粉末压片-能量色散X射线荧光光谱法快速测定铜钴矿中铜钴铁锰硫  

Rapid Determination of Copper,Cobalt,Iron,Manganese and Sulfur in Copper-Cobalt Ore by Powder Tableting-Energy Dispersive X-ray Fluorescence Spectrometry

作　　者：兰福荫 刘杰 李勇 李首刚 陆智国 LAN Fuyin;LIU Jie;LI Yong;LI Shougang;LU Zhiguo(La Sino-Congolaise Des Mines S.A.,Beijing 100039,China)

机构地区：[1]华刚矿业股份有限公司,北京100039

出　　处：《山东化工》2025年第4期175-177,181,共4页Shandong Chemical Industry

摘　　要：铜钴矿是生产阴极铜和氢氧化钴产品的重要矿物原料,采用传统方法测定铜钴矿中的主次元素检测周期长、成本高且各元素不能同时测定,不能满足批量样品的快速分析需求。市场上虽有铜矿石分析标准样品兜售,但其与刚果(金)地区实际开采投入生产的铜钴矿基体上有一定的差异,实验根据某铜钴矿的性质,选用与待测铜钴矿样品具有相似结构和化学成分且用化学法及红外吸收法定值的系列校准样品绘制校准曲线,采用粉末压片法制样,建立了ED-XRF测定铜钴矿中铜、钴、铁、锰、硫的方法。通过实验确定样品粒度为74μm以及保压压力为30 t、保压时间为15 s的制样条件,采用经验系数法进行基体校正,各元素校准曲线的相关系数均不小于0.997,方法检出限为0.00064%~0.015%。对同一铜钴矿样品平行制备11个样片上机测定,各元素测定结果的相对标准偏差(RSD)为0.44%~1.56%,满足DZ/T 0130—2006要求。选取4个实际铜钴矿样品开展方法比对,其测定差值符合GB/T 14353—2010、GB/T 5121—2008标准中的再现性限要求。Copper-cobalt ore is an important mineral raw material for the production of cathode copper and cobalt hydroxide products.The traditional method for determining the major and minor elements in copper-cobalt ore has a long detection cycle,high cost,and the elements cannot be determined simultaneously,which cannot meet the needs of rapid analysis of batch samples.Although there are copper ore analysis standard samples on the market,there are certain differences between them and the copper-cobalt ore matrix actually mined and put into production in the Democratic Republic of the Congo.According to the properties of a copper-cobalt ore,a series of calibration samples with similar structure and chemical composition to the copper-cobalt ore sample to be tested and calibrated by chemical method and infrared absorption method were selected to draw a calibration curve.The powder tablet method was used to prepare the sample,and the ED-XRF method for determining copper,cobalt,iron,manganese and sulfur in copper-cobalt ore was established.The sample preparation conditions of 74μm sample particle size,30 t holding pressure and 15 s holding time were determined by experiment.The empirical coefficient method was used for matrix correction.The correlation coefficient of the calibration curve of each element was not less than 0.997,and the detection limit of the method was 0.00064%~0.015%.Eleven samples were prepared in parallel from the same copper-cobalt ore sample and measured on the machine.The relative standard deviation(RSD)of the measurement results of each element was 0.44%~1.56%,which met the requirements of DZ/T 0130—2006.Four actual copper-cobalt ore samples were selected for method comparison,and the measurement difference met the reproducibility limit requirements in GB/T 14353—2010 and GB/T 5121—2008 standards.

关 键 词：能量色散 X射线荧光光谱法(XRF) 粉末压片 铜钴矿 快速测定 

分 类 号：O653[理学—分析化学]