New compounds based on tungstate were synthesized as environmentally friendly inorganic pigments. The pigments have been prepared by the solid state reaction. This work is focused on mixed d-block metal and neodymium(III) tungstate. The optimum conditions for synthesis of intermediate products MWO4 (M = Ni, Zn, Mn), Nd2WO6 and final products MNd2W2O10 were determined by TG/DTA analysis of starting materials mixtures. The thermal stability of MNd2W2O10 (M = Ni, Zn, Mn) was studied by heat microscopy with automatic image analysis. This value is at interval from 1,085 °C for ZnNd2W2O10 to 1,158 °C for MnNd2W2O10. Subsequent research was focused on the influence of d-block metals tungstates on the colour properties of the MNd2W2O10 pigments. All samples were found in interesting colour hues that were obtained for Mn ochre-yellow, for Ni brown and for Zn light violet. The effect of milling of final pigments in planetary mill on colour properties and particle size distribution was evaluated.