Abstract：There are relatively few reports on the analysis of nickel and cobalt polymetallic ores due to the complexity of matrix and lack of standard sample.Nickel and cobalt polymetallic ore sample was prepared by fusion sample preparation method. The contents of main components (SiO2, Al2O3, TFe (expressed in the form of Fe2O3), CaO, MgO, K2O, Na2O, TiO2, P2O5 and MnO) and mineralization elements (Ni and Co) were determined by X-ray fluorescence spectrometry (XRF). Several influencing factors were studied, including the flux for fusion sample preparation, the dilution ratio between flux and sample, the oxidizer, the pre-oxidation temperature and time, fusion temperature and time, and the correction of matrix effect. Moreover, the index test of method was conducted. It was found that the sample could be well prepared under the following conditions: the Li2B4O7-LiBO2-LiF (m∶m∶m=4.5∶1∶0.4) was used as mixed flux; the LiNO3 was selected as oxidizer; the dilution ratio between flux and sample was 20∶1; the pre-oxidation temperature and time was 650℃and 4min; the fusion temperature and time was 1050℃ and 9min, respectively. The precision of sample was investigated.The relative standard deviations (RSD) of determination results of each component were between 0.49% and 6.2%. The standard substance of nickel-cobalt ore was determined according to the experimental method, and the found results were consistent with the certified values.
曾美云, 邹棣华, 李小丹, 杨小丽. X射线荧光光谱法测定以镍和钴为主的多金属矿中主次成分[J]. 冶金分析, 2018, 38(4): 51-56.
ZENG Mei-yun, ZOU Di-hua, LI Xiao-dan, YANG Xiao-li. Determination of major and minor components in nickel and cobalt polymetallic ore by X-ray fluorescence spectrometry. , 2018, 38(4): 51-56.
韩平学.EDTA直接滴定测定镍[J].环境科学与技术,2006,29(B08):42-43.HAN Ping-xue.Determination of nickel by EDTA direct titration method[J].Environmental Science and Technology,2006,29(B08):42-43.
[3]
李波,孙宝莲,周恺,等.丁二酮肟光度法测定红土镍矿中的镍[J].稀有金属材料与工程,2012,41(10):1867-1870.LI Bo,SUN Bao-lian,ZHOU Kai,et al.Determination of nickel content in laterite nickel ores by dimetylglyoxime spectrophotometry[J].Rare Metal Materilas and Engineering,2012,41(10):1867-1870.
[4]
于建忠,朱虹,孙丽丽.多波长分光光度法同时测定钴精矿中钴和镍[J].冶金分析,2006,26(2):35-37.YU Jian-zhong,ZHU Hong,SUN Li-li.Simultaneous determination of cobalt and nickel in cobalt concentrate by multi-wavelength spectrophotometry[J].Metallurgical Analysis,2006,26(2):35-37.
[5]
朱国忠,徐艳燕,庞燕.连续光源火焰原子吸收光谱法测定氧化镍中钴铜锌铁钙镁[J].冶金分析,2017,37(3):48-52.ZHU Guo-zhong,XU Yan-yan,PANG Yan.Determination of cobalt,copper,zinc,iron,calcium and magnesium in nickel oxide by continuum source flame atomic absorption spectrometry[J].Metallurgical Analysis,2017,37(3):48-52.
[6]
黎金盛,王成刚,张广文,等.原子吸收光谱法快速测定镍钴合金镀液中镍、钴的含量[J].广东化工,2016,43(18):164-165.LI Jin-sheng,WANG Cheng-gang,ZHANG Guang-wen,et al.Rapid determination of nickel and cobalt in nickel alloy plating solution by atomic absorption spectroscopy[J].Guangdong Chemical Industry,2016,43(18):164-165.
