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The influence of the calcination process on the physicochemical properties and catalytic behavior of the Co/Mg/La catalysts for ammonia synthesis has been investigated. The catalysts were prepared using the different thermal pre-treatment methods prior to the activation, i.e., drying and calcination, and the respective activities for ammonia synthesis were assessed. It was found out that changing from air calcination prior to activation to direct activation of the co-precipitated species led to the different catalytic performances. The most favorable catalytic performance was achieved with Co/Mg/La prepared by calcination in air. Detailed characterization methods, employing e.g., XRPD, H2-TPD, N2-TPD, CO2-TPD, SEM, and TEM, showed that the superior catalytic behavior of this catalyst was attributed to its strong basicity and favorable adsorption properties toward hydrogen and nitrogen. [ABSTRACT FROM AUTHOR]