Document LKdnL9gvbgarRkYad8pXyEEV7

i! r r MONSANTO COMPANY / DAYTON LABORATORY / DAYTON, OHIO 45407 ESC/DAYTON (Department/Section) ANALYTICAL___________ (Type of Report.) aa u b* I CO r~ * (M o fct W H 0H fr. 0 01 IK 01 z a: REPORT NO.: MDA-565 JOB/PROJECT N O .: 484.4420 /^DA^E: 8 January 1985 PERIOD COVERED: TITLE: Analyses of Wipes for 2,3,7,8-TCDD AUTHORS: G * Thomas ABSTRACT: Wipe samples from the Nitro plant were analyzed for possible concentrations of 2,3,7,8-TCDD. The results of these analyses are shown in this report. TECHNICAL APPROVAL: Jc P . L . Sherman Sr. Research Group Leader in io in i gg SS g APPROVED BY: 1^?. C^~ ______________ R. F. Iv.dry C ) Environmental Sciences Center Service Project Manager APPROVAL DATE : /- 'J T RESTRICTED DISTRIBUTION: (see over) COMPANY CONFIDENTIAL This document it the property of Monsanto Company and the recipient it responsible for its safekeeping and disposition! xt contains CONFIDENTIAL INFORMATION which must not be reproduced, revealed to unauthorized persons or sent outside Monsanto Company without proper authorization. CONFIDENTIAL SUBJECT TO PROTECTIVE ORDER. 011059 DISTRIBUTION COPY NUMBER 1-3 M. Townsend, Nitro Plant 4 F. Kearney, St. Louis-E3NA 5-7 T. Bistline, St. Louis-E2ND 8 G. Thomas 9 R. F. Ivory 10 Technical Reports Library - R2C 11 Central Files ABSTRACT ONLY H. A. Woltermann NOTE: Distribution of this report is restricted. Requests for additional copies should be made through the principal contact at the Monsanto location involved or the Manager, Environmental Sciences Center, Dayton Laboratory, Dayton, Ohio. ACKNOWLEDGEMENT Contributions of the following Dayton Laboratory personnel to this project are gratefully acknowledged: Analyses: G. L. Thomas CONi^fcaNTIAL SUBJECT TO PROTECTIVE ORDER. C11060 0-1088(0 DOCUMENT CONTENTS Cover S h e e t .......... .......... Document Contents .............. Report ........................ Document Inventory Form ........ Sample Receipt Form ............ Chain of Custody Form .......... Analysis Request Form .......... Monsanto Notebook Pages For: a. Extraction/Preparation b. Analysts/Data Reduction Instrument Logbook Pages . . . . Computer Output and Chromatograms Additional Documentation . . . Page 1 3 4 9 10 11 13 14 15 16 17 70 OOO' ***' A \ v z u A., G11061 ANALYSIS REPORT FOR 2,3,7,8-TCDD IN HI.TRO SAMPLES INTRODUCTION On 18 Dac 84 eight 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--04-- 12-- 18--01. 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 analyzed. 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 chlorlne-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, 20X potassium hydroxide and water. The hexane was then dried with 10 grams of anhydrous sodium sulfate. Each sample was than 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), CONFIDENTIALchlorlne-37 labeled 2,3,7,8-TCDD (m/z 328), and carbon-13 labeled 2,3,7,8-TCDD (m/z 332,334). 00004 SUBJECT TO PROTECTIVE ORDER. C11062 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. Ocrni, CONuFx I*D- . ENTIAL SUBJECT TO PROTECTIVE ORDER, C11063 TCTjn DATA REPORT . NCWANTO C O M . PAYTON .ASORATCSY RF SCRLCFRfCJRACOTUtIt'TJpEEal:l SP12,,913923180 SiWE KWFR ........ *tfc 3 4 r A 7 ft 8 HIGHSPIKE ETTR NTHD J J J J J J J J J J NR CLEAN TCOO D.L. -- -- -- BC 1.15 BC .94 -- K NO .27 BC NO .11 BC D . 1 BC 1.24 - RC 1.28 BC .89 BC KO .14 BC 104.74 - 918) ANALYTICAL 370 337. X DATE TI 322 334 ACC ---- -- 320 12019 12/19 12/19 t2/l9 17/19 1041 .30 lint .82 1122 t m 1142 HH 1202 IH .80 (08. .81 103. ` .31 108. .80 108. .80 104. 4210. 3991, 0. 0. 0. 12/19 12/19 12/19 12/19 1242 .83 1302 .80 1322 .83 134J t m .80 107. ,81 tQ8. .81 107. .81 108. 7473. 5934, 4523. 0. 12/19 1442 .80 .79 109. 394327, 322 257 3ZJ* 332 314 N 5238, 3404, 119452. 105329. 132008. 4881. 3180. 130100. 121734. 149508. 0. 0. 87404. 72743. 90242. X 0. 0. 207749, 177494. 222731. 1 0. 0. 115823. 104544. 129977. X 8978. 4848, 192439. 170592. 213347. 7449. 3994. 151415. 1348 . 14MS15437, 3918. 141143. 143444. 177987. 0. 0. 152741. 135474. 147008. 1 493303. 145039. 122085. 104074. 13*320. CORRECTEDFOR OONTRIfdlOWHi NATIVE TOO (SUBTRACT ,009'OF N/E 322) KITE COOES* XI ISOTOPE RATIO OUT OF ACCEPTABLE RANGE yj Z KCLRACy OUT OF acceptable RANGE KEtfCTHCO BLAME R=PMTIAL SCAN R*PSP4TE C IW IW AND OTWI> (^OtFLICATEdtfTERLAB) FB=F1EL0 BLANC L.feNATI TOO SPIKES MWCT DETECTED a*tETECTl(K LIRIT iKJU FILENAit TC0C33 SUBJECT TO PROTECTIVE ORDER, C11064 TABLE 2. CALIBRATION .SUMMARY ug/Kg NATIVE TCDD 0.5010 5.010 50.10 1.2515 12.515 125.15 RRF (NATIVE) 0.9868 0.B551 0.8558 0.9019 0.8881 0.8551 DATE' 12/19 12/19 12/19 12/19 12/19 11/27 TIME 1001 1021 1222 1422 1505 1525 RRF (SURROGATE) 1.123 1.224 2.174 1.017 1.895 1.798 GTT2X 00007 SUBJECT TO PROTECTIVE ORDER, C11065 TABLE 3. QUALITY CONTROL SUMMARY ITEM SURROGATE ACCURACY SPIKE RECOVERY ff DATA POINTS 10 1 MEAN S.D. 107.2 1.7 * * Not technically correct to report recoveries for internal standard calculated results. GTT3X >1 r O O fifiS ^ r1 n A L Iti*. C11066 DOCUMENTATION INVENTORY FORM Monsanto Research Corporation Dayton Laboratory I. Sample Information Sample Identification: ^ / IK o Number of Samples: ^ Analyte: Matrix: \y Method: p<jf(rrTiovt"* o" 75 Documentation Control in Soil 3**^ StJi ft 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 /-W-/7-/jV/) Cg) Extraction/Freparatlon notebook pages (NBP) (h) Analysis NBP j Y 3 J 7 b Instrument Logbook pages / Computer Data Files hard copy output <?> *7 r Chromatograms U > Data Reduction NBP 3 7 3 7 b (j) Final Report (k) Additional Documentation (note immediately upon acquisition) Stenda reiS Prepa * y -- --- -- Is' y y \y y i/ y y y fctuir' jrftyr* &fyu.r~ f&a.tr' prfULtT' File Complete (signature) CONFIDENT0I0A0 0L9 SUBJECT TO PROTECT!VT n p n r o /(date) C11067 Sample Receipt Form Monsanto Research Corporation Dayton Laboratory Customer Id e n tific a t io n : N F iX O _________________________ MRC Log Number: V S i * f 1 ' (8 I______________________ A ir b il l Number: -- "" Date; i 3? "D tX . Sample Receipt Inform ation: (a) Shipping Containers (b) Custody Seals (c ) Chain o f Custody Forms (d) Sample Tags (e ) Sample Containers ( f ) Agreement o f Sample Documentation j ntact^ present damaged (d escribe below) No. \ In itia ls Sr /a b se n j)(d e sc rib e ^---- "sealin g below) in ta c t____ <Sir absent N o.Jl absent No. S damaged (d escribe below) No.?