Determination of water samples and ene-diols or thiols in samples inaccessible for direct K.Fischer titration

摘要

Novel reagents and the rapid technique were developed for the simultaneous determination of water and ene-diols or thiols in chemical products, drugs and other materials which are inaccessible for direct K.Fischer titration. The reagents consist of iodine, tetramethylammonium iodide or potassium iodide, base (diethanolamine, triethanolamine, sodium acetate and/or urea) in methanol mixed with N,N-dimethylformamide, or with formamide, or with dimethyl sulfoxide and N,N-dimethylformamide mixture as a solvent. The use of the reagents is based on the consecutive titration first of an ene-diol or thiol by the novel reagents and then of water by a conventional K.Fischer reagent in the same cell in a titration system protected from water vapour and oxygen, with a double burette and electrometric location of the end point in both titrations. The time for both titrations is 8–15 min.