,^-s -^ ?y y""^. '< UNITED STATES ENVIRONMENTAL PROTECTION AGENCY 5 »/ iBKiii 1 ' HOUSTON BRANCH REGION VI eeoo HORNWOOD DRIVE HOUSTON TEXAS 77074 Ref. Case No. Site Name l^/^T^^ Date: /A^-77 Subject: CLP Data Review 7&^-^~- ^ From: Michael L. Daggett, Chief, Organic Lab Section, 6E-HL CD r^ To: Hank Thompson, 6E-SH "H T-l A review of the laboratory raw data for the reference site has been 0 completed by members of the Laboratory Section. Samples were: INORGANIC: ORGANIC: 3^o?/gLZ>3 The data was found: ( ) Acceptable (W Provisional; use of data requires caution. Problems are noted In Review Sumrnai ( ) Unacceptable; data should not be used. Problems are noted in Review Summary. Questions regarding the review can be addressed to me. Attachments cc: David Stockton, 6E-HL Duane Geuder, WH-548A
197
Embed
VOA BNA - United States Environmental Protection Agency · TMS ^ ^ ^^ TMS ANALYTICAL SERVICES, INC. TANDEM MASS SPECTROMETRY 6376 Morenc; Trail Indianapolis, Indiana 46268 317-291-5697
This document is posted to help you gain knowledge. Please leave a comment to let me know what you think about it! Share it to your friends and learn new things together.
Transcript
,^-s -^?y
y"" .'< UNITED STATES ENVIRONMENTAL PROTECTION AGENCY5
»/iBKiii1' HOUSTON BRANCH
REGION VI
eeoo HORNWOOD DRIVEHOUSTON TEXAS 77074
Ref. Case No.
Site Name l^/^T^^
Date: /A^-77
Subject: CLP Data Review7&^-^~- ^From: Michael L. Daggett, Chief, Organic Lab Section, 6E-HL CD
r^To: Hank Thompson, 6E-SH "H
T-lA review of the laboratory raw data for the reference site has been 0completed by members of the Laboratory Section. Samples were:
INORGANIC:
ORGANIC: 3^o?/gLZ>3
The data was found:
( ) Acceptable(W Provisional; use of data requires caution. Problems are noted In Review Sumrnai( ) Unacceptable; data should not be used. Problems are noted in Review Summary.Questions regarding the review can be addressed to me.Attachmentscc: David Stockton, 6E-HL
Duane Geuder, WH-548A
^ .
ORGANIC QA CHECKLIST
Site Vertac____________ Contract No. 68-01-7390
Case No. 8019/04________ Contractor TMS Analytical
Reviewed By Melvin L. Ritter , , soi1_________
Date 11/13/87 & 11/16/87 Acct. # 8TFAJN38 SF TFAU04
Batch 04 for Case 8019 is considered as provisional. The sampleswere analyzed for 2,3,7,8-TCDD and problems noted by the lab forthese samples were reported in the narrative. The provisional ratingapplies because of the need for the lab to resubmit Form B-1S, theresults form. The lab listed samples -09, -10 and -11 as being positivehits for dioxin, when in fact, the results should have been listedas MFC, because of failure of the results to identify 2,3,7,8-TCDDas per the contract requirements. The lab has been requested toresubmit Form B-1S.Evaluation:
1. Calibrations- All contract requirements for initial and continuingcalibrations were met, including performance column checks. Allresponse factors and their calculations and subsequent use wereas per the contract.
2. Method Blank- Acceptable. Detection limit of 0.3 ppb; surrogatesignal/noise ratio good and internal standard recovery good.
3 . Internal standards and surrogate recoveries- Provisional.Lab reportedsevere problems with a number of samples due to recoveries and reransamples -09, -10 and -11. Supplemental data was Included In thereport to verify the problems. Results should have been reportedas MFC values, not as positive hits for these three samples; labrequested to resubmit resultstorm,B-iy.
4. Spike/Duplicate Results- Unacceptable high recovery was reportedby the lab for the native spike 1 ppb amount; the lab reported 3 . 5ppb,or 350% recovery; reruns confirmed this problem. Per David Anderson,FIT
ORGANIC CLP/QA REVIEWCONTINUATION PAGE
CASE NO. 8019__________ SITE vertac
COMMENTS:
this sample DF0213-11 used for the native spike (suppose to be cleanand used to demonstrate the lab ability to process and recover a_____'known amount of added TCDD) was Station 26 on the custody list and ^actually was a sample from an area that previously had shown an !>•amount of TCDD greater than 1 ppb. This native spike QC data Is ,_(thus useless. T-*—————————————————————————————————————————————————————— 0Duplicate results done by the lab for sample DF0213-12 showedgood agreement in that both sets of data had TCDD less than 1 ppb.
5. Performance Sample- Acceptable. The lab did DF0212-18 as the performanceevaluation sample and the result found of 6 . 7 5 ppb agrees with theknown result to within the 95% acceptance window. Data here was good.
6 . Compound Identity- Provisional due to need for resubrnlttal and dueto very poor internal standards and surrogate recoveries for thesesamples. Positive results reported for DF0213-06 ( 0.7ppb) and forDF0213-08 ( 2 ppb).
7. Case Assessment- Provisional. In addition to the required resubfor Batch 04 as noted earlier, three samples are being requestedfor re-extraction and reanalysisfrom earlier submissions fromthe lab In this Case 8019; samples DF0212-09 and DF0212-12 fromBatch 02 and DF0213-01 from Batch 03 were all reported by the labto have an MFC of greater than 1 ppb. By terms of the contract,Section C 2. 1 . 5 , page C-2, the samples showing >1 ppb MFC shall_____be reanalyzed.
