研究了氢还原重量法测定海绵铂、钯产品灼烧损失量的条件，考察了氧、氮、碳等非金属共存杂质元素含量对分析结果的影响，并与热重分析方法进行了对比。结果表明：称取2 g样品，氢还原分段升温至800℃，重量法测定海绵铂、钯的灼烧损失量分别为0.0018%~0.0769%和0.0018%~0.0694%，测定铂的相对允许差(RPD)、相对标准偏差(RSD)和重复性限(r)分别为2.1%~50%、0.7%~16.0%和0.0006%~0.0026%，对于钯分别为3.0%~15.8%、1.0%~5.3%和0.0003%~0.0020%。灼烧损失量主要由氧、氮含量组成，微量的炭对其影响忽略不计。氢还原重量法测定灼烧损失量操作简便，结果可靠，结果与热重分析方法的吻合，能够满足99.90%~99.99%的海绵铂、钯产品的分析要求。
Conditions for determination of weight loss ignition in sponge platinum and palladium production by hydrogen reduction gravimetry were systemic investigated. Effect of contents coming from oxygen, nitrogen, carbon and otherwise nonmetal coexist impurities on analytical result was investigated, and the determined results of the method were compared with that of thermo gravimetry. Results indicate that the weights loss ignition are of 0.0018%~0.0769% and 0.0018%~0.0694%, respectively, in sponge platinum and palladium under the conditions of 2 g sample, hydrogen reduction, subsection heating temperature to 800℃.Relative permissible deviation (RPD), relative standard deviation (RSD,n=11) and repeatability limit (r) are 2.1%~50%, 0.7%~16.0%, 0.0006%~0.0026%, for Pt, and 3.0%~15.8%, 1.0%~5.3%, 0.0003%~0.0020%, for Pd, respectively. The weights loss ignition was composed of oxygen and nitrogen contents, and it is not affected from charcoal content. The proposed method is easy to operated, reliable of analysis results, good accord with those of thermo gravimetry, and to satisfy the analytical requirement for 99.90%~99.99% sponge platinum and palladium production.
参考文献
| [1] | 贺小塘,郭俊梅,王欢,李勇,吴喜龙,赵雨,韩守礼,李锟,谭文进,刘文.中国的铂族金属二次资源及其回收产业化实践[J].贵金属,2013(02):82-89. |
| [2] | 从Pd/C废料中回收钯及制备试剂PdCl2的新工艺[J].贵金属,2012(04):9-13. |
| [3] | 刘时杰.铂族金属冶金学[M].长沙:中南大学出版社,2013:497-515. |
| [4] | 余建民.贵金属分离与精炼工艺学[M].北京:化学工业出版社,2006:222-223. |
| [5] | GB/T 1419-2004.海绵铂[S].北京:中华人民共和国国家质量监督检验检疫总局,2004. |
| [6] | GB/T 1420-2004.海绵钯[S].北京:中华人民共和国国家质量监督检验检疫总局,2004. |
| [7] | (Reaproved 2012)Standard specification for refined platinum[A].US,2012 |
| [8] | (Reapproved 2012)Standard specification for refined palladium[A].US,2012 |
| [9] | 罗一江,陶赛祥,杨媛媛,方卫,马媛,吴庆伟.铂、钯、铑、钌及其合金粉末灼烧损失量的测定[J].贵金属,2010(04):52-54. |
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