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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
引用本文:胡丹静,严雪俊,张旭,朱毅杰.密闭消解-重量法测定掺铱、锇和钌的黄金饰品中金量[J].贵金属,2019,40(4):42-46.
作者姓名:胡丹静  严雪俊  张旭  朱毅杰
作者单位:浙江方圆检测集团股份有限公司 浙江省黄金珠宝饰品质量检验中心,杭州 310018;浙江方圆检测集团股份有限公司 浙江省黄金珠宝饰品质量检验中心,杭州 310018;浙江方圆检测集团股份有限公司 浙江省黄金珠宝饰品质量检验中心,杭州 310018;浙江方圆检测集团股份有限公司 浙江省黄金珠宝饰品质量检验中心,杭州 310018
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)
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(RSDn=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。

关 键 词:分析化学  高压密闭消解  饰品掺杂  重量法  
收稿时间:2019/1/30 0:00:00

Determination of Gold Content in Iridium, Osmium and Ruthenium-doped Gold Jewelry by Reduction Gravimetric Method
HU Danjing,YAN Xuejun,ZHANG Xu and ZHU Yijie.Determination of Gold Content in Iridium, Osmium and Ruthenium-doped Gold Jewelry by Reduction Gravimetric Method[J].Precious Metals,2019,40(4):42-46.
Authors:HU Danjing  YAN Xuejun  ZHANG Xu and ZHU Yijie
Affiliation:Zhejiang Fangyuan Test Group Co. Ltd, Zhejiang Gold and GEM Testing Center, Hangzhou 310018, China,Zhejiang Fangyuan Test Group Co. Ltd, Zhejiang Gold and GEM Testing Center, Hangzhou 310018, China,Zhejiang Fangyuan Test Group Co. Ltd, Zhejiang Gold and GEM Testing Center, Hangzhou 310018, China and Zhejiang Fangyuan Test Group Co. Ltd, Zhejiang Gold and GEM Testing Center, Hangzhou 310018, China
Abstract: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.
Keywords:analytical chemistry  high-pressure closed digestion  jewelry doped  gravimetric method  gold
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