The autoradiography technique complex was realized for micromapping and determination of gold and uranium mineral particles in black shale and sulfide ores of gold deposit. Alpha radiography, fission track radiography and beta radiography were used for the gold and uranium distribution study in the natural and synthetic minerals and ores. New data on local spatial distribution of uranium and gold for both elements (gold-uranium deposits) and gold-bearing deposit of quartz-gold-sulfide-formation have been obtained.