硫化物イオンのHPLCにおける硫化物イオンからのテオシアン酸イオン生成の効果

概要

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A high performance liquid chromatographic method has been developed for determination of unstable sulfide in water samples. It is based on the conversion of sulfide into thiocyanate via a reaction of sulfide with cyanide in the presence of hydrogen peroxide, and on the chromatographic measurement of the thiocyanate with a UV-detector; the thiocyanate was separated as its ion-paired species with terapropylammonium cation (TPA) on a silica ODS column using a mobile phase (pH 5.0) containing 1.5×10^<-2> M TPA and 10 % acetonitrile. The formation of thiocyanate for sulfide determination is useful to stabilize sulfide and also to remove interferences from common anions such as bromide, nitrite and nitrate in water. The conditions for the formation of thiocyanate were investigated using various amounts of sodium hydroxide, cyanide and hydrogen peroxide in reaction solution and standing time for the reaction of sulfide with cyanide. When height of chromatographic peak for sulfide (as thiocyanate) vs. concentration was plotted, calibration graph was linear in the range from the origin up to 1.5×10^<-4> M. The measurement of sulfide as thiocyanate gave higher sensitive determination for sulfide compared with that of sulfide without conversion into thiocyanate.
2005-03-30