'SP2331/100-200e25/'209-24084/HOLD10RANGE: G1704,1900 LABEL; H 0, 4.0 QUAN; A 0, 1.0 J 0 BASE; U 20, 3

161280.

1787

1732 1884 18.14 1838 1349 1854 1867, 9

18-82 1892

1750IS; 57

189019; 39

185020:02

1900 SCAM20:35 TIME

MID MASS CHROmTOGRAHSe4-/23./S7 13; 96! 08SAMPLE; CALIBRATION 50LHCONDS.: llJL'SP2331/109-200@25/-200-240e4.. HOLD10RAHGE; G1704..1S00 LABEL; ^N 5, 2.5 QllfiH; A 1 , 1

10446.88268.

A

;i

175614180.16606S.!\

i• !

^ , . ..., J1759l".n;

D.4TH1 l lFRStMCi'iLI; Ciile^"^:'

I I I

\ 17845752.46162.

1 •"-.A'i\

"^ } '-.

,.7333.

5'r^312.A

/ ''.\1 'i

^ 1 \'•-.. /

J%0^ i ' ' ' '

til-7 ^^C:

.9 -J 8

;———

"'''

SCfiHS

BASE: 1-1 20..

1 . , , , 1

1764 TO 1908

3

194S0.

332.099± 0,500

1420S,

334.109± 0.500

1 , i . ....•i.- i |1358 1999 SCAN-a-m 2fl;35 TIME

MID RIC DHTn; i1FR23ll i,lC^LI; CHLS4^3S7 #5e4.-'23--'°7 l'?!?!5;na

SAMPLE; CALIBRATION SOLH I I ICOHDS.; lL!L/SP2331/-100-2ei0e25/200-24Si24/HOLD18RAHGE; G1794,1900 LABEL; N 0, 4.0 QURN; H 0

1757

17F;3/"\

SCANS 1704 TO 139@

1.0 .J 8 BASE; 1-1 20, 31E4352.

!718 1729 1742 1BH7 1818 1828 1841 1855 1867 1879 1S341758i i--,c- 185Q 1393 SCAN

20; 35 TIME

DhThii (-iFR2:3H ttlChLI; ?1^2337 £5

HID MASS CHROmTOGRAHS94.'23--S7 13; 35; 09SAMPLE! CALIBRATION SOLN IIICOHDS.: lUL/SP2331/-ie@-2e0e25/2Q0-240@4/HOLD10RANGE; G1794.1900 LABEL; H 5. 2.5 QLlHH: i1 1, 1.0 .-I

175310632.71616.

SCANS 1704 TO 1900

9 BASE; 1-1 20, 3

19032.

259.877± 0,560

•i"' —f " " " " ! •

6648.

328,938± 0.500

1358•••Ffi'r?

1900 SCAN20:35 TINE

386TTOMID MASS CHROMATOGRAMS DrtTft; APR23H til SCAHS 1794 TO 199S34-/23/S7 13;35!@S CHLI; CftLS4^337 ftSSAMPLE: CALIBRATION SOLH I I ICOHDS.; lUL/-SP2331/100-2e0e25/-2e@-240@4/HOLD10RANGE; G1704,1909 LABEL: N 5; 2.5 eUAH! A 1, 1.6 J 0 BASE: l-l 28, 3

54144.391804.

185071'l.fl-?

54144.

329.096± 9.508

76656.

322.936± 0.500

1900 SCAN20;35 TIME

HID MUSS CHROMATOGRANS OATH; nPR2311 ftlS4--23/87 13!35;0@ CClLI; CnL6423S7 ft5SAMPLE; CALIBRATION SOLH IIICOHDS.: lUL/SP2331.-'109-200e25.-'[email protected]; 01704,1906 LABEL: N 5.. 2.5 Wm: 0 1, 1.9 J

175510449.76299.

SCANS 1704 TO 1900

0 BASE; U 20, 3

1B464.

332.899± 0.580

13528.

334.10S± 0.5B0

190S SCAN29!35 TIME

SCANS 1704 TO 1980HID MASS CHROMATOGRAMS DATA; ftre23uS ttlCALI; CnLe-12337 »534/23/87 10;42;30

SAMPLE! CALIBRATION SOLH IIICONDS.! lUL/SP2331/100-230e25/26e-240@4/-HOLD10RANGE; G1704-1909 LABEL; N 5, 2.5 SUAN! A 1 1.9 -1 8 BASE; U 29, 31762

19347.74419. 10384.

