X射线荧光熔融法测定萤石中主次成分

详细信息    查看官网全文

• 英文论文题名：Determination of major and minor components in fluorite by fusion-X-ray fluorescence spectrometry
• 论文作者：吴超超 ; 马秀艳 ; 邢文青 ; 林丽芳 ; 李世晶
• 英文论文作者：WU Chao-chao ; MA Xiu-yan ; XING Wen-qing ; LIN Li-fang ; LI Shi-jing ; Baosteel Group shaoguan iron and steel co. ; LTD
• 年：2016
• 作者机构：宝钢集团广东韶关钢铁有限公司;
• 论文关键词：X射线荧光法 ; 熔融法 ; 萤石 ; 氟含量
• 英文论文关键词：X-ray fluorescence spectrometry ; fusion method ; Fluorite ; F content
• 会议召开时间：2016-12-02
• 会议录名称：第八届中国金属学会青年学术年会论文集
• 语种：中文
• 分类号：O657.34;TF044
• 学会代码：ZGJS
• 会议名称：第八届中国金属学会青年学术年会
• 会议地点：中国辽宁沈阳
• 主办单位：中国金属学会
• 学会名称：中国金属学会
• 页数：5
• 文件大小：310k
• 原文格式：O
• 会议级别：全国

摘要

采用四硼酸锂和碳酸锂混合熔剂,硝酸钠为氧化剂,实现了利用X射线熔融法对萤石中各组分含量的准确测定。探讨了熔融温度、稀释比、熔融时间等因素对氟含量测定的影响,得到了最佳试验条件。试验表明,当试样熔剂稀释比(m_(试样):m_(无水四硼酸锂))为1:4,碳酸钠0.5000g,硝酸钠氧化剂0.5000g,熔融温度980℃,熔融时间8 min时,氟、硫元素的损耗最小,且F的荧光强度最大。在最佳试验条件下,得到氟化钙、二氧化硅、硫、磷含量测定的线性相关系数分别为0.9989、0.9999、0.9993、0.9981,其精密度分别为0.31%、0.72%、0.92%、3.58%。试验结果表明,采用X射线荧光熔融法测定萤石,其测定值与标样值、化学分析值相符,符合常规检测要求。
The accurate determination method of CaF_2,SiO_2,S,P in fluorite by X-Ray fluorescence spectrometry(XRF)was established with fusion sample preparation of taking lithium tetraborate and lithium carbonate as mixed solvent and sodium nitrate as oxidant.In order to get the optimum experimental condition,the influences on the determination of fluorine content in fluorite,such as the melting temperature,dilution ratio and melting time were discussed.Testing results showed that on the condition that the sample dilution ratio(m_(sample):m_(Li2B407))was 1:4,the mass of sodium carbonate was 0.5000 g,the mass of sodium nitrate was 0.5000 g,melting temperature was 980℃ and the melting time was 8 minutes,the loss of F,S was minimum and the intensity of F yield maximum.Under the optimum conditions,the correlation coefficient of CaF_2,SiO_2,S,Pwere 0.9989,0.9999,0.9993,0.9981 respectively,and the precision of RSD were 0.31%,0.72%,0.92%and 0.31%respectively.The results showed that the XRF results were in conformity with the standard values and chemical analysis value,met the requirements of routine analysis.

引文

[1]付华.冶金辅料制样的可靠性及其保证措施[J].冶金分析,2004,24(4):73-74.FU Hua.Reliability of preparation of metallurgical assist material samples and its guarantee measure[J].Metallurgical Analysis,2004,24(4):73-74.
    [2]王兆利,马宏彦.杜建民,等.熔融制样X射线荧光光谱法测定萤石中成分[J].河南冶金,2009,17(6):24-26.Wang Zhao-li,Ma Hong—yan,Du Jian-mi,et al.Component Analysis of Fluorite by X-Ray Fluorescent Spectrometry[J].HeNan Metallurgy.2009,17(6):24-26.
    [3]杜燕,阚斌.玻璃熔融X射线荧光光谱法测定萤石中各组分[J].科学技术与工程,2006,6(18):2938-2939.DU Yan,HAN Bing.Determination of the Component of Fluorite by XRF Method[J].Science Technology and Engineering,2006,6(18):2938-2939.
    [4]李韶梅,杜彩霞,张慧娟.X射线荧光光谱法测定萤石中氟化钙、二氧化硅、氧化铝、全铁的含量[J].理化检验:化学分册,2011(10):1162-1164.LI Shao-mei,DU Cai-xia,ZHANG Hui-juan.XRFS Determination of CaF_2,SiO_2,Al_2O_3 and Total Iron in Fluorspar[J].PTCA(PART B:CHEM.ANAL.)2011(10):1162-1164.
    [5]袁家义.X射线荧光光谱法测定萤石中氟化钙[J].岩矿测定,2007,26(5):419-420.YUAN Jia-yi.Determination of Calcium Fluoride in Fluorspar by X-ray Fluorescence Spectrometry[J].Rock and Mineral Analysis,2007,26(5):419-420.
    [6]袁建,夏晨光,刘高辉,等.X射线荧光光谱法测定高氟地质样品中氟、钙等元素[J].铀矿地质,2016,32(3):175-179.YUAN J ian.XIA Chenguang.LIU Gaohui,et al.Determination of F,Ca and Other Major Elements in High Fluoride Concentration Samples by X-ray Fluorescence Spectrometry[J].Uranium Geology,2016,32(3):175-179.
    [7]偷云.粉末压片-X射线荧光光谱法与红外吸收光谱法联合测定萤石中各组分[J].中国无机分析化学,2014,4(1):50-52.XIAN Yun.Analysis of Component in Fluorite Using Pressed Powder Pellet X-ray Fluorescence Spectrometry Combined with Infrared Spectroscopy[J].Inorganic Analytical Abstracts of China,2014,4(1):50-52.
    [8]杨旗风,白晓华.小型X射线荧光光谱仪快速分析萤石的成分[J].光谱实验室,2003,20(3):344-346.YANG Qi-Feng BAI Xiao-Hua.Rapid Determination of Chemical Components in Fluorite by Small-Size X-Ray Fluorescence Spectrometer[J].Chinese Journal of Spectroscopy Laboratory,2003,20(3):344-346.
    [9]刘长春,郭慧,陈莹,等.X-射线荧光与红外联合测定萤石中各组分含量[J].辽东学院学报:自然科学版,2014,21(4):252-256.LIU Chang-chun,GUO Hui,CHEN Yin,et al.Determination of Component Concentration of Fluorite with X-ray Fluorescence and Infrared Absorption Spectroscopy[J].Journal of Eastern Liaoning University(Natural Science),2014,21(4):252-256.
    [10]陆晓明。吉昂,陶光仪.X射线荧光光谱法测定萤石中的氟,钙及二氧化硅[J].分析化学,1997(2):178-180.Lu Xiaoming,Ji Ang,Tao Guangyi.Determination of Fluorine,Calcium and Silicon Dioxide in Fluorite by X-Ray Fluorescence Spectrometry[J].Chinese Journal of Ana I ytical Chemistry,1997(2):178-180.
    [11]康智清,宋祖峰,牟新玉.X射线荧光光谱法测定萤石中CaF_2含量不确定度的评定[J].冶金分析,2010,30(11):74-78.KANG Zhi-qing,SONG Zu-feng,MOU Xin-y u.Evaluation of uncertainty for the determination of CaF_2 in fluorite by X-ray fluorescence spectrometry.Metallurgical Analysis,2010,30(11):74-78.