ML17353A264

Pyrolysis Gas Chromatography Analysis of 7 Thermo-Lag Fire Barrier Samples.

ML17353A264
Person / Time
Site:	Turkey Point
Issue date:	06/27/1995
From:	Freeman W, Keller T NUCON, INC.
To:
Shared Package
ML17353A263	List: ML17353A262 ML17353A264
References
NUDOCS 9507240040
Download: ML17353A264 (6)

Text

NUCON International, inc. TELEFXPNE; ~614) 846.57,0 OUTSIOE OHIO: 1400 992-5>')

P.O. SOX 29151 7000 HUNTLEY ROAD TELEX: 6974415 GOLUMSUS. OHIO 43229 U.SA. FAX: (614) 431 C.

PYROLYSIS GAS CHROMATOGRAPHY ANALYSIS OF 7 THERMO-LAG FIRE BARlGER SAMPLES Performed For:

Horida Power & Light Company Turkey Point Nudear Pfant 1O MI Zast/O Ho~a Ciy, Palm Drive Horida City, PL 33034 P.O. No. B 95691-5897 22 June 1995 Turkey Point: Frank Busch (1)

NEI: BiffBradley (1)

NUCON: 06IL830 Master File (1)

Lab (1) 9507240040 9507i3 PDR ADOCK 05000250 P PDR NUCON 06FL830/Ol

NUCON 06FL830/01 TELEPHONE: (514) 846.5r1O NUCON International, Inc. OUTSIDE OHIO: 1~992.5192 P.O. BOX 29151 rOOO XUNTLEY HOAO TELEX: 69744>5 COLUMSUS. OHIO 43229 U.S.A. FAX. (014) 431.0S58 Prepared By Reviewed By .

Onginal Issue W. P. Freeman pc~7 T. S. Keller D3 ~- /+5>

Date

NUCON 06FL830/01 I. ABSTRACT Inspection of thc pyzograms of 7 Thermo-'Lag Axe barrier samples indicated that they are all similar in chemical composition.

II. OBJECTIVE Pyrolysis Gas Clixomatogxaphy (PGC) with Mass Selective Detection (MSD) was used to qualitatively compare seven Thcano-Lag fixe bamcr samples.

III. DES CRIFHON OF METfiOD 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 thc Thermo-Lag s- apples were performed with a CDS pyxopxobe mounted in an independently hcatcd interface attached to the hjcction port of the GC. Analysis involved weighing 1-3 mgs. of sample in a quartz tube and placement af thc tube in the platinum coil element of the probe. The probe is then placed in the interface and pyrolysed balHstically 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 axe shown in Table 1. Pziot to each analysis, the column is heated to 250 C to elute any volatilcs which were not entralxtcd in thc polymer.

IY. PRESENTATION OF RESULTS Thc seven pyzogz ims (total ion chromatogt4LAQ) fof each of thc seven Thermo-Lag samples are shown in Figures 1, 3, 5, 7, 9, 11 and 13. 'He eazactcd ion chromatograms using thc acrylate base ion m/e of SS common to ethyl acryiate (EA) and m/c of 69 common to methyl mcthaczylate (MMh) for each sample are shown in Figures 2, 4, 6, 8, 10, 12 and

14. The sample name at the top of each figure is the NUCON Log // I. D. Samples 0395-25AM are further identified in Table 2 along with thdr respective EA/MMAarea zatios.

Each sct 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.

NUCON 06FL830/01 V. DISCUSSION OF RESULTS The average cxttactcd ion area ratio for EA/MMAof 1.26 Q0.07 (ka) shown in Table 2 is consistent with the avctage area ratio of 1.4 <0.1 (ko) obtained from other Thermo Lag samples tested under thc NEI generic testing program.

