摘要
钼酸铵中痕量杂质的准确测定是产品质量控制的关键,为了向钼酸铵质量检测和产品控制提供可靠的数据支撑,采用在线加入内标–电感耦合等离子体质谱法(ICP-MS)分析钼酸铵中镁、铝、钙、铬、铁、锰、镍、铜、砷、镉、锑、铅12种痕量元素的含量.利用盐酸–硝酸–氢氟酸溶解样品,对比探究了气溶胶稀释法、基体匹配和在线内标法消除基体干扰的效果,最终使用在线加入多种内标法以消除高纯钼基体带来的干扰.试验结果表明,各元素标准曲线的线性相关系数均大于0.9990,检出限为0.008~0.2 ng/mL,相对标准偏差在0.10%~0.38%范围内,各元素的加标回收率为90%~108%,并且有效消除了基体干扰.同时将样品送至权威的外检机构,测试结果均在允差范围内,表明方法准确度高、精密度好,满足市场上对钼酸铵产品中痕量杂质元素含量的准确检测需求.
Accurate determination of trace impurities in ammonium molybdate is the key to product quality control.In order to provide reliable data support for the quality testing and product control of ammonium molybdate,the contents of trace elements Mg,Al,Ca,Cr,Fe,Mg,Ni,Cu,As,Cd,Sd and Pb in ammonium molybdate were analyzed by online internal standard-inductively coupled plasma mass spectrometry(ICP-MS).The samples were dissolved in hydrochloric acid-nitric acid-hydrofluoric acid.The effectiveness of aerosol dilution,matrix matching and online internal standard methods for matrix interference elimination were compared.Finally,an online addition of multiple internal standards was used to eliminate the interference caused by the high purity molybdenum matrix.The results showed that the linear correlation coefficients were all greater than 0.9990,the limits of detection were 0.008~0.2μg/g,the relative standard deviations were 0.10%~0.38%,the recoveries were in the range of 90%~108%,and the matrix effect was effectively eliminated.At the same time,the samples were sent to the authoritative external inspection agency,and the test results were within the allowable range,indicating that the method had a high accuracy and good precision,and met the requirements for accurate detection of trace impurity elements in ammonium molybdate products on the market.
作者
肖子廉
李玲君
XIAO Zilian;LI Lingjun(Dexing Copper Mine,Jiangxi Copper Corporation Limited,Dexing 334224,Jiangxi China)
出处
《分析测试技术与仪器》
2025年第1期45-54,共10页
Analysis and Testing Technology and Instruments
