ML20094H400

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Pyrolysis Gas Chromatography Analysis of 3 Thermo-Lag Fire Barrier Samples
ML20094H400
Person / Time
Site: Waterford Entergy icon.png
Issue date: 05/30/1995
From:
NUCON, INC.
To:
Shared Package
ML20094H388 List:
References
NUCON-06LP829-0, NUCON-06LP829-01, NUCON-6LP829, NUCON-6LP829-1, NUDOCS 9511140157
Download: ML20094H400 (52)
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Text

.

3 NUCON International, Inc.

TELEPHONE: (614) 846-5710 OUTSIDE OHIO: 1-800-992 5192 P O. BOX 29151 7000 HUNTLEY ROAD TELEX: 6974415 COLUMBUS OHIO 43229 U.S.A.

FAX: (614) 4310858 I

1 l

i PYROLYSIS GAS CHROMATOGRAPHY i

ANALYSIS OF 3 THERMO-LAG 4

FIRE BARRIER SAMPLES j

Performed For:

j Entergy Operations,Inc.

Waterford 3 P.O. Box B i

Killona, LA 70066 1

l P.O. No. NWC0035 30 May 1995 i

Dicirihntion Waterford:

Tim Matey (1)

NEI:

Biff Bradley (1)

NUCON:

06LP829 Master File (1)

Lab (1)

NUCON 06LP829/01 9511140157 951109 PDR ADOCK 05000382 P

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I.

ABSTRACT InWon of the pyrograms of 3 Thermo-Lag fire barrier samples indicated that they are all similar in chemical composition. However, sample 0395-37B, a 3-hour rated panel sample had disproportionate amounts of characteristic compounds.

]

II.

OBJECTIVE Pyrolysis Gas Chromatography (PGC) with Mass Selective Detection (MSD) was used to qualitatively compare three Thermo-Lag fire barrier samples.

III.

DESCRIPTION OF METHOD The samples were compared by pyrolysis gas chromatography using ASTM D3452 as a l

general guide. A Hewlett-Packard model 5890 series II gas chromatograph equipped with a Hewlett Packard model 5972 mass selective detector was used to generate chromatograms of the pyrolysis products. Pyrolysis of the Thermo-Lag samples were performed with a CDS pyroprobe mounted in an indapaadantly heated interface attached to the injection port of the GC. Analysis involved weighing 1-3 mgs. of sample in a quartz tube and placement of the tube in the platinum coil element of the probe. The probe is then placed in the interface and pyrolysed ballistically for 2 seconds. Pyrolytic i

products are then swept by the carrier gas onto the fused silica capillary column where they are separated and detected with a MSD. Chromatographic and pyrolysis conditions are shown in Table 1. Prior to each analysis, the column is heated to 250*C to elute any volatiles which were not entrained in the polymer.

IV.

PRESENTATION OF RESULTS l

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The three pyrograms for each of the three Thermo-Lag samples are shown in Figures 1,

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3 and 5. The extracted ion dreiretogrms using the acrylate base ion m/e of 55 common to ethyl acrylate (EA) and base ion m/e of 69 common to methyl methacrylate (MMA) for each sample are shown in Figures 2,4 and 6. The EA/MMA area ratios and densities for each sample are shown in Table 2. Following each set of figures a library search is attached which identifies some of the major peaks for each sample followed by a summary area percent report.

1 e

NUCON 06LP829/01 V.

DISCUSSION OF RESULTS The average extracted ion area ratio of 1.34 i0.1 (t a) for EA/MMA shown in Table 2 is consistent with the average ratio of 1.3 i0.1 (i o) obtained from other Thermo-Lag samples.

The extracted ion chromatograms (Figure 2) for sample 0395-37A, a 3 hour3.472222e-5 days <br />8.333333e-4 hours <br />4.960317e-6 weeks <br />1.1415e-6 months <br /> rated panel sample, have an EA/MMA ratio of 1.43. Pyridine compounds identified in the pyrogram (Figure 1) are 3-methyl pyridine and 3, 4-dimethyl pyridine. Other key components identified are pentanedioic acid diethyl ester, trimethyl phenyl phaeah=*a, and octicizer.

De extracted ion duvir.eia rems (Figure 4) for sample 0395-37B, a 3 hour3.472222e-5 days <br />8.333333e-4 hours <br />4.960317e-6 weeks <br />1.1415e-6 months <br /> rated panel s

sample, have an EA/MMA ratio of 1.38. Pyridine compounds were not identified in the pyrogram (Figure 3) although visual iaW shows trace amounts present. Other key components identified are pentanedioic acid diethyl ester, octicizer, triphenyl phosphate and trimethphenyl phosphate. This sample showed a much higher content of organic phosphate c,v.i.pourids than other Hermo-lag samples.

Sample 0395-37B was retested and the extracted ion diss ;syems shown in Figure 7 have an EA/MMA ratio of 1.29. Pyridine compounds identified in the pyrogram (Figure

8) and library search (Figures 9,10,11 and 12) are 3-methyl pyridine, 3, 5-dimethyl pyridine and 2,5-dimethyl pyridine. Other key components identified are pentanedioic acid diethyl ester (Figure 13) 2, 3, 4, 5-tetramethyl 1-H-pyrrole (Figure 14) and octicizer (Figure 15).

De extracted ion chromatograms (Figure 6) for sample 0395-37C, a 3 hour3.472222e-5 days <br />8.333333e-4 hours <br />4.960317e-6 weeks <br />1.1415e-6 months <br /> rated panels sample, have an EA/MMA ratio of 1.21. Pyridine compounds identified in the pyrogram.

(Figure 6) are pyridme, 3-methyl pyridine, 2, 5-dimethyl pyridine, 3-ethenyl pyridine, 3, 5-dimethyl pyridine,2,3,5-trimethyl pyridine and 3-ethyl-5-methyl pyridine. Other key components identified are 2, 3, 4, 5-tetramethyl IH-pyrrole, pentanedioic acid diethyl ester, octicizer, triphenyl phosphate and trimethyl phenyl phosphate.

In conclusion, inspection of the pyrograms for the Hermo-Lag samples 0395-37A and C indicates that they are consistent with other Thermo-Lag samples in terms of chemical composition.

Sample 0395-37C has a much larger quantity of organic phosphate compounds than other Thermo Lag samples. This may be due to selection of the subsample used for analysis. The heterogeneity of this material is evidenced by the two sets of results for sample 0395-37B, where, in the first test, only trace amounts of pyridine compounds are found but a large amount of octicizer is present, while in the second test of the same sample only a small amount of octicizer is present.

J 2

NUCON 06LP829/01 TABLE 1 Chromatographic Conditions:

30 meter 0.25 mm narrow bore fused silica HP-5 CB capillary column.

Carrier Gas: Helium,0.9 mumin, split ratio 35:1 Column Conditions:

Initial Temperature: 50*C for 1 minute hold Temperature Ramp: 8'C/ min to 250*C Final Temperature: Hold at 250*C for 10 minutes Injector Temperature: 250*C Detector Temperature: 280*C Detector was an HP MSD in scan mode (30-550 amu)

Pyrolysis Conditions:

Pyrolysis Temperature: 650*C Interval: 2 seconds Ramp: 2*C/ millisecond Probe Type: Platinum Coil Interface Temperature: 205'C

NUCON 06LP829/01 TABLE 2 Sample EA/MMA Ratio Density i

NUCON Lab Log # 0395-37A 1.43 1.36 g/mL Pre-fabricated, 3 hour3.472222e-5 days <br />8.333333e-4 hours <br />4.960317e-6 weeks <br />1.1415e-6 months <br /> rated panel, trowel grade and top coat.

Location: RAB + 21 elev. diesel generator Room A FD-77-Fire Area, RAB 16 NUCON Lab Iog # 0395-37B 1.38 1.20 g/mL Pre-fabricated, 3 hour3.472222e-5 days <br />8.333333e-4 hours <br />4.960317e-6 weeks <br />1.1415e-6 months <br /> rated panel trowel grade and top coat.

Location: RAB-4 elev. boric acid concentrator Room A FD-177, Fire Area RAB 31 1

NUCON Lab Log # 0395-37C 1.21 1.50 g/mL Pre-fabricated 3 hour3.472222e-5 days <br />8.333333e-4 hours <br />4.960317e-6 weeks <br />1.1415e-6 months <br /> rated panel, trowel grade and top coat.

Iocation RAB + 21 elev. in front of tool room FD-3HV-B217B-Fire aren R AR 75

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C:\\ DATABASE \\NBS75K.L Minimum Quality:

0 Unknown Spectrum:

' Apex Integration Params: AutoIntegrate Pk#

RT Areat Library /ID Ref#

CAS#-

Qual 1

1.74 1.89 C:\\ DATABASE \\NBS75K.L No matches found 2-2.33 0.11 C:\\ DATABASE \\NBS75K.L Xanthatin, 8-(4-(((isopropylamino) 55737 000000-00-0.12 Benzeneathanamine, N-methyl-6311 000589-08-2 10 Amphetamine 6317 000300-62-9 10 3

3.03 1.37 C:\\ DATABASE \\NBS75K.L 2-Propenoic acid, 2-methyl, methy 63329 000080-62-6 68 2-Propenoic acid, 2-methyl, methy 63330 000080-62-6 64 2-Propenoic acid, 2-methyl, methy 1484 000080-62-6 64 4

3.87 0.07 C:\\ DATABASE \\NBS75K.L 2-Butenoic acid, 4-nitrophenyl est 24526 014617-88-0 50 2-Propenoic acid, 2-methyl, ethyl 2900 000097-63-2 45 2-Propenoic acid, 2-methyl, ethyl. 64113 000097-63-2 41 5

5.08 0.08 C:\\ DATABASE \\NBS75K.L Pyridine, 3-methyl-981 000108-99-6 92 Pyridine,-3-methyl-63046 000108-99-6 64 Pyridine, 3-methyl-63045 000108-99-6 64 6

7.13' O.03 C:\\ DATABASE \\NBS75K.L Pyridine, 3,4-dimethyl-63728 000583-58-4 90 Pyridine, 3,5-dimethyl-2047 000591-22-0 90 Pyridine, 3,4-dimethyl-2050 000583-58-4 90 7

9.27 0.07 C:\\ DATABASE \\NBS75K.L 2,3-Pyridinediamine 2194 000452-58-4 47 Butanamide, N- (4-hydroxyphenyl) -

17435 000101-91-7 43 2 (1H) - Pyridinone, 1-methyl-63813 000694-85-9 43 8

10.17 0.17 C:\\ DATABASE \\NBS75K.L Cyclopentasiloxane, decamethyl-51266 000541-02-6 76 Benzeneacetic acid,. alpha.,3,4-tr 74564 037148-65-5 43 Ergoline-8-carboxamide, 9,10-dideh 37179 000478-94-4 27 9

10.29 0.11 C:\\ DATABASE \\NBS75K.L Cyclopentasiloxane, decamethyl-51266 000541-02-6 76 Benzoic acid, 2,6-bis ( (trimethylsi 51296 003782-85-2 38 Silane, ( (4- (1,2-bis [ (trimethylsil 57393 056114-62-6 35 C:\\HPCHEM\\1\\ DATA \\EM31471A.D Thu Apr 13 13:34:03 1995 Page 1

10 11.03 0.03 C:\\ DATABASE \\NBS75K.L 3-AcGtyl-1-m3thylpyrrole 4027 000932-62-7 52 1H-Pyrrole, 3-ethyl-2,4-dimethyl-64742 000517-22-6 52 Acetamide, N- (4-methoxyphenyl) -

67892 000051-66-1 52 11 12.01 0.12 C:\\ DATABASE \\NBS75K.L Pentanedioic acid, 2-methyl, dime 68429'014035-94-0 38 Pentanedioic acid, diethyl ester 69156 000818-38-2 12 2,4,5-Tri-O-acetyl-3-O-methyl-6-de 42895 000000-00-0 12 12 12.28 0.03 C:\\ DATABASE \\NBS75K.L Benzaldehyde, 2,4,6-trinitro-32082 000606-34-8 12 5-Bromo-2-iodosobenzoic aicd 48296 000000-00-0 8

1 Cyanamide, [2-(1-bromo-6a,7,7a,10a 55409 055401-69-9 7

13 12.60 0.16 C:\\ DATABASE \\NBS75K.L j

Pentanedioic acid, diethyl ester 19778 000818-38-2 87 Pentanedioic acid, diethyl ester 69156 000818-38-2 59 l

Pentanedioic acid, 2,4-dimethyl,

38087 057983-50-3 37 14 13.32 1.63 C:\\ DATABASE \\NBS75K.L Cyclohexasiloxane, dodecamethyl-56711 000540-97-6 91 2 -Chloro (4 -methoxyphenyl) (4 -

