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In this work, it had been proposed a catalyst for carbonylation of methanol, which increases the efficiency of alternative GTL-processes without the stage of synthesis gas production. We chose the catalyst on the basis of NiCl2 and CuCl2 supported on highly porous carbon. It was selected because NiCl2 has a high methanol conversion index and CuCl2 possesses a significant selectivity towards methyl acetate. Such properties are necessary for carrying out the process of methanol carbonylation in the vapor phase without the addition of precursors. We investigated the physicochemical properties of the catalysts and worked out the method for quantitative spectrometric analysis of the elution of the active components from the catalyst surface during its operation.