X射线荧光光谱法测定硬质合金高钴、高镍残次料中钴、镍、铬、铁量

Determination of Cobalt, Nickel, Chromium and Iron in High Cobalt and High Nickel Residues of Cemented Carbide by X-ray Fluorescence Spectroscopy

硬质合金生产过程中产生的残次料中钴、镍、铬、铁通常采用《硬质合金化学分析方法 EDTA滴定法测定钴量和镍量》、《钨化学分析方法原子吸收分光光度法测定钴、镍、铁、锰、铜量》、《硬质合金化学分析方法硫酸亚铁铵滴定法测定铬量》等方法,周期长、效率低,在实际操作中存在高钴高镍样品滴定终点难判断问题,如何快速识别分类管理以便回收利用这些残次料对分析检测提出了更高要求。本方法将样品用丙酮脱成型剂后,采用经典的压片制样法,在X射线荧光光谱仪上建立钨钴混合样中钴、镍、铬、铁测定方法,校准曲线在Co质量分数6.00%~20.00%范围内相关系数为0.999,Fe质量分数0.05%~2.0%范围内相关系数为0.999,Ni质量分数7.00%~15.00%范围内相关系数为0.999,Cr质量分数0.5%~1.5%范围内相关系数为0.999,方法相对标准偏差(RSD,n=7)小于6.2%,准确度98.4%~100.7%之间,分析结果同化学方法一致,极大的提高了在线分析速度。

Cobalt, nickel, chromium and iron in the residual materials produced in the production process of cemented carbide are usually determined by EDTA titration, atomic absorption spectrophotometry and ammonium ferrous sulfate titration. Those methods have disadvantages of long cycle and low efficiency, and it is difficult to judge the titration end point of high content cobalt and nickel samples in practice. In order to recycle and utilize those residues, higher requirements on quick identification and classification have been put forward. In this paper, a method for the determination of cobalt, nickel,chromium and iron in tungsten-cobalt mixture samples by X-ray fluorescence spectrometer was established. Forming agent with acetone was removed and the sample was pressed by classic means before detection. Results show that the correlation coefficients of calibration curves are all 0.999 in the range of 6.00%~20.00% Co, 0.05%~2.0% Fe, 7.00%~15.00% Ni and0.5%~1.5% Cr(mass fraction). The relative standard deviation(RSD, n=7) of the method is less than 6.2% and the accuracy is 98.4%~100.7%. The analysis results are consistent with those of chemical methods, which greatly improves the on-line analysis speed.