^_ & ~ r no (d escribe d iscrep an cies) l. Additional D escription (1 f sample numbers not lis t e d on chain o f custody form, l i s t here and contact SMO). ) v* (T tf T / f? 00O10 ,rv % Y SU3JPI TC r^ 'JTEm V E CRDEiL '( S ig n a t u r e ) C11068 CHAIN OF CUSTODY RECOUD U) O EO m K- q * ' i- MRC JOD NUMBER _ CUSTOMER Rfc'PRfSCHTAIVE trH J L CONTRACT NUMBER MRC CONTRACT MANAGER PLANT AME 0 CODE V^.'W > MRC TEAM LEADER (S p e c ific Information on samples is a v a ila b le on attached "Sample Id e n tific a tio n Log*) H 9 Lsi I < m ... Q u-* 70 *. O `'e m K--' *t O o Signatures Team Leader V e rific a tio n o f Collected Samples: Relinquished by: Received by: Relinquished by: Logged-!n- by: Received Received fo r A nalysis by: Method o f Shipment: Oate Time Remarks $.0 Number o f C o n tain ers: K Special In stru c tio n s (Sample p re se rva tio n , s e c u r it y , d e liv e ry to e t c .) 2 H Z 2 _____ S 1 /fr-L-- gr.^1 ^ 2-------- fS~tr U;c.kcdc*^ { C s P ^ r^ A . .'Ci, r/i\\ O h its Y V Q 7 O o 05 <o i' SAMPLE IDENTIFICAI ION LOG MRC Job'Ha. _________ ___________________ _ Contract No. '_________________ P la n t Name or Code ^3\.v^o ________ _ Customer Representative \ S e - it H ( V l . u f i l L . MRC Contract Manager___________________ _ _ Team le a d e r __________ ________________________________ Semn ng Location K. / k V .3 lo.. 3 \i H to, f M , s> U7 Lj 2 Rur, data Type of Sa^pie & Muriber Sanpled fo. o f Containers A n a ly sis Required ampie recovered" By ( i n i t i a l s ) and Conment \Z-'H LAS* MlTT^O PAft 3 ,1 7 V - 7>6f) CAft a( _ t-AG (Lol~J<bCA\SOKYe\AP^#U0 , - ____ _ r ____________ 1 Vf "hA/T^rv "pA 7 9 'S*.n/c T>a yrpA> 7ati 10P hi3u.i<Orm P*t> Ib? aF UcJu* Asura. _ nir&o T>a -74 rti no " i t i 1________ 1i i i r r r-- 1 i - . . . L . L _____________ - . . -- 00012 C11070 ANALYSIS REQUEST Sl>cCdi|DATE LOG NO. MONSANTO RESEARCH CORPORATION REQUESTER , DAYTON LABORATORY . bi I I f -_AMPLE DESCRIPTION MJMBER OF BOTTLES: , * CHARGE NO. t -'M I L- Lfc 3NUMBER OF SAMPLES - MO l 1u ^AAJ --ti*UV,,-.ii L. so- jt- Lr\h . Ap, *v^ liMh- V.*) rji-,,*-1 ~'A (.Mv -/ iA\- - ' T i 'uv, Ai) . >*\fJ? 9 - VA, iTM. _.s L-t. - i - -N ) V- -7r ; \**' L-Vu- :'* JS' ;|V *::/] iV' i S i^^ -\ ) RECORDED BY: REQUIRED ANALYSIS' / W ' REPORT RESULTS TO FILES /KU LIK \\ V ANALYSIS REQUEST FILES z'JYfj.- c '~i N SAMPLES FOR: V SAMPLE LOCATION C Su KNOWN HEALTH HAZARD PRESENTED BY SAM PLE: REFERENCE TO PREVIOUS WORK (REQUEST#, JOURNAL,ETC.) COMPLETION DATE TIME ALLOTED FOR ANALYSES ANALYST HOURS INST. TIME ANALYTICAL TECHNIQUE GAS CHROMATOGRAPHY ULTRAVIOLET V IS IB LE INFRARED EM ISSION . EDAX XRF- M ICROSCOPY OTHER O llA L SEMI QUANT NMR HPLC O XRD IC P ATOMIC ABSORPTION M ASS SPEC IS s C /M S ' AUTO ANALYZER QUANT, REQUIRED QA/QC C c T i f y j ^ y r * IQ t v-<3r ir*T a t3 :f >:UBJEv:T 1u ^UTECTIVE ORDER O 1 3 " SAMPIE DISPOSAL: APTES REPORT COMPIETE 'f-| ,,DIS,,C,,AR,,D *| --J| RETURN OHOLD FOR 30 DAYS t u Tw cnoM flTTnN M iKTR FSIlPPlTFD BY ANALYSIS REQUEST ORIGINATOR O t t DAYS C11(171 OT> A J i ^ o A h "* HM- *WXX\ MONSANTO COMPANY N? 2831620 P P C P ARGO BY ttONATUREJL, . 'iiict ^ - & < y i t c A T I Xatt & U l __ M 'tfo bifts SheeX G>J No. . I P - V T 3 W ? . ff fA)t (fu fhck ____ 3Zb8_ j ^/9 r /t y* 3 Oari*R ol ^ ,, 1 35 70 327 4 pW e.idM ff.f W ,,.fW Bhi< 7< )8h . $(? C P 79 _ 3 2 7 2 "? AIP '6hX.tovSe "7 9 3 2 ? V #<9 &, to s 7 9 ?2 7 5 " L ^ck c * ^ 6 k *c. Lo V f - 3 277 >- f . ----------- flniT.. O ------- - by Sf.tal by ^7 3 1 /uMuru. aI C/f\f*lKtcr'Y( C>3 (O \s 1/ Q ch sa-fiU ree.um r\J v / j t/ LJ 0 Str/<ju.ti(A#i/]'fr$M h f v f /.w 't/.i'q 1 y^ >/ v; . `/O m ! M ! u 1/ i/ i/ j Mi/ lo ii f f i c u rtr a . J `^t/6 fahl*. T t n ------ --- . SUBJECT TO PROTECTIVE ORDER. 00014 ABAO ANO UNOCAATOOO BV "TC11072 MONSANTO COMPANY N? ,,2,,273276 ccrcuw spas fiF 7?.^ .379 P SMORBICI 1.12; W .F aw n i ** 3 4 5 4 7 8 .19 HI SPIKE SU rrra PMlYnCflL 3 33? I mW GJEM TOT O.L. UTE nie 322 334 arc 3 322 757 351* 332 334 4 JK j EC VX jX X gX uX 9> X ti X 4X 1.13 - 12/14 1041 .00 .30 ica. *210. 5733. 3404. 117452. 101377. 32CC3. .94 -- 12/14 1101 .32 .31 103. 3731. fit. 3130. 1X100. 171734. UTWS. ,V 12/14 1122 ft .31 ICS. 0. 0. 0. 824. 77743. 70742. 1 * .11 12/1* 1142 H .30 108. 0. 0. 3. 702747, 177474. 777731. I X .18 I/1* 1202 HW ,30 104. 0. !>. 3. 115373. 1Q4544. 177927, t i.:* - 12/14 17*2 .33 .30 1C7. 7473. 3778. 43. 177437. 17C592. 2131*7. 1.73 - 17/14 4vW4 .33 ,31 :C8. 5734. 7147, 3784. 51115. 343R5. IMfifl:. .3? - 12/14 1322 .33 .31 107. *K5. 5*37. 3713. 14H43. 143444. 177737. KO .14 12/14 13*2 H .31 108. 0. 0. 0. 152741. 135474, 147C83. X 1C4.74 - 12/1* 1**2 .77 107. ' 39433. *93353. IM039. 177035, 10/074, 134370. OTSETED FCR OTTm TIi BVKATtVC TOT tSQTMrr .007 HF !i/f3771 resasi n isespe sATto nur iy arcEPTjau: rucs viiaccwrvcirrcfiseptrie; -wmna aus p^st:* za $?? iichi & ran* XiFLCSTiXTHjai fWTP.3 auac ..WttTp.E TOT SPIKES i* * r CETCTD OE.*CFTECTCSriIIT kl TTOT3 fOTTO 9RKJJ0 1 < --- -------------------------- :____________ H ?p Analyst n O -^0 --1 f VA -- ^ V - w\ C C -J- it' o-i sJ\ - V* V :. w Jt?. V?cVC* -c< KOi i ^ V ~ - -VS, C* AVP-K-. '^", 4 V/ Cvo -rv^jyj 1 o Vw1| _ oO >K<?0i SV 1 " * 5i w* -P\ co rt s & fi Voltane M n i <c Ico O Q 3 *$ O M -'J f^ -.j 3 S^ ;7 frv ry ^-.1 s <,' ^ tefe " g fJ o c* < -<*-C LaJV ^ N*>- *J jw -- Vu\ ' S s l W^^ sT / C- ALS Bottle Number && - K* V o R & > m o * o vt Ul *a r^i o Ui > (C\ ` File >B3442 333.6-334.6 amu.2UL 0.1002/.43/.20 SP2330 200-1/3/250 BTL File >B3442 327.6-323.6 amu.2UL 0.1002/. 43/, 20 SP2330 200-1/3/250 BTL File >B3442 321 .6-322.6 amu.2UL 0.1002/.48/.20 SP2330 200-1/3/250 BTL -- File >B3442 313.6-320.6 amu.2UL 0.1002/ .43/ .20 SP2330 200-1/3/250 BTL File >B3442 256.7-257.7 amu.SUL 0.1002/.48/.20 SP2330 200-1/3/250 BTL--- C11076 MS data file header from : >B3442 Samples 2UL 0.1002/.48/.20 Operators GARY MS 12/19/34* -1-0r0ir Mi sc : SP2330 200t 1/3/250 BTL#03BTL# 3 Sys. #i 1 MS models 87 SW/HW rev.i Cfl ALS # 0 Method files SP2330 Tuning files APEI01 Mo. of extra rei Source temp.i 258 Analyzer temp.* 0 Transfer line 11 Chromatographic temperatures s 8. 0. Chromatographi c times, min. : 0.0 ' 0.0 Chromatographic rate, deg/min: 0.0 0.0 0. 0.00.0 0. 0.0 0.0 00. 0. 0.0 M/2 = 333.9 First peak is base 1ine drop corrected area. Second peak is tangent sk immed correc ted area. Peak * R.T. first max 1ast peak min. scan scan scan ui dt h rau area corr. area corr. 1 11.469 212 215 226 2 11.469 212 215 226 14 160949 133551 100.00 14 160949 130401 97.64 M/Z = 331.9 F irst peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R. T. first max 1ast peak min. scan scan scan wi dth rau area corr. area corr. `4 `i 11.469 211 215 230 2 11.469 211 215 230 19 146639 112933 100.00 19 146639 109522 96. 