Identification of hydrogen selenide and other volatile selenols by derivatization with 1-fluoro-2,4-dinitrobenzene.
A procedure is described for the trapping and identification of hydrogen selenide and methyl selenol ( CH3SeH ). The volatile selenols were generated by reducing selenious acid or dimethyldiselenide with Zn dust and hydrochloric acid under a stream of nitrogen and passing into a trapping solution composed of 50 mM 1-fluoro-2,4-dinitrobenzene plus 83 mM sodium bicarbonate in 67% dimethylformamide:33% water. The selenols react rapidly to form stable dinitrophenyl (DNP) selenoethers that can be extracted into benzene; these are easily identified by TLC, HPLC, or mass spectrometry. Hydrogen selenide is trapped in 90-99% yield, primarily as the di-DNP- monoselenide with a trace of di-DNP- diselenide .
D002851:Chromatography, High Pressure Liquid; D004139:Dinitrofluorobenzene; D013058:Mass Spectrometry; D000432:Methanol / Q000031:analogs & derivatives* / Q000032:analysis; D008722:Methods; D009578:Nitrobenzenes; D016566:Organoselenium Compounds; D012643:Selenium / Q000032:analysis*; D018036:Selenium Compounds; D012997:Solvents; D014835:Volatilization
D009578:Nitrobenzenes; D016566:Organoselenium Compounds; D018036:Selenium Compounds; D012997:Solvents; C019003:methaneselenol; D004139:Dinitrofluorobenzene; D012643:Selenium; C026372:hydrogen selenide; D000432:Methanol