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DISTRIBUTION COPY NUMBER 1-3 M. Townsend 4 F. E. Kearney 5-7 T. Bistline 8 R, Noble 9 G. Thomas 10 R. F. Ivory 11 Central Files 12 Technical Reports Library 1670 E3NA E2ND 1250 1250 1250 1250 R2C ABSTRACT ONLY 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. Thomas G. Pitts CO M PAN Y CONFIDENTIAL C11276 DOCUMENT CONTENTS Cover S h e e r ......................................................... Document Contents ................................................... Report .............................................................. Document Inventory ................................. . . . . . . . . Sample Receipt Forms ............................................... Chain of Custody F o r m s .......... ; ................................. Analysis Request Forms ............ . . . . . . ............ . . . Monsanto Notebook Pages For: a. Extraction/Preparation ................................... b. Analysis/Data Reduction . . . . . . . . ................... Instrument Logbook Pages ........................................... Computer Output and Chromatograms ................................... Additional Documentation . . . . . . ............................... Page 1 3 4 11 12 13 15 16 17 20 23 139 SUBJECT TO PROTECTIVE ORDER 0U CC3 C11277 All samples had 50 uL of dodecane keeper added to them and then they 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/HS 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 character 1st1c of both the native (unlabeled) 2,3,7,8-TCDO (m/z 257, 320, 322), chlorlne-37 labeled 2,3,7,8-TCDD (m/z 328) and carbon-13 labeled 2,3,7,8-TCDO (m/z 332, 334). 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 standards conformed to the levels specified by the method. RESULTS The results of the analyses of the samples are given In table 1, The tables also give all pertinent QA/QC information. It should be noted that small amounts of sample may lead to erroneously high or low concentrations due to possible 1nhomogene1ty of the sampleJ t SUBJECT TO PROTECTIVE ORDER, Ow rV-r - nW L^g C11279 TCDD DATA REPORT HCNSANTO CCiPANY. DAYTON LABORATORY TABLE la. SWEEPINGS GC CQUMs SP2330 & WTTVE: i.OOORF SURROGATE: l,50 ETTR KTHD ORAHS WET CLEAN u w t SURR PP8 ANALYTIC. 320 332 X TCDO D.L. DATE TINE 322 334 ACC 320 322 257 328+ 332 334 N DOOR J OORH J PEEN J lL J J RJ ;DOOR J *J 'AIN J FNER J O RF J OER J JST CO J ,.l BC 3.570 4.68 -- 9/7 BC 5.910 15.55 -- 9P 8C 1.700 1.99 -- 9/7 BC 2,010 3.87 -- 9/7 BC 4,580 ND .11 9/7 BC - 6,030 BC 3.940 BC 2.800 NO 8.24 13.56 .08 9/7 -- 9/7 -- 9/7 BC 4.360 12,51 -- 9/7 BC C 8 1 0 _97.7*\ -- 9/7 BC 5 ? 8 2 0 ^ 7 2 9/7 BC 1.120 3.05 -- 9/7 BC 1.260 ND BC 5.000 ND .29 9/7 .05 9/7 0503 .84 0523 ,76 0543 .81 0603 .80 0623 HH 0703 HH 0743 .75 0803 .69 0823 .73 0903 .67 0922 .73 0942 .80 1246 HH 1002 H H .86 100. .74 84. .87 105. .83 64. .74 63. .67 103, ,76 110. .79 118. .69 74, .81 128. .72 84. .69 65. .73 75. .84 90. 18882. 83727. 2709. 10577. 0, 0. 84155. 112218. 99006. 97684. 88864. 8451. 0. 0. 22496, 8719. 41604. 110660. 65853, 29751. 3358, 3246. 31486. 13269. 6672. 32783. 0, 0. 30429. 0. 0. 54167. 111929. 75663. 111576, 161839. 116064. 143014. 135442. 84807. 53068. 146866. 67821, 66480. 121024. 74700. 75374. 10520. 10379. 60689. 0. 0. 51944. Q. 0. 88063. 28586. 33353. 22426, 30462. 20803. 24016, 34763. 41898, 30539. 41192, l 31465. 46919. X 65192. 85792. 79736. 100672, 44015, 63417. 34523. 47703. 56049. 78200. 56861. 81910. 43098. 59336. X 66335. 78584. X iED FOR CONTRIBUTION BY NATIVE TCDO (SUBTRACT .009 OF H/E 322) . X: ISOTOPE RATIO CUT OF ACCEPTABLE RANGE Y: X ACUFACY aiT CF ACCEPTABLE RANGE 1 BLAWC 1 SCAN YTE SIGHING AND WORKUP :ate(interlab BUW< L.IWWTTVE TCDD SPIKES ND=NCT DETECTED DL=CTECTTON UNIT I. =TCDD94 C G r w '- S U B JtC T TO FROTECIiVc. ORDER, OGOC C11280 t TCDO DATA REPORT MCNSANTO Cn-PiWY, dayton LABORATORY TABLE la. SWEEPINGS (Continued) GC COUJW: SP2330 RE NATIVE: t.043 RF SURROGATE: .907 SA*LE N BER EXTR KTTC) ---- -- BASE O F STAIRS J CLEAN ---- BCD CRAMS WET U O tfT -- 1.180 SURR PPB ANALYTICAL 320 332 l T e tro D.L. DATE TIME 322 334 ACC 11,82 - 9/10 0844 ,72 .84 131. 320 5514. 322 257 328+ 332 334 7429. 4749. 10773, 10345. 12251, + 'ERECTED FOR CONTRIBUTION BY NATIVE TCDO (SUBTRACT ,009 OF H/E 322) WTE COOES: r. ISOTOPE RATIO a n OF ACCEPTABLE RANGE Y: I ACaRACY a T CF ACCEPTABLE RANGE W=NETHTO BLANK PARTIAL SCAN SEPARATE WEIGHING AND WORKUP tWIFU CATE(INTERLAB) f^-FIELD BLAMC l*H=NATIVE TCDO SPIKES ND=NOT DETECTED DL=DE7ECTI0N LIMIT KIAR F" P W =TCD096 SUBJECT TO PROTECTIVE ORDER. 0cG G 7 C11281 1 TCOO DATA REPORT WNSANTO COMPANY, DAYTON LABORATORY TABLE Lb. WIPES OC Cairti! SP2330 RF NATIVE: 1,000 RF SURROGATE: 1.480 SAWLE f (RFR SURR EXTR NG ANALYTICAL 320 332 X MTHO CLEAN TODD D.L. DATE TI> 322 334 ACC 320 322 257 328* -332 334 N INSIDE N UALL "TNSSTAOiER 1 SGER dryfw vac m > AMi 1 KioH SPIKE LOU SPIKE J J J J J J J J BC BO BO BO BC BO BC BC ND NO ND NP NO ND 18.15 6,54 .40 9/7 ,49 9/7 .42 9/7 .44 9/7 .52 9/7 .51 9/7 -- 9/7 -- 9/7 1022 H H 1304 H H 1326 H H 1344 H H 1404 H H 1451 H H 1511 ,72 1531 .82 ,71 44. .74 72. .76 74. .72 73. .69 82, .80 93, .70 88. 83 103. 0, 0. 0, 0, 0. 0. 18911. 4954. 0. 0, 0. 0. 0. 0, 26432, 8507. 0, 0. 0. 0, 0, 0, 17323. 7487, 45008. 39647, 48299. 45483. 42785, 49443. 39735. 43942. 40353. 33584. 40191. 37149. 30583. 33924. 26615. 27661. 56919. X 45152. X 53067. X 51649. X 44U0. X 42314. X 38083. 33383. CORRECTED FCR CONTRIBUTION BY NATIVE TCDD (SUBTRACT ,009 CF N/E 322) H)TE CODES: X: ISOTOPE RATIO OiJT OF ACCEPTABLE RANGE Y: l ACMWCY (XIT OF ACCEPTABLE RANGE NB=NETWD BLAHi PARTIAL SCAN =SEPARATE UE1GHINT. AND URWF [tOLFLICATE(INTERLAB) f^FIELO BLAW L>M=NATIVE TCDD SPIKES ND=NOT DETECTED OL=OETECTION UNIT =JAR -"".ENAflE =TCDD95 <^L A ' - J .y. ^ 71 VL SU3JECT TO PROTECTIVE ORDER CGC3 C11282 TABLE 2. CALIBRATION SUMMARY yg/Kg NATIVE TCDD 0.534 5.34 1.335 13.35 133.5 0.534 5.34 53.4 1.335 0.534 5.34 53.4 1.335 13.35 133.5 RRF (NATIVE) - 1.117 - 0.917 0.920 1.000 1.045 - 1.145 1.012 1.061 0.999 0.993 1.045 DATE 9/7 9/7 9/7 9/7 9/7 9/7 9/7 9/7 9/7 9/10 9/10 9/11 9/11 9/10 9/10 TIME 0423 0443 0843 1042 1102 1205 1224 1429 1554 2144 2204 0005 0205 1527 1547 RRF SURROGATE -- 1.712 - 1.808 1.520 0.906 0.919 0.848 0.896 0.900 . 0.970 SUBJECT i r) i'/E O R D E R - C11283 TABLE 3. QUALITY CONTROL SUMMARY ITEM SURROGATE ACCURACY //DATA POINTS 23 4 MEAN S.D. 88.9 20.3 * * Not technically correct to report recoveries for internal standard calculated results. i iY lA L S U 3 J E C T O P R O ! ACTIVE ORDER. -O .i.O 011284 DOCUMENTATION INVENTORY FORM Monsanto Research Corporation Dayton Laboratory I. Sample Information Sample Identification: ^ I T R o Number of Samples: )(p S A n a l y t e O , 3 ^ 0 - T c 3 > "D Matrix: Vy/pfS Method: j)rreR!VMfl.T)0^ o F 3 , V ; 3 - T C ) D // fc/i_ StsIME^ II. Documentation Control Copies Attached Initials (a) Sample Receipt Form (b) Internal Sample Tracking Form (c) Sample Tags (d) Airbill (Number ____________) (e) Chain of .Custody Form y --_ -- -- y <ST <ST -T < r (f) Analysis Request (Log Number /8/o9o43 /) ? t . _ (g) Extractlon/Preparatlon notebook pages (NBP) 2 7 3 A W 9 y (S r (h) Analysis NBP ____________ Instrument Logbook pages 15&fa"7H ,75 / <Sr _ y <5- r Computer Data Files ______________ hard copy output Chromatograms y &T <St (1) Data Reduction nbp <;e /ivfovsijs a/8P___ (j) Final Report j <$r <S-r (k) Additional Documentation <r _ (note lnmedlately upon acquisition) ,SrA^T>fK>S ? tf? rW ic ,/J / / B ? File Complete i W -'fj^elh (sfgjna'ture) -^ ,._i Vi. _,r.* j--*.'~j '4 3 OBJECT TO PROTECTIVE ORDER. O L O t.i n srrsi (date) C 1 1 2 R F> Sample Receipt Form Monsanto Research Corporation Dayton Laboratory Customer Identification: tlrfRO____________________ MRC Log Number: 1 - 0l- 0 5 >n 1__________________ Airbill Number: L . W C - Q v-k IaE?-__________ Date: H $g?r AS___________________________________ Sample Receipt Information: ( a ) Shipping Containers (b) Custody Seals ( 0 Chain of Custody Forms ( d ) Sample Tags (e) Sample Containers (f) Agreement of Sample Documentation C a n t a c i ) damaged (describe below) N o . J _ present Cahsin> (describe sealing below) intact ^presenf^ absent No. A . iresen')1 absent HO./la (''intact damaged (describe below) No./, C5D no (describe discrepancies) n .r x. St- (ST -- Additional Description (if sample numbers not listed on chain of custody form, list here and contact SMO). ^ W i t h Tnourff TFj fio fl?PtrfT T f f r f M S ^ H* 1*' PROTECTIVE ORDER* SUBJECT TO /> y\ IKmnAA QJi'gnature) 0CCJL2 C11286 SA .- m IDtKTIFICAT ION LOG HRC Job H a . ________________________ Customer Representative / v W Contract No. ________________________ MRC Contract Manager ____ ___________________ Plant Name or Code -M m * Team L e a d e r _____________________________ Samni1ng Rur. Date Type of Sample i Analysis Location Number Sampled No. of Containers Required Sample recovered 8y (Initials) and Conran \C Z S 7 ? 3 -7 ^ V,Q ' S aqO i ? r 2377 ( S - T ? '''D r * 3w\ S a s V 'Door' 6 * 7 4 fVl.-Di >c 3 T - ,<TiXyV) 7.3") 7 2.1 7? __ (a ifV\ ^ -7 q - ><? r > i,0?t<l )? tP L >vv T > a u l/alu<* oof" *2."i 7 a? T V i 2 ^ 5 L e o t l ^cre j y 7a/^, 3*>f iVr. cicSlla. - ^ f 2277 XS_A iCfA? H -7 3 "D ri S i i of* S-rv7*3 2.37? l< csr T2 - 7^ (V\.d[4*t s Ql-K sn ! "'baOX /c sn 1 > -7 ? yy,; ciJLL. S2i--Kls4^ >0UJ Car^^r* / C iA H oc ?-"> S lo ;9 r A '`e X c r v ' 5 /<?<: * )^ !i / . L1 . 1 1 <L. t A tA Oi sA 19 - J* "99 - FrdVi + r?r/iiO S'sT*C tc (Z . 7 ? - Hv-ti/D ( b ^ r /00r+^, Os_ IV 7 ? - `D/'i, / k . J iJc^CU O /M >M/Q r A7a -" X vs X S '/ 7 /< < A ____ S 4 f V - Tt ~ A-- /c- e J K- T] 9 - y - ? y C - ' v , -A' t... ..- - - ~ '--A; .-i0----JA."?-T-`- --.a--\ 71. SUEje c t r lAU/ ` '7CiWfc. OnOww Ot.o<r* C11287 CHAIN OF UnrODY RECORD fa ' fy s s s 1 2&8 HRC JOB HUMOUR ........................... ............ . CUSTOMER REWU'SCNTAU VL K S . /V/Z/'j- * CONTRACT NUMBER ________________________________________ W C CONTRACT MANAGER ____________________ PLANT NAME OR CODE y % K s v r ^ _________________ MRC TEAM LEADER _________________________ (Specific Information on samples 1s available on attached "Sample Identlflcatlon Log") O Signatures Date T Ime Remarks Team Leader Verification of Collected Samples: Relinquished by: Relinquished by: Logged-1n-by: Received by: Received by:tf a */*/&/ /2!oO e n ____________________________________ Y-:5o .J O Received for Analysis by: ____________ ________________ ^ ____________ Method of Shipment: U . r r i e r Kumber of Containers: / C o o /V - /6 v ' ------- Sp ed ai Instructions (Sample preservation, security, delivery to, etc.) . l \ t\ \f\t t.'i vt(- n . t-f 1 i p /S/S /fJ/c^Ais >6? \ i1 v- -----------------------------to - &. 7>u,^ ____________________________________________ , VjJ A y- **, o v y ^ y p y _____________________________________ I ; CO ------------------------ ^ A N A LY S IS REQUEST It ISANTO RESEARCH CORPORATION REQUESTER** DAYTON LABORATORY tlffitn VIPLE DESCRIPTION NUMBER OF BOTTLES: / > charge no." VM NUMBER OF SAMPLES ~ j^ *? REPORT RESULTS T0` FILES p SttF&AH 8 -t 9 X Y t / h W g r -fl w # / i > f A S r ' b o o Z ;-7 ? A ifi& Lt X " V f t T t o Ttot W i c l'7 //V it F t>osr tlArfk W / P F ANALYSIS REQUEST T FILES jT /o iC i 5 ttGWVl 3 - 7 ? Ai/DJLt s f c W T R Y ftc F -fl ' o-l 1 t t Y / V b ^ cV T l s t f E S V g o X T O P H - F f i & r l K r t $ S r f c < & / / o s l 'f c ' -7 7 A i t C L t " ^ / f s r 7# ) / / / 3 - 7? * y 4 a s f A P " ' ;-7 ^ /nitibLt SCT<rt S o u i H 'boc^ 8-71 AiS>Li Sl CTkW " i.-OUIRED A N A L Y S IS - / l W Co * a -f-ztfSi'bt F/i-Tsk 7f Tiw* RECORDED BY: SAMPLES FOR: THoW\<? SAMPLE LOCATION a ,3 , 7 , ? - T C i b i . KNOWN HEALTH HAZARD PRESENTED BY SAMPLE: REFERENCE TO PREVIOUS WORK (REQUEST#, JOURNAL,ETC. * 'COMPLETION DATE TIMEALLOTED FOR ANALYSES ANALYST HOURS INST. TIME ANALYTICAL TECHNIQUE GAS CHROMATOGRAPHY ULTRAVIOLET VISIBLE INFRARED EMISSION .* EDAXXRF MICROSCOPY OTHER -- ---- QUAL_____ SEMIQUANT. NMRI HPLC XRD ICP ATOMIC ABSORPTION MASS SPEC j^ g c /m s D AUTO ANALYZER __ QUANT_____ REQUIRED QA/QC ^ v-' - - s ~ . ! j. i A L , S U B J E C T T O P ^ r 7 r-TTi\/r r o n c o UH 2 8 9 t o o t m " w k E I CZI DISCARO RETURWJC G A 5*>LD FOR 30 DAYS f l 60 DAYS 07 MONSANTO COMPANY S U B JE C T JO B NO. f(ih / f y ' a l e i ! V& l- V211.7 N? 2273249 date lyC A y Ditc /-/?- <r o Mo. bt Ato-1 "Ctx S ^ e e t Code No. i / - O _LL03__ __ri.r.<^ir_ o r 2C M < jr 2 5 ~ J- >?r -~t Le ** My r *c~J ^s/^r U r J J j J mv SV. Xt '-T -?/J "> : '".zfif LT J / J S' u rjc u rjeso Ur Ji3 - j r _>b JJ. i **-*O--,<* *1A*T*J*-i-rm**."4jJi4*-.r'f-*T/JJ.m1i1f* V : *1 L' 7fr-W ur i JT -" Ji J 6 ; r T? U'- 7 ? ur -?jl U'"7 4 yr J ^ ' tyr JJ r.T Jfcrf ,.jr 's- >" / fr*H4rA-TiCT/*..-..^ r*'*.J -<*'*" r Z >hnni' Vr^t .le * L 7r**\ 4 'S-, V4*v w*A<**>'*A**'"4''w^"1 *1 'VV* *', Vi, f; *,, -1' 'V*-r l f t j i e J f .'u * t \ + $ ' `TV jy .k e uo*- A '-O '>/<f by oflJ*c*,.^ to Sfi'fceJt by cX uu\ LUZ. 3^pikivolf AWjo 3*57 a to JL Co t/ (O ^ Au*- SA**'--(.e _7_ ! 2,0/ *58 JL USfTS i*i-L S p r u it i 'Jw* P . *<T*r* 6 *'7 A/tL .7 *6 O J.L _o.j S isti / j o usra A*-u 5rt?Lc uSt> A l l ' Wc7> /*U- 5 A m ? L Olt Ai_l. 4**i_I" lSf /?uu S lnv,>. *u fluS1 ^ ~i * ? i 1 I uSti ^u- iV'li -* JO J 1 - /jl 7 10. iJ^/- jff'A"-/ -- -- J-A ' tcq O rfrj; SUBJECT 7~"T A T *_w*i ^M N C AO AMD U M O t M T O O D y O L O jJ 3 C11290 DATE MONSANTO COMPANY N? 227; 1ES0 DOTI PWT IWKTD CQPMA. Vn lOHT<pr w KamCaUTnMtW*i K1i..W80n0 s*nE ETTS IMF PU cum 1QO U . * lt -- -- -- ns:cE Mj. J r .*0 t/T mMSTop J K ,*1 1/7 max* J K FP .*7 1/7 n m r vr. m J 1C .u 1/7 .** J c Ml .37 1/7 * J K Ml .31 1/7 t*IO*SPUE J K 11.13 -- 1/7 i v u t J K .3* -- in UM 330 337 X TU 3S 33 320 3S 7Sf 370 333 33* N IOS MM IX MM 13 MM 1*4 MM 1*0 MM tai MM 1511 ,73 1331 .3 ,71 4. .7* 77. ,7 T*. .77 73. .1 7. 17, .70 a . .O 103. 0. 0. 0. 300. m 9Mlf. 1 0. 0. 0. 31?. 33BH. *9152. I 0. p. 0. TU. in . 33M7. 1 0. 0. 0. CHS. 371*1. 31*41. I 0. 0. 0. 7WB. xrm . *4110. 1 <L 0. o. *. 