ICP-OES法测定钴基碳化钨中钨、钴的含量

Deteroiination of tungsten and cobalt in cobalt-based tungsten carbide by ICP-OES method

钴基碳化钨粉末合金耐蚀性较高,溶解完全较为困难。对样品前处理方法以及仪器分析参数等影响因素进行了对比研究。最后确定使用盐酸及磷酸加热溶解样品,高温下滴加硝酸以破坏碳化物,样品完全消解后以电感耦合等离子体原子发射光谱法(ICP—OES)测定样品中常量元素钨、钴的含量。综合谱线发射强度和干扰重叠等因素,最终钨、钴的分析谱线分别选择224.876 nm、228.616 nm。实验结果表明,钨、钴在一定的质量浓度范围内与其对应的光谱强度呈线性关系,线性相关系数均大于0.9999。方法对于钴基碳化钨粉末合金测定值的相对标准偏差(n=10)在0.14%~0.78%之间,方法的加标回收率在95.7%~99.3%之间,测定结果具有较好的准确性。

Cobalt-based tungsten carbide powder alloy has high corrosion resistance and is difficult to dissolve completely.The influence factors such as sample pretreatment method and instrumental analysis parameters were compared.Finally,hydrochloric acid and phosphoric acid were heated to dissolve the sample,and nitric acid was added to destroy carbides at high temperature.After the sample was completely dissolved,the contents of tungsten and cobalt in the sample were determined by ICP-OES.Considering the spectral line emission intensity and interference overlap and other factors,the final analytical spectral lines of tungsten and cobalt were selected as 224.876nm and 228.616nm respectively.The experimental results show that there is a linear relationship between tungsten and cobalt and their corresponding spectral intensity within a certain range of mass concentration,and the linear correlation coefficients are both greater than 0.9999.Methods The relative standard deviation(n=10)of the determination value of cobalt-based tungsten carbide powder alloy is between 0.14%and 0.78%,and the recoveries of the method are between 95.7%and 99.3%.The determination results have good accuracy.