电感耦合等离子体原子发射光谱(ICP-AES)法测定石煤钒矿石中钒、铁、钛的含量

Determination of Vanadium,Iron and Titanium Contents in Stone Coal Vanadium Ore by Inductively Coupled Plasma Atomic Emission Spectrometry

研究一种快速准确测定石煤钒矿石中钒、铁、钛含量的方法对石煤钒矿检测行业的发展和石煤钒矿资源的开发利用、综合评价具有重要的意义。试样经过氧化钠在650℃完全熔融后保持1~3 min,取出冷却,热水浸提,盐酸酸化,定容稀释,选择V 292.402 nm、Fe 259.940 nm、Ti 334.941 nm为分析谱线,利用电感耦合等离子体原子发射光谱法(ICP-AES),建立了石煤钒矿石中同时测定钒、铁、钛含量的方法。优化了钒、铁、钛元素的分析谱线和背景校正模式,采用全程序样品空白稀释配制的校准曲线消除盐度钠基影响;研究了坩埚、熔剂种类、直接碱熔与灼烧-碱熔前处理方式、酸度效应的影响。结果表明:方法检出限为0.009%~0.019%,定量限为0.027%~0.057%;铁、钛、钒3种元素浓度在0.10~30.0μg/mL时,校准曲线线性回归方程的相关系数均大于0.9999;采用国家一级标准物质(GBW07876、GBW07877、GBW07878)进行验证,相对标准偏差(RSD,n=12)为0.49%~0.87%,且测定值与标准值吻合。方法具有快速简便、精密度好、准确度高、同时测定钒、铁、钛等优点,满足石煤钒矿石化学分析检测需求,且可为石煤钒矿化学分析标准方法的建立提供技术支撑。

It is of great significance to study a fast and accurate method for the determination of vanadium,iron and titanium contents in stone coal vanadium ore for the development of the stone coal vanadium ore detection industry and exploitation,comprehensive evaluation of stone coal and vanadium resources.In the study,the samples were completely melted with sodium peroxide at 650℃and kept for 1-3 min.Then the samples were removed to cool,extracted with hot water,acidified with hydrochloric acid,and diluted to a certain volume.The content of vanadium,iron and titanium in stone coal vanadium ore was simultaneously determined by inductively coupled plasma atomic emission spectrometry using Fe 259.940 nm,292.402 nm,Ti 334.941 nm as analytical spectral lines.The analytical spectrum lines and background correction modes of vanadium,iron and titanium elements were optimized in the experiment,and the effects of salinity and sodium base were eliminated by using the calibration curve of blank dilution configuration of the whole program sample.The effects of crucible,flux type,direct alkali melting and calcing-alkali melting pretreatment methods,and acidity effect were systematically studied.The results showed that the limits of detection and quantification were 0.009%-0.019%and 0.027%-0.057%,respectively.When the concentrations of Fe,Ti and vanadium were 0.10-30.0μg/mL,the correlation coefficients of calibration curves linear regression equations were greater than 0.9999.The relative standard deviation(RSD%,n=12)were 0.49%-0.87%and the measured values were basically consistent with the standard values,which were verified by the national standard material(GBW07876,GBW07877 and GBW07878).The method has many advantages,such as fast and simple,good precision,high accuracy,simultaneous determination of vanadium,iron and titanium,which can meets the needs of chemical analysis and testing of stone coal vanadium ore,and can provide technical support for the establishment of standard methods for chemical analysis of stone coal vanadium ore.