Abstract：The fluorspar sample was fused with sodium hydroxide in zirconium crucible followed by leaching with boric acid solution and acidification with nitric acid. The content of silicon, aluminum, iron, potassium, magnesium and titanium in fluorspar was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The determination method of silicon, aluminum, iron, potassium, magnesium and titanium in fluorspar was established. The influence of matrix effect was discussed. It was found that the signal intensity of potassium was slightly affected by much sodium in solution (4.37-4.83 mg/mL), but the error was less than 2.4%. Meanwhile, its influence on other elements could be negligible. Calcium (120-200 μg/mL), boron (56.8-85.2 μg/mL) and zirconium (<4 μg/mL) had no significant influence on the determination of elements. The effect of acidity was also investigated in experiments. The results indicated that the effect of acidity in certain range could be ignored. The calibration curves of elements were linear under the working conditions with correlation coefficients of r=0.999 9-1.000 0. The detection limits of method were between 3 μg/g and 105 μg/g. The determination range could cover the content range of silicon, aluminum, iron, potassium, magnesium and titanium in all fluorspar samples. The content of silicon, aluminum, iron, potassium, magnesium and titanium in certified reference materials including YSB 14791-02, GBW07252, GSB 08-1348-2001 and Fluorspar 2712 was analyzed according to the experimental method. The found results were consistent with the certified values. The relative standard deviations (RSD, n=5) were between 0.10% and 9.5%.
杨朝帅,周建辉,孔幸花,等.硅钼蓝光度法测定萤石及其精矿中二氧化硅的含量[J].冶金分析,2012,32(7):59-62.YANG Chao-shuai,ZHOU Jian-hui,KONG Xing-hua,et al.Silicon-molybdenum blue spectrophotometric determination of silica in fluorite and its concentrate[J].Metallurgical Analysis,2012,32(7):59-62.
[4]
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.
[5]
别富军.原子吸收光谱法测定萤石中氧化铝[J].有色金属:矿山部分,2010,62(1):76-78.BIE Fu-jun.Atomic absorption spectrometry in alumina fluorite[J].Nonferrous Metals:Mining Section,2010,62(1):76-78.
[6]
邹美娟,丰慧,楚明嘉.ICP-AES法测定萤石中铁、锰、磷的含量[J].安徽冶金,2004(2):39-41.ZOU Mei-juan,FENG Hui,CHU Ming-jia.ICP-AES method for determination of Fe, Mn and P in fluorite[J].Anhui Metallurgy,2004(2):39-41.
[7]
年季强,顾锋,朱春要,等.微波消解-电感耦合等离子体原子发射光谱法测定萤石中硅铁镁钾钠磷硫[J].冶金分析,2015,35(4):39-43.NIAN Ji-qiang,GU Feng,ZHU Chun-yao,et al.Determination of silicon, ferric, magnesium, potassium, sodium, phosphorus and sulfur in fluorite by microwave digestion-inductively coupled plasma atomic emission spectrometry[J]. Metallurgical Analysis, 2015, 35(4): 39-43.
[8]
闻向东,赵希文,文斌,等.电感耦合等离子体发射光谱法测定萤石中低含量的二氧化硅[J].冶金分析,2008,28(3):61-63.WEN Xiang-dong,ZHAO Xi-wen,WEN Bin,et al. Determination of low content silicon dioxide in fluorite by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2008,28(3):61-63.
[9]
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,1997,25(2):170-180.LU Xiao-ming, JI Ang, TAO Guang-yi. Determination of fluorine, calcium and silicon dioxide in fluorite by X-ray fluorescence spectrometry[J].Chinese Journal of Analytical Chemistry,1997,25(2):170-180.
[10]
袁家义.X射线荧光光谱法测定萤石中氟化钙[J].岩矿测试,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.
[11]
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):2938-2939,2975.DU Yan,HAN Bing.Determination of the component of fluorite by XRF method[J]. Science Technology and Engineering,2006,6(18):2938-2939, 2975.
[12]
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 Ying, 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.
[13]
佡云.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):50-53.XIAN Yun.Analysis of component in fluorite using pressed powder pellet X-ray fluorescence spectrometry combined with infrared spectroscopy[J]. Chinese Journa1 of Inorganic Analytical Chemistry,2014,4(1):50-53.
