为给铌、钽资源勘查和开发提供分析测试技术支撑,基于地球化学样品中铌、钽的特殊化学性质,应用电感耦合等离子体质谱技术(ICP-MS),对地球化学样品中铌、钽的检测方法进行了深入研究.结果表明:样品溶液制备和仪器测定参数对检测效果有重要影响,特别是前者,因此优化样品溶液制备的重要参数是检测技术的关键所在,试验选定条件是:试样重量为50　mg;氢氟酸用量为15　mL;样品溶液中硝酸、酒石酸浓度分别为2%和1.5%;溶液有效测定期限≤1　d.优化并确立的检测方法经国家一级地球化学标准物质验证,其准确度、精密度均达到行业标准的要求.方法检出限分别为Nb:1.05 μg·g-1和Ta:0.13　μg·g-1.实验研究证明:应用特定的样品溶液制备流程,并结合ICP-MS技术适用于地球化学样品中铌、钽的准确快速检测,尤其是样品量较大且铌、钽含量较低的地球化学勘查样品.

In order to provide the test analysis technology to support the exploration　and development of niobium and tantalum resource,based on the special chemical properties of Nb and Ta in geochemical sample,we studied the detection methods for the content of Nb and Ta in geochemical sample by using inductively coupled plasma mass spectrometry (ICP-MS).The results show that the sample dissolution and instrumental parameter of ICP-MS,especially the former have significant　influence?on detection results.Therefore,optimizing important parameters of sample dissolution is the key of the detection technology.The optimal parameters are that:the weight of sample is 50　mg;the dosage of HF acid is 15　mL;the concentration of nitric acid and tartaric acid in the sample solution is 2% and 1.5%,respectively;the validity period of detection for sample solution ≤1　d.The detection method has been validated by the national geochemistry standard reference material.The precise and exaction of method meet the required of industry standards.The detection limits of method for Nb and Ta are 1.05 and 0.13　μg·g-1,respectively.The experiment proved that the ICP-MS detection methods,which using certain preparation process of sample solutions,is suitable for accurate and rapid　determination of Nb and Ta in geochemical sample,especially geochemical survey samples which with a large　amount and low　content　of　Nb and Ta.