253.077± 0,599

6624.

328.698± 0.500

1858••'a-w1908 SCAN20;35 TIME

5g6TTO

MID MftSS CHROHATOGRAMS DATA: HPR23S5 #1 SCANS 1734 TO 190904/23---87 10;42;@0 CftLI; CHLS42387 S5SAMPLE; CALIBRATION SOLN I I ICOHOS.: lUL/'SP2331/-100-2e0@25/'20e-240@4/HOLD10RANGE; G1704..1900 LABEL; H 5, 2.5 QUflH; A 1, 1.0-I 9 BASE; U 20, 3

176253312.

74.2-^ w155- 53312.

329 1 328.896" " j ± 8.500

•_!±_——]————;————,————1————p.——i————r-—.——i————,————j————I————i————I————I————^————l————,————i————i————^1762

7180S.103.0-, 526872. 71S08.

322 I 322.036j I ± 0.509

^ __________^ \_ ^ ________________________

1750 1808 1850 1909 SCOH1"." r-'---"-' ''ci'a-' 20:35 TIME

386TTOHID MASS CHROHATOGRAHS DATA; nF'r-:23n5 ttl SCANS 1784 TO 190904/'23--'87 10:42:00 CnLI; C:HLS423;37 S5SAMPLE; CALIBRATION SOLH I I ICOHOS.; HJL/'SP2331/'100-200@25/'200-240@4/HOLD19RANGE: G1704..1906 LABEL; N 5. 2.5 QUAH: A 1, 1.0-1 0 BASE; 1-129, 3

175910573.

74.7-i 7G922. WQS.

.~ \ \ 17SS( • 5936.

j 44363.332 _ I A. 332.093

j ,1' 'i ± 0.5B0

•^_________. ^ .\\- j .^T-.___________________^___^.^175914169.

180.9-j 102124. ^4^3^^

( \\\ ^

334 | 1 5'/'^' 334.100j I I \ ± 0.500

I . / \

• j \ ! \_^____/ _ s--- • /_^. --T—.____^____1750 1S138 1858 1900 SCANi".'-- i.-:i.';.i-i ••ia.w-i 2(;!;3ci TIME

OS6TTOMID RIC DH-m: HFR2312 (tl SCANS 1704 TO 199084.-23/87 14s 83; 83 CALI; CrtLE'42387 SSSAMPLE; CALIBRATION SOLN IUCOHDS.! llJL/SP2331/'100-2e0e25/20S-240e4/HOLDH3RANGE; G1764.1900 LABEL: N 0.. 4.9 QIJAH: A Q, 1.8 J 0 BASE; U 26. 3

3-, 1 53 552968.

c-

/' \\ 1J-S51714 1724 1739__/______~-—---_^-^^_ 1822 _ l g 3 8 _ 1859 . 1872 1892

1750 1899 1850 1909 SCANi"-" n.-"-. •-•rrfl-5 29; 35 TIME

TC6TTOID MASS CHROMATOGRAMS DATA: APR2312 ttl SCANS 1704 TO 19004/23/87 14;03s0@ CnLI; CHL842387 #5AMPLE! CALIBRATION SOLN IUOHDS.; lUL/SP2331/'10@-200@25/200-24e@4/HOLDieftNGEi G1704,1999 LABEL; N 5, 2.5 6LIAN; A 1. 1.0 J 0 BASE; U 28, 3

175938784.303953.

586TTOM I D MASS CHROMATOGRAMS DATA; APR2312 ttl04-'23/87 14:03:08 CALI; CTLS423S7 #5SAMPLE; CALIBRATION SOLN IUCOHDS.; lUL/'SP233l/'108-20e@25/2e0-240S4/HOLD19RANGE: Gl?@4,l900 LABEL; H ^ 5 , 2.5 QUAH: A 1.. 1.8 J 9 BASE; U 20, 3

21324S.1633940.

1760276992.2109869.

SCANS 1704 TO 1938

213248.

326.03S± 8.503

276992.

322.895± 0.508

1858•?fl;W.

