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~ p x i S 3 -d M o n s a n to 7 di^C i MONSANTO COMPANY / DAYTON LABORATORY / DAYTON, OHIO 45407 __________ ESC/DAYTON_______________ (Department/Section) ______________ANALYTICAL_____________ (Type of Report) c- `a a ' I oo r. n A N a o CLOU Q_ <D L_ JO O O CO REPORT NO. : MDA-570 JOB/PROJECT NO.: 484.4340 DATE: 18 January 1985 PERIOD COVERED: TITLE: ANALYSIS OF WIPES FOR 2,3,7,8-TCDD . AUTHORS: R. W. Noble ABSTRACT: Wipe samples from th e N itr o P la n t were ana lyzed f o r p o s s ib le c o n c e n tra tio n s o f 2,3,7,8-TCDD. The r e s u lts o f these analyses a re shown in t h is r e p o r t. -z < <V1 Ed 05 o rL*O. 1 < Q 22 2o s o05 A*, u TECHNICAL APPROVAL: & C /***>* P. L . Sherman S r. Research Group Leader APPROVED BY . - _____________ R. F. Ivory </ Environmental Sciences Center Service Project Manager APPROVAL DATE: y-'7- RESTRICTED DISTRIBUTION: (see over) O COMPANY CONFIDENTIAL This d o c w e n t is the property of Monsanto Coopany and the recipient is responsible for its safekeeping and disposition*. It contains CONFIDENTIAL INFORMATION vhich Bust not be reproduced, revealed to unauthorized persons or sent outside Monsanto C o ^ a n y without proper authorization. CONFIDENTIAL C10904 SUBJECT TO PROTECTIVE ORDER. DOCUMENT CONTENTS Page Cover S h e e t ..................................................... 1 Document Contents............................... 1.............. 3 Report ......................................................... A Document Inventory Form ......................................... 11 Sample Receipt F o r m ............................................... 12 Chain of Custody F o r m ............................................. 13 Analysis Request F o r m ..............................................16 Monsanto Notebook Pages For: a. Extraction/Preparation 17 b. Analysis/Data Reduction .............................. 20 Instrument Logbook Pages ....................................... 23 Computer Output and Chromatograms .............................. 29 Additional Documentation ....................................... 154 SUBJECT TO PROTECTIVE ORDER C10906 ANALYSIS REPORT FOR 2,3,7,8-TCDD IN NITRO SAMPLES ! INTRODUCTION 1 On 1 Nov 84 thirty-five wipe samples were received for the analysis of 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD). For internal purposes, the samples were assigned MRC Log #1-84--11--01--02. The samples were analyzed according to the September 1983 EPA Region VII method "Determination of 2,3,7,8-TCDD in Soil and Sediment". For quality control purposes MRC Method #07-QAQC-R3 was followed. Briefly this method requires that for every set of samples of the same matrix type a replicate sample, a low (9.6 ng in this case) spiked sample, a high (96 ng in this case) spiked sample, and a method blank must be analysed. PREPARATION AND ANALYSIS (WIPES) The wipes were spiked with 24.0 ng of carbon-13 labeled 2,3,7,8-TCDD and 9.6 ng of chlorine-37 labeled 2,3,7,8-TCDD. Then ten grams of washed anhydrous sodium sulfate was added and the samples were stirred, allowed to stand and stirred again. Samples were mixed again immediately prior to addition of extraction solvents. The extraction process involved the addition of 15 mL of methanol (all solvents are Burdick and Jackson "distilled in glass" grade), stirring and the subsequent addition of 150 mL of hexane. The samples were then shaken for one hour on a wrist action shaker and the extraction solvent removed. The solvent was then successively extracted with 50 mL of water, concentrated sulfuric acid (until clear), water, 20% potassium hydroxide and water. The hexane was then dried with 10 grams of anhydrous sodium sulfate. Each sample was then placed on the head of a mixed phase column consisting of (top to bottom) 2 g of silica, 4 g of silica plus 40% sulfuric acid, 1 g of silica, 2 g of silica plus 36% potassium hydroxide and 1 g of silica. The column was eluted directly onto a column containing 2.5 g of Voelm basic alumina. The alumina column was first eluted with 10 mL of 2% methylene chloride/ hexane (v/v) and this fraction discarded. An additional elution was made with 15 mL of a 50% methylene chloride/hexane (v/v) solution to elute the TCDD off the column. All samples had 50 uL of dodecane keeper added to them and then were concentrated under a gentle stream of nitrogen and submitted for GC/MS analysis. The GC/MS analyses were conducted on a Hewlett/ Packard 5987 GC/MS instrument. The analysis was conducted using a 60 m SP2330 capillary column. The mass spectrometer was operated in the selected ion monitoring mode analyzing for ions characteristic of both the native (unlabeled) 2,3,7,8-TCDD (m/z 257,320,322), chlorine-37 labeled 2,3,7,8-TCDD fm/j^2jL^..yiaqd carbon-13 labeled 2,3,7,8-TCDD (m/z 332,334). I~ DENTIAL o,-,?H?JFCT T0 protective order. C10907 STANDARDS Standard solutions were prepared from standards that had been cross validated with a standard provided as a check sample by the EPA. Concentration of the internal standard conformed to the levels specified by the method. RESULTS The results of the analyses are given in tables 1-3. The tables also give all pertinent QA/QC information. SUBJECT TO PROTECTIVE ORDER. OOAnrj Aj. C10908 Tao data report mcuvTo cm , [wton labowtqry l OC d i r * : SPZ30 BF WTIVfi .973 PCStfKKTEi l.aa RW.E KKFB OtAtt ETO in m w OLEAH WXT FPp TCOO 0.1. SLR ANALYUC*. 320 332 X DATE T ilt 322 334 MX 320 322 257 328* 332 334 N LAPILL IA L fi^ F ia 18 LAWFH.L 18 L LACFILL 1C LANOFIU IC P LAKPILL 2 t AWFI |. 2 H LCF1U 3A LA<FILL 3A `JKF1UL 33 LA K iIU 3C ICQFIUL OC L IfiWFJU. *4 1AWTFIU AP LOEFILl 48 H LANOFILL 1C LACFIIL 5A LAWFILL 58 1U FU L W BLA* J J J J J J J J 0 J J J J J J .1 J 0 .1 J ec 10.410 BC 10.210 BC it . r o BC . 