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中国无机分析化学:2022,12(3):87-94
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巯基葡聚糖(SDG)分离富集-原子荧光光谱法测定地球化学样品中的锡
徐冰旭1, 寻倩男1, 刘亚轩2, 张鹏鹏2, 李刚1, 易建春1, 赵朝辉1, 袁超飞3
(1.中国地质科学院矿产综合利用研究所;2.中国地质科学院地球物理地球化学勘查研究所;3.河北省地质矿产勘查开发局)
Determination of Tin in Geochemical Samples by Atomic Fluorescence Spectrometry with Alkaline Fusion, Acid Solution Plus Alkaline Fusion and SDG Separation and Enrichment
XU Bing-xu1, XUN Qian-nan1, LIU Ya-xuan2, ZHANG Peng-peng2, LI Gang1, YI Jian-chun1, ZHAO Chao-hui1, YUAN Chao-fei3
(1.Institute of Comprehensive Utilization of Mineral Resources,CAGS Chengdu;2.Institute of Geophysical and Geochemical Exploration,Chinese Academy of Geological Sciences;3.Hebei Bureau of Geology and Mineral Resources Exploration)
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投稿时间:2021-07-01    修订日期:2021-07-05
中文摘要: 地球化学样品中锡的测定大多采用以电弧为光源的发射光谱法,该方法为固体进样具有一定的局限性,笔者建立了采用液体进样的原子荧光光谱法测定地球化学样品中的锡弥补了前者的不足。该方法采用了三种不同的前处理过程,分别为碱熔法,酸溶加碱熔法和巯基葡聚糖(SDG)分离富集法。选择4个国家一级地球化学标准物质对碱熔法的熔剂比例、熔样温度和熔剂与样品比例等条件进行了优化,结果表明:当过氧化钠与氢氧化钠比例为5:1,熔剂与样品比例为6:1,在750℃的温度下熔样时,锡的溶出效果最好。酸溶加碱熔的条件在文章不做详述。选择3个国家一级地球化学标准物质对SDG分离富集法的过柱溶液酸度、洗脱液酸度以及洗脱液体积等条件进行了优化,得出结论:当过柱溶液酸度为1%的盐酸时锡的吸附率最高;用3mol·L-1的盐酸作为洗脱液时锡的脱附率最高,且25mL的洗脱液可以把锡完全洗脱出来。碱熔法,酸溶加碱熔法和SDG分离富集法的方法检出限分别为1.03μg·g-1、0.60μg·g-1、0.58μg·g-1,方法精密度分别为3.0%~6.0%、7.0%~9.0%、8.0%~9.0%。选择多个国家一级地球化学标准物质进行方法验证,所有样品的准确度均在90%以上。三种前处理方法均可用于地球化学样品中锡的测定。
Abstract:The tin in geochemical samples mostly determined by emission spectroscopy using arc as light source, which has certain limitations for sample introduction with solid. The author established the atomic fluorescence spectrometry that introducing samples with liquid to measure tin in geochemical samples to make up for the former’s shortcomings. This method uses three different pre-treatment processes, namely the alkaline fusion method, the acid solution plus alkali fusion method and the sulfhydryl dextran (SDG) separation and enrichment method. Four national first-level geochemical reference materials were selected to optimize the flux ratio, melting sample temperature, and flux to sample ratio of the alkali fusion method. The results showed that when the ratio of sodium peroxide to sodium hydroxide was 5:1,the ratio of flux to sample was 6:1, the samples were melted at the temperature of 750℃, the dissolution effect of tin was the best. The conditions of acid fusion plus alkali fusion were not detailed in the article. Three national first-level geochemical standard materials were selected to optimize the column solution acidity, eluent acidity and eluent volume of SDG separation and enrichment method. It was concluded that when the column solution acidity was 1% hydrochloric acid, the adsorption rate of tin was the highest; when 3mol·L-1 hydrochloric acid was used as the eluent, the desorption rate of tin was the highest, and the tin can be completely eluted with 25 mL of the eluent. The detection limits of alkali fusion method, acid fusion plus alkali fusion method and SDG separation and enrichment method were 1.03μg·g-1, 0.60μg·g-1, 0.58μg·g-1, and the method precisions were 3.0 %~6.0%, 7.0%~9.0%, 8.0%~9.0%. A number of national first-level geochemical reference materials were selected for methods verification, and the accuracy of all samples was above 90%. All the three pretreatment methods can be used for the determination of tin in geochemical samples.
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基金项目:中国地质科学院物化探研究所基本科研业务费
引用文本:
徐冰旭,寻倩男,刘亚轩,张鹏鹏,李刚,易建春,赵朝辉,袁超飞.巯基葡聚糖(SDG)分离富集-原子荧光光谱法测定地球化学样品中的锡[J].中国无机分析化学,2022,12(3):87-94.
XU Bing-xu,XUN Qian-nan,LIU Ya-xuan,ZHANG Peng-peng,LI Gang,YI Jian-chun,ZHAO Chao-hui,YUAN Chao-fei.Determination of Tin in Geochemical Samples by Atomic Fluorescence Spectrometry with Alkaline Fusion, Acid Solution Plus Alkaline Fusion and SDG Separation and Enrichment[J].Chinese Journal of Inorganic Analytical Chemistry,2022,12(3):87-94.

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