Abstract：The portable X-ray fluorescence spectrometer (PXRF) has many advantages such as rapid detection speed and simultaneous determination of multi-elements, and it has been widely used in various on-site tests. The geological samples usually contain abundant associated minerals and complex matrix. Moreover, the interference is very easily caused among elements. Therefore, the on-site application of PXRF is limited. One fluorite associated antimony ore sample from Guizhou was selected as an example for the on-site analysis of calcium by PXRF. Due to the insufficient design of application software and the limitation of energy resolution of instrument, the energy of characteristic spectral line of antimony in sample was superposed on the characteristic spectral line of calcium, leading to higher detection result of calcium. The determination of actual sample indicated that the degree of deviation was relevant to the content of antimony in sample. By regression trend analysis and exponentiation regression, the equation of y=0.3519x0.8881 (x presented the content of antimony measured by PXRF, while y presented the content of false calcium which was affected by antimony) was obtained with correlation coefficient of R2=0.9992. Then, the actual content of calcium could be obtained by subtracting false calcium from total calcium. 15 samples were analyzed for verification. It was found that the determination results after correction were basically consistent with those obtained by EDTA titration in laboratory. The detection limit was 0.077%, the relative standard deviation (RSD) was 1.2%, and the determination range was 3%-30%. The experimental method well solved the problem for the on-site detection of calcium in this mine area. It could rapidly guide the searching of ore body, saving much cost and time.
宋新艳.萤石中二氧化硅和氟化钙的系统分析[J].冶金分析,2010,30(10):58-61.SONG Xin-yan.Systematic analysis of silicon dioxide and calcium fluoride in fluorite[J].Metallurgical Analysis,2010,30(10):58-61.
苏峥,马建平.X射线荧光光谱法与红外吸收法联合测定萤石中氟化钙[J].冶金分析,2008,28(8):73-75.SU Zheng,MA Jian-ping.Determination of calcium fluoride in fluorite with X-ray fluorescence spectrometry and infrared absorption[J].Metallurgical Analysis,2008,28(8):73-75.
[4]
吴超超,马秀艳,邢文青,等.熔融制样-X射线荧光光谱法测定萤石中主次成分[J].冶金分析,2017,37(4):42-47.WU Chao-chao,MA Xiu-yan,XING Wen-qing,et al.Determination of major and minor components in fluorite by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2017,37(4):42-47.
[5]
杨珍,孙银生,贺攀红,等.电感耦合等离子体原子发射光谱法快速测定萤石矿中氟化钙[J].冶金分析,2013,33(11):71-73.YANG Zhen,SUN Yin-sheng,HE Pan-hong,et al.Rapid determination of calcium fluoride in fluorite by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2013,33(11):71-73.
[6]
陆安祥,王纪华,潘立刚,等.便携式X射线荧光光谱测定土壤中Cr,Cu,Zn,Pb和As的研究[J].光谱学与光谱分析,2010,30(10):2848-2852.LU An-xiang,WANG Ji-hua,PAN Li-gang,et al.Determination of Cr,Cu,Zn,Pb and As in soil by field portable X-ray fluorescence spectrometry[J].Spectroscopy and Spectral Analysis,2010,30(10):2848-2852.
[7]
郭龙滨,赖万昌,张永涛,等.便携式能量色散X射线荧光仪测定矿渣中铟[J].冶金分析,2011,31(1):19-22.GUO Long-bin,LAI Wan-chang,ZHANG Yong-tao,et al.Determination of indium in slag using portable energy dispersive X-ray fluorescence spectrometer[J].Metallurgical Analysis,2011,31(1):19-22.
[8]
张鹏,张寿庭,邹灏,等.便携式X荧光分析仪在萤石矿勘查中的应用[J].物探与化探,2012,36(5):718-722.ZHANG Peng,ZHANG Shou-ting,ZOU Hao,et al.The application of portable X-ray fluorescence analyzer to fluorite prospecting[J].Geophysical & Geochemical Exploration,2012,36(5):718-722.
[9]
李向超.便携式X射线荧光光谱仪现场测定地质样品中钛[J].冶金分析,2014,34(4):32-36.LI Xiang-chao.On-site determination of titanium in geological samples by portable X-ray fluorescence spectrometer[J].Metallurgical Analysis,2014,34(4):32-36.