10.020 BC 10.630 BC 10.250 BC 10.410 BC 9.9 BC 10.150 BC 10.010 BC 10.770 BC 10.5 PC 10,400 BC 10.290 BC 11.020 BC 11.5 BC 10.110 PC 10.610 BC 10.050 BC 10.000 Kt 7.31 9.87 1.62 2.23 .78 9.19 .16 .14 .23 .83 1.20 K) m 9.41 .16 W NO NO .14 IW05 -- 11/CS -- 11/OS -- 11/05 -- 11/05 -- 11/05 -- 11/05 -- tl/0 5 -- 11/05 -- U/05 -- 11/05 -- 11/05 .13 M/OS .17 11/CS -- 11/05 -- 11/03 .08 11/05 .09 11/05 .09 11/CS .06 11/05 0100 .88 0120 .82 0140 .83 0200 .81 0220 .80 0305 .76 25 .81 03<3 .73 0405 .86 0*25 .81 0510 .76 0529. ,79 0549 1.26 0609 1.18 0629 .83 0714 .76 0734 1.10 0754 .90 0815 .72 0835 l.U .81 99. .79 100. .80 96. .81 97. .82 98. .81 99. .84 101. .81 101. .87 99. .82 101. .83 107. .83 102. .83 10?. .82 96. .83 104. .84 112. .85 112. .84 IIS . .84 110. .83 103. 9300. 10543. 6*21- 188778 160080. 197666. I ri6 9 9 . 331687. 157832. 110569, 91398, U3793. 598907. 721294. 318020. 155151 136036. 169062. 97976. 120374. 51704. 178032, 155214. 190628, 114939. 143415. 64206. IA5743. 126212. 153195. 15714. 20590. 12100. 169S73. 143702. 177596. 414889. 512623. 213577. 133019. 113*09. 135802. 7138. 9792. 5905, 149050. 124292- 153953. 7014. 8151. 4040. 1A53S4. 125136. 151916. 11163. 13833. 10304. 1*5463 122432. 148933. 77784. 36350. 17421. t04397 83700. 1003. 59021. 74343. 34156. 146212 122725. 1*7721. 8896. 7064. 8719. 1642?* 137733. JWM9. 9468. 7995, 0. 132433. 117207. 142756, T 513920. 618539. 290935. 154220. 177707. 1529*5, 8990. 11831. 7781. 169937 130522. 155119. 7967. 7715, 0. 286380. 221556. 260291. I 8272. 9185. 0. 250033, 212*45. 251975. 1 5359. 7441, 0. 212569 (66153. 198016. 4901. 4314. 0. 233633. 19X55. 232916. I CCRRECTED FOR OKTRBUTICN BY NATIVE IO T I O JSTM fT .009 OF R/E 322) mite coesi l i ISOTOPE RATIO (VT CF ACCEPTABLE RA* Vi : 6CGFACY CUT (F fiCTfPTAaE UtCE IW n U H-AMi PIARTI. SCAN R=SPARATE lilW IH fi UTRJOP W XM TEtIfERLW ) fb* hlq PL6MC L.JW ATM TCOO SPUES NDdflT ffTTECTED a-OTtCTT LIAIT XK# FILEW -TCODO? SUBJECT TO PROTECTIVE ORDER nnr.r C10909 TCCn TA REPCRT i tf.'T O O W U ff. CAYTi* LABORATORY 'T ^ u t l .o ^ n sccou"."sproc RF NATIVE: .7 *1 . ofSRCSSTf: 1.023 -PLE IWER CRAfS SUS ETTR tffT PPB ANALYTICAL 370 322 t TO CLEAN iiy r Tam D.L CATE T ilt 372 334 ACC 320 .322 257 328+ 332 334 N .SNKILL 68 J .A ffifia 6 H J .i F ia 7A J -SFIU 7B J AFILL 7B L J .ACFIU 7C J TO SITE 1A l TUS SITE lAfi J TO SITE IB J TO) site ith J TO SITE 1C J TO SITE 7 J TO SITE 21 J TO SITE 3A J TO SITE SB V1 TO SITE * J TO SITE 4A J TO SITE W J TO SITE 58 J TO SUE 5C J TO SITE 6 J TO SITE 7 J TO site e 5 J BC 10.6 BC 10.710 BC 10.7*0 PC 10.350 PC 10.S90 BC 10.CT 8*. 10.610 BC io.ro BC 11.410 BC 9.9 BC 11.0*0 BC 10.400 BC 11.110 BC It.MO BC 10.320 BC 11.660 BC J0.9S0 BC 11.5M BC 11.5 BC 10.290 BC 1 0 .*30 BC 10.300 BC U.060 DC 10.000 .11 _ 11/05 8.19 -- 1W .11 -- r./Cfl W .10 11/05 .9* -- t i/ n 1.76 -- 11/05 .t* -- 11/05 NO .12 :i/o e NO .48 H/CS 9,28 -- ll/C fi U .3* 11/05 K) .*6 11/05 1.53 -- 11/05 ND .13 u/ce ,t* -- 11/05 ND .09 11/05 NO .0* 11/05 .91 -- 11/05 .7* -- 11/08 .*7 -- 11/05 10.3* -- 11/05 NT .67 11/05 ND 20,9 11/05 ND .03 11/05 1802 .81 1827 .73 18*8 .84 1908 .84 1928 .73 2009 .70 2029 .8* 20*9 .87 2109 .85 2130 .75 2210 .82 2230 .81 2251 .78 2311 .71 2331 .76 0158 .83 0218 0.00 0239 .72 0259 .77 0319 .81 0405 ,75 0*25 .67 0*45 0.00 ores m * .79 94, .80 90, .78 93. .77 94. .77 97. .77 102. .78 98. .81 98. .76 107. ,81 99. .77 96. .82 107. .84 115. .78 122. .79 104. .80 110. .80 110. .78 102. .73 J03. .79 I . .79 m . .7* 97. .81 147. .78 no. 2CT9. 2320. 2201. 55395. 63*33. 8579*. 182902. 252199. 86382. 53406. 70261. 87733. 2779. 3319. 2556. 63706. 73302. r a n . 2258. 2693. 0. 53432. 65369. 85637. 19379. 2656*. 9399. 5 0 0 . 63820. fi?*75- 29327. *2*18. 1*0*3. 503*9. 52535, 411. 3061. 3627. 3137. 39**i. 6511*. 83298, 2673. 3072. 0. 57439, 639. 79259. 2516. 2960. 0. 1*0*5. 13870. 13171, 63*30. 8*734. 2835.2. 20723. 23306. 28326. 2819. . 3438. 0. 20721. 228F. 99628. . 2581. 3190. 0. 16760. 1727*. 21013. **69. 5694. 3370. 8780. 0725. 10428. 3100. *355. 0. 79913. 70151, 90*22. 3550, *663. 2*76. 75712. 78872. 99650. 216*. 2599. 0. 2195. 0. 66356. 65753. 695. 0. 6/859. 6S7S3. 695. X t9073. 26403. 8*19. 57525. 60593. 77400. 19325. 25090, 8327. 69985. 72337. 93277. 10611. 13085. 5*3*. 67502. 68851. 870*7. 2*0320, 320370, 92691. 75223, 73061, 92*81. S078. 753?. 0. 73110. 2*i:. 33*9*. 0. 36039. 3956. 2997. 30. 7745. IY 0. 0. 0, 71800. 69795. 89619. I corrected for ccKTRiBurirw a native tcsd csikto tt .c o c? h/e 3 2 ) !iT E CODES: I : ISOTOPE RATIO O i: OF ACCEPTABLE RAW v:iacc.racy an nravertable rank tod blaw P=PTTAL SCAN R=K?ATE U EIIH I AND V& OP WWwTWEt INTERLA81 FB*FIELP BLAHC (..NATIVE TCW SPIKES ND=N?T DETECTED PL^oeniTim umi ^!BK F llp w t -TO1D03 SUBJECT TO PROTECTIVE ORDER. G10910 TCT3 CATA REPORT NTiCSaTO CTWfiWf, KTTW LABORATORY Aflui 1 tc-J^ OCCi.LKj: SPtQO WTT'^i .7}\ RFSLSSnSSTE: .7:* SA.-FLF -- NITRO #7 NITRO '.fl NITRO HO L nitro a:: nitro *:? NITRO I? H NITRO 113 NITRO a R J* GRATS EHR ITT TH3 CLEAN MUT J BC 10,0 J BC 10.500 J BO 10.300 J RO 10.570 .1 BO 9.650 J 80 9.830 J BO 10.840 J BC 10.500 J BC 10.000 PFS TOO 0.1. SJ8 ANALYTICAL 3J0 332 I DATE T1HE 322 3 NX 320 .84 NO 1.72 3-70 .89 11.25 .22 .23 NO -- U /9 .98 11/9 -- 11/9 -- 11/9 -- 11/9 -- U/9 -- 11/9 -- n /9 ,07 U /9 1431 .82 1452 M 1512 .78 153? .71 1553 .R7 1*35 .74 US7 .48 1737 .48 1717 4 4 .73 108. .87 177. .74 79. .73 84. .82 113. .73 98. .02 108. .8? 108. .79 108- 1372. 0. 2033. 48191. 8174. 22410. 2031. 1814. 0. 322 1443. 0. 2483. 67584. 9422. 29118. 3030. 2451. 0. 257 1551. 0. 1913. 227784420. 11939. 2413. 2243. 0. 328* -- 4744. 2334. 2481. 3271*. 29140. 5844. 29933. 25770. 29747. 332 -- 5113. 2334. 4i30, *4181. 31437. 7104. 33994. 29237. 3W 0. 334 it --. 4340. 2498. I 5315. ' KST77. 38314. 9109. 4133U 35774. 417*8. I CCftRECTsD FOR CCfcTRIBJTICN W NATIVF TOO (SJBTRACT .009 OF H/E 3221 5CTt CCTSi *: ISOTOPERATIO0L7OFACCEPTABLERANGE YiIACCURACYcurOFacceptable rance T 8 = fT K * B.AM' TTAl SCAN ^SEPARATE KICKING and UCRWJ> P=5PLTCATFfIJTESl.yi) Fr=FILfl BLAW L .W ttT lV E TOOT SPIKES K=XX RTFCTcD X*0ETECTtW L I IT ,KIAR F IL P 2 TCT004 H ( .