With the purpose of establishing of an opportunity of photometric determination of gallium(III), complexoformation with 2,3,4-threeoxiphenilazo-5′-sulphonaphtalene in the presence of decamethoxin in acetate environments- ammoniac buffers, sulfuric and azotic acids has been studies. Spectrophotometric characteristics and constants of stability of a complex with relation of components Ga(III): R: Dek=1:2:1 which has the maximal yield at pH=4, 0.5 M H2SO4 and 0.1 M HNO3 have been calculated. It is positioned that a complex formative in the environment hydrogen nitrate characterized by the greatest (Δλ=117 nm) both the constant of stability (lgβ=15.29±0.17) and the least sensitivity (ε=6250). The technique of photometric determination of gallium in all researched environments has been developed and established, that reactions in milieu of acetate- ammoniac buffers (pH=4) and 0.1 M HNO3 possess sharp selectivity.