粉末压片—X射线荧光光谱法测定钨矿石中15种主次组分  

Determination of 15 primary and secondary components in tungsten ore by X-ray fluorescence spectrometry after powder sheeting

作　　者：徐佳佳 XU Jiajia(Heilongjiang Institute of Ecological Geological Survey,Harbin 150030,Heilongjiang,China;Heilongjiang Mining Group Co.,Ltd.,Harbin 150036,Heilongjiang,China)

机构地区：[1]黑龙江省生态地质调查研究院,黑龙江哈尔滨150030 [2]黑龙江省矿业集团有限责任公司,黑龙江哈尔滨150036

出　　处：《矿产与地质》2024年第6期1074-1080,共7页Mineral Resources and Geology

摘　　要：准确测定钨矿石的主次组分能够为钨矿石的冶炼和深加工提供关键数据,还对研究其矿物组成、钨矿床的资源开发和综合利用具有指导意义。通过优化样品粒度、粘结剂的类型及用量等条件,建立粉末压片—X射线荧光光谱同时测定钨矿石中的15种主次组分的分析方法。采用光谱纯的氧化物与钨矿石标准物质GBW 07241按不同质量比配制校准样品,解决校准系列的基体匹配和浓度梯度问题,并通过理论α系数法进一步校正基体效应和谱线重叠效应。结果表明:当样品粒度小于74μm,加入粘结剂硼酸的质量分数为2%时,在40 MPa压力下保持15 s,可以制成表面光滑、结果重现性好的样片。以钨矿石标准物质GBW 07369为研究对象,经理论α系数法进一步校正后得到的分析结果的相对标准偏差(RSD,n=12)为0.58%~7.79%,测定值与认定值的相对误差ε为-15.32%~5.00%。将该方法用于4个实际钨矿石样品(1#、2#为黑钨矿,3#、4#为白钨矿)中主次组分的测定,其结果与化学法的测定值一致。Accurately determining the main and trace components of scheelite can provide key data for the smelting and deep processing of scheelite,and also has guiding significance for studying its mineral composition,tungsten deposit resource development,and comprehensive utilization.By optimizing conditions such as sample particle size,type and dosage of binder,an analysis method for simultaneously determining 15 main and trace components in scheelite using powder pressing and X-ray fluorescence spectrometry is established.Calibration samples were prepared by mixing spectrally pure oxides with scheelite reference material GBW 07241 at different mass ratios to solve the problems of matrix matching and concentration gradient in the calibration series,and further corrected for matrix effects and spectral line overlap effects using the theoretical α coefficient method.The results show that when the sample particle size is less than 74 μm,with 2% boric acid as the binder by mass fraction,and maintained at 40 MPa for 15 s smooth surface samples with good repeatability can be prepared.Using scheelite reference material GBW 07369 as the research object,the analysis results further corrected by the theoretical α coefficient method have a relative standard deviation(RSD,n=12) of 0.58% to 7.79%,and the relative error ε between the measured values and the certified values is between 15.32% and 5.00%.This method was applied to determine the main and trace components in 4 actual scheelite samples(1# and 2# are black tungstenite,3# and 4# are white tungstenite),and the results are consistent with those obtained by chemical methods.

关 键 词：钨矿石 主次组分 X射线荧光光谱法 粉末压片 

分 类 号：P618.67[天文地球—矿床学]