(W' CONi SUBJECT TO PROTECTIVE ORDER. C10911 TABLE 2. CALIBRATION SUMMARY ug/Kg NATIVE TCDD .501 5.01 50.01 1.25 12.5 125.0 .501 5.01 50.01 1.25 12.5 125.0 RRF (NATIVE) .836 .662 .703 .729 .721 .677 1.11 .909 .944 1.04 .923 .923 DATE 11/9 11/9 11/9 11/9 11/9 11/9 11/5 11/5 11/5 11/5 11/5 11/5 TIME 13.51 14.11 16.14 17.58 18.19 18.39 00.38 02.43 04.47 06.52 08.55 09.15 RRF (SURROGATE) .925 .884 .940 .951 .952 .901 1.27 1.29 1.40 1.37 1.29 1.32 C O N F ID E N T IA L SUBJECT TO PROTECTIVE ORDER, C 10912 TABLE 3. QUALITY CONTROL SUMMARY ITEM* SURROGATE ACCURACY SPIKE RECOVERY # DATA POINTS 35 10 MEAN + S.D. 105 10.8 * * Not technically correct to report recoveries for internal standard calculated results. GTT3:GT n r in tO [H r 11 SUBJECT TO PROTECTIVE ORDER, 010913 DOCUMENTATION INVENTORY FORM Monsanto Research Corporation Dayton Laboratory I. .Sample Information Sample Identification: /J IT"& ^ Number of Samples: ^3 5 Analyte: J2,i3. ,V T C- j j) Matrix: L . ^ r M ethod: ' D T rvn o a t / o f - 2 , 3 , 1 . ? "Tc-ii on Sect. in < n T I I . D ocum entation C o n tro l Copies Attached Initials (a) Sample Receipt Form (b) Internal Sample Tracking Form (c) Sample Tags (d) Airbill (Number ) (e) Chain of Custody Form (f) Analysis Request (Log Number I - c 2 ) (s) Extraction/Preparation ^ notebook pages (NBPL?#7!?/ (h) Analysis NBP 2 ( ? Instrument Logbook pages /S7#il4-jp Computer Data Files hard copy output Chromatograms (i) Data Reduction NBP 1a . (j) Final Report ^ (R) Additional Documentation (note immediately upon acquisition) -- (fVijJ __ -- . /TUjrJ /ET J JJ 1/=>iA/rJ" J i/ FvJrt P\aW j j noni^ File Complete vjsignature0 / SUBJECT TO PROTECTIVE ORDER. Sample R e ceip t Form Monsanto Research C o rp o ra tio n Dayton Lab o ra to ry Customer Id e n t if ic a t io n : f \ i i T Q n _________ MRC Log Number: I - 9 ^ - i1 - i - 2^ A i r b i l l Number: ______ ^ ________________________ D a te: ________ ! nJ o v . 9 *4 __________________ Sample R eceipt In fo rm a tio n : (a) Shipping Containers (b) Custody Seals ( c ) Chain o f Custody Forms (d ) Sample Tags (e ) Sample C o nta ine rs ( f ) Agreement o f Sample D o cu m e n ta tio n in ta c t present (''presen^ ^ in tic ? ) (yes damaged (d e s c rib e below) No. Z In itia ls e&u/j /absntv (describe V ^ _ 3 e a lin g below) in t a c t ___ > absent No. absent No Qgrs damaged (d e s c rib e below) N o iy no (d e s c rib e d is c re p a n c ie s ) A d d itio n a l D e s c rip tio n ( i f sample numbers n o t li s t e d on c h a in o f custody fo rm , l i s t here and c o n ta c t SMO). <s> *<J*JZ*f -daeJL+j. nom g C G P * a-1 > N T I A L SUBJECT TO PROTECTIVE ORDER, C10915 MRC JOD NUMBER _______________________________________________ _____ CUSTOM Pfc'PRtSCHTAIIVE /Wf?s> ^ CONTRACT NUMBER __________________________________________________ MRC CONTRACT MANAGtR ____________________________________ PLANT NAME OR CODE V /T /V)__________________ MRC TEAM LEADER __________________________________________ ( S p e c ific In fo rm a tio n on samples 1s a v a lla b lc on a tta c h e d "Sample I d e n t if ic a t io n Lon") O S ig n a tu re s Da te Time Remarks Team Leader V e r if ic a t io n o f C o lle c te d Samples: R elinquished by R elinquished by: Logned-1n-by: Received by: Received by & U tr Wt h fo /y i /o''/ n iiil& L . D . I * f * r \ rA _______________ __________________ __ 1-- i o9l*. hi Received fo r A n a lysis by: Method o f Shipm ent; SR TT ___________________________________ r cT_Lpd;----- ^T----- Number o f C o n ta in e rs : O ------------------------------------------------------------------------------------ - - L at- -LL Spec ia l In s tr u c tio n s (Sample p re s e rv a tio n , s e c u r ity , d e liv e r y t o , e t c . ) I-^3 O ^ ---- is . .MRC Oct- Ko. Contraci No Plant o* Code SAJALE iOLKTIF-CATiCH LOG ___ Customer R e p re s e n ta tiv e P lg f ioN t i ___ KRC Contract Manager ____________________ Tea.n Leader SamruTg Location ; Ru*- Date Type o f Ta.'np1e L | Analys s " S am ple recovered" Sy iiiur.L-er SflnplfidjNo. of Containers* Required_____ ( I n i t i a l s ) and Conreents L -i ;3Tii " O J. N. ^ i.^ a j s u b j e v JT't o f w o /'El t j v t c s DEH. non-* 4 En <u/ C10917 MRC Oct* Hd. Contract: No. Plant hi'^e or Code K^-r(Co SWL.E lOLSnf I CATIox LOG Ou:ta r a r represe ntativ e MFC Contract Manager____________________ _______ Team Leader OATE i rA N A LY S IS REQUEST ]. LOG NO. !->?>} - ! ! MONSANTO RESEARCH CORPORATION REQUESTER" DAYTON LABORATORY f ). h- t __ r r \ CHARGE NO." /r? A -;0 SAMPLE DESCRIPTION '9 NUMBER OF BOTTLES: h i. S8 H , B K ' NUMBER OF SAMPLES - J4 2 1 B ~~1A REPORT RESUL FILES /KULIX ? o A -f lT ^'v- an alysis reql FILS/ / ^ . 13 SC S>, s Q il io }3 V i-s /i 1/ ' V A ' "C " 7 'A U B 2C MB 6. C C* 3A / <6 y8 Z /J-' "V SAMPLES FOR SAMPLE LOCA -,__________________________________________________________________RECOROEDBY: ,T C . REQUIRED AN ALYSIS" * A/,. ____ -- / y -- /* <r"O Q KNOWN HEALTH HAZARD PRESENTED BY SAMPLE: ANALYTICAL TECHNIQUE REFERENCE TO PREVIOUS WORK (REQUEST#, JOURNAL,ETC.) COMPLETION DATE TIME ALLOTED FOR ANALYSES ANALYST HOURS INST. TIME GAS CHROMATOGRAPHY NMR ULTRAVIOLET HPLC VISIBLE XRD INFRARED ICP EMISSION ATOMIC ASSORPt EDAX XRF MASS SPEC MICROSCOPY OTHER ^jSK2 ' GC/MS C AUTO ANALYZER OUAL SEMI QUANT. QUANTJ ' ' REQUIRED QA/QC ____f t ^ f /; '7- J.0 ^ r -' .p -- ---- -i... .Ta-----i t -- 6,-- sat___________________________________ "SAMPLE DISPOSAL: AFTER REPORT COMPLETE D DISCARD L. -! ' : i "-i ; ! H i . . i"i tt'. rr--/--r -r^ b U L v 1 1U ir f\U 1LY / U i U U*YUL.1L, n r r 11P_______ 1ZI RETURN HOLD FOR 30 DAYS ( 1 fllfl _ 60 DAYS - THIS INFORMATION MUST BE SUPPLIED BY ANALYSIS REQUEST ORIGINATOR MONSANTO COMPANY SUBJECT M o o ils m wo - ,,a d \ (( S . 'f c P R E P A R E D BY ( S IC N A IU P E ) y /'K fj' N? 2S31624 OATE rJ0u g -- I/.\U. -1 oc, Mo. ---------------------- b. \b------------ --^J8ijro Soils L ^c C |( Ihtcx SheeX by Cx- Zu\*L Mo. r ----------i ll. tu /^(uaI aJ'.^h tur. u T 3 0^11 _ L A . _ -------- . /0 C?3 na M 3 O.^I * tetwo Co "C/ (O 1/ v 1 1/ a e k s^ v rrr-Eur/ H3 i e f i Lo I I .-i? 90/J !OGu c4- ih 1c fo.o? f-' 9 _J J SL 97 V3 ! C\ a OA R cpl'ca il _ _ M' fo-C/3 10, 25" Ifl.MI 90?rz/l iy *. j / i/ y V1 3 4 ffy/iW e lo x5 (/ _j L C/O iri w,?>t io 7 7 l/ y V 11 ./ 1____________________ <T2 s c d T U e? k<: io.$r? io .A 10.9(7 v/ / ; C~f<T7 5~9 e n - s o i'? d HA d S 'f r < rn f t AtfoHtrr 4j / Sr* . r t^ T V // ff.-ry /PVY i(l, 0 in. ri.*? 