^ ^
CONTRACT LABORATORY PROGRAMRAS RE-ANALYSIS REQUEST/APPROVAL RECORD
SECTION A
fl. Case No. 8019 SAS No.______ ff2. DPO or RSCC David Scockton
S3. Details of Re-Analysis Request:
o Laboratory Name: TMS Analytical_______________________
CLP Sample Management OfficeViar & Go.209 Madison S t . , Suite 200Alexandria, VA 22314To whom it may concern:Enclosed is the complete Sample Da-fca Package for the analysis ofsamples for 2 , 3 , 7 , 8 - T C D D according to the procedures specifiedunder CLP contract »7390.These samples were received as Case ?8019, Batch #4 on September23. Results were sent by overnight courier on October 16 forarrival on the October 1 8 , four days late of the October 1 4 , 1987due date.On 09/23/87, Tony Neskey from SMO called Dan Delinger from TMS tonotify the lab that Case #8910 Batch 4 should be Case #8019 Batch4 . Adjustments were made by Kelly E. Mills, Sample Custodian, on09/23/87.Problems were experienced with three of these samples. Samples#213-09, 10, and 11 are invalid regarding proper ion. ratios andsignal to noise requirements. TMS Analytical was conscious ofthis discrepancy and re-ran the samples several times (seesupplement). In all cases, recovery proved to be extremely low-We believe an interfering substance within the samples causesthis problem- This conclusion is based upon: ( 1 ) no problems ofthis nature were encountered with the other samples, ( 2 ) allthese samples were of the same type (sludge), and ( 3 ) in allthree samples a 320/322 ion pair is present without theconfirmation ion.If you should have any questions regarding these data or thisreport, please contact Dan Delinger at (3 1 7 ) 2 9 1 - 5 6 9 7 .
Very truly yours,<y^\ ' J <LL,A_>^»L^vfc», •3< --•'YZ^l*^
Dennis L . Hearing Ph. D.President
CC'USEPA EMSL/LV QA Division944 E . Harmon Ave.Executive Center, Rm 228Las Vegas, NV 89109
USEPA REGION VI LABORATORYMonterey Park Plaza - Bidg. C6608 Hornwood DriveHouston, TX 77074Attn: Melvin Ritter
October 7 , 1987
CLP Sample Management OfficeViar & Co.209 Madison S t . , Suite 200Alexandria, VA 22314To whom it may concern: UT5Please replace the existing B-3 Forms found in the Sample Data ^Package and the Sample Data Summary Package with these corrected ^*B-3 Forms. Our files have been updated and corrected by C. Tn
Krauss, Document Control Officer. 'If you should have any questions please feel free to contact meat (317)291-5697.
Thank You,
Cynthia J . KraussDocument Control Officer
CC:USEPA EMSL/LV QA Division944 E . Harmon Ave.Executive Center, Rm 226Las Vegas, NV 89109
USEPA REGION VI LABORATORYMonterey Park Plaza - Bidg. C6608 Hornwood DriveHouston, TX 77074Attn: Melvin Ritter
DVELLOW'ir1"01^""1'n YELLOW III.M'-'; i . •-'• X -»i;? ^r^nNONC
THIS SHIPMENT IS WITHIN THELIMITATIONS PRESCRIBED FOB
POHT.OF D E S T I N A T I O N |{^\~Lrz^ 1?^^^PASSENGER 1AIRCRAFT }
NON-RADIOACTIVE^.- RADIO
(DELETE-NONAPPLICABLE
(DELETE-NONAPPLICABLE
IF ACCEPTABLE FOR PASSENGER AIRCRAFT, THIS SHIPMENT CONTAINS RADIOACTIVE MATERIAL INTENDED FOR USE IN, ORINCIDENT TO. BgSEABtiH.MEPICAL DIAGNOSIS OR TREATMENT.. r-l (.)) •-i.ii.i.iB ^,1; i(; ^nilliB^ •DnimBW .,, .,______
I HEREBY DECLARE THAT THE CONTENTS OF THIS CONSIGNMENT ARE FULLY AND ACCURATELY'DESiCftllBEO AB^VE BY PROPERSHIPPING NAME AND ARE'CLASSIFIED, PACKED, MARKED, .AND LABELED, AND ARE IN ALL RESPECTSilN'PROPEflrOONOITION FORTRANSPORT BY AIR ACCORDING TO THE APPLICABLE INTERNATIONAL AND NATIONAL GOVERNMENT REGULATIONS. • .
MID MASS CHROMATOGRAMS DATA: OCT021U ttl19/03/S7 e!38;09 CftLI; C:ftL832587 #3SAMPLE: CASE 3919; BHTCH4/213-04/9.96GCOHDS.; EClM SP2331/'100/ie0-2e0@25./2en-24@@4/8RANGE; 01704,1859 LABEL; H 5, 2.5 QUAH; A 1, 1.6 J S BASE; U 28; 3
SCANS 1794 TO 185S
S08TTOHID MASS CHROMATOGRAMS DATA: OCT9210 #1ie/63/87 El;38!@0 CALI; CftLe92587 S3SAMPLE; CASE 8013!BflTCH4/213-64/9.96GCOHDS.: 6@M SP233l/'100/106-2a@@25/2S0-240@4/'8RAHGE; 01704,1858 LABEL; N 5, 2.5 GUAH; A 1. 1.8 J 6 BASE: U 20. 3
SCANS 17@4 TO 1850
908TTOSCANS 1764 TO 1850MID MASS CHROMATOGRAMS DATA! OCTQ219 #1
CAL992587 #3is/es.-'s? 0:38 see CHLI;SAMPLE: CASE 8ei9:BATCH4/213-@4/'9.96GCOHOS.; Gt3M SP2331/l@e/10£i-20@e25''2e@-24i3e4.'8RANGE; G1794,1850 LABEL; H 5, 2.5 GUAH; A 1, 1-1 26, 31 . 9 J 6 BASE;1785
5871.53679.
17543440,31928.
5888.
