A promising strategy for trace analysis of hydrogen peroxide (H2O2) in natural water was established based on solid substrate room temperature phosphorimetry. The use of TiO2/SiO2 composite material as a phosphor for H2O2 detection was investigated. TiO2/SiO2 nanoparticle material was manufactured into a test kit for synchronous multilevel sampling test in the water sample reservoir. The proposed TiO2/SiO2 test kit displayed a wide linear response to H2O2 concentrations ranging from 1.0 × 10(-6) to 1.0 × 10(-1) M with a detection limit of 4.6 × 10(-7) M. When the concentration of other species was 100 times of 1.0 × 10(-4) M H2O2, the proposed test kit exhibited good selectivity toward the coexistence of 20 foreign ions. Satisfactory agreement between the proposed kit and spectrophotometric method was obtained, which demonstrated the possibility of its further development into a promising commercial phosphorescence sensor.