基体匹配-电感耦合等离子体质谱(ICP-MS)法测定萤石精矿中痕量有害元素  

Determination of Trace Harmful Elements in Fluorite Concentrate by ICP-MS with Matrix-matching Method

作　　者：谢卫宁 冯培忠[2] 张碧兰 刘亚南 蒯丽君 王帅 伏彩萍 XIE Weining;FENG Peizhong;ZHANG Bilan;LIU Ya′nan;KUAI Lijun;WANG Shuai;FU Caiping(Advanced Analyses&Computation Center,China University of Mining and Technology,Xuzhou,Jiangsu 221116,China;School of Materials Science and Physics,China University of Mining and Technology,Xuzhou,Jiangsu 221116,China;Hunan Shizhuyuan Non-ferrous Metal Limited Ltd.,Chenzhou,Hunan 423037,China;BGRIMM MTC Technology Co.,Ltd.,Beijing 102628,China)

机构地区：[1]中国矿业大学现代分析与计算中心,江苏徐州221116 [2]中国矿业大学材料与物理学院,江苏徐州221116 [3]湖南柿竹园有色金属有限责任公司,湖南郴州423037 [4]北矿检测技术股份有限公司,北京102628

出　　处：《中国无机分析化学》2023年第8期775-782,共8页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家重点研发计划项目(2021YFC2903105)。

摘　　要：为向萤石精矿质量检测和环境监管提供可靠的数据支撑,采用基体匹配-电感耦合等离子体质谱(ICP-MS)法测试萤石精矿中痕量有害元素铜、锌、砷、镉和铅的含量。利用硝酸溶解分析纯碳酸钙后,经ICP-MS测试溶液中钙元素含量与理论值偏差约6%。钙溶液经不同倍率稀释后配制基体浓度为1000、2000和5000 mg/L多元素标准溶液,在ICP-MS测试不同基体浓度混合标准溶液的内标回收率稳定性和一级真空(机械泵抽的采样与截取锥的真空,IF/BK)压降情况后,确定了1000 mg/L的最佳基体浓度。在传统四酸消解法基础上,通过改变加酸顺序、用量和温控水平,实现对萤石精矿的完全消解。消解实验中,同步设置消解加标、过程空白和空白加标实验。萤石精矿在消解定容及适度稀释后,溶液中离子浓度与复杂基体标准溶液的最佳基体浓度接近。在复杂基体标准溶液及样品消解液测试中,采用He模式的碰撞反应池技术,选用^(72)Ge、^(115)In和^(175)Lu作为内标元素。结果显示,各元素标准曲线线性大于0.9995,各样品内标回收率在80.0%~110%波动,表明基体匹配联合内标校正,有效消除了复杂样品测试中的非质谱和质谱干扰。消解实验中未产生过量的元素沉淀或挥发损失,加标样品各有害元素回收率在90.0%~120%。质控样品各元素含量测试误差在15%以内。此测试方法中铜、锌、砷、镉和铅的检出限分别为4.81、8.65、17.91、0.49和2.84μg/L,可满足复杂基体样品中痕量元素含量的准确测试需求。To provide reliable data support for quality inspection of fluorite concentrate and environmental supervision,ICP-MS with the matrix-matching method was applied for the determination of trace harmful elements,such as copper,zinc,arsenic,cadmium,and lead.Analytical pure calcium carbonate was firstly dissolved by nitric acid,and the deviation of calcium content measured by ICP-MS to theoretical value was about 6%.The calcium solution was diluted for various ratios to prepare multi-element standard solutions with matrix concentrations of 1000,2000 and 5000 mg/L.Based on the traditional four acid digestion method,fluorite concentration was digested completely by changing the addition sequence and dosage of acids,and control level of temperature.Digestion with the addition of standard solution,process blank,and blank with the additional standard solution were also set.After the moderate dilution,ion concentration in the digestion solution of fluorite concentration was closet to the optimal one of complex matrix standard solution.In the testing of complex matrix standard solutions and sample digestion solution,collision reaction cell technology within the He mode was used,and ^(72)Ge,^(115)In,and ^(175)Lu were selected as the internal elements.The results showed that the linearity of standard curves for each element was greater than 0.9995,and internal standard recoveries of each sample fluctuates was 80.0%—110%,indicating that the mass and non mass spectrometry interferences were eliminated well by the matrix matching and correction of internal standard during the measurement of complex solution.Excessive elemental precipitation or volatilization loss did not happen in digestion experiments,and the recoveries of harmful elements in samples with the addition of standard solution were 90.0%—120%.Testing error of the content of each element in quality control sample was within 15%.The detection limits for copper,zinc,arsenic,cadmium,and lead were 4.81,8.65,17.91,0.49 and 2.84μg/L,respectively,which can meet the accu

关 键 词：萤石精矿 电感耦合等离子体质谱 基体匹配 干扰校正 

分 类 号：O657.63[理学—分析化学] TH843[理学—化学]