98 332/334 CALCULATION R-Global< 0) a .3456 - M/Z 327.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak mi n. scan^ scan scan uiidth rau * corr. area area 1 11.498 212 216 220 2 11.490 212 216 228 8 L31339 115579 a 131339 99627 M/Z = 321.9 F irst peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R. T. first max 1ast peak min. scan scan scan ui dth rau area corr. area 1 11.490 2 11.490 . 7 v ` 'i r 213 213 216 227 216 227 a A L SUBJECT TO PROTECTIVE ORDER. 14 54304 14 54304 0CO19 29216 26605 co%rr. 100.00 86.20 corr. Ji 100.00 91.06 C ll s M/Z = 319.9 First peak is baseline drop corrected area. Second peak 1s tangent sk itnmed corrected area. Peak 4 R.T. first max 1ast peak min. scan 3can scan width raw area 1 11.490 212 216 224 2 11.490 212 216 224 12 ' 43110 12 43110 > 3 34i* corr. area 21558 19306 corr. * 100.00 91.87 320/322 CALCULATION R-G1obal< 1) = .7379 } M/Z => 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak 4 R.T. first max 1ast peak min. scan scan scan widt h raw area 1 11.510 213 217 226 13 40302 2 11.510 213 217 226 13 40302 ' corr.' corr. area Ji 11333 100.00 10930 96.46 <329 + 322)/<332 +334) CALCULATION R-Global< 3) ^ .2060 <320')/< 332 + 334) CALCULATION R-Global< 3) = .4678 ^ O !jjl. ocnco C11078 File >B3443 333.6-334.6 -amu.2UL 1.002/.43/.20 SP2330 200-1/3/250 BTL- 40000- 20000- 0I1i'i 1i1i1i -- i-- >-- i-- -- r~ i*' i ' i * t 't -|-- i-- 1-- i-- -- i-- <-- i 10.0 10.4 10.3 .11.2 11.6 12.0 12.4 12.3 13.2 13.6 14.0 File >B3443 321.6-322.6 -amu.SUL 1.002/.43/.20 SP2330 2O0-1/3/250 BTL-.;: File >B3443 319.6-320.6 amu.SUL 1.002/ .48/ .20 SP2330 2O0-1/3/250 BTL--- File >B3443 256.7-257.7 amu.2UL l`.0O2/.43/.20 SP2330 2O0-1/3/250 BTL;::: MS data, file header from : >B3443 Sample: 2UL 1.092/.48/.20 Operator: GARY MS 12/19/84 10:21 Mise : SP2330 200-1/3/250 BTL405BTL# 5 Sus. #: 1 MSmodel: 37 SW/HW rev.i Cfl fiLS # : 0 Method file: SP2338 Tuning file: APEI01 Ho. of extra records: 2 Source temp.: 250 Analyzer temp.: 0 Transfer line temp. : 0 - I Chromatographi c temperatures : Chromatographic times, min. : Chromatographic rate, deg/m in: 000.. 00. 00.0. 00. 000.. 00. 000.. 00. 000.. 00. M/Z a 333.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak mi n. scan scan scan width raw area corr. area corAmr. 1 11.495 208 213 225 2 11.495 208 213 225 17 190450 160593 100.00 17 19045O 156654 97.54 M/Z = 331.9 F irst peak is baseline <drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. fi rst max 1ast peak min. scan scan scan wi dth raw area corr. area coA'rr. 1 11.515 210 214 225 2 11.515 210 214 225 15 154735 127510 100.00 15 154735 124562 97.69 332/334 CALCULATION R-Global< 0) = .7940 M/Z = 327.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan ui dth raw area 1 11.515 210 214 223 2 11.515 210 214 223 13 184240 18 184240 M/Z * 321.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak 4 R.T. first min. scan 1 11.515 2 11.515 211 211 max scan 214 214 1ast peak scan wi dth 227 16 227 16 raw area 320991 320991 corr. area 149554 146764 cor'Ar. 100.00 93. 13 corr. area 290655 284407 cormAr. 100.00 97.35 SU1iPiJr r~r vT 00022 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 peak mi n. scan scan sc an u idth rau area 1 11.536 211 215 222 2 11.536 211 215 222 11 ,244228 11 244228 >&3M J corr. area 223625 210793 corr, 5i 100.00 94.26 320/322 CALCULATION R-Global< 1> = .7694 M/Z = 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak ft R.T. f irst max 1ast peak min. scan scan sc an wi dth raw area 1 11.536 211 215 225 2 11.536 211 215 225 14 123296 14 123296 corr. area 92762 89990 corr. y. 100.00 97.01 <320 + 322)/< 332 +334) CALCULATION R-Global< 3) =* 1.7850 <323')/<332 + 334) CALCULATION R-Glbal< 3) = .5100 i\3 SUBJECT TO PROTECTIVE ORDER, 00023 C11081 File >63444 333.6-334.6 amu.2U>- UT-3267 SP2330 200-1/3/2SQ BTL File >63444 321.6-322.6 .amu.2UL UT-3267 SP2330 290-1/3/250 BTL MS data file header from >B3444 Sample! 2UL UT-3267' Operator I GARY MS 12/19/34 10141 .. Mi sc : SP2330 200-1/3/250 BTL407BTL# 7 Sys. #i 1 MS model! 87- SW/HW re .: CA ALS # ! 0 Method file* SP2330 Tuning file: APE 101 Ho. of extra records! Source temp.: 250 Analyzer temp.! 0 Transf er 1ine temp. 0 Chromatograph! c temperatures : 0. 0. 0. 0. 0. Chromatograph!c times, min. : 0.0 0 .0 0.0 0.0 0.0 0. 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 4 R.T. first max 1ast peak min. scan sc an sc an width raw area corr. area crr. * 1 11.497 213 216 228 2 11.497 213 216 228 15 159473 132008 100.00 15 159473 129138 97.36 M/Z a 331.9 First peak is baseline drop corrected area. Second peak is tangent sk immed corrected area. Peak R.T. first max 1ast peak min. scan scan scan width raw area corr. area cory.r. 1 11.518 213 217 223 2 11.318 213 217 223 15 132464 105329 1 0 0. 00 15 132464 103199 97.93 332/334 CALCULATION R-Globat < 0 ) = .7979 M/Z 3 327.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. * Peak # R.T. fi rst max 1ast peak min. scan scan scan width raw area corr. area 1 11.518 214 217 229 2 11.518 214 217 229 15 143244 119699 15 143244 116139 M/Z = 321.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan u i.dth raw area corr. area 1 11.538 ,, 2, tJLI.Sga,, 212 218 227 ?12 ,218 ft ~ 227 SUBJECT TO PROTECTIVE ORDER. 15 31518 15 31518 cu re 5233 4953 corr. V. 100.00 97.07 corr. 7. 100,00 94.56 .. finnan s M/Z = 319.9 Fi rst peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak . R.T. first max 1ast peak # mi n. scan scan scan width raw area 1 11.538 215 218 224 9 '20140 'll 2 11.538 2is 218 224 9 20140 > 6 3 4 <j4 corr. area 4210 4007 corr. * 100.00 95. 18 320/322 CALCULATION R-Global< 1) .8037 M/Z = 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak 4 R.T. first max 1ast peak min. scan scan scan width raw area 1 11.538 214 218 222 2 11.538 214 218 222 8 20846. 8 20846 corr. area 3606 3586 coVr, r. 100.00 97.23 <320 + 322)/<332 +334) CALCULATION R-Global< 3) .0398 <328')/<332 + 334) CALCULATION R-Global< 3) .5041 Q u k . \T G11084 File >B3445 333.6-334.6 amu.^UL UT-3263 SP2330 200-1/3/250 BTL File >B3445 321.6-322,6 a.mu.2UL UT-3268 SP2330 200-1/3/259 BTL File >B3445 319.6-320.6 amu.SUL UT-3268 SP2339 290-1/3/259 BTL File >B3445 256.7-257.7 amu.ZUL UT-3268 SP2330 2O9-1/3/250 BTL 2000- 1009- 0"t ' I ' 1 *--r I-- 1 1-- '-- 1-- '-- 1-- ' 1-- 1-- I-- I 1-- '-- I 1-- I-- 1-- I~r1 r-]--r--t-- i-- I-- r-- T-- r--| 10.0 10.4 19.8 11.2 .11.6 12.0 12.4 12.3 13.2 13.6 14.0 T\T' a I _ : l i , 0(;r>i'.v C11085 SUBJECT TO PROTECTIVE ORDER. MS data file header from >B3445 Samples 2UL UT-3268 Operators GARY MS 12^19/84 11:01 Mise : .SP2330 200-1/3/250 BTL09BTL# 9 Sys. #: 1 MS model : 87 SW/HW reu. : Cfl RLS # : 0 Method fi1ei SP2330 Tuning file: APEI01 Source temp.: 250 Analyzer temp e t 0 No. of extra records e Transfer 1ine temp. Chromatographi c temperatures : 0. 