Determination of copper, silver, lead and cadmium in pure goldwith wide range purity by inductively coupled plasma massspectrometry after ethyl acetate extraction
LIN Yuan
Fujian Institute of Testing Technology, Fuzhou 350003, China
Abstract：The detection of pure gold sample has extensive market demand. However, the commonly used flame atomic absorption spectrometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were unable to determine pure gold samples when the mass fractions of lead and cadmium were both less than 0.0001%. In addition, inductively coupled plasma mass spectrometry (ICP-MS) with standard addition correction-internal standard method could not be used for determination of pure gold samples with high content of silver and copper (the mass fraction were both higher than 0.001%). After the sample was dissolved with aqua regia, the sample solution was directly extracted with ethyl acetate. Then a determination method of four main impurity elements including copper, silver, lead and cadmium in pure gold with purity in range of 99.9%-99.999% by ICP-MS was established with 2%-5% (volume fraction) nitric acid as determination medium. The interference tests indicated that the high content silver in pure gold did not interfere with the determination of copper, lead and cadmium. Under the selected experimental conditions, the correlation coefficients of calibration curves for all tested elements were not less than 0.9994. The low limit of determination was 0.01-0.19μg/g. The proposed method was applied for the analysis of pure gold actual samples. The relative standard deviations (RSD, n=6) of determination results were between 1.3% and 2.6%. The recoveries were between 99% and 105%. The experimental method was used for the determination of copper, silver, lead and cadmium in pure gold samples with three kinds of purity (99.9%, 99.99% and 99.999%). The results were basically consistent with those obtained by atomic absorption spectrometry (AAS) or ICP-MS with standard addition correction-internal standard method. The proposed method was applicable for the determination of copper, silver, lead and cadmium in pure gold with purity in range of 99.9%-99.999%.
林园. 乙酸乙酯萃取-电感耦合等离子体质谱法测定宽范围纯度足金中的铜银铅镉[J]. 冶金分析, 2018, 38(3): 41-45.
LIN Yuan. Determination of copper, silver, lead and cadmium in pure goldwith wide range purity by inductively coupled plasma massspectrometry after ethyl acetate extraction. , 2018, 38(3): 41-45.
杨加桂,李先和,张晓天,等.石墨消解-电感耦合等离子体质谱法测定海绵钯中18种杂质元素[J].冶金分析,2016,36(7):46-50.YANG jia-gui,LI Xian-he,ZHANG Xiao-tian,et al.Determination of eighteen impurity elements in sponge palladium by inductively coupled plasma mass spectrometry with graphite digestion[J].Metallurgical Analysis,2016,36(7):46-50.
[6]
周学忠,谢华林,李坦平,等.电感耦合等离子体质谱法测定石油焦中18种金属元素[J].冶金分析,2015,35(4):8-12.ZHOU Xue-zhong,XIE Huan-lin,LI Tan-ping,et al.Determination of eighteen metal element in petroleum coke by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2015,35(4):8-12.
[7]
钟胜贤,卢现友,刘景麟,等.电感耦合等离子体质谱法测定磷酸铁锂中杂质元素[J].冶金分析,2015,35(3):19-24.ZHONG Sheng-xian,LU Xian-you,LIU Jing-lin,et al.Determination of impurity element in lithium iron phosphate by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2015,35(3):19-24.
[8]
刘湘生,张安定,潘元海,等.高纯钯中痕量杂质的电感耦合等离子体质谱测定方法研究[J].现代科学仪器,2006 (6):66-68.LIU Xiang-sheng,ZHANG An-ding,PAN Yuan-hai,et al.Study on the determination of trace impurities in high purity palladium by inductively coupled plasma mass spectrometry[J].Modern Scientific Instrument,2006(6):66-68.
[9]
李丹,王锝,李彪.717阴离子交换树脂富集-电感耦合等离子体质谱法测定地质样品中痕量金铂钯[J].冶金分析,2011,31(4):36-40.LI Dan,WANG De,LI Biao.Determination of gold,platinum and palladium in geological samples by inductively coupled plasma mass spectrometry after concentration with 717 anion exchange resin[J].Metallurgical Analysis,2011,31(4):36-40.
[10]
迟明玉,董再蒸,薛惠芳,等.乙酸乙酯萃取-等离子体发射光谱法测定矿石中的金[J].黄金,2012,33(3):64-66.CHI Ming-yu,DONG Zai-zheng,XUE Hui-fang,et al.Determination of gold in ethyl acetate extracted ores by ICP-OES[J].Gold,2012,33(3):64-66.
[11]
成勇,袁金红,肖军,等.微波消解-电感耦合等离子体质谱法(ICP-MS)测定矿石中金和银[J].中国无机分析化学,2012,2(1):51-54.CHENG Yong,YUAN Jin-hong,XIAO Jun,et al.Closed microwave digestion-inductively coupled plasma mass spectrometry with standard addition for determination of gold and silver in ore[J].Chinese Journal of Inorganic Analytical Chemistry,2012,2(1):51-54.
[12]
王琳,唐志中,来新泽,等.混合吸附剂分离富集-电感耦合等离子体质谱法测定地质样品中的铂钯金[J].岩矿测试,2013,32(3):420-426.WANG Lin,TANG Zhi-zhong,LAI Xin-ze,et al.Bomb-inductively coupled plasma-mass spectrometry with concentrate and extraction by mixed adsorbent[J].Rock and Mineral Analysis,2013,32(3):420-426.
[13]
刘益锋,冯俊汉,李展江,等.电感耦合等离子体发射光谱法同时测定粗铜中金和银[J].冶金分析,2012,32(7):52-54.LIU Yi-feng,FENG Jun-han,LI Zhan-jiang,et al.Simultaneous determination of gold and silver in blister copper by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2012,32(7):52-54.
[14]
赵延庆.聚氨酯泡沫塑料吸附-电感耦合等离子体质谱法测定地质化探样品中金[J].冶金分析,2016,36(7):34-38.ZHAO Yan-qing.Determination of gold in geochemical samples by inductively coupled plasma mass spectrometry with polyurethane foam plastic absorption[J].Metallurgical Analysis,2016,36(7):34-38.
[15]
周红,宋艳合,李红霞,等.用载炭泡塑吸附原子吸收法测定地质样品中金[J].黄金地质,2001,7(2):64-66.ZHOU Hong,SONG Yan-he,LI Hong-xia,et al. Gold determination in geological samples by FAAS after their enrichment on carbon-loaded foam plastic[J].Gold Geology,2001,7(2):64-66.
