ML20092M206

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Pyrolysis Gas Chromatography Analysis of 3 Thermo-Lag Fire Barrier Samples
ML20092M206
Person / Time
Site: Crystal River Duke Energy icon.png
Issue date: 06/27/1995
From: Freeman W, Keller T
NUCON, INC.
To:
Shared Package
ML20092M202 List:
References
NUCON-06FP801-0, NUCON-06FP801-02, NUCON-6FP801, NUCON-6FP801-2, NUDOCS 9509290116
Download: ML20092M206 (4)
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N clear Pegulatory Comission Attachment 1

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NUCON Internotionol, Inc. TELEPHONE: 46141 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 PYROLYSIS GAS CHROMATOGRAPHY ANALYSIS OF 3 THERMO-LAG FIRE BARRIER SAMPLES Performed For:

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

P.O. No. N00989AX 27 JUNE 1995 l

l Distributian FPC: W. L. Rossfeld (1)

NEI: Biff Bradley (1)

NUCON: 06FP801 Master File (1)

Lab (1)

NUCON 06FP801/02 9509290116 950922 2 DR ADOCK 0500

U. S. Nucitar RIgulatory Comitssion Atttchment 1 3F0995-11

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Pagi 9 of 11 .

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NUCON 06FP801/02 NUCON Internationol, Inc. TELEPHONE. <614) 846 5710 OUTSIDE OHIO-. 1 800 992 5192 P O. BOX 29151 7000 HUNTLEY ROAD TELEX: 6974415 ,

COLUMBUS. CHIO 43229 U S.A. FAX: 614) 4310858 l

Prepared By Reviewed By Original issue f)'f .] ' '. /_ , ,; . . t; - &L &,-

W. P. Freeman T. S. Keller

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Date Date i

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U. S. Nuclear Regulatory Comisslor. Attachment 1

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, NUCON 06FP80!/02 I. ABSTRACT

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1 l Inspection of the pyrograms of 3 Thermo-Lag fire barrier samples indicated that they are

! all similar in chemical composition.

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

III. DESCRIPTION OF METHOD l 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 l a Hewlett Packard model 5972 mass selective detector was used to generate l chromatograms of the pyrolysis products. Pyrolysi: of the Thermo Lag samples were l 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

quartz tube and placement of the tube in the platinum coil element of the probe. The i 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 her - 1 to 250*C to elute any volatiles which were not entrained in the polymer.

IV. PRESENTATION OF RESULTS The thne pyrograms (total ion chromatograms) for each of the three Thermo Lag samples are shown in Figums 1, 3 and 5. 'Ihe extracted ion chromatograms using the acrylate base ion m/e of 55 common to ethyl acrylate (EA) and m/e of 69 common to methyl methacrylate (MMA) for each sample are shown in Figures 2, 4 and 6. The sample name at the top of each figure is the NUCON Log # I. D. Samples 0495-7A-C 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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1 U. 5. Nuclear Rsgulatory Comission Attachment 1 3Ft395-11 Page 11 of 11 ,

NUCON 06FP801/02 V. DISCUSSION OF RESULTS The average extracted ion area ratio for EA/MMA of 1.22 0.03 ( a) shown in Table 2 is consistent with the average area ratio of 1.4 i0.2 (i20) obtained from other Thermo-Lag samples tested under the NEI generic testing program.

The extracted ion chromatograms shown in Figure 2 for sample 0495-7A, a trowel grade sample, have an EA/MMA ratio of 1.19. Pyridine compounds identified in the pyrogram (Figure 1) are 3-methyl giyridine and 3,5-dimethyl pyridine. Other key components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole, pentanedioic acid diethyl ester, tris (methylphenyl) phosphate and octicizer.

The extracted ion chromatograms shown in Figure 4 for sample Od95-7B, 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 1.24. Pyridine compounds identified in the pyrogram (Figure 3) are 3-methyl pyridine (visual inspection). Other key components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole, pentanedioic diethyl ester, tris (methylphenyl) phosphate, and octicizer.

The extracted ion chromatograms shown in Figure 6 for sample 0495-7C, a i hour rated conduit sample, have an EA/MMA ratio of 1.23. Pyridine compounds identified in the pyrogram (Figure 5) are 3-methyl pyridine. Other key components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole, pentanedioic acid diethyl ester, tris (methylphenyl) phosphate, triphenyl phosphate and octicizer.

In conclusion, the results indicate that the three Thermo-Lag samples are consistent in

terms of chemical composition to other Thermo-Lag samples tested as part of the NEI

! generic testing program.

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