Analysis of cerium-substituted yttrium iron garnets by inductively coupled plasma atomic emission spectrometry with preliminary microwave decomposition

N. A. Korotkova, K. V. Petrova, V. B. Baranovskaya
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Abstract

An analytical procedure for inductively coupled plasma atomic emission (ICP-AES) analysis of iron garnets of the composition Y3 – xCexFe5 – yGayO12, where x = 0.4 – 0.5 and y = 2.4 – 2.6 with preliminary microwave decomposition of the sample is described. The compositions of acid mixtures (HCl/HNO3), as well as modes of microwave heating (holding time and temperature), providing complete dissolution of the samples are proposed. In addition to optimized sample preparation, conditions for ICP-AES analysis of cerium-doped yttrium iron garnets were studied. The effect of matrix components (Y, Ce, Fe, Ga) on the determination of doping elements was revealed and studied. The operating parameters of the spectrometer (ICP power and nebulizer flow rate) have been substantiated, which make it possible to reduce the matrix effect of Fe, Ga, Y, Ce on the elements 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, Pb in iron yttrium garnets by the ICP-AES. ICP-AES measurements were performed in the axial and radial mode for trace elements and in the radial mode for matrix elements. The limits of quantification (LOQs) of most elements ranged within n × 10–5 – n × 10–4 wt.%. The accuracy is confirmed by the spike recovery test. The relative standard deviation is in the range of 1 – 5% depending on the selected plasma view mode and the analyzed analytes. 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和初步微波分解分析铈代钇铁石榴石
本文介绍了对成分为 Y3 - xCexFe5 - yGayO12(其中 x = 0.4 - 0.5 和 y = 2.4 - 2.6)的铁榴石进行电感耦合等离子体原子发射(ICP-AES)分析的分析程序,并对样品进行了初步的微波分解。提出了可使样品完全溶解的酸混合物(HCl/HNO3)的成分以及微波加热模式(保温时间和温度)。除了优化样品制备,还研究了掺铈钇铁石榴石的 ICP-AES 分析条件。揭示并研究了基体成分(Y、Ce、Fe、Ga)对掺杂元素测定的影响。对光谱仪的操作参数(ICP 功率和雾化器流速)进行了论证,从而降低了 Fe、Ga、Y、Ce 对 Na、Mg、Na 元素的影响、铈对 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、Pb 等元素的影响。痕量元素的 ICP-AES 测量采用轴向和径向模式,基体元素的 ICP-AES 测量采用径向模式。大多数元素的定量限(LOQ)在 n × 10-5 - n × 10-4 wt.%之间。通过尖峰回收测试确认了其准确性。相对标准偏差在 1 - 5% 之间,具体取决于所选的血浆观察模式和所分析的分析物。所开发的方法可以在较宽的浓度范围内准确测定钇铁石榴石中的宏观和微观成分。
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