33171. Z1U. I itn i. 3n. (Tra. sirs. THIS. xnci. 15. men. 77. QHl. r**i. r r i . omero Fmrantitrnm r mti tob tsuratcr .amer <t m> nt OQDRi it ivnpt wtio a n cf atFT.t m c e r: KZitn Ult cf STAME ME U M L.WtfTtVIC TOB VU ES m uti. Sr m it errara fr*? uw M wo a c e ra n lwit . ( m u i!gkt::*te!u *> an FM1E10 L*N I FtLDMi raw. SUBJECT 'O P.OfEUlVE ORDER. KMAQ ANO UM OKHITOOO V 000.\7 Sl JECT MONSANTO COMPANY N? 2273252 T9BWlVOtT m m u mi.m t,tn>nrr wX aumt wnvci vis i.oo m amTti .m m e ff cn CT m ETTICM. no oe x ms xno asm KVT THU ILL me mc n u n no 38 257 32* S3 3to ---- " MC X 9T*US j ICS 1.1 u.n - 9/10 om* .72 .M Ul. SU. 7W*. 47*9. 10773. ine. 1831. otectp Faxnttmffta* t tus muer .00*x x/tini mt axe i:ISBTXET;cOUX ATTIMI AME ti ieawrranx itanmi Ma M T W C .M M W 7I H S t * Mpwt cioc o mo MiPLiriTTnmj) f#iL3K m l . W T I VC T a n X j g S UTEO n DLornncA uwn > jm F1UEMC MOFi i i SUBJECT PROTECTIVE ORDER. 011293 OLG! M CA D AMO U N O M I T O O O B r ATE Monsanto Rfsf.anoi Contonation HATTON l.AiiOBATOBT Su b je c t JOfl NO.. Da t e ------------------------------------------ 1)______Read And Understood Oy Me SlCHATURE --- -- ---------------- DATE................... IS MRC-DA N? I5r.67 IK>A3> i=Date CC Job Number Het Time Time of Day CRN 7920 AR Disc Pack FRN f r V r,lf X/ i i iP ol >^5^ ; I '! iI ' i : II !" : >1 'i c t* 'f 3. : V7.* V 'p '1 c*r W'Ol; I Of r^/*1 1Hit 1<'it l,t MM GC Conditions /j/tSc. Run KS Conditions Time K i l t Threi ADC KassR Del ?/..-l_/ l..I' \ H. o J o tr- ij a f " re 0 ui V -> x' G1'! 1 .V n- 1o r :"KU1 V to 0C023 C11297 File >B285 1 333.6-334.6 amu.2UI_ .1063/. 43/. 19 SP2330 200-1/3/250 BT File >B 2 3 S 1 321 .6-322.6 amu.2UL .1063/,43/.19 SP2330 200-1/3/250 BT 'J""71. . 4J. I A-* . -- . onA-rrrri'/E O R D ^ 0C024 C11298 GC/MS default file: >B2851::01 MS data file header from : >B2851 Sample: 2UL .1868/.48/.19 Operator: GARY Mise : SP2330 200-1/3/230 BTL#03 BTL# Sys. #: 1 MS model: 37 SW/HW reu.: CA Method file: SP2330 Tuning file: APEI01 Source temp.: 230 Analyzer temp.: 0 MS 9/07/84- 4:23 3 RLS 4 : 0 No. of e x t r a records: 2 T r a n s f e r line temp. : 0 C h r o m a t o g r a p h ic t em p e r a t u r e s : 50. 300. 0. 0. 0. Chromatographi c times,i min. : 0.0 2.0 0.0 0.0 0.0 C h r o m a t o g r a p h i c rat e , d e g / m in : 2 0 . 0 0.0 0 . 0 0.0 0.0 M/Z a 333.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R. T. f ir st min. sc an max scan 1ast peak scan width raw area corr. area corr. Ji 1 11.985 231 238 241 2 11.965 231 238 241 10 7 7 1 8 9 10 77 1 8 9 55769 32164 100.00 57. 67 M/Z = 331.9 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is ta n g e n t s k i m m e d c o r r e c t e d area. Peak # R. T. f irst min. sc an max sc an 1ast peak sc an w i d t h raw area corr. area corr. 1 11.965 196 238 232 2 11.965 196 238 232 86 212076 86 212076 39044 34135 100.00 S7.56 332/334 CALCULATION R-GlobalC 0) - .7001 M/Z = 327.9 SUBJECT TO First peak is b a s e l i n e d r o p c o r r e c t e d area, S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R. T. fi rst min. scan max sc an Iast peak scan width raw area corr. area 1 11.985 234 239 252 2 11.985 234 239 252 18 77420 18 77420 40394 38612 M/Z = 321.9 F i r s t peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak * 1 2 R. T. min. 11.985 11.935 f irst scan 236 236 max scan 239 239 1ast peak scan width 244 8 244 8 raw area 31404 31404 corr. area 14244 12784 d 'J corr. * 100.00 95.59 corr. y. 100.00 89.75 0025 C11299 S M/Z =* 319.9 First peak is baise 1 ne d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak n R.T. f irst min. sc an max sc an 1ast peak sc an u idth rau area 1 11,985 23 6 239 245 2 11.985 23 239 245 9 29683 9 29683 >Ba&5v- co r r . area 11035 10288 co r r . * 100.00 93.23 320/322 CALCULATION R - G 1o b a l < 1) a .7747 M/Z * 257.0 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R.T. f irs t min. scan max sc an 1ast peak scan width raw area 1 1 2 . 0 0 5 2 3 7 2 4 0 24 8 11 3 6 9 3 0 2 12.005 237 240 248 11 3 6 9 3 0 corr. area 8869 8456 corr. * 100.00 95.34 <320 + 322) / <332 +334) CfiLCULflTION R-Globai< 3) = .2666 <328' )/<332 + 334) CfLCULRTION R - G 1o b a l < 3) = .4247 "7 SUBJECT TO D"?ri irtr.CTiYE ORDER. 0G026 C11300 File >B2852 333.6-334.6 amu.2UL. 1 .068/.48/. 19 SP2330 290-1/3/250 BT File >B2S52 321.6-322.6 amu.2L 1 .968/.48/.19 SP2338 299-1/3/250 BT 0C0,7 Cl-1301 GC/MS default file: >B2852::01 MS data file header from : >B2852 Samp 1e: 2 U L 1 . 0 6 9 / . 4 8 / . 1 9 0perat o r : GARY Misc ; SP2330 200-1/3/250 BTL#05 BTL# Sys. #: 1 MS model: 87 S W / H U rev.: Cfl Method file: SP2330 Tuning file: RPEI91 Source temp.: 250 Analyzer temp.: , 0 MS 9 / 0 7 / 3 4 - 4 5 ALS : 0 Mo. of e x t r a records: 2 Transfer line temp. : 0 43' Chromatographic temperatures 50. 300. 0. 0. 0. Chromatographic times, min. 0.0 2.0 0.0 0.0 0.0 20.0 :0.0 0.0 0.0 0.0 M/Z = 333.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak . R. T. f irst min. sc an max scan 1as.t peak sc an u idt h raw area corr. area corr. X 1 11.990 233 238 240 2 11.990 233 238 240 7 78765 7 78765 64562 40461 100.00 62.67 M/Z = 331.9 F irst peak is b a s e l i n e d r o p c o r r e c t ed area. S econd peak is t a ngent s k i m m e d c o r r e c t e d area. Peak # R. T. f irst min. sc an max scan 1ast peak scan width raw area co r r . area corr. * 1 11.990 202 233 277 2 11.990 202 238 277 75 ` 196550 75 196550 44750 35862 100.00 30. 14 332/334 CALCULATION R - G l o b a l < 0) - .6931 M/Z = 327.9 First peak is b a s e l i n e d r o p c o r r e c t e d area, S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R. T. fi rst min. scan max scan 1ast peak sc an w idt h rau area 1 11.990 232 233 251 2 11.990 232 238 251 19 8 9 0 8 7 19 8 9 0 8 7 M/Z = 321.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R. T. f i r s t min. sc an max scan 1ast peak sc an w i d t h raw area 1 12.010 233 239 251 2 12.010 233 239 251 18 198299 18 198299 00028 J' corr. area 46052 459Q9 corr. X 100.00 99.69 c or r . area 161525 156530 corr. X 109.00 96.91 C11302 s HsZ = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak tt R. T. first min. scan max sc an 1ast peak sc an width raw area 1 12.051 237 241 253 2 12.051 237 241 253 16 119567 16 119567 corr. area 83727 83623 corr. */. 100.00 99.88 320/322 CALCULATION R - G l o b a l < 1) =* .7566 M/Z * 257.0 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is ta n g e n t s k i m m e d c o r r e c t e d area. Peak # R.T. first min. scan max scan 1ast peak sc an w idth raw area 1 12.051 237 241 248 2 12.051 237 241 248 11 1 1 1 2 3 9 11 1 1 1 2 3 9 corr. area 65853 65330 corr. 108.00 99.21 <320 + 322)/<332 +334) CALCULAT ION R - G 1o b a l < 3) = 3.6754 <328")/<332 + 334) CALCULATION R - G l o b a l < 3) = .5625 '.?j i I A L T TO PROTECTIVE CREER. ' 00035 C1309 file >B2855 333.6-334.6 amu.2UL UT-2625 3P2330 200-1/3/250 RUN BT File >B28S5 321.6-322.6 *mu.2UL UT-2625 SP2330 200-1/3/250 RUN BT C11310 s tl/Z = 319.9 First peak is baseline drop corrected area. Second peak is t angent sk imined corrected area. Peak # R.T. f irst min. sc an max scan 1ast peak sc an w i d t h raw area 1 12.050 239 : 241 242 3 9363 2 12.050 239 241 242 3 9363 corr. area 2709 2659 corr. 100.00 98. 15 320/322 CALCULATION R - G l o b a 1 < 1) = .8067 M/Z = 257.0 First peak is b a s e l i n e d r o p c o r r e c t e d area. Second peak is tangent s k i m m e d corre c t e d area. Peak # R. T. f irst min. sc an max scan 1ast peak scan width raw area 1 12.050 240 241 242 2 9286 2 12.050 240 241 242 2 9286 corr, area 3246 3187 corr. * 100.00 98. 18 <320 + 322)/<332 +334) C A L C U L A T I O N R-Global( 3) = .1354 <328')/<332 + 334) CALCULATION R - G l o b a l < 3) = .7025 c OG 028 fr\OTECTIVE ORDER, C11312 GC/r MS c Simp Mise Sys. Me Sou. M/Z Fir Sec oi Peak # 1 2 M/Z a F in Sec or Peak # 1 2 332/3 R-Glo M/Z = F irs Secon Peak # 1 2 M/Z = F ir s i Sec ont Peak # 1 2 File >B2S56 333.6-334.6 amu.2UL UT-2626 SP2330 200-1/3/250 F File >B2S56 321.6-322.6 amu.^UL UT-2626 SP2330 200-1/3/250 s Pt/2 - 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R. T. f i r s t min. sc an max scan 1ast peak sc an w i d t h raw area 1 12. 1 3 2 241 24 5 2 52 11 3 3 7 4 3 2 12.1 3 2 241 245 . 252 11 3 3 7 4 3 cor r . are a 10577 9829 corr. s *% 100.00 92.93 320^322 CALCULATI ON R - G l o b a K 1) = .7971 M/Z * 257.0 F i r s t peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # Ri T. f irst min. scan max scan 1ast peak scan width raw area 1 12.152 243 246 251 2 12.152 243 246 251 8 33332 8 33332 corr. area 6672 6624 corr. % 100.00 99.28 C320 + 3 2 2)/<332 +334) CLCULflTION R - G l o b a K 3) = .3111 <328 '>/<332 + 334) C A L C U L A T I O N R - G l o b a K 3) = .4276 C " --CT TO PSOiECTlVE ORDER. 0C041 C11315 amu.SUL UT-2627 SP2330 200-1/3/250 RUH CD 01 iS m CD CD OJ O nq CD CD CD CD 01 CD File >B2857 321.6-322.6 amu.SUL UT-2627 2P2330 200-1/3/250 RUN G1316 Ua GI' ti -to .* CO CO co CCll o co co TT-n o G> CP CJ -IO CJ -* r^- cj - Cl CJ KI r> - IO .Clli <Dn G> -- G) ^ C .| CO I IO CO 'o O' *-l ^ co - G> G> r- IO co CmJ CJ IO C'I o\> I G* Cl _ Ci Ci Cl. h- CJ \0 Cl --3 Cl eiDti r*. io CJ VO IO CJ N IO CJ co o- 00042 - t-- cijri n I i 1i--1 i> f' 0. o VuI til y ZL)O GC/MS default file.* >B2857::01 MS data file header from : >B2857 Samples 2UL UT-2627 Operators GARY MS 9/07/34 Mite : SP2330 200-1/3/230 RUN BLT#15 BTL#15 Sys. #: 1 MS m o d e l s 87 S W / H U reu.s Cfl A LS # : 0 Method files SP2330 Tuning file: APEI01 No. of e x t r a records: 2 Sourc e t e m p .: 2 5 0 A n a l y z e r temp.i: 0 Transfer line temp. : 6: Chromt ographi c t e m p e r a t u r e s : 50. 300. 0. 0. 0. Chromatographi c t im e s , min. : 0.0 2.0 0.0 0.0 0.0 Chromtographi c rate, deg/mins 20.0 0.0 0.0 0.0 0.0 M / Z =* 3 3 3 . 9 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak tt R. T. f irst min. scan 1 12.212 2, 1 2 . 2 1 2 246 246 max scan 249 249 1ast peak scan w idt h 253 7 253 7 raw area 92187 92187 corr. area 41192 39683 corr. ym 100,00 96.34 M/Z = 331.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak * R.T. f ir st min. scan max scan 1ast peak scan width raw area corr. area corr. y. 1 12.192 245 248 254 2 12.192 ,, 245 248 254 9 97418 9 97418 30539 29922 100.00 97.98 332/334 CALCULATION, R - G l o b a K 0) = M/Z = 327.9 .7414 V SUB First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t sk imm e d c o r r e c t e d area. Peak # R.T. fi rst min. scan max sc an 1ast peak sc an w i d t h raw area co r r . area 1 12.212 246 249 253 2 12. 2 1 2 L 2 4 6 24 9 253 7 87136 30429 7 87136 25973 M/Z = 321.9 F irst pe a k is- b a s e l i n e d r o p c o r r e c t e d area. -Second peak-^is tangent s k i m m e d c o r r e c t e d area. Peak # R.T. f irst min. sc an max sc an 1as t peak sc an w i d t h raw area corr. area 1 0.000 2 0.000 254 254 ' 0 253 0 253 -1 -1 0 2196 0 2196 corr. y 190.00 85.36 corr. y. 100.00 100.00 OC 043 C11317 S M/2 =< 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R. T. f irst min. scan max scan 1ast peak sc an ui dt h r au area 1 0.000 2 0.000 254 254 0 253 0 253 -1 -1 0 0 >$3S67 corr. area 12 1 9 0 2190 corr. i 100.00 100.00 320/322 CALCULATION R - G l o b a l C 1) = .9975 M / Z =* 2 5 7 . 0 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d p e a k is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R.T. fi rst min. scan max sc an 1ast peak sc an w i d t h raw area 1 0.000 2 0.000 254 254 0 253 -1 0 253 . -1 0 0 corr. area 4259 4259 corr. '4 100.00 100.00 (320 + 322) /< 3 3 2 +334) C A L C U L A T I O N R-G I o b a l ( 3) = .0512 (328')/(332 + 334) CALCULATION R - G 1o b a l < 3) = .4239 00044 _ C11318 Fil >B2859 20000-1 333.6-334.6 aiTiu.2UL UT-2628 10000H 10.0 File >B2859 T-i-- I-- r-- I-- 1-- r 1 --I--r--n --I--[--I--i--1--I--I--r 10.5 11.0 11.5 12.0 12.5 331.6-332.6 amu.2UL UT-223 SP2330 200-1/3/250 RUN ET SP2330 T-- -- J-- 1-- 1-- 1-- I-- ]-- I-- 1-- 1-- I-- I 14.0 , 14.5 15.0 2 0 0 - 1 / 3 / 2 5 0 RUN BT File >B2359 321.6-322.6 mu.2UL UT-2628 SP2330 200-1/3/2S0 RUN BT 2000-1 F ile \ \ \ i0 [ i t I--r------r ) I--I i - r-- --r t - | i i r i--r i i--[----i--i i-- ---t i i |- 1i i i | 10.0 10.5 11.0 11.5 12.0 12.5 13.0 13.5 14.0 14.5 15.0 >E2 3 5 9 3 1 9 . 6 - 3 2 0 . 6 -amu.SUL U T-2628 S P 2 3 3 0 2 0 0 - 1 ^ 3 ^ 2 5 0 RUN BT Visse SUBJECT TO PROTECTIVE ORDER. 0C-G45 GC/MS default file: >B2859::0i MS data file header from : >B2859 Sample: 2UL UT-2628 Operator: GARY MS 9/07/84 .7:03... Mi sc : S P 2 3 3 0 '2 0 0 - 1 / 3 / 2 3 0 RWN B T L # 1 9 B T L # 19 Sys. #: 1 MS model: 87 SW/HU rev.: CA ALS # : 0 M e t h o d file': S P 2 3 3 0 T u n i n g file: APEI01 No. of e x t r a records: 2 Source temp.: 250 Analyzer temp.: 0 Transfer line temp. : 0 - C h r o m a t o g r a p h i c t e m p e r a t u r es : 50. 300. 0. 0. 0. Chro m a t ographi c t im e s , min. : 0.0 2.0 0.0 0.0 0.0 Chromatograph:c rate, d eg / m in : 20.0 0.0 0.0 0.0 0.0 M/Z 3 333.9 First peak is b a s e l i n e ' drop c o r r e c t e d area. S e1c;o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R.T. f irst min. sc an max sc an 1ast peak scan width raw area 1 12. 112 2 4 2 24 4 2 47 2 12.112 242 244 247 5 34884 5 84884 corr. area 46919 36026 corr. 7. 100.00 76.78 M/Z - 331.9 F irst peak is b a s e l i n e d r o p c o r r e c t e d area. Second peak is tangent skimmed corrected area. Peak .# R.T. f irst min. sc an max scan 1ast peak sc an w i d t h raw area corr. area corr. 1 12.112 242 244 246 2 12.112 242 244 246 4 81589 4 81589 31465 29057 100.00 92.35 332/334 CALCULATION R - G l o b a l < 0) = .6706 M/Z = 327.9 Fi r s t peak is b a s e l i n e d r o p c o r r e c t e d area. Second peak is tangent s k i m m e d c o r r e c t e d area. ~ ^ ' **" >*---=i> 1 4\i I *7 J, . SUBJECT TO PROTECTIVE GPDEI Peak * R.T. f irst mi n. sc an max sc an 1ast peak scan width raw area corr. area corr. 1 12.112 242 244 247 \ 2 12.112 242 244 247 5 222323 5 222323 54167 50527 100.00 93.28 .- MfZ = 321.9 1 first peak Second peak is b a s e l i n e drop is tangent s k i m m e d corrected corrected area. area. Peak : R.T. f irst min. sc an max scan 1ast peak sc an w i d t h raw area corr. area c orr. 'A :i '2 t 0.000 0.000 248 248 0 247 0 247 -1 -1 0 0 O f n * r* 2667 2667 100.00 100.00 C11320/- S: fl/Z = 3 1 9 . 9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R. T. f irst min. sc an max scan 1as t peak sc an w i'dt h raw area 1 :2 0.000 0.000 243 243 0 247 0 247 -1 -1 0 0 corr. area 2230 2280 co r r . 