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| 氢还原重量法测定海绵铂、钯产品的灼烧损失量 |
| Determination of Weight Loss Ignition in Sponge Platinum and Palladium Production by Hydrogen Reduction Gravimetry |
| Received:March 31, 2014 |
| DOI： |
| 中文关键词: 分析化学 氢还原重量法 海绵铂、钯 灼烧损失量 |
| 英文关键词: analytical chemistry hydrogen reduction gravimetry sponge platinum and palladium weight loss ignition |
| 基金项目:国家高技术研究发展计划基金(863计划) (2012AA063203，2012AA063207)、云南省科技创新强省计划项目(2011AA004)、国家标准制(修)订基金项目(20131031-T-610、20131032-T-610)。 |
| Author Name | Affiliation | E-mail | | GUO Junmei | Sino-Platinum Metals Resources Yimen Co. Ltd., State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China | gjm@ipm.com.cn | | HAN Shouli | Sino-Platinum Metals Resources Yimen Co. Ltd., State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China | | | TAN Wenjin | Sino-Platinum Metals Resources Yimen Co. Ltd., State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China | | | HE Xiaotang | Sino-Platinum Metals Resources Yimen Co. Ltd., State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China | | | LI Kun | Sino-Platinum Metals Resources Yimen Co. Ltd., State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China | | | LIU Wen | Sino-Platinum Metals Resources Yimen Co. Ltd., State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China | | | LI Yong | Sino-Platinum Metals Resources Yimen Co. Ltd., State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China | | | WAN Huan | Sino-Platinum Metals Resources Yimen Co. Ltd., State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China | | | WU Xilong | Sino-Platinum Metals Resources Yimen Co. Ltd., State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum Metals Co. Ltd., Kunming 650106, China | |
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| 中文摘要: |
| 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。 |
| 英文摘要: |
| 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. |
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