树脂交换分离-电感耦合等离子体质谱法测定土壤中碘硼锗锡砷锑铌钽钨

Determination of iodine,boron,germanium,tin,arsenic,antimony,niobium,tantalum and tungsten in soil by ICP-MS with resin exchange separation

在土地质量评估分析的配套方法中,碘、硼、锗、锡、砷、锑、铌、钽、钨主要采用分组或者单元素分析的方法,分析效率低、成本高、劳动强度大。本实验建立了ICP-MS同时测定土壤样品中碘硼锗锡砷锑铌钽钨的方法。样品采用过氧化钠熔解,使难溶性锡、钨等元素分解完全,经过热水提取后加入铼内标,分取溶液后加入0.8%的柠檬酸溶液络合锡、钨等元素形成金属复合物,加入阳离子交换树脂分离高含量的钠盐及铁等大部分阳离子,使含盐量满足仪器分析的要求。经树脂交换后,钾钙钠镁铜铅锌铁铝的去除率达95%以上,基本消除了主量元素的干扰。碘硼锗锡砷锑铌钽钨的方法检出限分别为0.33μg/g、0.92μg/g、0.055μg/g、0.37μg/g、0.42μg/g、0.035μg/g、0.77μg/g、0.082μg/g、0.45μg/g,用土壤国家一级标准物质对该方法进行验证,各元素的△logc均小于0.1,相对标准偏差(RSD,n=6)≤5%,满足DZ/T 0258-2014《多目标区域地球化学调查规范1∶250000》要求。该方法具有简单快速等优势,在实际应用中得到满意的结果。

Sodium peroxide was used to completely decompose the insoluble tin,tungsten and other elements in soil samples.After hot water extraction,rhenium internal standard was added.Separating the solution,0.8%citric acid solution was added to complexing tin,tungsten and other elements to form metal complex.Cation exchange resin was added to separate most cations such as sodium salt and iron.The detection limits for iodine,boron,germanium,tin,arsenic,antimony,niobium,tantalum and tungsten were 0.33μg/g,0.92μg/g,0.055μg/g,0.37μg/g,0.42μg/g,0.035μg/g,0.77μg/g,0.082μg/g and 0.45μg/g,respectively.The method was verified by reference materials of soil.The△logc of each element was less than 0.1,and the relative standard deviation was less than 5%,which met the requirements of DZ/T 0258-2014 Specification for Multi-purpose Regional Geochemical Survey(1∶250000).This method has the advantages of simplicity and rapidity.