Rapid Weightless Determination of the Atomic Ratio of Iron and Platinum in Ferrocene Derivatives by X-Ray Fluorescence Analysis

IF 0.9 4区 材料科学 Q4 MATERIALS SCIENCE, MULTIDISCIPLINARY
D. Kh. Kitaeva, O. L. Lependina, V. N. Talanova, I. V Karandi, A. G. Buyanovskaya
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引用次数: 0

Abstract

In the course of the synthesis of new metalloorganic compounds, there is a need for rapid monitoring of the elemental composition of the resulting substances at different stages of the process. In the microanalysis laboratory of the Nesmeyanov Institute of Organoelement Compounds, the metal content in the composition of substances determined using the XRF method is based on the external reference method with dilution of the sample with emulsion polystyrene. When preparing analyzed reflector samples, accurate weighing of the sample and diluent is required, since the dilution coefficient is required to calculate the content of elements. In cases where chemists involved in chemical synthesis are not interested in the exact elemental composition of the resulting compound, but in the atomic ratio of metals included in the organic matrix, when preparing analyzed samples, we propose to eliminate the lengthy weighing procedure and use approximately selected amounts of substances. The technique was tested in the analysis of a number of ferrocene derivatives containing platinum atoms, and a rapid weightless method for determining the atomic ratios of Fe and Pt in synthesis products using the FeKα and PtLα lines was proposed. The metal content in the emitter samples was determined using calibration equations. Simplification of the analysis procedure and the absence of weighing significantly speeds up the analyst’s work. The proposed method can be used as a preliminary criterion for the success of the synthesis of the expected product before its full elemental analysis is carried out.

通过 X 射线荧光分析法快速无重量测定二茂铁衍生物中铁和铂的原子比
摘要 在合成新金属有机化合物的过程中,需要在不同阶段快速监测所得物质的元素组成。在内斯梅亚诺夫有机元素化合物研究所的微量分析实验室中,使用 XRF 方法测定物质成分中的金属含量是基于外部参照法,用聚苯乙烯乳液稀释样品。在制备分析反射样品时,需要准确称量样品和稀释剂,因为计算元素含量需要稀释系数。如果参与化学合成的化学家对合成物的确切元素组成不感兴趣,但对有机基质中金属的原子比感兴趣,那么在制备分析样品时,我们建议省去冗长的称重程序,使用近似选定量的物质。我们在分析一些含有铂原子的二茂铁衍生物时对该技术进行了测试,并提出了一种利用 FeKα 和 PtLα 线测定合成产物中铁和铂原子比的快速失重法。发射器样品中的金属含量是通过校准方程确定的。分析程序的简化和无需称重大大加快了分析师的工作速度。在对预期产品进行全面的元素分析之前,建议的方法可用作合成成功与否的初步标准。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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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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