0. 0. 0e 0. Chromatographi c times, mi n. : 0.0 .0.0 0 .0 0. 0 0 .0 Chromatographs c rat e, deg/mi n: 0.0 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. f irst max 1ast peak min. scan scan scan width raw area corr. area corr. 1 11.515 210 214 225 2 11.515 210 214 225 15 174963 149508 100. 00 15 174963 144265 96. 49 M/Z = 331.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R ,T . first max 1ast peak min. scan scan scan width raw area corr. area corr. 'A 1 11.515 210 214 228 2 11.515 210 214 228 18 143514 121234 100. 00 16 143514 117402 96. 34 332/334 CfLCULRTION R-Global< 0) a .8109 M/Z - 327.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan width raw ' corr. area area coyr. r. 1 11.535 212 215 226 2 11.535 212 213 226 M/Z = 321.9 14 160846 130144 100.00 14 160346 123772 93.95 First peak is base 1ine drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan width raw area 1 11.535 212 215 221 2 11.535 212 215 221 9 20406 20406 corr. area 4831 4570 corr. * 100.00 93.63 Q C ilV ,'. C11086 M/Z =*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 scan sc an uidt h raw corr. area - area l 11.533 212 213 220 2 11.535 212 213 220 8 13141 8 13141 3981 3793 7& 3 W S corr. * 100.00 95.28 320^322 CALCULATION R-Global< 1) 3 .3156 M/Z = 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak 4 R.T. first max 1ast peak min. scan scan scan uidt h raw area 1 11.553 214 216 219 2 11.555 214 216 219 3 14230 5 14230 corr. area 3180 2843 corr. 5i 100.00 89.47 <320 + 322)/< 332 +334) CALCULATION R-Global< 3) =* .0327 <328')/<332 + 334) CALCULATION R-G1obal< 3) - .4303 00029 A, 'T i SUBJECT TO PROTECTIVE ORDER. C11087 File >B3446 333.6-334.6 amu 2UL UT-3269 SP2330 200-1/3/250 BTL File >B3446 321.6-322.6 amu.ZUL UT-3269 SP2330 2O0-1/3/250 BTL o r o 3 o C11088 MS data file header from : >B3446 Sample: 2UL UT-3269 Operator: GARY MS 12/19/84 11:22 Misc : SP2330 200-1/3/250 BTLft 11BTLft 1l Sys, ft: 1 MS model: 87 SW^HW reu.: Cfl ALS ft : 0 Method file: SP2330 Tuning file: APEI01 No. of extra records: 2 Source temp.: 248 Analyzer temp.: 0 Transfer line temp. : 0 *. Chromatographi c temperatures : 0. 0. 0. 0. 0. Chromatographi c times, min. : 0.0 0.0 0.0 0.0 0.0 Chromatographi c rate, deg/min: 0.0 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 ft R.T. first max 1ast peak min. scan scan sc an wi dth raw area corr. area corr. 7. 1 11.513 211 215 226 2 11.513 211 215 226 15 117442 15 117442 90262 100.00 97764 97.23 M/Z 3 331.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corr ec ted area. Peak ft R.T. first max 1ast peak min. scan scan scan width raw area corr. area cory.r. 1 11.513 211 215 225 14 96885 72763 100.00 2 11.513 211 215 225 14 96885 70012 96.22 332/334 CALCULATION R-Global< 0) 3 .8061 M/Z - 327. 9 First peak is baseline drop correeted area. Second peak is tangent skimmed corrected area. Peak ft R.T. f irst max 1ast peak min. scan scan scan width raw area 1 11.513 211 215 227 2 11.513 211 215 227 16 112326 16 112326 M/Z 53 321.9 F irst peak is baseline drop corrected area. Second, peak is tangent skimmed corrected area. Peak ft R.T. first max 1ast peak min. scan scan sc an width raw area 1 0.000 ' 228 2 0.000 228 0 227 0 227 -1 -1 0 0 C G ? C i'- A 7 00033. SUBJECT TO PROTECTIVE ORDER." * corr. area 32406 79942 corr. * 100.00 97.01 corr. area 1803 1803 corr. y* 100.00 100.00 Cl 10 89 5 M/Z 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 3can scan u idth raw area 1 0.000 2 0.000 223 228 0 227 -1 0 227` -1 0 0 > 3M(o corr. area 1809 1809 corr. 7. 100.00 100.00 320/322 CALCULATION R-Global< 1) = l.0033 M/Z = 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan width raw area 1 0.000 2 0.000 223 223 0 227 0 227 -1 -1 0 0 corr. area 2153 2153 corr. */. 100.00 100* 00 <320 + 322)/<332 +334) CALCULATION R-Global< 3) = .0222 <328')/<332 + 334) CALCULATION R-Global< 3) = .5054 SU L!J__: : _______ _ OC032 . C11090 File >B3447 333.6-334.6 amu.SUL UT-3270 SP2330 200-1/3/250 BTL File >B3447 321.6-322.6 -amu.2UL UT-3270^ SP2336 200-1/3/250 BTL C11091 MS data file header from : >B3447 Sample! 2UL UT-3270 Operator! GARY MS 12/19/84 11:42 Mise ! SP2330 200-1/3/250 BTLftl3BTLftl3 SUS . ft! 1 MS model! 87 SW/HW rev .: CA ALS ft ! 0 Method file* SP2330 Tuning fi1ei APEI01 Ho. of extra records: 2 Source temp .1 250 Analyzer temp.* 0 Transfer line temp. : g Chromatograph ic temperatures ! 0. 0. 0. 0. 0. Chromatograph! c times, min. : 0.0 0.0 0.0 9.0 0.0 1 Chromatograph! c rate, deg/min: 0.0 0.0 0.0 0.0 0.0 M/Z = 333.9 F irst peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak ft R.T. first max 1ast peak min. scan scan scan uidth raw area corr, area coXr,r. 1 11.596 210 214 224 2 11.506 210 214 224 14 247707 222731 100.00 14 247707 215430 96.72 M/Z =* 331.9 F irst peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak ft R.T. first max 1ast peak min. scan scan scan uidth raw area corr. area corXr. 1 11.506 211 214 225 2 11.506 211 214 225 14 204163 14 204168 177694 100.00 173949 97.39 332/334 CALCULATION R-Global< 0) = .7978 M/Z = 327.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak ft R.T. first max 1ast peak min. scan scan scan uidth raw area 1 11.526 211 215 225 2 11.526 211 215 ` 225 14 230609 14 230699 M/Z = 321.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak ft R.T. first max last peak min. scan scan scan width raw area 1 0.000 2 0.000 226 226 0 225 0 225 -1 -1 0 0 -i corr. area 202749 197590 corXr. 100.00 97.46 corr. area 1735 1785 corXr. 100.00 100.00 G11092 s M/Z o 319.9 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 0.000 2 0.000 226 226 0 225 0 225 -1 -1 0 0 7-6 3^i7 corr. area 1772 1772 corr. * 100.00 100.00 320^322 CALCULATION R-G1obal< 1) * .9924 M/Z = 257.8 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 scan width raw area 1 0.000 2 0.000 226 226 0 225 0 225 -1 -1 0 0 corr. area 2151 2151 corr. 5i 100.00 100.00 <320 + 322)/<332 +334) CALCULATION R-Gl obal < 3) => .0089 C328')/<332 + 334) CALCULATION R-Global< 3) = .5063 \ T 000X5 <1 `y-1 -- --'i.L.J.i ;3 - t -- x-4 SUBJECT TO' PROTECTIVE ORDER. C11093 SP2330 280-1/3/250 BLT m_J L(VPI C\O N (VII (QV_I M 0L(V0PI \ CO \ I (VJ (CVLI CO F i l e >B3448 333.6-334.6 amu.2UL UT-3271 (CVOI (VJ I _r(VJoI 00 (VI CID CO (ZV)J De CO co (CVOI VD I(VVI. (O vf vf CD (VJ CcVqOf (VI vf m /V (VI u. amu.2UL UT-3271 SP2330 200-1/3/250 BLT 11094 MS data file header from >B3448 Samples 2UL UT-3271 Operator! GARY MS 12/19/84 12:02 -Misc : SP2330 200-1/3/250 BLT#15BTL#15 Sys. #i 1 MS modeli 87 SW/HW rev.! CA ALS # i 0 Method filei SP2330 Tuning file* HPEI01 No. of extra records: 2 Source temp.i 250 Analyzer temp.: 0 Transfer line temp, s 0 Chromatographi c temperatures i 0. 