Abstract：Aiming at the problem in simultaneous determination of major and minor components in serpentine, the sample was prepared by fusion sample preparation method with Li2B4O7-LiBO2 (m:m=33:67) as flux and ammonium iodide,ammonium bromide as releasing agent. The determination method of major and minor components (including SiO2, MgO, Fe2O3, Al2O3 and CaO) in serpentine by X-ray fluorescence spectrometry (XRF) was established. The optimized fusion conditions were as follows: the dilution ratio was 10:1; 4 drops of 400 g/L NH4Br solution and 14 drops of 400 g/L NH4I solution were added as the releasing agent; pre-oxidization at 700 ℃ for 4 min; fusion at 1 050 ℃ for 6 min. The national certified reference materials of talcum, brucite and non-metallic ore with similar mineral properties to serpentine were used to prepare the calibration samples. The calibration curve was established using fundamental parameter method to correct the matrix effect. The detection limit was 80-170 μg/g. The precision test was conducted with one serpentine sample from the East China Sea, and the relative standard deviations (RSD, n=10) were not more than 0.70%. The proposed method was applied to the determination of two serpentine samples. The results were consistent with those obtained by industrial standard method (HG/T 3575-2006).
冯晓军. 熔融制样-X射线荧光光谱法测定蛇纹石中主次组分[J]. 冶金分析, 2017, 37(4): 27-32.
FENG Xiao-jun. Determination of major and minor components in serpentine by X-ray fluorescence spectrometry with fusion sample preparation. , 2017, 37(4): 27-32.
杜建民,郑建道,杜娟.X荧光分析蛇纹石方法研究[J].河南冶金,2011,19(5):17-18.DU Jian-min,ZHENG Jian-dao,DU Juan.Study on X-ray fluorescence melting analysis to serpentine[J].Henan Metallurgy,2011,19(5):17-18.
[4]
蒋薇.X射线荧光光谱法测定蛇纹石成分[J].化学分析计量,2009,18(3):80-81.JIANG Wei.Determination of serpentine composition by X-ray fluorescence spectrometry[J].Chemical Analysis and Meterage,2009,18(3):80-81.
[5]
王曼娟,刘琰,戴国宜,等.X射线荧光光谱法测定蛇纹石组分的方法研究[J].安徽冶金,2012(3):22-23.WANG Man-juan,LIU Yan,DAI Guo-yi,et al.To determine the composition of serpentine with XRF[J].Anhui Metallurgy,2012(3):22-23.
[6]
李国会,李小莉.X射线荧光光谱分析熔融法制样的系统研究[J].冶金分析,2015,35(7):1-9.LI Guo-hui,LI Xiao-li.Systematic study on the fusion sample preparation in X-ray fluorescence spectrometric analysis[J].Meteallurgical Analysis,2015,35(7):1-9.
[7]
高志军,陈静,陈浩凤,等.熔融制样-X 射线荧光光谱法测定硅酸盐和铝土矿中主次组分[J].冶金分析,2015,35(7):73-78.GAO Zhi-jun,CHEN Jing,CHEN Hao-feng,et al.Simulatanous determination of major and minor components in silicate and bauxite by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2015,35(7):73-78.
[8]
施善林,郭阳,李东麟,等.熔融制样-X 射线荧光光谱法测定镍铁冶炼过程物料中10种组分[J].冶金分析,2015,35(7):54-59.SHI Shan-lin,GUO Yang,LI Dong-lin,et al.Determination of ten components in ferronickel smelting process materials by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2015,35(7):54-59.
[9]
赵恩好,岳明新,周国兴,等.X射线荧光光谱法测定镁质耐火材料及原料中10种成分[J].冶金分析,2013,33(7):62-67.ZHAO En-hao,YUE Ming-xin,ZHOU Guo-xing,et al.Determination of ten components in magnesia refeactory materials and raw materials by X-ray fluorescence spectometry[J].Metallurgical Analysis,2013,33(7):62-67.
[10]
张香荣,陈洁,张立新.铝质、硅质和镁质耐火材料的X射线荧光光谱快速分析[J].冶金分析,2005,25(1):15-18.ZHANG Xiang-rong,CHEN Jie,ZHANG Li-xin.Rapid analysis of silicon,magnesium and aluminium base refractory materials by XRF[J].Metallurgical Analysis,2005,25(1):15-18.
[11]
张殿英,李超,钱菁,等.X射线荧光光谱法测定转炉渣中8种成分[J].冶金分析,2009,29(6):41-46.ZHANG Dian-ying,LI Chao,QIAN Jing,et al.Determination of eight components in converter slag by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2009,29(6):41-46.
[12]
张鹏,曲月华,王一凌.X射线荧光光谱法测定镁砂、镁石及菱镁矿中主次成分[J].冶金分析,2010,30(9):28-31.ZHANG Peng,QU Yue-hua,WANG Yi-ling.Determination of major and minor elements in magnesia,humite and mangnesite by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2010,30(9):28-31.
[13]
王芙云,袁翠菊,任向阳.X射线荧光光谱法快速分析镁质耐火材料中硅铝铁钛钙镁[J].岩矿测试,2008,27(3):232-234.WANG Fu-yun,YUAN Cui-ju,REN Xiang-yang.Rapid determination of SiO2,Al2O3,Fe2O3,TiO2,CaO and MgO in magnesium-based refractory materials by X-ray fluorescence spectrometry with powder pellet sample preparation[J].Rock and Mineral Analysis,2008,27(3):232-234.
[14]
李可及,易建春,潘钢.X射线荧光光谱法测定磷矿石中11种主次组分[J].冶金分析,2013,33(9):22-27.LI Ke-ji,YI Jian-chun,PAN Gang.Determination of eleven major and minor components in phosphate ores by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2013,33(9):22-27.
