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Monoclinic BiVO 4 powders have been synthesized by means of homogeneous coprecipitation, followed by calcination at different temperatures. The effect of the calcination temperature on the changes in the physicochemical parameters has been evaluated. It has been deduced that the crystallite size and band gap are responsible for water oxidation. The effect of calcination temperatures on the variations, such as lone pair distortions on Bi 3+ and changes in the V−O bond length in the local structure of BiVO 4 , has also been confirmed from the changes in the intensities and the shift of the peak position in the Raman analysis.