48253 063673-76-7 35 Acetic acid, (bis [ (trimethylsilyl) 49839 053044-27-2 34 i

15 13.50 0.27 C:\\ DATABASE \\NBS75K.L 2-(Diethylamino)-3-methylcycloprop 11187 091295-98-6 32 2H-Quinolizin-3-ol, octahydro, tr 11200 015'69-36-5 32 Piperidine, 4-methyl-1421 0C0626-58-4 30 16 14.64 0.06 C:\\ DATABASE \\NBS75K.L Octadecanoic acid, 2-((trimethylsi 52732 056196-58-8 15 4-Amino-5-imidazole carboxamide, t 48317 000000-00-0 11 Octadecanoic acid, trimethylsilyl 73766 018748-91-9 10 17 15.55 0.05 C:\\ DATABASE \\NBS75K.L Dimethyl phthalate 69376 000131-11-3 42 Dimethyl phthalate 69379 000131-11-3 42 Dimethyl phthalate 69380 000131-11-3 38 18 16.11 1.74 C:\\ DATABASE \\NBS75K.L 3-Isopropoxy-1,1,1,7,7,7-hexamethy 60503 071579-69-6 37 Tetrasiloxane, 3,5-diethoxy-1,1,1, 59390 072439-78-2 27 1,1,1,3,5,7,9,9,9-Nonamethylpentas 48301 084409-41-6 16 19 16.47 0.12 C:\\ DATABASE \\NBS75K.L i

Phosphoric acid, tris (methylphenyl 73955 001330-78-5 92 Phosphoric acid, tris (methylphenyl 51123 001330-78-5 58 Phosphoric acid, tris (4-methylphen 51126 000078-32-0 53 20 17.19 0.10 C:\\ DATABASE \\NBS75K.L' 1,3,4,6-Hexanetetrone, 1- ( 4 -chloro 48347 058330-14-6 30 Ethanone, 1-[4-(1,1-dimethylethyl) 16773 000943-27-1 27 Pyridine, 3-(2-thienyl)-

12681 021298-53-3 27 C:\\HPCHEM\\1\\ DATA \\EM31471A.D Thu Apr 13 13:34:24 1995 Page 2

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Pk#

RT Arco %

Librcry/ID Rsf#

CAS#

Qual 21-17.68 0.11 C:\\ DATABASE \\NBS75K.L Buten3thioic Ecid, S-butyl actor 12349 002432-52-2 49 Propanoic acid, 2-methyl, 1-(1,1-40505 074381-40-1 47 2-Furanmethanol, tetrahydro-63508 000097-99-4 47 22 17.86 0.11 C:\\ DATABASE \\NES75K.L Phenol, 4-(2,2,4-trimethylpentyl)-

24397 000000-00-0 64 2H-Imidazo[4,5-b]pyridin-2-one, 1,

6253 016328-62-4 50 Phenol, 4-(1,1-dimethylpropyl)-

13527 000080-46-6 50 23 18.10 0.04 C:\\ DATABASE \\NBS75K.L Phosphoric acid, tris (3-methylphen 51124 000563-04-2 95 Phosphoric acid, tris (methylphenyl 51123 001330-78-5 91 Phosphoric acid, tris (methylphenyl 73955 001330-78-5 87 24 18.59 1.51 C:\\ DATABASE \\NBS75K.L Silane, [ [4- [1,2-bis [ (trimethylsil 74512 056114-62-6 55 3,4-Dihydroxymandelic acid, ethyl 55759 000000-00-0 49 1,3,5,7-Tetraethyl-1-ethylbutoxysi 56589 073420-30-1 47 i

25 19.10 0.12 C:\\ DATABASE \\NBS75K.L Butanoic acid, 2-amino-4,4,4-trifl 19090 061141-67-1 25

. delta.2-Tetrazaboroline, 5-ethyl-4392 020534-01-4 11 Phenol, 2,2'-((1-methyl-1,2-ethane 39799 000094-91-7 11 26 19.26 0.06 C:\\ DATABASE \\NBS75K.L 5-Acetoxymethyl-2-furaldehyde 14397 010551-58-3 11 Butanoic acid, 2-amino-4,4,4-trifl 19090 061141-67-1E11 i

Phenol, 2-[(1-methylethyl) thio]-

14457 029549-62-0 11 27 19.48 0.10 C:\\ DATABASE \\NBS75K.L Phenol, 2,2'-((1-methyl-1,2-ethane 39799 000094-91-7 25 Bendazol 24958 000621-72-7 18 1-Benzopyrylium, 2-phenyl-24651 014051-53-7 14 i

28 19.80 0.06 C:\\ DATABASE \\NBS75K.L Phosphoric acid, tris (4 -methylphen 51126 000078-32-0 95 Phenothiaphosphine, 2,8-dimethyl-1 51105 023861-49-6 45 Phosphoric acid, tris (methylphenyl 51123 001330-78-5 42 29 20.01 0.57 C:\\ DATABASE \\NBS75K.L 1,l'-Biphenyl, 3-azido-21582 014213-01-5 20 3-Cyclobutene-1,2-dicarboxylic aci 29069 055673-94-4 18 7, 8 -Dihydro methyl ( 6H) pyrazolo (3 27965 000000-00-0 16 30 20.22 0.38 C:\\ DATABASE \\NBS75K.L cis-2,4,5-Trimethoxy. beta.-methyl 34481 000000-00-0 30 1

1, 3 -Diphenyl- ( 4 H) 1, 2, 4 - tri azoline -

34507 000000-00-0 27 4-Hexen-2-yn-1-one, 1-phenyl-5-(1-34549 029743-43-9 25 31 20.34 0.61 C:\\ DATABASE \\NBS75K.L 1H-Purine, 6-(methylthio)-

67932 000050-66-8 27 Rheadan-8-ol, 2,3,10,11-tetrametho 54012 014028-91-2 25 7,8-Dihydro-2-methyl (6H)pyrazolo(3 27965 000000-00-0 25 C:\\HPCHEM\\1\\ DATA \\EM31471A.D Thu Apr 13 13:34:45 1995 Page 3 m

w

Bk#

RT Arac %

Library /ID Raf#

CAS#

Qual

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i

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32 20.48 0.25 C:\\ DATABASE \\NBS75K.L Phorphoric acid, tris (mathylphtnyl 51123 001330-78-5 97 Phosphoric acid, tris (4-methylphen 51126 000078-32-0193 l

Phosphoric acid, tris (methylphenyl 73955 001330-78-5 91 j

i 33 20.74 1;49 C:\\ DATABASE \\NBS75K.L

. beta.-D-Glucopyranosiduronic acid 62040 052092-53-2 43 I

Morphinan, 7,8-didehydro-4,5-epoxy 55885 055449-66-6 43 l

Estra-1,3,5 (10) -trien-17-one, 2- ( (

55893 077883-26-2 38 34 20.97 1.43 C:\\ DATABASE \\NBS75K.L Benzenamine, N,N,3-trimethyl-.

65619 000121-72-2 14 Acetic acid, (4-formylphenoxy), e 24812 051264-69-8 14 3-Pyridinecarbonitrile, 1,~4-dihydr 6098 000767-98-6 14 35 21.24 1.32 C:\\ DATABASE \\NBS75K.L 4-Amino-2-methyl-5,6-trimethylenep 9460 076881-49-7 25-1H-Purin-6-amine, N-methyl-66644 000443-72-1 20 4-Pyridinecarboxaldehyde, 3-hydrox 14236 000066-72-8 18 36 21.55 1.09 C:\\ DATABASE \\NBS75K.L Phosphoric acid, tris (3-methylphen 51124 000563-04-2 95 Phosphoric acid, tris (methylphenyl 51123 001330-78-5 89 Phosphoric acid, tris (methylphenyl 73955 001330-78-5 86

37. 21.83' O.63 C:\\ DATABASE \\NBS75K.L Phosphoric acid, tris (3-methylphen' 51124 000563-04-2 91 Phosphoric acid, tris (4-methylphen 51126 000078-32-0 86 Phosphoric acid, tris (methylphenyl 51123 001330-78-5 76 38 22.13 1.34 C:\\ DATABASE \\NBS75K.L Phosphoric acid, tris (methylphenyl 51123 001330-78-5 90 Phosphoric acid, tris (methylphenyl 73955 001330-78-5 64 Phenothiaphosphine,-2,8-dimethyl-1 51105 023861-49-6 46 39 22.25 0.63 C:\\ DATABASE \\NBS75K.L Phosphoric acid, tris (3 -methylphen 51124 000563-04-2 94 Phosphoric acid, tris (methylphenyl 73955 001330-78-5 87 Phosphoric acid, tris (4-methylphen 51126 000078-32-0 86 40 22.36 1.20 C:\\ DATABASE \\NBS75K.L Phosphoric acid, tris (4-methylphen 51126 000078-32-0 95 Phosphoric acid, tris (methylphenyl 73955 001330-78-5 92 Phosphoric acid, tris (methylphenyl 51123 001330-78-5 45 41 22.64 2.68 C:\\ DATABASE \\NBS75K.L 1,1,1, 5,7,7,7-Heptamethyl-3,3 -bis (

56714 038147-00-1 27 Benzene, 1-phenyl (2 -cyano-2 -phe 39643 027869-56-3 10 i

14. alpha.-Morphinan, 7,8-didehydro 39631 017939-34-3 10 42 23.18 2.32 C:\\ DATABASE \\NBS75K.L 2,4,6,8,9,10-Hexathiatricyclo[3.3.

46703 057289-12-0 16 43 23.38 1.30 C:\\ DATABASE \\NBS75K.L 2,4 (1H) -Cyclo-3,4 -secoakuammilan-1 52355 006472-42-0 35 2-Propanol, 1-(2-(2-methoxy-1-meth 24251 020324-33-8 27 Butanamide, 3-methyl-1621 000541-46-8 25 C:\\HPCHEM\\1\\ DATA \\EM31471A.D-Thu Apr 13 13:35:06 1995 Page 4

Pk#

RT Arsa%

Librcry/ID Rsf#

CAS#

Qunl j

44 23.76 2.96 C:\\ DATABASE \\NBS75K.L 4

POntEna, 2-msthoxy-1778 006795-88-6 43 Hydrazine, 1-methyl-1-(2-methylpro 1757 020240-63-5 38 Butanamide, 3-methyl-1621 000541-46-8 38 45 24.11 4.29 C:\\ DATABASE \\NBS75K.L 2,4,6,8,9,10-Hexathiatricyclo[3.3.

50037 057274-38-1 38 i

Butanamide, 3-methyl-1621 000541-46-8 38 3-Pentanol, 2-methyl-63561 000565-67-3 38 46 24.40 4.55 C:\\ DATABASE \\NBS75K.L Benzeneacetic acid,. alpha.,3,4-tr 74565 037148-65-5 32 1,3,5,7-Tetraethyl-1-ethylbutoxysi 56589 073420-30-1 30 Benzoic acid, 2,4 -bis [ (trimethylsi 73975 010586-16-0 25 47 24.74 5.03 C:\\ DATABASE \\NBS75K.L 1-Propanol, 2- (2-methoxy-1-methyle 9239 055956-21-3 43 Butane, 2-methoxy-854 006795-87-5 38 1-Propanol, 2- (2-methoxypropoxy) -

9232 013588-28-8 37 48 25.02 7.01 C:\\ DATABASE \\NBS75K.L 1-Propanol, 2-(2-methoxy-1-methyle 9239 055956-21-3 47 2-Naphthalenemethanol, decahydro.