332.999± 0,590
A...1755 i' \4371. '
38581. \
A . / \ 334-10
/ \ ' \/ \ /' \
T-' „ , , „ „ „ „ , „ ' • ' - - —•/ , < - - -.-172S 1749 1768 1780 180S 1829 184Q SCANIS;.^ is-^f"; l ^ - i O ''^S^ 19-3R 19:49 2M!@2 TIME
HID RIC DATA: riCTU2H ftl1S/03/87 1 i l l !@0 CftLI; CnLEi32587 tt3SAMPLE: CASE S019:BnTCH4/213-65/16.12GCOHDS.; 69M SP2331/l@e'100-20S@25/29£i-24H@4.'8RAHGE: G 1704,1859 LABEL; H O, 4.6 Ql-IAH; R £ i , 1 . 0 J 0 BASE: U 20,
1784
SCANS 1704 TO 1850
1711 1725 1733 1810__ 1S21 18.31 1846
1729i •"•.;) "•
174S1'-'. £':(':
1769iq. in
17891 i • •M
1899r=r:?R
182619:49
184028 562
808TTO
SCANS 1784 TO 1858MID MASS CHROMATOGRAMS DATA: 1X16211 #110/'93--'87 1 i l l : 86 CALI; CnLei925S7 #3SAMPLE: CASE 8@19;BATCH4/213-05/1£1.12GCOHDS.: 68M SP2331/-16t3/lH0-200@25--200-24u@4/3RANGE: G1704..1S50 LABEL: N 5, 2.5 6UnH; H 1; 1.8-1 0 BASE: LI 28, 3
122.
259.077± 8.589
24S.
328.038± 0.560
1848 SCAH28;92 TIME
"U32t
I1'. '.
•SSS3•T23^S^l
\'£S1•IZ7.SS^Is 'ez n sssya ^3 r u - i ••i H ;nynEi s's 's n naayi esarK^ia :33nya
8/t'a0t'3-003/s;s0e£-oai.'een.-'i££3ds nes = •sancio•:iST'9T.-'Se-£:ie/t-H31Hg!6I98 3Sy3 ••31dWSsft ^saeeeiyJ ii-ito u a s i i s i ^y/'so.'-ei
M I D NASS CHROMATOGRAnS OATH; IXT0213 Sl1Q/133-'87 2; 03 see CHLI; C,.U3325S7 if3SW1PLE: CASE 8019!BATCH4/'213-0?/9.91GCOHDS. i G0t'1 SP233l/ie0/ieO-208e25.'2@0-24ne4/'8RANGE: G17@4,185S LABEL; N 5, 2.5 OUHH! A 1, \.Q J 0 BASE; LI 29, 3
SCANS 1784 TO 1859
8T8TTOMID MASS CHROMATOGRAMS DATA; i:n;:Tu213 ftl SCANS 1704 TO 185@16/93/87 2s03s80 CALI; CALS32587 S3SAMPLE: CASE 8019:BATCH4/-213-@7/9.91GCONDS.: 69N SP2331.-''18e/l@@-2ea@25/209-240@4/SRANGE: G 1794,1356 LABEL; N 5, 2.5 QUAH; A 1. 1.6 J 0 BASE; U 20.. 3
17817476.71539. 7436.
332.699± 0.500
3S8S.
334.106± 8.509
SCANTIME
@3-'I-4 ••.•IQW
ZS8I £381 9T8T '-gQg-f-
I/3SZTs •B3 n sssya e r s't ••0 n ;|M-|Q u-t' ••e n siaayi esai't 'n^TO ;33nyas./t'est'z-£iee/e3ao0e-0ui/'0@'[/-T£e;ds HSS s 'saNoo
335 • 6/'S0-£ I S/t-HOiHg; G 108 3Sy:i •• 3"1dWS£tt ^ys-GR'il^ iIT'O WW-'i. ;8/£8/uT
6SST 01 t-O^I SH':'::i3 Vs 3^WW ^^W 3ia QII-1
011819
•!:;.£.[8S.1Is 'BE n !3sya u r eri • t 1.1 :n"l"li3 s's •s n ;"i3ay'i eesi't'o^ia ••^m
S88TTOMID RIC DATA; OCT6217 #116/03/87 4:10:00 CALI; CALE82587 #3SAMPLE: CASE 8019!BATCH4/213-S9/10.28GCONDS.! 6011 SP2331/100/'100-200e25/2ee-240(M/-8RANGE; G1794.1850 LABEL; H 0, 4.0 QUAN: A 8, 1.0 J
SCAMS 1704 TO 1859
0 BASE: U 20, 3
o o -nom u"i r~ M 3•• • rn N. n'"• " co 1/1ID -^ in—»(no
--3§°J(-n(«iS->®-0 (>-1 1-0 CT 1^s§ I
" M OiCT I
^"'5"'^^
0 03 0 0CT I 0 I> 3>CM 1~ —I3> 4». — 3>3: G> — —
-o. oo^ P30 Si
fr-k *^ ts^
" !»
^ s"OT3>in
SgSTTOSCANS 1704 TO 1850MID MASS CHROMATOGRAMS DATA: OCT0217 #1
10/83/87 4:10:60 CALI; CftL892587 #3SAMPLE: CASE 8019:8^1^4/213-09/19.282CONDS.; 60M SP2331/l00/10a-200e25/2S0-240e4/8RANGE: G1704/1850 LABEL; N 5. 2.5 QUAM; A 1, 1.0 J
1748
988TTOMID MASS CHROMATOGRAMS DATA; OCT0217 ttl SCANS 1704 TO 1850WQ3/87 4;10;00 CALI; CAL092587 #3SAMPLE; CASE Se^BATW-^-aS/ie.^GCONDS.: GBM SP2331/100/100-200(>25/200-240@4/8RANGE; G17B4/1850 LABEL; N 5, 2.5 QUAN: A I / 1.0 J 8 BASE: U 20; 3
MID RIC OATAs 0016508 #110/05.'87 7850:08 CALIi CAL692587 #3SAMPLE; CASE 8019:BATCH4/213-10/10.24GCONOS.: 6011 SP2331/100/'100-200e25/200-240@4/8RANGE: G17@4<1850 LABEL; H 0, 4.0 QUAN; A Q, 1.0 J
SCANS 1704 TO 1850
U 20, 3
1763
_1712 i723 1733 1741 1743
17201•^•.l•"i
174Q1'"' • '"c
1769) n. 1 n
17801 q .'-••?
