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投稿时间:2023-02-23 修订日期:2023-09-22
投稿时间:2023-02-23 修订日期:2023-09-22
中文摘要: 钨锡矿石共生与伴生元素多,为克服常用的钨锡矿石中锡、钨、钼、铜、铅、锌、硫、砷等8种元素检测过程程序繁琐,效率低下问题,通过在刚玉坩埚中直接加入氢氟酸挥发掉样品中的二氧化硅,用过氧化钠熔融已除硅的样品,再以酒石酸+磷酸+盐酸提取,解决了碱熔酸化的样品溶液中硅胶的影响和钨、锡等元素的不稳定性问题,建立了电感耦合等离子体发射光谱(ICP-OES)法直接测定样品中的锡、钨、钼、铜、铅、锌、硫、砷的方法。系统研究了过氧化钠熔剂的用量对各元素的影响,考察了引入单一酒石酸的络合作用和酒石酸+磷酸的混酸对各元素的影响,结果表明,过氧化钠用量为1.0 g时样品可以完全分解;单一酒石酸的络合作用有限,钨含量高的样品容易发生沉淀,而酒石酸+磷酸的混酸可以使钨在溶液中长期稳定,而对其他元素没有影响。选用5个钨、锡矿石国家一级标准物质按照本方法进行处理,测定结果均在认定值的误差范围内;采用4个实际样品与标准方法进行比对实验,各元素检测结果无显著差异。各元素的光谱强度在0~200 μg/mL浓度范围内呈良好的线性关系,相关系数(r)均在0.999 9以上,方法检出限值为3.0μg/g~25.0 μg/g,相对标准偏差RSD(n=12)为0.33%~7.0%。方法测试过程操作简便,检测结果准确、可靠,在多元素大批量的样品检测中具有明显优势。
中文关键词: 电感耦合等离子体发射光谱(ICP-OES)法 过氧化钠 氢氟酸 磷酸 钨锡矿石
Abstract:There are many symbiosis and associated elements in tungstannic tin ore. In order to overcome the cumbersome and inefficient detection process of 8 elements in common tungstannic tin ore, such as tin, tungsten, molybdenum, copper, lead, zinc, sulfur and arsenic, the silica in the sample was volatilized by adding hydrofluoric acid directly into the corundum crucible, and the silicon removed sample was fused with sodium peroxide, and then extracted with tartric acid + phosphoric acid + hydrochloric acid. The effect of silica gel and the instability of tungsten and tin in sample solution of alkali melt acidification were solved. A method for the direct determination of tin, tungsten, molybdenum, copper, lead, zinc, sulfur and arsenic in samples by inductively coupled plasma emission spectrometry (ICP-OES) was established. The influence of sodium peroxide flux dosage on each element was systematically studied. The complexation of single tartric acid and the influence of mixed acid of tartric acid and phosphoric acid on each element were investigated. The results showed that the sample could be completely decomposed when the dosage of sodium peroxide was 1.0 g. The complexation of single tartric acid is limited, and the samples with high tungsten content are easy to precipitate, while the mixed acid of tartric acid and phosphoric acid can stabilize tungsten in the solution for a long time, but has no effect on other elements. Five national first-class reference materials of tungsten and tin ores were selected for treatment according to this method, and the measured results were all within the error range of the confirmed values. Four actual samples were compared with the standard method, and there was no significant difference in the detection results of each element. The spectral intensities of each element showed a good linear relationship in the concentration range of 0 ~ 200 μg/mL, and the correlation coefficients (r) were above 0.999 9. The detection limits of the method were 3.0μg/g ~ 25.0 μg/g, and the relative standard deviations (RSDS) (n=12) were 0.33% ~ 7.0%. Methods The test process is simple, the test results are accurate and reliable, and it has obvious advantages in the multi-element sample detection.
keywords: Inductively coupled plasma emission spectrometry (ICP-OES) method Na2O2 HF H3PO4 Tungsten-tin ore
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基金项目:国家自然科学基金项目(面上项目,重点项目,重大项目)
引用文本:
杨林,邹国庆,周武权,李瑞娟,李海娟,隋东,张行荣.碱熔-电感耦合等离子体发射光谱(ICP-OES)法测定钨锡矿石中钨锡钼铜铅锌硫砷[J].中国无机分析化学,2023,13(11):1191-1196.
yang lin,Zou Guoqing,Zhou Wuquan,Li Ruijuan,Li Haijuan,Sui Dong,Zhang Xingrong.Determination of W, Sn, Mo, Cu, Pb, Zn, S, As in Tungsten-tin Ore by Alkali Fusion-Inductively Coupled Plasma Emission Spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2023,13(11):1191-1196.
杨林,邹国庆,周武权,李瑞娟,李海娟,隋东,张行荣.碱熔-电感耦合等离子体发射光谱(ICP-OES)法测定钨锡矿石中钨锡钼铜铅锌硫砷[J].中国无机分析化学,2023,13(11):1191-1196.
yang lin,Zou Guoqing,Zhou Wuquan,Li Ruijuan,Li Haijuan,Sui Dong,Zhang Xingrong.Determination of W, Sn, Mo, Cu, Pb, Zn, S, As in Tungsten-tin Ore by Alkali Fusion-Inductively Coupled Plasma Emission Spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2023,13(11):1191-1196.