The objectives of this study are the painting technique and the materials used by Master Athayde in six paintings attributed to him. The Brazilian painter and gilder lived and worked in the region of Ouro Preto, Minas Gerais, Brazil, during the second half of the 18th-beginning of the 19th century. Along with Aleijadinho, Master Athayde was the most important artist of the Rococo period in Minas Gerais. Analytical methods used include physical and chemical tests of solubility, of coloration, microchemistry, x-ray diffraction, as well as the stratigraphic analysis of thin sections. Results indicate that the painter used mainly oil-based binders (a protein/oil emulsion); the presence of white and brown preparations is an important element for the characterization of the artist's working methods.