28205 051317-08-9 37 Butanamide, 3-methyl-1621 000541-46-8 35 49 25.42 8.21 C:\\ DATABASE \\NBS75K.L 3-Pentanol, 2-methyl-63561 000565-67-3 43 Propane, 1-ethoxy-2-methyl-63544 000627-02-1 43 Butanamide, 3-methyl-1621 000541-46-8 38 50 25.98 3.89 C:\\ DATABASE \\NBS75K.L Morphinan, 7,8-didehydro-4,5-epoxy 55885 055449-66-6.46 1,1,1,5,7,7,7-Heptamethyl-3,3-bis (

56714 038147-00-1 42 Estra-1,3,5(10)-trien-17-one, 2-[(

55893 077883-26-2 27 51' 26.34 1.81 C:\\ DATABASE \\NBS75K.L 2,4 (1H) -Cyclo-3,4-secoakuammilan-1 52355 006472-42-0 30 Benzo [1, 2 -c : 4, 5 -c ' ] dipyrrole-1, 3, 5 53562 031663-79-3 11 Benzo [1,2 -c : 4, 5 - c ' ] dipyrrole-1, 3,5 53561 031663-75-9 11 52 26.46 1.28 C:\\ DATABASE \\NBS75K.L Bikaverin 52326 033390-21-5 59 2,4 (1H) -Cyclo-3,4 -secoakuammilan-1 52355 006472-42-0 35 Sarpagan-16-carboxylic acid, 3,17-52356 053632-75-0 22 53 26.65 1.35 C:\\ DATABASE \\NBS75K.L 2 -Propanol, 1- (2 -ethoxypropoxy) -

12860 010143-32-5 47 2-Pentanone, 5-methoxy-64282 017429-04-8 47 Ethane, 1-ethoxy-1-methoxy-1926 010471-14-4 47 54 27.06 0.89 C:\\ DATABASE \\NBS75K.L Amylene Hydrate 62940 000075-85-4 47 2-Pentanol, 2-methyl -

1763 000590-36-3 38 2-Propanol, 1-(2-ethoxypropoxy)-

12860 010143-32-5 38 C:\\HPCHEM\\1\\ DATA \\EM31471A.D Thu Apr 13 13:35:24 1995 Page 5

~

Pk#

RT ArOS%

Librdry/ID R$f#

CAS#

Qu21 55 27.33 3.58 C:\\ DATABASE \\NBS15K.L 1,1,1,5,7,7,7-H;ptcmathyl-3,3-bio (

56714 038147-00-1 45 Morphinan, 7,8-didehydro-4,5-epoxy 55885 055449-66-6 42 1

. beta.-D-Glucopyranosiduronic acid 62040 052092-53-2 27 56 27.70 1.76 C:\\ DATABASE \\NBS75K.L j

1,1,1,5,7,7,7-Heptamethyl-3,3-bis (

56714 038147-00-1 38 Benzoic acid, 2,4 -bis [ (trimethylsi 73975 010586-16-0

',5 Benzoic acid, 2,5-bis (trimethylsil 73978 003618-20-0 10 57 28.16 14.62 C:\\ DATABASE \\NBS75K.L Octicizer 50542 001241-94-7 38 i

Benz [b] acridine, 1,2,3,4,7,8,9,10-34157 055044-74-1 23 Benz [c] acridine, 1,2,3,4,8',9,10,11 34155 055044-73-0 23

)

58 28.58 2.76 C:\\ DATABASE \\NBS75K.L 1-Propanol, 2-(2-methoxy-1-methyle 9239_055956-21-3 47 1,2-Propanedicl, 2-methyl, 1-meth 14343 074792-80-6 38 2,5,8,11-Tetraoxadodecane 17074 000112-49-2 38 59 28.76 3.59 C:\\ DATABASE \\NBS75K.L 1-Propanol, 2- (2-methoxy-1-methyle 9239 055956-21-3 43 Butane, 1-echoxy-63550 000628-81-9 38 2-Butanol, 2,3-dimethyl-63570 000594-60-5 35

)

60 29.41 0.60 C:\\ DATABASE \\NBS75K.L Pentane, 2-methoxy-1778 006795-88-6 25 Ethanedioic acid, dimethyl estor 3458 000553-90-2 25 4

1-Chloro-2-ethoxyethane 2079 000628-34-2 25 61 29.63 0.29 C:\\ DATABASE \\NBS75K.L 1,2-Benzenedicarboxylic acid, mono 39132 004376-20-9 43 1,2-Benzenedicarboxylic acid, 3-ni 25513 000603-11-2 43 Bis (2-ethylhexyl) phthalate 53128 000117-81-7 43 62 29.85 0.50 C:\\ DATABASE \\NBS75K.L l

Benzoic acid, 2,4-bis [(trimethylsi 73975 010586-16-0 20 Benzoic acid, 2,5-bis (trimethylsil 51295 003618-20-0 18 Silane, [ [4- [1,2-bis [ (trimethylsil 74512 056114-62-6 16 63 30.43 0.15 C:\\ DATABASE \\NBS75K.L i

Tanshinone II-b 44270 017397-93-2 39 4H-1-Benzopyran-2-carboxylic acid, 39264 030192-14-4 22 3-Aminodiftalone 39292 067483-30-1 20 64 30.86 0.63 C:\\ DATABASE \\NPS75K.L Phenol, dimethyl, phosphate (3 :1) 54605 025155-23-1 51 Cholesta-5,7-dien-3-one, 4,4-dimet 54634 000000-00-0 12 C(14a)-Homo-27-norgammacer-14-ene 54655 018046-86-1 10 65 31.77 0.11 C:\\ DATABASE \\NBS75K.L Phosphoric acid, tris (3-methylphen 51124 000563-04-2 90 Phosphoric acid, tris (methylphenyl 73955 001330-78-5 86 Phosphoric acid, tris (methylphenyl 51123 001330-78-5 49 1

C:\\HPCHEM\\1\\ DATA \\EM31471A.D Thu Apr 13 13:35:49 1995 Page 6 j

Pk#

RT Arcs %

Library /ID R

CAS#

QuS1 66 32.41 0.02 C:\\ DATABASE \\NBS75K.L Phorph;ric ccid, trio (mathylphnnyl 51123 001330-78-5 91 1H-12a,5- (Epoxymethanol pyrido [3 ',4 51134 003329-92-8 25 Phosphoric acid, tris (4-methylphen 51126 000078-32-0 25

)

l 67 32.86 0.59 C:\\ DATABASE \\NBS75K.L 1,1,1,5,7,7,7-Heptamethyl-3,3-bis (

56714 038147-00-1 12 Heptasiloxane, hexadecamethyl-59695 000541-01-5 12 Benzoic acid, 2,5-bis (trimethylsil 73978 003618-20-0 11 68 33.13 0.01 C:\\ DATABASE \\NBS75K.L 2-Naphthalenemethanol, decahydro.

28205 051317-08-9 47 Heptane, 1-ethoxy-15325 016624-06-9 27 8517 001969-43-3 30 Cyclooctanemethanol,. alpha.,.alph 69 33.62 1.62 C:\\ DATABASE \\NBS75K.L 1,1,1,5,7,7,7-Heptamethyl-3,3-bis (

56714 038147-00-1 38 Heptasiloxane, hexadecamethyl-59695 000541-01-5 14 Benzoic acid, 2,5-bis (trimethylsil 73978 003618-20-0 11 70 35.69 0.21 C:\\ DATABASE \\NBS75K.L 2 - Propanol, 1 - ( 2 -me thoxyp ropoxy) -

9233 013429-07-7 38 j

Pentane, 2-methoxy-1778 006795-88-6 38 i

Butanamide, 3-methyl-1621 000541-46-8 38 l

71 35.88 0.11 C:\\ DATABASE \\NBS75K.L Butanamide, 3-methyl-1621 000541-46-8 38 2 - Propanol, 1- ( 2 -methoxypropoxy) -

9233 013429-07-7 38 Propanoic acid, 2-hydroxy-2-methyl 3494 002110-78-3 36 I

i C:\\HPCHEM\\1\\ DATA \\EM31471A.D Thu Apr 13 13:36:00 1995 Page 7

Area Percent Report -- Sorted by Signal Information from Data File:

File

C:\\HPCHEM\\1\\ DATA \\EM31471A.D operator _
Marti Acquired
13 Apr 95 12:57 pm using AcqMethod EM31492 Sample Name: 0495-37a Misc Info
Thermolag sample Vial Number: 1 CurrentMeth: C:\\HPCHEM\\1\\ METHODS \\EM31492.M Retention Time Area Area %

. Ratio %

Total Ion Chromatogram 1.742 601393536 1.891 12.936 2.'335 35461107 0.112 0.763 3.027 434519950 1.366 9.347 3.866 22070112 0.069 0.475 1

5.078 26666286-0.084 0.574 7.130 10965117 0.034 0.234 1

9.274 22612605 0.071 0.486 10.173 53471448 0.168 1.150

'10.290 34352204 0.108 0.739 11.032 10335885 0.032 0.222 i

12.002 385"0794 0.121 0.830 12.280 9140554 0.029 0.197 12.604 51331931 0.161 1.104 13.312 516844108 1.625 11.118 13.494 85651901 0.269 1.842 14.644 19755558 0.062 0.425 15.543 14726153 0.046 0.317 16.107 554815668 1.745 11.934 16.466 39303151 0.124 0.845 17.-190 31161994 0.098 0.670 17.677 35868588 0.113 0.772 17;864 34835411 0.110 0.749 18.094 14137921 0.044 0.304 18.587 479371689 1.507 10.312

.19.104 36818758 0.116 0.792 19.259 20506049 0.064 0.441 19.478 31975393 0.101 0.688 19.799 20146385 0.063 0.433 20.004 181939663 0.572 3.914 20.225 122243376 0.384 2.630 20.336 193466228 0.608 4.162 20.483 80764082 0.254 1.737 20.733 474225524 1.491 10.201 20.979 454847358 1.430 9.784 21.232 418319486 1.315 8.998 C:\\HPCHEM\\1\\ DATA \\EM31471A.D Thu Apr 13 13:33:37 1995 Page 1

~~

Area Percent. Report -- Sorted by Signal Information from Data File:

File

C:\\HPCHEM\\1\\ DATA \\EM31471A.D Operator
Marti Acquired
13 Apr 95. 12:57 pm using AcqMethod EM31492 Stmple Name: 0495-37a Misc-Info
Thermolag sample Vial Number: 1 CurrentMeth: C:\\HPCHEM\\1\\ METHODS \\EM31492.M Retention Time-Area Area %

Ratio %

21.545 347601288 1.093 7.477 21.833 199517775 0.627 4.292 22.133 427224089 1.343 9.190 22.254 200848722 0.632 4.320 22.361 381247456 1.199 8.201 22.642 852348617 2.680-18.334 23.180 737361875 2.319 15.861 23.385 414625472 1.304 8.919 23.767 940298835 2.957 20.226 24.11?

1363159995 4.286 29.322

.24.393 1447207021 4.550 31.130 24.743 1599518140 5.029 34.406 25.016 2228418622 7.007-47.934 25.417 2609952331 8.207-56.141 25.980 1237946489 3.893 26.629 26.340 577189096 1.815 12.416 26.455 406990370 1.280 8.755 26.649 428636001 1.348

-9.220 27.058 281595199 0.885 6.057 27.327 1139525626 3.583 24.512 27.703 559735188 1.760 12.040 28.171 4648891930 14.618 100.000 28.587 878228811 2.761 18.891' 28.766 1142368693 3.592 24.573 29.410 190822799 0.600 4.105 29.633 90861797 0.286 1.954 29.845 159718577 0.502 3.436 30.429 47831864

-0.150 1.029 30.861 201454672 0.633 4.333 31.768 34752574 0.109 0.748 32.415 6300133 0.020 0.136 32.860 187537080 0.590 4.034 33.121 4663432 0.015 0.100 33.620 515022573 1.619 11.078 35.686 67680920 0.213 1.456 35.880 33755208 0.106 0.726 C:\\HPCHEM\\1\\ DATA \\EM31471A.D Thu Apr 13 13:33:40 1995 Page 2

Area Percent Report -- Sorted by Signal Information from Data. File:

File

C:\\HPCHEM\\1\\ DATA \\EM31471A.D Operator
Marti J
13 Apr 95 12:57 pm using AcqMethod EM31492 Acquired Simple Name: 0495-37a Thermolag sample Misc Info Vial Number: 1 CurrentMeth: C:\\HPCHEM\\1\\ METHODS \\EM31492.M

')

Retention Time Area Area %

Ratio %

l l

l i

C:\\HPCHEM\\1\\ DATA \\EM31471A.D Thu Apr 13 13:33:41 1995 Page 3

~

Ien. 55.00 (54.70 to 55'.7d) : EM31471A,D

-0495-37a Pock #

R3t Tima Type Width Arso

.Stcrt Time End Tim 2

- l '-

2.345 BB 0.128 3286432 2.136 2.721 2

2.898 BB 0.109 86746091 2.751 3.386 9

- _ _ _... _ _ _. _. _ _. _.. _ _ _ =...._

Ion. 69.00 (68.70 to 69.70): EM31471A.D~

0495-37c Pack #

RCt Time Type Width Arsa Stcrt Tima End Tima

.1 3.028 BV 0.103 60439623 2.820 3.425 2

3.862 VV 0.086 5842676 3.425 4'100 L

0 4

t 4

t r

e b

l I

f f

i l

?

l

9 File

C:\\HPCHEM\\1\\ DATA \\EM31471B.D Operator
Marti Acquired
13 Apr 95 2:25 pm using AcqMethod EM31492 Instrument :