100.00 100.00 320/322 CALCULATION R - G l o b a l < 1) = .8547 M/2 = 257.0 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak :4 R. T. f irst min. sc an max scan 1ast peak scan width raw area 1 0.000 2 0.000 243 243 0 247 0 247 -1 -1 0 0 corr. area 16042 16042 corr. 7. 100.00 100.00 <320 + 322)/< 332 +334) CALCULATION R - G 1o b a l < 3) = .0631 < 3 2 8 0 / 0 3 2 + 334) CALCULATION R - G l o b a l < 3) = .6907 7 k 00047 C11321 File >B2861 333.6-334.6 inu.2UL UT-2630 SP2330 200-1/3/250 RUN BT F i l e >2361 3 2 1 . 6 - 3 2 2 . 6 a m .j.2UL U T - 2 6 3 0 SP2333 200-1/3/250 RUN BT 00048 C11322 GC/MS default files >B2861:;01 MS data file header from : >B2S61 Sample: 2UL UT-2630 Operator; GARY MS 9 / 0 7 / 8 4 _ .7:43 Mi sc : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 R U N B T L 2 3 B T L # 2 3 S y s . #: 1 MS model: 87 ' SU/HUI reu.: Cft 'ALS : 0 Method file: SP2330 T u n i n g file: A P E 101 N o . of e x t r a r e c o r d 3 ! Scure e t e m p .: 25 2 A n a l y z e r t e m p .: 0 Transfer 1ine temp. : 5 C h r o m a t ographic te m p e r a t u r e s : 50. 300. 0. 0. 0. ; Chro m a t ographic t imes, min. : 0.0 2.0 0.0 0.0 0.0 ) Chromatographic rate, deg/min; 20.0 0.0 0.0 0.0 0.0 < Mi'Z = 3 3 3 . 9 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak * R. T. f irst min. scan max scan 1ast peak sc an w i d t h raw area corr. area corr. V. . 1 12.051 238 241 247 2 12.051 233 241 247 9 116086 9 116036 85792 77314 100.00 90. 12 M/Z = 331.9 F irst peak is b a s e l i n e dr o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak 4 R. T. f irst min. scan max scan 1ast peak sc an w i d t h raw area corr. area corr. % 1 12.071 237 242 243 2 12.071 237 242 243 11 1 3 9 1 5 6 11 1 3 9 1 5 6 65192 58449 100.00 89.66 332/334 CALCULATION R - G l o b a l < 0) = .7599 M/Z = 327.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d ' p e a k is t a n g e n t s k i m m e d c o r r e c t e d area. Peak . r ;t . f irst min. scan max sc an 1ast peak sc an w i d t h raw area 1 12.091 239 243 247 2 12.091 239 243 247 3 522313 8 522313 M/Z = 321.9 F irst peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is ta n g e n t s k i m m e d c o r r e c t e d area. Peak R. t . f irst min. scan max sc an 1ast peak scan width raw area 1 12.091 238 243 252 ' 2 12.091 233 243 252 14 1 6 6 6 1 3 14 .166613 0G049 c orr. area 112583 85895 corr. / *% 100.00 76.29 corr. area 111929 111474 corr. Ji 100.00 99.59 C11323 s M>Z 319.9 First, peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak R. T. f irst min. scan max scan 1ast peak sc an w i d t h raw area i i 12.091 236 243 254 2 12.091 23 6 243 254 13 12 5 2 8 5 18 12 5 2 8 5 > 6^1 corr. area 84155 31356 corn. X 130.00 96.67 320/322 CALCULATION R 7 G 1 o b a l < 1) * .7519 M/Z = 257.0 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak * R. T. f i r s t min. sc an max scan 1ast peak scan width raw area 1 12.091 240 243 248 2 12.091 240 243 248 8 237648 8 237648 corr. area 75663 69135 corr. * 100.00 91.37 <320 + 322) /<332 +334) CALCULATION R - G 1o b a l < 3) a 1.2987 <3 2 8 /)/<332 + 334) CALCULATION R - G 1o b a l < 3) = .7390 00050 C11324 File > B2862 333.6-334.6 amu.2UL UT-2631 SP2330 200-1/3/250 RUN BT File >B2S62 321.6-322.6 amu.SUL UT-2631 SP2330 200-1/3/250 RUN BT OC 051 C11325 M$ data file header from : >B2862 Sample: 2UL UT-2631 Operator: GARY MS 9/07/84 .8:03. Mi sc : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 R U N B T L U 2 5 B T L # 2 5 Sys, #: 1 MS model: 87 SU/HW rev.i CA ALS # : 0 Method file: SP2330 Tuning file: APEI01 No. of extra records: 2 S o u r c e t e m p . : 25 2 A n a l y z e r t e m p . i: 0 Transf er line t e m p . s C h r o m t o g r a p h ic t e m p e r a t u r e s : 50. 300. 0. 0. 0. : Chromtographic times, min. : 0.0 2.0 0.0 0.0 0.0 : C h r o m a t o g r a p h ic rate, d e g / m i n : 2 0 . 0 0. 0 0. 0 0. 0 0 . 0 n'(2 3 3 3 . 9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is ta n g e n t s k i m m e d c o r r e c t e d area. Pfrak R.T. f irst min. scan max scan 1ast peak sc an w idt h raw area corr. area co r r . y. 1 12.051 237 241 249 2 12.051 237 241 249 12 140692 1 00672 100.00 12 1 4 0 6 9 2 94366 93.74 M/Z = 331.9 First peak is base 1ine drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak tt R.T. f irst min. scan max scan 1ast peak sc an w i d t h raw area corr, area corr. V. 1 12.051 237 241 253 2 12.051 237 241 253 16 17 2 0 5 3 16 172058 79786 7569S 100.00 94.38 332/334 CALCULATION R-GlobalC 0) = .7925 M/Z = 327.9 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. SUBJECT TO PROTECT. Peak :# R.T. min. 1 12.071 ' 2 12.071 f irst sc an 233 233 max scan 242 242 1ast peak scan width 247 9 247 9 raw area 624209 624209 corr. area 144471 112S99 corr. y. 100.00 73. 15 M/Z 321.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak * R.T. min. 1 12.071 2 12.071 fi rst sc an 237 237 max sc an 242 242 1ast peak sc an w i d t h 2 5 6 19 256 19 raw area 226344 226344 oc 052 corr. area 161839 159537 co r r . y 100.00 93.61 C11326 s M/Z = 319.9 First peak is baseli ne drop c o r r e c t e d area. Second peak is tangent skimmed c orr e c t e d area. Peak .# R. T. f irst min, scan max sc an 1ast peak sc an u idt h rau area i 1 12,071 236 242 257 2 12.071 236 242 257 21 1 5 8 7 9 6 21 1 5 8 7 9 6 Vt 320/322 CRLCULATI OH R f G l o b a K 1) = .6934 M>Z = 257.0 first peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak *:# R. T. f irst min. sc an max scan 1ast peak sc an u idth rau area 1 12.071 239 242 251 2 12.071 239 242 251 12 3 6 5 3 5 7 12 3 6 5 8 5 7 corr. area corr. y. 112218 100.00 110695 98.64 corr. area 116064 114768 corr. y. 100.00 93.33 C320 + 3 2 2 ) / ( 3 3 2 + 334) C A L C U L A T I O N R - G l o b a l < 3) = 1.5187 (328')/(332 + 334) CALCULATION R - G l o b a l < 3) = .7925 "1s u b j e c t t o p r o t e c t ;'. - o * OG053 C1327 File >B2363 333.6-334. amu.2UL UT-2632 SP2330 200-1/3/250 RUH BT File >B2363 321 .6-322.6 amu.^UL UT-2632 SP2330 200-1/3/250 RUN BT 0G054 C11328 MS data fite header from : >B2863 Samples 2UL UT-2632 Operator: GARY MS 9 / 0 7 / 8 4 8 l 23 Mi sc : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 R U N B T L # 2 7 B T L # 2 7 Sys. #: 1 MS model! 87 SU/HU reu.: CA ALS # ! 0 Method fite: SP2330 Tu n i n g file: APEI01 No. of e x t r a records: 2 Source temp.* 250 Analyzer temp.: 0 Transfer line temp. : 0 - 'Chromat o g r a p h ic t e m p e r a t u r e s : 50. 300. 0. 0. 0. C h r o m a t o g r a p h i c t im e s , min. : 0.0 2.0 0.0 0.0 0.0 C h r o m a t o g r a p h ic rate, d e g / m i n : 2 0 . 0 0.0 0 . 0 0. 0 0. 0 M/Z = 333.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak * R. T. min. 1 12.091 2 12.091 first sc an 238 238 max sc an 243 243 1ast peak scan width 2 4 9 11 2 49 11 raw area 95515 95515 corr. area 63417 57070 corr. y. 100.00 39.99 M/Z = 331.9 F i r s t peak is b a s e l i n e d r o p c o r r e c t e d area.. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak R. T. f i r s t min. sc ah max sc an 1ast peak sc an w i d t h raw area corr. area corr. 1 12.091 233 243 250 2 12.091 233 243 250 12 97163 12 9 7 1 6 3 44015 39011 100.00 88.63 .- 332/334 CALCULATION R - G l o b a l C 0) = .6941 M/Z * 327.9 First peak is b a s e l i n e drop c o r r e c t e d area Sec ond peak is t an g e n t s k i m m e d c o r r e c t e d area e SUBJECT TO PROTECTIVE ORDER. Peak #. R. T. f irst min. scan max sc an 1ast peak sc an w idth raw area corr. area corr. y. 1 12.111 243 244 245 2 12.111 243 244 245 2 154992 2 154992 54287 53495 100.00 98.54 M/Z = 321.9 First peak is b a s e l i n e drop corrected area m S e c o n d peak is t an g e n t s k i m m e d c o r r e c t e d a r e a Peak 4 R.T. f ir s t min. scan max sc an 1ast peak sc an width raw area corr. area corr. 7. 1 12.111 240 244 253 2 12.111 240 244 253 13 1 8 4 6 7 3 13 18 4 6 7 3 135442 134675 100.00 99.43 00055 C11329 M/Z = 319.9 First peak is baseline drop corrected are*. Second peak is tangent skimmed corrected area. Peak # R. T. f i r s t min. 'sc an max scan 1ast peak sc an w i d t h r au area 1 12.111 239 244 257 2 12.111 239 244 257 18 1 4 3 1 0 6 18 1 4 3 1 0 6 com. area 99006 98016 com. y. 100.00 99.00 . 320/322 CALCULATION R - G l o b a l ( 15 =* .7310 M/Z = 257.0 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak * R. T. f irst min. scan max scan 1ast peak sc an w i d t h raw area 1 12.111 241 244 251 10 2 5 7 7 6 8 2 12.111 241 244 251 . 10 257768 com. area 84807 83287 com. Js 100.00 98.21 (320 + 3225/(332 +3345 CALCULATION R - G 1obalC 35 = 2.1823 (328'5/(332 + 3345 CALCULATION R-Global< 35 = .4940 00056 r--rhM' C11330 File >B2864 333.6-334.6 amu.2UL .2669/. 43/. 19 SP2330 200-1/3/259 RUH BT F i l e > B 2 8 6 4 3 3 1 , 6 - 3 3 2 . 6 a,mu.2UL .2 6 6 9 / . 48/. 19 S P 2 3 3 0 2 0 8 - 1 / 3 / 2 5 0 R U H BT File > B2864 321 .6 - 3 2 2 .6 am u.2UL . 2 6 6 9 / . 4 3 / . 19 SP2330 20 9 - 1 /3 /2 5 0 RUN BT 10900- : 5000H 0 10.0 File >B2364 T "I--I--I--I--I--I--j--I" i --I--I--I--] I I--j--i--r 10.5 11.0 111..5 122..00 12.5 T T -- I-- I-- I-- :-- I-- :-- I-- I-- I-- I-- i-- ,|-- 1 I 1 1 1 1 13.0 13.5 14.0 14.5 15.0 3 1 9 . 6 - 3 2 0 . 6 a m u . ^ U L .2 6 6 9 / . 4 8 / . 19 S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 R U N BT /I .--- icrT T O drotECt !VE ORDER. 0CQ57 C11331 GC/MS default f i U >B2864;;0l MS data file header from : >B2864 Sample: 2UL .2669/.48/.19 Operator: GARY MS 9/07/84 Mi sc : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 3 0 R U N B T L # 2 9 B T L # 2 9 Sys. #: 1 MS model 87 SU/HU r e u . : CA ALS * : 0 Method file: SP2330 Tun i n g file APE 101 N o . of e x t r a records: Sourc e t e m p .: 23 0 A n a l y z e r temp. 0 Transfer line temp -8:43 Chromat ographi c t e m p e r a t u r e s : 50. Chromatographi c times, min. : 0.0 Chromatographi c rate, deg/min: 20.0 300. 2.0 0.0 0. 0.0 . 0.0 0. 0.0 0.0 0. 0.0 0.0 fl/Z = 3 3 3 . 9 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is ta n g e n t s k i m m e d c o r r e c t e d area. Peak M R. T. min. 1 12.051 2 12.051 f irst scan 239 239 max scan 241 241 1ast peak sc an w i d t h 247 8 247 3 raw area 93249 93249 corr. area 57993 57461 corr. 3 100.00 99.08 M/Z 3 331.9 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R. T. f irst min. sc an max sc an 1ast peak sc an w i d t h raw area corr. area corr. y. 1 12.071 237 242 251 2 12.071 237 242 251 14 ' 8 5 3 7 4 14 85374 41946 39741 100.00 94. 74 332/334 CALCULATION R - G l o b a K 0) = M/Z = 327.9 .7233 SUBJECT TO PROTECTIVE First peak is b a s e 1 ine d r o p c o r r e c t e d area. Second peak is t angent skimmed corrected area. Peak 4 R. T. fi rst min. scan max sc an 1ast peak sc an wi d t h raw area corn. area corr. y, 1 12.091 241 243 247 2 12.091 241 243 247 6 236832 6 236832 68111 509O3 100.00 74.74 M/Z = 321.9 F irst peak s base 1 ine drop corrected' area. Second peak is t angent skimmed corrected area. Peak * R. T. f irst min. sc an max sc an 1ast peak sc an w i d t h raw area corr. area corr. 1 12.091 238 243 252 2 12.091 238 243 252 14 8 5 3 3 0 14 8 5 3 3 0 42934 42482 100.00 98.76 OC 05 m 1335! s M/Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak * R.T. f irst min. scan max sc an 1ast peak scan width r aw area 1 12.091 238 243 252 2 12.091 238 243 252 14 5 9 5 6 4 14 59564 corr. area 29450 28659 co r r . y. 100.00 97.31 320/322 CALCULATION R - G l o b a l < 1) * .6859 M/2 = 257.0 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R.T. fi rst min. scan max scan 1ast peak sc an w i d t h raw area 1 12.091 241 243 247 2 12.091 241 243 247 6 79116 6 79116 corr. area 22764 21423 corr. y. 100.00 94. 1 1 <320 + 322)/<332 +334) CALCULATION R - G l o b a l < 3) = .7243 <328')/<332 + 334) CALCULATION R - G l o b a l < 3) = .6777 ^ _,? j i7 A.7_j SUBJECT TO PCOTECTiVE ORDER, ' 00059 C11333 rile >B2865 333.6-334. amu.SUL UT-2633 SP2330 200-1*-'3/250 RUIN BT r i l e >B 2 S 6 5 3 2 1 . 6 - 3 2 2 . 6 a m u .2 U L U T-2633 SP2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 RUH BT 00060 C11334 GC/MS default file: >B2865::01 MS data file header from : >B2865 Sample: 2UL UT-2633 Operator: GARY MS 9/07/84 .3.-03 M isc : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 3 0 RUN BTL431 B T L # 3 1 Sys. : 1 MS model: 87 SW/HU rev.: CA ALS 4 : 0 Method file: SP2330 Tuning file: APEI01 No. of e x t r a records: 2 Source temp.: 250 Analyzer temp.: 0 Transfer line temp. : 0 - Chromatographi c tempe r a t u r e s : 50. 300. 0. 0. 0. C h r o m a t o g r a p h ic t im e s i min. : 0 .0 2.0 0 . 0 0 .0 0. 0 Chromatographi c rate, deg/m in : 20.0 0.0 0.0 0.0 0.0 M/Z = 333.9 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak 4 R. T. f irst min. scan max sc an 1ast peak scan width raw area corr. area co r r . Ji 1 12.044 243 244 247 2 12.044 243 244 247 4 75275 42703 100.00 4 75275 31329 73.36 M/Z = 331.9 Fi rst peak is b a s e l i n e d r o p c o r r e c t e d area. Se c o n d peak is t a ngent s k i m m e d c o r r e c t e d area. Peak R.T. f irst min. sc an max sc an 1ast peak sc an wi d t h raw area corr. area corr. * 1 12.044 242 244 248 2 12.044 242 244 248 6 57725 6 57725 34523 30395 100.00 88.04 332/334 CALCULATION R - G l o b a l < 0? = .8084 ^: M/Z = 327.9 First peak is b a s e l i n e dr op c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. SUBJECT TO rs^ ^ _ r -' * --- .'Ve Peak 4 R.T. first min. scan max scan 1ast peak scan width raw area corr.' area corn. * 1 12.065 242 245 249 2 12.065 242 245 249 7 171017 7 171017 67802 57949 100.00 85.47 M/Z. = 3 2 1 . 9 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R.T. f ir st min. sc an max sc an 1ast peak sc an w i d t h raw area corr. area corr. * 1 12.065 239 245 238 2 12.065 239 245 258 19 196646 146866 100.00 19 1 9 6646 143408 97.65 O r rip Cl 1335 s n/Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R. T. f irst min. sc an max scan 1ast peak sc an w i d t h raw area 1 12.085 241 246 255 2 12.085 241 246 255 14 12 9 2 1 2 14 129 2 1 2 corr. area 97684 95332 corr. y 100.00 97.59 320/322-CALCULATION R - G l o b a l < 1) 3 .6651 M/2 = 257.0 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R.T. f irst min. scan max scan 1as t peak scan width raw area 1 12.085 243 246 250 2 12.085 243 246 250 7 126026 7 126026 corr. area 67821 62536 corr. * 100.00 92.21 <320 + 322) /<332 +334) CALCULATION R - G l o b a l < 3) * 3.1667 <328' )/ <332 + 334) CALCULATION R - G l o b a l < 3) = .8609 S U B JE C T 7j-v r" 1Cl T -I`/c. 0 00G62 C11336 File > B2S66 333.6-334.6 mu . SUL UT-2634 S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 RUN BT 20000- fi 10 000" File l ______1 -------------------------- 1r * -- 1 1 I 1-- i i i 1 l 10 .0 10.5 11.0 J 1j ! i 1 1 .5 11| 1i 12.0 1i | 1i 12. S > B2S66 331 .6-332.6 a m u . 