0. 0. 0. 0. ,,, Chromatographi c times,' min. : 0.0 0.0 0. 0 0. 0 0.0 I- Chromatographi c rate, deg/mim 0.0 ' 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 4 R.T. first min. scan 1 11.506 2 11.506 210 210 max scan 214 214 1ast peak scan w idt h 225 15 225 15 raw area 155377 155877 corr. area. 129927 125599 corAr. 100.00 96.67 - M/Z =* 331.9 Fi rst peak is baseline drop corrected area. Second peak is tangent skimmed corrected area.1 Peak R.T. f irst max 1ast peak min. scan scan scan width -raw area corr. area corr. */. 1 11.506 211 214 226 2 11.506 211 214 226 15 131604 104544 100.00 15 131604 101559 97. 14 332/334 CALCULATION R-Global< 0) = .8046 M/Z = 327.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak mi n. scan scan scan width raw . corr. area area 1 11.526 212 215 226 2 11.526 212 215 226 14 145349 115923 14 145349 113232 M/Z * 321.9 F irst peak is baseline >drop corrected area. Second peak is tangent sk immed corrected area. Peak * R.T. fi rst max 1ast peak min. scan scan scan width raw area 1 0.000 2 0.000 227 227 0 226 0 226 -1 -1 0 0 corr. area 1736 1736 coyr. r. 100.00 97.31 - corr. * 100.00 100.00 ; - *'~l SUBJECT TO PROTECTIVE ORDER. onori? C11095 s M/Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent sk immed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan wi dth raw area 1 0.000 2 0.000 227 227 0 .226 0 226 -l -1 0 0 corr. area 1772 1772 covr. r. 100.00 100.00 320/322 CALCULATION R-Global C l-> = 1.0207 M/Z = 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak 4 R.T. first max 1ast peak min. scan scan scan width raw area 1 0.000 2 0.000 227 227 0 226 0 226 -1 -1 0 0 corr. area 2131 2131 corr. 100.00 100.00 <320 + 322)/<332 +334) CALCULATION R-Global< 3) .0150 <328')/<332 + 334) CALCULATION R-Global< 3) a .4939 000-8 C11096 File >B3449 333.6-334.6 amu.2UL 10.02/. 48/.29 SP2330 200-1/3/259 BTL- * File >B3449 321.6-322.6 amu.2UL 10.92/ .43/ .29 SP2339 290-1/3/259 BTL- SUBJECT TO PR nnrrT n/r n o n n MS data file header from : >B3449 Sample! 2UL 10.02/.49/.20 Operator* GARY MS 12/19/84 12i22 Mise s SP2330 200-1/3/253 BTLitl7BTL# 17 Sys. #: 1 MS'model : 37 SU/HW reu .i CR ALS # ! 0 Method fi lei SP2330 Tuning fi 1es APEI01 No. of e>:tra records: Source temp.i 250 Analyzer temp,: 0 Tran sfer 1ine temp. Chromatographic temperatures i 0. 0. 0. 0. 0. Chromatographi c times, min. : 0.0 . 0.0 0.0 0.0 0.0 Chromatographi c rate, deg/mini 0.0 0.0 0.0 8 .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 1ast peak mi n. scan scan scan ui dth raw area corr. area, corr. * 1 11.540 213 219 226 2 11.540 213 219 226 13 375536 352524 100.00 13 375586 344119 97.62 M/Z = 331.9 Fi rst peak is baseli ne drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. fi rst max 1ast peak min. scan scan sc an ui dth rau area corr. area corr. * 1 11.540 213 219 228 2 11.540 213 219 223 15 311230 285295 100.00 15 311230 279340 97.91 332/334 CALCULATION R-Global< 0> * .3093 M/Z =* 327.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak it R.T. first max Iast peak mi n. scan scan scan ui dth rau area 1 11.560 213 220 225 2 11.560 213 220 225 12 659443 12 659443 M/Z = 321.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. R.T. min. ------------ 11.560 11.560 f rst scan ----- 215 215 max scan --- -- 220 220 last scan -- 227 227 peak ui dth -- ---- 12 12 rau area --- -- -- 6397695 6397695 corr. area 635033 530627 corr. * 100.00 83.55 corr. corr. area '/. -- --- -- -- ------ 6369733 100.00 6229515 97.80 00040 C11098 M/Z = 319.9 First peak is baseline drop corrected area. Second peak is tWigent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan sc an w idth raw area 1 11.560 216 220 228 2 11.560 216 220 223 12 5116912 12 5116912 corr. area 5025148 4966198 >8 . corr. Ji 100.00 98.83 320/322 CALCULATION R-GlobaK 1> - .7989 M/Z = 257.0 First peak is baseline drop corrected area. Second peak is tangent sk 1mined corree ted area. Peak 11 R.T. first max 1ast peak min. scan scan scan width raw area 1 11.560 216 220 230 2 11.560 216 220 230 14 2017666 14 2017666 corr. area 1969254 1946945 corr. /. 100.00 98.87 <320 + 322>/<332 +334) CALCULATION R-Global< 3) =* 17.8655 <328')/<332 + 334) CALCULATION R-Global< 3) .9058 ni^;^ j ^ r r i a l SUBJECT TO PROTECTIVE ORDER. 00041 C11099 File >B3450 333.6-334.6 amu.2UL UT-3272 I SP2330 200-1/3/250 BTL File >B3450 327.6-329.6 amu.2UL UT-3272 SP2330 200-1/3/250 BTL File >B3450 321 .6-322.6 4inu.2UL UT-3272 SP2330 23O-1/3/2S0 BTL C 11100 MS data file header from >B3450 Samples 2UL UT-3272 Operatori GARY MS 12/19/34 12i42 Mise i SP2330 200-1/3/250 BTL#19BTL#19 Sys. #1 1 MS modeli 97 SW/HW re .i CA ALS tt : 0 Method file! SP2330 Tuning file* APEI01 No. of extra 'records! 2 Source temp.i 250 Analyzer temp.: 0 Transfer line temp. : 0 Chromatograph! c temperatures : 0 . 0 . 0 . 0 . 0 . Chromatographi c times, min., : 0 .0 0.0 0.0 0. 0 0.0 Chromatographic rate, deg/mini 0 . 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. f irst max 1ast peak min. scan scan scan width raw area corr. area coyr. r. 1 11.506 210 214 225 2 11.506 210 214 225 15 238802 213347 100.00 15 233302 206537 96.31 M/Z * 331.9 Fi rst peak is baseli ne drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan ui dth raw area corr. area coyr.r. 1 11.527 210 215 226 2 11.527 210 215 226 16 199520 170592 100.00 16 199520 166048 97.34 332/334 CALCULATION R-Global < 0> =* .7996 M/Z 327.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak R.T. first max 1ast peak min. scan scan scan ui dth raw area 1 11.527 212 215 225 2 11.527 212 215 225 13 220262 13 220262 M/Z a 321.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak R.T. first max 1ast peak min. scan scan scan width raw area t 11.547 213 216 222 2 11.547 213 216 222 9 25907 9 25907 L.-.4* j T SUBJECT TO PROTECTIVE ORDER. ^ 0 0 ^ 3 corr. area 192520 138425 coyr. r. 100.00 97.87 *" corr. area 8978 8789 cory.r. 100.00 97.89 C l1101 s W/ Z = 319.9 First peak is base line drop corrected area. Second peak is tangent skimmed corrected area. Peak # R. T. first max 1ast peak min. scan sc an scan width raw area 1 11.547 213 216 223 2 11.547 213 216 223 10 26183 10 ' 26183 >6 3'H5 corr. area 7473 7303 covr%r. 100.00 97. 