-5972 --33 Sample Name: 0's95-37b wr'#it N I Misc Info

Thermolag sample Vial Number: 1 FIGURE 3 Abuncance tic: EM31471a.D 3e+07-i I

2.8e+07-l 2.6e+07-2.4e+07_

j 1

2.2e+07-2e+07-

1.Be+07 3

i i

81.6e+07-i l

l l

l 1.4e+07-1.2e+07_

le+07_

i 8000000_

f i

l i

6000000_

l l

4000000_

g I

3 l

!2000000j g

ifqw.L,J' '"

N*(

0' Time-->

5.'00 10.00 15.00 20.00 25.00 30.00 j

d E

File

C:\\HPCHEM\\1\\ DATA \\EM31471B.D Operator
Marti Acquired
13 Apr 95 2:25 pm using AcqMethod EM31492 i

Instrument :

5972 - 33 0495-37b Sample Name: Th'ermolag 'g,,7,; 4.4,9f f

Misc Info sample Vial Number: 1 FIGURE 4 ADundance 100 55.00 (54.70 to 55.70): EM31471B.D g

j 2.,190 1

l 3

I i

1 1000000q i

1 800000_

600000-400000,

I 1

1 200000_

2.36 I

0

~

frime-->

1.'00 2.'00 3.'00 4.00 5.00 Anuncance Ion 69.00 (65.70 to 69.70): EM31471B.D a

1000000-3.03 80C000_

1 j 600000-l 3

i i

400000J 1

{

200000 1

I l

1 l

i i

oN Time-->

1.00 2.00 3.00 4.00 5.00 l

i

Infcrmation from Datn File:

File

C:\\HPCHEM\\1\\ DATA \\EM31471B.D Operator
Marti Acquired
13 Apr 95 2:25 pm using AcqMethod EM31492 Sample Name: Of95-37b w/r e n6 Misc Info
Tnermolag sample Vial Number: 1 Search Libraries:

C:\\ DATABASE \\NBS75K.L Minimum Quality:

0 Unknown Spectrum:

Apex Integration Params: AutoIntegrate Pk#

RT Areat Library /ID Ref#

CAS#-

Qual 1

0.16 -12.73 C:\\ DATABASE \\NBS75K.L 2-Hexanol, 2-methyl-64355 000625-23-0 35 1

2-Hexanol, 2-methyl-64354 000625-23-0 35 2-Propanol, 1-(2-(2-methoxy-1-meth 24251 020324-33-8 32 1

2 1.74 6.46 C:\\ DATABASE \\NBS75K.L No matches found i

3 2.33 0.61 C:\\ DATABASE \\NBS75K.L

. beta.-D-Allofuranuronic acid, 5-[

59138 019396-06-6 25 I

Meprobamate 70443 000057-53-4 25 Acetamide, N-(aminocarbonyl)-

1671 000591-07-1 25 4

2.91 1.37 C:\\ DATABASE \\NBS75K.L 2-Propenoic acid, ethyl ester 63318 000140-88-5 91 2-Propenoic acid, ethyl ester 1461 000140-88-5 91 2-Propenoic acid, ethyl ester 63320 000140-88-5 83 5

3.04 4.05 C:\\ DATABASE \\NBS75K.L 2-Propenoic acid, 2-methyl, methy 63329 000080-62-6 68 2-Butenoic acid, methyl ester, (E) 1458 000623-43-8 64 2-Propenoic acid, 2-methyl, methy 63330 000080-62-6 64 6

3.86 0.49 C:\\ DATABASE \\NBS75K.L 2-Propenoic acid, 2-methyl, ethyl 2900 000097-63-2 64 2-Propenoic acid, 2-methyl, ethyl 64113 000097-63-2 60 2-Butenoic acid, 4-nitrophenyl est 24526 014617-88-0 50 7

5.15 0.20 C:\\ DATABASE \\NBS75K.L p-Xylene 63701 000106-42-3 70 Benzene, 1,2-dimethyl-63706 000095-47-6 70 Benzene, 1,3-dimethyl-63697 000108-38-3 70 8

7.39 0.10 C:\\ DATABASE \\NBS75K.L 1,2,4-Trimethylbenzene 3771 000095-36-3 90 Benzene, 1,2,3-trimethyl-64576 000526-73-8 86 Benzene, 1,3,5-trimethyl-64570 000108-67-8 86 9

11.98 0.49 C:\\ DATABASE \\NBS75K.L Pentanedioic acid, diethyl ester 69155 000818-38-2 27 Pentanedioic acid, 2-methyl, mono 12301 072088-36-9 25 1,3,2-Dioxaborinane, 4,6-dimethyl-22867 052964-02-0 22 C:\\HPCHEM\\1\\ DATA \\EM31471B.D Thu Apr 13 15:02:33 1995 Page 1

Pk#

RT Araa%

Librcry/ID Raf#

CAS#

Quni 10 12.58 0.57 C:\\ DATABASE \\NBS75K.L Pentanadioic acid, diethyl ester 19778 000818-38-2 87 Pentanedioic acid, diethyl ester 69156 000818-38-2 64 Pentanedioic acid, diethyl ester 69155 000818-38-2 58 j

11 13.08 0.09 C:\\ DATABASE \\NES75K.L 3-Pentanone, dimethylhydrazone 4996 016795-73-6 30 3-Piperidinol 63447 006859-99-0 30 Pyrimidine, 5-chloro-2-dimethylami 11664 081568-09-4 25 12 13.34 1.12 C:\\ DATABASE \\NBS75K.L Cyclohexasiloxane, dodecamethyl-56711 000540-97-6 93 Acetic acid, (bis [(trimethylsilyl) 49839 053044-27-2 34 2,4,6(1H,3H,5H)-Pyrimidinetrione, 49865 052988-92-8 32 i

13 13.47 0.60 C:\\ DATABASE \\NBS75K.L Piperidine, 4-methyl-63292 000626-58-4 38 Piperidine, 4-methyl-1421 000626-58-4 38 2 - (Diethylamino) methylcycloprop 11187 091295-98-6 32 14 16.10 1.53 C:\\ DATABASE \\NBS75K.L 3-Isopropoxy-1,1,1,7,7,7-hexamethy 60503 071579-69-6 25 Tetrasiloxane, 3,5-diethoxy-1,1,1,.59390 072439-78-2 22 1-[2,4-Bis (trimethylsilyloxy)pheny 58102 000000-00-0 16 j

15 17.17 0.15 C:\\ DATABASE \\NBS75K.L 4,5,6,7-Tetramethylphthalide 20315 029002-54-8 42

Benzene, 1- (1-ethylpropyl) propy 20374 054789-16-1 38 Benzene, 1-(1,1-dimethylethyl)-3-e 16799 006630-01-9 38 16 17.66 0.09 C:\\ DATABASE \\NBS75K.L Pentane, 3-bromo-66684 001809-10-5 38 Borane, diethyl[1-ethyl-2-(methoxy 21917 053670-48-7 38 Pentane, 2,3,4-trimethyl-64229 000565-75-3 38 17 17.81 0.09 C:\\ DATABASE \\NBS75K.L Phenol, 4-(1,1,3,3-tetramethylbuty 24424 000140-66-9 64 Phenol, 4-(2,2,3,3-tetramethylbuty 24409 054932-78-4 52 Phenol, 4-(1,1,3,3-tetramethylbuty 70047 000140-66-9 52 18 18.58 1.43 C:\\ DATABASE \\NBS75K.L Silane, [(4-[1,2-bis ((trimethylsil 57393 056114-62-6 55 1,2-Benzenediol, 4- (2-amino-1-hydr 57358 056145-09-6 47 Silane, ((4-(1,2-bis [(trimethylsil 74512 056114-62-6 46 19 19.08 0.15 C:\\ DATABASE \\NBS75K.L Phenol, 2,2'-[(1-methyl-1,2-ethane 39799 000094-91-7 42 SH-Dibenzo(a,d]cyclohepten-5-one, 70114 001210-35-1 41 Naphthalene, 1,2,3,4-tetrahydro 25032 003018-20-0 41 20 19.22 0.20 C:\\ DATABASE \\NBS75K.L Phenol, 2,2'-[(1-methyl-1,2-ethane 39799 000094-91-7 32 Ethyl N'-isopropylureidoacetate 19738 000000-00-0 30 Ethanamine, N-methyl ( (2-methylp 34965 015301-93-6 27 C:\\HPCHEM\\1\\ DATA \\EM31471B.D Thu Apr 13 15:02:58 1995 Page 2

(.- - ~

Pk#

RT.

Ar@c%

Library /ID Raf#

CAS#

Quni 21 19.45 0.23 C:\\ DATABASE \\NBS75K.L 1H-Inden-1-ol, 2,3-dihydro-65500 006351-10-6 18 Dibenzo[b,e]-1,4-diazabicyclo(2.2.

24947 000000-00-0 15 1

1,2,4-Oxadiazol-5-amine, 3-phenyl-12634 003663-37-4 14 22 19.60 0.15 C:\\ DATABASE \\NBS75K.L 5-Bromo-2-iodosobenzoic aicd 48296 000000-00-0 25 N-Desmethyldiphenhydramine 32185 000000-00-0 25 Pheno.'., 2, 2 ' - ( (1-methyl-1, 2 -ethane 39799 000094-91-7 25 23 19.97 1,72 C:\\ DATABASE \\NBS75K.L Benzo [b] thiophene, 2- (butylthio) -

28074 054965-46-7 15 1,l'-Biphenyl, 3-azido-21582 014213-01-5 15 3-Cyclobutene-1,2-dicarboxylic aci 29069 055673-94-4 11 24 20.12 0.25 C:\\ DATABASE \\NBS75K.L 2-Iodohistidine 39529 000000-00-0 38 1,4-Oxathiin-3-carboxylic acid, 2-24692 117238-98-9 15 Pyridine, 2-ethyl-4,6-dimethyl-6309 001124-35-2 14 25 20.21 0.66 C:\\ DATABASE \\NBS75K.L 1, 3 -Diphenyl- (4H) 1, 2, 4 -triazoline -

34507 000000-00-0 38 2,5-Cyclohexadien-1-one, 2,5-dimet 34546 054245-93-1 27 Triamterene 34464 000396-01-0 18 26 20.31 1.77 C:\\ DATABASE \\NBS75K.L 7,8-Dihydro-2-methyl (6H)pyrazolo[3 27965 000000-00-0 25 Flavone 28172 000525-82-6 18 Urea, 1-neopentyl-3-phenyl-2-thio-28087 015093-39-7 11 27 20.45 0.32 C:\\ DATABASE \\NBS75K.L Propanedioic acid, bis (2-methyl 31923 074793-47-8 30 1H-Indole-3-ethanamine, 6-fluoro.

20703 077590-52-4 22 Acetic acid, oxo-62541 000298-12-4 11 28 20.71 1.28 C:\\ DATABASE \\NBS75K.L 2H-1,4-Benzodiazepin-2-one, 7-chlo 55928 055319-93-2 15 Cyclohexasiloxane, dodecamethyl-56711 000540-97-6 14 Heptasiloxane, hexadecamethyl-59695 000541-01-5 12 29 20.95 3.99 C:\\ DATABASE \\NBS75K.L Benzene, 1-methyl-4-(nitromethyl)-

9997 029559-27-1 14 Pyridine, 2-ethyl-4,6-dimethyl-6309 001124-35-2 14 Pyridine, 2,6-diethyl-6323 000935-28-4 14 30 21.20 1.24 C:\\ DATABASE \\NBS75K.L 3-(3-Pyridyl)propenoic acid 9438 001126-74-5 22 4-Amino-2-methyl-5,6-trimethylenep 9460 076881-49-7 20 7H-Purin-6-amine, '/-me thyl-9421 000935-69-3 18 31 21.52 0.13 C:\\ DATABASE \\NBS75K.L Cobalt, [ [3,3 ' - (1,2-ethanediyldini 54324 036466-12-3 11 8-Methyl-13,14-dioxo-8H,13H,14H-na 46504 059050-31-6 10 12,13-Dihydro-12-methyl-13,14-diox 46505 059050-19-0 10 C:\\HPCHEM\\1\\ DATA \\EM31471B.D Thu Apr 13 15:03:27 1995 Page 3

Pk#

RT AraS%

Library /ID Raf#

CAS#

Qual 32 21.81 0.25 C:\\ DATABASE \\NBS75K.L Pyridine, 3,5-dichloro-4-methoxy-2 24013 051050-42-1 49 1,3-Dioxolane, 2-(2,4-dimethylphen 27648 074752-98-0 47 6-Phenylisoquinoline 24117 070125-61-0 46 33 22.63 1.25 C:\\ DATABASE \\NBS7CK.L 1,1,1,5,7,7,7-Heptamethyl-3, 3 -bis (

