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| 密闭消解-重量法测定掺铱、锇和钌的黄金饰品中金量 |
| Determination of Gold Content in Iridium, Osmium and Ruthenium-doped Gold Jewelry by Reduction Gravimetric Method |
| Received:January 30, 2019 |
| DOI： |
| 中文关键词: 分析化学 高压密闭消解 饰品掺杂 重量法 金 |
| 英文关键词: analytical chemistry high-pressure closed digestion jewelry doped gravimetric method gold |
| 基金项目:浙江省市场监督管理局科研计划项目(20190321)、国家自然科学基金(21506187) |
| Author Name | Affiliation | E-mail | | HU Danjing | Zhejiang Fangyuan Test Group Co. Ltd, Zhejiang Gold and GEM Testing Center, Hangzhou 310018, China | hu_danjing@126.com | | YAN Xuejun | Zhejiang Fangyuan Test Group Co. Ltd, Zhejiang Gold and GEM Testing Center, Hangzhou 310018, China | 4849523@qq.com | | ZHANG Xu | Zhejiang Fangyuan Test Group Co. Ltd, Zhejiang Gold and GEM Testing Center, Hangzhou 310018, China | | | ZHU Yijie | Zhejiang Fangyuan Test Group Co. Ltd, Zhejiang Gold and GEM Testing Center, Hangzhou 310018, China | |
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| 中文摘要: |
| 掺杂铱、锇和钌的黄金饰品中金的量难于用密度法或X射线荧光光谱法(XRF)测定。将样品在高压密闭条件下经过王水消解后，掺杂的难溶金属可过滤分离，以80%水合肼(用水稀释6倍)作还原剂，将滤液中的金还原成沉淀，以重量法测定金含量，金粒的纯度用火花原子发射光谱法测定。方法加标回收率为96.2%~101.6%，相对标准偏差(RSD，n=6)为0.09%~0.23%，可满足掺杂铱、锇和钌的黄金饰品中金的测定。 |
| 英文摘要: |
| The gold content in iridium, osmium, ruthenium-doped gold jewelry is hard to determine by either density method or X-ray fluorescence. Samples were first digested with aqua regia in a high- pressure sealed container, then separated the doped insoluble metals by vacuum filtration. 80% hydrazine hydrate (diluted 10 times by water) was used as a reduction reagent to reduce the gold in the filtrate to precipitation. After filtering, washing and sintering, the gold content in samples was determined by gravimetric method, and the purity of gold was measured by spark source atomic emission spectrometry. The recovery rate of the gold was between 96.2% and 101.6%, and the relative standard deviation (RSD, n=6) was between 0.09% and 0.23%. The proposed method can be used for the determination of gold in iridium, osmium, ruthenium-doped gold jewelry. |
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