73 320/322 CALCULATION R-Gl obal < 1) a .8324 M/2 a 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak tt R.T. first max 1ast peak min. scan scan scan width raw area 1 11.547 214 216 221 2 11.547 *214 216 221 7 . 20443 7 20443 corr. area 4868 4388 corr. J: 100.00 90. 14 <320 322)/<332 +334) CALCULATION R-Global< 3) a .0423 <328')/<332 + 334) CALCULATION R-Global< 3) = .5012 \\ sue.,. \, .. '\ on<M4 C11102 File >B3451 333.6-334.6 amu.2UL UT-3273 SP2330 200-1/3/250 BTU File >B3451 321.6-322.6 amu.2UL UT-3273 * SP2330 200-1/3/250 BTL MS data, file header from >B3451 Samplei 2UL UT-3273 Operator: GARY MS 12/19/84 13:02 Mise : SP2330 200-1/3/250 BTL#21BTL#21 Sys. #: 1 MS model: 87 SU/HW rev.: Cft ALS ft : 0 Method file: SP2330 Tuning file: APEI01 No. of extra records: 2 Source temp.: 230 Analyzer temp.: 0 Transfer line temp. : 0 Chromatographi c temperatures : 0. 0. 0. 0. 0. Chromatographic times, min. : 0.0 0.0 0.0 0.0 0.0 Chromatographic rate, deg/min: 0.0 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. first max 1ast peak min. scan scan sc an width raw area corr. area corr. W 1 11.508 214 217 228 2 11.508 214 217 223 14 191195 166051 100.00 14 191195 161459 97.23 M/Z = 331.9 . First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak R.T. first max 1ast peak mi n. scan scan sc an width raw area corr. area coryr. . 1 11.528 214 218 228 2 11.528 214 218 223 14 159869 134305 100.00 14 159669 130794 97.02 t-- 332/334 CALCULATION R-Global< 0> a .8118 M/Z = 327.9 First peak is baseline drop corrected area. Second peak is tangent sk immed correeted area. Peak # R.T. first max 1ast peak min. scan scan scan ui dth raw area 1 11.528 215 213 228 2 11.528 215 213 . 228 13 178652 13 178652 M/Z = 321.9 First peak is baseline drop corrected area. ' Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan width raw area 1 11.548 216 219 227 11 26941 2 11.543 216 219 227 11 26941 SUBJECT TO PROTECTIVE ORDER. corr. area 151432 147355 cory.r. 100.00 97.61 corr. area 7449 7080 corr. * 100.00 95.05 C1110J s M/Z 3 319.9 First peak is base 1ine drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan wi dth raw area 1 11.543 216 219 223 2 11.543 216 219 225 9 22125 9 22125 y 6 3 iS I corr. area 5934 5745 corXn. 100.00 96.81 320/322 CALCULATION R-G1obal< 1) a .7966 M/Z 3 257.0 *L*. 11. peak is baseline drop corrected area. Second peak is tangent sk immed corrected area. Peak 4 R.T. first max 1ast peak min. scan scan scan ui dth raw area 1 11.548 216 219 223 2 11.548 216 219 223 7 19363 7 19363 corn. area 3934 3731 corn. 5 100.00 94.90 <320 + 322)/<332 +334) CALCULATION R-Global< 3) = .0443 <328')/<332 + 334) CALCULATION R-Global< 3) = .5033 ..... . ; - 7rr~^ 5 " /)l-*ir-*A7- C11105 File >B3452 333,6-334.6 amu.2UL UT-3274 SP2330 200-1/3/250 BTL File >B3452 321 .6-322.6 amu.2UL UT-3274 SP2330 200-1/3/250 BTL File >B3452 319.6-320.6 amu.2UL UT-3274 SP2330 200-1/3/250 BTL MS data file header from : >B3452 Samp 1ei 2UL UT-3274 * Operator! GARY MS 12/19/84 13i22 Mi sc : SP2330 200-1/3/250 BTL#23BTL#23 Sys. M i 1 MS- model! 87 SW/HI4 reu.i Cft ALS # : 0 Method filei SP2330 Tuning file: APEI01 No. of extra record! 2 Source temp.i 250 Analyzer temp.: 0 Transfer line temp. : 0 Chromtographi c temperatures ! 0. 0. 0. 0. 0. Chromatographic times, min. : 0.0 0.0 0.0 0.0 0.0 I Chromatographic rate, deg/min: 0.0 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. ftrst max 1ast peak mi n. scan scan scan width raw area corr. area corr. 1 11.520 210 214 224 2 11.520 210 214 224 14 202720 177932 100.00 14 202720 173761 97.63 M/Z 331.9 F irst peak is base line drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. fi rst max 1ast peak min. scan scan scan width raw area corr. area corr. * i 11.520 210 214 223 2 11.520 210 214 223 13 166115 143664 100.00 13 166115 139036 96.78 332/334 CALCULATION R-GlobalC 0) * .8072 M/Z 327.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R. T. first max 1ast peak min. scan scan scan width raw area 1 11.540 210 215 225 2 11.540 210 215 225 15 190577 15 190577 M/Z =* 321.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak R.T. first max 1ast peak mi n. scan scan scan width raw area 1 11.540 2 11.540 211 215 221 211 215 221 10 10 :**1* * N - \>i i--- ;n 23097 23097 corr. area 161192 156609 corr. 5 100.00 97. 16 9^ corr. area 5437 5182 corr. i 100.00 95.31 C11107 s M/Z = 319.9 F irst peak is baseline drop corrected area. Second peak is tangent sk immed corrected apea. Peak R.T. first max 1ast peak min. scan scan scan ui dth raw area 1 11.540 212 215 221 2 11.540 212 215 221 9 . 20428 9 20428 corr. area 4525 4426 co%rr. 100.00 97.81 320/322 CALCULATION R-GlobaU 1) .8323 M/Z 237.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan sc an width raw area l 11.540 212 215 221 2 11.540 212 213 221 9 23016 9 23016 corr. area 3918 3648 corr. >i 100.00 93.11 <320 + 322)/<332 +334) CALCULATION R-Global( 3) .0310 <328/)/<332 + 334) CALCULATION R-G1oba1< 3) = .5010 A f : :s o SUBJECT TO ?=OTEC ' VE OR**D' EiR~,>xri C11108 File >B3453 333.6-334.6 amu.SUL UT-3275 SP2330 200-1/3/250 BTL File >B3453 321.6-322.6 amu.2UL UT-3275 ' SP2330 200-1/3/250 BTL MS data file header from >B3453 Sample: 2UL UT-3275 Operator: GARY MS 12/19/84 13:42 Mise : SP2330 200-1/3/250 BTL#25BTL#23 y Sys. it: 1 MS- model : 87 SW/HW rey .: CA ALS it : 0 Method file: SP2330 Tuning file: APE 101 No. of extra records: 2 Source temp.i 238 Analyzer temp.: 0 Transfer line temp. : 0 Chromatograph!c temperatures : 0. 0. 0. 3. 0. Chromatographic times, min. : 0.0 ' t 0.0 0.0 0.0 0.0 Chromatographi c rate, deg/mi n: 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 tangent skimmed corrected area. Peak # R.T. fi rst max last peak min. sc an scan scan width raw area corr. area corr. V. 1 11.502 213 216 223 2 11.502 213 216 228 15 194788 167083 100.00 13 194788 163130 97.63 M/Z 3 331.9 F irst peak i3 base 1ine drop corrected area. Second peak is tangent skimmed corrected area. Peak tt R.T. first max 1ast peak mi n. scan scan scan width raw area corr. area cor'4r. 1 11.523 213 217 230 2 11.523 213 217 230 17 165359 135626 100.00 17 165359 132438 97.65 332/334 CALCULATION R-Global< 0) .8117 M/Z = 327.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak it R.T. first min. scan 1 11.323 2 11.523 213 213 M/Z * 321.9 max scan 217 217 1ast peak scan ui dth 238 17 239 17 raw * corr. area area 185976 152741 135976 149001 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. R.T. first max 1ast peak min. scan scan scan width 0.000 0.000 231 231 0 238 0 239 -1 -1 J, \j_L "4 !i SUBJECT TO PROTECT,V :r . *52 raw area 0 0 corr. area 1802 1302 cory.r 100.00 97.55 cory.r. 100.00 100.00 cimo M/Z = 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 scan scan width raw area 1 0.000 2 0. 