1900 SCAN20; 35 TIME

MID MASS CHROMATOGRAMS DATA; APR2312 ftl SCANS 1704 TO 199804/23/S7 14;33!@e CALI; Cfil-842387 tt5SAMPLE; CALIBRATION SOLH IIICONOS.: lUL/'SP2331/100-2@0@25/'20a-24ee4/HOLD19RANGE: G1704/1900 LABEL; N 5, 2.5 QUAH! A 1.. 1.0 J 8 BASE: U 20, 3

17579868.76974.

17355627.43009.

9888.

332.899i 8.500

12S96.

17857333.54752.A 334,109

* 0.500

\

1750 1880 1858ia-•:;- )'-r--'i-i •''flsFr?

1999 SCAN20:35 TIME

MID RIC DATA; APR2313 ttl84--'23-"37 14;32!00 CALI; CftLe423S7 »5SAMPLE; CALIBRATION SOLN IUCONOS.! lUL/SP2331/10B-200e25/26e-240@4/HOL010RANGE; G1704,19@0 LABEL; H 6- 4.0 QLIftN: A 0

17581.0-1 0 BASE; U 20. 3

SCANS 1704 TO 1998

1715__1730 1817 1843T"

1875 1890

17591 0. C:"'

1850W.i-r''

386TTOSCANS 17@4 TO 1900MID MASS CHROMATOGRAMS DATA: APR2313 ftl

04/23/S7 14;32;00 CALI; CAL0423S7 #5SAMPLE! CALIBRATION SOLH I'JCOHDS.: 1UL/SP2331/100-200@25/200-240@4/HOLD10RANGE; G1704/1900 LABEL; H 5; 2.5 QUAH; A 1, 1 . 6 J 0 BASE; U 20, 31759

41325.303846.

1300 SCAN29:35 TIME

41344.

259.077± 3.588

2628.

328.038± 0.500

986TTOSCANS 1794 TO 1999MID MASS CHROMATOGRAMS OATA; HPR2313 #1

94/23/87 14;32!@e CALIi CALO-S2387 »5SAMPLE; CALIBRATION SOLN IIICONOS.! 1UL/SP2331/1B0-208@25/-20S-24084/HOLD10RANGE; G1704,1900 LABEL; N 5. 2.5 QIJAH: A 1 , 1.9 J 8 BASE; IJ 2Q, 3

1758212992.1S57120.

1758286208.2183070.

212992.

328.896± 3.508

28623S.

322.096± 0.500

1758^••^

1»3v^-^n

1850•?Pl!0-3

1999 SCAN29:35 TIME

tg6TTOMID MASS CHROMATOGRAMS DATA; APR2313 #1 SCANS 1704 TO 190804/23/'S7 14! 32; 08 CftLI; CAL8423S7 #5SAMPLE; CALIBRATION SOLN IIICOHDS.; lUL-/SP2331/l@0-200@25/200-24Be4/'HOLD19RANGE; G1704,190@ LABEL; N 5, 2.5 QIJAN: A 1. 1,0 J 0 BASE; U 28. 3

1 »"5616560.

78.9-1 79!?6' 10560.

I I 1784( 6141.v 45729.332 _ A 332.099: A i\

175613484.

100.0-, 10^94- 13536.

I I 17S47700.

5648G.334 A 334,100

/ \ ± 8.500

^ ,/ \ _________ ^ _ _ _ ^ _ . , ^ ^ ^ v ^ -/ ';•- ^ . - ^ . - _ ^ _ - _ ^ -^__^._1750 1898 1850 1906 SCAH4 rt- C-? 1 .-i . •-.1-4 •••ifi. {'v-i ^(5. '5C TTMC

986TTOMID RIC DATA: APR2163 ftl84..-23/87 9i43;09 CALI; CALe42387 #5SAMPLE: CALIBRATION SOLN IUCONDS.; 1UL.'SP2331/100-200@25/200-240@4/HOLD16RANGE: 01704,1900 LABEL; N 9, 4.0 QIJflN: A 8,

17661.0 J 0 BASE; U 20, 3

1731

SCANS 1704 TO 1909

1716 1728 1759 _1827. . 1S43 1854 ^ 1376 18801800 1850

••fl-fl?

