ML20092M205

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Pyrolysis Gas Chromatography Analysis of 5 Thermo-Lag Fire Barrier Samples
ML20092M205
Person / Time
Site: Crystal River Duke Energy icon.png
Issue date: 05/11/1995
From: Freeman W, Keller T
NUCON, INC.
To:
Shared Package
ML20092M202 List:
References
NUCON-06FP801-0, NUCON-06FP801-01, NUCON-6FP801, NUCON-6FP801-1, NUDOCS 9509290115
Download: ML20092M205 (4)
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i U. S. Nuclear Regulatory Comission Attachment 1 3F0995-11 Pagi 4 of 11

' NUCON Internotional, Inc. TELEPHONE. +614) 846-5710 OUTSIDE OHIO. : 800-992 5192 P O BOX 29151 7000 HUNTLEY ROAD TELEr 6374415 COLUMBUS. OHIO 43229 U S.A. . FAX .614 431-0358 ,

. PYROLYSIS GAS CHROMATOGRAPHY ,

ANALYSIS OF 5 THERMO-LAG
FIRE BARRIER SAMPLES i

Performed For:

Florida Power Corporation Crystal River Energy Complex 15760 W. Power Line Street i Crystal River, FL 34428-6708 i

P.O. No. N00989AX 10 May 1995 j Distribution

FPC: W. L. Rossfeld (1) q i

, NEI: Biff Bradley (1)

NUCON: 06FP801 Master File (1) ~

Lab (1) 1 i I NUCON 06FP801/01 4-4

9509290115 950922 ADOCK 05000302

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PDR 1 P. _ _ PDR

U. 5, Huchar Rsgulatory Comission Attachment 1 3F0095-11 Pagi 5 of 11 4

NUCON 06FP801/01 NUCON Internotionol, Inc. TELEPHONE. t614) 846 5710 OU'SICE OHIO 1-800 992 5192 I

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

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f' Prepared By Reviewed By f

1 Original Issue ,

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W. P. Freeman T. /Keller

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U. S Nucisar Regul.aory Connission . Attachment 1 3F0995-11 Pagi 6 of 11 NUCON 06FP801/01 <

I. ABSTRACT Inspection of the pyrograms of 5 Dermo-Lag fire barrier samples indicated that they are all similar in chemical composition.

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

111. 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 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 independently heated interface attached to the injection port of the GC. Analysis involved weighing 1-3 mgs. of sample in a l quartz tube and placement of the tube in the platinum coil element of the probe. The l

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 RESUI TS The five pyrograms for each vi the five Thermo-Lag samples are shown in Figures 1, 3, 5, 7, 9. Figures 2, 4, 6, 8,10 are extracted ion chromatograms using the acrylate base ion m/e of 55 common to ethyl acrylate (EA) and a m/e of 69 common to methyl methacrylate (MMA). The area ratios of these two peaks are shown in Table 2 for each ,

sample. Following these two figures is attached a library search which identifies some of the major peaks for each sample tested and a summary area percent report. j V. DISCUSSION OF RESULTS The average area ratio of 1.35 i0.1 ( a) for EA/MMA shown in Table 2 is consistent with the average ratio of 1.4 i0.1 (i a) obtained from other Thermo-Lag samples.

1

U. S. Nuclear Regulatory Comission

. NUCON 06FP801/01 The extracted ion chromatograms (Figure 2) for sample 0395-4A, a trowel grade sample, have an EA/MMA ratio of 1.28. Pyridine compounds identified in the pyrogram (Figure

1) are 3-methyl pyridine, 2, 5-dimethyl pyridine, 3-ethyl pyridine, 3-ethenyl pyridine, 3, 5-dimethyl pyridine, 2, 3-dimethyl pyridine, 2, 3, 5 trimethyl pyridine. 3-ethyl methyl pyridine and 3-ethenyl-2-methyl pyridine, all consistent with other Thermo-Lag samples. Other key components identified are 2-phenoxy ethanol, pentanedioic acid diethyl ester, triphenyl phosphate, octicizer and trimethylphenyl phosphate.

The extracted ion chromatograms (Figure 4) for sample 0395-4B a 1 hour1.157407e-5 days <br />2.777778e-4 hours <br />1.653439e-6 weeks <br />3.805e-7 months <br /> rated conduit sample have an EA/MMA ratio of 1.25. Pyridine compounds identifed in the pyrogram are pyridine, 3-methyl pyridine, 2, 5-dimethyl pyridine, 2, 3-dimethyl pyridine, 3-ethyl pyridine, 3-ethenyl pyridine, 3, 5-dimethyl pyridine 2, 3, 5-trimethyl pyridine, 3-ethyl methyl pyridine and 5-ethenyl-2-methyl pyridine, all consistent with other Thermo-Lag samples. Other key components identified are 2-phenoxy ethanol, pentanedioic acid diethyl ester and octicizer.

The extracted ion chromatograms (Figure 6) for sample 0395-4C, a 3 hour3.472222e-5 days <br />8.333333e-4 hours <br />4.960317e-6 weeks <br />1.1415e-6 months <br /> rated conduit sample had an EA/MMA ratio of 1.40. Pyridine compounds identifed in the pyrogram (Figure 5) are 3-methyl pyridine, 3, 5 dimethyl pyridine, 2, 3, 5-trimethyl pyridine and 5-ethenyl-2-methyl pyridine, all consistent with other Thermo lag samples. Other key components identified are 2-phenoxy ethanol, pentanedioic acid diethyl ester, and octicizer.

The extracted ion chromatograms (Figure 8) for sample 0395-4D a 1 hour1.157407e-5 days <br />2.777778e-4 hours <br />1.653439e-6 weeks <br />3.805e-7 months <br /> rated panel sample, have an EA/MMA ratio of 1.50. Pyridine compounds identifed in the pyrogram (Figure 7) are pyridine, 2, 5-dimethyl pyridine, 3,5 dimethyl pyridine and 5-ethenyl methyl pyridine, all consistent with other Thermo-Lag samples. Other key components identified are 2-phenoxy ethanol, oentanedioic acid diethyl ester, octicizer and trimethylphenyl phosphate.

The extracted ion chromatograms (Figure 10) for sample 0395-4E, 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 1.34. Pyridine compounds identifed in the pyrogram (Figure 9) are 3-methyl pyridine, 2, 5-dimethyl pyridine, 3-ethyl pyridine, 3, 5-dimethyl pyridine,2, 4-dimethyl pyridine and 5-ethenyl-2-methyl pyridine, all consistent with other Thermo Lag samples. Other key components identifed are 2-phenoxy ethanol, pentanedioic acid diethyl ester and octicizer. _

in conclusion, inspection of the pyrograms for these five 'Thermo-Lag samples indicates that they are consistent with other Thermo Lag samples in terms of chemical composition.

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