000 231 231 0 230 0 230 -1 -1 0 0 76 3 ^ 3 corr. area 1794 1794 co%rr. 100.00 100.00 320^322 CALCULATION R-GlobaK 1> = .9956 M/Z 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak ft R.T. first max 1ast peak min. scan scan scan width raw area 1 0.000 2 0.000 231 231 0 230 0 230 -1 -1 0 0 corr. area 2175 2175 corr. 7. 100.00 100.00 <320 + 322>/<332 +334) CALCULATION R-Global< 3) * .0119 <328')^<332 + 334) CALCULATION R-Global < 3) =* .5045 '4 t< cum F i l e >B3454 333.6-334.6 amu.SUL UT-3276 SP2330 200-1/3/250 BTL File >B3454 321.6-322.6 amu.2UL UT-3276 SP2330 200-1/3/250 BTL File >B34S4 256.7-257.7 amu.2UL UT-3276 SP2330 200-1/3/250 BTL SUBJECT TO PROTECTIVE ORDER. G11112 MS data file header from : >B3454 Sample: 2UL UT-3276 Operator: GARY MS 12/19/84 14:82. Mise : SP2330 200-1/3/250 BTL#27BTL#27 Sys. tti 1 MS'model : 37 SU/HW rev. : Cfl ALS # : 0 Method file: SP2330 Tuning file: APEI01 No. of extra records: Source temp.: 250 Analyzer temp .: 0 Transfer 1ine temp. : Chromt ograph ic temperatures : 0. 0. 0. 0 0. Chromatographi c times, mi n. : 3.0 -, 0.0 0. 0 0. 0 0.0 Chromatographi c rate, deg/mim 0.0 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 1ast peak min. scan scan scan width raw area corr. area coyr. r. 1 0.000 2 0.000 231 231 0 230 0 230 -1 -1 0 1751 100.00 0 1751 100.00 M/Z =* 331.9 First peak is baseline drop corrected area. Second peak is tangent sk immed corrected area`. Peak # R.T. first max 1ast peak min. scan scan scan widt h raw area corr. area corr. % i 0.000 2 0.000 231 231 0 230 0 230 -1 -1 0 1736 100.00 0 1736 100.00 332/334 CALCULATION R-Global< 0) a .9914 M/Z = 327.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak * R.T. first max 1ast peak min. scan scan scan width raw area corr. area 1 0.000 2 0.000 231 231 0 230 0 230 -1 -1 0 1940 0 1940 M/Z = 321.9 First peak is baseline drop corrected area. Sec ond peak is tangent skimmed corrected area. Pea*k R.T. first max 1ast peak min. scan scan scan width raw area corr. area 1 0.000 2 0.000 231 231 0 230 0 230 -1 -1 0 1781 0 1731 corr. Ji 100.00 100.00 corr. 100.00 100.00 5 C11113 s tV2 = 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 scan scan width raw area 1 0.000 2 8. 000 231 231 0 .230 0 230 -1 -1 0 0 com. area 1717 1717 com. * 100.00 100.00 320/322 CALCULATION R-Global< 1) .9641 M/Z a 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak .R.T. first max 1ast peak # min. scan scan sc an width raw area 1 0.000 2 0.000 231 231 0 230 0 230 -1 -1 0 0 corr, area 2955 2055 c oXm . 100.00 100.00 <320 + 322)/<332 +334) CALCULATION R-Global< 3) = 1.0029 <328')/<332 + 334) CALCULATION R-Global< 3) = .5516 SUBJECT TO P307 L/i C11114 File >B3455 333.6-334.6 amu.2UL .2503/.49/. 20 SP2330 200-1/3/250 BTL-- File >B3455 321.6-322.6 amu.2UL .2503/.43/.20 SP2330 200-1/3/250 BTL- G11115 MS data, file header from : >B3455 Sample* 2UL .2503/.48/ .29 Operator* GARY MS 12/19/84 14*22 Mise * SP2330 200-1/3/250 BTL#29BTL#29 Sys. #i 1. MS modeli 87 SU/HU rev. * CA ALS it * 0 Method f1lei SP2330 Tuning file* APEI01 No. of extra records* 2 Source temp.i 250 Analyzer temp .* 0 Transfer line temp. * 0 - Chromatographi c temperatures 1 0. 0. 0. 0. 0. Chromatographi c times i mi n. * 0.0 '0.0 0 .0 0.0 0.0 Chromatographi c rate, deg/m in: 0.0 0.0 0 .0 0.01 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 1ast peak min. scan scan scan width raw area corr. area corr. y. 1 11.511 211 215 225 2 11.511 211 215 225 14 156520 131978 100.00 14 156520 127701 96.76 M/Z 331.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan ui dth raw area corr. area corr. y. 1 11.511 210 215 226 2 11.511 210 215 226 16 135374 107950 100.00 16 135374 103582 95.95 332/334 CALCULATION R-GlobaU 0) .8179 M/Z = 327.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak ft R.T. first max 1ast peak min. scan scan scan ui dth raw area 1 11.531 212 216 218 2 11.531 212 216 218 6 113307 6 113807 M/Z 321.9 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 scan ui dth raw area 1 11.531 212 216 225 2 11.531 212 216 225 13 13 ... WJ i'4 ; _ j 4` SUBJECT TO PROTECTIVE ORDER. " r 3 86205 86205 corr, area 102269 70481 corr. 100.00 68.92 corr. area 63169 60731 corr. * 100.00 96. 14 C11116 s tl/Z * 319.9 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 scan ui dth raw area 1 11.531 213 216 226 2 11.531 213 216 226 13 72934 13 72984 >&54S5 corr, area 49662 48039 corr. 100.00 96.83 320/322 CALCULATION R-GlobalC 1) .7862 M/Z - 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak 1* R.T. first max 1ast peak min. scan scan scan ui dth raw area 1 11.531 213 216 226 13 49277 2 11.531 213 216 226 13 49277 corr. area 22328 21704 co%rr. 100.00 97. 21 mm <320 + 322)/<332 +334) CALCULATION R-Global< 3) => .4703 <328')/<332 + 334) CALCULATION R-Global< 3) = .4239 7- \ T r-.vCi SCTTVE CRDEH.6; 000*9 C11117 File >B3456 333.6-334.6 amu.2UI_ UT-3277 SP2330 200-1/3/259 BTL :i f File >83450 321 .5-322.6 amu .2<JL UT-3277 SP2330 200-1/3/250 BTL SUBJECT TO PROTECTIVE ORDER* O ? T i o C11118 MS data file header from ! ,>B3456 Sampl e: SUL ,UT-3277 Operators GARY MS 12/19/84 Mi sc : SP2330 200-1/3/250 BTL#31BTL#3t Sys. #i 1 MS- mode 11 87 SU/HW rev. i CA ALS # 0 Method filei SP2330 Tuni ng file: APEI01 No. of extra records: Source temp.i 250 Analyzer temp .: 0 Transfer 1ine temp. ; Chromtographi c temperatures : 0. 0. 0. 0 0. Chromatographi c times, min. : 0.0 0.0 0 .0 0. 0 0.0 Chromatographi c rate, deg/mim 0.0 0.0 0.0 0. 0 0.0 M/Z a 333.9 F irst peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan width rau area corr. area coyr. r. 1 11.537 212 216 226 2 11.537 212 216 226 14 159982 134320 100.00 14 159982 132101 98.35 M/Z =* 331.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan wi dth rau area corr. area cor%Ar. i 11.537 212 216 225 2 11.537 212 216 225 13 130399 106076 100.00 13 130399 103913 97.97 332/334 CALCULATION R-GlobalC 0) = .7897 M/Z = 327.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak R.T. first max Tast peak mi n. scan scan scan width raw corr. area area 1 11.558 213 217 226 2 11.558 213 217 226 13 152228 126527 13 152228 123863 M/Z a 321.9 F irst peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak tt R.T. first max Tast peak min. scan scan scan width raw area corr. area 1 11.558 213 217 227 2 11.558 213 217 227 14 519977 14 519977 AL, 000. ------- -- ._ i Li w Cl -- r l.;!ir.v*fVK Otf.OKU, ` . 