3g6TTO

ID MASS CHROMATOGRAMS4.-23/87 9! 43:90AMPLE; CALIBRATION SOLN IUDUOS.; lUL-/SP2331/100-200e25/209-24Be4/•HOLD10ftHGE: G1704,1900 LABEL; H 5, 2,5 QUAN; A 1,

1766

DATA; APR21S3 #1CALl! CAL0423S7 »5

41920.305594.

SCANS 1704 TO 1900

1.6 J 0 BASE: U 20, 3

41929.

259.977± 0,508

2564.

328.09S± 0,508

1750i".^

isser-r-Ti

1859pa-fl?

1900 SCAN29;35 TIME

3mTOMID MASS CHROTOTOGRAMS DATft: APR2163 #1 SCANS 1764 TO 190804/23/87 9; 43! 08 CALI; CAL642387 #5SAMPLE! CALIBRATION SOLN WCOHDS.; lUL/SP2331/10a-2a9a25/208-24ae4/HOLD10RftNGE; G1704/1908 LABEL; H 5, 2.5 QLIflH; A 1.. 1.9 J 9 BASE; 1.1 20. 3

11 bb214016.

77.7-1 156^040. ^g^

329 _ / I. 320,0961 | ± 0.508

1766275456.

inn n 2038476. i-c.iccl@fi, 0-i A 2i'545b.

1\322 j I 322.036j I - ± 0.500

1750 1SSO 1858 1960 SCANIR;''? l^W 2i3;02 20:35 TIME

irnroMID MASS CHROMATOGRAMS DATA: APR2103 ttl , SCANS 1794 TO 193994/23/87 3;43;80 CALI; CAL8423S7 #5SAMPLES CALIBRATION SOLN IUCOHDS.: 1UL/SP2331/100-200@25/'200-240@4/-HOL010RAHGEi £1704,1909 LABEL; N 5, 2.5 QUAHs A 1, 1.8 ..I 9 BASE; U 20, 3

17639856.

78.8-j 75?36- 9856.

1 1791( \ 5681." | | 41338.332 _ / A 332.099

/ i n i 0.538

j [ ]\________I-—,-——-,————1_-—r ^ '•—i————r———i • I f ' • I————I————r-^—T°——"'I1 ' "• I———^ r "I I———1

176412454.

108.6-1 95191- 12512.

| | 1791/ 7149.( 52871.

334 j A 334.180I i / \ ± 0.500

• } \ A____1750 1830 1858 1900 SCAN1?^7 rrW) -20; 62 20; 35 TIME

?mToMID RIC DATA; APR2314 (H SCANS 1704 TO 190004/-23^87 15 s 62; 08 CALI; CAL842387 #5SAMPLE! COLUMN PERFORMANCE MI?<CONDS.; lUL/'SP2331/100-209e25/-200-24ae4/HOLD10RANGE; 01704,1900 LABEL; H Q, 4.0 QUAN: A 0.. 1.8 -I 0 BASE; U 20; 3

100.01 17!4 26560.

c2,3-7.8TCDD

1757

ftRIC_

' \h1738 / ' / \

1710 1728 . ^ " ' ' ^ i " '''•—'-—^ 1 24 1848 1859 . 1872 1894

1750 1800 1859 1303 SCANf R . ^ 7 ^•Wl •?fl!?2 20;35 TIME

3WTOMID MASS CHROMATOGRAMS DATA: APR2314 #1 SCANS 1704 TO 1903 :

04/-23/-87 15; 82; 60 CALI; CAL@42387 #5SAMPLE; COLUMN PERFORMANCE MIXCONDS.: lUL/SP2331/109-290e25/200-240e4/-HOL010RANGE: G1784/1980 LABEL; N 5, 2.5 QUAN; A 1; 1,8 J 8 BASE: U 28; 3

17591931.

62 6-1 14;?95- 1786 194E—-1 A 1684. 194b-I 13985.

A320 _ 1 / \ 320.896n ' [ • ± 0'509

1738 /\375. / V2331. J i ' | 1

,...\.^f-'^-\_^^..,-' i ^' „ , „ i V /•"- 'V /\^-—•'•^\/'—V^^/^^^AAAA^.^vA^^^/s^^A.^175S .-,j,g7111 1'0-- 7-249171^1 ^ .t-i.

100.0-1 "/T" 16736. 2356.

