高效液相色谱法分离检测亚氯酸盐与硫氧化合物混合物

Separation and Analysis of Chlorite and Sulfur Oxyanions in Mixture Using High Performance Liquid Chromatography

采用反相离子对高效液相色谱法对亚氯酸盐、硫代硫酸盐、亚硫酸盐及连多硫酸盐混合物进行了分离。采用Phenomenex Gemini C18分析柱(250mm×4.6mm,5μm),乙腈-水(含四丙基氢氧化铵(TPAOH)离子对试剂)作为流动相,利用紫外检测器在230nm处对各物质进行分离检测。当流动相组成为:乙腈-7.0mmol/LTPAOH水溶液(15∶85,V/V,pH5～9),流速为1.0mL/min时,各物质在15min内都可以得到完全分离。用此方法对亚氯酸盐-硫代硫酸盐反应过程中各物质进行跟踪检测,并进行动力学分析,在亚氯酸盐过量的准一级条件下,测得pH9.0时,亚氯酸盐-硫代硫酸盐反应体系的速率常数为9.75×104(mol/L)-2s-1,这与文献报道的结果相符。

A reversed phase ion-pair high performance liquid chromatographic method has been used for the separation of chlorite,thiosulfate,sulfite and polythionate in mixture.The separation of the species was accomplished on a Phenomenex C18 column（250 mm×4.6 mm,5μm） with an acetonitrile-water containing tetrapropylammonium hydroxide（TPAOH） ion-pairing reagent as mobile phase and the ultraviolet absorption detection was used for the determination of each species at 230 nm.When an acetonitrile-water（15∶85,V/V） solution（pH 5-9） containing 7 mmol/L TPAOH was used as a mobile phase at flow-rate of 1.0 mL/min,all compounds could be completely separated.The method can be applied to the separation and analysis of sulfur oxyanions and chlorite,and also to kinetic analysis between chlorite and thiosulfate.The rate constant of the reaction between chlorite and thiosulfate was determined to be 9.75×10 4（mol/L） -2 s-1,which was consistent with the result reported in the literature.