Thc extracted ion chromatogtams shown in Figurc 2 for sample 0395-25A, 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/MMAratio of 1.28. Pyridine compounds identified jn the pyrogram (Figure 1) arc pyridinc, 3-methyl pyridinc, 2-methyl pyridine, 3, 5<imethyl pyridinc, 2, 3, 5-trimethyl pyridine, 3<thyl-5-methyl pyridine and 5-ethcnyl-2 methyl-pyridine. Other key components identified are 2, 3, 4, 5-tetramcthyl-lH-pyrrole, pentancdioic acid diethyl ester, tris (mcthylphenyl) phosphate, octicizer and triphcny]

phosphate.

The extracted ion chromatograms shown in Figure 4 for sample 0395-25B, 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, have an EA/MMAratio of 1.31. Pyridinc compounds identified in thc pyrogtam (Figtae 3) are 3-methyl pyridinc. Other key components identified 2, 3, 4, 5-tettamethyl-lH-pynole, pentanedioic acid diethyl ester, tris (methylphenyl) phosphate and octiclzcre

'Iho cxttactcd ion chromatogtams shown in Figurc 6 for sample 0395-25C, 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 EAlh&fA ratio of 1.33. Pyridine compounds identified in thc, pyrogram (Figuxe 5) are 3-methyl pyridinc and 3, 5-dimethyl pyridinc. Other key components idcntifiicd are 2, 3, 4, S-tctramethyl-1H-pyrrole, pcntanedioic acid diethyl ester, octicizer and tris (methylphcnyl) phosphate-The extracted ion chromatograms shown in Figure 8 for sample 0395-25D, a 3 hour3.472222e-5 days <br />8.333333e-4 hours <br />4.960317e-6 weeks <br />1.1415e-6 months <br /> tated panel sample, have an EA/MIMAratio of 1.26. Pyridine compounds identifie in the pyrogram are 3-methyl pyridine. Other kcy components identificd are pcntancdioic acid diethyl ester (visual inspection), triphcnyl phosphate, octicizcr and tris (methylphcnyl) phosphate.

The extracted ion chromatograms shown in Figure 10a for sample 0395-25E, a trowel grade sample, had an EA/MMAratio of 0.51. As this was not consistent with other Thermo-Lag samples tested,'ample 0395-25E was rctestcd. The extracted ion chromatoipans for the tetest sample shown in Figure 10b have an EA/MMAtatio of 1.21, which is consistent with other Thermo-Lag samples tested. Pyridine compounds identified in the pytogaun (Figure 9b) are 3-methyl-pyridine, and 3, 5<imcthyl pyridine. Other key components identifie are 2, 3, 4, S-tetramethyl-1H-pyrrole, pentanedioic acid diethyl ester, octicizer and tris (methylphenyl) phosphate.

NUCON 06FL830/01 The extracted ion chromatograms shown in Figurc 12 for sample 0395-2SF, 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/MMAratio of 1. 13. Pyridine compounds identiycd in the pyrogram (Figurc 1 I) arc 3-methyl pyridine. Other key components identified are 2, 3, 4, S-tctramcthyl-IH-pyrrolc, pentanedioic acid diethyl ester, octicizer and (methylphenyl) phosphate.

Thc extracted ion chn)matograms shown in Figure 14 for sample 039S-2SG, 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/MMAratio of 1.31. Pyridinc compounds identiQed in the pyrogram (Figurc 13) are pyridlne, 3-methyl pyridinc, 2, 5-dimethyl pyridinc, 3~thyl pyridine, 3~yl pyridine, 3, dimethyl pyridinc, 2, 3, 5-trimethyl pyridine, 3&yl-S-methyl pyridine and Methyl-2-methyl pyridine. Other key components identified are 2, 3, 4, S-tetramethyl-lH-pyrrolc, pentanedioic acid diethyl ester, octicizcr, triphcnyl phosphate and tris (mcthylphenyl) phosphate.

In conclusion, thc results indicate that the seven Thermo-Lag samples are consistent in terms of chemical composition to other Thermo-Lag samples tested as part of the, NEt gcncnc testing program.

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