基体匹配-电感耦合等离子体质谱法定量金矿各浮选产物中有害元素  

Determination of Harmful Elements in Flotation Products of a Gold Mine by ICP-MS with the Matrix-Matching Method

作　　者：刘骐榕 楚部 陈树航 贾筱旭 张智航 谢卫宁[1,3] 王帅 冯培忠 LIU Qirong;CHU Bu;CHEN Shuhang;JIA Xiaoxu;ZHANG Zhihang;XIE Weining;WANG Shuai;FENG Peizhong(School of Chemical Engineering&Technology,China University of Mining and Technology,Xuzhou 221116,China;School of Environment and Spatial Informatics,China University of Mining and Technology,Xuzhou 221116,China;Advanced Analyses&Computation Center,China University of Mining and Technology,Xuzhou 221116,China;School of Materials Science and Physics,China University of Mining and Technology,Xuzhou 221116,China)

机构地区：[1]中国矿业大学化工学院,江苏徐州221116 [2]中国矿业大学环境与测绘学院,江苏徐州221116 [3]中国矿业大学现代分析与计算中心,江苏徐州221116 [4]中国矿业大学材料与物理学院,江苏徐州221116

出　　处：《岩矿测试》2024年第6期957-966,共10页Rock and Mineral Analysis

基　　金：国家重点研发计划项目(2021YFC2903105);国家自然科学基金项目(52474446)。

摘　　要：与金元素品位同级别或含量更高的有害元素(如镍、铜、镉和铅)在定量分析时,金矿的复杂基体会产生抑制效应,削弱离子化率和信号响应而影响测试结果。本文采用基体匹配-电感耦合等离子体质谱法(ICP-MS),与纯试剂有害元素标准溶液相比,复杂基体有害元素标准溶液可减少与样品消解液间的基体差异,在基体匹配与内标法联合校正非质谱干扰后实现对有害元素的准确定量。在确定金矿各浮选样品主要基体元素后,采用盐酸-硝酸-氢氟酸体系配合微波消解方法溶解样品。500μg/mL和1000μg/mL单一和混合基体元素溶液中10μg/L有害元素定量结果的相对偏差小于±10%,高浓度基体对痕量有害元素定量结果的影响较小。在基体浓度1000μg/mL条件下,单一和两种基体元素的有害元素标准溶液对不同基体种类的金矿浮选样品中有害元素定量结果偏差小于20%,因此采用铁硫基体的有害元素标准溶液实现金矿浮选样品的有害元素定量。利用该标准溶液测试代表性样品的加标回收实验中,元素加标回收率为92.08%~106.05%;对代表性样品进行6次平行测试,各元素相对标准偏差(RSD)为1.21%~4.69%。表明基体匹配ICP-MS法可作为金矿浮选样品有害元素的定量方法。For the quantification analysis of harmful elements(such as Ni,Cu,Cd and Pb),which may have the same grade or high content as gold,the complex matrix of gold ore can produce inhibitory effects,weaken the ionization rate and signal response,and show a negative effect on measurement results.In the work described here,inductively coupled plasma-mass spectrometry(ICP-MS)with matrix-matching was applied.Compared with the standard solution of harmful elements with pure reagent,a standard solution of harmful elements in a complex matrix reduced the difference in the matrix when the solution of the sample was dissolved.The accurate determination of harmful elements was achieved with the calibration of non mass spectrometry interference by the internal standard solution and matrix-matching.Main matrix elements of each flotation product of gold ore were determined by the mineralogical analysis,and sample dissolution was conducted by the microwave digestion with HCl-HNO3-HF.Recovery rate of 10μg/L harmful element were 90%-110%in 500μg/mL and 1000μg/mL matrix solution of single and multiple types of matrix elements.Quantitative deviation of harmful elements in flotation samples of various matrix types was less than 20%,which was measured by harmful elements standard solution with single and two types of matrix elements of 1000μg/mL.Hence,the harmful element standard solution with the Fe-S matrix was applied for the determination of harmful elements in flotation products of gold ore.For the spiked recovery experiment of representative samples measured by the standard solution,the elemental spiked recovery rate ranged from 92.08%to 106.65%.Six parallel tests were conducted on representative samples,and the relative standard deviation(RSD)of each element was 1.21%-4.69%.ICP-MS with matrix matching method is suitable for quantification determination of harmful elements in flotation samples of gold ore.

关 键 词：电感耦合等离子体质谱法 金矿浮选样品 基体匹配 定量分析 有害元素 

分 类 号：O657.63[理学—分析化学] TH84[理学—化学]