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采用高效液相色谱-氢化物发生原子荧光光谱联用测定了北京大气颗粒物中As(III),As(Ⅴ),二甲基砷酸(DMA)和一甲基砷酸(MMA)的含量。研究了仪器条件、流动相组成和梯度洗脱程序对砷形态分离的影响。实验结果显示,在优化的色谱与氢化原子荧光检测条件下,采用pH6.0,浓度为10 mmol/L和200 mmol/L NH4H2PO4为流动相A和B,在1~3 min内用60%的A和40%的B洗脱使砷的4种形态达到最佳分离效。As(III),As(Ⅴ),DMA和MMA的检出限为1.45,1.22,1.91和1.64 mg/L,回收率为90.5%~93.2%,相对标准偏差为0.38%~1.7%。方法适用于大气颗粒物中砷的形态分析研究。
The content of As (III), As (Ⅴ), dimethyl arsenate (DMA) and monomethylarsenic acid (MMA) in Beijing atmospheric particulates were determined by high performance liquid chromatography-hydride generation atomic fluorescence spectrometry. The effects of instrument conditions, mobile phase composition and gradient elution program on the separation of arsenic species were studied. The experimental results showed that under the optimized conditions of fluorescence and hydrogen fluoride detection, the mobile phases A and B were prepared with pH6.0, 10 mmol / L and 200 mmol / L NH4H2PO4, and 60% A and 40% of B eluted the four kinds of arsenic to achieve the best separation efficiency. The detection limits of As (III), As (Ⅴ), DMA and MMA were 1.45, 1.22, 1.91 and 1.64 mg / L, respectively. The recoveries were 90.5% -93.2% with relative standard deviations of 0.38% -1.7%. The method is suitable for the speciation analysis of arsenic in atmospheric particulates.