^ 'ft322 _ I 322.036

f ; | - ± 0.5001739 A \

AS-. ', / V \

.-.• .. •• ^^^ . / __^>^ ^1- \ / ______^i, J'-_^--^.'~^t.-.'\^^i^^-M^\^\f\——^^^^j^V^^"^^^^^-^^;-^/^^^

1750 1898 1850 1900 SCANi?-^ 19!'<n Sd;!^ 20; 35 TIME

MID MASS CHROMATOGRAMS DATA: APR2314 ttl04/23/S7 l5!02!00 CALI; CAL0423S7 1(5SAMPLES COLUMN PERFORMANCE MIXCONDS. s HJL/SP2331^100-2001»25/200-240@4/HOLD10RANGE; G1704,1900 LABEL; N 5i 2.5 QUAN; A 1..

17849526.71994.

1.0 J 0 BASE; U 20, 3

SCANS 1704 TO 1900

9536.

332.099t 0.500

11760.

334.100± 0.500

175018;57

188019; 38

185020:02

1900 SCAN20:35 TIME

^ ° S l=i S S^S ®m 1.1-11—1—3•• • m \ i-— .. 03 i.i-io -'J 1-1-1

•pi s•- yi :s; i: c:'a3^^iCT i.i.i m ca o" ?3 £-:'. -n xi

r— »- o re-x> d ?3

!IICT ms iI-:' 3

cn 'S' :

'-!} r'.'13''=>

':'^' CCi —'-1-1, ; Ki -•J'"" r^":' "••it—S -••J -i-"si

0 "T-'- 7.r" —ii— r-

o oE'"".'

I.,;. Qi-n i--1

^4.

^t0 M

MCTCT1-0010

i:C'cno

SCANS 1?@4 TO 1859i'HD MASS CHROMATCGRAMS C . i i i i . , ; OC.ruHE Sl18/91/87 13; 33; 89 Crii-Ii CnL632587 #3SAMPLE; COLUMN PERFORMANCE MIXCONDS.: £UM SP2331/ie0,/l£iCi-2Sai?25/2u£i-2-!ua4./SRANGE! G1704;185@ LABEL: N 5, 2.5 QUAHs A 1..

1S40 SCAN29! 92 .TIME

1764.

320.096± 6.509

2176.

322.036± 3.5@0

M I D RIC Ily-'ei/s? 2e! is; 00 i^W'LE: COLUI'IN PERFORHtilICE N1:";COIIDS.; 6MH SP2331.' 100/100--2(3(t@25'^i1-•;: !RUhRE; G1704,1858 LhBEL: tl 0; - i .O i l l , , ; ! ; ,

SCHHS 1794 TO 1859. , l n ; l u . l ! . , i l L ^ ,11nl.l; i. .. ':;L;7 ft3

1.6 -I 9 BASE; 1-1 29, 3ires

TCDD17S2

1719 ,-.1804 . IS 17 1S38

18S9< a - ic

18281^;4q

184S28; 52

M I D MASS CHROMA ruC,RnHS H , ! l i , . ^ I ' J l i n til10,-oi.'S7 29;lS!ee r-;,l.u r,,i i.:yS«7 a3SHNPLE; COLLIMH PERFORMANCE HI:";C i i l IDS.! bOM SP2:331/lMel/l&^-2@9lil2?••;•l-"-l- : l i . • I ;';PhHGE: dl7ei4,lS59 LnBELi H 5, 2.':. r i i , , i i ; , , 1, 1.0 J 0 BASE: 1-1 29.. 3

1733885.

SCANS 1784 TO 185@

dUIi 60S0Z et^Gl :3t;-ot .^•t^ • - ' i - ' . - . t - . , . -1tTOS Bt'81 03ST 6981 98.'1 n^ ' I Eit'^l

\

aes's TiOIat'SS:

8S'@ T60'Z££

•£8S;^: - .-•33be ?ez^ic 'ei.7 n ••3wa e r e ' T • i n inyfiLi e's •s n naayi essi^a^io ;33nya

e/t?ltl-3-6Li;-SS8)Ei02-0@t/OOT/I£S£dS M09 "£01)03KIN 33nyNaoda3d HMrnoa 'aidNys

Sft .ISS^bO-iTO U'K'3 eiSiSISQS 28/-IS/9Ies8T 01 wi SHyos itt CITIH-LOLI :yiyu sNyaarnyi.ioaHo ssyn OIH

