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目的建立土壤中形态砷的高效液相色谱-氢化物发生-原子荧光光谱分析方法。方法采用磷酸-盐酸混合浸提体系和超声振荡提取土壤中不同形态的砷。阴离子交换柱分离,高效液相色谱-氢化物发生-原子荧光光谱法测定,保留时间定性,峰面积定量。结果该方法线性相关系数均大于0.999。三价砷、五价砷、一甲基砷和二甲基砷的测定范围分别为0.5 mg/kg~28.0 mg/kg、1.2 mg/kg~21.0 mg/kg、0.3 mg/kg~20.8 mg/kg和0.6 mg/kg~29.2 mg/kg。平均回收率达到96.2%~101.6%,日内精密度(RSD)≤3.7%,日间精密度(RSD)≤6.5%。3种污泥土壤样品均检测到三价砷和一甲基砷,浓度范围分别为1.3 mg/kg~6.2 mg/kg和3.7 mg/kg~9.1 mg/kg之间,五价砷和二甲基砷均低于检测限。结论本法灵敏、准确、精密度好,适于土壤中砷的形态分析。
Objective To establish a method for the determination of arsenic in soil by high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry. Methods Phosphoric acid - hydrochloric acid mixed extraction system and ultrasonic oscillation were used to extract different forms of arsenic in soil. Anion exchange column separation, high performance liquid chromatography - hydride generation - atomic fluorescence spectrometry, retention time qualitative, peak area quantification Results The linear correlation coefficients of the method were all greater than 0.999. Trivalent arsenic, pentavalent arsenic, monomethyl arsenic and dimethyl arsenic were measured in the range of 0.5 mg / kg to 28.0 mg / kg, 1.2 mg / kg to 21.0 mg / kg, 0.3 mg / kg to 20.8 mg / kg and 0.6 mg / kg to 29.2 mg / kg. The average recovery rate reached 96.2% ~ 101.6%, intraday precision (RSD) ≤3.7%, intraday precision (RSD) ≤6.5%. Trivalent arsenic and monomethyl arsenic were detected in the three kinds of soil samples. The concentrations ranged from 1.3 mg / kg to 6.2 mg / kg and from 3.7 mg / kg to 9.1 mg / kg. Arsenic were lower than the detection limit. Conclusion The method is sensitive, accurate and precise, and is suitable for the speciation analysis of arsenic in soil.