甲基异丁基甲酮萃取-电感耦合等离子体质谱法测定铜精矿中金  

Determination of gold in copper concentrate by inductively coupled plasma mass spectrometry with methyl isobutyl ketone extraction

作　　者：杨春艳 王宴秋[2] 常欢[2] 张秀艳[3] YANG Chunyan;WANG Yanqiu;CHANG Huan;ZHANG Xiuyan(Baotou Customs Comprehensive Technical Service Center,Baotou 014010,China;Technical Center of Inner Mongolia Baotou Steel Union Co.,Ltd.,Baotou 014010,China;Baotou Rare Earth Research Institute,Baotou 014010,China)

机构地区：[1]包头海关综合技术服务中心,内蒙古包头014010 [2]内蒙古包钢钢联股份有限公司技术中心,内蒙古包头014010 [3]包头稀土研究院,内蒙古包头014010

出　　处：《冶金分析》2025年第3期25-30,共6页Metallurgical Analysis

摘　　要：金为铜精矿的常规计价元素,准确测定其含量对铜精矿冶炼和开发及工厂结算有着重要的指导意义。选择王水-HF-HClO4体系溶解样品,以20 mL甲基异丁基甲酮(MIBK)对溶解液中金进行萃取,用^(196.967)Au^(+)为测定同位素,建立了甲基异丁基甲酮萃取-电感耦合等离子体质谱法(ICP-MS)测定铜精矿中金的方法。以金质量浓度为横坐标,金强度与铯内标强度的比值为纵坐标绘制校准曲线,其线性相关系数大于0.999,方法检出限为0.039 g/t,定量限为0.13 g/t。选择铜精矿标准物质和铜精矿样品,按照实验方法进行测定;对于实际样品,采用火试金重量法进行方法对照试验,同时在铜精矿样品中加入金标准溶液进行加标回收试验。结果表明:对于标准物质,测定值与认定值基本一致;对于实际样品,实验方法与火试金重量法测定值基本一致,加标回收率在96%~109%之间。应用实验方法测定2个铜精矿样品中金,测得结果的相对标准偏差(RSD,n=10)分别为0.77%和2.1%。Gold is a kind of conventional pricing elements in copper concentrate,and the accurate determination of its content has important guiding significance for the smelting,development and factory settlement of copper concentrate.In this study,the sample was dissolved with aqua regia-HF-HClO4 system,and gold in solution was extracted with 20 mL of methyl isobutyl ketone(MIBK).^(196.967)Au^(+)was selected as the measuring isotope.The method for the determination of gold in copper concentrate by inductively coupled plasma mass spectrometry(ICP-MS)with MIBK extraction was established.The calibration curve was prepared using the mass concentration of gold as x-axis and using intensity ratio of gold to cesium internal standard as y-axis.The linear correlation coefficient was higher than 0.999.The limit of detection of was 0.039 g/t,and the limit of quantification was 0.13 g/t.The certified reference material and sample of copper concentrate were selected and determined according to the experimental method.For the sample,the fire assay gravimetry was used for the method contrast test.Meanwhile,the standard solution of gold was added into copper concentrate sample for the spiked recovery test.The results showed that the measurement results of certified reference material were basically consistent with the certified values.For the sample,the determination results of experimental method were basically consistent with those obtained by the fire assay gravimetry.The recoveries were between 96%and 109%.The content of gold in two copper concentrate samples were determined according to the experimental method,and the relative standard deviations(RSD,n=10)of determination results were 0.77%and 2.1%,respectively.

关 键 词：铜精矿 金 甲基异丁基甲酮(MIBK) 萃取 电感耦合等离子体质谱法(ICP-MS) 

分 类 号：O657.63[理学—分析化学] TF03[理学—化学]