Abstract:The ferronickel smelting process materials such as laterite-nickel ore calcine, dust and electric furnace slag were pretreated by oxidization for the fusion sample preparation. The calibration curves for the X-ray fluorescence spectrometry (XRF) analysis were prepared using the certified reference materials of iron ore and converter slag and the self-made standard sample of laterite-nickel ore. The rapid and accurate determination of ten components (Ni, Fe, SiO2, MgO, CaO, P2O5, Al2O3, Cr2O3, MnO and Co) in ferronickel smelting process materials was realized. It was found that the mass fraction of reducing components was relative low when the sample (200-mesh, 74 μm) was oxidized in air at 900 ℃ for 45 min. Under the tested oxidization conditions, the mass fraction of elementary metals and residual carbon in laterite-nickel ore calcine, dust and electric furnace slag samples could be reduced below 0.1%, which met the requirements of platinum-gold alloy crucible in fusion sample preparation. The fusion results were good when the mixed lithium metaborate and lithium tetraborate was used as the flux, the dilution ratio was 10, and the sample was fused at 1 050 ℃ for 15 min. The matrix effect was corrected by the theoretical α coefficient method. The linear correlation coefficients of calibration curves of components were all higher than 0.999. The laterite-nickel ore and its calcine, dust and electric furnace slag were analyzed by the proposed method. The results of precision test showed that the relative standard deviations (RSD, n=9) was less than 5%. The determination results were corrected according to the loss on ignition to calculate the contents of components in sample. The found results were consistent with those obtained by chemical method.
施善林,郭阳,李东麟,王永海. 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,WANG Yong-hai. Determination of ten components in ferronickel smelting process materials by X-ray fluorescence spectrometry with fusion sample preparation. , 2015, 35(7): 54-59.
李艳军,于海臣,王德全,等. 红土镍矿资源现状及加工工艺综述[J]. 金属矿山, 2010(11):5-15. LI Yan-jun,YU Hai-chen, WANG De-quan,et al. The current status of laterite nickel ore resources and its processing technology[J]. Metal Mine, 2010(11):5-15.
[2]
褚宁,蒋晓光,李卫刚,等. 过硫酸铵-丁二酮肟光度法测定红土镍矿中的镍[J]. 岩矿测试, 2012, 31(3):479-483. CHU Ning, JIANG Xiao-guang, LI Wei-gang, et al. Determination of Ni in nickel laterite ores by ammonium persulfate dimetylglyoxime spectrophotometry[J]. Rock and Mineral Analysis, 2012, 31(3):479-483.
[3]
司银奎. 磷锑钼蓝光度法测定红土镍矿中磷量[J]. 山东国土资源, 2012, 28(12): 52-54. SI Yin-kui. Determing phosporus content in lateritenickel ore used of antimonphosph molybdate blue spectriphotometry method[J]. Land and Resources in Shandong Province, 2012, 28(12): 52-54.
[4]
阮桂色. 重铬酸钾滴定法测定红土镍矿中全铁含量[J]. 矿冶, 2011, 20(4): 113-115. RUAN Gui-se. Determination of total iron in laterite nickel ore by potassium dichromate titration[J]. Mining and Metallurgy, 2011, 20(4): 113-115.
[5]
孙宝莲, 张俊芳, 李波, 等. 氟硅酸钾滴定法测定红土镍矿中二氧化硅[J]. 冶金分析, 2012, 32(4):65-69. SUN Bao-lian, ZHANG Jun-fang, LI Bo,et al.Determination of silicon dioxide in laterite nickel ores by potassium fluosilicate titrimetric methed[J]. Metallurgical Analysis, 2012, 32(4):65-69.
[6]
王虹,冯宇新,苏明跃,等. 火焰原子吸收光谱法测定红土镍矿中铬[J]. 冶金分析, 2007, 27(9): 54-56. WANG Hong, FENG Yu-xin, SU Ming-yue, et al.Determination of chromium in laterite-nickel ore by flame atomic absorption spectrometry[J]. Metallurgical Analysis, 2007, 27(9): 54-56.
