电感耦合等离子体质谱法测定大批量钼多金属矿中钼及4种主要伴生元素的含量  

Determination of Molybdenum and 4 Major Associated Elements in Large-Scale Molybdenum Polymetallic Ores by Inductively Coupled Plasma Mass Spectrometry

作　　者：贾雷 李俊东 黄青春 祁伟 何文江 左修源 JIA Lei;LI Jundong;HUANG Qingchun;QI Wei;HE Wenjiang;ZUO Xiuyuan(Hohhot General Survey of National Resources Center,China Geological Survey,Hohhot 010010,China;Liaoning Provincial Key Laboratory of Synthesis and Separation of Chemical Additives,School of Chemistry and Environmental Engineering,Yingkou Institute of Technology,Yingkou 115014,China)

机构地区：[1]中国地质调查局呼和浩特自然资源综合调查中心,呼和浩特010010 [2]营口理工学院化学与环境工程学院辽宁省化学助剂合成与分离重点实验室,营口115014

出　　处：《理化检验（化学分册）》2024年第3期260-265,共6页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：营口理工学院引进人才科研启动经费项目(YJRC202105);营口理工学院第四批产教融合项目(2023CJRH0410)。

摘　　要：目前采用电感耦合等离子体质谱法(ICP-MS)测定大批量常量元素时存在检测器信号强、稳定性差、准确度低等问题,为此优化了分析条件,提出了题示方法。取0.05 g样品,用少量水润洗,加入4 mL硫酸和8 mL硝酸的混合溶液,混匀后,于250℃加热18 h蒸干溶液,冷却至室温,用3~4 mL的10%(体积分数)硝酸溶液溶解,并用水定容至25 mL,利用自动稀释系统将样品溶液稀释100倍后采用ICP-MS测定其中Mo、W、Cu、Zn、Ag的含量,以0.6 mL·min^(-1)的稀释气流量来降低物理干扰。结果表明,5种元素的质量浓度在1.00 mg·L^(-1)内与对应的响应值呈线性关系,检出限(3 s)为0.006~0.201 mg·kg^(-1)。方法用于分析钼矿石国家标准物质GBW 07142、GBW 07143,测定值与认定值基本一致,测定值的相对标准偏差(n=8)均小于8.0%。仪器稳定性试验表明,进行大批量长时间测试时,需及时重新更换零件和重新校正标准曲线。At present,there were some problems with strong detector signal,poor stability,and low accuracy to determine large-scale of constant elements by inductively coupled plasma mass spectrometry(ICP-MS).Therefore,the analytical conditions were optimized and the method mentioned by the title was proposed.0.05 g of the sample was taken and rinsed with a small amount of water,and a mixture of 4 mL of sulfuric acid and 8 mL of nitric acid was added.After mixing well,the solution was heated to dryness at 250℃for 18 h.After cooling to room temperature,the residue was dissolved in 3-4 mL of 10%(volume fraction)nitric acid solution,and made its volume up to 25 mL with water.The sample solution was diluted 100 times with an automatic dilution system,in which Mo,W,Cu,Zn,and Ag were determined by ICP-MS,reducing physical interference with a dilution gas at flow rate of 0.6 mL·min-1.As shown by the results,linear relationships between the corresponding response values and mass concentrations of 5 elements were found within 1.00 mg·L^(-1),with detection limits(3 s)of 0.006-0.201 mg·kg^(-1).This method was used to analyze the national standard substances GBW 07142 and GBW 07143 for molybdenum ores,and the determined values were basically consistent with the certified values,with RSDs(n=8)of the determined values less than 8.0%.It was shown by the instrument stability test that it was necessary to replace parts and recalibrate the standard curve in a timely manner when conducting large-scale and long-term tests.

关 键 词：钼矿石 Mo W Cu Zn Ag 电感耦合等离子体质谱法(ICP-MS) 

分 类 号：O657.63[理学—分析化学]