Document 0qZkmn1prjYjQmXdK154aeq6J
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RECEIVED
atOvv JUL 051974
R. N. WHEELER7JR:
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R. M. Arnold, 515
R. A. Bleidt, 511
G. P. Bigelow, NYO
Mr . M . E. Eisenhour, 515
R. E. Gulick, NYO
C. J. Haines, 514
R. J. Hanna, 511
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G. F. Tacquard, 515,,^---
R. N. Wheeler, <611"*
W. E. Whitehurst, 511
Dole July 2, 1974
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Research and Development
i 7 VCl Mdnpmer in ( Resins:\ ASTM Study
Gentlemen:
The ASTM task group studying methods for quantitative determination of VC1 monomer in PVC resins held their initial meeting on June 26. Gas chromatographic methods were submitt d and the essentials of these procedures were summarized in th attached sheet by the task group chairman, Mr. Ed DeCapita of B. F. Goodrich. These methods used a solution of the vinyl resin in either 1HF (UCC method) or in dimethyl acetamide.
The initial round robin study will include 3 homopolymer resins (2 to contain ~10 ppm residual VC1) to be provided as solid resin and as 5% solution in THF and dimethylacetamide. Methods provided by Goodrich and Dow will be investigated in the initial study. Approximately 18 laboratories plan to participat .
On the basis of the discussions it is concluded that the current UCC procedure is technically sound and capable of detection of VC1 at a level equivalent to the methods used in the industry.
Hie Goodrich method, which will be obtained soon, is being Installed to monitor production at all the Goodrich plants: the output is handled by a computer. At the moment, we see no advantage to this system over the UCC procedure.
The Dow system uses a "silicone" column which may provid a satisfactory approach for the definition of vinylidene chlorid in the presence of water. This column will be investigated.
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We plan to participate in these round robin studies and will promote the evaluation of vinyl chloride-vinyl acetate copolymers in subsequent investigations.
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RVCH IN POLYVINYL CIILORI JK S'lHMART OF ANALYTICAL PROCEDURES
Cn*tiyr Flmt4M
Column Type
1/S" 0D X 6' S.S., Poropek S, 80/100
Onion Carbide 1/8" OD X Poropek Q
Goodyear
1/8* 00 X 22' S.S., 10* OV 225, 80/110 Chrom. W-HP
01 In
1/8* OD X 30' S.S. 23* UCON SO HB 5100 70/80 Chrom. V-HW
Dow 3mn ID X 20* Olaes, 10* OV-17, 100/120 Chrom. W-HP
Diamond Bniroyal
1/8" X 12* S.S., 10* OC-98, 80/100 Chrom. H-HP
1/8" OD X 2m, IQS C-98 80/100 Chrom. W-HP
PPO 1/8" OD X 2w, 10% W-20n, 60/80 Gaapack F 1/8" 00 X 2a, 15* Aplexon L, 80/100 Gaachram. P
BP1 1/8" XT* 1/8" X 2', 80/100 Fni opak QS
Polymer Solvent
THF
Polymer Cone. *
5
InJ.
Det.
Col. Sample
Temp.C Tcmp.C Tep.0C Siie pi
-- -- 150
3
Analyala Tima
--
Calibration Type
`bt
THF
4
-- -- 150
1
-- Ext.
THF
5
150 150
60 15
-- Int. 2-Hethyl Pentane
THF 1
75 300 50 1
-- Ext.
DHPtTHF MAC
5
125
MAC ' 3.6 200 260 \
80 70 2-20
THF 5 THF 10
150 260
liO 10
110 280 105
-- bt. -- bt. -- bt.
bt.
DHAC
5
200 250 HiO 10
15" , Ini. Pentane BF
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