4 (7jK 1 i/ / / 1/ i i/ j V _j_ \S -- --- SUBJECT TO PROTECTIVE OROER 00017 C10920 V ^ d r MONSANTO COMPANY SUBJECT /|/W rb Sa 6 JOB NO. ^A^diiil HQ HAZHo fl^Co St{e- LAAi.?fl ______" N? 2831625 DATE Date. / / A / g T jLc/Njo_=S&_ V! Shet Cede No. (fT'&M . a 6& flilLptt* ' . 7 7 / 77 y t ' -7,r vd louJ 7<? l F ------- 0iA t i fA Z2 ;& r ' "" 5 !& g* } J' & ._ .i_ . \ J Va-/ a- 7 ZA *A A <? i V f CA te/ofamf* f. 51 -T 51 r< 54 6 , <?< 7 ? `57 i /7rfeA 1l**t - ok^ M by A 1 / " Z . ***** ty iftilci te lito Altad iur. S/p)*XtiJof Airtiue Co co /-<2J7<-l /C. r. 7/ 4*J2. __ , ^Cow/ne.n'fe ^AcJ to.14 o. 34" .24 ,fr /.t "n-irfb *JjU a. /OOjJ /o-Y 4o~ ftf.sa. La *il* . /<?<( /a 34" _ I ma vjr_______ /M AoO^J (f-oA to. io tun AtjL . if03_ /e ia . / (.4" /-P ton io.4i (ajo fioc $u b j e c t JOS NO. MONSANTO COMPANY J tilf P R E P A R E D b y (SIG NATUR E! ~ -- N? 2637230 DATE /0 Strflf TOT T* *FT osanoora- S*n*iuca*nrr T `6 .i l z a'/= spro * T lffl .TT3 t f SLMTGATEl 1.326 ww rem Iw * SUV rn f ut pm mcinio. 3 oe i uno or toff rot u . vti tik ia w c a m s r a* m tv la C F tti. I la c r t t l 1 LO CFia t l L la a n u . io LaC F ia 1C 1 LMETILI 2 le w m 2 N LUCF1U. 3 la c n iL 3 L T ia n laarru . x UW FIU. X L la c rriL a i a e riti LACFfU. <1 H '. n i l *c la c m 5 ia c m i a i M ir iti n i SJMC J j J J J j J J J J J j J j J 1 J J 1 J R 1U I w .1 * u /ts 0100 .61 . tre. 10543. 1421. 18877. lUQ m . 1974*6. I R 10.210 T.H -- 11/05 01 .82 .71 ICO. 2716. 3316*7. 157*2. 110519. 918. 115793. R 11.7 * . -- 11/05 01 .S3 .80 H . SW907. 721791. 3180. 1 2 1 0 . 134U. H # . R 10.0 1.12 -- 11/00 00 .81 .81 97. 97771. 120374. 2704. 1 7 * . 12214. ',9(108. R 10.1 R 10.750 2.23 -- 11/05 02 .so . n . 114939, 143415. 64201. 1457*3. 17CS. 153195. .71 -- I l /OS 83 .71 . f i , 15714. W W . 12100. H 9S3. ] 43707. I775H. r 10.410 U T -- 11/05 03 .81 .8* 101. 414689. 512623. 218527, 133011. 11340*. 1 3 *2 . R 1 .9 .1 -- U/05 crus .72 ,81 IB I. 7138. 97*2. 5905, 1490, 12492. 153*53. R 10.ISO .14 -- 11/00 04 .81 .87 . 1 *. 8151, 4040, 1*5*4. 1131a 151*16. R 10.110 .23 -- 11/05 04 .81 .82 101. t l l i l . 13B33. 1CB4. !4f*63. 15412. 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I l OMCD TO CWT!RfT! tT T II* TOT (SJPTWCT .0 Cf WE 32) xrtaaESt II ISOTOPE PiTIO (WT OF 4GPT4RE UCE iecoRAoror rractttaimce ^ETNRttlf MARTI. stak ^SEMATEIEI(X10)Kl* >a\irATE(iifTTO.i m*mo RjMc l.**6TIVE TOT SPIRES io*n rosoni x*irECTiw imn XJM FILEME-TOT Oo/"ior| /^/ir-v v-. : AT SUBJECT TO PROTECT!'/, ORDER. G10923 RK AO A N O U M D I M T O O O Y DATE SUBJECT JOS NO. MONSANTO COMPANY ^ r^.kc ^ PS E P A R E O BY [S IG N A T U R E ! 7 < 9 - 1*- t* . _ i _______ _ . f X J - T i c t e . N? 2637231 DATE /J^ Tomsa*pan KWJssTDcruwr. c*rrt*u k m u w "T *4 k t 1 i u w n re ca uffa r a e K MATlUFl .7 SfiZZiTU 1.C3 is-p. f in * -- Em frm --- ttaPTtL a i J if f tU. 4* w .B iO ria 7* .BFIU 71 ii T U 7 1 1 j j j j j SCT1U. 7T, j .1TO SITE in j *17Hr, SITE ISA j CTW SITE 1 j i!TB!) 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(t' U 3 IVIUIX J m i I v> w w m P R E P A R E D BY (SIG NATUR E! Z ^ U . 9 ijd - < N? 2637232 DATE r e s sat* Birarr nasanocnren. nevraiiakutort t m v ! i ii.jfj <e c:?roo W KTT'Jtt .T31 jstsatei .: S r.r s ia fR (Rffi ETTI HCT KW CLEW 10(1 SM m aisltt:Oft. 330 333 T TES) O.L. te T I 331 334 ore 320 331 757 328* va 33* 4 KlTBfl I f N'.TBS in J BC 10.113 .fii 1 1 * 1131 .13 .75 1* . 1372. U t . 1551. ir a . 5115. 4360. J r . 10.V 1 1 * M ia MM .87 127. 0. 0. 0. 7X4. 2314. 74. I * :tbs> i o u J K 10.700 u n -- U * ISU .74 .7* 7S. 2S3. 6S61 im . IM I. *030. T3-.5. (TTC ! J K 10.5 3 . -- 1 1* t r a .71 .75 04. 475S*. m e 377J1. M IR I. WE77. K'.TB :2 .) BC 4.PM -- 1 1 * is n .*? .S I i a 17. a . 4* . 17160. 3 l 7 . TC14, e ir a 117 " J K 4.1W 11. -- 11 1135 .7* .7 * . 71*10. 2*11*. U 93. S U , 7104. 10. :n n 113 J X 10.s u 2.a -- 1 1 * 1T7 .41 . t i 108, ffll. 3036. 4&tX 29783. 33W4. tr m . MITO l ]3 * J X 10.500 . a -- 11 1737 . a 1ins. *1*. 7451. 72C. 25770. 2TO7. zm *. J K 1C. ,07 I I * 1717 m i .71 108. 0. 0. 0. 27747. 33?, *17, 1 rawiCTEP fop cttbrt v mth* tot isjptmct .ow cf v e 3221 TECC3FU i: STTTE MT10 XT X AOTT4R.E MK x:76TJWCTX CfSRIFTW.C M flwTwr.p.we vetrai stak tx^y^TE ue:i> uc ac im p MP.lEATTHATRSl n-FlQJ BUM L,MWl*TES!SPIKES *07 STTirtni i'DTiCTlfffLinn .K PJLPWlc TOW4 TV,T V"'\'7 a>^.3:--I .i SUBJECT TO PROTECTIVE ORDER. C10925 onogj R IA D A N O 'U N O K A ITO O O IV CATE oe Antlyit 5'-' s. JL Sit > -C * ui Xr\ rj x> 4 O CD oC& o0 1 -a -1 C' U v* w - V i\ O l_ -D wC --1 C ^ -- L-4 V - V 0 "t -a c V* -J * $ Vl a* -I c- ^ ^V c J( wp -* s * ^ rQ j 7" -- O -!) V J ? ^ ^ 7^ V y *4 Volum (vl) <: i \*4 -- ---> ' iC --L J 1^1 J&V A ^cv .1. Vk O'i V4 -- ^ ^ J\ V . j --~J ^ W .5 Sottl Kimber < rN ^0v\T : c* ;r ,\1 t-.-\ T'0^"r" '-- "'V P ' vj Cn f 00023 C10926 <- -CM?m > o l/t a 2 6t#T f i \ i I i t A hO rr o c tA vi -- 0_P < J S' lj\ ~ ^ U - CD_tOO --1 f O' n it nm--noj V oA Volum (ul) pi H o Tn O/ T - -_ o-- ifi -c "jt'v ?/51 S *C*i 4 -- _j -I O \S_l >Uil- ----- C b * >* -I ; c ^ ** ?' vA v -- cs _*Jr-- o23-- S3 Zo Tfc~ ` & 4 VA vr - W . ____ 0 s sIVAW V v s j T- ^ C * ** -i w'-`--, J Zfi a J 0 ^ .S Botti I Number o & r e o vt*^. ^ - - --C f-lE r-: W W W t# w rr T;YE ORDER. 0 QP2A ______________0109.27 I ? i_ _ -- * _ 1__ Z. o>a ss - *c t <- -f> J -1 ^ o e <- 2. -i n < r -c -c < t vT" ?- T~ -= ^ < r $ A n jljrit -CxP * 5" ?e- -X V ? ^ C -J V ^0 \ v C* VV-A- Volum e M) =O S-- Bl O fI AJioxvtitiuvn N o iiy ti 5 'i 9^ V* ? -D w ~ J j o US >v *\- _ s ,, <^ - c .5 Bottlc Nwter D> 5->3 > II nn^o ^TIAL W u D c, C10928 K" 4- 3 > Jte___ * o (jc- f t SS Aftiljrit 4r -C O o jo ggo 3 S cQ -J ( T <A- Jct -G Volume (vl) l .S fto ttla Number l I i oa !S O N > ^ __ x * Ia L SUBJECT TO PROTECTIVE ORDER. 010929 5? =o *4 > m ia n to Re se a r c h Co r po r a t io n DAYTON LABORATORY SUBJECT. job No.. I i>j ^ ' J _____ Da t e __ Sig n a t u r e I j V -d '_________ L s a 4_ \ 'n o t -- --- =^*=sr JiD _ Q 3 7P3 J L . y i _ 'TV* Q .tb t U i t)*7L JL - A 0 ? - h \ UF:_ 9 0 f 2 _ <% . l ct i li ry P. k krt. 7 . / L !f/+'i W . l L S* V - * _ 1,, J- ' 0 -Ceil / % a . vf ito - Q C ii.. 7 3 - -- -- / ff JL- f - A`V - -- lO fl2 . ._ . U T - JMl s --- -- -- ---- -- -- -- 7 ------ ... 