Document zbdgq0nbgBkLGNB89GqOz7Jgm

L A Major Component of TENNECO /NC. TENNECO PLASTICS DIVISION P.0. Box 116, Burlington, N. J. 08016 November lj5, 1969 Mr. James C. Hahn, Technical Assistant Tenneco Plastics Division Pronociones Industriales Mexicanas, S. A. KM 2 Oarretera La Resurreccion Arpartado Postal Num, 604 Puebla, Puebla, Mexico Dear Jim: Attached is a copy of the gas chromatographic method (B.A.C.M. #201) utilized in Burlington for the analysis of mixed recovered monomer. A typical chromatogram is attached to the method to serve as a guide in optimizing conditions on your model 88l Perkin Elmer gas chromatograph. As we indicated in earlier correspondence regarding monomer analysis, your Perkin Elmer instrument should perform this job very nicely. However, if you encounter any difficulties, we should be able to readily line these out by an interchanges of samples and chromatograms. Very truly yours TENNECO PLASTICS DIVISION Tenneco Chemicals, Inc. HBC/rjl Enclosure cc: M. G. Caine E. J. Hourihan R. K- Marks M. W. Williams Primex Pile $ H. B. Carr, Manager Quality Control COLORITE 016283 TENNECO CHEMICALS. INC. TENNECO PIASTICS DIVISION Burlington, New Jersey B.A.C.M. #201 DATE ISSUED: November 6, 1969 Determination of Vinyl Chloride Monomer, Vinyl Acetate Monomer, and Trlchlorethylene In Recovered Copolymer Monomer APPLICATION: The stripped off monomer from the production of polyvinyl chloride/polyvinyl acetate copoly mers is recovered and proportionally mixed in with virgin monomers for each batch charged. To achieve the correct ratio of virgin mcnomer versus recovered monomer, the composition of the recovered monomer is quantitatively analy zed by gas chromatography. The level of tri- chlorethylene (TCE) is analyzed for at the same time to calculate the additional amount of TCE needed for each batch charged. The sensi tivity for this method as written, is in the 0.1. range for each conponent to be analyzed. APPARATUS: 1. Hewlett and Packard Gas Chromatograph F & M 5754A, or equivalent (equipped with flame ionization detector (FID) or thermo conductivity detector (TC) and septum covered injection port). 2. Hamilton syringe 50*1 (# 705 LT). 5* Hypodermic needle, luer short hub point style #1, 2" long, 24 gauge ($1-724). 4. Two stage regulators for, helium, air, hydro gen with secondary gauge capacity 0-100 psig. 5- 1/8" OD copper tubing. 6. 1/8" OD stainless steel 516 tubing. 7- 1/8" Swagelok nuts and ferrules 8. Adjustable wrench 6" and 12". 9. Hoke gas bomb 150 ml, fitted with two valves (Cat. # 4HD150). 10. Vibrator (Scientific Glass Apparatus (SGA) Cat. #M-1425). 11. Glass wool. 12. Glass rod. 15. Evaporating dish, 200 mm diameter 14. Vacuum oven. COLORITE 016284 B.A.C.M. #201 Page No. 2 15. Analytical balance with 0.1 mg readout. 16. Hot plate. IT. 80 and 100 mesh Tyler screen assembly. 18. Funnel, long stem, 75 mm upper ID. 19. Tygon tubing, 3/16" ID, 3/52" wall thick ness. 20. Dry ice chest. 21. 25 ml beaker 22. Planimeter (if available) REAGENTS: 1. Silicone Gum Rubber UCC-W982 (methyl vinyl) (Hewlett and Packard Cat. #8501-3840). 2. Diatoport S 80 - 100 mesh (Hewlett and Packard Cat. #8501-6302). 3. Methylene chloride, analytical reagent. 4. Vinyl chloride monomer, virgin. 5. Vinyl acetate monomer, virgin. 6. Trichlorethylene, virgin. 7- Dry ice (frozen COg). COLUMN PREPARATION: For column preparation see B.A.C.M. #1 sub stituting the following reagents, apparatuses and conditions: Under 2., 5 gm of Silicone Gum Rubber UCC-W982 for 10 gm of Trlbutyl Phosphate. Under 3-, 50 gm of Diatoport S 80 - 100 mesh for 50 gm of Chromosorb p/AW 60 - 80 mesh. Under 6., an assembly of 80 and 100 mesh Tyler screens for an assembly of 60 and 80 mesh Tyler screens. Under 7., transfer the packing on the 100 mesh screen for 80 mesh screen (the size is now 80 - 100 mesh). Under 8., cut a 12' length .of l/8M S3 tubing for a 12' length of l/4" SS tubing. Under 12., condition the column with about 50 cc/min. Helium flow overnight at an oven temperature of 250 C for an oven temperature of 50C. CONDITIONS: Column: 12' x 1/8" SS 10$ Silicone Gum Rubber UCC-W982 on Diatoport S 80 - 100 mesh Carrier Gas: Helium 50 cc/min. 40 psig in line If FID is used: Hydrogen: 60 cc/min. 40 psig in line Air: 350-Cc/min. 20 psig in line FID Oven: 310C COLORITE 016285 STANDARDIZATION: PROCEDURE: CALCULATION: B.A.C.M. #201 Page No. 5 If TC Detector Is used: TC Detector Oven: 350C Detector bridge current output: Oven: Ambient Injection Port: 25C 150 milli005)6res No standardization is required since area normalization is used. Retention times and approximate sensitivities should be estab lished for the components analyzed. 1. Cool the bomb sample of the recovered MVC in the dry ice chest together with the 50^1 syringe (hypodermic needle mounted) and the 25 ml beaker. 2. After at least ?0 minutes, transfer about 10 ml of the liquid in the bomb into the cooled 25 ml beaker. 3. Rapidly withdraw about 20*1 of the sample in the 25 ml beaker and Inject the saiqple into the gas chromatograph. (Note 1) 4. Attenuate the three component peaks as they elute. 1. Determine the individual peak areas with either a planimeter or by measuring the width of the peak at half the peak height. (The planimeter area is direct reading.) The area for the half width of peak height determination is found by: Total peak height in mm x width of the peak at half the peak height in mm = Area 2. Normalize all peak areas to one attenuation. % component in recovered copolymer monomer = Area of componenet analyzed x'100 Total Peak Areas COLORITE 016286 B.A.C.M. #201 Page No. 4 Note: All steps described in 1.) through 3.) should be performed as fast as possible and in the dry ice chest. To best accomplish the inject, the dry ice box should be in close proximity of the gas chromatograph. Figure 1 shows a typical chromatogram. Analysis run with FID. Attachments Written by: F. W. Kanzler H. B. Carr Manager - Quality Control COLORITE 016287 COLORITE 016288