氢还原重量法测定海绵钯产品灼烧损失量的研究

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。

Study on Determination of Weight Loss Ignition in Sponge Palladium Production by Hydrogen Reduction Gravimetry

Conditions for determination of ignition loss in sponge palladium product by hydrogen reduction gravimetry were systematically investigated. The effect of nonmetallic impurity content on analytical result was investigated. Our results were compared with those obtained by thermogravimetry. 1-2 g sample was weighted and the heating temperature was increased stepwise to 800 -C. The ignition loss in sponge palladium were determined to be 0. 0019%,0. 0142%,0. 0302% and 0. 0694% with the range（R）, standard deviation（S）, relative standard deviation （RSD, n = 11） and repeatability limit （r） of ±0. 0005% 0.0028%,0.0001%-0.0007%,1.0%-5.2% and 0.0003%-0.0020%, respectively. The ignition loss was mainly composed of oxygen and nitrogen, but charcoal content was neglectable. Analytical results using the proposed method were accurate, precise and in good agreement with those by thermogravimetry and can meet the requirement for analysis of 99.90%-99.99% sponge palladium product.