电感耦合等离子体质谱(ICP-MS)法测定闪长岩中的高场强元素  

Determination of High Field Strength Elements in Diorite by Inductively Coupled Plasma Mass Spectrometry

作　　者：黎卫亮[1] 王鹏[1] 程秀花[1] 李忠煜[1] 赵江华[1] 吴婷 朱津蕊 张明祖[1] LI Weiliang;WANG Peng;CHENG Xiuhua;LI Zhongyu;ZHAO Jianghua;WU Ting;ZHU Jinrui;ZHANG Mingzu(Xi′an Geological Survey Center of China Geological Survey,Xi′an,Shaanxi 710019,China)

机构地区：[1]中国地质调查局西安地质调查中心,西安710019

出　　处：《中国无机分析化学》2024年第10期1425-1430,共6页Chinese Journal of Inorganic Analytical Chemistry

基　　金：陕西省科技计划项目(2021JQ-327)。

摘　　要：闪长岩中高场强元素主要赋存在难溶的矿物(角闪石、锆石等)中。采用常规的密闭酸溶法导致高场强元素特别是锆、铪元素溶出率偏低。针对这一问题,根据高场强元素的赋存状态,首先增加预消解过程,其次对溶解样品所需试剂添加量(氢氟酸、硝酸)以及消解时间设计了3因素3水平的正交实验,从而得到最佳试剂添加量为2 mL氢氟酸和1 mL的硝酸,消解时间为36 h,影响高场强元素溶出率的最主要因素是氢氟酸。以在最佳前处理实验方案下溶样,在所溶解完全的溶液介质中添加浓度为0.1%的盐酸(体积比),以保证高场强元素在溶液里的稳定性。建立的方法用于北山地区闪长岩样品分析,并与碱熔、X射线荧光光谱法测定值对比,分析结果具有良好的一致性,方法检出限0.004~2.5μg/g,相对标准偏差1.5%~8.4%,加标回收率93.0%~108%。实现了闪长岩中高场强元素的准确分析。The high-field-strength elements in diorite mainly occur in insoluble minerals(hornblende,zircon,etc.).The recoveries of high-field-strength elements,especially zirconium and hafnium,are low due to the conventional sealed acid digestion method.To solve this problem,according to the occurrence state of high-field-strength elements,this study added the pre-digestion process,and designed three-factor and three-level orthogonal experiment includeing the amount of reagents(hydrofluoric acid,nitric acid) and the digestion time.According to the experiment,the optimal reagent addition amount was 2 mL hydrofluoric acid and 1 mL nitric acid,and the digestion time was 36 hours.The most important factor affecting the recoveries of high field strength elementswas hydrofluoric acid.This study added 0.1% hydrochloric acid(volume ratio) to the dissolved solution to ensure the stability of high field strength elements.High-field-strength elements contents of diorite in the Beishan area were determined by the method,which was consistent with the results determined by alkali fusion and X-ray fluorescence methods.Detection limits of the method were in the range of 0.004-2.5 μg/g with relative standard deviations of 1.5%-8.4% and recoveries of 93.0%-108%.As a result,accurate analysis of high-field-strength elements in diorite is realized.

关 键 词：电感耦合等离子体质谱 高场强元素 闪长岩 

分 类 号：O657.63[理学—分析化学]