56714 038147-00-1 30 Cyclohexasiloxane, dodecamethyl-56711 000540-97-6 10 4,5-Ethylene-8,9-dimethoxy-6-phena 39611 000000-00-0 10 34 23.16 0.20 C:\\ DATABASE \\NBS75K.L Isoxazole, 5 - (4 -methoxyphenyl) p 34124 003672-51-3 35 Pregn-5-en-20-one, 3,16-bis (acetyl 56086 023357-24-6 7

35 24.37 1.27 C:\\ DATABASE \\NBS75K.L Benzoic acid, 2,4-bis [(trimethylsi 51292 010586-16-0 42 Silane, [ [4 - [1,2-bis [ (trimethylsil 74512 056114-62-6 40 Silane, [ [4 - [1,2-bis [ (trimethylsil 57393 056114-62-6 40 36 24.72 0.33 C:\\ DATABASE \\NBS75K.L Ethanol, 2 - (2 - [4 - (1,1, 3, 3 - tetrame t 41793 002315-61-9 90 Octicizer 50542 001241-94-7 42 6-(Methylamino)phenanthren-3-ol 28427 098033-23-9 38 37 24.99 0.26 C:\\ DATABASE \\NBS75K.L Octicizer 50542 001241-94-7 46 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 27 2-Hydrazino-8-hydroxy-4-phenylquin 34111 000000-00-0 11 l

38 25.30 4.23 C:\\ DATABASE \\NBS75K.L 2,5,8,11-Tetraoxatetradecan-13-ol, 36541 020324-34-9 43 Propane, 1-ethoxy-2-methyl-63543 000627-02-1 38 2 - Propanol, 1 - ( 2 -me thoxypropoxy) -

9233 013429-07-7 38 39 25.65 0.27 C:\\ DATABASE \\NBS75K.L 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 52 Octicizer 50542 001241-94-7 50 2-Hydrazino-8-hydroxy-4-phenylquin 34111 000000-00-0 25 40 25.78 0.42 C:\\ DATABASE \\NBS75K.L 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 53 Octicizer 50542 001241-94-7 47 2 - ( 4 - Cyanophenyl ) dime thylaminom 34091 000000-00-0 27 41 25.88 0.33 C:\\ DATABASE \\NBS75K.L 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 72 9 - ( 3 - Fluorobenzyl) hydroxy-3, 6,1 50407 000000-00-0 22 2-Hydrazino-8-hydroxy-4-phenylquin 34111 000000-00-0 22 42 25.97 1.94 C:\\ DATABASE \\NBS75K.L 1,1,1, 5, 7, 7, 7 -Heptamet hyl-3, 3 -bi s (

56714 038147-00-1 40 Morphinan, 7,8-didehydro-4,5-epoxy 55885 055449-66-6 38 Benzoic acid, 2,4-bis [ (trimethylsi 51292 010586-16-0 35 i

C:\\HPCHEM\\1\\ DATA \\EM31471B.D Thu Apr 13 15:03:44 1995 Page 4

~_ _

Pk#

RT Aront Library /ID R2f#

CAS#

Quni 43 26.10 0.43 C:\\ DATABASE \\NBS75K.L Octicizer 50542 001241-94-7 47 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 47 Heptane, 1-ethoxy-8517 001969-43-3 18 44 26.22 0.41 C:\\ DATABASE \\NBS75K.L 3 - ( 2 -Hydroxy-6 -me thylphenyl) me t 36963 000000-00-0 38 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 38 Benzeneacetaldehyde, 3,4-dimethoxy 34066 000000-00-0 38 45 26.31 0.54 C:\\ DATABASE \\NBS75K.L Octicizer 50542 001241-94-7 50 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 50 2 - ( 4 - Cyanophenyl ) dimethylaminom 34091 000000-00-0 49 46 26.78 0.14 C:\\ DATABASE \\NBS75K.L Octicizer 50542 001241-94-7 70 2 - ( 4 - Cyanophenyl ) dime thylaminom 34091 000000-00-0 49 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 45 47 26.83 0.16 C:\\ DATABASE \\NBS75K.L Octicizer 50542 001241-34-7 78 2 - ( 4 - Cyanophe nyl ) dime thyl aminom 34091 000000-00-0 58 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 50 48 27.26 0.17 C:\\ DATABASE \\NBS75K.L Octicizer 50542 001241-94-7 60 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 59 Benzenamine, ar,ar-dibromo-33621 050307-05-6 43 49 27.59 1.08 C:\\ DATABASE \\NBS75K.L Phosphoric acid, triphenyl ester 73338 000115-86-6 99 Phosphoric acid, triphenyl ester 46311 000115-86-6 95 Phosphoric acid, triphenyl ester 73337 000115-86-6 93 50 27.70 1.18 C:\\ DATABASE \\NBS75K.L 1,1,1,5,7,7,7-Heptamethyl-3,3-bis (

56714 038147-00-1 38 Benzoic acid, 2,4-bis [ (trimethylsi 73975 010586-16-0 15 Benzeneethanamine, N- ( (pentafluoro 74706 055429-13-5 10 51 28.12 43.60 C:\\ DATABASE \\NBS75K.L Octicizer 50542 001241-94-7 38 Benz [b] acridine, 1,2,3,4,7,8,9,10-34157 055044-74-1 23 Benz (cl acridine, 1,2,3,4,8,9,10,11 34155 055044-73-0 23 52 28.20 4.41 C:\\ DATABASE \\NBS75K.L No matches found 53 28.52 4.77 C:\\ DATABASE \\NBS75K.L Propane, 2-ethoxy-2-methyl-1790 000637-92-3 35 2-Butanol, 2,3-dimethyl-63571 000594-60-5 35 Butanamide, 3-methyl-1621 000541-46-8 35 54 28.70 1.94 C:\\ DATABASE \\NBS75K.L Propanoic acid, 2-hydroxy-2-methyl

'3494 002110-78-3 38 3-Pentanol, 2-methyl-63561 000565-67-3 38 2 -Propanol,

1- ( 2 -me thoxypropoxy) -

9233 013429-07-7 38 C:\\HPCHEM\\1\\ DATA \\EM31471B.D Thu Apr 13 15:04:01 1995 Page 5

P'k#

RT Arant

-Library /ID Raf#

CAS#

Quni

.55 28.83 1.08 C:\\ DATABASE \\NBS75K.L Pentane, 2-methoxy-'

1778 006795-88-6 38 i,

Nonanamide 11725 001120-07-6 35 Hexylene Glycol 64445 000107-41-5 35 56 29.82 0.89 C:\\ DATABASE \\NBS75K.L Benzoic acid, 2,4-bis ((trimethylsi 51292 010586-16-0 25 3-Isopropoxy-1,1,1,7,7,7-hexamethy 60503 071579-69-6 22 Heptasiloxane, hexadecamethyl-59695 000541-01-5 14 57 30.37 0.16 C:\\ DATABASE \\NBS75K.L 4H-1-Benzopyran-2-carboxylic acid, 39264 030192-14-4 41 2,4,6,8-Tetrathiatricyclo(3.3.1.13 39250 057289-09-5 12 i

4H-1-Benzopyran-2-carboxylic acid, 39266 030095-84-2 10 58 30.77 1.40 C:\\ DATABASE \\NBS75K.L j

2-Naphthalenemethanol, 2,3,4,4a,5, 28228 063891-61-2 12 Tricyclo(4.3.1.13,8]undecane, 3-ch 18853 027011-47-8 12 Benzamide, N- (1,1-dimethylethyl) -3 24615 049834-28-8 11 59 31.74 2.62 C:\\ DATABASE \\NBS75K.L Phosphoric acid, tris (3-methylphen 51124 000563-04-2 99 Phosphoric acid, tris (methylphenyl 73955 001330-78-5 91 Phosphoric acid, tris (methylphenyl 51123 001330-78-5 91 60 32.39 1.56 C:\\ DATABASE \\NBS75K.L 4

Phosphoric acid, tris (3-methylphen 51124 000563-04-2 99 Phosphoric acid, tris (methylphenyl 51123 001330-78-5 94 Phosphoric acid, tris (methylphenyl 73955 001330-78-5 76 61 32.58 0.16 C:\\ DATABASE \\NBS75K.L Phosphoric acid, tris (4-methylphen 51126 000078-32-0 38 trans-4-Methoxy-3-propoxy. beta.-m 34070 000000-00-0 16

. alpha.-t-Butyl. alpha.-isopropyl-31118 000000-00-0 16 62 32.84 0.79 C:\\ DATABASE \\NBS75K.L 1,1,1,5,7,7,7-Heptamethyl-3,3-bis (

56714 038147-00-1 52 3,6-Dioxa-2,4,5,7-tetrasilaoctane, 41682 004342-25-0 12 i

Benzoic acid, 2,5-bis (trimethylsil 51295 003618-20-0 11 63 33.08 0.91 C:\\ DATABASE \\NBS75K.L j

Phosphoric acid, tris (3-methylphen 51124 000563-04-2 99 Phosphoric acid, tris (methylphenyl 73955 001330-78-5 92 Phosphoric acid, tris (methylphenyl 51123 001330-78-5 86 64 33.31 1.06 C:\\ DATABASE \\NBS75K.L Trisiloxane, 1,1,1,5,5,5-hexamethy 74103 003555-47-3 25 3-Isopropoxy-1,1,1,7,7,7-hexamethy 60503 071579-69-6 25 1,1,1,5,7,7,7-Heptamethyl-3,3-bis (

56714 038147-00-1 10 65 33.45 0.99 C:\\ DATABASE \\NBS75K.L Pentasiloxane, dodecamethyl-52458 000141-63-9 38 Heptasiloxane, hexadecamethyl-59695 000541-01-5 33 1,1,1,5,7,7,7-Heptamethyl-3,3-bis (

56714 038147-00-1 25 C:\\HPCHEM\\1\\ DATA \\EM31471B.D Thu Apr 13 15:04:19 1995 Page 6

i Area Percent Report -- Sorted by Signal Information from Data. File:

i File

C:\\HPCHEM\\1\\ DATA \\EM31471B.D operator
Marti
13 Apr 95 2:25 pm using AcqMethod EM31492 Acquired Sample Name: %95,37,b Misc Info
Tne olag sample Vial Number: 1 CurrentMeth: C:\\HPCHEM\\1\\ METHODS \\EM31492.M Retention Time Area Area %

Ratio %

Total Ion Chromatogram 0.166

-940991759

-12.730

-29.201 1.744 477714650 6.463 14.824 2.336 45118082 0.610 1.400 2.904 100951042 1.366 3.133 3.032 299430828 4.051 9.292 3.866 36385987 0.492 1.129 5.151 14676265 0.199 0.455 7.393 7713126 0.104 0.239 11.981 36416239 0.493 1.130 12.583 42069998 0.569 1.306 13.077 6720577 0.091 0.209 13.341 82553068 1.117 2.562 13.474 44243710 0.599 1.373 16.101 113445396 1.535 3.520 17.170 11435878 0.155 0.355 17.663 6291396 0.085 0.195 17.809 6406232 0.087 0.199 18.573 105712108 1.430 3.280 19.077 11009494 0.149 0.342 19.224 14806605 0.200 0.459 19.448 17014260 0.230 0.528 19.604 10994816 0.149 0.341 19.978 127290902 1.722 3.950 20.116 18277055 0.247 0.567 20.210 48738878 0.659 1.512 20.309 130898074 1.771 4.062 20.455 23328295 0.316 0.724 20.718 94695151 1.281 2.939 20.951 295043716 3.992 9.156 21.203 91627953 1.242 2.850 21.525 9855411 0.133 0.306 21.805 18501093 0.250 0.574 22.626 92106796 1.246 2.858 23.157 14491603 0.196 0.450 24.379 93814414 1.269 2.911 C:\\HPCHEM\\1\\ DATA \\EM31471B.D Thu Apr 13 15:02:00 1995 Page 1

t Area Percent Report -- Sorted by Signal Information from Data File:

C:\\HPCHEM\\1\\ DATA \\EM31471B.D File Operator

Marti
13 Apr 95 2:25 pm using AcqMethod EM31492 Acquired Srmple Name: OQ5-j7b g

TWer,molag sample Misc Info Vial Number: 1 CurrentMeth: C:\\HPCHEM\\1\\ METHODS \\EM31492.M Retention Time Area Area %

