以H3PO4为提取剂,利用高效液相色谱与氢化物发生原子荧光光谱联用(HPLC-HG-AFS)实现了大气颗粒物中砷形态的温和提取测定,并通过标准样品的形态加标实验确定了最佳提取方法。在优化的色谱及光谱条件下,AsⅢ,AsⅤ,MMA(甲基胂酸)和DMA(二甲基胂酸)均可达基线分离,其方法检出限分别为1.40,1.26,1.97和1.16 mg/L,RSDs〈2%(n=5)。形态加标后的西藏土壤成分分析标准物质(GBW08302)经1.0 mol/L H3PO4超声提取40 min,各形态的提取效率均达到或接近90%,且无明显的形态转化。利用本方法对北京某地区大气颗粒物中砷的形态进行测定,确定砷的主要存在形式为无机砷AsⅢ和AsⅤ。
With phosphoric acid as the extractant,arsenic species in atmospheric particles,including AsⅢ,AsⅤ,monomethylarsonic acid(MMA) and dimethylarsinic acid(DMA),were gently extracted and detected by high performance liquid chromatography conjugated hydride generation atomic fluorescence technique(HPLC-HG-AFS).The original arsenic species contents and the spiking species of the standard material(GBW 08302) were determined to seek the best extraction method.Under the optimized chromatographic and spectrographic conditions,the arsenic species were baseline separated,with the RSDs2%(n=5).The method detection limits of As,As,MMA and DMA were 1.45,1.26,1.97 and 1.16 mg/L,respectively.After ultrasonic extraction 40 min with 1 mol/L phosphoric acid,the extraction efficiency of arsenic species in the spiked standard material achieved 90% without speciation transformation.The developed method was applied to the determination of arsenic species concentration in the atmospheric particles.The results showed that the main arsenic species in one place of Beijing were AsⅢand AsⅤ.