Document KJrNo61v86NJ3eL4mZ4XGEOro

V 4 UNION CARBIDE INTERNAL CORRESPONDENCE CHEMICALS AND PLASTICS * P. O. BOX 8361, SOUTH CHARLESTON, WEST VIRGINIA 25303 To (Name) Division Location Mr. R. N. 514 Wheeler Copy to Mr. R. L. Barker, 514 Mr. M. E. Griffith, 514 Mr. J. B. Johnson, 511 Mr. N. H. Ketcham, 511 Mr. R. E. Peele, 511 Mr. J. L. Worstell, 514*^ Mr. W. C. Young, 514 o.te October 1, 1976 originating Dept Research and Development subiecr EPA Method 106, Determination of Vinyl Chloride from Stationary Sources Dear Mr. Wheeler: Results of analyses for vinyl chloride, which you requested on a cylinder containing four components in nitrogen are given in Table I. The analyses were run using the EPA Method Number 106 for vinyl chloride. The components and their calculated concentration in the cylinder are: vinyl chloride, 10 ppm; acetalde hyde, 50 ppm; acetone, 50 ppm; and vinyl acetate, 50 ppm. The gas chromatographic procedure given in Method 106 failed to separate vinyl chloride and acetaldehyde. The results in Table I, calcu lated as vinyl chloride, reflect the combined total of vinyl chloride and acetaldehyde because the two components elute together and are integrated as a single response. Table I also gives the results of the analysis of calibrating standards for vinyl chloride, prepared in nitrogen in a Tedlar bag, according to the instructions given in Method 106. Two bags were prepared and the analyses of the contents are shown under Bag A and Bag B. Copies of the gas chromatographic scans illustrating the response obtained in analyzing the sample and standards are shown in the attached figures. Figure 1 is the chromatogram for a 10 ppm vinyl chloride in nitrogen standard prepared in a Tedlar bag as called for in Method 106, showing a retention time of 2.84 minutes. Figure 2 is for acetaldehyde prepared in a Tedlar bag, showing retention time of 2.71 minutes. Figure 3 is the chromato gram from the analysis of the four--component cylinder sample, illustrating that the vinyl chloride and acetaldehyde elute as a single peak at a retention time of 2.71 minutes. Table II gives the instrument parameters used with the Hewlett-Packard Model 5831A gas chromatograph to analyze the sample. UCC 103720 Mr. R. N. Wheeler Page 2 October 1, 1976 me know. II you need any additional information, please let Very truly yours, JEN: Iks Attachments J. E. Neff UCC 103721 TABLE I RESULTS OF ANALYSES ON KNOWN CONCENTRATIONS OF VINYL CHLORIDE IN NITROGEN Four-Component Standard in Nitrogen Run No. 1 2 3 4 5 Average Acetaldehyde plus Vinyl Chloride Calculated as ppm Vinyl Chloride 63.51 61.63 65.03 63.23 63.45 63.37 10 ppm by Volume Vinyl Chloride in Nitrogen Made in Tedlar Bag EPA Method 106 Run No. 1 2 3 4 Average ppm by Volume Vinyl Chloride Bag A Bag B 9.98 9.98 10.05 9.97 10.00 9.52 9.50 9.995 9.67 VJCC 103722 TABLE II GAS CHROMATOGRAPHIC CONDITIONS Instrument Column Column Temperature Detector Temperature Gas Sampling Loop Loop Temperature Carrier Gas Hewlett-Packard Model 5811A gas chromatograph with dual flame ionization detectors. 2.5 m x 3.2 mm stainless steel packed with 80/100 mesh Chromosorb 102 155C. , Isothermal 225 C. 2.0 cc 70" C. Nitrogen at 15 cc/min UCC 103723 FIGURE 1 GAS CHROMATOGRAPH IC SCAN OF 10 PPM BY VOLUME VINYL CHLORIDE IN NITROGEN r r VINYL CHLORIDE FIGURE 2 GAS CHROMATOGRAPHIC SCAN OF 10 PPM BY VOLUME ACETALDEHYDE IN NITROGEN ACETALDEHYDE * h- UCC 103724 FIGURE 3 GAS CHROMATOGRAPHIC SCAN OF FOUR-COMPONENT STANDARD FROM STAINLESS STEEL CYLINDER if i rt P i C t~t ' M-P jin R T jfi/ </ VINYL CHLORIDE + ACETALDEHYDE # ACETONE 1 5a30ft D RT .l VINYL ACETATE t IK P K T b4 MrlhH ' O h3 ti i, duae i + l? L ML f? 1 rt f'1 i h :,^ UCC 103725