ML20094H052
| ML20094H052 | |
| Person / Time | |
|---|---|
| Site: | Peach Bottom, Limerick  |
| Issue date: | 06/30/1995 |
| From: | Freeman W, Keller T NUCON, INC. |
| To: | |
| Shared Package | |
| ML20094H046 | List: |
| References | |
| NUCON-06PB847-0, NUCON-06PB847-01, NUCON-6PB847, NUCON-6PB847-1, NUDOCS 9511130310 | |
| Download: ML20094H052 (8) | |
Text
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TELEPHONE: (614) 846 5710 NUCON International, Inc.
OUTSIDE OHIO: 1-800 992 5192
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P.O. BOX 29151 7000 HUNTLEY ROAD TELEX: 6974415 COLUMBUS. OHIO 43229 U.S.A.
FAX: (614) 4314858 1
PYROLYSIS GAS CHROMATOGRAPIn' ANALYSIS OF 21 THERMO-LAG FIRE BARRIER SAMPLES Performed For:
PECO Energy Company
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2301 Market Street P.O. Box 8699 Philadelphia, PA 19101-8699 P.O. No. GN265985 28 June 1995 I
1 Distribution PECO:
George J. Siefert (1)
NEI:
Biff Bradley (1)
NUCON:
06PB847 Master File (1)
Lab (1)
J NUCON 06PB847/01 P
O 00 77 P.
NUCON OoPB847/01 NUCON International, Inc*
TELEPHONE: (614) 846 5710 h,
OUTSIDE OHIO: 1-800-992-5192 P.O. BOX 29151 7000 HUNTLEY ROAD TELEX: 6974415 COLUMBUS. OHIO 43229 U.S.A.
FAX: (614) 431-0858 i
b Prepared By Reviewed By Original Issue 2
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W. P. Freeman T. S.
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NUCON 06PB847/01 4
i I.
ABSTRACT 9
Inspection of the pyrograms of 21 'Ihermo-Lag fire barrier samples indicated that they are j
all similar in chemical composition.
1 II.
OBJECTIVE j
Pyrolysis Gas Chromatography (PGC) with Mass Selective Detection (MSD) was used to l
qualitatively compare twenty-one Thermo-Lag fire barrier samples.
1 III.
DESCRIPTION OF METHOD The samples were compared by pyrolysis gas chromatography using ASTM D3452 as a 1
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 quartz tube and placement of the tube in the platinum coil element of the probe. The
[g probe is then placed in the interface and pyrolysed ballistically for 2 seconds. Pyrolytic j
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 l
volatiles which were not entrained in the polymer.
{
IV.
PRESENTATION OF RESULTS l
The twenty-one pyrograms (total ion chromatograms) for each of the twenty-one Thermo-Lag samples are shown in Odd numbered Figures 1-41. The 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 even numbered Figures 2-42. The sample name at the top of each figure is the NUCON Log # I. D.
Samples 0495-5A-F for Peach Bottom and 0495-6A-O for Limerick are further identified in Table 2 along with their respective EA/MMA area ratios and sample densities. 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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DISCUSSION OF RESULTS i
The average extracted ion area ratio of EA/MMA of 1.30 i0.10 ( o) for the Peach Bottom samples, of 1.28 i0.05 ( o) for the Limerick Unit 2 samples, of 1.28 i0.M l
(io) for the Limerick Unit I samples, of 1.29 i0.07 ( o) for the Limerick Control l
Building samples and of 1.29 0.07 (to) for all twenty-one samples is consistent with
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average EA/MMA area ratio of 1.4 i0.1 (io) obtained from other Thermo-Lag samples J
3 tested under the NEI generic testing program.
The extracted ion chromatograms shown in Figure 2 for sample 0495-5A 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 of 1.35. Pyridine compounds identified in the pyrogram (Figure 2) are pyridine, 3-methyl pyridine, 3, 5-dimethyl pyridine, 2, 3, 5-trimethyl pyridine 3-ethyl-5-methyl pyridine and 5-ethenyl-2-methyl pyridine.
Other key components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole, pentanedioic acid diethyl ester (visual inspection), triphenyl phosphate, octicizer and tris (methylphenyl) phosphate.
1 The extracted ion chromatograms shown in Figure 4 for sample 0495-58, a trowel grade sample, have an EA/MMA ratio of 1.25. Pyridine compounds identified in the pyrogram (Figure 3) are pyridine, 3-methyl pyridine and 2, 5-dimethyl pyridine. Other key S
components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole, pentanedioic acid diethyl
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ester, triphenyl phosphate, octicizer and tris (methylphenyl) phosphate, j
The extracted ion chromagrams shown in Figure 6 for sample 0495-5C, 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 5) are 3-methyl pyridine, 2, 5-dimethyl pyridine, 3-ethyl pyridine, 3-ethenyl-pyridine, 3, 5-dimethyl pyridine, 2, 3, 5-trimethyl pyridine, 3-ethyl-5-methyl pyridine and 5-ethenyl-2-methyl pyridine. Other key components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole.pentanedioic acid diethyl ester, triphenyl phosphate, octicizer and j
tris (methylphenyl) phosphate.
