X射线荧光光谱法测定钴渣料中过渡金属含量

Quantifi cation of Transition Metals in Cobalt Residue by X-ray Fluorescence Spectrometric Method

钴渣料具有基体复杂与多种谱线相近的过渡金属共存的特点,使得采用X射线荧光法分析时,元素含量与谱线强度之间相关性差。其中,以钨、钽、铜、钴、镍、铁、铬等多种元素共存的钴渣料的检测最为困难。试样首先通过半定量软件初步判定组成元素,然后通过高倍稀释熔融制样,采用生产原料绘制校准曲线,根据元素谱线特征优化测试条件,进而对谱线重叠和基体效应进行校正,有效地降低共存元素的干扰。将该方法用于钴渣料样品中钴、镍、铜、铁、铬、钽以及钨7种主要过渡金属元素含量的测定,测定结果与化学法相符,相对标准偏差(RSD,n=11)均小于5%,符合生产要求。

The quantification of elements in cobalt residue X-ray fluorescence spectrometric method is extremely c hallenging owing to the matrix effect and the spectral line interference of complex elements especially when W,Ta,Cu,Co,Ni,Fe and Cr are present.This work developed a new analytic process to solve the problem.The samples were first semiquantified with XRF to roughly estimated the content of those elements.Based on the results,the samples were then diluted and sampled for further accurately analyzing.With the raw materials in the industry as the standard substance for drawing the standard curve and selecting the suitable test condition as well as spectral lines for the different elements,the interference of the spectral lines can be calibrated.Employing the method,seven unknow cobalt residue samples were tested with XRF method and the relative standard deviation of the results was less than 5%compared with the chemical analytic method.