01195C

XI 0 I-l'l —'• 3X;' 0 X- d 1-13: 3: 3 ••, 0[T.I 0 -13 Sim 1.1-1 r— i-^) ?3— • rn s 1-1

"• " 1:0 oir-i -Ji— 0-1 o-..i o o i—Gi C1-"

t'^^03 r-.;ir-n IAI TJ 0is tAi m © _,— ?3 vn

"••• "'1 >»»i—— o 10r- o ."a /«.en o 3 03

— © o _io m ^ ^^s 0

•s11'"*13 .3 ;<- tSr-.'i-n. i-nco r-iis.

'3 O 0s:' i r; rE? r;-' i" ^1

• nil

cc' r" - 1.3 i2> i^.t,;. 0

i;.n r-.;.^' -" as

7-..1CT —

",_ S

^h.-' S:13 '.n

-.J(»? Gi

-fr

SS6TTON10 MASS CHROt'lftTOGRAHS DATi-i: OCT62U2 Sl SCANS 1704 TO 18581H,-'02/87 15;27;e@ Cftl-l! Cft'-S32587 S3SAMPLE; COLUMN PERFORMANCE MI/iCONDS.; 60M SP2:331/100/109-2e@@25.-'20Q-240@4/8RHHGE; G1784,lS5i3 LABEL; H 5, 2.5 QUHH; H 1, l .H J 0 BASE; U 29, 3

17784S78.

4P786. 4920.

332.039± 0.599

334.1S@± S.59@

SCAi,TIF'E

DATA; uc'rai'az ftiCAL I; CAL992587 #3

HID I'lRSS CHROMATOGRHMS19/02/87 15;27;60SAriPLE; COLUMN PERFORMANCE HIHCONDS.; F.W SP2331/160/l@0-209@25/200-24a@4/8RftHGE; G1704,185@ LABEL; H 5. 2.5 m-lnN! A 1; 1.9 J 0 BASE; U 2Q, 3

17S1105S,940S.

SCANS 1704 TO 1S50

^.-, ltl.3t.,

952; 9^s• 1063.7333, / i

A\ /1' \ • \ 328.096/ \ p, / 1. ± 8.599

1735 | j-1 •••-,.185.1222, i 1 /i 1 /

/ • /S. / \ /

' i ' 1 ' 1 ' ' 1 ' 1 i f '1752 1?8!r^n l^c4.S37@: IT4- 1394.

;1 .•' 1

1\ • /i' 'i • i 1

/ \ • / i 322.036; I .'-'•., i1 \ t 0.590

1737 1' 11, / S/ \250. ( / '1842- ! \ I

• .-"••.. / \ /-/ •••; '•'. /i \ ' • '-/--.".. .•".---., r-' '.-, / ',, ;•

i ( n "- I- - ] - i - j I 1 ' [ •" ' 1 ^ 1 | r i

1728 1746 1769 1780 1809 1829 1S48 SCAMir' . , i ' - ' -.-...— •q . i - ' i '".•T-. ••s."i- 19;49 2n;£i2 TIME

i^

" . /•i..^/'..'\^^. .-^~^;.,.,J'\. ^--vJ" /-,

I\'...^ -- -•-• A -. /'--'"r ^—-—-'•• ~-i /"-.-. ••- ^ -i

MID RIC10/63/87 2; 37;08SAMPLE: COLUMN PERFORMANCE my-,COHDS.: 60M SP2331/'100/ie0-2eae25/'200-240i?4.''8RANGE; G1704.1850 LABEL: H 9, 4.0 QLIAH; ft

DMTA: OCT6214 #1CALI; CAL@32587 #3

SCANS 1704 TO 1850

1_886 1826__ 1836 1844

172Si.-.. --. 1740 1769 1780< .-•. •i^,

1800fq-iF:

182019:49

184020:92

Al^1005

0

SCANS 1704 TO 1850MID MASS CHROMATOGRAMS DATA; OCT8214 »1CALI; CAL032537 »310/93/87 2;37;88

SAMPLE: COLUMN PERFORMANCE MIXCOUDS.: 60M SP2331/189./100-200@25/20e-240@4/'3RANGE; 01764,1850 LABEL; N 5, 2.5 QUAH; A 1, l.@ J 0 BASE; LI 20,1782

6640.58359.

