开发用于分析铁矿石原料的 ICP-AES 方法

IF 0.9 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY
I. I. Chernikova, A. A. Potokina, O. V. Farafonova, T. N. Ermolaeva
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引用次数: 0

摘要

摘要 利用电感耦合等离子体原子发射光谱法(ICP-AES),在分析高压釜中进行微波样品制备,开发了一种测定铁矿石原料(即球团矿、铁矿团块、吸尘和废渣中的矿渣成分)中Fetot、SiO2、P、V2O5、TiO2、Cr2O3、Ni、Cu和Zn的方法。提出了使样品成分完全溶解的酸混合物成分,并选择了微波分解参数,其中不包括高压釜减压和形成挥发性化合物的样品元素损失。所开发的在封闭高压釜中进行微波样品制备的方法可以在 45 分钟内用最少的酸(17 立方厘米)分解铁矿石样品。确定了微波样品制备后采用 ICP-AES 法测定铁矿石样品中归一化元素的条件:优化了光谱仪的运行参数,选择了每种测定元素的分析线,避免了光谱重叠,并通过实验证明了使用镉作为内标物的效率。文中给出了校准相关方程和可确定的含量范围。在分析铁矿石时使用镉作为内标,测定 Cr2O3 时,标准偏差值从 0.17 降至 0.04;测定 Fe 时,标准偏差值从 0.02 降至 0.004;测定 SiO2 时,标准偏差值从 0.03 降至 0.002;测定 TiO2 时,标准偏差值从 0.015 降至 0.008;测定 V2O5 时,标准偏差值从 0.17 降至 0.02。使用与被分析材料成分相似的有证标准样品 (CRS) 对所开发方法测定标准元素的正确性进行了评估。根据开发的方法测定标准元素的结果与使用 GOST 批准的分析方法获得的数据进行了比较,然后根据 RMG 76-2014 的建议进行了检查。与 GOST 批准的技术相比,所开发的 ICP-AES 技术的特点是测定浓度的线性范围更广,因此可以测定以前无法控制的铁矿石原料中的成分。
本文章由计算机程序翻译,如有差异,请以英文原文为准。

Development of ICP-AES Method for Analysis of Iron Ore Raw Materials

Development of ICP-AES Method for Analysis of Iron Ore Raw Materials

Abstract

A method for the determination of Fetot, SiO2, P, V2O5, TiO2, Cr2O3, Ni, Cu, and Zn in iron ore raw materials (i.e., pellets, iron ore agglomerate, aspiration dust and slag component of scrap) by the method of atomic emission spectrometry with inductively coupled plasma (ICP-AES) has been developed using microwave sample preparation in analytical autoclaves. The composition of the acid mixture for the complete dissolution of the sample component was proposed, and the parameters of microwave decomposition, excluding the depressurization of the autoclave and the loss of sample elements which form volatile compounds, were selected. The developed method of microwave sample preparation in closed autoclaves made it possible to decompose iron ore samples using the minimum amount of acid (17 cm3) in 45 min. Conditions for the determination of normalized elements in iron ore samples by the ICP-AES method after microwave sample preparation were determined: the operating parameters of the spectrometer were optimized, the analytical lines of each determined element free from spectral overlaps were selected, and the efficiency of using cadmium as an internal standard was experimentally proved. The equations for calibration dependences and the ranges of determinable contents are presented. When using cadmium as an internal standard in the analysis of iron ore, a decrease in the value of the standard deviation from 0.17 to 0.04 is observed when determining Cr2O3; from 0.02 to 0.004 when determining Fe; from 0.03 to 0.002 when determining SiO2; from 0.015 to 0.008 when determining TiO2; and from 0.17 to 0.02 when determining V2O5. The correctness of the determination of the standardized elements by the developed method is evaluated using certified reference samples (CRS) similar in composition to the analyzed material. The results of determining the standardized elements according to the developed methodology were compared with the data obtained using GOST-approved methods of analysis and then checked in accordance with the recommendations of RMG 76-2014. The developed ICP-AES technique is characterized by a wider linear range of the determined concentrations than that in GOST-approved techniques, thus providing determination of the components in iron ore raw materials that could not be controlled before.

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来源期刊
Inorganic Materials
Inorganic Materials 工程技术-材料科学:综合
CiteScore
1.40
自引率
25.00%
发文量
80
审稿时长
3-6 weeks
期刊介绍: Inorganic Materials is a journal that publishes reviews and original articles devoted to chemistry, physics, and applications of various inorganic materials including high-purity substances and materials. The journal discusses phase equilibria, including P–T–X diagrams, and the fundamentals of inorganic materials science, which determines preparatory conditions for compounds of various compositions with specified deviations from stoichiometry. Inorganic Materials is a multidisciplinary journal covering all classes of inorganic materials. The journal welcomes manuscripts from all countries in the English or Russian language.
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