ML20094P423

Pyrolysis Gas Chromatography Analysis of 10 Thermo-Lag Fire Barrier Samples

ML20094P423
Person / Time
Site:	Comanche Peak
Issue date:	09/29/1995
From:	Freeman W, Keller T NUCON, INC.
To:
Shared Package
ML20094P422	List: ML20094P419 ML20094P423
References
NUCON-06TU935-0, NUCON-06TU935-01, NUCON-6TU935, NUCON-6TU935-1, NUDOCS 9511290139
Download: ML20094P423 (5)

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NUCON Internotionol, Inc. TELEPHONE: (614) 846-5710 OUTSIDE OHIO: 1 800-992-5192 TELEX: 6974415  ;

. P.O. BOX 29151 7000 HUNTLEY ROAD '

COLUMBUS. OHIO 43229 U.S.A. FAX: (614) 431-0858 i  ! PYROLYSIS GAS CHROMATOGRAPHY ANALYSIS OF 10 THERMO-LAG FIRE BARRIER SAMPLES 4 Performed For:

Texas Utilities Electric

! Comanche Peak SES .

FM56-5 Miles N.W. of Glen Rose TX 76043 d  !

P. O. Number S 0164511601 29 September 1995 1

l Dictribution ,

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Texas Utilities: Obaid Bhatty

NEI

Biff Bradley (1)

NUCON: 06TU935 Master File (1)

Lab (1) i

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NUCON 06TU935/01 TELEPHONE: (614) 846-5710

- - NUCON Intemationof, Inc. OUTSIDE OHIO: 1-800-992 5192

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' TELEX: 6974415 P.O. BOX 29151 7000 HUNTLEY ROAD FAX: (614) 4310858 COLUMBUS. OHIO 43229 U.S.A.

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Prepared By Reviewed By OriginalIssue j

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W. P. Freeman T. S Keller

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!; I. ABSTRACT  ;

Inspection of the pyrograms of 10 Thermo-Lag fire barrier samples indicated that eight of ,

the samples were similar in chemical composition. Two samples labeled "Flexi-Blanket" did not generate pyrograms typical of Thermo-Lag samples.

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

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III. DESCRIPTION OF METHOD The samples were compared by pyrolysis gas chromatography using ASTM D3452 as a general guide. A Hewlett-Packard model 5890 series II gas chromatograph equipped with 1

a Hewlett Packard model 5972 mass selective detector was used to generate chromatograms of the pyrolysis products. Pyrolysis of the Thermo-Lag samples were ,

l performed with a CDS pyroprobe mounted in an independently heated interface attached i

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 ,

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 The ten pyrograms (totalion chromatograms) for each of the ten Thermo-Lag samples are

' shown in Figures 1,3,5,7,9,11,' 13,15,17 and 19. The extracted ion chror6atograms using the acrylate base ion m/e of 55 common to ethyl acrylate (EA) and m/e of 69 4

common to methyl methacrylate (MMA) for each sample are shown in Figures 2, 4, 6, 8,  ;

10,12,14,16,18 and 20. The sample name at the top of each figure is the NUCON Log

1. I. D. Samples 0795-7A-J are further identified in Table 2 along with their respective EA/MMA area ratios. Each set of figures is followed by a library search, which identifies some of the major peaks from each sample's pyrogram, and a summary area percent report.

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I V. DISCUSSION OF RESULTS .

The average extracted ion area ratio for EA/MMA of 1.23 0.09 ( a) shown in Table -

2 for the eight samples 0795-A-H is consistent with the average area ratio of 1.3' O.2 l

i' ( 20) obtained from 6ther Thermo-Lag samples tested under the NEI generic testing  !

progmm. The EA/MMA ratio of 2.68 for sample 0795-71 and 2.48 for sample 0795-7J are not consistent with other Thermo-Lag samples tested.

The extracted ion chromatograms shown in Figure 2 for sample 0795-7A, a conduit sample, have an EA/MMA ratio of 1.29. Pyridine compounds identified in the pyrogram l

(Figure 1) are 3-methyl pyridine, 3, 5-dimethyl pyridine, 2, 3, 5-trimethyl pyridine, 3-p ethyl-5-methyl pyridine and 5-ethenyl-2-methyl pyridine. Othe key components identified in the pyrogram are 2,3,4,5-tetramethyl-lH-pyrrole, pentanedioic acid diethyl ester,

triphenyl phosphate, octicizer and tris (methylphenyl) phosphate.