3 m - - M <r -- ---- r -- Lv. - - -- . .1 . - - / . a t / i i (T - M r bsHi 19 read And Understood by me DATE___________________________ 19 NAH IO KkSItAHCH CORPORATION DAYTON LABORATORY Job No. Si g n a t u r e ---- 1 A Sm5 Job Nuftber Net Tim Tim of Day CRH 7920 AR. Disc Pack FRH r>8O--pWa Staple Idontlflcatlon fxAt1'fri *1^*10 "H trt hr-? t a f 0.6 S i t i / f' o i1 /-J 7 iiC i ' -- t j3 ib^ iir_ % ___ <L j f i - .0"! Soil _o/.. JLr r -- CJA' iO f. <ld i] .r Jr C>3 V iii <T 6 3fcfj: / Qn2ran 2 ftf- 30< l ? ** >ir< ri r l t 7 Z<0/ J j<D V/*. ti f 'fwi /JLV) )ik Z*SL3ftg^ J jii l Paf r H* i / . A a n*n z&r? 21^J) Vo ' a a j rp. Cl3- Qc/if 7rntL _ m f i - rir *5 of 4*; a -in hit. `1 2rj TPCC[f;Fp(f$ti f/o U '(X J ^ -- ) t--- i- / r"v JT Date Comments err -Jpu _23) n L ir r i, C\tf--- ft i H e ------- ^ o f*-ff?pspi ------- rJfuM (TaV o ? m I74oD->41tA_i GC Conditions V*X Run Tim " n &CKj S 7/l /? tH 7 CO 1 CD 71 o * "- 1 r7 V 7r 7* t7 / V 17*S Ic,/io o -1* "So - \ Ai' //ro/ OO 2*10- ^fi2x r -2 \%4 ? TT i j U If /O ,7 'u s a n o ai3aij.o 3 SOUd ryo H O O c C10933 File / 160 3 . 6 - 3 2 4 . 6 iITtU. 2 UL . 10 0 2 / . 4 8 / . 2 P2330 2 0 0 - 1/ 3 / 2 8 0 GT.. File >00160 321.6-322.6 amu.^UL .1002/. 43/ P22:30 200- 1/3/250 GT.. '-''.'so CONFIDENTIAL C10933 MS data tile header from >G0160 Samp! i 2UL .I'2/. 43/. 2 S Operai or i GfiRY MS2 11/09/84 13?S 1- Mise i P2330 200-1/3/2S0 GT ETL#03ETL#3 Sys . it* 1 MS model! 87 SN/HW rev*! Cfi fiLS tt ! 0 Method file: SP2330 Tuning file: fiPEIOl No. of extr a records: 2 Source temp.! 50 finalyzer temp.: 265 Tr arisfer 1ine temp. : 65 Chrornatographic temperat ures : 200. *.Chromat ographic t imes, min. : 1.0 Chrom atogr aph ic r ate, deg/m in: 3.0 250. 25.0 0.0 0. 0. 0.0 0.0 0.0 ' 0.0 0 0. 0 0. 0 M/Z = 333.9 First peak is baseline drop corrected area. Sec ond peak is t*ange fit skimtried corrected area. Peak # R. T. first ftiin. scan 1 10.754 2 10.754 163 163 max sc an 179 179 1ast peak sc an width 195 27 195 27 raw area 100828 100328 corr. area 65566 63716 corr. 5 100.00 97. 18 M/Z = 331.9 - First peak is base 1ine drop corrected area. Second pe ak is tang ent skimmed corrected area. Peak it R. T. firs t m ax 1ast peak miri. scan sc an scan w idth raw area corr. ar ea corr. 1 10.754 171 179 06 35 9S202 54452 100.00 10.754 171 179 20b 35 98202 52754 96.88 332/334 CALCULATION R-GlobaK 0'1 = .8365 First pc ak iis baselin e drop corr ct(j ari;> Sec end (i*eak iis tangent skimmed corrected CLf"<[:i Peak tt R. T. fi rst max 1ast peak min. sc an sc an scan w idth raw arc a co rr . area 1 10.774 165 180 196 31 85238 46364 2 10.774 165 180 196 31 85238 43853 M/Z = 321.9 First pc ak i : base 1ine drop corr ec ted area. Second peak iis tangent- sk irnmed cor*rected ci.r:' Pe ak it P. T. firs t max 1ast pe ak min . sc an sc an S-c an i.iidth raw ar e a corr. are a 1 10.774 175 180 190 10.774 175 ISO 190 15 15 pr\npi 31299 31299 12159 11611 CONFIDENTIAL cor r. . 100.00 94.58 corr. y 100.00 95. 49 010931 s nsZ = 31?.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. ak R. T, first max 1as t peak # mi n. scan sc an scan u fdt h raw area 1* 18.774 176 130 191 2 10.774 176 180 191 15 28813 15 28013 | Li o corr. area 8798 3588 corr. * 100.00 97.61 320.'322 CALCULATION R-GlobaK 1> = .7236 tl'Z = 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R. T, first max 1ast peak fiiin, scan scan scan width raw area 1 10.795 178 131 136 2 10.795 178 131 136 3 17155 3 17155 corr. area 5723 5443 corr. % 100.00 95.11 <320 + 322 )/ <332 +334> C A L C UL A T ION R-Global< 3) = .1746 (32S')/<332 + 334 > CALCULATION R-Global< 3> = .3854 p o o *3 J> SUBJECT TO PROTECTIVE ORDER C10935 :n Q O' M. [>j cd O CO 05 V 'P n. CO ro 7' I to ro ro CT> (3* C ro G* D ro \ .u C\O ro M T) ro to to G ro CD CD r -* \ to \ ro tn a <n ton o T> O <2> <7 to G> O CD CD L -J io 03 tIo :o U of?r' c ro a o fO \ a 00 \ fO CO roO w to o ro o a J *-- \ 03 \ vroi o o o oo MS data file header from : >G0161 Sample: 2UL 1.0O2/.48/.2 S Operator: GARY MS2 11/09/84 14:11 Mi sc : P2338 200-1/3/250 GT BTL#05 BTL# 5 Sys. #: 1 MS model: 87 SW/HW rev,: CA ALS # : 0 Method file: SP2330 Tuning file: RPEI01 Mo. of extra records: 2 Source temp.: 250 Analyzer temp.: 265 Transfer line temp. : 265--. Chromat ographi c temperat ures : 200. 250. 0. 0. 0. Chromatographic times, min. : 1.0 25.0 0.0 0.0 0.0 Chromtographic rate, deg/min: 3.0 0.0 0.0 0.0 0.0 M/2 333.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. f irst max 1ast Peak min. scan scan sc an width raw area corr. area corr. V. 1 11.424 198 212 232 2 11.424 198 212 232 34 109186 34 109186 66788 100.00 62232 93. 18 M/Z = 331.9 First peak is base1ine drop corrected area. Second peak is tangent sk imm*d corrected area. Peak # R.T. first max 15 t peak min. Sc an scan sc an width raw area corr. area corr. * 1 11.424 2 11.424 193 212 193 212 235 235 37 100274 Wl' 1G0274 56170 100.00 53247 94.30 332/334 CALCULATION R-Global< 6) = .8410 M/Z = 327.8 First peak is base1ine drop corrected area. Sec ond peak is tangent sk immed cor: ected area. Peak # R.T. first fitax 1as t pe ak min. sc an scan sc an width raw ar-ea 1 11.444 203 213 227 24 75197 2 11.444 203 213 227 24 75197 M/Z = 321.9 First peak is bas e1ine drop corrected area Second pe ak is tangent skimmed corrected area. Peak it R rT. first max 1ast peak min. sc an scan scan width raw area 1 11.444 2 11.444 199 213 199 213 238 O 39 147338 39 147338 iWU I corr. are a 46265 43335 corr. 100. O0 93.90 corr. area cori'. 989O0 100.00 94142 95. 19 C10937" ri/2 = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected are*. Pe ak t* R .T . fi rst max 1ast peak min. sc an sc an scan width raw area 1 j*-11.444 201 213 229 ' 28 104678 2 11.444 201 213 229 28 104678 s to lto ' corr. area 71022 65394 corr. li 100.00 92. 08 320/322 CftLCULftTI ON R-G1obal( 1> = .7181 M/2 = 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Pe ak R. T. first max 1ast peak min. scan scan scan width raw area 1 11.444 2 11.444 199 213 232 33 199 213 232 . 33 85S60 85860 corr. area 40386 37746 corr. i 100.00 93. 46 (320 + 322)/(332 +334) CRLCULftTI ON R-G 1obal < 3) = 1S'20 (3280/(332 + 334) CftLCULftTION R-Global( 3) = .3685 0 nri3 5 " /> Cl0938 File >0362 3 3 .