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文章摘要
陈景伟,宋江涛,陈朝阳.X射线荧光光谱法测定重晶石中的硫酸钡方法研究[J].岩矿测试,2017,36(4):382-387
CHEN Jing-wei,SONG Jiang-tao,CHEN Zhao-yang.Method Research on Determination of Barium Sulfate in Barite by X-ray Fluorescence Spectrometry[J].Rock and Mineral Analysis,2017,36(4):382-387.DOI:10.15898/j.cnki.11-2131/td.201608040115
X射线荧光光谱法测定重晶石中的硫酸钡方法研究
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Method Research on Determination of Barium Sulfate in Barite by X-ray Fluorescence Spectrometry
投稿时间:2016-08-04  修订日期:2017-07-15
DOI:10.15898/j.cnki.11-2131/td.201608040115
中文关键词: 重晶石  硫酸钡  酸处理  氧化铝  玻璃熔片制样  波长色散X射线荧光光谱法
英文关键词: barite  barium sulfate  acid treatment  alumina  sample preparation of glass melting  Wavelength Dispersion X-ray Fluorescence Spectrometry
基金项目:
作者单位
陈景伟 山东省第四地质矿产勘查院, 山东 潍坊 261021 
宋江涛 山东省第四地质矿产勘查院, 山东 潍坊 261021 
陈朝阳 济南大学, 山东 济南 250022 
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中文摘要:
      应用XRF可快速测定重晶石中钡元素的总量,但当测定硫酸钡含量时,由于样品中的碳酸钡计入钡量造成硫酸钡的测定结果不准确,铜、铅、锌等有色金属元素对熔样坩埚会造成损害,需要进行酸处理除去碳酸钡、铅等干扰。而样品经酸处理后不同样品的剩余量不同,造成熔剂与样品的比例不确定,也不能准确测定硫酸钡的含量,因此保证熔剂与样品比例一致是解决该问题的关键。本文优化了样品前处理、熔片制样和仪器工作条件,将一定量样品以10%盐酸和10%硝酸溶解,过滤除去碳酸钡、硫酸钙及铜、铅、锌等有色金属元素,未溶解样品在700℃下灼烧后以氧化铝补充到原取样量,实现了熔剂与样品比例一致,再以硝酸铵作氧化剂,溴化锂和碘化铵作脱模剂,1075℃熔融制片,即可用XRF准确测定硫酸钡的含量。本方法的相对标准偏差(RSD)小于0.4%,检出限为72 μg/g,较ICP-OES等方法的检测周期短、干扰元素少,提高了测试效率和分析质量。
英文摘要:
      X-ray Fluorescence Spectrometry (XRF) can be used to rapidly determine the total content of barium in barite. However, the barium carbonate included in the total barium will result in inaccurate results of barium sulfate. Moreover, copper, lead, zinc and other non-ferrous metal elements can damage the sample melting pot. Acid treatment is required to remove interference such as barium carbonate and lead. The residue ratio of the different samples after the acid treatment is different to before and the ratio of the flux to sample is uncertain, and thus the content of barium sulfate cannot be accurately determined. Therefore, it is essential to ensure that the melting agent has the same proportion as the sample. The sample pretreatment conditions, melting conditions and equipment conditions were optimized and are described in this paper. 10% hydrochloric acid mixed with 10% nitric acid was used to dissolve the sample. The sample solution was filtered to remove barium carbonate, calcium sulfate and copper, lead, zinc and other non-ferrous metal elements. Alumina oxide was added to undissolved samples after 700℃ calcination to reach the original sample weight, which attains the same proportion of flux and sample. Ammonium nitrate was used as the oxidant, and lithium bromide and ammonium iodide were used as demoulding agents. Samples were melted at 1075℃, and barium sulfate content in the barite was determined by XRF. The relative standard deviation (RSD) of the method is less than 0.4% and the detection limit is 72 μg/g. This method needs less detection time and suffers from less interference elements than determination by Inductively Coupled Plasma-Optical Emission Spectrometry, improving the test efficiency and analysis quality.
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