Document V3B4xOb03BY8XYp7gLmYQYmXw

(conoco) Technical Service Report Repoit Nr; 455-81-839-9 To L. Soncs Conoco Inc. Research and Development Department Analytical Research Section Ponca City, Oklahoma f ' *i From Date ('. 15. lie r r i n April 2?, 1981 11 US I........ . .! : and iiir; priori my u tv: : Subject CC/MS EXAMINATION OF TWO LAKE CHARLES EFFLUENT WATERS FOR ACROLEIN AND ACRYLONITRILE Conclusion: Neither of the title pollutants was found in either sample. Int roduc tion This is a continuation of the work described in TSR 429-81-804-8. The samples examined were 4236-93-12 front the chemical plant and 4236-93-2 from the VCM plant. Both were stored in the cold room until shortly before they wore run. Both samples were run on the fifteenth of April. F.xpc r iraenta 1 Preparation of the Analytical Column: An empty glass column ^6' x 2 mm i.d. was thoroughly cleaned and dried, it was silanized by filling with "Sylon" and allowing it to stand at room temperature for five minutes. The "Sylon" solution was removed by suction, and the tubing was washed with toluene and anhydrous methanol. Air was pulled through until the methanol had evaporated, and then the empty column was installed in a chromatograph and heated to 150C with He flow. The packing, Chroinosorb 101 80/100 mesh, was preconditioned overnight in .i large diameter metal column at 180C with He flow. The packing was dumped from the large column and resieved. The. glass column was packed, and the ends were plugged with silanized glass wool. The column was installed in the Sigma III (GC/MS chromatograph) oven with the column exit disconnected and conditioned overnight at 150C. ! im ( r i nne n ( a I Co n<l L t; i on a Sample - on-column injection of 5 pJ. Injector - 13 00 C Co l ninn - 1 300 C Carrier Gas - He @ 20 cc/rrin Scan - 20 AMU to 100 AMU in 4 sec. 1' r oc iuiu re Siandards of acrolein and acrylonitrile were injected to determine retention times and obtain good quality spectra. Detection limits were estimated by injecting aqueous standard solutions and obtaining mass chromatograms at 53 and 56 AMU. The samples wore run, and the recon structed ion and selected ion chromatograms were examined. SAL 000088.133 Technical Service Report No. 43 5-81-839-') P;,go 3 Discussion of Results Tin.' dot net ion limits worn about the same as those reported in TSR 429-81804-8, and those limits am determined by the level of inLcrJerences rather than instrumental limitations. When water elutes from a column, it apparently "steam strips" organic impurities along with it. This is a commonlv observed phenomenon in gas chromatography. In this case the elution of water generated a very broad peak which encompassed the elution range "I acrolein and acrylonitrile. The spectra of Lhc organic peaks throughout the broad peak were similar to background spectra taken before' and after the peak. The generation of this peak seemed to result from a general increase of background intensities. These spectra contained peaks at. every mass number. Therefore, the mass chromatograms, regardless of the ion selected, had a high noise background and the same general appearance as the reconstructed ion chromatogram. Mass chromatograms at 53 and 56 AMU, the base peaks for acrylonitrile and acrolein, did not reveal any peaks above the noise background. The amounts present., if any, are certainly less than 1 ppm for either pollutant. In this work there was no evidence of a peak with the same retention time as acrolein (see TSR 829-81-804-8). The peak observed with the FID was probably an artifact peculiar to the chromatographic system used. Relorence: TSR 824-81-804-8 C. B. Herrin Research Group Supervisor Gas Chromatography Croup Analytical Research Section KW Copy to Library SAL 000088134