Document Nee6epNeLgvkg4YpyB9eDZZ1g

MM (SOM) inter-office memo T E N N E C 0 CHEMICALS, INC. To H.B. Carr \ from Kanzler AT Burlington at Burlington subject Analyses of Vinyl Chloride Monomer (VCM) in the Stripper Headspace and Recovery Slurry December 8, 1972 copy to E.J. Hourihan M Q Wilkenfeld Gas chromatographic analyses were performed on a stripper headspace sample and a slurry sample to determine the VCM level after recovery. The follow ing is a summary of the analyses work and results: X. Sampling Two medium pressure sample containers were used to obtain the samples: A. Headspace Sample An evacuated sample container was attached to a sample line normally used for lonol addition. At the time of sampling the stripper had been pressurized to 20 psig with nitrogen just prior to transfer of the slurry to the blend tank. B. Slurry Sample A sample container was attached to the slurry transfer line on a sam ple tap just before leading to the chip basket. A slow sample flow was noted during the filling of the sample container. This may be at tributable to the fact that the sample tap is in a right angle to the slurry transfer line. II, Analyses Two different analyses conditions were utilized for the samples: A, Headspace Sample 1. Sample Preparation A septum covered Swaglok fitting was attached to one valve outlet of the sample container. The sample was withdrawn from the con tainer with a Hamilton gas syringe. Two ml of this sample was then transferred onto the gas chromatographic column. 2. Instrument Conditions and Calibration The gas phase analyses were accomplished with a 12' x SS column packed with 20% tributyl phosphate on Chromosorb P(AW), an inject port temperature of 130C, oven temperature of 60C and a flame ionization detector (FID) temperature of 260C. COLORITE 013987 2. Instrument Conditions and Calibration (continued) Calibration was made by injection of 0.5 ml of VCM in the same manner as mentioned for the sample in 11.A.1.. The detector response of this inject was used as a 25% by nrc>l VCM standard. 3. Results The VCM level was calculated to be 21.9% in the stripper headspace (see Table I, attached). B. Slurry Sample 1. Sample Preparation a. Slurry Liquid As before a septum-covered Swaglok fitting was attached to one valve outlet of the- sample container. After sampling with a syringe, five ml of the liquid was injected onto the column for analyses. b. Slurry Sample After analysis of the slurry liquid, a slurry sample was transferred directly from the sample container into an Erlenmeyer flask containing 87.9 gms tetrahydrofuran (THF). The resin contained in the slurry was allowed to dissolve for about fifteen minutes. A 5Jul aliquot of the solution was subsequently transferred onto the column for analysis. 2. Instrument Conditions and Calibration For the analysis of the liquid, a 12' x SS column packed with 10% Diethylene Glycol Succinate (DEGS) on Chromosorb W(AW). The instrument conditions were set as follows: inject port 180C, oven 70C and~the t'LD'260^(7; The calibration standard was prepared by saturating 100 ml of water with VCM. This was "accomplished by bubbling about 1000 ml of VCM through the 100 ml*of water. The VCM content in the saturated water was calculated to be 0.73% by weight. __ 3. Results The dissolved VCM level in the slurry water was* found to be 0.15% by weight. The total VCM level in the resin slurry THF sample was 1,6% by weight based on the slurry sample weight in the THF. Attachment. FWK/jt __ Ari-td yf. , ----------------- ------------------ ----- F.W. Kanzler COLORITE 013988 TABLE X VINYL CHLORIDE MONOMER IN STRIPPER HEADSPACE AND RECOVERY SLURRY SAMPLE Stripper Headspace @20 psig B-5212-3120M30-225/I6R Slurry Sample B-5212-3120-225/16R a. Liquid b. Slurry (Total) VCM 21.9% by mol 0.15% by weight 1,56% by weight COLORITE 013989