The extracted ion chromatograms shown in Figure 8 for sample 0495-5D have an EA/MMA ratio of 1.26. Pyridine compounds identified in the pyrogram (Figure 7) are pyridine, 3-methyl pyridine, 3, 5-dimethyl pyridine, 2, 3, 5-trimethyl pyridine, 3-ethyl-5 methyl pyridine and 5-ethenyl-2-methyl pyridine. Other key components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole, pentanedioic acid diethyl ester, triphenyl phosphate, octicizer and tris (methylphenyl) phosphate.
The extracted ion chromatograms shown in Figure 10 for sample 0495-5E, have an EA/MMA ratio of 1.15. Pyridine compounds identified in the pyrogram (Figure 10) are 3-methyl pyridine and 3,5-dimethyl pyridine. Other key components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole, pentanedioic acid diethyl ester, triphenyl phosphate, octicizer C
and tris (methylphenyl) phosphate.
2
NUCON 06PB847/01 The extracted ion chromatograms shown in Figure 12 for sample 0495-5F, a trowel grade sample, have an EA/MMA ratio of 1.38. Pyridine compounds identified in the pyrogram (Figure 11) are pyridine, 3-methyl pyridine, 3, 5-dimethyl pyridine, 2, 3, 5-trimethyl pyridine and 5-ethyl-2-methyl pyridine. Other key components identified are 2, 3, 4, 5-
- tetramethyl-lH-pyrrole, pentanedioic acid diethyl ester, octicizer, triphenyl phosphate and tris (methylphenyl) phosphate.
The extracted ion chromatograms shown in Figure 14 for sample 0495-6A, a trowel grade sample, have an EA/MMA ratio of 1.30. Pyridine compounds identified in the pyrogram (Figure 13) are pyridine, 3-methyl pyridine, 3, 5-dimethyl pyridine, 2, 3, 5-trimethyl pyridine and 5-ethenyl-2-methyl pyridine. Other key components identified are 2, 3, 4, 5-tetmmethyl-lH-pyrrole, pentanedioic acid diethyl ester, triphenyl phosphate, octicizer, and tris (methylphenyl) phosphate.
The extracted ion chromatograms shown in Figure 16 for sample 0495-6B, a 3 hour3.472222e-5 days <br />8.333333e-4 hours <br />4.960317e-6 weeks <br />1.1415e-6 months <br /> ratui panel sample, have an EA/MMA ratio of 1.27. Pyridine compounds identified in the f
pyrogram (Figure 15) are 3-methyl pyridine, 2, 5-dimethyl pyridine, and 3-ethenyl methyl pyridine. Other key components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole, pentanedioic acid diethyl ester, tris (methylphenyl) phosphate and octicizer.
N The extracted ion chromatograms shown in Figure 18 for sample 0495-6C, 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/MMA ratio of 1.20. Pyridine compounds identified in the pyrogram (Figure 17) are 3-methyl pyridine. Other key components identified are 2, 3, 4,5-tetramethyl-lH-pyrrole, pentanedioic diethyl ester, octicizer and tris (methylphenyl) phosphate.
The extracted ion chromatograms shown in Figure 20 for sample 0495-6D, 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 1.34. Pyridine compounds identified in the pyrogram (Figure 19) are pyridine 3-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, tris (methylphenyl) phosphate, and octicizer.
The extracted ion chromatograms shown in Figure 22 for sample 0495-6E, 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 1.30. Pyridine compounds identified in the pyrogram (Figure 21) 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-lH-pyrrole, pentanedioic acid diethyl ester, octicizer and tris (methylphenyl) phosphate.
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J NUCdN 06PB847/01 q-e The extracted ion chromatograms shown in Figure 24 for sample 0495-6F, a trowel grade j -
sample, have an EA/MMA ratio of 1.28. Pyridine compounds identified in the pyrogram (Figure 23) are 3-methyl pyridine, 2, 4-dimethyl pyridine, 2, 3, 5-trimethyl pyridine, 3-ethyl-5-methyl pyridine and 5-ethenyl-2-methyl pyridine. Other key components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole, pentanedioic acid diethyl ester, octicizer and tris (methylphenyl) phosphate, i
The extracted ion chromatograms shown in Figure 26 for sample 0495-6G, a 1 hour1.157407e-5 days <br />2.777778e-4 hours <br />1.653439e-6 weeks <br />3.805e-7 months <br /> rated j
panel sample, have an EA/MMA ratio of 1.30. Pyridine compounds identified in the I
pyrogram (Figure 25) are 3-methyl pyridine (visual inspection). Other key components identified are 2,3,4,5-tetramethyl-lH-pyrrole, pentanedioic acid diethyl ester, octicizer 4
and tris (methylphenyl) phosphate.
