ICP-OES法测定钒的光谱干扰研究

doi:10.3964/j.issn.1000-0593(2020)07-2283-06

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摘要：钒是重要的稀缺资源和重要战略金属，在自然界中往往以次要矿物相形式与多种复杂金属共伴生存在。采用PE Optima 7300V，在仪器入射功率1 300 W、观测高度15 mm、雾化气流量0.65 L·min^-1条件下研究了常见钒共伴生元素对电感耦合等离子体原子发射光谱（ICP-OES）法测定钒含量时谱线选择的影响，结果表明，Al，Mo，Ti，Cr，Ni对V的六条推荐谱线测定均会产生显著影响，且V测定相对误差与对应元素/V（质量比）基本呈线性关系。其中，微量Al的存在即会导致V 309.31 nm谱线产生剧烈变化，其次是Mo，当Mo/V＞0.89，Mo/V＞5.98，将分别导致290.88和292.402 nm谱线出现±5%以上的相对误差，且Mo存在条件下V 270.093 nm谱线亦不稳定；当Ti/V＞5.98，Cr/V＞10.33，Cr/V＞13.6及Ni/V＞13.56时，311.07，290.88，270.093和310.23 nm谱线测量结果相对误差分别达±5%以上。综合以上影响及谱线稳定性，当含钒原料中无Ti时，可采用较稳定的311.07 nm谱线，含Ti时可采用310.23 nm谱线。在光谱仪最佳工作条件下，利用该方法测定了钒钛磁铁矿、石煤、含钒催化剂等典型含钒原料中的钒含量，其检出限在310.23 nm为0.054 mg·L^-1，311.07 nm为0.194 mg·L^-1，加标回收率为93.4%~103.1%，相对标准偏差0.59%。与硫酸亚铁铵滴定法进行对比实验，结果基本吻合，相对误差在±4.34%以下。该方法简便快捷，精密度和准确度高，适用于含钒原料中钒含量测定的科研及生产。

关键词：电感耦合等离子体发射光谱；钒；钒钛磁铁矿；石煤

Abstract：Vanadium is an important scarce resource and strategic metal, and often coexists with a variety of complex metals in the form of secondary mineral phases in nature. The effect of co-exist elements on the selection of spectral lines in the determination of vanadium with Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-OES) was studied in this article. The selected PE Optima 7300V instrument was operated under the conditions of incident power 1 300 W, observation height 15 mm and atomization gas flow rate 0.65 L·min^-1. The results show that Al, Mo, Ti, Cr and Ni have significant effects on the determination of vanadium under six recommended spectral lines, and the relationship between the relative error of measurement results and the mass ratio of the corresponding element to V waslinear. The presence of trace Al leads to drastic changes when V 309.31 nm spectral lines was adopted. The relative error of V 290.88 and V 292.402 nm spectral lines were increased to more than ±5% as the Mo/V mass ratio increased to 0.89 and 5.98, separately. The Mo measurement results were unstable when V 270.093 nm spectral lines was adopted, but nothing regular. The relative error of V 311.07, 290.88, 270.093 and 310.23 nm spectral lines were increased to more than ±5% as the Ti/V mass ratio increased to 5.98, Cr/V mass ratio increased to 10.33, 13.6, and Ni/V mass ratio increased to 13.56, respectively. Considering the above effects and spectral stability, V 311.07 nm spectral lines can be adopted when there has no titanium in vanadium-containing raw materials, and V 310.23 nm can be used when there has titanium contained. Under the optimum analytical conditions of the spectrometer, the method was used for the determination of vanadium in typical vanadium-containing raw materials such as vanadium-titanium magnetite, stone coal and vanadium-containing catalysts with the detection limit of 0.054 mg·L^-1 at 310.23 nm, 0.194 mg·L^-1 at 311.07 nm, recoveries between 93.4% and 103.1%, and relative standard deviation of 0.59%. By comparing with the results of ammonium ferrous sulfate titration method, the results were basically consistent with the relative error of less than ±4.34%. In conclusion, the method was simple and efficient, with high precision and accuracy, which can be used for research and routine production of vanadium determination in raw materials containing vanadium.

Key words：ICP-OES; Vanadium; Vanadium titanomagnetite; Stone coal

收稿日期: 2019-06-19 修订日期: 2019-10-23

中图分类号:

TF841.2

基金资助: 河北省自然科学基金项目（E2019318015，B2019318014），河北省省级科技计划项目(19044011Z)，国家自然科学基金面上项目（51774261）资助

通讯作者: 杜浩 E-mail: hdu@ipe.ac.cn

作者简介: 王少娜，女，1979年生，中国科学院过程工程研究所副研究员 e-mail: shnwang@ipe.ac.cn

引用本文:

王少娜，靳星，刘彪，赵备备，李兰杰，李明，杜浩，张懿. ICP-OES法测定钒的光谱干扰研究[J]. 光谱学与光谱分析, 2020, 40(07): 2283-2288.
WANG Shao-na, JIN Xing, LIU Biao, ZHAO Bei-bei, LI Lan-jie, LI Ming, DU Hao, ZHANG Yi. Study on Spectral Interference in the Determination of Vanadium by ICP-OES. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2020, 40(07): 2283-2288.

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https://www.gpxygpfx.com/CN/10.3964/j.issn.1000-0593(2020)07-2283-06 或 https://www.gpxygpfx.com/CN/Y2020/V40/I07/2283