The influence of pyrite pre-oxidation in alkaline solutions on gold recovery by cyanidation from Twin Creek refractory gold ore in which pyrite was identified as the major sulfide mineral has been investigated with the aid of electrochemical measurements, leaching experiments, and direct analysis of reaction products for selected residues. It was found that gold recovery by cyanidation in bottle roll experiments mainly depended on the extent of pyrite pre-oxidation. The rate of pyrite oxidation in alkaline solutions measured by electrochemical measurements, including chronoamperometry and linear sweep voltammetry, increased with an increase in pH, potential, and temperature. All alkaline reagents used for the electrochemical measurements, NaOH, NH 4OH, Na 2CO 3 and Ca(OH) 2, showed a similar effect on pyrite oxidation kinetics. However, the results of alkaline pre-oxidation for pyrite of the Twin Creek refractory gold ore suggested that NaOH and Na 2CO 3/Ca(OH) 2 were superior to Ca(OH) 2. Without pre-oxidation, cyanide leachable gold was found to be only 20% which could be increased to 70% under appropriate pre-oxidation conditions. At the same time, cyanide consumption decreased from 2.5 kg/t ore to 1.5 kg/t ore. Selected residues after pre-oxidation and cyanidation were examined by X-ray diffraction. Backscattered electron images of pyrite particles in these residues were taken. The reaction products at the surface of pyrite particles were found to be iron-, silicon-, and calcium-bearing compounds with variable amounts of sulfur as determined by X-ray energy dispersion analysis. Additionally, some mineral fines, such as aluminum and/or potassium-bearing minerals, were found to be present at the partially oxidized pyrite surface.