180019;W
1S2019; 49
184320:02
8S8TTO
MID MASS CHROMATOGRAMS DATA: OCT0508 #1CAL632587 #3
SCANS 1704 TO 1850IQ.'Q5/87 7;50!00 CALI:SAMPLE; CASE 8019;BATCH4/'213-10/'10.24GCONDS.; CBM SP233l/l08/100-20Q@25/200-240@4/'8RANGE; G1794,1S50 LABEL; N 5. 2.5 QIJAN: ft
175987.414. ,
1. 1.0 J 0 BASE; U 20, 3
CO<M00
088TTOMID MASS CHROMATOGRftMS DATA: OCT0588 #1 SCANS 1704 TO 185010/05/87 7!50!@0 CALIs CAL692587 #3SAMPLE; CASE 8ei9;BATCH4/'213-10/10.24GCONDS. s 6011 SP2331/100/100-200@25/'200-24ee4/8RANGE; G1704,1859 LABEL; H 5, 2.5 QUAN; A 1 , 1.0 J 0 BASE; U 20, 31789
5856.54040.
1762154.
.-U12-
5856
332.09A 9.59
7000
334,101± 0.501
17G1218.1461, / v.—-—-^ // \_
1729 1740 1769 1780 1800 1820 1840 SCANIP-4-'! i".^- i q - i n iq.""' I'a.'sR 19;49 20;02 .TIME
61'=61ezsi
at'bi6081
Ul ^tu9;l
c,y6leszi
y sNyna e't- ••e H naayi as8T't'ezi3 saawa8./t'86t'2-0BZ/'fieBeez-e0i/00i/'iessds nag i'sano3
M I D RIC Wf(\i i:ii::'!u5£i';i »119/05/37 6! 19; 0i3 Ci',1-^ ?1.632587 -S3SAMPLE: CfiSE 8019!BATCH4/212-18/9.99GCOHDS.; 60M SP2331/ia0/ieu-2eie@25/2UM-240a4.'3RANGE: 01704,1850 LABEL: H 0, 4.0 num); 9 i3, 1.0 J i3 BASE; U 2*3, 3
1 *' b I
SCA113 17S4 TO 1S50
17S9
••: /1743 .-• ^-.1888 1828 1:340
1749._.——^_--... .-..,-..-
1769 1780; .3, •-•':•
1809^•."'•K
1820 134019; 49 20; 02
SCAHS 1784 TO 1858MID MASS CHROMATOGRAtIS DnTu; OC.'fiKi35 11118/85/87 6s19;89 CALI; CfiLOS^K? ii3SAMPLE i CASE 8819:BATCH4/212-18/3.33GCOHDS.: GSM SP2331/le9/100-2eee25/•2e0-24G@4.'SRANGE; G 1784..1853 LABEL; H 5, 2,5 OLihH; n 1. 1.0 J 0 BASE; U 20. 3
1 ;-'b31431,
1568.
259,077± 9.5S0
1789212.1764./""'-"•-•,
.. .^ ''--"v.. ^ ^ ^ ^ . ^ ^ , ^ ^
338.
328.09S± 0.599
^^-^H}^•r" 1 i ' i ' i ' '-SO 1809 1828 1840 SCANi ; 1 ' " ' ' • I'-i.-'- !9;49 20;!32 TIMF
smioM I D MASS CHROIWTOGRAMS DOTH: OCT05u5 wl SCHHS 1764 TO 1858le/SS/S? 6!l3;@@ CnLI; Cr,L632587 #3SHHF'LE! CASE 8919: BATCH4/212-18/9.99GCOHDS.! GOM SP2331/109/lS0-20ue25/2He-24G6;-l.'SRHHGE; G 1704..1850 LftBEL: H 5, 2.5 QU9H; H 1, 1.0 J B BftSE; 1-1 20.. 3
1?.S3c- ^-17
OS8TTO
MID MASS CHROHATOGRANS DnTA: OCT(35e5 #1 SCANS 1704 TO 1S5810/05/87 6; 19:08 CnLI; C..L692587 #3SAMPLE; CASE S@19;BATCH4/-212-18/9.99GCOHDS. i 6HM £P2S31/10i3./10a-200@25/20a-24uiM/'SRANGE: G.1704..1853 LABEL; N 5.. 2.5 QUHN; n 1, 1.6 J @ BASE; LI 28, 3
A / V.'z '•--.. ..•'' <1728 1749 l7£i:t 1788 1809 1820 1848 SCANi.-..^- f . - . . c ^ - f . . , i i , .q.-i ra-T- t9;43 2u;02 T T M F
T98TTOMID RIC DATA; OCT1583 ftl SCANS 1784 TO 185019/15/87 14;37;00 CALI; CflL@92587 1t3SAMPLE; CASE 8819;BHTCH4/213-89/9.93GCOHDS.: 68M SP2331/l@0-200@25/20e-240@4/HOLD 9RANGE: G17@4,1S59 LABEL; N 9, 4.6 Q U A N T A 0, 1.9 J 0 BASE; U 20, 3
?Q8TTOM I D MASS CHROMATOGRAMS DATA; OCT1563 #1 SCANS 1704 TO 1850le/lS-'S? 14; 37; 60 CALI; CAL092587 tt3SAMPLE; CASE 8019:BATCH4/213-09/9.93GCONDS.: 66(1 SP2331/100-200e25/200-249@4/HOLD 9RflNGE: G17@4,1850 LABEL; N 5, 2.5 QUAH; A 1; 1.6 J 0 BASE; U 20, 3
-:JJA,ilq|Ayi//l^.-:=-'^1 l'f|;^|''lf^^|1720 174@ 1760 1789 1800 1828 1840 SCANffi .d-; )H.«=:C I ' -r in iq;^? l'?-'7^ 19;49 29:92 TIME
S98TTOM I D MASS CHROMATOGRANS DATA; OCT1593 ftl SCANS 1704 TO 185818/15/87 14!37;89 CALI; CAL092537 #3SAMPLE; CASE 8019;BATCH4/213-09/'9.93GCOHDS.; 60H SP2331/l@a-200@25/200-24e@4/HCiLD 9RANGE; G17@4,1850 LABEL; H 5; 2.5 QUAN; A 1, 1.6 J 8 BASE; U 29> 3
1738224. -. . > .
8S.3n r-21;4- ^ \P 242.