2UL UT-2634 13.0 13.5 14.0 14. 5 I ri 15.0 SP23 3 0 2 0 0 - 1 / 3 / 2 5 0 RUN BT File >B2366 321.6-322.6 amu.SUL UT-2634 SP2330 200-1/3/250 RUN BT 0G063 C11337 GC/MS default file: >B2866::01 MS data file header from : >B2866 Sample: 2UL UT-2634 ` Operator: GARY MS 9/07/84 Mi sc : S P 2 3 3 0 2 3 0 - 1 / 3 / 2 5 0 R W N B T L # 3 3 B T L # 3 3 Sys. 4: 1 MS model: 87 S U / H U reu. : Cfl flLS # : 0 Method file* SP2330 T u n i n g file: APEI01 No. of e x t r a records: Source temp.: 232 Analyzer temp.: 0 Transfer line temp. : Chromatographi c temperatures 50. 300. 0. 0. 0. Chromatographic times, min. 0.0 2. 0 0.0 0. 0 0. 0 20.0 0.0 0.0 0.0 0.0 9:.22 M/Z 333.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak R. T. f ir st min. sc an max scan 1ast peak sc an w i d t h raw area 1 12.031 236 240 246 2 12.831 236 240 246 10 105110 10 105110 corr. area 78200 70850 corr. V. 100.00 90.60 M/Z = 331.9 First peak is b a s e l i n e drop c o r r e c t e d area. Second peak is tangent s k i m m e d c o r r e c t e d area. Peak # R.T. first min. sc an max scan 1ast peak scan width raw area corr. area corr. 1 12.031 237 240 243 2 12.031 237 240 248 11 9 5 1 9 7 11 9 5 1 9 7 56043 51785 100.00 92.39 332^334 CALCULATION R - G l o b a l < 0) = .7167 M/Z = 327.9 First peak is b a s e l i n e drop c o r r e c t e d area. Second peak is tangent sk i m m e d c o r r e c t e d area. r'--" 7\ 7 ^ 'T A f SUBJECT TO P R O TE C TIVcE of?r="- Peak 4 R.T. first min. scan max sc an 1ast peak sc an w i d t h raw area corr. area corr. 1 12.851 237 241 246 2 12.051 237 241 246 9 298800 9 29S800 76463 60119 100.00 78.62 9-- M^Z 321.9 First peak is b a s e l i n e drop corrected* area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak 4 R.T. f irst min. scan max scan 1ast peak sc an w i d t h raw area corr. area corr, * 1 12.051 238 241 247 2 12.051 238 241 247 9 150832 121024 100.00 9 150832 109243 90.27 0G064 C11338 s P1/Z = 319.9 Fi rst peak is b a s e 1 ine d r o p c o r r e c t e d area. Second peak is tangent skimmed c o r r e c t e d area. Peak # R. T. f irst min. sc an max sc an 1ast peak sc an w i d t h r au area 1 12.051 236 241 256 2 12.051 236 241 256 20 133584 20 133584 corr. area 88864 86054 cor r . V. 100.00 96.84 320/322 CALCULATION R-Global( 1) = .7343 MAZ = 257.0 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak R. T. f irst min. sc an max sc an 1ast peak sc an w i d t h raw area 1 12.071 2 12.071 233 242 247 233 242 247 9 152622 9 152622 corr. area 74700 63855 corr. Ji 100.00 85.48 (320 + 322>/<332 +334) CALCULATION R - G l o b a K 3) = 1.5634 <328')/<332 + 334) CALCULATION R-Clobal < 3) = .5615 CCi ii^ISNTfAL SUBJECT TO PROTECTIVE ORDER. 00065 C11339 File >B2S67 333.6-334.6 amu.2UL UT-263S SP2330 200-1/3/250 RUN BT File >B2367 321.6-322.6 amu.SUL UT-235 SP2330 200-1/3/259 RUN BT MS data file header from i >B2867 Sample: 2UL UT-2635 Operator: GRRY MS 9/07/84 .9:42... Mi sc : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 3 0 RU N B T L # 3 5 B T L # 3 5 Sys. #: 1 MS m o d e l : 87 S U / H U rev.: CR RLS ft : 0 Method file: SP2330 Tuning file: RPEI01 No. of e x t r a records: 2 Source temp.: 250 Analyzer temp.: 0 T r a n s f e r line temp. : -- C h r o m a t o g r a p h ic t e m p e r a t u r e s : 50. 300. 0. 0. 0. Chro m a t ographic times, min. : 0.0 2.0 0.0 0.0 0.0 Chromato g r a p h ic rat e , deg/min : 20.0 0.0 0.0 0.0 0.0 M/Z = 333. 9 F irst peak is b a s e l i n e d r o p c o r r e c t ed area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak ft R. T. f irst min. sc an max scan 1ast peak scan width raw area corr. area corr. y. 1 12.030 234 240 252 2 12.030 234 240 252 18 13 0 3 6 6 18 130366 81910 78688 100.00 96.07 M/Z = 331.9 F irst peak is b a s e 1 ine d r o p c o r r e c t e d area. Sec ond peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak ft R. T. f i r s t min. sc an max scan 1ast peak scan width raw area corr. area corr. ym 1 12.030 236 240 251 2 12.030 236 240 251 15 108161 15 108161 56861 55758 100.00 98.06 332/334 CALCULATION R - G l o b a l C 0) = M/Z = 327.9 .6942 fTAT SUBJECT TO PROTECTIVE ORDEfl First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak * ft R.T. f irst min. sc an max sc an 1ast peak scan width raw area corr. area corr. 5i 1 12.051 237 241 246 2 12.051 237 241 246 9 203074 9 203074 60784 56904 100.00 93. 62 M/Z = 321.9 F irst peak is base 1ine drop corrected area. S e c o n d peak is t a ngent s k i m m e d c o r r e c t e d area. Peak ft R.T. first min. scan max sc an 1ast peak sc an wi d t h raw area corr. area corr. y. 1 12.051 238 241 246 2 12.051 238 241 246 8 34928 8 34928 10520 9928 100.00 94.37 00067 C11341 s M/Z = 319.9 First peak is base 1ine drop corrected area. Second peak is tangent skimmed corrected area. Peak tt R. T. f i r s t min. scan max sc an 1ast peak scan width raw area 1 12.051 238 241 247 2 12.051 238 241 247 9 28746 9 28746 corr. area 8451 7780 corr. J; 100.00 92.06 320/322 CflLCULATION R - G l o b a l C 1) - .8033 M/Z = 257.0 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak it R. T. f irst min. sc an max sc an 1ast peak sc an w i d t h raw area 1 12.051 239 241 244 2 12.051 239 241 244 5 46929 5 46929 corr. area 10379 10161 corr. '4 160.00 97.90 (320 + 322)/(332 +334) CALCULATION R - G 1o b a l < 3) = .1367 ( 3 2 8 0 / 0 3 2 + 334) CALCULATION R - G l o b a l < 3) = .4373 00068 j. '-i_ Ja SUBJECT TO PROTECTIVE ORDER C11342 File >B2368 333.-334.6 amu.SUL UT-2636 SP2330 200-1^3/250 RUN BT File >B2363 321.6-322.6 amu.^UL UT-2636. SP2330 200-1/3/250 RUN BT '-i...i .- . , SUBJECT TO PROTECTIVE ORDER. 0C069 C11343 MS data fil? header from : >B2868 Sample: 2UL UT-2636 Operator: GARY MS 9/07/84 10r02 Mise : SP2330 200-1/3/230 RUN BTL*37 BTL#37 Sys. #: 1 MS m o d e l : 87 S W / H U rev.* CA ALS # : 0 Method file: SP2330 Tu n i n g file: APEI01 No. of e x t r a records: 2 Source temp.: 230 Rnalyzer temp.: 0 Transfer line temp. : 0 ~ C h r o m a t og r a p h i c t e m p e r a t u r e s : 50. 300. 0. 0. 0. C h r o m a t o g r a p h ic times,, min. : 0 . 0 2.0 0 . 0 0. 0 0. 0 C h r o m a t o g r a p h ic rate, deg/mi n: 2 0 . 0 0.0 0 . 0 0. 0 0 . 0 M/Z - 333. 9 F irst p e ak is b a s e l i n e dr o p c o r r e c t e d area. S e c o n d peak is t angent s k i m m e d c o r r e c t e d area. Peak * R. T. f irst min. scan max sc an 1ast peak s c an width raw area corr. area co r r . % 1 12.010 236 239 244 2 12.010 236 239 244 8 107248 8 107248 78584 74548 100.00 94.86 M/Z = 331.9 First peak is b a s e l i n e dr op c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R.T. fi rst min. sc an max scan 1ast peak sc an w i d t h raw area corr. area c orr. y. 1 12.010 231 239 256 2 12.010 231 239 256 25 139010 25 139010 66335 62047 100.00 93.54 332/334 CALCULATION R-GlobalC 0) = .8441 M/Z = 327.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. Se c o n d peak is ta n g e n t s k i m m e d c o r r e c t e d area. Peak # R. T. f irst min. scan max sc an 1ast peak sc an w i d t h raw area 1 12.030 229 240 252 2 12.030 229 240 252 23 318017 23 318017 M/Z = 321.9 First peak is b a s e l i n e dr op corrected, area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R.T. f irst min. sc an max sc an 1ast peak sc an w i d t h raw area 1 0.000 2 0.000 253 253 0 252 0 252 -1 -1 0 0 OC 070 . ; "* S U B J EwCl'*T T o rr'SrO-T--F-Tj..'f-.t'- corr. area 88063 53839 corr. * 100.00 61.14 corr, area 2708 2708 corr. s`. 100.00 100.00 C11344 s M.'Z = 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak # R.T. fi rst min. scan max scan 1ast peak sc an w i d t h raw area 1 0.00O 2 0.000 253 253 0 252 6 252 -1 -1 0 0 corr. area 2193 2193 Corr. *4 100.00 108.00 3ZQ/322 C A L C U L A T I O N R-G 1o b a l < 1) S .8100 M.'Z = 2 5 7 . 0 First peak is b a s e l i n e dr o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Pe ak # R.T. fi rst min. sc an max sc an 1ast pe ak sc an width raw area 1 0.000 2 0.000 253 253 0 252 ' -1 0 252 -1 0 0 corr. area 6477 6477 corr. Ji 100.00 100.00 <320 + 322>/<332 +334> CALCULATION R - G 1o b a l < 3) -- .0338 ( 3 2 8 " >/<332 + 334) CfLCULfTIOH R-Gl obal < 3) = .6075 . i U i.5rkXj SUBJECT TO PROTECTIVE ORDER* C11345 File >*2869 333.6-334.6 A m u . SUL UT-263' SP2330 200-1/3/250 RUM BT File- > 2 6 6 9 i 1 .6-322 s* am u 2 U L U T - 2 6 3 7 SP2330 200-1/3/250 RUM BT 8080t 4000- : e10.0 L lv.x 10.5 11.0 11.5 10.9 12.5 13.0 I m m \ \ Oc 072 13.5 14.0 -v: 14.5 15.0 C11346 mini hois roHronniio* ihimmo Niwtim a file header from ! >B2869 2UL UT-263? Operator: GARY MS 9/07/84 10:22 SP2330 200-1/3/250 RUN BTL#39 BTL#39 : 1 (IS model: 87 S U / H W rev.: CA A L S # : 0 od file: SP2330 Tuning file: BPEI01 e temp.: 250 R n a l yztr t e m p .: 0 Ho. of extra records: 2 Transfer line temp : 0 .. Chromat ographi c t e m p e r a t u r e s : 50. 300. 0. 0. 0. C h r o m a t o g r a p h i c times, min. : 0 . 0 2. 0 0.0 0. 0 0. 0 C h r o m a t o g r a p h ic rate, d e g / m i n : 2 0 . 0 0. 0 0.0 0.0 0. 0 - 333.9 pe ak is b a s e 1 ine d r o p c o r r e c t e d area. i peak is t a n g e n t s k i m m e d c o r r e c t e d area. R.T. f irst min. scan max scan 1ast peak scan width raw area corr. area corr. % 12.010 233 239 247 12.610 233 239 247 14 9 3 7 8 7 14 9 3 7 6 7 56919 53699 100.00 94.34 331.9 t p e ak is b a s e l i n e d r o p c o r r e c t e d area. d peak is tangent s k i m m e d c o r r e c t e d area. R.T. 'f irst m iri. s c a n max sc an 1ast peak sc an ui dt h raw area corr. area corr. y. 12.010 231 239 253 12.010 231 239 253 22 104329 22 104329 40353 38571 100.00 95.58 i34 C A L C U L A T I O N z>b a 1 i 0 = .7090 -* r*i-/- , __ n-- ^ J *' - > if4| n T c m i o i w c st peak is b a s e l i n e d r o p c o r r e c t e d area, nd peak is tangent s k i m m e d c o r r e c t e d area. R.T. fi rst min. sc an max scan 1ast peak scan width raw area 12.051 237 241 245 12.051 237 24 1 245 8 133144 8 133144 321.9 : pe ak is b a s e l i n e d r o p c o r r e c t e d area, peak is t angent skimmed corrected area. R.T. f irst min. scan max sc an 1 ast p e ak scan w idth r aw area 0.000 0.000 246 246 0 245 0 245 -1 -1 00073 0 0 corr . ar ea 45068 37980 corr. y. 108.00 84.38 corr . area 2725 2725 corr. y. 100.00 100.00 Ci l 347 File >B2S70 333.6-334.6 *mu UL 2.669/.48/. 19 SP2330 200-1/3/250 RUN BT File > 2 8 7 0 321 . 6 - 3 2 2 . 6 iHiu .2UL 6 6 9 / . 4 8 / . 1 9 S P 2 3 3 0 2 0 8 - 1 / 3 / 2 5 0 RU N BT 80000- . 40000- 0-T^ ^ 1i' 10.0 10.5 11.0 11 12.0 12.5 13.0 13.S 14.0 14.5 15.0 C11349 MS data file header from >B2870 Sample: 2UL 2.669/. 48/. 19 Operator: GARY MS 9 / 0 7 / 8 4 l*8:42--,, Misc : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 R U N ` BTL*t4 1 BT L 4 1 Sys. 0: 1 MS model: 87 S U / H M r e u . : Cfi RLS # : 0 Method file: SP2330 T u n i n g file: APE I 6 1 No. of e x t r a records: 2 Source temp.: 250 Analyzer temp.: 0 T r a n s f e r line temp. : 0 C h r o m a t ogr aph ic t e m p e r a t u r e s : 50. 300. 0. 0 . 0. Chromat og r a p h ic times, min. : 0.6 2. 0 0 . 0 0. 0 0.0 C h r o m a t o g r a p h i c rat e , deg/mi n : 2 0 . 0 0 . 0 0 . 0 0. 0 0.0 M/Z * 333.9 First peak is b a s e l i n e drop corrected area. S e c o n d pe ak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak * R. T. f irst min. sc an max scan 1ast peak s c a n uiidt h raw area corr. area c orr. y. 1 12.011 234 239 249 2 12.011 234 239 249 15 130146 15 130146 95136 93606 100.00 98.39 M/Z = 331.9 F i r s t pe ak is b a s e l i n e d r o p c o r r e c t e d area. Se c ond p e ak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak * R. T. fi rst. riiin . sc an max scan 1ast peak scan width raw area co r r . area corr. * 1 12.011 234 239 249 2 12.011 234 239 249 15 .*107070 15 107 0 7 0 68550 66667 100.00 97.25 332/334 CALCULATION R - G l ob al f 0> a .7 2 0 5 M/Z = 32?. 9 cc S ' '-- v __ _ : - ' -i i \ - 11t O R Z *s First pe ak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d pe ak is t a n g e n t s k i m m e d c o r r e c t e d area. -- Pe ak * R. T. first m in . sc an max scan 1ast peak scan width raw area corr. are a c orr. 1 12.031 237 240 243 2 12.031 237 240 243 8 147271 6 147271 60493 58330 100.00 96.42 M/Z = 321.9 ! First peak Sec ond peak is b a s e l i n e d r o p is t a n g e n t s k i m m e d corrected corrected area. area. P e ak # R. T. mi n . first sc an max sc an 1ast peak s c an wi d t h raw area corr. area c orr. ** 1 12.031 236 240 246 2 12.031 236 240 24 8 12 531792 496500 100.00 12 5 31792 4 8 0 1 6 8 96.71 C1135 n ( >- * r z 3z 17 Q C J* z S M '2 * 319.9 First peak is baseline drop corrected area. Second peak is tan gent skimmed corrected area. Fe ak ft R. T. f irst min. sc an max scan 1ast peak sc an u idt h rau area 1 12.031 235 240 248 2 12.031 235 240 246 13 366 2 3 0 13 366230 corr. area 337682 323096 corr. X 106.00 95.68 320^322 CFlLCULRT ION R-GlobalCl)* .6801 1V2 = 257.0 First peak is b a s e l i n e dr o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. P e ak R. T. Ai f 'i . firs t scan m ax scan 1ast peak 5 can width rau area 1 12.031 236 240 &4& 2 12.031 236 240 246 10 3 5 5 8 3 7 10 3 5 5 8 3 7 corr, area 300237 282357 c orr. 'Iy 100.00 94.04 C320 + 3 2 2 ) / C332 +334) CRLCULRTION R - G l o b a l C 3) = 5.0962 (328')/C332 + 334) C R L C U L R T I O N R - G 1obal >. j> ~ ,341 j ff;i ntconking ciiftRisl t.iunm ittonnij.rournn.HON C -: SUBJECT TO PROTECTIVE ORDER. n r C11351 File >B2S71 333.6-334,6 amu.2UL 26.69/.48/.19 SP2336 266-1/3/259 RUH BT 'i. vini*iinn X F i l e >E 2371 3 2 1 . 6 - 3 2 2 . 6 a m u .^ U L 2 6 . 6 9 / . 4 8 / . 19 SP2 3 3 2 6 0 - 1 / 3 / 2 5 0 RUM BT 8066 0O- 4 OOOOO* 0-J-- :-- i-- r-i-- i-- !-- :-- !-- i-- [-Ti-- i-- i-- i-- I-- i-- n -- r*-j-- r--- i-- -- !-- n -- t--j-- i-- i-- i-- :-- ;-- i-- i-- i-- -- ]-- i-- r-i-- i-- -- :-- i-- i-- :-- j 10.0 10.5 11.0 11.5 12.0 12.5 13.0 13.5 1 4 .G 14.5 15.6 F i l e >B 2671 3 1* . 6 - 3 2 0 .6 an,u . 2UL 2 6 . 