Stability of selenium and its speciation analysis in water using automatic system separation and HR-ICP-MS measurement

摘要

A simple and convenient method has been developed for the pre-concentration and separation of inorganic selenium species from environmental water samples using anion exchange chromatographic column combined with high resolution inductively coupled plasma mass spectrometry(HR-ICP-MS)measurement.^(75)Se(Ⅳ) and ^(75)Se(Ⅵ)were prepared and used as tracers during the experiments.The volatility of selenium during solution evaporation was investigated to establish a reliable water samples pretreatment procedure.The parameters which affect the uptake of Se(Ⅳ)and Se(Ⅵ)on Dowex1×8 resin was optimized and the procedure for Se(Ⅳ)and Se(Ⅵ)separation was proposed.Both Se(Ⅳ)and Se(Ⅵ)are retained on the column in natural or alkaline solution with high distribution coefficient.The successive gradient elution of pre-concentrated species of selenium with HNO_(3)solution allows to differentiate between them.Se(Ⅳ)and Se(Ⅵ)finally were eluted with 0.05 mol/L HNO_(3) and 5.0 mol/L HNO_(3),respectively.The proposed method has been successfully verified using the certified reference materials(CRMs)of real water samples,and spiked recoveries for real samples were 98%-104%with 5%relative standard deviations(RSDs).The developed procedure is proved to be reliable and can be used for the rapid determination of selenium species in environmental water samples.