Determination of thirty-nine major and minor elements in ilmenite by inductively coupled plasma mass spectrometry with high pressure closed digestion
CHENG Yi, WANG Lin*, ZHANG Fang, LIU Jun, CHEN Haofeng, ZHANG Fan
Henan Province Rock & Mineral Testing Centre, Key Laboratory of Precious Metals Analysis and Exploration Technology Ministry of Land and Resources,Zhengzhou 450012, China
摘要 准确测定钛铁矿中主次元素对提高钛铁矿的选钛技术及有益元素的综合回收具有指导意义。钛铁矿难溶易水解,一般很难实现一次分解多元素同时测定。采用3 mL HF-1 mL HNO3-0.5 mL H2SO4于180 ℃高压密闭消解10 h,用5 mL逆王水180 ℃高压密闭方式溶解盐类5 h,在线引入Rh、Re混合内标,采用标准模式测定Li、Be、Sc、Ti、V、Cr、Mn、Co、Ni、Cu、Zn、Ga、Rb、Sr、Y、Mo、Cd、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、W、Pb、U,动能歧视模式测定Fe、Zr、Nb、La、Ce、Hf、Ta,对于受质谱干扰严重的V、Ni、Cd、Eu、Gd、Tb,通过数学校正方程在线进行校正,建立了电感耦合等离子体质谱法(ICP-MS)测定钛铁矿中39种主次元素的方法。方法校准曲线的相关系数均不小于0.999 6,检出限为0.002～2.4 μg/g,将其应用于钛铁矿成分分析标准物质分析,结果的相对误差(RE)为－10.0%～13.0%,相对标准偏差(RSD,n=12)均不大于3.5%;对主量元素及缺少认定值的元素进行加标回收试验,回收率为96%~104%。采用实验方法对钛铁矿样品进行分析,测得结果的相对标准偏差(RSD,n=12)均不大于4.1%。
Abstract：The accurate determination of major and minor elements in ilmenite had guiding significance to improve the beneficiation technology of ilmenite and the comprehensive recovery of beneficial elements. Ilmenite sample was hardly dissolved and easily hydrolyzed, so it was difficult to realize the simultaneous determination of multiple elements. The sample was digested with 3 mL of HF, 1 mL of HNO3 and 0.5 mL of H2SO4 at 180 ℃ for 10 h with high pressure pressure closed digestion. Then the salts were dissolved with 5 mL of reverse aqua regia at 180 ℃ for 5 h. The mixed internal standard of Rh and Re was introduced on line. Li, Be, Sc, Ti, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, Rb, Sr, Y, Mo, Cd, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, W, Pb and U were determined at standard mode (STD), while Fe, Zr, Nb, La, Ce, Hf and Ta were determined at kinetic energy discrimination (KED) mode. For the elements with serious mass spectrometry interference such as V, Ni, Cd, Eu, Gd and Tb, the online correction by mathematical equation was adopted. Consequently, a determination method of 39 major and minor elements in ilmenite by inductively coupled plasma mass spectrometry (ICP-MS) was established. The correlation coefficients of calibration curves of method were all not less than 0.999 6. The limits of detection were between 0.002 μg/g and 2.4 μg/g. The proposed method was applied to analysis of certified reference materials of ilmenite for composition analysis. The relative errors (RE) of results were between -10.0% and 13.0%. The relative standard deviations (RSD, n=12) were not more than 3.5%. The standard recovery tests of major elements and the elements in lack of certified values were conducted. The recoveries were between 96% and 104%. The ilmenite samples were analyzed according to the experimental method, and the RSDs (n=12) of results were not more than 4.1%.
程祎, 王琳, 张芳, 刘军, 陈浩凤, 张帆. 高压密闭消解-电感耦合等离子体质谱法测定钛铁矿中39种主次元素[J]. 冶金分析, 2021, 41(9): 24-33.
CHENG Yi, WANG Lin, ZHANG Fang, LIU Jun, CHEN Haofeng, ZHANG Fan. Determination of thirty-nine major and minor elements in ilmenite by inductively coupled plasma mass spectrometry with high pressure closed digestion. , 2021, 41(9): 24-33.
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