| 泡塑分离富集-火焰原子荧光光谱法测定地球化学样品中的痕量金 |
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| 引用本文： | 申玉民,罗治定,郭小彪,吴刚,王趁荣,付爱瑞,高树林,肖凡.泡塑分离富集-火焰原子荧光光谱法测定地球化学样品中的痕量金[J].岩矿测试,2020,39(1):127-134. |
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| 作者姓名： | 申玉民 罗治定 郭小彪 吴刚 王趁荣 付爱瑞 高树林 肖凡 |
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| 作者单位： | 河北省地质实验测试中心, 河北 保定 071052,河北省地质实验测试中心, 河北 保定 071052,河北省地质实验测试中心, 河北 保定 071052,河北省地质实验测试中心, 河北 保定 071052,河北省地质实验测试中心, 河北 保定 071052,河北省地质实验测试中心, 河北 保定 071052,北京金索坤技术开发有限公司, 北京 亦庄 102600,河北省地质实验测试中心, 河北 保定 071052 |
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| 基金项目： | 首都科技条件平台科学仪器开发培育项目“火焰法与氢化法联用原子荧光光谱仪的完善及产业化”（Z151100002415012） |
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| 摘 要： | 火焰原子荧光光谱法(FAFS)测定痕量金的灵敏度好、稳定性高及线性范围广,但在测定时干扰极为严重,如果干扰元素不加以分离或扣除,对0.5ng/g以下金无法进行准确测定。本方法在传统泡塑分离富集金的基础上,研究了FAFS法测定痕量金的最佳条件:在选定仪器条件下,提出了选择低背景值(≤0.25ng/g Au)泡塑分离富集Au,采用3.0g/L硫脲-1%盐酸为解脱液可消除记忆效应,在标准系列中加入5μg/mL的Fe3+溶液扣除铁对测定金的干扰。采用本分析方法对国家标准物质GBW07805、GBW07242、GBW07244a、GBW07245a和GBW07247进行测定,相对误差≤4.7%,相对标准偏差(RSD)≤23.2%;采用FAFS法与ICP-MS法对90个原生晕样品和4个控制样品中痕量金同时进行测定,两组测定结果数统计分析的F检验值为1.23,相关系数为1.01,符合性较好,无显著性差异。本分析方法简便、快速与实用,金检出限为0.08ng/g,线性范围为0.08~500ng/g,可达3个数量级。
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| 关 键 词： | 痕量金 火焰原子荧光光谱法 硫脲-盐酸 基体干扰 记忆效应 |
| 收稿时间： | 2018/9/26 0:00:00 |
| 修稿时间： | 2019/6/10 0:00:00 |
Determination of Trace Gold in Geochemical Samples by Flame Atomic Fluorescence Spectrometry with PUFP Separation and Enrichment |
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| SHEN Yu-min,LUO Zhi-ding,GUO Xiao-biao,WU Gang,WANG Chen-rong,FU Ai-rui,GAO Shu-lin and XIAO Fan.Determination of Trace Gold in Geochemical Samples by Flame Atomic Fluorescence Spectrometry with PUFP Separation and Enrichment[J].Rock and Mineral Analysis,2020,39(1):127-134. |
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| Authors: | SHEN Yu-min LUO Zhi-ding GUO Xiao-biao WU Gang WANG Chen-rong FU Ai-rui GAO Shu-lin and XIAO Fan |
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| Institution: | Hebei Research Center for Geoanalsis, Baoding 071052, China,Hebei Research Center for Geoanalsis, Baoding 071052, China,Hebei Research Center for Geoanalsis, Baoding 071052, China,Hebei Research Center for Geoanalsis, Baoding 071052, China,Hebei Research Center for Geoanalsis, Baoding 071052, China,Hebei Research Center for Geoanalsis, Baoding 071052, China,Beijing Gold-Suokun Technology Developing Co. LTD, Beijing 102600, China and Hebei Research Center for Geoanalsis, Baoding 071052, China |
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| Abstract: | BACKGROUND: The detection sensitivity, stability, and linear range of Au using flame atomic fluorescence spectrometry(FAFS) is comparable to the method of inductivity coupled plasma-mass spectrometry(ICP-MS). When Au concentration is below 0.5 ng/g, it is difficult to accurately determine Au if the interference elements in FAFS are not separated and eliminated.OBJECTIVES: To optimize the conditions during determination of trace Au by FAFS method.METHODS: The optimized conditions for trace Au detection using FAFS were provided based on the conventional Au separation and enrichment method of polyurethane foam plastics(PUFP). Using the thiourea(3.0 g/L) and HCl(1%) as desorption solution can effectively eliminate the Au memory effect after separation by PUFP with low Au background value(≤0.25 ng/g), and 5μg/mL of Fe3+ solution added into Au standard solutions was used to eliminate the interference during Au detection using FAFS.RESULTS: The method was used to analyze national standard materials GBW07805, GBW07242, GBW07244 a, GBW07245 a and GBW07247, which yielded the relative error(RE) and relative standard deviation(RSD) of less than 4.7% and 23.2%, respectively. The Au contents for 90 primary halo samples and 4 monitor samples were analyzed simultaneously using FAFS and ICP-MS. Results showed that no significant differences existed between the two methods with F=1.23 and the correlation coefficient of 1.01, which further proved the accuracy and reliability of FAFS. CONCLUSIONS: FAFS is simple, convenient, fast and practical. Method detection limit of Au is as low as 0.08 ng/g, and the linear range(0.08-500 ng/g) is three orders of magnitude. |
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| Keywords: | trace gold flame atomic fluorescence spectrometry thiourea-hydrochloric acid matrix interference memory effect |
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