6 9 / . 43 .19 S P 2 33 20 0- 1/ J / 250 RUM BT I- 11 4 0 0 0 0 O- 0 n' I ' I '! ! J I 10.0 10.5 1 1 . - j ..u /*!L'BJECT TO PROTECTIVE ORDER. ' I 1 ` 1 1 ' 1 1 J 1 1 ' I 1 > I 1 - i 1"1! 1 - i 11.5 12.0 12.5 13.0 13.5 14.6 14.5 15.0 OC0 7 8 C11352 MS data file header from i >B2S7l S a m p l e : SUL 2 6 . 6 9 / . 48''. 19 Operator: GARY MS 9/07/84 11:02* Misc : SP2330 200-1/3/250 RUN BTL#43 BTL#43 Sys. #: 1 MS modeli 87 S U / H U rev.: Cfi ALS # : 0 Method file: SP2330 T u n i n g file: APEI01 No. of e x t r a records: 2 Source temp.: 250 Analyzer temp.: 0 Transfer line temp. : 0 - C h r o m t ographi c t e m p e r a t u r e s : 50. 300. 0. 0. 0. Chro m t ographi c times, min. : 8.0 2.0 0.0 0.0 0.0 C h r o m t ogr a p h i c r at e , d e g / m in : 2 0 . 0 0.0 0. 0 0 . 0 0.0 M/2 * 333.9 First peak is base 1 ine d r o p c o r r e c t e d area. S e c o n d peak is tan g e n t s k i m m e d c o r r e c t e d area. Pe ak # R.T. first min. scan max scan 1ast peak scan width raw area corr. area corr. * 1 11.99 233 238 243 2 11.990 233 238 243 M/Z = 331.9 10 119581 10 119581 95141 65461 100.00 68.80 First- peak is b a s e l i n e drop corrected area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Pe ak R.T. first min. scan max scan 1ast peak sc an w i d t h raw area corr. area c orr. y. 1 12.010 234 239 243 <" 1 2 . 0 1 0 234 23 9 243 9 - 93295 9 93295 65854 47853 100.00 72.67 332-'334 C A L C U L A T I O N R - G 1o b a 1 i 0> = .6922 n/2 = 327.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. ,,-- ______ v ., SUBJECT TO iE C 7 P e ak # R.T. first min. sc an m ax sc an 1ast p e ak sc an w i d t h raw area corr. area c orr. * 1 12.010 232 229 248 2 12.01O 232 239 248 16 483585 220832 100.80 16 4 8 3 5 8 5 119551 5 4 . 3 3 M/2 = 321.9 F irst peak is b a s e l i n e drop corrected area. S e c o n d peak is t a n gent s k i m m e d c o r r e c t e d area. Pe ak # R.T. f ir st min. sc an ma sc an 1ast pe ak scan width raw area corr. area corr. 4 1 12.010 235 239 244 2 12.010 235 239 244 9 4944280 9 4944280 4816579 3347396 100.00 69.50 OC079 C11353 m /Z * 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak R.T. first i min. scan max sc an 1ast peak sc an u idt h raw area 1 12.030 235 240 245 2 12.030 235 240 245 10 3 4 9 5 8 9 8 10 3 4 9 5 8 9 8 corr. area 3421448 2367786 corr. 100.00 69.20 320/322 C L C U L A T ION R - G l o b a K 1) = .7103 M/Z * 257.0 First peak is b a s e l i n e drop c o r r e c t e d area. Second peak is t an g e nt skimmed corrected area. F e ak * R.T. f irst min. scan max scan 1as t peak s c a n ui dt h raw area 1 12.030 235 240 245 2 12.030 235 240 245 10 2 8 9 9 0 8 5 10 2 8 9 9 0 6 5 corr. area 2808645 1870499 corr. 100.00 66. 60 C320 + 322 )/(332 +334) CALCULATION R - G 1o b a l < 3) = 51 . 1695 ; (.SI'S-' >' (332 + 334) C A L C U L A T I O N R - G l o b a H 3) = 1 .0974 _ M * I Z | X sZ 1 1lIus If re SUBJECT m __ ' ' " -1-* ^-L< 1- r u i ECTIVE C.lDr-; 000JO C11354 i !* i" . i i_u,i j v t . nr C11355 z F i l e > 3 2 8 7 4 3 3 3 . 8 - 3 3 4 . 8 & nmiuu .-UL .1 6 68/ .48 .1? SF233G 266-1/3/256 BT F i l e > B 2 $ 7 4 3 2 1 . 8 - 3 2 2 . 5 a m u . . 1O S / .4 5 / . 1 9 SF2336 200-1/3/256 BT SUBJECT TO PROTECTIVE ORDER. nr C11356 MS data file header from i >32874 Sample: 2UL .1068/.48/.19 Operator* GARY Misc : SP2330 200-1/3/250 . BTL403 BTL# Sys. *** 1 MS model* 87 SW/HU rey.: CA Method file: SP2330 Tuning file: .APEI01 Source temp.: 250 A n a l y z e r temp.:' 0 MS 9/07/84 -12:65*_3 ALS : 0 No. of e x t r a reco r d s : 2 Transfer line temp. * 0 C h r o m a t o g r a p h i c t e m p e r a t u r e s : 50. 300. 0. 0. 0. Chromatographic times, min. : 0.0 2.0 0.0 0. 0 0.0 20.0 0.0 0.0 0.0 0.0 M/2 * 333.9 F irst peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d p e ak is t angent s k i m m e d c o r r e c t e d area. Peak p R. T. f irst min. scan m ax scan 1ast peak sc an w i d t h raw area corr. area corr. y. 1 11.984 239 241 246 11.984 239 241 246 7 64648 7 64648 40526 39133 100.00 96.56 M/Z = 331.9 First p e ak is b a s e l i n e drop c o r r e c t e d area. Sec ond peak is t ang e n t s k i m m e d c o r r e c t e d area. Peak it R. T. f irst min. sc an m ax sc an 1ast peak scan width raw area corr. area corr. *4 1 12.004 237 242 250 2 12.004 237 242 250 13 59914 13 5 9 9 1 4 31392 29949 100.00 95.40 332/334 CALCULATION R - G l o b a K 0? = .7746 M/2 = 327.9 C O JV , SUBJECT TO P.^OTCv-- O`ROC F i rst peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. P e ak # R.T. f irst min. scan max sc an 1ast peak sc an w i d t h raw area corr. area co r r . * 1 12.004 237 24 2 251 2 12.004 237 242 251 14 8 8 0 2 9 14 8 8 3 2 9 25389 34063 100.00 96.08 M/Z = 321.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d p e ak is t angent s k i m m e d c o r r e c t e d area. Pe ak # R.T. fi rst min. s c an m ax scan 1ast peak scan width raw area c or r . area corr. 1 12.024 241 243 246 2 12.024 241 243 246 5 23343 5 23343 9683 7598 100.00 83.65 C11357 |C-irn"l c u r u i n g C i i * m s 1 i.nAriiii; C o n i hoi s t r>iiriin*iinN m u o i l * Nt w v<mn S Y\'Z 319.9 First peak is baseline drop corrected area. Second.peak is tangent skimmed corrected area. Feak R. T. first min. scan max scan 1ast peak sc an w i d t h raw ,a r e a 1 12.024 241 243 247 2 12.024 241 243 247 6 22029 6 22029 corr. area 6999 5748 corr. V. 100.00 83.20 320.'322 CALCULATION R - G l o b a l C 1) = .7607 Pl-'Z = 2 5 7 . 0 F i rst peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is ta n g e n t s k i m m e d c o r r e c t e d area. Re ak * R. T. first min. sc an max sc an 1ast peak sc an w i d t h raw area 1 12 . 0 2 4 238 243 248 10 3 9 6 7 6 2 12. 8 2 4 238 24 3 248 10 3 9 6 7 6 corr. area 9536 8586 c orr. y. 100.00 90.04 C320 + 322 ) / C332 +334) CALCULATION R - G l o b a C 3.'1 = .2224 C328')x<332 + 334) CALCULATION R - G l o b a K 3 > = .4909 M O Ml' OOOS4 *7i C11358 ul.il l>l'lI<1111 ij'`v*k**>'*;timiM i Ui t\J \ CO \ t <S O M O co Ci CM . (O o* CO oo o <9 n cm D * CCOO I ' CO CCOO l/l r- oj cm M Ci Ci CM O O M C< Cm Ui "tfl C< U i Ui I/* (VI CM \\ CO CO \ \ VH II Ci C< OO CM CM ") C i Ui OO CO . ' CO (O CO CM n CM `co li. M CO.. ____ (T i. vH U) \ 05 _ CM H CO M \ 00 CO C i 'D _ Ci __ ___ CM vH VH CM D iH ` - cm <vi CO I oo CO ui -J vH vt 1 fc ll -Cl ^ *-H J vH CM ` CO . U i ` fl ~ r` vH CM CO U i - o l/i Iw CCi n n y n ri 11n p, l- Ci Ci . C i O i CM M O Ci 9 CM CO C i Ui vH l^l 1^1 D vH U` 'cm ( i / ) 1 Ii U i \ 1 .1 Ui 11 / 1{ ll*lti>('* .'I* I1I 1fI C11359 oh fu * ri - U) o Li) - *r U> OJ V _ 0 \ - 11 CD * - 1^1 OJ 11- CO -u >. o O' CO OJ 1 ^- i*0 C-l . </> 1 LL C'> !- a* i* i- a* *- Li) r \ C'J CO - CO - Oj - ** O "OJ o> \ b> O) CO0OJ#. . "Or--l# ab> \ (r: l.J < C\ cr. o h LiJ > Ii) hi f- VI (. ' 0. i1 I } ( i (; f ; ca V'-- "to LO l/> CO 111 'oj J "og -j - u:> Ol w--i ri Li) . I'l Mn t=it - <3 _* M H c*t `I I 'j . Ij'l r. r-. -- LO C'J 1 LO I - Ol ~ u LO CO Ol LO I- ii ' <^i o o iji LO o \: VJ! IM 1-- *-- 1-- r - T o 1 ~ _. U LU C'J Cm 1 Tl | 1 II m O A`. \ ' f OJ a< CM Hi OJ r i Ll`> U\t ' . L V L C lata file he a d e r from ! >B2875 -.le: 2UL 1 . 0 6 8 / . 4 8 / . 19 O p e r a t o r i GfiRY MS 9/07/84 : SP2330 200-1/3/250 BTL05 BTL# : 1 MS model : 87 S U / H U r e v . : Cfi fiLS : 0 rthod file: SP2330 Tuning file: .RPEI01 No. of e x t r a records: jrc e t e m p . : 252 finalyzer t e m p . : 0 Transfer line temp. : 12:-24 . Chromat ograph ic t e m p e r a t u r e s : 59. Chromat ograph ic t im e s , min. : 0.0 C h r o m a t og r a p h i c r at e , deg/mi n: 2 0 . 0 300. 2.0 0.0 0. 0.0 0.0 ' 0. 0.0 0.0 0. 0. 0 0.0 S 333.9 r st peak is b a s e l i n e `d r o p c o r r e c t e d area. on d peak is t arg e n t s k i m m e d c o r r e c t e d area. < R.T. f ir s t max last peak min. sc an s c a n sc an width raw area corr. area corr. 1 11.990 237 236 242 2 11.99 237 238 242 5 62220 56745 100.00 5 82220 15262 26.96 = 331.9 rst peak is b a s e l i n e d r o p c o r r e c t e d area. ond peak is t ang e n t ski m m e d c or ree ted area. .k R.T. first min. sc an 1 11.99D 2 11.990 235 235 max scan 238 238 last peak sc an w i d t h 244 9 244 9 raw area 66175 66175 corr. iarea 42136 41195 c orr. y. 10 0 . 0 0 97.77 :T 2/334 CRLCULRTION *1c<b a 1 i 0J = .7426 I = 327.9 irsi peak is b a s e l i n e d r o p c o r r e c t e d area. :ond peak is t a n g e n t s k i m m e d c o r r e c t e d area. ak R.T. fi rst ma x 1ast peak # min. scan scan sc an w i d t h raw area 1 12.010 234 239 246 2 12.016 234 239 246 12 9 8 3 8 2 12 9 8 3 8 2 2 * 321.9 irst peak is b a s e l i n e d r o p c o r r e c t e d area, cond peak is t a n g e n t s k i m m e d c o r r e c t e d area. ak R.T. first m a x 1ast peak 4 min. sc an sc an sc an w id t h raw area 1 12.010 237 239 243 2 12.010 237 239 243 6 180719 6 180719 r\ f n n Ar - <--<GTE'-^V'E ORDER. ,c o r r . ar e a 56154 54390 corr. y. 100.00 96.86 * corr. area 127919 95278 corr. y. 100.08 74.48 C11360 162 I nikiw h ritKHMOi s cw*f*>*>'** MS data file header from : >B2876 Sample: 2UL UT-2638 Operator: GARY MS 9 / 0 7 / 8 4 -12::46 =. . Mise : SP2330 206-1/3/250 RUN BTL445 BTL445 Sys. 4: 1 MS model: 87 S U / H U rev. : Cfl ALS 4 : 0 Method file: SP2330 Tu n i n g file: APEI01 Ho. of e x t r a records: 2 Source temp.: 230 Analyzer temp.: 0 Transfer line temp. : 0 - C h r o m atographie t emperat ures : 50. 300. *0. 0 e 0. C h r o m a t o g r a p h i c times, min. : 0 .0 2. 0 0 . 0 0. 0 0.0 Chroma tographi c rate , deg/min : 20.0 0.0 0.0 0. 0 0.0 M/Z * 333.9 First pe ak is b a s e l i n e d r o p c o r r e c t e d area. Sec en d peak is- t a n g e n t s k i m m e d c o r r e c t e d area. Peak 4 R. T. f irst min. sc an max scan 1ast peak scan u id t h rau area corr. area corr. y. 1 11.970 236 237 242 2 11.970 236 237 242 6 86132 6 86132 59336 38648 100.00 65. 13 M/Z = 331.9 First peak is ba s e 1 ine dr o p c o r r e c t e d area. Se c on d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak 4 R. T. f i r s t min. sc an max sc an 1ast peak sc an w i d t h rau area corr. area corr. * 1 11.970 233 237 246 13 70827 43098 100.00 2 11.970 233 237 246 13 70827 41590 96.50 332/334 CALCULATION R-GlobaU 0) = .7263 M/Z = 327.9 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d Are a . Peak 4 R. T. fi rst min. scan max scan 1ast peak sc an wi d t h raw area 1 11.990 235 238 248 2 11.990 235 238 248 13 93453 13 93453 M/Z 321.9 First peak is b a s e l i n e dr o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak 4 R. T. fi rst m in . sc an max scan 1ast peak sc an wi d t h raw area 1 0.000 2 0.000 249 249 0 248 0 248 -1 -1 0 0 c or r . area 51944 49747 c orr. 100.00 95. 77 cor r . area 2224 2224 c orr. '/ 100.00 100.00 G11363 I nfl CnnmnC C N tnlT I S IVZ * 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area.' Fe ak * R. T. f irst min. scan max scan 1ast peak sc an ui dt h rau area 1 0. 000 2 0.000 249 249 0 248 0 248 -1 ' -1 0 0 > > 2 T 7 U> corr. area 2144 2144 corr. y. 100.00 100.00 320^322 CALCULATION R - G l o b a U 1) = .9640 M/Z = 257.0 First peak is b a s e l i n e dr o p c o r r e c t e d areal S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak '# R. T. first min. scan max scan 1ast peak s c a n ui dt h raw area 1 0.000 2 0. 080 249 249 0 246 0 248 '1 ' -1 .0 10 corr. area 2759 2759 c orr. y. 100.00 100.00 C320 + 322 )/< 332 +334) C A L C U L A T I O N R - G 1o b a l < 3) = .0426 C328')/<332 + 334) CALCULATION R - G l o b a l C 3) = .5069 ;<Sl n r c o h o i N n c i l * n i * | i.ntt'H'U cu N in o i s r ,n n r < i n n n N j I If1 * / O <>(" i n r '3 j cr ro DC 090 * C11364 C11365 <i> ro isp> O -t 5 jok S Vil ,IIM '/III)l.-ll) i> i* w iii -i <I-W.1 1T1 tr(-.I\.0i` Cii dg1 c O ctv-> WtrfT/..J)> o roo 01 to M\ eon jn W i'Hi-tvri'.* n tiMiiiu. F i l e >B2S77 3 3 2 . 6 - 3 3 4 . amu .2UL U T - 2 6 3 9 o? rron - jr:k< oo 0O0 Oo rw-oi o*_| i ,r> O ro -- a3* C ro en c-- ro o D erss S P 2 3 3 Q 2 6 - 1/3-y25G RUN Mn IWO *O <.0` ro en o ?M - cNo o r\o ton *T t tn en o w >,1111111,I ipuflAlhlN (II*IAll*l<.% w |P MS data file header from i >B2877 Sample: 2UL UT-2639 Operators GARY MS 9 / 0 7 / 8 4 -13i.06 Mise : SP2330 200-1/3/250 RUN . BTL447 BTL#47 Sys. #: 1 MS models 87 SW/HW r t v . ! CA ALS # : 0 Method file: SP2330 T u n i n g file: APE 101 No. of e x t r a records: Source temp.: 250 Analyser temp.: 0 T r a n s f e r l i n e temp.i m - , C h r o m a t o g r a p h ! c tem p e r a t u r e s : 50. Chromat ograph ic times, min. : 0.0 Chromat ograph ic rate, deg/min: 20.0 300. 2.0 0. 0 0. 0.0 0. 0 0. 0.0 0. 0 0. 0.0 0.0 M/Z - 333.9 F i rst peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. P c ak 4 R. T. first min. sc an m ax scan 1ast peak sc an w i d t h raw area corr. area corr. /. 1 11.990 236 238 242 2 11.990 236 238 242 6 71474 45152 100.00 6 71474 33140 73.40 M/Z = 331.9 First pe ak is b a s e l i n e drop corrected area. S e c o n d p c ak is t a n g e n t s k i m m e d c o r r e c t e d area. Pe ak 4 R. T. f i rst min. sc an max sc an 1ast peak scan width raw area corr. area c orr. * 1 11.990 234 238 244 10 52794 33584 100.00 2 11.99D 234 238 244 10 52794 30404 90.53 332/334 CALCULATION R -G 1o b a 1 i 0 ) = .7 4 3 8 M = 327.9 Fi r s t peak is b a s e l i n e d r o p c o r r e c t e d area. Second peak is tangent skimmed c o r r e c t e d area. C 5"i^ t--'---rJ P e ak 4 R. T. f irst min. sc an 1 12.610 2 12.018 235 235 M/Z * 321.9 max sc an 239 239 1ast peak sc an w i d t h 249 14 249 14 raw area 83067 83067 c orr. area 39667 39492 First peak is b a s e l i n e dr o p c o r r e c t e d area. S e c o n d peak is ta n g e n t s k i m m e d c o r r e c t e d ar ea. Peak 4 R.T. f irst min. sc an m ax sc an 1ast peak scan width raw area 1 0.000 2 0.000 250 250 0 249 0 249 -1 -1 0 0 cor r . area 2178 2178 00092 :'i I a l c orr. y. 160.00 99.56 C11366 corr. s 100.00 100.00 S Mx2 = 319.9 >V)sm First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. ak R. T. first max 1ast peak min. sc an sc an s c a n w i d t h raw area corr. area 1 0.000 2 0. 