地质样品中微量元素的高效测试方法

High Efficiency Determination of Trace Elements in the Geological Samples

设计并加工了具有双内弧密封结构的防腐高效溶样罐，在消解地质样品时，加入内标103-Rh校正样品中元素的浓度，以内标183-Re校正分析信号的漂移，使用电感耦合等离子体质谱测定深海沉积物标准物质和国际地质标准物质中的34种微量元素浓度。与以往消解方法相比，该方法密封性好、酸消耗少，只需1．5m1．浓HF、0．5mL浓HNO3和0．25mL HCIO4就可将40mg地质样品在短时间内消解完全，消解效率高。前处理过程中加入内标103-Rh，样品稀释时无需准确定容，节省操作时间。方法检测下限为0．001～0．62lμg／g，精密度（RSD，n=10）小于5％，准确度小于6．5％（其中大多数元素小于3％），适用于多种地质样品中多元素的分析。

A method for determining 34 trace elements in deep-sea marine sediments and in- ternational geological samples by ICP-MS was proposed. Samples were digested in anticor- rosive efficient digestion vessel, which had a double inner arc seal design. The internal standard 103Rh was used to calibrate the trace element concentrations, and the internal standard 185 Re was selected to compensate the drift of analytical signals. Compared with previous digestion methods, this method used less acid in a good seal condition, only 1. 5 mL HF, 0.5 mL HNO3 and 0.25 mL HC104 can digest 40 mg geological samples completelyin a short time. Because the internal standard 103Rh was added process, so there was no need to dilute the digested sample to an saved a lot of time. This method detection limits are 0. 001-0.62 precisions （RSD, n=10） are less than 6.5%, and the relative err the recommend values are less than 5%, in which most are less t during the pre-treatment accurate volume, and thus 1 μg/g, the determination ors between this work and han 3%. This method can in many geological