*-334 .c- emu. UL UT-3169 3P2330 200-l''3-'256 GT File File File >G0162 321.6-322.6 imu.2UL UT-3169 SP2336 266-1^3^250 GT File File criR?rrT rn p s o T F m v r A t 0003 b C1.0939 MS data file header from ! >G0162 Sample! 2UL UT-3109 Operator: GfiRY MS2 11-"09/84 14 :-3i Mi sc : SP2330 200-1/3/250 GT BTL#07BTL# 7 Sys. #: 1 MS model: 87 SW/HN rev.: CR RLS # : 0 Method file: SP2330 Tuning file: RPEI01 No. of extra records: 2 Source temp.: 250 Analyser temp.: 265 Transfer line temp. : 265 '- .Chroma!tographi c temperat ures : 20Q. 250. 0. 0. 0. Chromat ograph ic times., m in. : 1.0 25.0 0. 0 0.0 0.0 Chromatographi c rate, deg/m in: 3.0 0.0 0.0 0. 0 0. 0 M/Z = 333.9 First peak is base! ine drop corrected area. Second peak is tange nt sk ifumed corrected area. Pe ak # R. T. first max 1ast peak min. scan sc an scan ui dth raw area corr. area corr. 7. 1 11.462 210 214 219 2 11.462 210 214 219 9 26045 9 20845 860 100.00 5717 83.34 M/Z = 331.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Pe ak # K f irst fil-X 1ast peak m in. sc an sc an scan uh dth ra u area corr. area corr. V 1 11.462 212 214 218 11.462 212 214 21 S 6 13497 6 13497 5115 100.00 4614 90.21 332/334 CALCULATION R-GlobaK 0) = .7456 IVZ = 327.9 First peak is baseline drop corrected area. Sec ond peak is tarigent skimmed corrected area . Peak # R.T. first max 1ast pe ak min. scan scan sc an u idt h raw area 1 11.482 212 215 219 2 11.482 212 215 219 7 13620 7 13620 M/Z = 321.9 First peak is baseline >drop corrected area. Second peak is tange nt skimmed corrected area. Pe ak * R. T. first max 1as t peak min. sc an sc an sc an w Pdt h raw area 1 11.502 213 216 2 11.502 213 216 .. *-- --- ^ --- , --- --- \ '-? 218 5 2 '? 5 OOG7 8075 8075 corr. area 4779 4089 corr. * 108.60 85.56 corr. area 1665 1482 corr. / 180.00 89.01 Cl094 s fV2 = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R. T. first max 1ast peak min. scan sc an scan u i'dth rau area 1 *1*11.482 215 215 217 2 4026 2 11.4S2 215 215 217 2 4626 -><21^2- corr. area 1372 1330 corr. / 100.00 96.94 320-'322 CALCULATION R-G 1obal< l> = .6240 M/2 = 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R. T. first rnax 1ast peak min. sc an sc an sc an ui dth rau area 1 11.462 213 214 214 2 11.462 213 214 214 1 2961 1 2961 corr, area 1551 1480 corr. x 100.00 95.42 <320 + 322)''<332 +334) CALCULATION R-GlobalC 3) = .2536 <328'' ) / <332 + 3 3 4 ) CALCULATION R-G1obal< 3 ) = .3978 0003 SUBJECT TO P R C i l CTVE fiK T im C10941 rile > C~01 6 3 3 3 3 - 3 3 4 ini u . ^ U T~ 3110 C P 2 3 3 0 2 G O - l / ? / 2 0 GT File5 File Fi le >60163 321.6-322.6 amu .'-'L- UT-3110 F'2330 200-1/3/250 GT Fi le File o o o 'i.q C10942 MS data file header from >G013 Sample: 2UL UT-3110 S Operator: GARY MS2 11/09/84 14:52 Mi sc : P2330 200-1/3/250 GT BTL#09BTL# 9 Sys. #: 1 MS model: 87 SW/HW rev.; CA ALS # : 0 Method file: SP2330 Tuning file: APEI01 Ho. of extra records: 2 Source temp.: 250 Analyzer temp.: 265 Transfer line temp. : 265-- '- r Chromatograph:c temperat ure s : 200. 250. 0. 0 0. Chromatograph!c times, min. : 1.0 25. 0 0.0 0.0 0.0 Chroma tographi c rat e, deg/m in : 3.0 0.0 0.0 0.0 0. 0 M/2 = 333.9 First peak is base1ine drop corrected area. Sec ond pe ak is tangent skimmed corrected area. Pe ak R. T. first max 1ast peak miin. scan scan scan width raw area corr. area corr. * 1 11.583 218 220 222 2 11.5S3 213 220 222 4 9162 4 9162 2698 100.00 2662 98. 67 11/2 = 331.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Pe ak ft R. T. first max 1ast pe ak min. sc an sc an scan width raw area corr. area corr. X 1 11.5S3 218 220 221 11.583 218 220 221 3 6354 3 6854 2336 106.00 2079 39.00 332/334 CALCULATION R-Global< 0) = .8658 M/Z = 327.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R. T. first max last peak min. sc an sc an scan width raw area 1 11.603 219 221 223 4 8028 2 11,603 219 221 223 4 8028 M/2 = 321.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak ft R. T. first max last peak * raw min. scan scan scan w idt h area 1 0.000 2 0.000 224 224 e 0 f**-->* *.1 /..* / H A L 223 -1 223 -1 QC'f^n 3 0 cor r. ar ea 2 5o 2052 corr. 'i 100.00 87.10 corn, ar e a 134 1 1341 corr. * 100.00 100.00 Cl0943 M/2 = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak ft R.T. First max 1ast peak min. scan sc an sc an u rdt h rau area 1?. 0. DOS 2 0. COO 224 224 0 223 0 223 -1 -1 0' 0 = > C *o \ (d 3 corr. area 1345 1345 corr. `4 100.00 100.00 320/322 CALCULATION R-GlobaK 1) = 1.003Q M/2 = 257.G First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. PS'ak * R.T. first max 1ast peak min. scan scan scan width raw area 1 0.000 2 0.000 224 224 0 223 0 -1 -1 0 0 corr. area 1605 1605 corr. '4 100.00 100.00 <320 + 322 >/< 332 +334) CALCULATION R-GlobaK 3) = .5336 <328'' )/<332 + 334) CALCULATION R-Global< 3) = .4656 nor 41 J Liw a*ir C10944 Til* > 6 0 1 6 4 3 33 .-3-34 6 amu -^'L U T - j l l l P2330 2 0 0 - 1/3^250 GT File >G01 4 321 .6-322.6 sjtiu .2UL UT-3 11 1 SP2330 20- 1/3/259 GT GC/MS de faul f i1e >G8164 A4 MS data file header from >G0164 Samp 1e: 2UL UT-3111 Operator: GARY MS2 11^09/84 15:12 Mise : SP2330 200-1/3/250 GT BTL#11ETL411 Sys. #: 1 MS model: 87 SW/HU rev.: CR RLS # : 0 Method file: SP2330 Tuning file: APEI01 No. of extra records: 2 Sourc e temp.: 250 Analyzer temp.: 265 Transfer line temp. : 265---'- Chromat ogr aph ic temperatures : 200. 250. 0. 0. 0. Chr om atograph ic t imes, min. : 1.0 25.0 0.0 6.0 0.0 Chromatographi c r ate, deg/m in : 3.0 0.0 0.0 0.0 0.0 M/Z = 333.9 First peak is baseline dr op corr ec ted area. Second peak is tangent sk imm ed corrected 4tP`cL* Peak # R.T . first max 1ast peak min . sc an sc an scan width raw area corr. area corr. M 1 11.746 224 223 232 2 11.746 224 228 232 8 16531 8 16531 5315 100.00 4231 79.60 M/Z = 331.9 First peak is baseline drop corrected area. Second peak is tanqent sk immed corree ted area. Peak 4 R.T. first rnin. sc an 1 11.766 2 11.766 226 226 max scan 229 229 1ast scan ^ 232 Pe ak wi dth 6 6 raw area 12238 12238 corr. area 4030 3346 corr. 100.00 83. 03 332/334 CALCULATION R-G1obal< 0> = .7582 M/Z = 327.9 First peak is base1ine drop corrected dPda See ond peak is tangent sk immed corrected ara Peak 4 R.T. first max 1ast peak min. scan scan scan uidth raw ar e*a corr. are a 1 11.737 223 236 232 2 11.787 223 230 .Z*tL 4 H 3937 3937 2705 2613 M/Z = 321.