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A highly sensitive fluorescence system of the europium gadolinium thenoyltrifluoroacetone tri(salicyloylaminoethyl)amine cetylpyridium bromide polyvinyl alcohol was established and the luminescence mechanism was studied. The excitation and emission wavelengths were 362.5 nm and 613.1 nm respectively. Optimum concentrations of gadolinium, thenoyltrifluoroacetone (TTA), and tri(salicyloylaminoethyl) amine (TSA) were found at room temperature. The effects of surfactants cetylpyridium bromide (CPB) and polyvinyl alcohol (PVA) were also described. The fluorescence intensity varies linearly with the concentration of europium (Ⅲ) in the range 5.00×10 -11 ～6.00×10 -8 mol/L and 1.00×10 -7 ～9.21×10 -7 mol/L. The detection limit is down to 9.02×10 -12 mol/L. The standard addition method was used for the determination of europium in high purity yttrium oxide with satisfactory results.