高分辨电感耦合等离子体质谱(HR-ICP-MS)法测定土壤污染状况调查样品中的49种元素

全国重点行业企业用地土壤污染状况调查样品分析工作的特点是项目复杂、配套分析方法种类多,缺乏针对大多数无机元素同时测定的方法。建立了一种基于高分辨电感耦合等离子体质谱法(HR-ICP-MS)的分析方法,采用密闭酸溶消解样品,HR-ICP-MS法测定样品中Li、Be、Ti、V、Cr、Mn、Co、Ni、Cu、Zn、Ga、Ge、As、Rb、Sr、Zr、Nb、Mo、Cd、In、Sn、Sb、Te、Cs、Ba、Hf、Ta、W、Tl、Pb、Bi、Th、U以及稀土元素等49种元素。系统研究了质谱干扰并择优选择了测定元素同位素,采用国家一级有证土壤标准物质对方法性能进行了考察,49种元素方法检出限为0.001~0.46 mg/kg,相对标准偏差(RSD,n=8)为0.75%~8.9%,准确度(相对误差RE,Be、As、Cd、Sb)为-5.4%~7.4%,准确度(对数误差ΔlgC,除Te外其余元素)为-0.05~0.04。方法的主要技术参数满足13个企业用地调查分析标准的要求,可为本次调查工作提供一种可借鉴的高效率分析手段。

Determination of 49 Elements in Samples of the Soil Contamination Investigation by High Resolution Inductively Coupled Plasma Mass Spectrometry

The sample analysis of the soil contamination investigation in nationwide key industry enterprisesis characterized by complex analytes and a variety of analytical methods.However,existing standard methods for soil sample testing suffer from a limitation which lack simultaneous determination aiming at most inorganic elements.Here we report an analytical method to decompose soil samples by HF-HNO3 in a sealed device and determine 49 elements by high resolution inductively coupled plasma mass spectrometry(HR-ICP-MS):Li,Be,Ti,V,Cr,Mn,Co,Ni,Cu,Zn,Ga,Ge,As,Rb,Sr,Zr,Nb,Mo,Cd,In,Sn,Sb,Te,Cs,Ba,Hf,Ta,W,Tl,Pb,Bi,Th,U and REEs.The mass spectral interferences and the selection of measured element isotopes were systematically studied.Furthermore,the method performance was investigated through using national first-class certified soil reference materials.The method detection limits of 49 elements were 0.001—0.46 mg/kg.The range of precision(RSD,n=8)was 0.75%—8.9%.The range of accuracy(RE)for Be,As,Cd and Sb was-5.4%—7.4%and the range of accuracy(ΔlgC)for other elements except tellurium was-0.05—0.04.The results indicate that the main technical parameters of the method meet the requirements of 13 standard methods for soil contamination investigation and the method can provide an efficient means for multi-elements analysis in the investigation work.