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

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.