微波消解—电感耦合等离子体原子发射光谱法测定矿石样品中铌钽

来源期刊：冶金分析2010年第8期

论文作者：倪文山 张萍 姚明星 李贤珍

文章页码：50 - 53

关键词：微波消解； 酒石酸； 铌； 钽； 电感耦合等离子体原子发射光谱法

Key words：microwave digestion； tartaric acid； niobium； tantalum； inductively coupled plasma atomic emission spectrometry

摘    要：通过微波加热,氢氟酸溶解矿石样品,再以酒石酸溶液处理,使铌、钽完全进入溶液。以铌316.340{106}nm光谱线和钽268.517{125}nm光谱线为分析线,在选定的仪器参数下用电感耦合等离子体原子发射光谱法(ICP-AES)测定了溶液中的铌和钽。铌、钽原子发射光谱强度与ρ(Nb₂O₅)和ρ(Ta₂O₅)在0~6μg/mL范围内呈良好的线性关系,铌、钽的校准曲线相关系数r均为0.999 9,方法检出限分别为0.018μg/mL、0.051μg/mL。用于实际样品分析,加标回收率为97%~102%,铌和钽的相对标准偏差(n=6)分别为0.23%~0.86%和1.5%~2.3%;用于标准样品分析,测定值与认定值相符。

Abstract: The ore sample was digested with hydrofluoric acid by microwave heating,and then treated with tartaric acid solution to make niobium and tantalum in ore sample completely dissolve in solution.The niobium and tantalum in the prepared solution were determined by inductively coupled plasma atomic emission spectrometry(ICP-AES) under the selected instrumental parameters using Nb 316.340{106} nm and Ta 268.517{125} nm as analytical lines.The emission spectral intensity of niobium and tantalum showed good linear relationship with ρ(Nb₂O₅)and ρ(Ta₂O₅)in the range of 0-6 μg/mL.The correlation coefficients of calibration curve for niobium and tantalum were both 0.999 9.The detection limits for niobium and tantalum were 0.018 μg/mL and 0.051 μg/mL,respectively.The proposed method was applied to the determination of actual sample,giving the recovery rate of 97%-102% and the relative standard deviations(RSD,n=6) of 0.23%-0.86% for niobium and 1.5%-2.3% for tantalum.This method was applied to the analysis of standard sample,and the results were consistent with the certified values.