/ A \ . < - / \ \ 320 _ | v! \/ 320.696
I \ ' ± 9.508
f A /A^J^i/\/-—-^^AA /AA/^W^/yJi^vA/V/^^^ ^•—^———i——'——i———-7—1—r^——'———i———'——\———'———T———'———i •"'
1738 -/--"249.^ i
100.0-1 r T' '71 274.
c U__M-^322 ^ 322.896
\. " ± 0.500
/ \ i \
yVM .!-/——^nW^V^^ . ^ ^,1720 1740 1760 1780 1800 1S20 1840 SCAN1?.. ,-(•-, r--c,- f q . l F l iq.'i'? 19-3?; 19s49 20S02 TIME
^SSTTO
MID MASS CHROMATOGRAMS DATA; OCT1503 #1 SCANS 1794 TO 1850IQ/IS/S? 14;37;98 CALI; CAL092587 tt3SAMPLE; CASE 8019:BATCH4/213-09/9.93GCOHDS.; 60M SP2331/'100-2e0e25/2@0-246e4/HOLD 9RANGE: G1704,1850 LABEL; H 5, 2.5 QUAH: A 1. 1.0 J 0 BASE: LI 20, 3
17659285.
5.0-, s™ 9232.
32 _ I' ', 332.699l ' ± 0.509
173G / \312. / \2944. / \
176410864.
3.0-, wm- 10864.
/ \34 _ J \ 334.108
j \ ± S-500
, 1737 ?'385. ,' \
__3315. / \
1720 1740 17E.0 1789 18S0 1820 1840 SCAN1F;-4? IS-W l ^ - I O I?.?'? l9;3K i9;49 20!02 TI11E
398TTO
NID RIC DATA; OCT1584 #1CHL032587 S310/15/87 15;07;@8 CALI;SAMPLE: CASE 8@19;BATCH4/213-1@/[email protected]
COHDS.; 69M SP2331/ie0-2eee25/200-240@4/HOLD 9RANGE: G1704.1850 LABEL: N 6 , 4.@ QUAN; A 117b3
1735
SCANS 1784 TO 1S5@
1.9 J B BASE; U 20. 3
1710 1717 1805 1816 1792 1828 1840
17281 0 - ^
1743 1769l'"rlf>
17801 <?•'?•'<
1808^9•':'R
182019:49
184029:02
998TTOMID MASS CHRQMATOGRAMS DATA; OCT1584 #1
C.ftL992587 #3SCANS 1704 TO 1859
10/'15.'87 15;87;90 CAL1;SAMPLE; CASE 8919!BATCH4/'213-10/'10.17GCOHDS.: 68M SP2331•/^00-200@25/•2e0-240@4/HOLD 9RANGE: G1704,1850 LABEL: N 5, 2.5 QIJAH: ft 1..
17361.0 J 0 BASE; U 20; 3
77.939. 91.
259.877± 3.53B
70.
328.098± 0.500
SCANTIME
'1> g 3> S >—
?? 0 5 *-*m 1/11^ cn 3. .. CO LI
S^o-^®§S5iS^^'^sg—> -13 03 -•J 303 M (S " X>i-Jl (A.I "• i3 —IGl C«) ID •3> 0
>I»»^0;unmm " TO\ co o)03<n 3> o •• i» >— CT —t) IXi '3 0
£5^ro is om i a-r-ME" <s> \131 r\)
r-n '-. 0
:^g^§^i-n t-i -'J
-B. -•J1=1 ID 0 0o ra ]> i;-in -&. i— —<
33- ' l-l X1
2: n: "• ••— oI— 1-1 0» 0 E 1-1LD isi-n ui^
998TTOHID MASS CHROMATOGRAMS DATA: OCT1685 #110/16/87 IS;36;08 CALI; CAL9925S7 #3SAMPLE: CASE 8019;BATCH4/213-09/'7.77GCOHDS.: 60M SP2331/'100-2e0(»25/200-240@4/'HOLO 9RANGE: G1704..1850 LABEL! N 5, 2.5 6UAN: A 1, l.S J
1775
SCANS 1784 TO 1858
0 BASE: U 20, 3
1758158.1537.
7928.
332.899± 0,500
1747225.2143.
9792.
334.100± 0.500
1729l'-;.^
1746l'''.1^"
1769in . l l l
1780IQ.'.'i
180019;3K
182019; 49
164020;02
SCANTIME
MID RIC DATA; OCT160G ttl10-'16/87 17;08;S0 CALIi CAL032537 #3SAMPLE; CASE 8019!BATCH4/213-1@/'9.59GCONDS.! 60M SP2331''10e-200@25/20S-24@e4/HOLD 9RANGE; G17@4,1859 LABEL; N 0, 4.6 QUAH; A 0, 1.0 J 0 BASE: U 20.
SCANS 1784 TO 1859
A
1719 1747
1729IS: 4:''
1746i •"'."-'-
1769('"'• 1F)
1780iq.'>-!
1800iq-^R
182919; 49
184920; 92
S98TTOMID MASS CHROMATOGRAMS DATA: OCT1696 ftlW[^S7 17; 88; 00 CHLI; CAL692587 »3SAMPLE; CASE 8ei9;BATCH4/213-10/9.59GCONDS.; 60M SP2331/'109-290('25/203-240@4/HOLD 9RANGE; G1794,185@ LABEL; N 5; 2.5 QUAH; A 1, 1.0 J
SCANS 1704 TO 1850
0 BASE; U 20, 3
88.
259.077± 9.508
74.
328.098± 0.598
SCANTIME
698TTOSCANS 1704 TO 1850MID MASS CHROMATOGRAMS DATA; OCT1606 #1
18/16/S7 17;08;08 CftLl! CftL@92587 #3SAMPLE! CASE 8@19!BATCH4/213-ie/9.59GCOHDS.! 6aM SP2331/'100-2ae@25/200-24ee4/HOLD 9RANGE: 01784,1859 LABEL; H 5, 2.5 QIJAN: A 1, 1.0 J 0 BASE; U 20; 3
1747118.979. 133.