SCANS 1704 TO 1859MID RIC DATA: OCT6218 #1CftLI; CAL692587 »31@/63--'S7 4s 39; 68

SAMPLE! COLUMN PERFORMANCE MXCOHDS.; 60M SP2331/10S/ieO-28S@25/2e9-24£i@4/8RHHGE: G17@4,185@ LABEL! H 9, 4.6 QUAH; ft Q, 1.6 J @ BASE; U 29,

1785

1763 1717 1738

18394.

1824 1836 1844

172131' '.,1^

1749 i7eei q - m

1788lq.'>"

1S28 1S40 SCftH19;49 28:92 TIME

SCANS 1704 TO 1850HID MASS CHROMATOGRAMS DATA: OCT6218 #1CALl! CAL992587 fr31@/@3-'-87 4! 39; 98

SftflPLE: COLUMN PERFORMANCE MIi<COHDS.: 60M SP2331/ie0/iee-2@0C!25/'200-24>3e4/8RANGE; G1704..1850 LABEL; H 5, 2.5 QIJAH: A 1, 1.0 J 0 BASE: U 26,

178S1185.11125.

3^6TTO jMID MASS CHROMATOGRAMS DATA: OCT0218 #1 SCANS 1764 TO 1858IS/BS/e? 4839;@0 CftLIs CAL692587 #3SAMPLE; COLUMN PERFORMANCE MIXCONDS.: 6@M SP2331/'100/'100-2a0@25/200-240@4./8RANGE: 01784,1850 LABEL; N 5, 2.5 6UAH: A 1, l .@ J 0 BASE: U 29, 3

17845993,

84.2-1 53b3f. ggg^

1757 I I332 . 2760- / \ 332.099

2.b^3•J• /' \ i 0,500

17857898.

108.0-1 68256' 7136.

1755 / \3712. / \

334 34849- 334.100/V, ' / ' ± 0-580

^ ! / V I \1728 1749 17eS 1760 1808 1829 1849 SCANlfi-4- j I R - R f i 19;lFi 19;23 19S36 19;49 20!02 TIME

396TTOl - l in R I C I lu ' ln : 1 . ' : ! ' . i:....-'2 i , l SCHtIS 1704 TO 1850

SntlPLE!'COLUMN'FbRFiiRHiinCE t'll;;COtlUS.! £0n SP2331. l£i0.'10Q-200i:::25/^Ou -W.^ •^RnHr;E: r,17a'L185U LuBEL; I I 0, 4.0 i i ; ' i , ! i : i , n , 1 . U . J a^_BH3E: U 20, 3

i m . i - i - -i1* 25792.

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17?n 17 in i , - ^ lyau i890 1S28 1840 SCAN• •• • ' ' ' • ' • " • ' l?-.!^ 2B-@2 TIME

F96TTOH I D 1'lnSS CHRi:i|lnTCir.:|;:i'ltl3 [JHI'H! Lii::iu502 ttl SCANS 1794 TO 185Qie.'05."S7 4;33;iJ!3 C,,L1; Cnl 032587 tt3SHtlPLE; COLLim FERFORt'lnUCE HI;;COUDS.: e9H SP2331./l^M.'lUO--20n@25/•£i^i^-24l3li!4./flRHt'GE; G 1704,1850 LHBEL; H 5, 2.5 QUAil; A 1, 1.8 J 9 BASE; 1 1 2 0 , 3

17SS1786.

-; 17K lbF'• 1786,1494. / t.