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. p'eak # R.T. first max 1ast peak rnin. sc an scan sc an width raw area corr, ar e a 1 11.787 227 230 233 2 11.787 227 238 ; 233 6 19530 6 10530 2638 2370 corr. * 100.60 96.60 co r r . 100.00 88. 17 C10946 M/Z = 319..99 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Pe ak il R. T. first max 1ast peak min. scan scan scan width raw area r " 11.766 223 229 233 5 3333 2 11.766 223 229 233 5 3833 > Q o\ Lp 4 corr. area 2053 1938 corr. * 100.00 94.40 320/322 CALCULATION R-GlobalC 1) = 7638 M/Z = 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak It R.T. first max 1ast peak min. scan scan sc an width raw area 1 11.787 229 236 232 3 6677 2 11.787 229 230 232 3 6677 corr. area 1913 1357 corr. 'A 100.00 97.07 <320 + 322) /C332 +334) CALCULATION R-GlobalC 3) 5073 (323 ')y C332 + 334) CALCULATION R-Global< 3) = .2369 -- fO'MA -i.mr-r-r r n sarTT.cnVE ORDER- C10947 r i U >GQl5 333. -33*. 6 ir,u`L UT-3112 SP2339 200-U 3^2 o O CD LO CM C\O w\~4 I CD O cm o CO 0) CM _ O 1 -3I CM D EU M> CM CO <0 I CO CO u> CD CD U CD LO CM C\O \ H I CD O CM O 00 <0 CM . (M 00 I CM 3 T) ' CO CCMO N CM CO W) Ci OO CD D <D O o ti LI OJ \ 01 I co co iti . iti co I CO OJ co 01 OJ u;o< tu* Li'i L> CO OJ \ 01 II OJ CO 0 co co co co 01 <0 co n co co tq 4 fDtci ' o.| K U1 CO o> ^-1 LI co CO LI Lf> ri o u> ti \ di oo 05 o TH o ir, K.I C Cc MS data file header from >G0165 Sample: 2UL UT-3112 Operator: GRRY MS2 11/09/84 15:32 Mise i SP2330 200-1/3/250 GT BTL#13BTL#13 Sys. (is 1 MS model : 87 SW/HU rev. : CR RLS ft : 0 Method file: SP2330 Tuning file: RPEI01 No. of extra records: Source temp.: 250 er temp .: 265 Transfer line temp, : ii Ov cr Chromat.ograph ic temperat u res : 200. 250. 0. 0. 0. Chrornat ograph ic times, min. : 1.0 25.0 0.0 0.0 8.0 Chromatograph ic rate, deg/min : 3.0 0.0 0.0 0.0 0.0 M/Z = 333.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. fi rst max 1as t peak min. scan sc an sc an width raw area corr. area corr. /. 1 11.913 230 235 246 2 11.913 230 235 246 16 81281 16 81231 58577 100.00 53057 90.58 M/Z = 331.9 First peak is baseline drop corr ec ted area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak m in. scan sc an sc an width raw area corr. area corr. ym 1 11.933 228 23o 243 2 11.933 223 236 243 15 64086 15 64086 44181 100.00 34348 77.74 332/334 CfiLCULflTION R-GlobaK 0> = .7542 M/Z = 327 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. fi rst max 1ast peak min. sc an sc an sc an width raw ar e a 1 11.933 223 236 241 2 11.933 228 236 241 13 53953 13 53953 M/Z = 321.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Pe ak # R.T. f irst - max last peak min. scan scan sc an width raw area 1 11.953 229 237 p _J.1*353-- - -22*--- (T * " c n o i r r T TO PROTECTIVE ORDER. 247 18 247 18 Oon^g 92820 92820 corr. area 33322 22363 corr. `4 1.60 67 i 11 corr. area 67584 58962 cor r . Ji 100.00 87.24 C10949 M/Z =319. 9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. ,k R, T. fi rst max 1ast peak min. scan sc an scan uidth raw area 1 ' 11.953 229 237. 244 15 68471 11.953 ^ 71$ 237 244 15 6S471 mj>b 0 [ip 5 corr. area 48191 37301 corr, J; 100.03 77. 40 320/322 CflLCULATI ON R-Clobal< 1) = .7131 M/Z = 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Pe ak # R. T. fi rst max 1ast peak min. sc an sc an sc an width raw area 1 11.953 233 237 241 8 -71 11.953 233 237 241 8 36664 36664 corr. area 22728 17964 corr. *4 100.00 79.04 <320 + 322)/<332 +334) CALCULATION . F:-G1obal < 3) = 1.1267 (32S')/<332 + 334) CALCULATION F:-G1obal < 3) = .3184 j O n r> A > y C10950 ril >-01 6 I-:33.- 334 .5 mu .4UL UT-113 SP2330 300-1/3/250 GT Fili >Gl6 321.6-322.6 amu.-UL UT-3113 SF'2330 200-1/3/250 GT > el \r j e c t " t o ..\ T . _ , -a J. pr o tec tive o rder. O^n 4 C10951 GC/NS default files >G0166::A4 MS data file header from : >G0166 Sample: 2UL UT-3113 Operator: GARY MS2 11/G9/34 15 Misc : SP2330 200-1/3/250 GT BTL#15BTL#15 Sys. #: 1 MS model: 87 SU/HW rev.: CA ALS It : 0 Method file: SP2330 Tuning file: APEI01 Mo. of extra records: 2 Source temp.: 250 Analy^er temp.: 23 Transf er line temp. : 265 * *Chrom atognaph ic temperatures : 200. 250. 0. 0. 0. Chromatographic times, min. : 1.0 25.0 0.0 0. 0 0.0 Chromatographic rate, deg/min: 3.0 0.0 0.0 0.0 0.0 333.9 t peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Pe ak it R.T. first max 1ast peak min. sc an sc an sc an width raw area corr. area corr. >. 1 11.804 225 231 236 2 11.S04 225 231 236 11 58402 11 58402 38316 100.00 31276 81.63 M/2 = 331.9 First peak is base 1ine drop corrected area. Sec ond peak is tangent skimmed corrected area. Peak # R. T. fi rst m in. sc an 1 11.825 2 11.825 227 2< max sc an 232 i .. wO **N* 1ast peak sc an width 2^'b 9 23^ 9 raw area 46526 46526 corr. area 31487 26010 corr. * 100.00 82.61 332/334 CALCULATION R-Global< 0) .8218 M/Z = 327.9 First peak is base 1ine drop corrected area. Second peak is tangent skimmed correeted area. Peak # R.T. fi rst max 1ast peak min. sc an sc an scan width raw area 1 11.845 227 233 239 2 11.845 227 233 239 12 47209 12 47209 M/Z = 321.9 First peak is baseline drop corrected area. Second peak is targent skimmed corrected area. Peak it R.T. first max 1ast peak min. sc an sc an scan width raw area 1 11.845 230 233 236 2 11.845 230 233'. \ .236 6 2Q150 6 20158 .. corr. are a 29245 25331 corr. ;/ 100.00 86,79 corr. ar ea 9422 8732 core. 100.00 92.68 C10952 s M/ Z =* 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R. T. first max 1ast p.eak min. sc an scan sc an width raw area f *11.845 230 233 235 2 11.S45 236 233 235 5 18949 5 18949 ^ isf O ( L> io corr. area 8174 6364 corr. '4 160.00 77.86 320/322 CALCULATION R~Globa1( 1) = .8675 M/Z = 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. f irst max 1ast peak m in. sc an sc an sc an width raw area 1 11.845 236 233 236 2 11.345 230 233 236 6 36162 6 30162 corr. area 6420 6324 corr. * 160.60 98.50 <320 + 322)/(332 +334) CALCULATION R-GlobaK 3) = .2521 <323')/<332 + 334) CALCULATION F:-G1 obal ( 3) - .4177 .r \J K -- -i J 5113JFCT TO PROTECTiVE C10953 Fili- >G'O167 siliU . :`UL 10.02/ .43/ .20 SP22-30 200-1 /3/2 50 GT. II J T 1 -i--i--|--i--[--i--i--|-- ri--i--i--J--i--i--i-- [--i--i--i--i--i--i--i--i--i--i--i--i--i--i--i--]--i--i--i--i--| 1 G . 