能量色散X射线荧光分析镍基催化剂中镍和镧的含量

Determination of Nickel and Lanthanum in Nickel-Based Catalyst by Energy-Dispersive X-Ray Fluorescence Spectrometry

建立了一种可用于能量色散X射线荧光谱(EDXRF)分析的简单、快捷的微量试样制样方法,并用EDXRF法分析了Ni基甲烷化催化剂中Ni和La的含量。通过实验确定了最佳分析条件及检测范围,考察了方法的准确度和精密度。根据2个系列标准试样得到的2个标准工作曲线得知,当Ni含量在10.0%～45.0%(w)时,特征X射线强度与Ni含量呈现良好的线性关系;La含量在0.2%～4.0%(w)时,特征X射线强度与La含量呈现良好的线性关系。由加标回收实验得知,Ni回收率为99.24%～102.75%,La回收率为100.55%。精密度实验结果表明,Ni含量的相对标准偏差(n=10)为2.52%～2.73%,La含量的相对标准偏差为2.02%。经ICP化学法验证,该EDXRF法可用于测定试样中的金属元素的含量;该方法快速、高效、应用价值高。

A fast sample-preparation method for energy dispersive X-ray fluorescence （EDXRF） analysis was established, and the contents of Ni and La in a nickel-based methanation catalyst were measured by means of EDXRF. The optimal analysis conditions and detection range were determined, and the accuracy and the precision of the measurement was investigated. The two standard working curves were obtained from two standard samples. In the ranges of 10.0%-45.0%（w） for the Ni content and 0.2%-4.0%（w） for the La content, the intensities of the characteristic X-rays showed good linear relationships with the contents. According to the recovery test by standard addition, the recoveries of Ni and La reached 99.24%-102.75% and 100.55%, respectively. The RSDs（n=10） were in 2.52%- 2.73% for the Ni content and 2.02% for the La content. It was validated by ICP chemical method that EDXRF could be used in the determination of metallic element contents..