HUMIDITY, TEMPERATURE, AND OTHER PARAMETER STUDIES ON THE QUANTITATION OF ACRYLONITRILE IN AMBIENT AIR (SOLID SORBENT, TRACE ORGANIC POLLUTANT ANALYSIS)

We have developed and validated the solid sorbent system Ti(IV)-exchanged zeolite 3A for ambient industrial site monitoring of acrylonitrile (AN) at trace PPM levels. In earlier work (M.S. Thesis) it was found that Titanium (IV)-exchanged zeolite 3A preconcentrated the AN favorably down to 0.1 PPM under nitrogen atmosphere by polymerization to polyacrylonitrile (PAN). Transmission IR was used for AN detection employing solid KBr pellet technique. Proton FT-NMR detected PAN at lower sensitivities than transmission IR. Working under ambient atmospheric conditions, however, neither transmission IR or proton FT-NMR were successful in detecting PAN or AN below 700 ug. HPLC using a 250 mm cyano column with UV detector retained the AN but because of the small sampling size and possible on column polymerization reactions, this method was abandoned. Nitrogen (PPM) elemental analysis was investigated for quantitative use, but was found to be nonspecific for AN detection. For final quantitation purposes for AN preconcentration at 25 and 12 ug, high resolution EC/CI Mass Spectrometry with packed column GC was employed. Cointerferent studies were conducted at 25 ug preconcentrated Acrylonitrile. For example, analogous compounds of Acrylonitrile, ambient air conditions typical of the manufacturing environment, and humidity effects were investigated. Short term storage conditions were also examined. Breakthrough phenomena was experienced, and to obtain high percentage yields, backup beds were needed depending upon the concentration rate being studied. In future field monitoring operations, the Ti(IV)-3A can be used in a personal device or stationary point source to detect AN in PPB ranges.