0 10.5 11 .0 11.5 1 2 . 0 13.0 13.5 14.0 0 Frie 1C-0167 38 200-1/3/25O File >G0167 327.6 11.0 11 .5 1 2 . 0 12.5 13.0' 1 14.5 10.02/.48/.20 SP2230 200-1/3/250 0 11.0 i'111 i1 1 T1 | 11r 1 |T 13.5 14.5 .15 ,0 10.0 T - i-- |-- i-- i-- i-- i-- |-- r 11.0 T-- i-- |-- i ! I-- r-- |-- i-- i-- i-- i-- i-- r- 1-- i-- !-- j-- i-- i-- i-- i-- |-- i-- i-- i-- i-- J-- i-- n -- i-- ]-- i-- i-- i-- i-- | 14.0 14.5 0 2OO-1 /3/250 GT ... File >G0167 100000- 11.0 11 .5 12.5 13.0 200-1/3/25 0 10.5 11.0 11 .5 12.0 13.0 14 .5 O C10954 MS dita file header from i >G01'67' S amp 1e: 2UL 10.02 /.-48/. 20 Oper at or: GARY MS 2 11/G9/S4 -1-6: t4 Mise : SP2230 280-1/3/250 GT BTL#17BTL#17 Sys, #: 1 MS model* 87 SW/HU reu. : CR RLS : 0 Method file: SP2330 Tuning file: RPEI01 No. of extra records: 2 Source temp.: 250 Analyzer temp.: 265 Transfer line temp. : 265--'- Chrornatograph ic temperatures : 280. 250. 0. 0. 0 * Chrom atograph ic times, min. : 1.0 25.0 0.0 0. 0 0. Chrornat ograph ic rate, deg/min : 3.0 0.0 0. 0 0. 0 0. M/Z = 333. 9 F irst peak is baseline drop corrected area. Second peak is tangent sk immed corrected area. Peak # R. T. first max last peak min. scan scan scan width raw area corr. area corr *4 1 11.26G 194 2G2 210 2 11.260 194 262 210 16 16 90032 90032 68336 100.00 60928 89.16 M/Z = 331.9 First peak is baseline drop corrected area, Second peak is tangent skimmed corrected area. Peak # R. T. f1irst max 1ast peak m in, sc an sc an sc an width raw area corr. area corr. y 1 11.266 196 202 211 11.260 196 282 211 15 75797 15 75797 56597 100.00 51129 90.34 332/334 CALCULATION R-Glcb&l< Qy ~ .8282 M/Z - 327.3 First peak is baseline drop corrected area. Sec ond pcak ii s tangent skimmed corrected an ea Peak # R. T. fi rst max 1ast peak min. sc an scan scan width raw area corr, area 1 11.280 198 2G3 211 13 76469 58451 2 11.2S0 198 203 21 1 13 76469 53459 M/Z = 321.9 F irs t peak is base 1ine drop corrected area. Second peak iis tangent skimmed corrected area. Peak # R. T. first max 1ast peak min . scan scan sc an width raw area corr, area 1 11.280 192 283 212 2 11.28G 192 283 212 2D 1085361 157321 28 1885361 926731 corr. '4 108.00 91.46 corr. v. 180.60 87.65 SUBJECT TO PROTECTIVE ORDER. C10955 M/Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Feak R. T. Fi rst max 1ast peak min. sc an sc an sc an width raw area 1 /11 300 135 24 212 2 11.3O0 185 204 212 17 800010 17 800010 corr. area 776958 695145 corr. * 1*00.00 89.47 320/322 CALCULATION R>G1obal< 1) = .7348 M/Z = 257.0 Fi rst peak is base 1ine drop core ec ted area. econd peak is tangent ski mmed corrected area. eak R. T. Fi rst max 1ast peak # min. sc an scan sc an width raw area 1 11.30O 192 204 212 20 451265 2 11.300 192 204 212 . 20 451265 cor r. area 416825 363455 corr. * 100.00 87. 20 <320 + 322 )/ <332 +334) CALCULATION R-Global< 3) = 14.8821 <323')/<332 + 334) CALCULATION R-G1obal< 3) = .331? O n n (-> c* * r CPDEP, C10956 File >G16S 321.6-322.6 *mu .2UL -UT-31 14 SP2336 200-1/3^250 GT g> Ci' U> OJ s. CO \ 'I _o 0> CO Ol Cl If 01 \ CO r\t I CO 01 CO >--I 2) _l ZD Ol 3 tij - ^ C'J *'0 t Q` O'j CO > , T*--< Li' 'f o- I t~ ZD J O2l) 3 ti I- rio CO r r- U) Oj G* Li' MS data file header from : >GG168 Sample: 2UL UT-3114 Operator: GARY MS2 11/09/84 16:35. Mi sc : SP2330 208-1/3/250 GT BTLftl9BTLftl9 Sys. ft: 1 MS model: S7 .SU/HW rev.: Cfl ALS ft : 8 Method file: SP2330 Tuning file: APEI01 Ho. of extra records: 2 Source temp.: 258 Analyzer temp.': 265 Transfer line temp. : 265---'- 200, 250. 0 . 0 . 0 . Chr omat ogr aph ic timesi min. 1.0 25.0 0.0 0.0 0. 0 Chromt ographic deg/min: 3.0 0.0 0.0 0.0 0.0 M/Z = 333.9 First pe ak is baseline drop corrected area. Sec ond peak is targent sk immed corrected area. Peak ft R. T. fi rst max 1ast peak min. scan scan sc an width raw area corr area corr. * 1 12.164 240 245 250 10 23759 2 12.104 240 245 250 10 23759 9109 100.00 6349 69.70 M/Z = 331.9 First peak is baseline drop corrected area. Second peak is tangent skiMmed corree ted area. Pe ak ft R. T. f irst max 1ast peak min. sc an sc an sc an width raw area cor r. area corr. 1 12.104 242 245 250 2 1 2.104 242 245 250 8 18562 8 18562 7106 100.00 5590 78.67 332/334 CALCULATION R-Global< 0) = .7601 M/Z 32' 3 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak ft R. T. first min. scan 1 12.124 2 12.124 243 243 max sc an 246 246 1ast sc an 25G 250 peak width -r> 7 raw area 16139 16139 M/Z = 321.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak ft R.T. first max 1CLS t- pe ak min. scan sc an s c an width raw area 1 12.124 240 246 255 15 50273 2 12.124 . 240 246 255 15 50273 I corr. area 6 108 504 4 corr, y. 10000 82.58 corr. ar e a 29318 2334 0 corr. 100.00 79.61 C10958 tl/2 = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Feak # R.T. fi rst max 1ast peak min. scan sc an scan width raw area 1 % 12.124 2 12.124 241 - 246 241 24 6 254 254 13 43223 13 43223 corr, area 22410 13094 corr. Ji 100.00 88.74 320/322 CALCULATION R-G 1C 'b a l < 1> = .7644 M/Z = 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. R.T. first max 1ast peak min. sc an sc an sc an width raw area 12.124 242 246 252 12.124 242 246 252 10 33539 Id 33539 corr. area 11939 9289 corr. * 100.00 77.80 C320 + 322)/C332 +334) CALCULATION R-GlobalC 3) = 3.1901 <328')/<332 + 334) CALCULATION R-Global< 3) - .3604 sr* SUBJECT TO ? iCTECnVE C.iDEH. onr> re C10959 File -601 69 i.TiU 2L U T - 3 1 1 S P2330 200-1/3/250 GT lD.O T m'Ts 11.0 11 .5 13.0 iV . s Fils- >G01 69 3 3 7 . 6 - 3 2 8 . 6 a m u . ^ U L U T - 3 1 1 5 1I ' 1 1 I 13.0 13.5 ' 1' ' ' ' ! ' 14.0 14.5 1?.0 SP2330 200-1/3/250 GT File >G0169 321.6-3: 6 aniu -- U L U T - 3 1 1 5 1O00 . A .. .V './W 'I.'V X J 'W ji' ` 'V y,-- SP2330 2 S 0 - 1/3/250 GT 1.1-" T 1 i i-- i--i--i i ]--i i--i--i--] i i i --i--|--i--i--i--!--|--i--r -1--I ]-- 1--1-- [--1--J-- 1--1-- 1-- 1--|--I I I ! --|--I- 1--1--1--| 10 . 0 1 0 . 5 1 1 . 0 1 1 . 5 1 2 . 0 1 2 . 5 1 3 . 0 1 3 . 5 1 4 . 0 1 4 . 5 1 5 . 0 > GO1 69 3 1 9 . 6 - 3 2 0 . 6 iTiU, 2U L U T - 3 1 1 5 S P 2 3 3 0 2 0 O - 1 / 3 / 2 5 0 GT n n n tr*y , \..L j C10960