A simple and quick on-line derivatization method for the gas chromatographic trace analysis of 13 carbamate pesticides in water is described. Sample preparation consisted of solid-phase extraction with RP C18 cartridges. Trimethylsulfonium hydroxide solution was added to the concentrated eluate, and an aliquot of the mixture was injected in a programmed temperature vaporizer (PTV) at 60 eC. After solvent purging and a subsequent heating step, carbamate pesticides underwent methylation in the PTV, and the derivatives were separated, detected, and quantitated using high-resolution gas chromatography/mass spectrometry. The average recoveries at four concentration levels in water (25, 50,100, and 200 ng/L) ranged from 46 to 104% with determination limits of 25 and 50 ng/L, depending on the compounds.

Die Halogensilanabspaltung aus den Diorganyl‐(trimethylsilylmethyl)‐ phosphinen (III) und den Chlorophenylphosphinen (IIa) oder (IV) bzw. Chlorodiphenylarsin (IIb) werden die Diphosphinomethan‐Derivate (Ia), das erste methylenverbrückte Triphosphin (V) bzw. das Phosphinoarsinomethan (Ib) gewonnen.

Die Verfasser demonstrieren an einer Vielzahl von Beispielen, daß Hexachloräthan (II) ein gutes und leicht zu handhabendes Chlorierungsmittel für Phosphin (I) ist.

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Die Titelverbindung (II) reagiert mit Chlorodiphenyl‐, Methyldiphenyl‐ und Phenyldipropylphosphin zu den unterschiedlich substituierten Salzen (I), (III) und (IV) mit einem P‐C‐ P‐Gerüst.