320.096± 3.586
139,
322.896± 0.500
SCANTIME
m m r- 013":..?.» 5So -slint-^ <n o-SJ Q 3»— 0IS131/1-%1 I^ m •• ^-%0.§§ayss,^Q &JLDOO
»—• •« 0
r^g 5
®K>01®§
WiZ
t~M •*»Q M
^SSUI I
(Jl \ '^ M QCS '».
f-l 'S LD01 S:'£5
GI CT 0 0§2 PSr' '"• " 2?^ o
U8TTOSCANS 1764 TO 1858N10 R I C
10/Q1/S7 13!S3;e@SflNPLE; CALIBRATION SOU I 1COHDS.; e.on £p233i/-ioo/'ieo-2oei.];.:5^'.:!\. :.;^., • ; ;RAHRE; G1704,1850 LnOEL: 11 0 ^ 4 . S I ' i i . i i ; , ; 6. 1.0 J 0 BASE: U 20, 3
M I D WiSS CHROMflTOGRHNS DAm: UCT6291 til SCHHS 1704 TO 1850li3-'i32/'87 14i57!£'@ Cr,LIi CiM-C325S7 S3SWI.E; CftLIBRATIOH SOLH 1COHDS.i 60n SP233l/lOel/l0£l-2^1ue25/20^-2-lHe.!.^!RnHGE; G 1704,1850 LABEL; H 5, 2.5 i3l..lftil! rt 1,. \.V J 0 EUSE; U 28.. 3
e 'ee n !3sya a r e'l 'i " snnri9 s's •s N •• "13991 £ifi8t't'e^rs saoHya8./t'S!:it'S-G8?..-'SS39u3-00t/U0I/I££'3dS N89 •• "SOH03
i n"ios noiiyagnyo s3idnnsss zseseeiyj snyo easzssN ^s/zu/ei
13SST 01 t-921 SNH::IS Itt I93i?J.::iO ii;ijm.1 SH9a3019UOaH3 SSW QIH
011877
^ 8^8TTO• W
M I D MASS'C1-IROMATUGRHN-'; LmTn: nr:T0201 ftl SCAISS 1764 TO 185010/@2---37 14;57;90 CftLI; ?1.892587 %3SAMPLE: CRLIBRATIOH SOLH 1COUDS.: F.m SP2331/-100/ie8-2nu@25/20Ci-2')0e4.'aRAHGE; G17134..1S50 LABEL: H 5. 2.5 QUfti); H 1, 1.0 J 6 BASE: U 28, 3
17362571.
A'11 \ ^
/ \ )373.\ 11^J• 332. S991 . ' \ ± 9.5^38
\ 1 \.^ \ 1 \
i ••-... J \, ^. . - - ^1736321S.2^9- 3244.
\\S.
,( 1 A 334.10S/ \ ± 5-566
' \ 1 \• ! \ 1 \/ '\ / '.---1720 1740 1769 178S 18S9 132Q 1848 SCAN10..I--. i . - , . r ' . - •I1-:,'!-! ; - i , ^ " i q - ^ ^ l'5-^^ 20!02 TIME
smioHID R I C ! . „ ( ; , ; ... 1 . 1 1 ' . l i i l SCfiHS 1764 TO 1S5019/81/87 13!i33!en - . , . 1 . 1 ; U-.j&;::;;7 i;3SAMPLE; CALIBRATION SOLiI 1COHUS.: 6(iH SP2331/lHu/ien-2R&6S ;'L!. .:;"•.-! .;RHHGE; G17U4,1S50 LRBEL: H 0^4.9 L'!!.!!; , , 6. 1.0 J 6 BASE; U 20. 3
988TTOH I D HflSS CHROt'lHTOffihIiL; i : , i T . ; . " . . i . - i - . i i H I SCiiNS 1704 TO 1858iM/m/SF ISii- '^inil 1 , 1 ! ; : . . : , , [ ;-.. -,:;;7 ;?3SAMPLE: CHLIBRHTIOH SOLU 1CTIDS.: CTt'l ?P2331/ln•;i/100-2e!'^^;•v^-.l'', - ! - • • • I •::F'HllCr: 01704,1858 L.HC.EL: H 5, ^^J i . i ! . . . ! . , . 1. I." J 8 BASE: U 2S, 3
:;:!,. .:•- • ; ' ^ 1 " 378.! ''i 'i[ 1.
\
:-••:< I I 259.07;i •, ± s.5Bei1 i
/ r 1 ' 1
/',/-' w'^H---- • ' .''•V'-^A^^^AS^^^^^^-':;- - - l r ; -.--, •••---;--•--,- • i , • • • • --•r———••———-i———;———i———r'———]——^
175.-:I1 L.' ^. ' J
i i . ' ; . n - 7'•;,'';;- 943.i'
[-'I I
j ^3^ ; i 328.898
/ !, ± 0.509
:.. ^ Z .., r .':;,r: .zl... -.-.:-. .:.: • • . "• 1 • / f ^^-A^^-^A^^^/V^--^172n 17..!Q i . . . ' . . 1783 1890 1S2S 1840 SCAM,.-.•, i - . . - - • , ,——:. 1^.01; i9;49 29;e2 TIME
0"1 <3:io IT.ICD 0C'40 -H
cnc:iCi:l U-J
c-'! isC-.1(•:«
•a-(0 COr'-
i-''i c:i=: C-4
.!'<-
J<'/
< Q C:'
<
<
/
\
i IJ-1< 13 '?•a |:M •-^ CO C-1
!{
<1 .-S;.S—i c'-i
-
'l3 f:
— CO 0
0
00 § =;-00 o o i—i i"'".' o. , !— e:i i— i"'"; inf—^ -z •" a: r-j 1:0^ '"'"' cc. a. —io 's (Xi i-i-i -.i_..i—i -i-
: c'"i —] : •n._, ti o r--(_• i-:i -<1-1:1 r.- i_;
:£-<_] l-l-'l !d u-. Q 1-3
TlCJ.•"i—.u
S88TTOHID NHSS C.HRi:iNHTOffiHNS n ; i i i . ; i . . i . . i ' : i l i . i l Sl SCHUS 1794 TO 1850IS/Ol-'S? 1^;(13!@9 C-LIs f.,!.^.::^'^ i;3SANPLE; CALIBRATIOH Sul-H 1CHHDS.; tUH SF•2331/'loEl• /lC.e-2a£l@25.•20^•^•!l :.;! .:;RHHGE; G17H4-1S50 Lnia.; N 5;,J.5 ^li^! ' i 1. 1.0 •J 6 BftSE; U 28, 3
.1 .::;•;] a.
