F. Sherman et al., DETERMINATION OF WATER SAMPLES AND ENE-DIOLS OR THIOLS IN SAMPLES INACCESSIBLE FOR DIRECT K.FISCHER TITRATION, Talanta, 43(7), 1996, pp. 1035-1042
Novel reagents and the rapid technique were developed for the simultan
eous determination of water and ene-diols or thiols in chemical produc
ts, drugs and other materials which are inaccessible for direct K.Fisc
her titration. The reagents consist of iodine, tetramethylammonium iod
ide 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 consecut
ive 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 doub
le burette and electrometric location of the end point in both titrati
ons. The time for both titrations is 8-15 min.