酸溶-电感耦合等离子体发射光谱测定不同类型铍矿中的主次量元素方法优化  

Determination of 9 Major and Minor Elements in Beryllium Ore byICP-OES with Acid Dissolution

作　　者：于汀汀 王蕾[1] 郭琳[1] 安子怡[1] 臧慧媛 马生凤[1] YU Tingting;WANG Lei;GUO Lin;AN Ziyi;ZANG Huiyuan;MA Shengfeng(National Research Center for Geoanalysis,Beijing 100037,China;Shougang Institute of Technology,Beijing 100144,China)

机构地区：[1]国家地质实验测试中心,北京100037 [2]首钢工学院,北京100144

出　　处：《岩矿测试》2023年第5期923-933,共11页Rock and Mineral Analysis

基　　金：国家重点研发计划项目(2021YFC2903000)课题“战略性矿产多元素同时分析技术和标准化”。

摘　　要：铍矿石是中国的紧缺金属矿产之一,已在多领域有广泛应用,但其组分复杂,铍含量差别较大,且常与其他金属矿物伴生,给分析测试带来诸多挑战,制约了铍矿产的勘查开发。电感耦合等离子体发射光谱法(ICP-OES)目前用于分析铍矿石仅针对单一类型样品,且存在基体干扰、分解不完全等不足,需建立适用于多种类型的铍矿石样品、仪器分析溶液基体干扰小的多元素同时测定方法。本文选用绿柱石、香花石、日光榴石样品,比较了电热板、高压密闭、微波消解、不同种类消解酸和提取酸等8种酸消解条件对铍矿石的分解效果,优化了称样量、加酸量、消解时间和仪器测定参数,建立了ICP-OES测定铍矿石中铝铍钙铁钾钠镁锂锰9种主次量元素的分析方法。结果表明,电热板消解的混合酸为硝酸-盐酸-氢氟酸-高氯酸最佳,提取酸为盐酸优于硝酸或王水,高压密闭法不能完全消解绿柱石Al、Ca、Mg元素,微波法对绿柱石Mg元素消解效果较差。通过优化现有方法的混合酸消解条件和仪器测定条件,建立的方法对精矿样品也能准确测定,仪器测定溶液的基体简单。本方法 Be元素检出限0.0001%,低于铍矿石边界品位,其他元素检出限均优于现有的标准方法,主量元素精密度(RSD)均<5%,经标准物质验证,准确度满足铍矿石测定需要。该方法适用于不同类型和不同含量铍矿石样品的多元素同时分析。BACKGROUND:Beryllium ore is one of the scarce metal minerals in China.Beryllium ore is widely used mineral resources,but it has complex components,and is always concomitant with other metallic minerals.Accurate determination of primary and secondary elements in beryllium ore is significant for its comprehensive utilization.Inductively coupled plasma-optical emission spectrometry(ICP-OES)has been used in elemental analysis of beryllium ore.However,there are some disadvantages:It is considered that beryllium concentrate is difficult to completely decompose by acid dissolution;determination of beryllium concentrate by alkali fusion has serious matrix interference;the existing research focuses on analysis of a single type of beryllium ore.OBJECTIVES:To establish a multi-element simultaneous determination method,which is suitable for various types of beryllium ore samples and has little interference with the matrix of instrumental analysis solution.METHODS:Beryl,hsianghualite and helvite samples were selected in the experiment.Digestion effect on beryllium ore under eight different acid digestion conditions were compared,such as digestion on electric heating board,high pressure sealing,microwave digestion,different kinds of acid digestion and extraction acid.The weight of the sample,the volume of the acid,the digestion time and instrument measurement were optimized.At the same time,according to beryllium ore’s mode of occurrence of elements,the best spectrum lines of each element were determined.RESULTS:(1)The results show that the best mixed digested acid on electric heating board is nitric acidhydrochloric acid-hydrofluoric acid-perchloric acid.The best extracted acid is hydrochloric acid,which is better than nitric acid or aqua regia.The high-pressure sealing method cannot completely dissolve Al,Ca and Mg elements of beryl,and the microwave method has poor effect on the digestion of Mg elements of beryl.(2)The digestion conditions are determined.Weigh the sample of 0.1000g into polytetrafluoroethylene crucible,mo

关 键 词：铍矿石 电感耦合等离子体发射光谱法 酸消解 仪器测定参数 多元素同时分析 

分 类 号：P585.3[天文地球—岩石学]