This paper describes the mineralogical studies of the solid products of autoclave oxidation. These products were obtained during autoclave pilot tests at a temperature of 225 oС and total pressure 3.25 МPa. Autoclave tests were carried out on the samples of sulfide gold-bearing concentrate of the Malomyr deposit. Mineralogical studies were provided using Mossbauer spectrometry, scanning electron microscope, X-ray fluorescence and X-ray diffraction analysis. It was found that the solid autoclave residues consist of basic ferric arsenate sulfate (Fe(AsO4)x(SO4)y(OH)z·wH2O), sodium jarosite (KFe3(SO4)2(OH)6), basic ferric sulfate (Fe(OH)SO4) and gangue minerals (muscovite, quartz, feldspars and others). The main relationships of the phase transformations in the autoclave oxidation process were described. Data obtained during these studies shows that some part of the gold may be associated with a secondary arsenic-containing phase formed in the autoclave oxidation process. This gold may be isolated from cyanidation solution and remain in the tailings. It was considered to subject the autoclave slurry to an additional treatment — Hot Cure process. This can minimize the loss of the precious metal during autoclave aftertreatment. As a result, a part of the secondary soluble phases (up to 10–50%) decomposes and dissolves. After that gold becomes accessible to the cyanide solution during sorption cyanidation. The increase in precious metal recovery is 2–5% for various samples.