S88TTOSCANS 1794 TO 1850HID RIC DATA; QCT0215 #1
CALI; CAL092587 tt319/03/87 3;87;00SAtlPLE: CALIBRrtTION SOLH 1COHDS.: eeM SP233l/190/'100-2@0@25/'200-240@4/8RAHGE! G1704-1850 LABEL; H Q, 4.6 WM: A 6. 1,8 J 9 BASE; U 28,
1755
SCAHS 1794 TO 1850MID MASS CHROMATOGRAMS DATA; Ui;re215 ftlCftLIs CAL032587 #318--'e3/87 3;S7!06
SAMPLE: CALIBRATION SOLN 1COHDS.; 60M SP2331/10@/100-200625/200-240@4/8RANGE; G1704..1S50 LABEL: H 5, 2.5 G'I-IAH! A 1, 1.0 J 0 BASE; LI 20, 3
HID MASS CHROmTOGRAHS94.'23--S7 13; 35; 09SAMPLE! CALIBRATION SOLN IIICOHDS.: lUL/SP2331/-ie@-2e0e25/2Q0-240@4/HOLD10RANGE; G1794.1900 LABEL; H 5. 2.5 QLlHH: i1 1, 1.0 .-I
175310632.71616.
SCANS 1704 TO 1900
9 BASE; 1-1 20, 3
19032.
259.877± 0,560
•i"' —f " " " " ! •
6648.
328,938± 0.500
1358•••Ffi'r?
1900 SCAN20:35 TINE
386TTOMID MASS CHROMATOGRAMS DrtTft; APR23H til SCAHS 1794 TO 199S34-/23/S7 13;35!@S CHLI; CftLS4^337 ftSSAMPLE: CALIBRATION SOLH I I ICOHDS.; lUL/-SP2331/100-2e0e25/-2e@-240@4/HOLD10RANGE; G1704,1909 LABEL: N 5; 2.5 eUAH! A 1, 1.6 J 0 BASE: l-l 28, 3
ID MASS CHROMATOGRAMS4.-23/87 9! 43:90AMPLE; CALIBRATION SOLN IUDUOS.; lUL-/SP2331/100-200e25/209-24Be4/•HOLD10ftHGE: G1704,1900 LABEL; H 5, 2,5 QUAN; A 1,
1766
DATA; APR21S3 #1CALl! CAL0423S7 »5
41920.305594.
SCANS 1704 TO 1900
1.6 J 0 BASE: U 20, 3
41929.
259.977± 0,508
2564.
328.09S± 0,508
1750i".^
isser-r-Ti
1859pa-fl?
1900 SCAN29;35 TIME
3mTOMID MASS CHROTOTOGRAMS DATft: APR2163 #1 SCANS 1764 TO 190804/23/87 9; 43! 08 CALI; CAL642387 #5SAMPLE! CALIBRATION SOLN WCOHDS.; lUL/SP2331/10a-2a9a25/208-24ae4/HOLD10RftNGE; G1704/1908 LABEL; H 5, 2.5 QLIflH; A 1.. 1.9 J 9 BASE; 1.1 20. 3
11 bb214016.
77.7-1 156^040. ^g^
329 _ / I. 320,0961 | ± 0.508
1766275456.
inn n 2038476. i-c.iccl@fi, 0-i A 2i'545b.
1\322 j I 322.036j I - ± 0.500
1750 1SSO 1858 1960 SCANIR;''? l^W 2i3;02 20:35 TIME
irnroMID MASS CHROMATOGRAMS DATA: APR2103 ttl , SCANS 1794 TO 193994/23/87 3;43;80 CALI; CAL8423S7 #5SAMPLES CALIBRATION SOLN IUCOHDS.: 1UL/SP2331/100-200@25/'200-240@4/-HOL010RAHGEi £1704,1909 LABEL; N 5, 2.5 QUAHs A 1, 1.8 ..I 9 BASE; U 20, 3
17639856.
78.8-j 75?36- 9856.
1 1791( \ 5681." | | 41338.332 _ / A 332.099
/ i n i 0.538
j [ ]\________I-—,-——-,————1_-—r ^ '•—i————r———i • I f ' • I————I————r-^—T°——"'I1 ' "• I———^ r "I I———1
1750 1898 1850 1900 SCANi?-^ 19!'<n Sd;!^ 20; 35 TIME
MID MASS CHROMATOGRAMS DATA: APR2314 ttl04/23/S7 l5!02!00 CALI; CAL0423S7 1(5SAMPLES COLUMN PERFORMANCE MIXCONDS. s HJL/SP2331^100-2001»25/200-240@4/HOLD10RANGE; G1704,1900 LABEL; N 5i 2.5 QUAN; A 1..
17849526.71994.
1.0 J 0 BASE; U 20, 3
SCANS 1704 TO 1900
9536.
332.099t 0.500
11760.
334.100± 0.500
175018;57
188019; 38
185020:02
1900 SCAN20:35 TIME
^ ° S l=i S S^S ®m 1.1-11—1—3•• • m \ i-— .. 03 i.i-io -'J 1-1-1
•pi s•- yi :s; i: c:'a3^^iCT i.i.i m ca o" ?3 £-:'. -n xi
r— »- o re-x> d ?3
!IICT ms iI-:' 3
cn 'S' :
'-!} r'.'13''=>
':'^' CCi —'-1-1, ; Ki -•J'"" r^":' "••it—S -••J -i-"si
0 "T-'- 7.r" —ii— r-
o oE'"".'
I.,;. Qi-n i--1
^4.
^t0 M
MCTCT1-0010
i:C'cno
SCANS 1?@4 TO 1859i'HD MASS CHROMATCGRAMS C . i i i i . , ; OC.ruHE Sl18/91/87 13; 33; 89 Crii-Ii CnL632587 #3SAMPLE; COLUMN PERFORMANCE MIXCONDS.: £UM SP2331/ie0,/l£iCi-2Sai?25/2u£i-2-!ua4./SRANGE! G1704;185@ LABEL: N 5, 2.5 QUAHs A 1..
1S40 SCAN29! 92 .TIME
1764.
320.096± 6.509
2176.
