地质样品中微量元素的高效测试方法

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¹⁰³Rh校正样品中元素的浓度，以内标¹⁸⁵Re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1.5 mL浓HF、0.5 mL浓HNO₃和0.25 mL HClO₄就可将40 mg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¹⁰³Rh，样品稀释时无需准确定容，节省操作时间。方法检测下限为0.001~0.621 μg/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。

High Efficiency Determination of Trace Elements in the Geological Samples

A method for determining 34 trace elements in deep-sea marine sediments and international geological samples by ICP-MS was proposed. Samples were digested in anticorrosive 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 ¹⁸⁵Re 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 HClO₄ can digest 40 mg geological samples completely in a short time. Because the internal standard ¹⁰³Rh was added during the pre-treatment process, so there was no need to dilute the digested sample to an accurate volume, and thus saved a lot of time. This method detection limits are 0.001-0.621 μg/g, the determination precisions (RSD, n=10) are less than 6.5%, and the relative errors between this work and the recommend values are less than 5%, in which most are less than 3%. This method can meet the requirements for analyzing a large number of trace elements in many geological samples.