Determination of gold in primary halo sample from Yangshan gold deposit in Wenxian County of Gansu Province by inductively coupled plasma mass spectrometry
LU Haichuan1,2, YE Zhixiang2, DING Yang1, XIONG Tao1, GONG Cang*1
1. Civil-Military Integrated Geological Survey Center of China Geological Survey, Chengdu 610036, China; 2. College of Resources and Environment, Chengdu University of Information Engineering, Chengdu 610225, China
Abstract:The gold content in primary halo sample from Yangshan gold deposit in Wenxian County of Gansu Province varied from μg/g to ng/g. There are many high value outliers (0.5-15.4 μg/g), and the memory effect of gold in determination is outstanding problem. The primary halo sample from Yangshan gold deposit in Wenxian County of Gansu Province was digested with 70 mL of aqua regia (1+1). The gold was adsorbed and enriched with polyurethane foaming plastic followed by desorption with 3 g/L thiourea solution. The on-line internal standard method using rhenium (5 ng/mL) as internal standard was selected for correction. The determination of gold in primary halo sample from Yangshan gold deposit in Wenxian County of Gansu Province by inductively coupled plasma mass spectrometry (ICP-MS) was realized. The primary halo sample with relatively high gold content [Y2-1(w(Au)=5.14 μg/g)] was determined according to the experimental method. Then the pipelines were cleaned with 2% nitric acid and 3 g/L thiourea solution before determination of blank. The results showed that the cleaning effect of 3 g/L thiourea solution was better than 2% nitric acid. When the cleaning time with 3 g/L thiourea solution was in range of 30-90 s, the value of blank was close to 0. Therefore, the pipelines were cleaned with 3 g/L thiourea solution for 30 s to eliminate the influence of memory effect of gold. The correlation coefficient of calibration curve was 0.999 8. The linear range was 0.12-500 ng/g. The limit of detection was 0.03 ng/g, and the limit of quantification was 0.12 ng/g. The contents of gold in seven certified reference materials of geochemical prospecting and gold for the analysis of gold were determined according to the experimental method. The results were consistent with the certified values. Three primary halo samples with different types (Y3-1 phyllite, Y3-2 tattered altered phyllite, and Y3-3 plagioclase granite porphyry gold ore) were selected and determined for 6 times according to the experimental method. Moreover, certain amount of gold standard solution was added for the recovery test. The relative standard deviations (RSD, n=6) of determination results were between 5.3% and 9.0%. The recoveries were between 90% and 105%. Three primary halo samples with different types were determined according to the experimental method, and compared with graphite furnace atomic absorption spectrometry (GFAAS). The determination results of two methods were basically consistent.
陆海川, 叶芝祥, 丁洋, 熊韬, 龚仓. 电感耦合等离子体质谱法测定甘肃文县阳山金矿床原生晕样品中金[J]. 冶金分析, 2022, 42(1): 64-70.
LU Haichuan, YE Zhixiang, DING Yang, XIONG Tao, GONG Cang. Determination of gold in primary halo sample from Yangshan gold deposit in Wenxian County of Gansu Province by inductively coupled plasma mass spectrometry. , 2022, 42(1): 64-70.
[1] 王亮,熊韬,罗涛,等.甘肃文县阳山金矿床葛条湾-安坝矿段原生晕地球化学特征及深部找矿远景评价[J].矿床地质,2021,40(1):143-155. WANG Liang,XIONG Tao,LUO Tao,et al.Geochemical characteristics of primary halo and evaluation of deep mineralizaton prospect of Yangshan gold deposit,Wenxian,Gansu Province[J].Mineral Deposits,2021,40(1):143-155. [2] 刘崇明.金属矿床原生晕研究进展[J].地质学报,2006,80(10):1528-1537. LIU Chongming.Progress in studies on primary halos of ore deposit[J].Acta Geologica Sinica,2006,80(10):1528-1537. [3] 任志海,夏照明,万兵.王水密闭溶矿-火焰原子吸收光谱法测定金矿石中的金[J].中国无机分析化学,2015,5(1):35-37. REN Zhihai,XIA Zhaoming,WAN Bing.Determination of Au in gold ore by FAAS with closed disgestion by aqua regia[J].Chinese Journal of Inorganic Analytical Chemistry,2015,5(1):35-37. [4] 胡明,关逸考.石墨炉原子吸收测定化探样品中痕量金的研究[J].黄金,2006,27(8):47-50. HU Ming,GUAN Yikao.Study on trace gold determination in geochemical samples by AAS with graphite furnace[J].Gold,2006,27(8):47-50. [5] 樊勇,修凤凤,韩一凡.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,2017,7(2):18-21. FAN Yong,XIU Fengfeng,HAN Yifan.Determination of trace gold in geochemical samples by inductively coupled plasma mass spectrometry with water-bath digestion[J].Chinese Journal of Inorganic Analytical Chemistry,2017,7(2):18-21. [6] 张勇,王玉功,刘建军.封闭溶样-电感耦合等离子体质谱法测定地质样品中的痕量金[J].中国无机分析学,2013,3(1):34-37. ZHANG Yong,WANG Yugong,LIU Jianjun.Determination of trace gold in geological samples by inductively coupled plasma mass spectrometry with pressurized sample decomposition technique[J].Chinese Journal of Inorganic Analytical Chemistry,2013,3(1):34-37. [7] 宋丽华,郝原芳,高慧莉.地质样品中金的测定方法研究[J].地质与资源,2014,23(6):577-579. SONG Lihua,HAO Yuanfang,GAO Huili.Study on the determination of gold in geological samples[J].Geology and Resources,2014,23(6):577-579. [8] 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的金[J].冶金分析,2016,36(7):34-38. ZHAO Yanqing.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. [9] 邱红绪,杨建博,边朋沙,等.蒸汽加热消解-电感耦合等离子体质谱法测定化探样品中痕量金[J].冶金分析,2019,39(12):31-37. QIU Hongxu,YANG Jianbo,BIAN Pengsha,et al.Determination of trace gold in geochemical samples by inductively coupled plasma mass spectrometry with steam heating digestion[J].Metallurgical Analysis,2019,39(12):31-37. [10] 金倩,李晓敬,陈庆芝,等.聚氨酯泡沫塑料吸附-电感耦合等离子体质谱法测定化探样品中的微量金[J].黄金,2018,39(3):80-82. JIN Qian,LI Xiaojing,CHEN Qingzhi,et al.Determination of trace gold in geochemical samples by the polyurethane foam plastics absorption-inductively coupled plasma mass spectrometry[J].Gold,2018,39(3):80-82. [11] 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 Xiaoling,YU Zhaoshui,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. [12] 中华人民共和国国土资源部.DZ/T 0279.4—2016 区域地球化学样品分析方法 第4部分:金量测定 泡沫塑料富集-电感耦合等离子体质谱法[S].北京:地质出版社,2016. [13] 张洁,阳国运.电感耦合等离子体质谱法测定金矿石中金[J].冶金分析,2018,38(11):18-23. ZHANG Jie,YANG Guoyun.Determination of gold in gold ore by inductively coupled plasma mass spectrometry [J].Metallurgical Analysis,2018,38(11):18-23. [14] 中华人民共和国国土资源部.DZ/T 0011—2015 地球化学普查规范(1∶50 000)[S].北京:中国标准出版社,2015.