CAJ | 학술논문

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50mg ；氢氟酸用量为15mL ；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≤1d。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N b：1.05μg · g －1和T a：0.13μg · 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。
위급니、단자원감사화개발제공분석측시기술지탱，기우지구화학양품중니、단적특수화학성질，응용전감우합등리자체질보기술（ICP‐MS），대지구화학양품중니、단적검측방법진행료심입연구。결과표명：양품용액제비화의기측정삼수대검측효과유중요영향，특별시전자，인차우화양품용액제비적중요삼수시검측기술적관건소재，시험선정조건시：시양중량위50mg ；경불산용량위15mL ；양품용액중초산、주석산농도분별위2％화1.5％；용액유효측정기한≤1d。우화병학립적검측방법경국가일급지구화학표준물질험증，기준학도、정밀도균체도행업표준적요구。방법검출한분별위N b：1.05μg · g －1화T a：0.13μg · g －1。실험연구증명：응용특정적양품용액제비류정，병결합ICP‐MS기술괄용우지구화학양품중니、단적준학쾌속검측，우기시양품량교대차니、단함량교저적지구화학감사양품。
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 de‐tection results .Therefore ,optimizing important parameters of sample dissolution is the key of the detection technology .The op‐timal 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 .T he precise and exaction of meth‐od meet the required of industry standards .The detection limits of method for Nb and Ta are 1.05 and 0.13 μg · g -1 ,respec‐tively .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 .