稀氨水密封溶解—电感耦合等离子体质谱测定土壤沉积物及生物样品中的碘溴

介绍了一个适合于电感耦合等离子体质谱直接测定土壤、沉积物和生物样品中碘、溴的快速简单的样品前处理方法。样品在φ(NH3·H2O)=10%的水溶液中,于190℃下密封分解18h,溶液适当稀释后放置澄清,用电感耦合等离子体质谱法直接测定溶液中的碘、溴。选用126Te作为内标,补偿基体效应和仪器漂移对分析结果的影响。碘、溴的方法检出限(10σ,DF=100)分别为0.01μg/g、0.04μg/g。用土壤、水系沉积物以及头发等标准物质验证了方法的准确度及精密度,绝大多数样品分析结果在标准值的允许误差范围内。对国家一级标准物质10次测定的RSD为2.0%～8.6%。但方法分析岩石样品结果偏低,不适用于岩石样品的分析。     

A Rapid Acid Digestion Technique for the Simultaneous Determination of Bromine and Iodine in Fifty‐Three Chinese Soils and Sediments by ICP‐MS

Bromine and iodine are important tracers for geochemical and environmental studies. In this study, a rapid acid digestion (HNO₃ + HF) with ammonia dilution for the simultaneous determination of bromine and iodine in soils and sediments using ICP‐MS was developed. The recoveries of Br and I were controlled by the synergic effect of temperature and time. It took only 15 min at 140 °C for the complete recovery of Br and I in sediment (GSD‐2) and soil (GSS‐24) reference materials, which is a process that needs 2–6 h at 90 °C. A serious loss of Br and I was found at a higher digestion temperature of 190 °C. A 5% v/v NH₄OH dilution effectively eliminated the memory effects and stabilised the signals of Br and I. Moreover, ammonia dilution also avoided the corrosiveness of HF on the sample introduction system and torch of ICP‐MS. Tellurium is a more suitable internal standard element than In in the ammonia medium. To avoid the adsorption of residues of dissolution on Te, addition of Te should be carried out after centrifuging the solution. The developed method was successfully applied to determine Br and I in fifty‐three Chinese soil and sediment reference materials. This simple method shows great potential for the rapid determination of Br and I in large batches of geological and environmental samples commonly analysed for mineral exploration and environmental geochemistry studies.