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Nowadays the actual problem of geochemistry is a deep and complex processing of mineral raw materials. Data on the quantitative content of precious and rare metals in various types of ores and rocks are necessary. It stimulates the development and improvement of chemical analytical methods for determination of these elements. Such methods are not applicable without sample preparation stage. Preparation of samples for analysis is the decomposition and preconcentration of rare and precious metals from matrix of mineral raw materials. The sample preparation schemes of platinum, palladium and rhenium are described in this paper.