建立了反相离子对色谱(RPIPC)与电感耦合等离子体质谱(ICP—MS)联用技术快速分离测定水中痕量Cr(Ⅲ)和Cr(Ⅵ)的方法。通过考察流动相的pH值、离子对试剂及甲醇的浓度和EDTA的添加等对不同形态铬的保留时间及分离度的影响,确定当流动相组成为2.0mmol/LTBA,5%(V/V)甲醇,pH=5.5时,Cr(Ⅲ)与Cr(Ⅵ)可达最佳分离。ICP—MS测定时选用碰撞池技术以消除40Ar^12^+与^35Cl^16OH^+对^52Cr^+的谱学干扰;进样100μL时,Cr(Ⅲ)与Cr(Ⅵ)的检出限分别为0.15μg/L和0.16μg/L。加标回收率在93.6%~106.2%之间;RSD〈4%(n=3)。以本方法分析了某市自来水、雨水及某品牌纯净水中Cr(Ⅲ)与Cr(Ⅵ)的含量,结果令人满意。
A method was developed to simultaneously determine trace chromium species in water using ionpairing reversed phase chromatography (RPIPC)-inductively coupled plasma mass spectrometer (ICP-MS). The chromatographic parameters were optimized to get the best separation, including the pH value of mobile phase, the concentrations of ion-pair reagent and methanol and the addition of EDTA in the mobile phase. The optimium mobile phase was 2.0 mmol/L tetrabutylammonium(TBA) , 5% methanol(v/v) , pH =5.5. Using collision cell technology to eliminate the mass interferences of 40Ar12C + and 35 Cll6 OH + in the analysis of 52 Cr+ , and the detection limits of Cr( Ⅲ ) and Cr( Ⅳ ) were 0.15 μg/L and 0.16 μg/L for 100μL injections. The recovery range of spiked Cr( Ⅲ ) and Cr( Ⅳ) in water samples was 93.6% - 106.2% and the RSDs were less than 4% (n = 3 ). The results were satisfying when analyzing the chromium speciation in drinking water and rain water using this method.