322.036± 3.5@0
M I D RIC Ily-'ei/s? 2e! is; 00 i^W'LE: COLUI'IN PERFORHtilICE N1:";COIIDS.; 6MH SP2331.' 100/100--2(3(t@25'^i1-•;: !RUhRE; G1704,1858 LhBEL: tl 0; - i .O i l l , , ; ! ; ,
SCHHS 1794 TO 1859. , l n ; l u . l ! . , i l L ^ ,11nl.l; i. .. ':;L;7 ft3
1.6 -I 9 BASE; 1-1 29, 3ires
TCDD17S2
1719 ,-.1804 . IS 17 1S38
18S9< a - ic
18281^;4q
184S28; 52
M I D MASS CHROMA ruC,RnHS H , ! l i , . ^ I ' J l i n til10,-oi.'S7 29;lS!ee r-;,l.u r,,i i.:yS«7 a3SHNPLE; COLLIMH PERFORMANCE HI:";C i i l IDS.! bOM SP2:331/lMel/l&^-2@9lil2?••;•l-"-l- : l i . • I ;';PhHGE: dl7ei4,lS59 LnBELi H 5, 2.':. r i i , , i i ; , , 1, 1.0 J 0 BASE: 1-1 29.. 3
1733885.
SCANS 1784 TO 185@
dUIi 60S0Z et^Gl :3t;-ot .^•t^ • - ' i - ' . - . t - . , . -1tTOS Bt'81 03ST 6981 98.'1 n^ ' I Eit'^l
\
aes's TiOIat'SS:
8S'@ T60'Z££
•£8S;^: - .-•33be ?ez^ic 'ei.7 n ••3wa e r e ' T • i n inyfiLi e's •s n naayi essi^a^io ;33nya
SAMPLE! COLUMN PERFORMANCE MXCOHDS.; 60M SP2331/10S/ieO-28S@25/2e9-24£i@4/8RHHGE: G17@4,185@ LABEL! H 9, 4.6 QUAH; ft Q, 1.6 J @ BASE; U 29,
1785
1763 1717 1738
18394.
1824 1836 1844
172131' '.,1^
1749 i7eei q - m
1788lq.'>"
1S28 1S40 SCftH19;49 28:92 TIME
SCANS 1704 TO 1850HID MASS CHROMATOGRAMS DATA: OCT6218 #1CALl! CAL992587 fr31@/@3-'-87 4! 39; 98
SftflPLE: COLUMN PERFORMANCE MIi<COHDS.: 60M SP2331/ie0/iee-2@0C!25/'200-24>3e4/8RANGE; G1704..1850 LABEL; H 5, 2.5 QIJAH: A 1, 1.0 J 0 BASE: U 26,
178S1185.11125.
3^6TTO jMID MASS CHROMATOGRAMS DATA: OCT0218 #1 SCANS 1764 TO 1858IS/BS/e? 4839;@0 CftLIs CAL692587 #3SAMPLE; COLUMN PERFORMANCE MIXCONDS.: 6@M SP2331/'100/'100-2a0@25/200-240@4./8RANGE: 01784,1850 LABEL; N 5, 2.5 6UAH: A 1, l .@ J 0 BASE: U 29, 3
17845993,
84.2-1 53b3f. ggg^
1757 I I332 . 2760- / \ 332.099
2.b^3•J• /' \ i 0,500
17857898.
108.0-1 68256' 7136.
1755 / \3712. / \
334 34849- 334.100/V, ' / ' ± 0-580
^ ! / V I \1728 1749 17eS 1760 1808 1829 1849 SCANlfi-4- j I R - R f i 19;lFi 19;23 19S36 19;49 20!02 TIME
396TTOl - l in R I C I lu ' ln : 1 . ' : ! ' . i:....-'2 i , l SCHtIS 1704 TO 1850
SntlPLE!'COLUMN'FbRFiiRHiinCE t'll;;COtlUS.! £0n SP2331. l£i0.'10Q-200i:::25/^Ou -W.^ •^RnHr;E: r,17a'L185U LuBEL; I I 0, 4.0 i i ; ' i , ! i : i , n , 1 . U . J a^_BH3E: U 20, 3
?96TTOM I D t-lnSS CHROHATOGMlNS I'nTu; i . i . l ' i r i l ? ' ,.1 SCAIIS 1704 TO 1S5S10.-e5.S7 15!ll!&9 Cnl.l; i..,,l CJ^S7 K.SAMPLE; COLLW PERFORMANCE MI;::CUNDS.; bOM bP2331/iau/10£i-2UUii'25''2ULi-2-tWl ..{RftHGE: G1704,1S5@ LftBEL; H 5, 2.5 rimil; ( ; 1, 1 . U . J 0 BASE: U 2@.. 3
^' ! \ / \1726 17-ifl l i ' ^ U l?L;t) 18U9 1828 1849 SC9H) • • i - r • • " - r . . . i . • - • • • • )1;';F; 19549 26:82 TIME
(•IID MASS CHROMHTOGRnNS rii,Tn: i:n::fn;Jl7 f t l SCfiHS l7@4 TO 185010/05--37 I S s l l s e a Cni-1; i;,,L."32537 S3SAMPLE; COLI..IHH PERFORmHCE MI;;CONDS.; fW SP2331/109-100-200@25-'2un-24a-:.1/3RfttlGE: G 17S4,l;:;5u LABEL; H 5. 2.5 C!UH|I: n 1, 1.0 J 9 E;RSE; LI 20, 3
173£4272.46563.
;\4272,
1-2 \ly7 ' ' - / \ 332.039-a^u. ; ' ± 0,580
A \./ \ / v17965099.56002. „,.„-1 n
-/1 / "\^. ' l 334,180',;A ' | \ ± 0-598
172Q 17'IEi l^ r ; ' . ) 17HU 1800 1820 1S40 SCANi.;.. 1-. i . , ^ - ) , ; , , i . , .^ i.i.-.i-; )q;49 20S02 TIME
?96TTOMil.) I? 1Cie./05-/B7 15 i l l ; 69SWLE; COLI..II-IN PERFORIlnUCE HIrtCOHDS.: 60M SP2331/lU8.--lU(j-20H@25/2M-.;'l(J^l..iRHHGE: 01704,1556 LhBEL; N 0, 4 .0 Q l i . i i l i i ; 0, l .n J Q BASE; U 20^ 3