Determination of gold in gold ore by high resolution continuum source flame atomic absorption spectrometry combined with antimony fire assay and microwave digestion
MAO Xiangju1,2,3, ZHAO Yifan1,2,3, NI Wenshan*1,2,3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources,CAGS,Zhengzhou 450006, China; 2. China National Engineering Research Center for Utilization of Industrial Minerals, Zhengzhou 450006, China; 3. Key Laboratory for Polymetallic Ores' Evaluation and Utilization,MNR,Zhengzhou 450006, China
Abstract：Gold in the sample was captured by antimony particles generated in the redox reaction of antimony trioxide and reducing reagent flour. The antimony granule was dissolved with 40% aqua regia (V/V, the same below) in a microwave digestion instrument. Thus, a novel method for determination of gold in gold ore by high resolution continuum source flame atomic absorption spectrometry was established. Taking the certified reference materials for composition analysis of gold and silver in ore as the research object, the mixed reagent with same formula as sample ingredient was used as covering agent for experiments. The result showed that the determination value of gold was closer to the certified value than that without covering agent. The cupellation utensil test was conducted, and the results showed that the separation of antimony granule with scum formed by high temperature peeling of antimony button could be realized by quickly removing the utensil and immersing in water after cupellation with magnesia ash dish. The spectral interference tests showed that λAu=242.795 nm has no interference from other coexisting elements in the range of 242.65-242.94 nm. Under the optimized experimental conditions, the calibration curve of Au absorbance and its corresponding mass concentration in the range of 0.01-10.00 μg/mL was fitted by the least square method of quadratic equation. The determination coefficient was 0.999 8, the characteristic concentration was 0.065 94 μg/mL, the limit of detection was 0.003 7 μg/mL, and the limit of quantification was 0.012 3 μg/mL. The contents of gold in gold ore sample, the certified reference material for composition analysis of gold and silver in ore, and the gold certified reference material for geochemical exploration were determined according to the proposed method. For the actual samples, the relative standard deviations (RSD, n=9) were between 1.5% and 4.7%, and the recoveries were between 95% and 103%, which could meet the requirements of recovery for the geological and mineral industry standard of DZ/T 0130-2006. For the certified reference materials, the results were consistent with the certified values, and the RSDs (n=9) were between 1.2% and 3.9%.
郭晓瑞, 樊蕾, 王甜甜, 毛香菊, 赵一帆, 倪文山. 锑试金-微波消解-高分辨率连续光源火焰原子吸收光谱法测定金矿石中金[J]. 冶金分析, 2022, 42(12): 45-51.
MAO Xiangju, ZHAO Yifan, NI Wenshan. Determination of gold in gold ore by high resolution continuum source flame atomic absorption spectrometry combined with antimony fire assay and microwave digestion. , 2022, 42(12): 45-51.
[1] 王力军,刘春谦.难处理金矿石预处理技术综述[J].黄金,2000(1):38-45. WANG Lijun,LIU Chunqian.Overview of pretreatment technique of refractory gold ores[J].Gold,2000(1):38-45. [2] 金绍祥.微量金测定方法研究进展[J].理化检验(化学分册),2011,47(10):1248-1252. JIN Shaoxiang.Recent progress of methods for determination of trace amount of gold[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2011,47(10):1248-1252. [3] 任曼,邓海琳,龚国洪,等.分离富集金、铂、钯的碲共沉淀物研究[J].冶金分析,2005,25(3):13-15. RE Man,DENG Hailin,GONG Guohong,et al.Study on Te-coprecipitates for separation and preconcentration of gold,platinum,palladium[J].Metallurgical Analysis,2005,25(3):13-15. [4] 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 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. [5] 吴瑞林,李茂书,吴立生.贵金属试金分析方法评论[J].贵金属,1997(1):46-50. WU Ruilin,LI Maoshu,WU Lisheng.Development in fire assay of precious metals[J].Precious Metals,1997(1):46-50. [6] 刘亮,柯玲.铅试金法测定铅精矿及粗铅中的金、银[J].分析试验室,2007(S1):111-115. LIU Liang,KE Ling.Determination of gold and silver in lead concentrate and crude lead by lead fire assay[J].Chinese Journal of Analysis Laboratory,2007(S1):111-115. [7] 孙启亮,毛香菊,郭晓瑞,等.铅试金富集-高分辨率连续光源石墨炉原子吸收光谱法测定地球化学样品中痕量金铂钯[J].冶金分析,2021,41(7):10-16. SUN Qiliang,MAO Xiangju,GUO Xiaorui,et al.Determination of trace gold,platinum and palladium in geological samples by lead fire assay pre-concentration high resolution continuum source graphite furnace atomic absorption spectrometry[J].Metallurgical Analysis,2021,41(7):10-16. [8] NI W S,MAO X J,ZHANG H L,et al.Simultaneous determination of ultra-trace Pt,Pd,Rh and Ir in geochemical samples by inductively coupled plasma mass spectrometry following tin fire assay preconcentration and microwave digestion[J].Currrent Analytical Chemistry,2021(17):552-563. [9] 唐志中,王君玉,孙红林,等.锡试金分离富集-ICP-MS法同时测定地质样品中的金铂钯[J].贵金属,2013,34(2):51-55,60. TANG Zhizhong,WANG Junyu,SUN Honglin,et al.Determination of Au, Pt and Pd in geological samples by inductively coupled plasma massspectrometry with tin fire assay[J].Precious Metals,2013,34(2):51-55,60. [10] NI W S,MAO X J,ZHANG H L,et al.Determination of ultra-trace platinum,palladium,ruthenium,rhodium,and iridium in rocks and minerals by inductively coupled-plasma mass spectrometry following nickel sulfide fire assay preconcentration and open mixed acid digestion[J].Analytical Letters,2019,52(11):1699-1710. [11] NI W S,MAO X J,YAO M X,et al. Bismuth-remaining cupellation fire assay preconcentration combined with inductively coupled plasma mass spectrometry for the simultaneous determination of ultra-trace Au,Pt,Pd,Ru,Rh and Ir in geologic samples[J].International Journal of Analytical Chemistry,2021,170:9960673. [12] 李可及,赵朝辉,范建雄.铋试金-电感耦合等离子体质谱法测定贫铂矿石中痕量金铂钯[J].冶金分析,2013,33(8):19-23. LI Keji,ZHAO Chaohui,FAN Jianxiong.Determination of trace gold,platinum and palladium in lean-platinum ore by bismuth fire assaying-inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2013,33(8):19-23. [13] 林玉南,胡金星,沈振兴,等.锑试金富集痕量金的研究——地质样品中ng/g级金的测定[J].分析化学,1988(1):1-4. LIN Yunan,HU Jinxing,SHEN Zhenxing,et al.A new fire assay of gold using antimony as a collector-determination of gold at ng/g levels in geochemical materials[J].Analytical Chemistry,1988(1):1-4. [14] NI W S,ZHANG H L,MAO X J,et al.Simultaneous determination of ultra-trace Au,Pt,Pd,Ru,Rh,Os and Ir in geochemical samples by KED-ICP-MS combined with Sb-Cu fire assay and digestion[J].Microchemical Journal,2020,158:105197. [15] 中华人民共和国国土资源部.DZ/T 0130—2006 地质矿产实验室测试质量管理规范[S].北京:中国标准出版社,2006.
