||Micro Derivatization Technique for the Confirmation of Trace Quantities of Kepone.
Moseman, Robert F. ;
Ward, M. Keith ;
Crist, Howard L. ;
Zehr, Robert D. ;
||Health Effects Research Lab., Research Triangle Park, NC. Environmental Toxicology Div.
Chemical analysis ;
Trace elements ;
Chlorine organic compounds ;
Gas chromatography ;
Electron capture gas chromatography ;
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A rapid and simple procedure has been devised for the confirmation of nanogram quantities of Kepone that is sensitive to part per billion levels in environmental and biological samples. Electron-capture gas chromatography of the perchlorinated derivative enabled confirmation often not possible by other techniques such as gas chromatography combined with mass spectrometry. Conversion of Kepone to mirex was accomplished by a high-temperature closed-tube reaction. Mirex that might have been present in the original sample extract was separated from Kepone by a micro Florisil column cleanup step. The absence of mirex in cleaned-up sample extracts was verified during the electron-capture gas chromatographic quantitation for Kepone. The conversion of Kepone to mirex was quantitative, allowing for the estimation of Kepone by a separate technique. Thus, considerable confidence is added to analytical results. Details of the methodology and results obtained are discussed.