00 0 25G 250 0 249 0 249 -1 -1 0 2047 0 2047 corr. * 100.00 100.00 3 2 0 '3 2 2 C A L C U L A T I O N R - G 1o b a l k 1> = .9399 M^2 = 257.0 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak t R.T. first min. sc an max sc an 1ast peak scan width raw area 1 0.000 2 0.000 250 25G 0 249 0 249 -1 -1 0 0 corr. area 2717 2717 c orr. 100.00 100.00 <320 + 322)-'<332 +334) CALCULATION R - G l o b a K 3) = .0537 <328'* > / < 3 3 2 + 334) C A L C U L A T I O N R - G 1o b a 1 < 3> - .5035 c o H i n m s i; n n r . miai nifi fr-ifni c o n u iN ii c u a t i s ! SUBj Euj iO 00093 \1 iVE RzJR. C11367 iP r\) G> V <3? -* M I> Otosd. G11368 i-ii ih i.' >( t(ti./.il I1illlI.IIMOlNU ClilM'il Ol W 00 V W ro wro'ooj 00 OJ m n. OIJ ro to <oOjiU'>) O' P=1 c Vo a m u .2UL U T - 2 4 0 I 1O'0 SP2330 200-l'3^2S0 RWH M rTo to ro -i* \ C\O rcon 73 l.ll*l'l<nIMil ...... l`l|(I/(itNiVI(IUt* CO o MS data file header from : >B28?8 Sampl e: 2UL U T - 2 6 4 0 Operators GARY US 9 / 0 7 / 8 4 1 3 : : 2 6 t .., Mi sc ! S P 2 3 3 0 2 0 0 - 1 ^ 3 ^ 2 5 0 R W N B T L # 4 9 B T L # 4 ? Sys. 4: 1 MS model i 87 S U / H U rev. s Cfi A L S # : 0 Method files SP2330 Tuning file: APEI01 No. of e x t r a records: 2 Source temp.: 250 Analyzer temp.:-' 0 T r a n s f e r line temp. : 0 C h r o m t ograph ic t e m p e r a t u r e s : 50. 300. 0. 0. 0. Chromtographic time s i min. : 0.0 2.0 0.0 8.0 0.0 C h r o m a t o g r a p h ic r at e , d e g / m i n : 2 0 . 0 0.0 0.0 0.0 0.0 M/Z *= 3 3 3 . 9 First pe ak is b a s e 1 ine d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peal; R.T. f irst min. sc an max scan 1ast peak sc an width raw area corr. area corr. 1 11.964 238 240 244 2 11.964 238 240 244 6 82683 53067 100.00 6 82683 48456 91.31 M.-'Z = 3 3 1 . 9 First pe ak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d pc ak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak R.T. fi rst min. sc an max sc an 1ast pe ak sc an w i d t h raw area corr. area corr. y. 1 11.964 235 240 250 2 11.964 235 240 250 15 6 9 9 0 6 15 69906 40191 37866 100.00 94.22 c.nap.itri.iinihiii s riinrniiAliUN litiIlAi<nivi c CliilnI(i 332^334 CALCULATION R - G l o b a W 0) = .7574 M.-Z = 3 2 7 . 9 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak R.T. fi rst min. scan max sc an 1ast peak sc an w i d t h raw area 1 11.964 237 241 250 2 1 1.984 237 241 256 13 8 1 9 8 2 13 8 1 9 8 2 M/Z - 321.9 F irst peak is base line drop corrected area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R.T. f irst m in . scan max s c an 1ast peak sc an wi d t h raw area 1 0. 060 2 0.000 251 251 0 250 0 250 -1 -1 0 0 OC 095 T- - corr. area 48299 45575 corr. y 160.00 94.36 corr. area 2192 2192 c orr. X 100.00 100.00 C11369 319.9 'st peak is baseline drop corrected area. 2 nd peak is tangent skimmed corrected area. V R. T. first max 1ast peak min. sc an sc an s c a n w i d t h raw area 1 12.186 251 251 251 2 12.186 251 251 251 0 2216 0 2216 corr. area 2216 2216 corr. V. 100.00 160.00 '322 C A L C U L A T I O N lobalC 1> = 1.0107 = 257.0 rst peak is- b a s e l i n e d r o p c o r r e c t e d area. :ond peak is tang e n t s k i m m e d c o r r e c t e d area. -ik R. T. f irst max 1ast peak l nin . s c an sc an s c a n w i d t h raw area 1 0.000 2 6.060 252 252 0 251 6 251 -1 -1 8 0 c orr. area 2692 2692 corr. % 160.00 100.06 0 + 32 2 )/<332 +334) CALCULATI ON G l o b a l < 3) = .0473 23 /)/<332 + 334) CALCULATION Globali 3) = .5177 ? 3 Fr - --- -- v-v i0 _ 7 A "T *\ ; ?1D ai M L , - i - -i ?" 0C096 C11370 MS data file header from >B2879 Sample: 2UL UT-2641 Operator; GARY MS 9 / 0 7 / 8 4 13:46. .. Mise i SP2330 200-1/3/250 RUN BTL451 BTL#51 Sys. #: 1 MS model: 87 SU/HU rev.: CA ALS : 0 Method file: SP2330 Tuning file: APEI01 No. of e x t r a records: 2 Source temp.: 250 Analyzer temp.: 0 Transfer line temp. : 0 - Chr o m a : ogr a p h i c t e m p e r a t u r e s : 50. 300. 0. 0. 0. Chromatographi c t imes t min. : 8.0 2. 0 0.0 0.0 0.0 C h r o m a t o g r a p h i c rate, d e g /min: 2 0 . 0 0. 0 0. 0 0 . 0 0.0 M/Z = 333.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d pe ak is t a n g e n t s k i m m e d c o r r e c t e d area. P t ak * R.T. first min. s c an max sc an 1ast peak scan width raw area corr. area c orr. 1 11.969 236 237 242 2 11.969 236 237 242 6 79315 51649 100.00 6 79315 28558 55.29 M/Z = 331.9 Firs t peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. P e ak I R.T. first min. scan m ax sc an 1ast peak sc an w i d t h raw area corr. area c orr. X 1 11.99 234 238 246 2 11.990 234 238 246 12 63 3 5 7 12 6 3 3 5 7 37149 36297 190.00 97.71 332/33 4 CALCULATION R - G 1o b a 1 C 0> = .7193 -- .... M/Z = 327. 9 F i r s t p e ak is b as e li n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. P ak R.T. f ir s t min. s c an max sc an 1ast peak sc an w i d t h raw area 1 11.990 233 238 248 2 11.990 233 238 248 15 82503 15 82503 " ' ''' 1Hv corr. area corr. * 45483 ` 108.00 43998 96.74 M/Z * 321.9 First peak is b a s e l i n e dr o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d ar ea. ! Peak * 1 2 R.T. first min. scan 0.060 0.000 249 249 m ax sc an 0 0 1ast peak sc an w i d t h 248 -1 248 -1 raw area 0 0 corr. are a 2164 2164 corn. 100.08 100.00 00098 C11372 : 5 tl/Z * 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Peak R. T. f ir s t min. scan max scan 1asi peak scan width raw area 1 0.000 2 0.00O 249 249 0 248 0 248 -1 -1 0 0 corr. area 2180 2180 c orr. * 100.00 100.00 320^322 CflLCULRTION R - G l o b a l < 1> = 1.0074 ns2 = 257.0 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. P ak # R. T. f i r s t min. sc an max sc an 1ast peak sc an wid t h raw area 1 0.000 2 0.000 249 249 0 248 0 248 -1 -1 0 0 corr. area 2651 2651 corr. /i 100.00 100.00 (320 + 322)/(332 +334) CflLCULRTION R - G l o b a l ( 3) = .0489 (328' )/(332 + 334) CflLCULRTION R - G 1o b a 1( 3) = .5120* 00099 V * tr C11373 n i e >BZS 3 3 3 . 6 - 3 3 4 . 6 *mu.2UL UT-2642 SP2330 266-1/3/250 RUH BT ir*, at >m tv ( m u N'lttvi'ii ii i' 1( *: t * * m n i f >nt,ivir File >2600 321.6-322.6 Amu.2UL UT-2642 SF'2330 2 6 6 - 1 / 3 / 2 5 0 RUN BT 2000- - 9-t"1'...... I T . 10,0 10,5 11.0 ; 11.6 12.0 . :.\L " L' 3JCr T: -- T :~ " 'E ORDER. 12.5 13.0 13.5 14.G 14.5 15.0 n m nr\ C l1374 Im nicniiirvn cH*nr$| tinai'MiccuNiHoisrip"'OHtniN i*1r)o niyvon* MS data, f i l e h e a d e r f r o m ! > B 2 8 8 0 Sample: 2UL UT -2642 Operat or: CARY MS 9/07/84--14::06- . Mise : SP2330 200-1/3/250 RUN BTL453 BTL#53 S v s . ft: 1 MS model: 87 SW/HU rev.: CA ALS : 0 Method file: SP2330 Tuni ng file: APEI01 No. of e x t r a records: 2 Source temp.: 250 Analyzer temp.: 0 T r a n s f e r 1 ine temp. : 0 * Chromatograph!c temperatures : 50 C h r o m t o g r a p h i c times, min. : 0. 0 C h r omatographi c rate, deg/min: 20. 0 300. 2.0 0.0 0 0. 0 0. 0 0m 0. 0 0. 0 0. 0.0 0.0 M/Z * 333.9 F i rst p e ak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t ar g e n t s k i m m e d c o r r e c t e d area. Peak # R.T. first min. sc an max sc an last peak scan width raw area corr. are a c orr. 'A 1 11.970 235 237 241 2 11.970 235 237 241 6 71890 6 71890 44110 37189 100.00 84.31 M/Z = 331.9 First peak is b a s e l i n e drop corrected area. S e c o n d p e ak is t an g e nt s k i m m e d c o r r e c t e d area. Peak # R.T. first m in . sc an rriax scan 1as t p e ak sc an w i d t h raw area corr. area c orr. /. 1 11.970 233 237 246 ' 13 2 11.970 233 237 246 13 57077 57077 30583 29023 100.00 94. 90 332/334 CALCULATION P - C l o b a l < 0) = .6933 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. * Peak *# R.T. first min. scan max sc an 1ast peak sc an width raw area 1 11.990 234 238 249 2 1 1.996 234 238 249 15 80120 15 8 0 1 2 0 M / Z = '3 2 1 . 9 First peak is b a s e l i n e drop correc ted area. S e c o n d pc ak is t a n g e n t sk im m e d c orr.ee t ed area. Peak * R.T. "firs t ruin . s c a n max sc an 1ast peak scan width raw area 1 0.000 -c"k 0 . 0 0 0 250 250 0 249 0 249 -1 -1 0 0 olici corr. are a 42785 42425 corr. * 100.00 99.16 cor r . ar e a 2146 2146 corr. 100.00 100.00 Cl1375 Nri iif I M-'Z = 319.9 ^7880 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Pe ak R. T. fi rst min. sc an max sc an 1ast peak scan width raw area corr. area 1 0.000 2 0.000 250 250 0 249 0 249 -1 -1 0 2025 0 2025 c orr. 100.00 100.00 320.-322 CALCULATION R - G l o b a l C 1) = .9434 M-'Z = 2 5 7 . 0 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Pe ak *# R. T. f irst m in . scan max sc an 1ast peak sc an w i d t h raw area 1 0. 008 2 0.000 250 250 0 . . 249 0 249 -1 -1 0 0 corr. are a 2635 2635 corr. y. 100.00 100.00 (320 + 3225/(332 +334) CALCULATION R - G l o b a l ( 35 = .0558? <32S 5/ (332 + 334 > C A L C U L A T I O N R - G l o b a l < 35 = .5726 t 'W 00102 c c c (5\ z G11376 HU NiMfi HIV*MIN Oinlllll MM`1HIIM1*>11i^iiM | 10.08^.48^.19 SP2330 206-l''3^'250 RUN M OJ to b) OS.J CO \ I OJ (00> Cl. M \ oj r> 01 D ' - OC<0OJ to to to to (M wC'l A A C 'l lb OL <LV|> \ \ I OJ CM CL <A a* t*sor to OJ U Xi 01 C 'l oI> L* 0<10 Cto'l ib -H L_ File >B2S81 333.6-334,6 iJif <<'* *ir.r.ii.t:i t ; ilit ,..111 in T S { I 1 *5 C11377 00103 li OJ Ii C'J Ca.'J ov:i* C'J D 1= a. <> Cf'ml Gj SOr (VJ O(i> C 'J f-r I C'l vji( ivi W u. W a. >< xr >:o Si * I*- !- Li I r>'L>t C'J 0C0O C 'l G) A SQ' j C'J 400000 GC/MS default file: >B2881::01 MS data file header from : >B2S61 Sample: 2UL 10.68/.48/.19 O p e r a t o r s GfiRY MS 9/07/84 Misc : SP2330 260-1/3/250 RUN BTL#17 BTL*17 Sys. is 1 MS model: 87 S U / H U reu.s Cfi RLS # : 0 Method files SP2330 Tuning file: RPEI01 No. of e x t r a records: S o u r c e t e m p . : 25 0 R n a l y z e r temp. :' 0 Transf er 1ine temp. : 14:29 0- 1 Chromatographi c t e m p e r a t u r e s : 50. 300. 6. 0. 0. Chromatographi c times, min. : 0.0 2.0 0.0 0. 0 0.0 Chromatographi c rate, deg/min: 20.0 0.0 0.0 0.0 0.0 - j. !_ M/Z * 333.9 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak R. T. first min. scan max scan 1ast peak sc an w i d t h raw area corr. ar ea corr. Ji 1 11 .996 236 2 33 24 0 2 11 .990 236 2 3 8 2 4 0 4 92020 54400 100.00 4 92020 44332 81.49 M/Z = 331.9 First pe ak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d pe ak is tangent. s k i m m e d c o r r e c t e d area. Peak R ,T .' first min. sc an m ax scan 1ast peak sc an width raw area c orr. area c orr. Ji -C"1.i 1 1.990 11 .990' 235 235 233 238 246 246 11 11 68116 68116 42409 36254 100.00 85.49 m in im o n<w m im r.o m m u s (fi) m c n u u i n c cM *nsJ 332/334 CRLCULBTION R - G 1ob al < 0) = .7 7 9 6 M-Z = 327.9 F i rst peak is b a s e l i n e d r o p c o r r e c t e d area. Second peak is tangent s k i m m e d c o r r e c t e d area. P e ak * R. T. f i r s t min. sc an max scan 1ast peak sc an w i d t h raw area 1 12.010 233 239 247 2 12.010 233 239 247 14 120 0 5 7 14 12 0 0 5 7 M/Z = 321.9 : First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak R. T. first min. scan 1 12.010 2 12.010 236 236 max sc an 239 239 1ast peak sc an w i d t h 243 7 243 7 raw area 2264061 2264061 00104 -- ____ " .. `P JD i-- -!---- :* t, corr. area 85295 82537 corr. J; 100.00 96.77 *" corr, are a 1781339 1746367 corr. 100.00 98.04 C11378 N< l I i p < i p V O f i f n I O WbO.M.N o iv ijo ii kotitinjiio.t s ft.yZ = 319.9 >%M\ First peak is baseline drop corrected are*. Second peak is tangent skimmed corrected area. Feak R.T. fi rst min. sc an tnax sc an 1ast peak sc an wi d t h raw area corr, area 1 12.010 235 239 252 2 12.010 235 239 252 17 1508291 1 4 2 5 9 3 3 17 1500291 1 4 1 2 4 3 5 corr. * 100.00 99.05 320-^322 CflLCULRTI ON R-GlobaK 1) = .8005 M.'Z = 2 5 7 . 0 F irst peak is b a s e l i n e drop c o r r e c t e d area. Second peak is tangent sk i m m e d c o r r e c t e d area. Pe ak R.T. first min. sc an max scan 1ast peak sc an w id t h raw ar e a 1 12.018 234 239 250 2 12.010 234 239 250 16 1201846 16 1 2 0 1 8 4 6 corr. area 1160166 1137966 corr. * 100.00 98.09 (320 + 322 5/(332 +3345 CALCULATION R - GlobalC 35 = 33.1299 ( 3 2 8 " 5 / ( 3 3 2 + 3345 CfLCULflTION R.-Globa1( 35 = .7155 m u H 3 U M P U o a i u 1`j; SU3JECT TO P R O T rc -:- -r ' c\fAr\r- C11379 t i n him Mii-trM in iiivumi >.iiMiino'i i,i< ra n A RUH (inO <VJ m\ \ W-- i <3 (VI CCDO 00 (Vi /.) SF'2336 Tile >B23S2 333.6-334.6 amu.^UL UT-2643 C'IOV OJ IzI-> C'l Al 'LP 0CC-OO1 I 'L P I- l>l CO C-J C C /J C*J A i v < n Li: ili w i :j * `i . n l i * <>fi ' I; >j LJ Mi 'll rH Z 33 oc - lo ; U> u* oj O J \sV o \ C%fi rH I a I ICi o j OJ I-IO- ccoo c--o< ocoo O l 01 bM. Cu . C) CO *r ' 01 l - Ol OJ I 0J <D0 ' OoJj cIo y? Ol (0 OJ M'1 'Ir.' Ucio \ CO01 0-*1> c'oT 'Otl I3--I . co uOr-J> fiu IcOo cOoJ co M OJ C11380 CC/MS default file: >B2882::01 MS data file header from i >B2882 Sample: 2UL UT-2643 Operator: GARY MS 9/07/84 Mise : SP2330 200-1/3/250 RUN BTL#55 BTL455 Sys. #: 1 MS model : 87 SU/HU rev. : CA ALS : 0 Met hod file: SP2330 Tuning file: APEI01 No. of e x t r a records: S o u r c e temp . : 2 5 0 A n a l y z er t e m p 0 Transfer line temp. : 14:51. C h r o m t ographi c temperatures : 50. Chro m a t o g r a p h ic t imes, min. : 6.0 C h r o m a t o g r a p h ic rate, d e g / m in : 2 0 . 0 309. 2.0 0. 0 0. 0.0 0. 0 0 0. 0 0. 0 0. 6.0 0.0 M/Z = 333.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. Second p e ak is tangent s k i m m e d c o r r e c t e d area. Peak -4 R. T. f i rst min. scan max scan 1ast peak sc an w idt h raw area corr. area c orr. '4 1 11.969 235 237 246 2 11.969 235 237 240 5 73051 5 73051 42316 32978 100.06 77.93 M/Z = 331.9 F i rst p t ak is b a s e l i n e dr o p c o r r e c t e d area. Se c ond peak is t a n g e n t s k i m m e d c o r r e c t e d area. P e ak R. T. f i rst m in . scan max scan 1ast peak sc an u idt h raw area corr. -a r e a corr. '4 1 11.969 233 237 248 15 64 164 33924 100.00 11.969 233 237 248 15 64164 32559 95.98 . n tim o t R rm ipf'nam tN mir tM O w w fn n k^nr, cnitpiN G C M in r il 332/334 CALCULATION P - G 1 b a 1< 0> = .8017 M-'-Z = 3 2 7 . 