Analysis of Cerium-Substituted Yttrium Iron Garnets Using Inductively Coupled Plasma Atomic Emission Spectrometry with Preliminary Decomposition in a Microwave System

IF 0.9 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY Inorganic Materials Pub Date : 2024-07-19 DOI:10.1134/s0020168524700122
N. A. Korotkova, K. V. Petrova, V. B. Baranovskaya
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Abstract

A method for analyzing iron garnets of the composition Y3–xCexFe5–yGayO12, where x = 0.4–0.5 and y = 2.4–2.6, using inductively coupled plasma atomic emission spectroscopy (ICP-AES) with preliminary decomposition of the sample in microwave system is described. During the investigation, conditions for microwave decomposition of samples are studied and selected—the composition of acid mixtures (HCl/HNO3) and modes of microwave heating (holding time and temperature) providing complete dissolution of the samples. Conditions for ICP-AES analysis of cerium-doped yttrium iron garnets and the effect of matrix components (Y, Ce, Fe, and Ga) on the determination of impurity elements are studied. The operating parameters of the spectrometer (high-frequency generator power and argon spray flow rate) making it possible to reduce the matrix effect when determining Na, Mg, Al, Si, P, K, Ca, Sc, Cr, Mn, Co, Ni, Cu, Zn, Se, Cd, Sn, Te, La, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu, and Pb impurities in yttrium iron garnets using ICP-AES are selected in order to minimize the matrix effect. ICP-AES studies are carried out in axial and radial modes for impurity elements and in radial modes for matrix elements. The limits of quantification (LOQs) of most analytes are in the range from n × 10–5 to n × 10–4 wt %. The accuracy is confirmed by the “spike–recovery” method, as well as by the analysis of samples with certified element contents. The standard deviation is in the range from 1 to 5% depending on the selected plasma viewing mode and the elements being detected. The developed method makes it possible to determine macro- and microcomponents in yttrium iron garnets in a wide range of concentrations with a high accuracy.

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利用电感耦合等离子体原子发射光谱法分析铈取代钇铁石榴石并在微波系统中进行初步分解
摘要 描述了使用电感耦合等离子体原子发射光谱(ICP-AES)分析成分为 Y3-xCexFe5-yGayO12(其中 x = 0.4-0.5 和 y = 2.4-2.6)的铁榴石并在微波系统中对样品进行初步分解的方法。在研究过程中,对微波分解样品的条件进行了研究和选择--酸混合物(HCl/HNO3)的成分和微波加热的模式(保持时间和温度)可使样品完全溶解。研究了 ICP-AES 分析掺铈钇铁石榴石的条件以及基体成分(Y、Ce、Fe 和 Ga)对杂质元素测定的影响。在测定 Na、Mg、Al、Si、P、K、Ca、Sc、在使用 ICP-AES 测定钇铁石榴石中的 Na、Mg、Al、Si、P、K、Ca、Sc、Cr、Mn、Co、Ni、Cu、Zn、Se、Cd、Sn、Te、La、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu 和 Pb 杂质时,为了将基体效应降至最低,选择了 ICP-AES。对杂质元素的 ICP-AES 研究采用轴向和径向模式,对基体元素的 ICP-AES 研究采用径向模式。大多数分析物的定量限 (LOQ) 在 n × 10-5 到 n × 10-4 wt % 之间。通过 "尖峰回收 "法以及对经认证元素含量的样品进行分析,可以确认其准确性。标准偏差在 1%至 5%之间,具体取决于所选的等离子观察模式和检测的元素。采用所开发的方法,可以高精度地测定钇铁石榴石中各种浓度范围的宏观和微观成分。
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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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