Ratio %

24.714 24091389 0.326 0.748 24.992 19059905 0.258 0.591 25.300 312595369 4.229 9.700 25.648 19622723 0.265 0.609 25.783 31365149 0.424 0.973 25.880 24731593 0.335 0.767 25.968 143739453 1.945 4.460 26.107 31511870 0.426 0.978 26.219 30664316 0.415 0.952 26.305 39590163 0.536 1.229 26.788 10305991-0.139 0.320 26.827 12057232 0.163 0.374 27.263 12793678 0.173 0.397 27.590 79518975 1.076 2.468 27.696 86866396 1.175 2.696 28.114 3222515027 43.596 100.000 28.199 325968746 4.410 10.115 28.523 352471792 4.768 10.938 28.708 143447592 1.941 4.451

~

28.830 79747261 1.079 2.475 29.825 65838100 0.891 2.043 30.373 12169538 0.165 0.378 30.767 103484203 1.400 3.211 31.743 194030722 2.625 6.021 32.383 115536827 1.563 3.585 32.577 11814532 0.160 0.367 32.843 58374995 0.790 1.811 33.074 67218295 0.909 2.086 33.309 78624229 1.064 2.440 33.448 73011166 0.988 2.266 l

i C:\\HPCHEM\\1\\ DATA \\EM31471B.D Thu Apr 13 15:02:03 1995 Page 2

QK95-37b 3

12/MM/a(I W

.P0ck#

Roc Timo Typ3 Width Arso Start Tima End Tima 1,

2.357 BB 0.116 6332151 2.166 2.702 2.

2.904 BV 0.102 78729031 2.781 3.466 e

i t

i i

1l t

b l

l i

l 9

Ion,69.00 (68.70,to 69.70): EM31471B.D

' ' ~ " ~ ~ ~

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l

~

Og95-37b

.l fg j

g 9 u)pt-t P3nk#~ Rst Tima Typa Width Aren Stcre Tima End Tima i

1 3.033 PV 0.097 57150189 2.851

-3.436

'2 3.866 BV 0.077 10004129 3.594 4.150 l

I s

i 1

7 1

)

File

C:\\HPCHEM\\1\\ DATA \\EM31471D.D Operator
Marti i

Acquired 8-May )5 1:02 pm using AcqMethod EM31492 Instrument :

5972 - 33 Sample Name: thermolag 0395-37c Misc Info

(2nd run)

Vial Number: 1 FIGURE 5 Abuncance TIC: EM31471D.D l

i 1.2e+07.2 1

J 1.le+07 t'

le+07,)

i I

l 9000000-i 1

8000000-l l

i 1

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60000001 i

i 5000000 l

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l 40000003 i

I 30000003 -

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i 2000000.'

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2 i

Time-->

10.00 20.d0 30.00

..-. ~ _..

File

C:\\HPCHEM\\1\\ DATA \\EM31471D.D Operator
Marti i

Acquired 8 May 95 1:02 pm using AcqMethod EM31492 Instrument :

5972-- 33 Sample Name: thermolag- 0395-37c Misc-Info

(2nd run)

Vial Number: 1 i

FIGURE 6 Acundance Ion 55.00 (54.70 to 55.70): EM31471D.D 2.58 350000-1 i

300000; 3,

i l

i, l 250000'

]

200000; 150000 il i;

100000; i

l 2j70 50000; e

7 f

O

~

e" Time-->

1.00 2.'00 3.'00 4.'00 5.00 Acundance Ion 69.00 (68.70 to 69.70): EM31471D.D I

350000; 3000002 2.70 i

2500002 l

)

2000002 150000_

100000_

i 50000_

2.54 0 ~^

~N

\\ \\

t Time-->

1.00 2.'00 3.00 4.00 5.00

Information from D ta Filo:

C:\\HPCHEM\\1\\ DATA \\EM31471D.D Filo Oparctor

Mnrti 8 May 95 1:02 pm using AcqMethod EM31492 Acquired Scmple Name: thermolag 0395-37c Misc Info
(2nd run)

Vial Number: 1 Saarch Libraries:

C:\\ DATABASE \\NBS75K.L Minimum Quality:

0 Unknown Spectrum:

Apex Integration Params: AutoIntegrate Pk#

RT Areat Library /ID Ref#

CAS#

Qual 1

0.14 1.08 C:\\ DATABASE \\NBS75K.L Hydrazine, (1-methylpropyl)-

832 030924-14-2 30 2-Propanol, 1- (2 -methoxy-1-methyle 9238 020324-32-7 27 4-Ethoxyamphetamine 17479 000000-00-0 22 2

1.50 4.40 C:\\ DATABASE \\NBS75K.L No matches found 3

1.65 1.45 C:\\ DATABASE \\NBS75K.L No matches found 4

1.87 0.31 C:\\ DATABASE \\NBS75K.L 2-Propenal, 2-methyl-62430 000078-85-3 50 Furan, 2,3-dihydro-62438 001191-99-7 46 Butanal 62486 000123-72-8 43 5

2.05 0.33 C:\\ DATABASE \\NBS75K.L Furan, 2-methyl-62666 000534-22-5 91 Furan, 2-methyl-463 000534-22-5 76 Furan, 2-methyl-62665 000534-22-5 64 6

2.57 0.28 C:\\ DATABASE \\NBS75K.L j

2-Propenoic acid, ethyl ester 63318 000140-88-5 67 2-Propenoic acid, ethyl ester 63319 000140-88-5 78 2-Propenoic acid, ethyl ester 63317 000140-88-5 72 7

2.70 0.70 C:\\ DATABASE \\NBS75K.L 2-Propenoic acid, 2-methyl, methy 1484 000080-62-6 58 2-Propenoic acid, 2-methyl, 3-hyd 8333 002761-09-3 50 2-Butenoic acid, methyl ester, (E) 1458 000623-43-8 38 8

3.06 0.15 C:\\ DATABASE \\NBS75K.L Pyridine 62632 000110-86-1 95 Pyridine 62633 000110-86-1 76 i

Pyridine 62631 000110-86-1 76 9

3.16 0.12 C:\\ DATABASE \\NBS75K.L 1-Penten-3-yne, 2-methyl-62647 000926-55-6 50 1H-Pyrrole, 1-methyl-62656 000096-54-8 46 1H-Pyrrole, 2-methyl-444 000636-41-9 43 C:\\HPCHEM\\1\\ DATA \\EM31471D.D Mon May 08 13:44:24 1995 Page 1

I Pk#

RT Aran %

Librcry/ID R3f#

CAS#

Quel

)

,10 4.64 0.66 C:\\ DATABASE \\NBG75K.L Pyridine, 3-methyl-63044 000108-99-6 97 l

Pyridine, 3-methyl-981 000108-99-6 94 Pyridine, 3-methyl-63046 000108-99-6 91 I

i 11 4.78 0.16 C:\\ DATABASE \\NBS75K.L Benzene, 1,2-dimethyl-63706 000095-47-6 38

)

Benzene, 1,2-dimethyl-63705 000095-47-6 38 i

p-Xylene 2032 000106-42-3 38

}

12 5.84 0.07 C:\\ DATABASE \\NBS75K.L Pyridine, 2,5-dimethyl-2046 000589-93-5 93 Pyridine, 2,5-dimethyl-63719 000589-93-5 90 l

Benzenamine, 3-methyl-63727 000108-44-1 68

[

i 13 6.53 0.06 C:\\ DATABASE \\NBS75K.L Pyridine, 3-ethenyl-1970 001121-55-7 87 Pyridit.e, 2-ethenyl-1972 000100-69-6 74 Pyridine, 4-ethenyl-1971 000100-43-6 64 l

I 14 6.69 0.37 C:\\ DATABASE \\NBS75K.L Pyridine, 3,5-dimethyl-2047 000591-22-0 95 j

Pyridine, 3,5-dimethyl-63720 000591-22-0 91 j

Pyridine, 3,4-dimethyl-2050 000583-58-4 91 l

15 7.44 0.06 C:\\ DATABASE \\NBS75K.L Pyridine,'2-ethyl-6-methyl-3834 001122-69-6 43 6H-Purine, 5,7-dihydro-6-(1-methyl 17628 056247-56-4 35 l

1H-Pyrrole, 2,3,5-trimethyl-2225 002199-41-9 27 16 8.20 0.08 C:\\ DATABASE \\NBS75K.L Pyridine, 2,3,5-trimethyl-3839 000695-98-7 91 i

Pyridine, 2,3,6-trimethyl-3822 001462-84-6 81 Pyridine, 2,3,6-trimethyl-64607 001462-84-6 81 l

17 8.49 0.09 C:\\ DATABASE \\NBS75K.L Pyridine, 3-ethyl-5-methyl-3821 003999-78-8 94 Pyridine, 5-ethyl-2-methyl-64621 000104-90-5 90 i

Benzenamine, 2,6-dimethyl-64611 000087-62-7 81 l

l 18 8.69 0.21 C:\\ DATABASE \\NBS75K.L

{

4-Aminostyrene 3652 001520-21-4 83 l

Pyridine, 5-ethenyl-2-methyl-3656 000140-76-1 76 t

Benzoic acid, 2,5-dimethyl,

(2,4-37433 055000-48-1 59 j

19 8.86 1.01 C:\\ DATABASE \\NBS75K.L 1H-Pyrrole-2-carboxaldehyde, 1-met 63814 001192-58-1 50 2,6-Pyridinediamine 2190 000141-86-6 47 l

3,4-Pyridinediamine 2193 000054-96-6 45

)

f 20 9.54 0.16 C:\\ DATABASE \\NBS75K.L i

1H-Pyrrole, 2,3,4,5-tetramethyl-4056 001003-90-3 94

)

1H-Pyrrole, 3-ethyl-2,4,5-trimethy 65853 000520-69-4 37 Pyrazine, 5-butyl-2,3-dimethyl-67853 015834-78-3 23 C:\\HPCHEM\\1\\ DATA \\EM31471D.D Mon May 08 13:44:42 1995 Page 2

Fk#

RT Aran %

Library /ID Rof#

CAS#

Quni

,21 10.62 0.26 C:\\ DATABASE \\NBS75K.L Ethanone, 1-(1-methyl-1H-pyrrol 64728 000932-16-1 78 1H-Pyrrole 3-ethyl-2,4-dimethyl-64741 000517-22-6 56 1H-Pyrrole, 2-ethyl-3,5-dimethyl-4057 032990-59-3 56 22 :11.62 0.07 C:\\ DATABASE \\NBS75K.L Pentanedioic acid, 2-methyl, mono 12301 072088-36-9 32 Butanedioic acid, 2,2-dimethyl, d 16117 049827-44-3 27 Dimethyl ethylbutane-1,4-dioate 16107 000000-00-0 27 23 12.23 0.21 C:\\ DATABASE \\NBS75K.L Pentanedioic acid, diethyl ester 19778 000818-38-2 87 Pentanedioic acid, diethyl ester 69155 000818-38-2 72 Pentanedioic acid, diethyl ester 69156 000818-38-2 72 24 12.98 0.15 C:\\ DATABASE \\NBS75K.L Cyclohexasiloxane, dodecamethyl-56711 000540-97-6 90 Acetic acid, (bis [ (trimethylsilyl) 49839 053044-27-2 53 1,3,5,7,9-Pentaethylcyclopentasilo 51267 017995-44-7 32 25 13.13 0.07 C:\\ DATABASE \\NBS75K.L 2H-Quinolizin-3-ol, octahydro, tr 11200 015769-36-5 38 2-(Diethylamino)-3-methylcycloprop 11187 091295-98-6 38 Diethyl isopropylidenemalonate 69708 006802-75-1 35 26 15.08 0.09 C:\\ DATABASE \\NBS75K.L Propanamide 62531 000079-05-0 46 Methanesulfonamide, N,N-dimethyl-4001 000918-05-8 38-dl-3-Aminobutyric acid 1815 002835-82-7 35 27 15.76 0.50 C:\\ DATABASE \\NBS75K.L

(

3-Isopropoxy-1,1,1,7,7,7-hexamethy 60503 071579-69-6 37 1-(2,4-Bis (trimethylsilyloxy)pheny 58102 000000-00-0 27 Tetrasiloxane, 3,5-diethoxy-1,1,1, 59390 072439-78-2 22 28 17.31 0.05 C:\\ DATABASE \\NBS75K.L Julolidine 16010 000479-59-4 32 1,2,3,7-Tetramethylindole 15993 000000-00-0 25 4- (2-Hydroxyphenyl) pyrimidine 15723 068535-55-7 25 29 17.73 0.36 C:\\ DATABASE \\NBS75K.L j

Cyclopentanone, dimethylhydrazone 4509 014090-60-9 27 1,3,5-Benzenetriol 64864 000108-73-6 22 Thiazole, 2,4-dimethyl-5-propyl-11176 041981-70-8 22 30 17.90 0.12 C:\\ DATABASE \\NBS75K.L