9 su^ fic r ro P R o n c r iV5 ` ; one First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. $t Peak # R.T. first m in . sc an max s c an 1ast peak sc an w i d t h raw area corr. area c orr. y 1 11.990 233 238 248 2 11.990 233 238 248 15 85508 15 8 5 5 0 8 49448 47153 166.00 95.36 M/Z - 321.9 First peak is b a s e l i n e drop correc ted area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Pe ak P. T. first min. sc an m ax scan 1ast pe ak sc an w i d t h raw area corr, area corr. 1 0.060 2 0.060 249 249 0 248 6 248 -1 -1 0 2233 106.00 0 2233 160.00 --j G 11381- 'c-'| ni r i i n u i N i i i : n i n r s | cnni'itir.rnNmnt s r,(mrin.iioM n i i f i i i n wrw on* s M/Z 319.9 First peak is baseline drop corrected area. Second peak is tangent skimmed corrected area. Feak R. T. first min. sc an max sc an 1ast peak s c a n ui dt h rau area 1 0.000 2 0.000 249 249 0 248 0 248 -1 -1 0 0 corr. area 2162 2162 c orr. J; 100.00 100.00 320/322 CALCULATION R - G l o b a l C 1) = .9682 M/Z - 257.0 First peak is baseline drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R. T. first min. sc an max scan 1ast peak sc an w i d t h rau area 1 0.000 2 0.000 249 249 0 248 0 248 -1 -1 0 0 corr. ar c a 2557 2557 c orr. * 100.00 100.00 <320 + 322)/< 332 +334) CALCULATION R - G l o b a l < 3> = .0 5 7 6 <328')/<332 + 334) CALCULATION R -- G l o b a l e i1 ~ .6483 c j 7 0 iMt'IO NO Iic rr- - .. ..c \_ L , SUBJECT TO PROTECTIVE CRCET. 0010A C11382 File >E2SS3 333.6-334.6 .2UL UT-2644 SP2336 20O-1/3/250 RUIN BT 100005000- J 0 -i-- i-- i-- i-- i-- i-- i-- i-- |-- i-- i-- i-- i-- | i i i-- i-- |-- i-- i-- i-- i-- |-- i-- i-- i i |-- i-- i-- i-- r - ]-- i-- i-- i-- i-- |-- i-- n -- r--j-- i i i-- r - ) 10.0 10.5 11.0 11.5 12.0 12.5 13.0 3.5 ' 14.0 14.5 15.0 File >B2B83 331.6-332.6 amu .2UL UT-2644 SP2330 200-1/3/250 RUH BT 4000- 1 '' ' | i 1 ' 1 1 i 1 11 i i 10 .0 18.5 1.0 11.5 12.0 12. >B2883 327.6- . 6 artiu .2 U L U T - 2 6 4 4 13*. 0 '13*. 5 ' '14*. 0 ' '14*. 5 ' 'lV.0 SP2330 200-1/3/250 RUH BT 8000- 4000-- /v-- ^ o- ----1--T-- -10.0 10.5 11.0 V_/\-- 1i ' 11 1 i 1 1 1 i 1 11 1i 1* ' i1 ' 1 1 i i 1 1 1'i 11.5 12.0- 12.5 13.0 13.5 14.0 14.5 15.6 File >2883 3 2 1 . 6-322.6 amu.2UL UT-264'4 J 8600" S P 2 3 3 0 2 6 0 - 1 / 3 / 2 5 0 RUIN BT 4000- J F ile 0 " |-- -- -- [--1-- -- i-- 1-- I-- I-- I-- 1-- i-- 1-- i-- |-- i-- i--i-- i-- I-- i-- i-- I I 1-- m -- i-- r-|-- i-- i-- i-- i-- |-- i-- i-- i-- i-- -- i-- r--i-- i-- |-- i-- i-- i-- i-- | 1O.0 10.5 11.0 11.5 12.0 12.5 13.0 13.5 14.0 14.5 15.0 >2833 3 1 3 . 6 - 3 2 0 . 6 amu . 2UL U T-2644 3F'2330 200 - 1/3'250 RUN BT 4000- ''Van* 10'. 0 F i l e >2883 4000- 10'.5 11'.0 11'.5 12.0 12'.5 2 5 6 . 7 - 2 5 7 . 7 amu . 2UL U T-2644 V-- 1 3 .0 1 3 . 5 14'.0 1 4 .5 153'. O... (T^;-"SP*'233-0"2 0 0 - 1 / 3/ 2 5 0 RUN BT _ i .,* f & i r - ------ ' ._ ! -- t'- . \ J c L ` l 0 PHOTECTJ','E OROER. .................................................. 10.0 10.5 11.0 .p 11.5 12.0 12.5 13.0 1I || 13.5 14.0 14.5 15.0 OCIOS C11383 (oil n ic a n p iN G c h a r t s '] r.n .p iu c itmnihoi 5 ctinpnHArioN hvffm o nfw tP* GC/nS default file: >B2883::Q1 MS data file header from i >B2883 Sample: 2UL UT-2644 Operator: GARY ns 9/07/84 15:11. disc : SP2330 200-1/3/230 RUN BTL#57 BTL#57 Sys. #! 1 ns model : 87 S U / H U r e v . : CA A L S : 0 dethod file: SP2330 T u n i n g file: APEI01 No. of e x t r a r e c o r d s : 2 Source temp.: 250 Analyzer temp. 0 T r a n s f er 1ine temp. : 0 - C h r o m a t o g r a p h ! c t e m p e r a t u r e s : 50. 300. 0. 0. 0. C h r o m a t o g r a p h ! c t imes, mi n. : 0 .0 2. 0 0. 0 0 . 0 0. 0 Chromatographic rate, deg/min: 20.0 0.0 0.0 0.0 0.0 n/2 333.9 F i rst peak' is b a s e l i n e d r o p c o r r e c t e d area. Second peak is tangent s k i m m e d c o r r e c t e d area. Peak tf R. T. fi rst min. scan max scan 1ast peak scan u idth raw area corr. area corr. * 1 11.963 239 240 245 2 11.963 239 240 245 6 64015 38083 100.00 6 64015 27307 71.70 M/Z = 331.9 First peak is b a s e l i n e drop c o r r e c t e d area. Second peak is tangent s k i m m e d c o r r e c t e d area. Peak * R.T. f irst min. scan max scan 1ast peak sc an w i d t h raw area corr. area corr. 1 11.984 235 241 251 11.984 235 241 251 16 59207 16 5 9 2 0 7 26615 25775 100.00 96.84 332/334 CALCULATION R - G l o b a l C 0) = .6989 * First peak is b a s e l i n e d r o p c o r r e c t e d area. Second peak is tangent s k i m m e d c o r r e c t e d area. P e ak 4 R.T. first m in . sc an max scan 1ast peak sc an width raw area 1 12.084 238 242 251 2 12.004 238 242 251 13 7 2 1 8 7 13 72187 n/z * 321.9 F irst peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is ta n g e n t s k i m m e d c o r r e c t e d area. Peak R.T. f irst min. sc an max scan 1ast peak scan width raw area 1 12.004 240 242 247 2 12.004 240 242 247 7 49469 7 49469 ocim corr. area 39973 38348 c orr. * 100.00 95.93 - corr. area 26432 19372 corr. % 100.00 73.29 01138^ NO HP 9 2 7 0 O M O s M/Z 319.9 First peak is baseline drop corrected res. Second peak is tangent skimmed corrected ire*. Peak R. T. f irst min. scan max scan 1ast peak sc an ui dt h rau area 1 12.004 ' 240 242 249 2 12.004 240 242 249 9 39755 9 39755 corr. area 18911 13560 c orr. % 100.00 71.70 320^322 CRLCULRTI OH R - G l o b a l < 1) * .7155 M/Z- 257.0 First peak is b a s e l i n e d r o p c o r r e c t e d area. Second peak is tangent s k i m m e d c o r r e c t e d area. Peak R. T. fi rst min. sc an max sc an 1ast peak scan width rau area 1 12.004 240 242 249 2 12.004 240 242 249 9 41947 9 41947 corr. area 17323 14335 corr. * 100.00 82.75 C320 + 322 ) / ( 3 3 2 + 3 3 4 ) `C R L C U L R T I ON R - G l o b a l C 3) = .7008 328')/<332 + 334) CRLCULRTION R - G l o b a l C 3) .6142 OCill C11385 File >B2884 333.6-334.6 amu SUL UT-2645 SP2330 200-1/3/250 RUN BT i<'i n> <:u n u i f i u * ; n T ; p t; iM r n ir File >B2884 321 .6-322.6 amu.^UL UT-2645 SP2330 200-1/3/250 RWN BT _s ! i "w :i i SUB.iFTT T O PDATri-Tu/ir o n n r n n r - f -i o G11386 fJi 1 H(* U ^ y ( > C * f t A O GC/ilS default file* >B2684*i01 MS data file header, from i >B2884 Sample* 2UL UT-2645 Operator* GARY US 9/07/84 Hi sc t S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 R U N B T L 4 5 9 B T L 4 5 9 $y%. t 1 MS Model* 67 S W / H W rev.i CA ALS * 0 . Hethod file* SP2330 T u n i n g file* APEI01 No. of e x t r a record: Source temp.: 250 Analyzer temp.it 0 T r a n s f er 1 ine temp.. : 1S 3 1 ___ C h r o m a t o g r a p h ic t e m p e r a t u r e s : 50. C h r o m a t ographi c t imes i min. : 0.0 Chromatographic rate, deg/mini 20.8 3 0 0 i^ 2. 0 0. 0 0. 0.0 0.0 0e 0. 0 0. 0 0. 0.0 0.0 n/Z 333.9 F i rst pcalc is b a s e l i n e d r o p c o r r e c t e d area. Second peak is tangent sk i m m e d c o r r e c t e d area. Peak * R. T. f i r s t min. scan max sc an 1ast peak scan width raw area corr. area corr. y. 1 11.969 236 237 240 2 11.969 236 237 240 4 63191 4 63191 33383 28653 100.80 85.63 n/Z 3 3 1 . 9 First pe ak is b a s e l i n e dr o p c o r r e c t e d area. Sec ond peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak R. T. f irst min. scan max scan 1ast peak scan width raw area corr. area corr. y. 1 11.990 235 238 246 11 52378 27661 100.00 2 11.990 235 238 246 11 52378 26385 95.39 coniroisi:oh>h*ion pufpalowrwtora * fSTREConutNo crtnii] 332/334 CALCULATION R - G l o b al < 0> = .8286 n/z = 3 2 7 . 9 F irst peak is b a s e l i n e drop c o r r e c t e d area. Se c o n d peak is ta n g e n t s k i m m e d c o r r e c t e d area. c T- S U B J E C T 1: ^ __ 1 ' -TCVE ORDER. Peak 4 R.T. f irst min. sc an max scan 1ast peak sc an w i d t h raw area corr. area corr. y. 1 11.990 235 238 248 13 73204 4 4 0 1 9 1 0 0 . 0 0 2 11.990 235 238 248 13 73204 42550 96.66 n/z - 32 1 . 9 F irst peak is b a s e l i n e d r o p c o r r e c t e d area. Second peak is tangent s k i m m e d c o r r e c t e d area. Peak * R.T. fi rst min. scan max sc an 1ast peak sc an w i d t h raw area corr. area 11387 corr. 1 12.010 237 239 243 2 12.010 237 239 243 6 23045 6 23045 0G113 8567 6206 100.00 72.95 No Hp(i? 7 0 0 firt0 5 M/2 319.9 First peak is baseline drop corrected tret. Second peak is tangent skimmed corrected &rr*. Peak R.T. fi rst min. sc an max sc an last peak scan. w i d t h raw area 1 11.990 235 238 245 10 2844 2 11.990 235 238 245 10 28464 >3w&\ corr. area 6954 6474 corr. 4 100.00 93. 10 320/322 C L C U L T ION R - G l o b a l < 1) = .8174 M / 2 = 2 5 7 . 0 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R.T. first min. scan max scan 1ast peak sc an w i d t h raw area 1 12.010 235 239 245 10 3 1 6 8 7 2 12.010 235 239 245 10 31687 corr. area 7487 6737 corr. 4 100.00 89. 98 <320 + 322)/<332 +334) CflLCULRTION R - G l o b a l < 3) = .2533 <328') / <332 + 334) CRLCULflTlON R - G l o b a l < 3) - .7198 C* X o z u6 -- ____________ - i i - > A ! L SUBJECT TO PROTECTIVE ORDER. 00114 C11388 rc- c\ z File >B2S85 333.6-334.6 *mu 2UL .2669/.48/.19 SP2330 206-1/3/250 RUN BT File > B 2 8 8 5 3 2 1 . 6 - 3 2 2 . 6 a m u . 2 U L .2669/ .48/ .19 S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 RUN BT < , n * P m c i,iiriMir>i GC/NS default filet >B2885::01 US data file header from t >B2885 Samplet 2UL .2669/.48/.19 Operalori GRRY HS 9/07/84 15:54- ttisc : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 R U N B T L # 2 9 B T L # 2 9 S y s . #: 1 NS modelt 87 SU/HU reu.i CR ALS : O Nethod filet SP2330 T u n i n g file: RPEI01 No. of e x t r a records: 2 Source temp.: 250 Analyzer temp.i 0 Transfer line temp, : 0 - C h r o m a t ographi c t e m p e r a t u r e s t 50. 300. 0. 0. 0. C h r omatographi c t im e s , min. : 0.0 2.0 0.0 0.0 0.0 Chromatograph! c rate, deg/mint 20.0 0.0 0.0 0.0 0.0 n/Z 333.9 First peak is bas e l i n e drop c o r r e c t e d area. S e c o n d peak is ta n g e n t s k i m m e d c o r r e c t e d area. Peak # R. T. f irst min. sc an max sc an 1ast peak sc an w i d t h rau area corr. area corr. */. 1 11.969 236 237 242 2 11.969 236 237 242 n/z = 331.9 6 66036 41466 100.00 6 66036 25473 61.43 First peak is base 1ine drop c o r r e c t e d area. S e c o n d p e ak is t a n g e n t s k i m m e d c o r r e c t e d area. P e ak R. T. fi rst min. scan max sc an 1ast peak sc an uh dt h raw area corr. area corr. 7. 1 11.969 227 237 255 28 85164 29164 100.00 2 11.969 227 237 255 28 85164 27330 93.71 le l'm c o n iM t c i i a m s i G iu rin e i.P N tn o is C im ra n M iO N n u i u i i t n i w i m 332/334 CALCULATION R - G l o b a K 6> = .7033 n/Z = 327.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. Second peak is tangent s k i m m e d c o r r e c t e d area. Peak R.T. fi rst min. sc an max sc an 1ast peak scan width raw area 1 11.990 231 238 251 20 85511 2 1 1.990 231 238 251 20 85511 N/Z - 321.9 F irst peak is base 1ine drop corrected area. Second peak i s t angent skimmed corrected area. Peak 4. R.T. f irst min. sc an max sc an 1ast peak sc an width raw area 1 12.010 237 239 243 2 12.010 237 239 243 6 47193 6 47193 corr. area 42731 41161 corr. * 100.06 96.33 c orr. area 25685 18531 corr. * 100.00 72.37 C11390 N il u p (*? 7 0 0 fi/10 IUO. M ill OlVJJiltl NOIlVIlU.mOJ SIOIIINI) I s n/Z - 319.9 First peek is baseline drop' corrected ere*. Second peek is tengent skimmed corrected ere*. Peek tf R.T. fi rst min. seen mex sc en 1est peek seen u idt h r*u eree 1 11.990 235 238 247 2 11.990 235 236 247 12 46973 12 46973 corn. eree 22229 21065 corr. 7. 100.00 94.76 320/322 CALCULATION R - G 1 o b * l < 1) = .6662 M/Z = 257.0 F irst peek is b a s e 1 ine d r o p c o r r e c t e d eree. Second peek is tengent s k i m m e d c o r r e c t e d eree. Peak R.T. first min. seen max seen 1est peek seen u idt h ray eree 1 12.010 235 239 246 2 12.010 235 239 246 11 4 5 6 6 6 11 4 5 6 0 6 corr. eree 18933 17981 c orr. 7. 100.00 94.97 <320 + 322)/<332 +334) CALCULATION R - G 1 o b e l C 3) = .6772 C328'')/(332 + 334) CALCULATION R - G l o b a l C 3) = .6017 e ? m n H J 0 I QUO 3 1 u [.-J ( c l 11 o n / V-r" SUBJECT TOprotective o r d e r OC 117 011391 OC 118 C11392 e >2890 3 3 3 . 6 - 3 3 4 . 6 * m u . 2 U L .i0 6 8 / . 4 8 / . 19 SP2330 200-1/3/250 ET 44 .le > 2 8 9 6 3 2 1 . 6 - 3 2 2 . 6 a m u .S U L .10 6 8 / . 4 8 / , 1 9 SP2330 200-1/3/250 BT * z 3 |4 z3 0C119 C11393 QQ/I |( h i r o n t i i N t ; c H n n i < i | i;nptiic c o m i n o ) S coneniiAiioN n u f r * io n f w ( " * S M/Z * 319.9 > > 9^ o First peak is basel i nt drop corrected ere*. Second peak is tangent skimmed corrected area. Peak R.T. fi rst min. sc an max sc an .1 ast peak s c a n ui dt h raw area 1 11.777 218 225 238 20 71761 2 11.777 218 225 238 20 71761 corr. area 30181 29711 c or r . 5! 100.06 98.44 320/322 CALCULATION R - G 1obal < 1) * .8200 M/Z 257.0 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak * R.T. f irst m in . sc an itiax scan 1ast peak scan w id th raw area 1 11.777 219 225 237 18 2 11.777 219 225 237 18 64139 64139 c orr. area 19013 17528 com. * 100.00 92. 19 (328 + 322 >/(332 +334) CALCULATION R - G l o b a l ( 3) = .2547 (3 2 S ' >/(332 + 334) C A L C ULATION R - G 1obalC 3> = .3587 / CT r o protective: \s * \ k n 0G1 2 1 z C11395 Flit >B2691 333.6-334.6 *mu.2UL 1.058/.48 19 SP2339 208-1/3/250 BT F i l e > 2 8 '?1 3 2 1 . 6 - 3 2 2 . 6 a m u . S U L 1 . 6 8/. 48/. 19 SP2330 200-1/3/250 BT OC 122 cll396 MS data file header from : >B2891 Sample: 2UL 1.868/.48/.19 Operator: GARY Mise : SP2330 200-1/3/250 BTL405 BTL# $ys. #: 1 MS model : 87 S U / H U rev.: Cfi Method file: SP2330 Tuning file: RPEI01 Source temp.: 250 Rnalyzer temp.: 0 MS 9/10/84 22:04--- ^ 5 RLS # : 0 No. of e x t r a record: 2 T r a n s f e r line temp. : 0 Chromat ographi c t emperatures : 50. 300. 0. 0. 0. Chromatographi c times, min. : 0.0 2. 0 0.0 0.0 0.0 C h r o m a t o g r a p h ic rate, d e g / m i n : 2 0 . 0 0.0 0. 0 0. 0 0. 0 M/Z - 333.9 Fir s t peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak 4 R. T. fi rst min. scan 1 11.764 2 11.764 223 223 max scan 229 229 1ast peak scan width 254 31 254 31 raw area 225099 225099 corr. area 166447 162045 corr. * 100.00 97.36 . M/Z * 331.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is ta n g e n t s k i m m e d c o r r e c t e d area. P e ak R.T. first min. sc an max scan 1ast peak scan width raw area corr. area corr. * 1 11.764 223 229 243 2 11.764 223 229 243 20 172067 130947 100.00 20 172067 128637 98.24 (oil n i c o r d in o t i i a H T S l r.tiA .i.ii; r o N in tn s cOHf**R*iON n u r i i n h i * to 332/334 CALCULATION R - G l o b & l < 0? = .7867 M/Z * 327.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. s u b j e c t to p*o t; _ ' - n u ltCTIVr , Peak /4 R.T. fi rst min. sc an max scan 1ast peak scan width raw area corr. area corr. 4` 1 11.785 223 238 24 6 2 11.785 223 230 246 23 158160 111378 100.00 23 158160 108813 97.70 M/Z 321.9 F irst peak is base 1ine drop corrected area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak * R.T. fi rst min. sc an max sc an 1ast peak sc an w i d t h raw area corr. are a corr. 1 11.785 225 230 246 2 11.785 225 230 246 21 401804 359909 100.08 21 4 0 1 8 0 4 3 5 1 2 7 8 97. 