121U5. / I

i\ 1 \i .1' 'i / \ 320.095

i' \ '._ i' '., ± 0.599

1740 ,11 \ I | ^362. / '., „•• \24^-, \ / \', i i, 1 i/ \ / \ ! \

1- ' '"' ' 17871753 2826.ISP9. 20053, .-, .-

""1 15302, /l-. 2926-A n/ 1 /: _ I , ,' I. 322.S36i' 'i ,"-', -..•'• 'i ± S.580

1742 / \ / \^. / \ /

¥^' 1 •'. 1 \

172n 1748 17C.S 17QH 1809 1820 1840 SCHH1-...1-. lo.^r f ^ . i n Ki.-- I Q , W i9;49 2g;fl7 T^E

^96TTONID MASS CHROI1nTOGRnl'lS DuTu: Ui.:Ki5y2 ftl SCANS 17S4 TO 185ie-85-'fi7 4;SS;SU C,il I; i:i'.l.i;!32587 )l3SAt'lPLE: COLIJMH PERFORnnHCE HI;.;corns.: GOM spsssi/iau.'iso^ea^s.^es-^^ue-i-'sRnt)QE: i'.17i34,lS5n LfiBEL; H 5, 2.5 QUHH; H 1, l .Q ..I 6 BASE; 1.129, 3

178591318.82093.

^ \2 .

ICO.O

".• 9346.

„.. 1\[ i .Jb ] |4595.4ri2lM. \ 332.699

,' ! T P.,?™A n./ \. / v17S616948.len20- 10976.

„-,. 1 \b049. | 'iEa;0- | ^ 334.100/ '•, ' ; 'i ± 0.58t3

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1720 174U 1769 1780 1806 1826 1840 SCANi"- • • " • ' ~ •^ ' •"" ' 1 •""••"' <q.-"- !9;49 2S;62 TIME

?96TTOM I D t-lnSS CHROHATOGMlNS I'nTu; i . i . l ' i r i l ? ' ,.1 SCAIIS 1704 TO 1S5S10.-e5.S7 15!ll!&9 Cnl.l; i..,,l CJ^S7 K.SAMPLE; COLLW PERFORMANCE MI;::CUNDS.; bOM bP2331/iau/10£i-2UUii'25''2ULi-2-tWl ..{RftHGE: G1704,1S5@ LftBEL; H 5, 2.5 rimil; ( ; 1, 1 . U . J 0 BASE: U 2@.. 3

179SQ~'-~fUJ.-J i

31.7. ^P9- 823.

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32M ,•-',.-; / 328.096/ ^ j \ ± "•5(3-'3

1758 /' '1 / \104. ,1' 'i ,/ \736. i' \ / \-A'-'Y, / \ / \... ^• . •^" /-,. —^—^^^^ \^_ __ VNAA^A/XA^^X^.^. ^

' 1 "- 17931097.

l O O . O - i 13819- 1807.n^ ^. ^J^- \"f f ^

323 _ ^!\ ^ I 322.096/ '\ j \ ± 0.503

1754 / \ f S1^4. / \ ./ i,

^' ! \ / \1726 17-ifl l i ' ^ U l?L;t) 18U9 1828 1849 SC9H) • • i - r • • " - r . . . i . • - • • • • )1;';F; 19549 26:82 TIME

(•IID MASS CHROMHTOGRnNS rii,Tn: i:n::fn;Jl7 f t l SCfiHS l7@4 TO 185010/05--37 I S s l l s e a Cni-1; i;,,L."32537 S3SAMPLE; COLI..IHH PERFORmHCE MI;;CONDS.; fW SP2331/109-100-200@25-'2un-24a-:.1/3RfttlGE: G 17S4,l;:;5u LABEL; H 5. 2.5 C!UH|I: n 1, 1.0 J 9 E;RSE; LI 20, 3

173£4272.46563.

;\4272,

1-2 \ly7 ' ' - / \ 332.039-a^u. ; ' ± 0,580

A \./ \ / v17965099.56002. „,.„-1 n

-/1 / "\^. ' l 334,180',;A ' | \ ± 0-598

172Q 17'IEi l^ r ; ' . ) 17HU 1800 1820 1S40 SCANi.;.. 1-. i . , ^ - ) , ; , , i . , .^ i.i.-.i-; )q;49 20S02 TIME

?96TTOMil.) I? 1Cie./05-/B7 15 i l l ; 69SWLE; COLI..II-IN PERFORIlnUCE HIrtCOHDS.: 60M SP2331/lU8.--lU(j-20H@25/2M-.;'l(J^l..iRHHGE: 01704,1556 LhBEL; N 0, 4 .0 Q l i . i i l i i ; 0, l .n J Q BASE; U 20^ 3

1796h

SCHHS 1704 TO 1S5B

l,7i

1"-' H i"'I U :1 1823 1834

17,:'U 182019;')S

1S4628:02