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中国无机分析化学:2023,13(8):883-887
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阳离子树脂交换分离-电感耦合等离子体质谱(ICP-MS)法测定地质石膏样品中硼
刘金龙1, 何汉江2, 冯慧琳2, 张 霞2, 王艳超2
(1.中化地质矿山总局地质研究院;2.中化地质矿山总局 地质研究院,河北 涿州 072750)
Determination of Boron in Geological Gypsum Samples by Inductively Coupled Plasma Mass Spectrometry with Cationic Resin Exchange Separation
LIU Jinlong1, HE Hanjiang2, FENG Huilin2, ZHANG Xia2, WANG Yanchao2
(1.China Chemical and Mine Bureau Research Institute Of Geological;2.China Chemical and Mine Bureau Research Institute Of Geological,Zhuozhou,Hebei 072750 ,China)
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本文已被:浏览 858次   下载 249
投稿时间:2023-04-21    修订日期:2023-05-10
中文摘要: 硼石膏近些年在水泥、沥青混合材料等领域应用广泛,其主要成分为CaSO4·2H2O和B2O3以及其他杂质,因此准确、快速测定石膏样品中的硼元素对石膏的应用、资源综合利用等方面具有重要意义。而国家标准GB/T 5484-2012《石膏分析方法》中并没有硼元素的化学分析方法,且相关文献报道也很少。目前测定硼元素主要采用电感耦合等离子体质谱法(ICP-MS),样品前处理多采用酸溶法,而碱熔法应用不多,主要原因是碱熔后溶液中产生大量盐分影响等离子体焰的稳定性,而732型阳离子交换树脂能吸附大量的钠离子,同时吸附了钙、镍、铁及稀土等阳离子,减少盐分干扰。基于此原理,本文采用氢氧化钠碱熔-732型阳离子交换树脂交换分离,在线加入铑内标的方式,建立了ICP-MS法测定石膏中硼的方法,同时由于石膏国家标准物质不包含硼元素的含量,采用高纯硫酸钙分别与岩石标准物质、水系沉积物国家标准物质和土壤国家标准物质混合配置成人工标准物质,并讨论了熔矿体系、阳离子加入量与吸附时间、清洗液、同位素的选择等实验条件。本方法的检出限为0.76μg/g,精密度(RSD,n=7)为0.9%~1.7%,相对误差为1.56%~3.96%,加标回收率在97.5%~102%,该方法快速、准确,记忆效应小,适合石膏中硼元素的测定。
Abstract:Boron gypsum has been widely used in cement and asphalt mixed materials in recent years. Its main components are CaSO4·2H2O, B2O3 and other impurities. Therefore, accurate and rapid determination of boron in gypsum samples is of great significance for the application and comprehensive utilization of gypsum resources. However, there is no chemical analysis method of boron in GB/T 5484-2012 Gypsum Analysis Method, and there are few related literature reports. At present, the determination of boron is mainly by inductively coupled plasma mass spectrometry (ICP-MS), and the sample pretreatment is mostly by acid solution, while the alkali fusion method is not used much. The main reason is that a large amount of salt is produced in the solution after alkali fusion, which affects the stability of plasma flame, and 732 cation exchange resin can absorb a large number of sodium ions. At the same time adsorbed calcium, nickel, iron and rare earth cations, reduce salt interference. Based on this principle, an ICP-MS method for the determination of boron in gypsum was established by using sodium hydroxide alkali melt -732 type cation exchange resin for exchange and separation, and rhodium internal mark was added online. At the same time, since the national standard material of gypsum does not contain boron content, High purity calcium sulfate was mixed with rock reference material, river sediment national reference material and soil national reference material to form artificial reference material, and the experimental conditions such as melting system, cationic addition amount and adsorption time, cleaning solution and isotope selection were discussed. The detection limit of this method is 0.76μg/g, the precision (RSDS, n=7) is 0.9%~1.7%, the relative errors are 1.56%~3.96%, and the recoveries are 97.5%~102%. The method is rapid, accurate and suitable for the determination of boron in gypsum.
文章编号:     中图分类号:    文献标志码:
基金项目:中国地质调查局项目(DD20190816)
引用文本:
刘金龙,何汉江,冯慧琳,张 霞,王艳超.阳离子树脂交换分离-电感耦合等离子体质谱(ICP-MS)法测定地质石膏样品中硼[J].中国无机分析化学,2023,13(8):883-887.
LIU Jinlong,HE Hanjiang,FENG Huilin,ZHANG Xia,WANG Yanchao.Determination of Boron in Geological Gypsum Samples by Inductively Coupled Plasma Mass Spectrometry with Cationic Resin Exchange Separation[J].Chinese Journal of Inorganic Analytical Chemistry,2023,13(8):883-887.

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