60 C11397 n f-i/lfl NO u p 5 MxZ * 319.9. First peak is b a s e l i n e drop c o r r e c t e d area. Second peak is tangent s k i m m e d cprre c t e d r*. Peak tt R. T. f irst min. scan max scan 1ast peak s c a n ui d th rau area 1 11.765 219 230 256 2 11.785 219 230 256 37 380462 37 380462 corr. area 309718 300357 corr. 4% 100.00 96.98 . 320*'322 C A L C U L A T I O N R - G l o b a l < 1) * .6605 M / Z '* 2 5 7 . 0 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is tangent, ski mm e d c o r r e c t e d area. P ak - R.T. f irst min. sc an max sc an 1ast peak scan width rau area 1 11.785 224 230 251 2 11.785 224 230 251 27 252992 27 252992 corr. area 185114 182408 corr. 4` 100.00 98. 53 <320 + 322)s <332 +334) CALCULATION R - G l o b a l < 3) = 2.2516 <328'> '(3 3 2 + 3 3 4 ) C A L C U L A T I O N R - G l o b a l < 3) = .3636 i I I ? G . object'TO r;R O T ? -- 00123 C11398 c crrc\>. zC le >B2897 333.6-334.6 *mu.2UL 19.68/.48/.19 SP2330 200-1/3/256 RUH BT 'ile > B 2 8 9 7 3 2 1 . 6 - 3 2 2 . 6 an.u.2UL 10.68/. 48/. 19 S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 RUN BT l' I|f| i 351 OC 124 C11399 nu*M Ln w * r n n s M/Z 319.9 yinum First peak is baseline drop corrected area. Second peak is tangent skimmed, corrected area. Peak R.T. first mi n. sc an max sc an 1ast peak sc an ui dt h raw area corr. area 1 11.610 213 229 253 2 11.810 213 229 253 40 2778746 2694226 40 2778746 2666846 c orr. ii 100.00 99.06 *" 320/322 CALCULATION * R - G 1 o b a l ( 1> - .6272 M / Z ` 257.0 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak -# R.T. f irst min. sc an max scan 1ast peak sc an w i d t h raw area 1 11.830 216 230 249 . 33 1801888 2 11.836 216 236 249 33 1601888 corr. area 1722160 1693268 corr. 106.00 98.32 C320 + 3 2 2 > / C 3 3 2 + 334) CALCULATION R - G l o b a l < 3> = 23.6167 (328'' > / < 3 3 2 + 3 3 4 ) C A L C U L A T I O N R - G l o b a l < 3) = .3356 ( S ( n t c o n o i M O c i < * n i s | f i n * . m e r u N i n o i s i :<i h m * m a m o n N o HP n ? / 0 iir 1 0 00126 C11401 File >B2S99 333.6-334.6 amu.2UI_ UT-2629D SP2330 200-1/3/258 RUH BT File >2399 321.6-322.6 amu.SUL UT-2629D SP2330 208-1/3/250 RUH BT I; i 0G12.-7 011402 GC/MS default filii >B2899:i01 MS data file header from i >B2899 Sample* 2UL UT-2629D Operatori GARY MS 9/11/84 Mi sc I S P 2 3 3 0 2 0 0 - 1 ^ 3 / 2 5 0 R U N B T L * 2 1 B T L # 2 1 Sys. : l MS m o d e l i 87 S U / H U reu.t Cfl A L S i 0 Method filei SP2330 Tuning file! APEI01 No. of e x t r a records: 2 Source temp.: 250 Analyzer temp. : 0 Transfer 1ine temp. : 01.44.. Chromatograph!c temperatures i 50. 300. 0. 0. 0. C h r o m a t o g r a p h ! c t imes| min. i 0. 0 2 . 0 0 . 0 0 . 0 0. 0 Chromatograph!c rate, deg/mint 20.0 0.0 0.0 0.0 0.0 M/Z - 333.9 First peak is bas e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n g e n t sk im m e d c orreci ed area. Peak R. T. fi rst min. sc an max sc an 1ast peak ' s c a n ui dt h rau area corr. area corr. 7. 1 11.789 225 228 238 2 11.789 225 228 238 13 3 9 4 0 8 13 3 9 4 0 6 12251 11952 100.00 97.56 M/Z 331.9 First peak is b a s e l i n e dr o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d 'area. Peak * R. T. f irst min. sc an max scan 1ast peak sc an ui dt h rau area corr. area corr. * 1 11.809 224 229 234 2 11.809 224 229 234 10 31155 10 3 1 1 5 5 10345 9205 100.00 68.98 C Oftpfrvo C H A R r r ] ORIFft'C CIJNIHOIS rDPWHArp>M IM IfM lO NiW yl 332/334 CALCULATION R-Global( ii G .8444 M/Z - 327. 9 First peak is b a s e l i n e d r o p c o r r e c t e d area. Second peak is tangent s k i m m e d c o r r e c t e d area. , Peak # R.T. fi rst m in scan max sc an 1ast peak s c a n wi dt h rau area 1 1 1 . 6 0 9 2 2 6 22 9 23 7 11 4 2 3 2 4 2 1 1 . 8 0 9 2 2 6 2 2 9 2 3 7 11 4 2 3 2 4 M/Z - 321.9 First peak is bas e l i n e drop c o r r e c t e d area. Second peak is tangent sk i m m e d c o r r e c t e d area. Peak R. T. fi rst min. scan max sc an 1ast peak sca n u idt h rau area 1 11.809 225 229 239 14 35923 2 1 1 .809 225 229 239 14 3 5 9 2 3 0C128 ------- --1 'i'.i, ;^ -- ,_ s u b j e c t t . ' j - ^ '* ` -1 '-'TECTIVE , corr. area 10842 10039 corr. y. 100.00 92. 59 corr. area 7629 7104 corr. v. 100.00 93.12 elidila N O IIP f*? mi i m i ' n i w w * M-'Z 319.9 F irst peak- is b a s e l i n e d r o p c o r r e c t e d area, Seco n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak ft R.T. first min. scan max scan last peak scan uidth rau area 1 11.630 225 230 234 2 11.830 225 230 234 9 24198 9 24198 co r r . area 5514 4443 corr. 100.00 80.58 320/322 CALCULATION R - G l o b a l ( 1> = .7228 M/Z * 257.0 F irst peak is b a s e l i n e d r o p c o r r e c t e d area. Second peak is tangent s k i m m e d c o r r e c t e d area. Peak tt R.T. f irst min. sc an max sc an 1ast peak sc an width rau area 1 11.8B9 227 229 233 2 11.809 227 229 233 6 20973 6 20973 corr. area 4749 4080 c orr. * 100.00 85.91 (320 + 322 >/(332 +334) CALCULATION R - G l o b a l < 3> = .581? (32S'>/(332 + 334) CALCULATION R - G l o b a l ( 3) = .4768 jStl R f c o M i N Q c i i f t m s ) a f l * r m c r o N t f l o i s M O IH * 'l i '7 0 0 (> * 1 0 w3JECT TO PROTECTIVE ORDER. OC15c9 C l 1404 Fil* >B2903 333.6-334.6 *mu.2UL .2669^.46/.19 SP2330 290-1/3/250 RUN BT t ! F File >B2903 321 .6-322.6 amu.SUL .2669/.48/. 19 SP2339 2 0 0 - 1 / 3 / 2 5 0 RUN BT T 3 0G130 C11405 MS data file header from i >B2903 Sample: 2UL .2669/.48/.19 Operator: GARY MS 9/11/84- 2:05 Mi sc : S P 2 3 3 0 2 0 0 - 1 / 3 / 2 5 0 RUN- B T L 4 2 9 B T L 4 2 9 Sys. 4: 1 MS mod e l : 87 S W / H M rev.: Cfi AL S # : 0 Method file: SP2330 Tuning file: RPEI01 No. of e x t r a records: 2 Source temp.: 250 Analyzer temp.: 0 T r a n s f e r line temp. : 0 ... _. Chromat ograph ic t e m p e r a t u r e s : 50. 300. 0. 0. 0. C h r o m a t o g r a p h i c t im e s , min. : 0. 0 2.0 0 . 0 0 . 0 0. 0 Chromatographi c rate, deg/min: 20.0 0. 0 0.0 0.0 0.0 M/Z * 333.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak 4' R.T. first min. scan max scan last peak s c a n ui dt h rau area corr. area c orr. y. 1 11.763 219 225 241 2 11.763 219 225 241 22 154286 109670 100.00 22 154286 105347 96.06 M/.Z = 3 3 1 . 9 First peak is b a s e l i n e drop c o r r e c t e d area. S e c o n d peak is t a n gent s k i m m e d c o r r e c t e d area. P e ak 4 R.T. f irst min. scan max scan 1ast peak sc an w i d t h raw area corr. area corr. y. 1 11.763 221 225 241 2 11.763 221 225 241 20 132155 20 132155 92415 88415 100.00 95.67 t i l t i l R CO n o m o C H A F S I nnAPMlC CONINOi S CnnrfTHAnON M IM U tO NfW TlW i1 332/334 CALCULATION R - G l o b a K 6) = .8427 CJ. . M/Z = 327.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak 4 R .T . f irst min. sc an max scan 1ast peak scan width raw area 1 11.783 221 226 242 2 11 .7 8 3 221 226 242 21 1 i e 8 3 9 21 1188 3 9 M/Z * 321.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak 4 R.T. f irst min. scan max sc an 1ast peak sc an w i d t h raw area 1 11.783 221 226 241 2 11.783 221 226 241 20 101979 20 101979 SUBJECT TO protective:o r d e r corr. area 72248 68670 c orr. X 100.00 95. 06 c orr. area 61939 60189 c orr. 100.00 97. 17 C11406 N l) H P (l ? 7 0 O filO s M/Z 319.9 First peak is b a s e l i n e drop c o r r e c t e d Ares. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak R.T. f irst min. sc an max sc an 1ast peak sc an ui dt h raw area 1 11.803 222 227 240 2 11.603 222 227 240 18 66129 18 68129 corr. area 50347 50275 corr. * 100.00 99.66 320^322 CRLCULflTION R - G 1o b a l < 1> = .6128 M / Z `= 2 5 7 . 0 First peak is b a s e l i n e dr o p c o r r e c t e d area. S e c o n d p e a k is t a n g e n t s k i m m e d c o r r e c t e d area. Peak * tt R.T. fi rst min. scan max sc an 1as t peak scan width raw area 1 11.803 223 227 239 2 11.603 223 227 239 16 7 6 5 7 9 16 76579 corr. area 35907 3521 1 corr. 5i 160.00 98.66 <320 + 322 )/(332 +334) CALCULATION R - G l o b a K 3)= .5556 < 3 2 8 0 / ( 3 3 2 + 334) CALCULATION R - G 1o b a l < 3)= .3547 - fiII [ m i'M to jcl n t c a n o i x n E M .n r s j GRtF-iitc ri>Ntni>i 5 N(1 M P < i ; ' 7 0 r i f i l o J. -j 4 SUBJECT TO PROTECTIVE ORDER. 00132 C11407 File >B2907 333.6-334.6 *mu.2UL 2.669/ .48/ .19 SP2330 200-1/3/250 RUH BT File >B2907 321.6-322.6 *mu.2UL 2.669/.48/.19 SP2330 200-1/3/250 RUN BT C l1 4 0 8 MS d*t* file he*der from i >B2907 Sample: 2UL 2.669/.48/. 19 Operator* GARY MS 9 / 1 l/84--15:-2? _ Mise i SP2338 208-1/3/250 RUN BTL#41 BTL441 Sys. 4: 1 MS model : 87 SU/HM r e v . i CA ALS : 0 Method file: SP2330 Tuning file: APE 101 No. of e x t r a records: 2 Source temp.: 250 Analyzer temp.i 0 T r a n s f er 1 in e temp. : . 0 *" Chromatographi c t emperatures i 50. 300. 0. 0. 0. C h r o m a t o g r a p h ! c times, min. : 0. 0 2. 0 0 . 0 0 . 0 0. 0 C h r o m a t o g r a p h i c rate, deg/mi n: 2 0 . 0 0. 0 0.0 0 . 0 0.0 *. . M/Z 333.9 F i r s t peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak * R.T. fi rst min. sc an max scan 1ast peak s c a n ui dt h raw area corr. area corr. y. 1 11.774 218 229 250 2 11.774 216 229 250 34 205931 34 205931 134089 133953 100.00 99.90 M/Z = 331.9 F irst pe ak is b a s e 1 ine d r o p c o r r e c t e d area. S e c o n d peak is t a n gent s k i m m e d c o r r e c t e d area. Peak R.T. fi rst min. sc an max sc an 1ast peak scan width raw area corr. area corr. y 1 11.774 216 229 248 2 11.774 216 229 248 32 177960 112232 100.00 32 177960 108600 96.76 m c'i wi c t i R o i m o C N A n f f | r . n * p n j c l u n i m o i s :4 o n r c m M i o n o u r r * L O N f w n ' w ^ 332/334 CALCULATION R-Global(0>= M/Z = 327.9 .8370 t? First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak R.T. fi rst mi n. s c a n max scan 1ast peak sc an w i d t h raw area corr. area 1 11.794 220 230 251 2 11.794 228 230 251 31 160851 31 160851 94325 94170 M/Z * 321.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak 4 R.T. f irst min. sc an max sc an .last peak scan width raw area corr. area 1 11.794 215 230 246 2 11.794 215 230 248 33 800755 735019 33 800755 717677 nrt,i o a tjv e o r d e r . c orr. y* 100.00 99.84 corr. y. 100.00 97.64 C11409 N O IH J i * ? 7 D O lia li ) tHOiHIN tlltn iM I NOMVtHMMU) S IOMINOJ ItlK.IVMO ( S i m i l i DWIOItOJIM I1- >1 M-Z 319.9 First pe ak is b a s e l i n e drop c orrec ted area. S e c o n d pe ak is t a n g e n t s k i m m e d c o r r e c t e d ar ea. Feak # R. T. f ir st min. sc an m ax scan 1ast pe ak sc an w i d t h r au area 1 11.794 223 230 257 2 11.794 223 230 257 34 694491 34 694491 c or r . are a 624893 616699 c or r . y. 100.00 98.69 320^322 CRLCULRTION R - G 1o b a 1 c 1) * .8502 M 'Z . 2 5 7 . 0 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peek is t a n g e n t s k i m m e d c o r r e c t e d area. Peak R. T. f ir s t min. sc an max sc an 1ast pe ak scan width r aw area 1 11.794 224 2 33 252 C. 11 . 7 9 4 224 2 33 2 52 28 504553 28 504553 corr. ar e a 434217 425355 corr. V, 100.00 97.96 (320 + 322 >/ ( 332 *-334) CftLCULftTION R - G 1o b a l ( 3 ) * 5.5209 (328')/(332 334 ) CRLCULRTI ON R - G 1o b a l ( 3) = .3561 * I I l1 O N 0C 135 C11410 File >B2906 333.6-334.6 *mu.2UL 26.69/. 48/. 19 SP2330 208-1/3/250 RUH BT File >E2?6B 3 2 1 . 6 - 3 2 2 . 6 amu.^UL 2 6 . 6 9 / . 4 8 / . 1 9 SP2330 2 0 0 - 1 / 3 / 2 5 0 RUN BT OCI06 Cll411 MS data file header from : >B290S Sample: 2UL 26 .69/.48/.19 Operatori GARY 1MS 9 / 1 1 / 8 4 -15 :-4? . . Mise * SR2330 200-1/3/250 RUN . BTL43 BTL43 Sys. il 1 MS model 1 87 SU/HU reu. i CA ALS i I 0 M e t h o d fi 1e I S P 2 3 3 0 T u n i n g fi lei R P E I 0 1 Source temp.: 250 Analyzer temp .i 0 No. of e x t r a recordsi T r a n s f e r l i n e temp. ms 2 0 Chromatograph!c temperatures I 50 300. 0. 0. 0. C h r o m a t o g r a p h i c t i m e s , min. I 0. 0 2 . 0 0 . 0 0 . 0 0 .0 C h r o m a t ographic ratei deg/mini 20. 0 0.0 0.0 0.0 0 .0 M/2 333.9 First peak is b a s e l i n e d r o p c o r r e c t e d area. Second peak is tangent skimmed corrected area. Peak #` R . T. f i r s t min. scan max scan last peak sc an wi dt h raw area corr. area corr. % 1 11.796 219 231 252 2 11.796 219 231 252 33 242219 171830 100. 00 33 242219 171401 99. 75 - M<2 * 331.9 First peak is baseline drop corrected area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak # R.T. first min. scan max scan 1ast peak scan width raw area corr. area corr. Am 1 11.816 224 232 244 2 11.816 224 232 244 20 181045 139325 100. 00 20 181045 1 3 9 2 2 5 99. 93 332/334 CALCULAT ION R-Gl obal (. 0) = .8108 M/2 = 327.9 First peak is base 1ine drop corrected area. Second peak is tangent skimmed corrected area. ^ W J L u /'?J'T7 + S U!BR Jrcv-r * - ____ ^ PPOTP'-- -' -- ' - -U n 'pVE O RvD E Z . - Peak 4 R.T. first min. scan max scan 1ast peak sc an width raw area corr. area corr. * 1 11.837 226 233 242 2 11.837 226 233 242 16 243276 208908 100.00 16 2 4 3 2 7 6 205100 98. 18 M/2 321.9 , First peak is base 1 ine drop corrected area. Second peak is tangent skimmed corrected area. Peak 4 R.T. first min. scan max scan 1ast peak sc an wi d t h raw area corr. area corr. y. 1 11.837 222 233 248 2 11.837 222 233 248 26 9985550 26 9985550 9930924 9824702 100.00 98.93 n r -f C11412 s, W/Z - 3 1 9 . 9 'pVf&rf First peak is b a s e l i n e d r o p c o r r e c t e d area. Second peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak ft R. T. f i r s t min. sc an max sc an 1ast peak sc an wi dt h rau area corr. area 1 11.837 2 11.837 219 ' 233 219 233 250 250 31 8 2 0 8 8 5 7 8 1 4 7 1 6 7 31 8 2 0 8 8 5 7 8 0 5 6 9 5 7 corr. y. 100.00 98.89 320/322 CALCULATION R - G l o b a l < 1) - .8204 tt/Z 2 5 7 . 0 First peak is b a s e l i n e d r o p c o r r e c t e d area. S e c o n d peak is t a n g e n t s k i m m e d c o r r e c t e d area. Peak .ft R.T. fi rst min. scan max scan 1ast peak sc an width rau area 1 11.837 224 233 246 2 11.837 224 233 246 22 5182106 .22 5 1 8 2 1 0 6 corr. area 5128184 5047290 corr. y. 100.00 98.42 (320 + 322 )/<332 +334) CALCULATION R - G 1o b a l C 3) = 58. 1000 <3 2 8 / )/ (332 + 334) CflLCULfiTION R - C l o b a H 3) = .3841 if"- r : ~ ____-- p!-T A. 1 J,.- i -i SUBJECT TO PROTECTIVE ORDER. OCI08 Cl1413 Jl T wo. 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