论文部分内容阅读
系统地研究了氢还原重量法测定海绵钯灼烧损失量的条件,考察了非金属杂质元素含量对分析结果的影响,并将本法结果与热重法的测定结果进行对照。结果表明:1~2g样品,氢还原分段升温至800℃,重量法测定海绵钯中0.0019%,0.0142%,0.0302%和0.0694%灼烧损失量的极差、标准偏差(S)、相对标准偏差(RSD)和重复性限(r)分别为±0.0005%~0.0028%,0.0001%~0.0007%,1.0%~5.2%和0.0003%~0.0020%。灼烧损失量主要由氧、氮含量组成,碳含量对其影响忽略不计。方法结果准确、精密,且与热重法的分析结果吻合,能够满足99.90%~99.99%的海绵钯产品的分析要求。
The conditions of determination of loss on ignition of sponge palladium by hydrogen reduction gravimetric method were systematically investigated. The influence of non-metallic impurity elements on the analysis results was investigated. The results of this method were compared with the results of thermogravimetry. The results showed that: 1 ~ 2g samples, the hydrogen reduction temperature was raised to 800 ℃ in sections, the standard deviation (S), the standard deviation (S), of 0.0019%, 0.0142%, 0.0302% and 0.0694% The deviations (RSD) and repeatability (r) were ± 0.0005% to 0.0028%, 0.0001% to 0.0007%, 1.0% to 5.2% and 0.0003% to 0.0020%, respectively. Loss of ignition is mainly composed of oxygen and nitrogen content, the impact of carbon content neglected. The method is accurate and accurate, and it is in good agreement with the results of thermogravimetric analysis. It can meet the analytical requirements of sponge palladium products from 99.90% to 99.99%.