Abstract:After the sample was roasted and digested in aqua regia by steam heating. The trace gold in sample solution after digestion was adsorbed for twice with two pieces of polyurethane foam plastics. The foam plastics were merged and ashed followed by dissolution with aqua regia. The internal standard Re was selected for correction. Thus, a determination method of trace gold in geochemical sample by inductively coupled plasma mass spectrometry (ICP-MS) was established. The conditions of digestion, adsorption and desorption were optimized. The results showed that when the sample was digested by steam heating, the determination results of gold were the same as those obtained by electric heating plate digestion. However, the steam heating digestion could save electrical energy and effectively reduce the external pollution. The certified reference materials of geochemical gold were selected for comparison tests. Two pieces of foam plastics were used for absorption in twice with absorption time keep the same. The recoveries of gold were between 97% and 101%, which were more close to 100% compared to those obtained by two pieces of foam plastics for once absorption (i.e., 87%-92%). The gold-loaded foam plastics were firstly ashsed at 180℃ for 20min. Then the temperature was increased to 700℃ within 50min and the foam plastics were further ashed for 1h. The recoveries of gold in certified reference materials of geochemical gold were stable near 100%. Under the selected experimental conditions, the linear correlation coefficient of calibration curve was 0.9996. The detection limit of method was 0.13ng/g. The lower and upper determination limit was 0.43ng/g and 120ng/g, respectively. The proposed method was applied for the determination of gold in three certified reference materials of geochemical gold, three soil samples and three stream sediments. It was found that the results of certified reference materials of geochemical gold were consistent with the certified values. The relative standard deviations (RSD, n=12) of the determination results of gold were between 2.9% and 6.4%. The recovery test of standard addition was conducted according to the experimental method with certified reference materials of geochemical gold. The recoveries were between 98% and 104%.
陈永欣,韦新红,黎香荣,等.巯基棉分离富集-电感耦合等离子体质谱法测定岩矿中痕量金和钯[J].冶金分析,2011,31(6):14-18.CHEN Yong-xin,WEI Xin-hong,LI Xiang-rong,et al.Determination of trace gold and palladium in rock and mineral by inductively coupled plasma mass spectrometry after separation and enrichment with sulfhydryl cotton[J].Metallurgical Analysis,2011,31(6):14-18.
[2]
陈景伟,李玉明,宋双喜,等.载炭泡塑吸附-电感耦合等离子体发射光谱法测定金矿石的金量[J].岩矿测试,2015,34(3):314-318.CHEN Jing-wei,LI Yu-ming,SONG Shuang-xi,et al.Determination of gold in gold ores by inductively coupled plasma-optical emission spectrometry with carbon-loaded foam plastic adsorption[J].Rock and Mineral Analysis,2015,34(3):314-318.
[3]
樊勇,修凤凤,韩一帆.电感耦合等离子体质谱(ICP-MS)法测定地球化学样品中的痕量金[J].中国无机分析化学,2011,7(2):18-21.FAN Yong,XIU Feng-feng,HAN Yi-fan.Determination of trace gold in geochemical samples by indutively coupled plasma-mass spectrmetry with water-bath digestion[J].Chinese Journal of Inorganic Analytical Chemistry,2011,7(2):18-21.
[4]
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.
[5]
方宏树,叶江.活性炭动态吸附-火焰原子吸收法测定金[J].现代矿业,2016(2):74-76.FANG Hong-shu,YE Jiang.Determination of gold by activater carbon dynamic adsorption-flame atomic absorption spectromtry[J].Modern Mining,2016(2):74-76.
[6]
申玉民,张宁,郭秀平,等.泡沫塑料吸附-电感耦合等离子体原子发射光谱法测定地质样品中的金[J].中国无机分析化学,2013,3(4):24-26.SHEN Yu-min,ZHANG Ning,GUO Xiu-ping,et al.Determination of Au in geological samples by inductively coupled plasma atomic emission spectrometry (ICP-AES) after pre-concentration using polyurethane foam[J].Chinese Journal of Inorganic Analytical Chemistry,2013,3(4):24-26.
[7]
孙晓玲,于照水,张勤.泡沫塑料吸附富集-石墨炉原子吸收光谱法测定勘查地球化学样品中超痕量金[J].岩矿测试,2002,21(4):266-270.SUN Xiao-ling,YU Zhao-shui,ZHANG Qin.Determination of ultra-trace gold in geochemical exploration samples by GFAAS after preconcentration with polyurethane foam[J].Rock and Mineral Analysis,2002,21(4):266-270.
[8]
YU Bo.Determination of trace amounts of gold in soil sample using plastic foam enrichment ICP-MS method[J].Agricultural Science & Technology,2008,19(4):149-152.
[9]
王瑞敏.泡沫塑料富集-电感耦合等离子体质谱法测定土壤中超痕量金铂钯[J].岩矿测试,2011,30(3):295-298.WANG Rui-min.Determination of ultra-trace Au,Pt and Pd in topsoil samples by foam plastics enrichment-inductively coupled plasma-mass spectrometry[J].Rock and Mineral Analysis,2011,30(3):295-298.
[10]
聂凤莲,张蜀冀,陈雪,等.ICP-MS法测定地电化学(泡塑)样品中痕量金[J].黄金,2011,32(12):58-60.NIE Feng-lian,ZHANG Shu-ji,CHEN Xue,et al.Determination of trace gold in geoelectrochemical (foam plastic) samples by ICP-MS[J].Gold,2011,32(12):58-60.
[11]
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.
[12]
郑大中.聚氨酯泡沫塑料富集金若干问题的探讨[J].黄金,1990,11(9):44-49.ZHENG Da-zhong.Discussion on some problems concentrating gold in polyurethane foam plastics[J].Gold,1990,11(9):44-49.
[13]
程文翠,付永立,马会春,等.纸上层析分离-ICP-AES 测定稀有金属矿中的铌钽[J].分析试验室,2018,37(2):168-173.CHENG Wen-cui,FU Yong-li,MA Hui-chun,et al.A method for the determination of Nb and Ta contents in rare metal ores by paper chromatography separation and ICP-AES[J].Chinese Journal of Analysis Laboratory Chinese,2018,37(2):168-173.
[14]
岩石矿物分析编写组.岩石矿物分析:第3分册[M].4版.北京:地质出版社,2011:376.
[15]
王英滨.ICP-AES法测定地质样品中微量锆、铪的研究[J].现代地质,1997,11(3):358-362.WANG Ying-bin.Study on determination of microamounts of zirconium and hafnium in geological samples by ICP-AES[J].Geoscience,1997,11(3):358-362.