[7]
冯学珠,唐清华,张秀香,等.火焰原子吸收光谱法连续测定钴矿中Co,Ni和Cu[J].冶金分析,2003,23(3):36-37.FENG Xue-zhu,TANG Qing-hua,ZHANG Xiu-xiang,et al.Successive determination of trace Co,Ni and Cu in cobalt ore by flame atomic absorption spectrometry[J].Metallurgical Analysis,2003,23(3):36-37.
[8]
王国新,许玉宇,王慧,等.电感耦合等离子体发射光谱法测定红土镍矿中镍钴铜[J].岩矿测试,2011,30(5):572-575.WANG Guo-xin,XU Yu-yu,WANG Hui,et al.Determination of Ni,Co and Cu in laterite-nickel ores by inductively coupled plasma-atomic emission spectrometry[J].Rock and Mineral Analysis,2011,30(5):572-575.
[9]
荚江霞,陆军,陆尹.微波消解-电感耦合等离子体原子发射光谱法测定镍铁合金中7种元素[J].冶金分析,2016,36(5):58-63.JlA Jiang-xia,LU Jun,LU Yin.Determination of seven elements in nickel-iron alloy by microwave digcstion-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2016,36(5):58-63.
[10]
王艳君,蒋晓光,李卫刚,等.ICP-AES法测定红土镍矿中镍、钙、钛、锰、铜、钴、铬、锌与磷的含量[J].分析试验室,2012,31(9):50-53.WANG Yan-jun,JIANG Xiao-guang,LI Wei-gang,et al.Determination of Ni,Ca,Ti,Mn,Cu,Co,Cr,Zn and P in laterite-nickel ores by inductively coupled plasma-atomic emission spectrometry[J].Chinese Journal of Analysis Laboratory,2012,31(9):50-53.
[11]
李岩,董秀文,赵军峰,等.能量色散X荧光光谱法测定红土镍矿中镍等化学成分[J].分析科学学报,2014,30(2):191-196.LI Yan,DONG Xiu-wen,ZHAO Jun-feng,et al.Investigation of energy-dispersive X-ray fluorescence spectrometry for determination of chemical composition of lateritic nickel ores[J].Journal of Analytical Science,2014,30(2):191-196.
[12]
李国会,卜维,樊守忠.X-射线荧光光谱法测定硅酸盐中硫等20个主、次、痕量元素[J].光谱学与光谱分析,1994,14(1):105-110.LI Guo-hui,BU Wei,FAN Shou-zhong.Determination of twenty major,minor and trace elements in silicate by XRF spectrometry[J].Spectroscopy and Spectral Analysis,1994,14(1):105-110.
[13]
李小莉,吴良英,王力强,等.X射线荧光光谱法分析碳酸盐时两种制样方法的比较[J].理化检验:化学分册,2016,52(6):664-668.LI Xiao-li,WU Liang-ying,WANG Li-qiang,et al.Comparative study on the 2 methods for preparation of sample discs in XRFS analysis of carbonates[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2016,52(6):664-668.
[14]
李小莉.熔融制片-X射线荧光光谱法测定锰矿样品中主次量元素[J].岩矿测试,2007,26(3):238-240.LI Xiao-li.Determination of major and minor elements in manganese ores by X-ray fluorescence spectrometry with fusion sample preparation[J].Rock and Mineral Analysis,2007,26(3):238-240.
[15]
李红叶,许海娥,李小莉,等.熔融制片-X射线荧光光谱法测定磷矿石中主次量组分[J].岩矿测试,2009,28(4):379-381.LI Hong-ye,XU Hai-e,LI Xiao-li,et al.Determination of major and minor components in phosphate ores by X-ray fluorescence spectrometry with fused bead sample preparation[J].Rock and Mineral Analysis,2009,28(4):379-381.
[16]
杨小丽,李小丹,杨梅.X射线荧光光谱法测定以钨和钼为主的多金属矿中主次成分[J].冶金分析,2013,33(8):38-42.YANG Xiao-li,LI Xiao-dan,YANG Mei.Determination of major and minor components in tungsten and molybdenum polymetallic ore by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2013,33(8):38-42.