. delta.2-Tetrazaboroline, 5-ethyl-4392 020534-01-4 38 1-Ethylamino-1-butylcyclohexane 18625 000000-00-0 38 3H-Pyrazol-3-one, 1,2-dihydro-1,2, 4441 003201-26-1 22 31 18.05 0.12 C:\\ DATABASE \\NBS75K.L N,N-Diethyltrifluoroacetamide 14830 000360-92-9 38 Benzene, 1-chloro ( 2, 2 -dichloro-27960 054965-40-1 25 1-Nonanone, 1- ( 2 -thienyl) -

28638 059782-24-0 22 i

C:\\HPCHEM\\1\\ DATA \\EM31471D.D Mon May 08 13:45:06 1995 Page 3 4

Pk#

RT

Arant-Library /ID Raf#

CAS#

Qual 32 18.24 0.40 C:\\ DATABASE \\NBS75K.L Benzeneethanamine, N-[(pentafluoro 60339 055429-13-5 43 Phenethylamine, N-methyl. beta.,3, 74238 010538-85-9 43 i

Benzeneacetic acid,. alpha.,3;4-tr 57997 037148-65-5 38 33' 19.89 13.30'C:\\ DATABASE \\NBS75K.L Octicizer 50542 001241-94-7 93 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 59 l

2 - ( 4 - Cyanophenyl) dime thylaminom 34091 000000-00-0 45 l

34 20.23 22.91 C:\\ DATABASE \\NBS75K.L l

Octicizer 50542 001241-94-7 90 7-Amino-2,3-dihydro-5-phenyl-1H-1,

_34112 004928-02-3 53 2 - ( 4 - Cyanophenyl ) dime t hylaminom 34091 000000-00-0 42 l

35 20.39 1.34 C:\\ DATABASE \\NBS75K.L 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 35 Octicizer 50542 001241-94-7 20 Benzenamine, ar,ar-dibromo-33621 050307-05-6 16 i

36 20.74 4.62 C:\\ DATABASE \\NBS75K.L No matches found l

37 21.07 0.90 C:\\ DATABASE \\NBS75K.L 7-Amino-2,3-dihydro-5-phenyl-1H-1, -34112 004928-02-3 49 Octicizer 50542 001241-94-7 38 2 - ( 4 - Cyanophenyl ) dime thylaminom 34091 000000-00-0 38 i

38 -21.59 2.47 C:\\ DATABASE \\NBS75K.L Octicizer 50542.001241-94-7 66 l

7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3-47 2-Propanol, 1-(2-(2-methoxy-1-meth 24251 020324-33-8 27 39 21.92 1.84 C:\\ DATABASE \\NBS75K.L 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 35 Butanamide, 3-methyl-1621 000541-46-8 30 Butane, 2-methoxy-854 006795-87-5 30 40 22.12 1.26 C:\\ DATABASE \\NBS75K.L 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 27 Methyl 16-methoxyheptadecanoate 44818 000000-00-0 27 Octicizer 50542 001241-94-7 25 41 22.30 1.13 C:\\ DATABASE \\NBS75K.L Trisiloxane, 1,1,1,5,5,5-hexamethy 52459 003555-47-3 14 1,1,1,5,7,7,7-Heptamethyl-3,3-bis (

56714 038147-00-1 10 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 10 42 24.05 0.61 C:\\ DATABASE \\NBS75K.L Octicizer 50542 001241-94-7 35 2,4 (1H,3H) -Quinolinedione, 3-benzo 49822 070611-42-6 32 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 27 43 24.31 1.10 C:\\ DATABASE \\NBS75K.L 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 47 Octicizer 50542 001241-94-7 25 2,4,6,8,9,10-Hexathiatricyclo[3.3.

50037 057274-38-1 18 C:\\HPCHEM\\1\\ DATA \\EM31471D.D Mon May 08 13:45:24 1995 Page 4

Pk#

RT Arac %

Library /ID Raf#

CAS#

Qugl 44 24.98 1.59 C:\\ DATABASE \\NBS75K.L 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 38 2-Propanol, 1-(2-(2-methoxy-1-meth 24251 020324-33-8 35 Octicizer 50542 001241-94-7 35 45 25.46 0.68 C:\\ DATABASE \\NBS75K.L 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 43 i

Octicizcr 50542 001241-94-7 42 2-Propanol, 1-[2-(2-methoxy-1-meth 24251 020324-33-8 22 46 25.65 0.66 C:\\ DATABASE \\NBS75K.L 3-(2-Hydroxy-6-methylphenyl)-2-met 36963 000000-00-0 47 Octicizer 50542 001241-94-7 45 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 43 47 25.94 0.53 C:\\ DATABASE \\NBS75K.L Octicizer 50542 001241-94-7 70 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 43 2-Propanol, 1 - [1-me thyl ( 2 -prope 68438 055956-25-7 18 48 26.35 1.12 C:\\ DATABASE \\NBS75K.L Phosphoric acid, tris (3-methylphen 51124 000563-04-2 99 Phosphoric acid, tris (methylphenyl 51123 001330-78-5 94 Phosphoric acid, tris (methylphenyl 73955 001330-78-5 93 49 26.97 0.42 C:\\ DATABASE \\NBS75K.L Phosphoric acid, tris (3-methylphen 51124 000563-04-2 97 Phosphoric acid, tris (methylphenyl 73955 001330-78-5 95 Phosphoric acid, tris (methylphenyl 51123 001330-78-5 78 50 27.16 0.32 C:\\ DATABASE \\NBS75K.L Phosphoric acid, triphenyl ester 73338 000115-86-6 99 Phosphoric acid, triphenyl ester 73337 000115-86-6 92 Phosphoric acid, triphenyl ester 46311 000115-86-6 83 51 27.50 2.69 C:\\ DATABASE \\NBS75K.L Occicizer 50542 001241-94-7 90 7-Amino-2,3-dihydro-5-phenyl-1H-1, 34112 004928-02-3 59 2 - ( 4 - Cyanophenyl) dimethylaminom 34091 000000-00-0 59 52 27.70 0.76 C:\\ DATABASE \\NBS75K.L Isothiazole, 3-methyl-5-phenyl-68481 001732-45-2 37 2H-1-Benzopyran-2-one, 7-amino-4-m 16440 026093-31-2 28 Oxycarboxin 71900 005259-88-1 25 53 28.20 0.92 C:\\ DATABASE \\NBS75K.L Propanoic acid, 2-hydroxy-2-methyl 5790 000080-55-7 47

{

2-Butanol, 3-methoxy-1908 053778-72-6 43 Butanamide, 3-methyl-1621 000541-46-8 38 54 28.37 0.39 C:\\ DATABASE \\NBS75K.L Butane, 2-methoxy-854 006795-87-5 43 Propanoic acid, 2-hydroxy-2-methyl 3494 002110-78-3 38 i

Pentanamide, 4-methyl-3136 001119-29-5 38 C:\\HPCHEM\\1\\ DATA \\EM31471D.D Mon May 08 13:45:42 1995 Page 5

~

Pk#

RT Arce%

Library /ID Raf#

CAS#

Quni

.55 29.79 0.09 C:\\ DATABASE \\NES75K.L Pregna-4,6-dieno-3,20-dione,

2. alp 56634 005234-56-0 27 10H-Phenoxaphesphine, 8-fluoro 39085 037041-13-7 25 4H-1-Benzepyran-2-carboxylic acid, 39266 030095-84-2 16 56 30.65 0.14 C:\\ DATABASE \\NBS75K.L

. alpha.-D-Xylo-Hex-5-enofuranose, 19338 007284-07-3 10 Hexane, 1-ethoxy-65280 005756-43-4 10 8-Hydroxycarvotanacetone 14600 007712-46-1 9

57 31.14 5.94 C:\\ DATABASE \\NBS75K.L Phosphoric acid, tris (3 -methylphen 51124 000563-04-2 99 Phosphoric acid, tris (methylphenyl 73955 001330-78-5 93 Phosphoric acid, tris (methylphenyl 51123 001330-78-5 91 58 31.54 0.37 C:\\ DATABASE \\NBS75K.L Sarpagan-16-carboxylic acid, 3,17-52356 053632-75-0 22 Benzeneethanamine 64604 000064-04-0 14 Bikaverin 52326 033390-21-5 11 59 31.73 4.03 C:\\ DATABASE \\NBS75K.L Phosphoric acid, tris (3-methylphen 51124 000563-04-2 99 j

Phosphoric acid, tris (methylphenyl 51123 001330-78-5 94 Phosphoric acid, tris (methylphenyl 73955 001330-78-5 93 60 31.89 0.45 C:\\ DATABASE \\NBS75K.L Acetophenone, 2',4'-dimethoxy-3'-m 21229 060512-80-3 30 9H-Fluorene, 9,9-dimethyl-21436 004569-45-3 22 9H-Fluoren-9-imine 17504 004440-33-9 18 i

61 32.21 0.37 C:\\ DATABASE \\NBS75K.L Sarpagan-16-carboxylic acid, 3,17-52356 053632-75-0 22 Morphinan, 6,8a-etheno,-3-acetoxy-52348 000000-00-0 18 Acridine 68683 000260-94-6 15 62 32.38 1.90 C:\\ DATABASE \\NBS75K.L Phosphoric acid, tris (3-methylphen 51124 000563-04-2 98 Phosphoric acid, tris (methylphenyl 73955 0013?0-78-5 96 Phosphoric acid, tris (methylphenyl 51123 001330-78-5 93 63 32.57 0.62 C:\\ DATABASE \\NBS75K.L 4

Ethanol, 2-[4-(1,1-dimethylethyl)p 21346 000713-46-2 22 Acetophenone, 2',4'-dimethoxy-3'-m 21229 060512-80-3 22 2',4'-Dimethoxy-3'-methylpropiophe 24862 077942-13-3 14 64 32.72 1.61 C:\\ DATABASE \\NBS75K.L 2,2,6,6-Tetrachloro-1,5-dioxa-2,6-52155 063503-14-0 23 Morphinan, 6,8a-etheno,-3-acetoxy-52348 000000-00-0 22 Sarpagan-16-carboxylic acid, 3,17-52356 053632-75-0 22 65 33.08 1.62 C:\\ DATABASE \\NBS75K.L Butanamide, 3-methyl-1621 000541-46-8 22 2,3,3-Trimethyl-2-pentanol 5510 023171-85-9 22 Ethane, 1-bromo-2-ethoxy-10074 000592-55-2 22 C:\\HPCHEM\\1\\ DATA \\EM31471D.D Mon May 08 13:45:59 1995 Page 6

Pk#

RT Arsc%

Librcry/ID Rof#

CAS#

Quni

.66 33.32 1.50 C:\\ DATABASE \\NBS75K.L 2-Propanol, 1- (2 -me thoxypropoxy) -

9233 013429-07-7 38 2-Propsnol, 1-(1-methyl-2-(2-prope 16196 055956-25-7 38 Butanamide, 3-methyl-1621 000541-46-8 38 4

67 33.52 3.46 C:\\ DATABASE \\NBS'T5K.L 2 - Propanol, 1 - ( 2 - me thoxypropoxy) -

9233 013429-07-7 14 1-Butanol, 3-methoxy-1922 002517-43-3 14 Butanamide, 3-methyl-1621 000541-46-8 14 68 33.95 0.87 C:\\ DATABASE \\NBS75K.L 1-Propanol, 2-(2-methoxy-1-methyle 9239 055956-21-3 43 2 - Propanol, 1 - [ 2 - ( 2 -me thoxy-1 -me th 24251 020324-33-8 37 Methane, diethoxy-1915 000462 95-3 27 69 34.33 0.62 C:\\ DATABASE \\NBS75K.L 1H-Benzimidazole, 5-chloro-2-(1-me 21182 004886-29-7 20 Acridine 68684 000260-94-6 11 Acridine 68685 000260-94-6 11 70 34.76 0.28 C:\\ DATABASE \\NBS75K.L Bikaverin 52326 033390-21-5 38 p-Quinquiphenyl 52398 000000-00-0 18 1,l':3',l:3,l:3,l'-Qu 52399 016716-13-5 18 71 35.23 0.08 C:\\ DATABASE \\NBS75K.L Pentane, 2-methoxy-1778 006795-88-6 30 2-Propanol, 1- (1-methyl ( 2 -prope 68438 055956-25-7 27 2,4,6,8,9,10-Hexathiatricyclo(3.3.