The extracted ion chromatograms shown in Figure 28 for sample 0495-6H, a 1 hour1.157407e-5 days <br />2.777778e-4 hours <br />1.653439e-6 weeks <br />3.805e-7 months <br /> rated j
4 conduit sample, have an EA/MMA ratio of 1.31. Pyridine compounds identified in the pyrogram (Figure 27) are 3-methyl pyridine, 3, 5-dimethyl pyridine and 2, 3, 5-trimethyl f
pyridine.
Other key components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole, i
pentanedioic acid diethyl ester, octicizer and tris (methylphenyl) phosphate.
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The extracted ion chromatograms shown in Figure 30 for sample 0495-6I, 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 1.19. Pyridine compounds identified in the pyrogram (Figure 29) are pyridine, 3-methyl pyridine, 2-methyl pyridine and 3, 5-l dimethyl pyridine. Other key components pentanedioic acid diethyl ester, octicizer and tris (methylphenyl) phosphate.
The extracted ion chromatograms shown in Figure 32 for sample 0495-6J, a 3 hour3.472222e-5 days <br />8.333333e-4 hours <br />4.960317e-6 weeks <br />1.1415e-6 months <br /> rated l
conduit sample, have an EA/MMA ratio of 1.36. Pyridine compounds identified in the pyrogram (Figure 31) are pyridine, 3-methyl pyridine, 3, 5-dimethyl pyridine, 2, 3, 5-i trimethyl pyridine,3-ethyl-5-methyl pyridine and 5-ethenyl-2-methyl pyridine. Other key components identified are 2, 3, 4, 5-tetramethyl-1H-pyrrole, pentanedioic acid diethyl 4
l ester, triphenyl phosphate, octicizer and tris (methylphenyl) phosphate.
l The extracted ion chromatograms shown in Figure 34 for sample 0495-6K, a trowel grade i
sample, have an EA/MMA ratio of 1.30. Pyridine compounds identified in the pyrogram (Figure 33) are pyridine, 3-methyl pyridine, 3, 5-dimethyl pyridine, 2, 3, 5-trimethyl i
pyridine, 3-ethyl-5-methyl pyridine and 5-ethenyl-2-methyl pyridine.
Other key components identified are 2, 3, 4, 5-tetramethyl-1H-pyrrole, pentanedioic acid diethyl ester, triphenyl phosphate, octicizer and tris (methylphenyl) phosphate.
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NUCON 06PB847/01 w
The extracted ion chromatograms shown in Figure 36 for sample 0495-6L, 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/MMA ratio of 1.28. Pyridine compounds identified in the pyrogram (Figure 35) are 3-methyl pyridine. Other key components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole, pentanedioic acid diethyl ester and tris (methylphenyl) phosphate (visual inspection).
The extracted ion chromatograms shown in Figure 38 for sample 0495-6M, a 1 hour1.157407e-5 days <br />2.777778e-4 hours <br />1.653439e-6 weeks <br />3.805e-7 months <br /> rated pane! sample, have an EA/MMA ratio of 1.19. Pyridine compounds identified in the pyrogram (Figure 37) are 3-methyl pyridine. Other key components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole (visual inspection), pentanedioic acid dimethyl ester, (visual inspection), triphenyl phosphate, octicizer and tris (methylphenyl) phosphate.
The extracted ion chromatograms shown in Figure 40 for sample 0495-6N, 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 1.32. Pyridine compounds identified in the pyrogram (Figure 39) are pyridine, 3-methyl pyridine, 3, 5-dimethyl pyridine, 2, 3, 5-f trimethyl pyridine,3-ethyl-5-methyl pyridine and 5-ethenyl-2-methyl pyridine. Other key components identified are 2, 3, 4, 5-tetramethyl-lH-pyrrole, pentanedioic acid diethyl ester, octicizer and tris (methylphenyl) phosphate.
Q The extracted ion chromatograms shown in Figure 42 for sample 0495-60, 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 1.37. Pyridine compounds identified in the pyrogram (Figure 41) are 3-methyl pyridine and 3, 4-dimethyl pyridine. Other key components identified are 2, 3, 4, 5-tetramethyl-1H-pyrrole, pentanedioic acid diethyl ester, triphenyl phosphate, octicizer and tris (methylphenyl) phosphate.
In conclusion, the results indicate that the twenty-one Thermo-Lag samples tested are consistent in terms of chemical composition with other Thermo-Lag samples tested as part of the NEI generic testing program.
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NUCON 06PB847/01
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- i TABLE 1 Chromatographic Conditions:
30 meter 0.25 mm narrow bore fused silica HP-5 CB capillary column.
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Carrier Gas: Helium,0.9 mLJmin, split ratio 35:1 Column Conditions:
Initial Temperature: 50*C for 1 minute hold Ternperature 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 n
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