[7]
石晶晶, 赵明理, 马旭利. 火焰原子吸收光谱法测定红土镍矿中钴的含量[J]. 煤炭与化工, 2014, 37(3): 68-70. SHI Jing-jing, ZHAO Ming-li, MA Xu-li. Determination of cobalt in laterite nickel ore by flame atomic absorption spectrometry[J]. Coal and Chemical Industry, 2014, 37(3): 68-70.
[8]
高亮. 碱熔—电感耦合等离子体原子发射光谱法测定红土镍矿中硅钙镁铝锰钛铬镍钴[J]. 冶金分析, 2013, 33(2): 51-54. GAO Liang. Determination of silicon, calcium, magnesium, aluminium, manganese,titanium, chromium, nickel and cobalt in laterite nickel ore by alkali fusion-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis, 2013, 33(2): 51-54.
[9]
刘久苗. 电感耦合等离子体发射光谱法测定红土镍矿中镍钴镁铝铁[J]. 岩矿测试, 2013,32(6):893-896. LIU Jiu-miao. Determination of Ni, Co, Mg, Al and Fe in laterite nickel ore by inductively coupled plasma-atomic emission spectrometry[J]. Rock and Mineral Analysis, 2013,32(6):893-896.
[10]
何飞顶, 李华昌, 冯先进. 电感耦合等离子体原子发射光谱法(ICP-AES)测定红土镍矿中的Cd、Co、Cu、Mg、Mn、Ni、Pb、Zn、Ca 9种元素[J]. 中国无机分析化学, 2011, 1(2): 39-41. HE Fei-ding, LI Hua-chang, FENG Xian-jin. Simultaneous determination of Cd, Co, Cu, Mg,Mn, Ni, Pb, Zn and Ca in laterite nickel ore by inductively coupled plasma atomic emission spectrometry (ICP-AES) [J]. Chinese Journal of Inorganic Analytical Chemistry, 2011, 1(2): 39-41.
[11]
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]. 分析实验室, 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.
[12]
张丽微, 徐玉蓉, 张微, 等. ICP-AES法同时测定红土型镍矿中镍、钴、铁、镁研究[J]. 云南地质, 2010, 29(3):346-350. ZHANG Li-wei, XU Yu-rong, ZHANG Wei, et al.A study on the simultaneous testing of Ni, Co, Fe, Mg in laterite type Ni deposit with ICP-AES method[J]. Yunnan Geology, 2010, 29(3):346-350.
[13]
彭南兰, 李小莉, 华磊, 等. X射线荧光光谱法测定红土镍矿中多种元素[J]. 中国无机分析化学, 2012, 2(1):47-50. PENG Nan-lan, LI Xiao-li, HUA Lei, et al.Determination of multiple elements in nickel laterite ore by XRF spectrometry[J]. Chinese Journal of Inorganic Analytical Chemistry, 2012, 2(1):47-50.
[14]
张建波,林力,王谦,等. X-射线荧光光谱法同时测定镍红土矿中主次成分[J]. 冶金分析, 2008, 28(1):15-19. ZHANG Jian-bo, LIN Li, WANG Qian, et al. Determination of major and minor components in nickel laterite ores by X-ray fluorescence spectrometry[J].Metallurgical Analysis, 2008, 28(1):15-19.
[15]
林忠,李卫刚,褚宁,等. 熔融制样-波长色散X射线荧光光谱法测定红土镍矿中铁、镍、硅、铝、镁、钙、钛、锰、铜和磷[J]. 分析仪器,2012(4):53-57. LIN Zhong, LI Wei-gang, CHU Ning, et al. Determination of iron, nickel, silicon, aluminum, magnesium, calcium, titanium, manganese,copper and phosphorus in laterite nickel ores by wavelength dispersive X-ray fluorescence spectrometry with fusion sample preparation[J]. Analytical Instrumentation,2012(4):53-57.