The extracted ion chromatogams shown in Figure 4 for sample 0795-7B, a panel sample, l  ;

have an EA/MMA mtio of 1.25. Pyridine compounds identified in the pyrogram (Figure L  :

i 3) are pyridine, 3-methyl pyridine, 4-methyl pyridine, 3, 5-dimethyl pyridine, 2-ethyl '

methyl pyridine, 2, 3, 5-trimethyl pyridine, 3-ethyl-5-methyl pyridine and 5-ethenyl  :

methyl pyridine. Other key components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole, pentanedioic acid diethyl ester and tris (methylphenyl) phosphate.

The extracted ion chromatograms shown in Figure 6 for sample 0795-7C, a panel sample, '

have an EA/MMA ratio of 1.11. Pyridine compounds identified in the pyrogram (Figure i

5) are 3-methyl pyridine and 3,5-dimethyl pyridine. Other key components identified are 2, 3, 4, 5-tetramethyl-1H-pyrrole (visual inspection), pentanedioic acid diethyl ester .

(visual inspection), octicizer and tris (methylphenyl) phosphate.

i The extracted ion chromatograms shown in Figure 8 for sample 0795-7D, a panel sample, I have an EA/MMA ratio of 1.22. Pyridine compounds identified in the pyrogram (Figure

7) are 3-methyl pyridine and 3, 5-dimethyl pyridine (visual inspection). Other key j

components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole, pentanedioic acid diethyl '

ester, octicizer and tris (methylphenyl) phosphate.

f The extracted ion chromatograms shown in Figure 10 for sample 0795-7E, a panel sample, ,

have an EA/MMA ratio of 1.34. Pyridine compounds identified in the pyrogram (Figure i 9) are pyridine, 3-methyl 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- '

2 1H-pyrrole, pentanedioic acid diethyl ester, octicizer and tris (methylphenyl) phosphate.

The extracted ion chromatograms shown in Figure 12 for sample 0795-7F, a conduit i sample, have an EA/MMA mtio of 1.09. Pyridine compounds identified in the pyrogram i

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< (Figure 11) are 3-methyl pyridine and 4-methyl pyridine. Other key components are 2, 3, 4, 5-tetramethyl-1H-pyrrole, pentanedioic acid diethyl ester and octicizer (visual inspection). ,

The extracted ion chromatograms shown in Figure 14 for sample 0795-7G, a panel sample, have an EA/MMA ratio of 1.24. Pyridine compounds identified in the pyrogram (Figure 13) are 3-methyl pyridine and 3, 5-dimethyl pyridine (visual inspection). Other key components identified are 2, 3, 4, 5-tetramethyl-1H-pyrrole (visual inspection),

pentanedioic acid diethyl ester, octicizer and tris (methylphenyl) phosphate.

The extracted ion chromatograms shown in Figure 16 for sample 0795-7H, a conduit sample, have an EA/MMA ratio of 1.36. Pyridine compounds identified in the pyrogram are pyridine, 3-methyl pyridine, 2, 5-dimethyl 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-lH-pyrrole, pentanedioic acid diethyl ester, octicizer and tris (methylphenyl) phosphate.

The extracted ion chromatograms shown in Figure 18 for sample 0795-7I, a "Flexi-Blanket" sample, have an EA/MMA ratio of 2.68. Pyridine compounds identified in the pyrogram (Figure 17) are 3-methyl pyridine (visual inspection) and 3-5-dimethyl pyridine (visual inspection). Other key components identified are 2, 3, 4, 5-tetramethyl-1H-pyrrole, pentanedioic acid diethyl ester, octicizer and tris (methylphenyl) phosphate.

The extracted ion chromatograms shown in Figure 20 for sample 0795-7J, a "Flexi-Blanket" sample, have an EA/MMA ratio of 2.48. Pyridine compounds identified in the pyrogram (Figure 19) are 3-methyl pyridine and 4-methyl pyridine. Other key components identified are pentanedioic acid diethyl ester, octicizer and tris (methylphenyl) phosphate.

In conclusion, the results indicate that eight of the ten Thermo-Lag samples are consistent in terms of chemical composition to other Thermo-Lag samples tested as part of the NEI generic testing program. The remaining two, sample 0795-7I and 7J !abeled "Flexi-Blanket" are not consistent with other Thermo-Lag samples.

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