The photocatalytic activity of (Ga
1-xZn
x)(N
1-xO
x), a solid solution of GaN and ZnO, for H
2 and O
2 evolutionin the presence of methanol and silver nitrate as sacrificial reagents under visible light (
> 420 nm) isinvestigated in detail. (Ga
1-xZn
x)(N
1-xO
x) evolves H
2 from an aqueous methanol solution when loaded withnanoparticulate Rh
2-yCr
yO
3 as a cocatalyst, and evolves O
2 from an aqueous silver nitrate solution without acocatalyst. Structural analyses indicate that the H
2 evolution activity is strongly dependent on the crystallinityand composition of the catalyst, while the rate of O
2 evolution is proportionally related to the specific surfacearea. The activity for H
2 evolution from methanol solution is of the same order as for overall water splitting,but is an order of magnitude lower than that for O
2 evolution from silver nitrate solution. The results ofphotocatalytic reactions and photoelectrochemical measurements suggest that the rate-determining step foroverall water splitting using (Ga
1-xZn
x)(N
1-xO
x) is the H
2 evolution process.