熔片制样-X射线荧光光谱法测定铜精矿中7种组分  

Determination of 7 Components in Copper Concentrate by X-ray Fluorescence Spectrometry with Melt Sample Preparation

作　　者：杨林 周武权 隋东 邹国庆 刘洪艳 胡乔青[2] YANG Lin;ZHOU Wuquan;SUI Dong;ZOU Guoqing;LIU Hongyan;HU Qiaoqing(CMGB Bu-1(Hebei)Analysis&Technology Co.,Ltd.,Langfang,Hebei 065201,China;Institute of Natural Resources,Chinese Academy of Geological Sciences,Beijing 100037,China)

机构地区：[1]中冶一局(河北)检测技术有限公司,河北廊坊065201 [2]中国地质科学院资源研究所,北京100037

出　　处：《中国无机分析化学》2024年第9期1313-1319,共7页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家重点研发计划项目(2022YFC2903602)。

摘　　要：铜精矿中硫化物重金属含量较高,样品需要充分氧化后才可熔片,否则熔融过程严重腐蚀铂-金坩埚。一般方法采用硝酸盐作为氧化剂,单一的硝酸盐难以完全氧化铜精矿样品,并且氧化反应剧烈容易发生样品喷溅。采用四硼酸锂-偏硼酸锂混合熔剂(m∶m=67∶33),样品和熔剂质量比为1∶35,通过考察氧化剂过氧化钡-硝酸钠-碳酸钠的氧化效果,以及脱模剂的用量和加入方式、预氧化和熔融条件等,样品在高温炉中预氧化后转移至熔样机熔融,可制成合格的玻璃样片。选用合适的铜精矿国家一级标准物质,以标准物质相互混合或向标准物质中添入纯氧化铜的方式扩大校准曲线含量范围,以熔片法制样,建立了波长色散X射线荧光光谱法测定铜精矿中的铜、硫、全铁、氧化钙、氧化镁、二氧化硅、三氧化二铝等7种组分含量的方法。各组分检出限在0.054%~0.22%,校准曲线相关系数(r)均在0.9998以上,选用的3个铜精矿矿石国家一级标准物质按建立的方法进行处理后,测定结果均在认定值的误差范围内,各组分测试结果的相对标准偏差(RSD,n=12)在0.28%~4.1%;选取3个铜精矿实际样品做方法比对实验,测定值与标准分析方法的测定值无明显差异。The heavy metal content of sulfide in copper concentrate is high,and the sample needs to be fully oxidized before melting,otherwise the melting process will seriously corrodes the platinum-gold crucible.The general method uses nitrate as oxidizing agent,and a single nitrate is difficult to completely oxidize copper concentrate samples,and the oxidation reaction is violent and prone to sample spatter.Using lithium tetraborate-lithium metaborate mixed flux(m∶m=67∶33),and the mass ratio of sample to flux was 1∶35,the oxidation effect of oxidizing agent barium peroxide,sodium nitrate and sodium carbonate,as well as the dosage and adding method of release reagent,pre-oxidation and melting conditions were investigated.The sample was transferred to the fusion machine for melting after pre-oxidation in high temperature furnace,and qualified glass samples were made.Appropriate national first-class standard materials for copper concentrate were selected,and the content range of the calibration curve was expanded by mixing the standard materials with each other or adding pure copper oxide to the standard materials.The content of seven components,including copper,sulfur,total iron,calcium oxide,magnesium oxide,silica and aluminum oxide was determined by wavelength dispersive X-ray fluorescence spectrometry after the sampling by fusion method.The detection limit of each component was between 0.054%and 0.22%,and the correlation coefficient(r)of the calibration curve was above 0.9998.Three national first-class standard substances of copper concentrate ores were selected for processing according to this method,and the measured results were all within the error range of the identified values.The relative standard deviation of the test results of each component(RSD,n=12,)were between 0.28%and 4.1%.Three actual copper concentrate samples were selected for comparison experiment,and the measured values of the method were not significantly different from those of the standard analysis method.

关 键 词：X射线荧光光谱法(XRF) 熔片制样 铜精矿 过氧化钡 

分 类 号：O657.34[理学—分析化学]