Nanocrystalline　GaSbO4　with　small　particle　size　and　large　BET　specific　area　was　successfully　prepared　via　a　facile　hydrothermal　method　from　Sb2O5.　The　influence　of　the　reaction　pH　on　the　formation　of　the　final　product　was　investigated.　The　obtained　sample　was　characterized　by　X-ray　diffraction　(XRD),　N-2-sorption　BET　surface　area,　UV-vis　diffuse　reflectance　spectroscopy　(DRS),　transmission　electron　microscopy　(TEM),　high-resolution　transmission　electron　microscopy　(HRTEM).　The　photocatalytic　activity　for　the　degradations　of　salicylic　acid　and　acetone　over　nanocrystalline　GaSbO4　under　UV　irradiations　was　for　the　first　time　revealed.　Based　on　the　electron　spin　resonance　(ESR)　result,　the　reactive　species　involved　in　the　photocatalytic　reaction　over　nanocrytalline　GaSbO4　are　determined　to　be　HO　center　dot　and　O-2(-center　dot).　The　photocatalytic　mechanism　of　GaSbO4　was　proposed.　(C)　2012　Elsevier　B.V.　All　rights　reserved.