50037 057274-38-1 25 72 39.57 0.34 C:\\ DATABASE \\NBS75K.L 2-Propanol, 1-(2-methoxy-1-methyle 9238 020324-32-7 38 Butane, 2-methoxy-854 006795-87-5 35 Propanoic acid, 2-hydroxy-2-methyl 3494 002110-78-3 35 C:\\HPCHEM\\1\\ DATA \\EM31471D.D Mon May 08 13:46:12 1995 Page 7

f Area Percent Report -- Sorted by Signal l

~

j Information from' Data File:

C:\\HPCHEM\\1\\ DATA \\EM31471D.D File Operator

Marti 8.May 95 1:02 pm using AcqMethod EM31492:

Acquired Snmple Name: thermolag 0395-37c MiscEInfo

(2nd'run) l Vial Numbert 1 l

CurrentMeth: C:\\HPCHEM\\1\\ METHODS \\EM31492.M l

Retention Time.

Area Area %

Ratio %

Total-Ion. Chromatogram 0.140 92722369 1.082 4.723 1.495 377302691

'4.403 19.218 l

1.657 124284126 1.450 6.330 1.871 26406527 0.308 1.345 2.050 28477981 0.332 1.451 2.578 24074246 0.281 1.226 2.698 60276495 0.703 3.070 l

3.058 13211834 0.154 0.673 L

3.154 10119389 0.118 0.515 I

4.638 56653564 0.661 2.886 4.777 14011580 0.164 0.714 5.844

'5834804 0.068 0.297 6.528 5096275 0.059 0.260 6.683 31886156 0.372 1.624 7.443 4983175 0.058 0.254 i

8.197 7042570 0.082 0.359 8.489 7286336 0.085 0.371 8.695 18230036 0.213 0.929 8.861 86836671 1.013 4.423 l-9.542 13358226 0.156 0.680 10.624 21907773 0.256 1.116 11.630 5640899 0.066 0.287 12.235 186*0730 0.210 0.918 12.987 1274 725 0.149 0.649 l

13.128 L.

7453 0.074 0.322 15.077 7925161 0.092 0.404 l

15.760 42928444 0.501 2.187 17.310-4197339 0.049 0.214 17.725 30486288 0.356 1.553 17.893 10339636 0.121 0.527 18.048 9924107 0.116 0.505 18.239 34576125 0.403 1.761 19.885 1140080553 13.305 58.070 10.23d 1963278058 22.911 100.000 20.388 114747435 1.339 5.845 l

C:\\HPCHEM\\1\\ DATA \\EM31471D.D Mon May 08 13:43:56 1995 Page 1

l

. Area Percent Report -- Sorted by Signal 3

Information from Data File:

I' File

C:\\HPCHEM\\1\\ DATA \\EM31471D.D operator.
Marti 8 May 95 1:02 pm using AcqMethod EM31492 i

Acquired Stmple Name: thermolag 0395-37c Misc Info

(2nd run)

' Vial Number: 1 CurrentMeth: C:\\HPCHEM\\1\\ METHODS \\EM31492.M Retention Time Area Area %

Ratio %

.20.735 396014951 4.621 20.171 l

21.069 76964275 0.898 3.920 21.593

.211678932 2.470 10.782 21.910

'157992826 1.844 8.047 j

22.115 107867502 1.259 5.494 22.302 96593679 1.127 4.920 3

24.056 51858646 0.605 2.641 i

24.311 94559977 1.104' 4.816 24.978 136006512 1.587 6.928 25.455 58452866 0.682 2.977'

~

.25.650 56829877 0.663 2.895 25.938 45328226 0.529 2.309

)

26.358 95901695 1.119 4.885 i

26.976 35700684 0.417 1.818 27.160 27420393 0.320 1.397 27.496 230192488 2.686 11.725

[

27.706 65082688 0.760 3.315 l

28.196 79075966 0.923 4.028 28.369 33750458 0.394 1.719 29.793 7314431 0.085 0.373

'~

30.651 12384558 0.145 0.631 31.134 508619835 5.936 25.907 l

31.544 31367955 0.366 1.598 31~. 73 7 345037129 4.027 17.575 31.888 38957251 0.455 1.984 32.204 31981791 0.373 1.629 32.374 162852128 1.900 8.295 32.566 52874565 0.617 2.693 32.723 138104414 1.612 7.034 l

'33.080 138933784 1.621 7.077 33.312 128192081 1.496 6.529 4

33.524 296709585 3.463 15.113

{

33.948 74164746 0.865 3.778

.34.326 52854560 0.617 2.692

-34.759 24222641 0.283 1.234 35.227 6807583 0.079 0.347

/

4 C:\\HPCHEM\\1\\ DATA \\EM31471D.D Mon May 08 13:43:58 1995 Page 2

j l

Area Percent Report'-- Sorted by Signal l

Information from Data File:

C:\\HPCHEM\\1\\ DATA \\EM31471D.D File Operator

Marti 8 May 95 1:02 pm using AcqMethod EM31492 Acquired SOmple Name: thermolag 0395-37c Misc Info _ : (2nd run)

Vial Number: 1 CurrentMeth: C:\\HPCHEM\\1\\ METHODS \\EM31492.M Retention Time Area Area %

Ratio %

39.568 29192820 0.341 1.48T l

l l

i l

ll' l

I l

C:\\HPCHEM\\1\\ DATA \\EM31471D.D Mon'May 08 13:44:00 1995 Page 3

Eon

99. Le)(o) (Wd.T@ 8o ME.Y@) : L6MZ7J7hlo).lg

~

~

th;rmolcg 0395-37c

.PsaA#

rot Time Typ3 Width Arca Stcrt Tim 3 End Tima 1

2.577

. BV 0.048 11671429

.2.444 2.667 2

2.696 W

0.079 1914898 2.667 2.920

g..

,.EM31471D J ' ~~~~~

~"~

~~

g

~

thOrmolcg 0395-37c Pack #

Rst Tim 2

'Typa Width Arco Stcrt Time.

End Tima 1

2.536-BV 0.058 483214 2.484 2.638 i

2 2.700 VV 0.052 9629230 2.638 3.109 t

i l

l l

l l

1

~..

+

I

- File

C:\\HPCHEM\\1\\ DATA \\EM31471E.D Operator
Marti Acquired
23 May 95 10:14 am using AcqMethod EM31492 Instrument :

5972 - 33 Sample Name: Og95-37b 3-4/#.78 N 47 l

Misc. Info Vial Number: 1 FIGURE 7 Aouncance Ion 55.00 (54.70. to 55.70) : EM314'71E.D 700000f l

6000004 i

l i

J 500000J lj i

1 ji.

t 6

i I

400000-300000_

l I

i 200000 l

i l

)

I 100000 j

1 2!65

)

I 4

i i

0 Time-->

1.00 2.00 3.00 4.00 5.00 Abundance Ion 69.00 (68.70 to 69.70) : EM31471E.D 1

700000 1

600000J l

.I 2.66 500000_

i i

4 i'400000J i

)

i 3000002 t

200000~

100000_

0' k -

s Time-->

1.00 2.00 3.00 4.00 5.00

._.. ~.

l l

t File.

C:\\HPCHEM\\1\\ DATA \\EM31471E.D Operator
Marti Acquired
23 May 95 10:14 am using AcqMethod EM31492 Instrument :

5972 - 33 Sample Name: Q495-37b

$#

  • Y >

3 Misc Info Vial Number: 1

  1. O l

tor'F J

l FIGURE 8 ADundance TIC: EM31471E.D l

6500000'l l

16000000 l

1

]

l l

5500000 j

I 1

5000000l 1

l 4500000y i

4 4000000I l

1,3500000.

I

'3000000l l i

i

i 2500000 20000002 l

y I

15000001 i

i,1000000.

i I

500000_

l I-0%

C

'I Time-->

10.00 20.00 30.00

Librcry Sacrchid :.C:\\ DATABASE \\NBS75K.L Quality

93 Pyridina, 3-msthyl-ID Sam /LE 0396-378 ADundance Scan 394 (4.733 min): EM31471E.D (*)

i 91 a

93 8000}

lj li 6000 -

FIGURE 9 -

t I

4000; 39 66 l

)

.1j 32 2000q l

g t.;

Pi k

0,

' l' '

ll '.

lll"d' j

l i,

207 I "

pt/z-->

2'O 4'O 6'O 8'O 1$0 120 ido 150 15d 2d0 Aouncance

  1. 63045: Pyriclne, 3-methyl- (*)

j 9!3 4

8000 J i

3 6000d 4

39

]

66 4000 j

l 92 i

l l

1 2000J 38 i

4 a

.I 15 ll l l

+l' ' '

,l 1

,4 "d

1 6

l i

j 0'

H l'i pt/z-->

20 40 6'O 8'O 100 120 140 160 180 20 i

Library Sacrchtd : C:\\ DATABASE \\NBS75K.L' Quality

96 Pyridin9, 3-msthyl-ID CAkhc 05?S 378 I

ADuncance Scan 389 (4. 673 min) : EM31471E.D

(*)

93 80002-I i

6000 --

FIGURE 10 4000-]

39 66 92 a

1 i

2000j 32 I,

0 207

!--' I l'I' d"I'

! M' 1

O

'O' 6'O 8'O 10 120 140 160 180 200 4'

m/z-->

2'O Aoundance-

  1. 981: Pyridine, 3 - me tnyJ. -

(*)

I j

9'3 i

s 1

i 8000J l

i t

6000_

I I

66 I

4000_

t 39 92 1

il 2000 1

'l i

l 38

!"i i

0

'l I

l

,m/z-->

2'O 4'0' 6'O 8'O 100 id0 140 160 180' 20 i

Library Sacrchid : C:\\ DATABASE \\NBS75K.L Qunlity-

94 Pyridina, 3,5-dimethyl-ID

.S,98194E C395-3?s AbTncance scan 561 (6.724 min): EM3T471E. D (*)

107 I

8000?

60002 44 4

1 I

4000; 32 79 l

39 i

92 j

2000J

{

1 54 66 l

9 3

lllI t!i!II S

.i i

120' 0

i

{/z-->

'20 3'O 40 50 6'O 70 8'O

'9'O 100 lid 120 m

ADuncance

  1. 2047: Pyridine, 3,5-dimethyl- (*)

107 l

8000g 4

6000j l

4 i

I i

.4 40002 39 79

'l I

I i

i

~

92 2000-27 51 l

l l

65

)

54

, "u

'Il'.

-,l 91 0

l/z-->

t >

i-

,m 20 3'O 40 50 60 7'O 8'O 9'0' 100 lio 120 FIGURE 11

=

Library Sacrch;d : C:\\ DATABASE \\NBS75K.L

'Qunlity

64 i

ID

w Pyridina, 2,5-dimethyl-CAM /Lc o5?S- *B Acundance scan 581 (6.963 min): EM31471E.D (*)

1 4'4 105 d

107 8000-32 6000

]

~

4000 79 1

3 i

3, I

!ij t

0 2000 l'

J em l

l l.

lt il 281 1

i!

0

. 't l a[

'l l l1 i j i

i i

C i

I o

l m/z-->

5'O 100 150 200 250 Abundance

  1. 2046: Pyridine, 2,5-dimethyl-(*)

107 l

8000$

i i

106 6000$

[

4 40001 39 79 2000 27 d

I i

1 d

kh l

o

m/z-->

5'O

'L O O 150 200 250 j

FIGURE 12 i

l

Library S3 arched : C:\\ DATABASE \\NBS75K.L Quality

68 ID
PtntenIdioic ccid, disthyl GctGr SA/N2s 0399 '313 puncance scan 1022 (12.221 min) : EM31471E.D (*)

I j

143 l

4 80001 a

114 87 j

i l

6000i 42 l

-i

.J i.

r 3

4000,

9 l

h 67

]

39!

i 2000-lI 95 I -

-l 168 i

155 ll'I' di l lll

.I 't!

; l' 207 j

l

' "ll nl l

l i

0 pt/ z - -_ >

2'O 40 6'O 8'O 1d 1$0 140 180 180.

20 ADuncance

  1. 19775: Fentaned101c acid, diethyl ester (*)

143 8000_

29 6000_

114 j

)

42 87 4000 J l'

j

{

i i

'l i

2000.

l

)

I i

i l

I, 73 101 l

l i

15 j

g, i,,

1,1 l/z-0; i

20 40 60 80 100 120 140 160 180 200

'pt FIGURE 13

Libr ry SacrChsd : C:\\ DATABASE \\NBS75K.L Quclity

91 1H-Pyrrolo, 2,3,4,5-totrcm^2thyl-ID 94mA5 a396-372 ADuncance Scan 794 (9.502 min): EM31471E.D (*)

122 8000-6000.

108 i

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4 ATTACHMENT No. 3 UPDATED GENERIC LETTER 86-10 EVALUATION OF i

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