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建立了HPLC-ICP-MS联用技术测定土壤中二甲基砷(DMA),一甲基砷(MMA),As5+,As3+的方法。采用Hamilton PRP-X100阴离子交换柱分离砷形态,DMA,MMA,As5+,As3+方法检出限(以As计)分别为0.27,0.28,0.27,0.25μg/L,可满足痕量砷形态的测定。通过对土壤样品砷形态前处理方法的优化,最终确定60℃水浴4 h为土壤砷形态分析的样品前处理方法,加标回收率为74.4%~124%,可保证样品处理过程中砷形态的稳定。对湖南6个土壤样品中砷形态进行了测定,验证了方法的可行性。
A method for the determination of dimethyl arsenic (DMA), monomethyl arsenic (MMA), As5 +, As3 + in soil was established by HPLC-ICP-MS. The detection limit of As (superscript +) by Hamilton PRP-X100 anion exchange column was 0.27,0.28,0.27 and 0.25μg / L, respectively, which could meet the determination of trace arsenic species by DMA, MMA, As5 + and As3 + methods. Through the optimization of the arsenic pretreatment method in soil samples, the sample pretreatment method of soil arsenic speciation analysis at 60 ℃ for 4 h was finally determined, the recoveries were 74.4% -124%, which could ensure the arsenic speciation stable. The arsenic speciation in six soils of Hunan Province was tested to verify the feasibility of the method.