493503 483157 cor'Ar. 100.00 97.90 cor*Ar. 100.00 :: 97.90_ C11119 s M/Z a 319.9 F irst peak is base 1ine drop corrected area. Second peak is tangent skimmed corrected area. Peak 4 R.T. first max 1ast peak mi n. scan scan scan width raw area 1 11.558 213 217 226 2 11.558 213 217 226 13 419649 13 419649 >6 corr. area 396327 385732 cory.r. 100.00 97.33 320/322 CALCULATION R-Global< 1> .3031 M/Z = 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak * R.T. fi rst max 1ast peak mi n. scan scan scan ui dth raw area 1 11.558 213 217 226 2 11.558 213 217 226 13 193015 13 193015 corr. area 165039 160671 corr. * 100.00 97.35 <320 + 322)/<332 +334) CALCULATION R-GIobal< 3) = 3.7015 <328'')/<332 + 334) CALCULATION R-Global< 3) .5079 ., --jJ SUBJECT TO PROTECT V ORDER. C11120 File >B3457 333.6-334.6 amu.2UL 2.503/.48/.20 - 40000- SP2330 200-1/3/250 BTL- 20000- 0- 10.0 10.4 ' 10.8 \' I ' 11.2 r lir.6 ' 11it22.. 00t i t T ~ r 1 i 1 i 1 i 1 i i-- i 12.4 ' 12.8 13.2 13.6 14.0 File >B3457 331.6-332.6 amu.2UL 2.503/.48/.20 SP2330 200-1/3/250 BTL- Fi le >B3457 321.6-322.6 -amu.2UL 2.503/.43/ .20 SP2330 200-1/3/250 BTL- :*.. MS data file header from : >B3457 Sample: 2UL 2.503/. 48/. 20 Operator: GARY MS 12/19/84"l5r05 -- Mise : SP2330 200-1/3/250 BTL#41BTL#41 Sys. #: 1 MS.model I 87 SW/HW reo. CA ALS # : 0 Method fi lei SP2330 Tuning file: APEI01 No. of extra records: 2 Source temp.i 250 Analyzer temp.: 0 Transfer line temp. : 0 Chromatographi c temperatures : 0. 0. 0. 0. 0. Chromatographi c times, min. : 0.0 0.0 0.0 0.0 0.0 Chromatographi c rate, deg/min: 0.0 0.0 0.0 0.0 0.0 M/Z 3 333.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak * R.T. first max 1ast peak min. scan scan scan width raw area corr. area coyr*r. 1 11.521 207 210 220 2 11.521 207 210 220 13 178007 152722 100.00 13 178007 149576 97.94 M/Z - 331.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan ui dth raw area corr. area cor%r. 1 11.521 207 210 221 2 11.521 207 210 221 14 151238 126332 100.00 14 151288 123554 97.76 332/334 CALCULATION R-Gl obal < 0) = .8275 M/Z 3 327.9 First peak is base 1ine drop corrected area. Second peak is tangent skimmed corrected area. Peak 4 R.T. first max 1ast peak min. scan scan scan ui dth raw area 1 11.562 208 212 218 2 11.562 208 212 213 10 247964 10 247964 M/Z = 321.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan width raw area 1 11.542 2 11.542 208 208 211 211 ^ * .~jli '4 SUBJECT TO PROTECTIVE ORDER, 222 222 14 745665 14 745665 >^4 .* corr. area 226824 179939 corr. area 714193 700333 corr. V. 100.00 79.33 cory.r. 100.00 93.06 C11122 s M/2 = 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 scan scan width raw area 1 11.562 208 212 222 2 11.562 208 212 222 14 ,605571 14 605571 y z+ tsi corr,. area 578425 565776 corr. v. 100.00 97.81 320/322 CALCULATION R-Global < l) a .8099 - M/Z = 257.0 Fi rst peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak ft R.T. first max 1ast peak min. scan scan 3can width raw area l 11.562 208 212 222 2 11.562 208 212 222 14 268977 14 268977 corr. area 239297 234334 cor*Ar. 100.00 97.93 <320 + 322>/<332 +334) CALCULATION R-Gl obal < 3) = 4.6313 <328')/<332 + 334) CALCULATION R-Gl obal < 3) =* .7897 .j T jA L SUBJECT TO PROTECTIVE ORDER, '.O k S C11123 File >B3453 333.6-334.6 amu.2L)L 25.03/ .48/ .20 SP2330 200-1/3/250 BTL File >B34S8 321.6-322.6 amu.2UL 25.93/ .48/.20 SP2330 200-1/3/250 BTL CL'DJECT TO PROTECTIVE ORDER- MS data file header from : >B3458 Sample: 2UL 25.03/.48/.29 Operator: GARY MS 12/19/84"15r25 Mise : SP2330 200-1/3/250 BTL#43BTL#43 Sys. #i 1 MS modeli 8? SW/HW re CA ALS # : 0 Method file: SP2330 Tuning file: APEI01 No. of extra records: Source temp.: 250 Analyzer temp.: 0 Transfer line temp. : Chromatographic temperature* : 0 . 0. 0. 0. 0. Chromatographic time*, min. : 0.0 0.0 0.0 0.0 0.0 Chromatographic rate, deg/min: 0.0 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. first max 1ast peak min. scan scan scan ui dth raw area corr, area corr. 7. 1 11.569 2 11.569 M/Z 331.9 212 218 212 218 226 226 14 265886 246630 100.00 14 265886 236892 98.45 , First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak * R.T. first max 1ast peak min. scan scan scan ui dth raw area corr. area co%rr. i 11.569 212 218 226 2 11.569 212 218 226 14 221396 14 221396 193858 100.00 192199 99. 14 332/334 CALCULATION R-Global< 0) .8056 M/Z 327.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan width raw area . corr. area 1 11.590 214 219 227 2 11.590 214 219 227 13 468201 13 468201 422324 324206 M/Z = 321.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. R.T. first max !ast peak min. scan scan scan width raw area corr. area 11.590 213 219 226 11.590 213 219 226 13 10803684 10758432 13 10803634 16548668 SUBJECT TO PROTECTIVE ORDER. ,, j ^ corr. 5i 100.00 76.77 coVr, r. 100.00 98.05 TM G11125 s M/2 =< 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 scan scan width raw area l 11.590 213 219 223 .2 11.590 213 219 228 15 3654242 15 3654242 com. area 3615902 8487532 7 3VS~? coym. . 100.00 98.51 320/322 CALCULATION R-Global< 1) * ,8009 M/2 257.0 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. first max 1ast peak min. scan scan scan width raw area 1 11.590 213 219 223 2 11.590 213 219 228 15 3489204 15 3489204 com. area 3455499 3400336 c oym. . 100.00 98.40 (320 + 322)/<332 +334) CALCULATION R-GlobaK 3) 44.5912 <323')/<332 + 334) CALCULATION R-Global< 3) .7492 C11126 File >B3459 333.6-334.6 amu.DODECANE SP2330 200-1/3/250 RUN-v^.BT File >B3459 321 .6-322,6 amu.DODECflNE SP2330 200-1/3/250 RUNs^ BT *: File >B345'9 256.7-257 ,7 amu.DODECflHE SP2333 200-1/3/250 RUN.. BT*:r*. CDr^ZI^siNTIAL., SUBJECT TO PROTECTIVE ORDER./ -, C11127 SUBJKCT JOS NO. MONSANTO COMPANY * * * $ .1 0 0 )1 PNCPAflttO SY (SIGNATURE 7 \ o ^ IteM A A - N? 2273264 OATS 3l o<cT3 Y M3$ T*-4- Y<J^u ^ / . o o o i ^ Bs&'JZb - /.Ooo6 ^ ^ T&^P & - ^ 5foo."7*M- rt i . A - //^_ -tV < yv<. -- sb.o"7 -+ ^ t* - r 7JL0T--T*Jo$. bT-43C^>-47l0. jf)JKL.bJJ&S/2Tz>ofgSgJL ljuGyJ^rfj.u*^***oO%.dSta*2ML. CKU<^jy^ CcT'VC' ~ l^Cs ' T ^ ip p ^ & cJ l j (^ ^Aa^4tAJiX ^\oji y) l<3J^jxJt- J2;>fcLvi\diife j i 7 # ^* $ " r*-_ ^ Y^^l 3 j- T > > SJkfcJ J?) 3< ^ V W , fJ^J) ' - - - u^(S^.JL'./iy "U (fa- rt J J U ^ y iXc ) ^ f ^Jlrfb m * ^ yZl) /TO /*-. ~^r **&C * ~ c & 'd i7* r5*00 2 ,, ^ ^^S * i j f f i J L '3c / , ' o ^ c L /^- J ^d Z v n u d C u ^ / mJL h & d iJ / ) /C tA -$ - l r^ t J CV<, -- O' hrJL ^ - 5 O " 7 / &**c " ti^-6 *Q ~{ f / J r y C k & > ^ * ~ `0~5 3 -r-" ^ -u^/^2- d J ^ d & ./^D ^ m J I , AiTVX-, " ? %O "$ ***G^/*<J) 5twJL < ^ 0 * 5 d 7 - j ^ . Jji * f $ \f y t . o .5U?^3 ..f O v 7 0 7 :Jf ASAO ANO UNOSRSTOOO IT OATS ------ 12 C11128