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This study evaluates naproxen (NP) degradation efficiency by ozonation using nickel oxide films (<inline-formula><math display="inline"><semantics><mrow><mi>N</mi><mi>i</mi><msub><mi>O</mi><mrow><mo>(</mo><mi>F</mi><mo>)</mo></mrow></msub></mrow></semantics></math></inline-formula>) as a catalyst. The <i>NiO</i> films were synthesized by chemical vapor deposition and characterized by X-ray diffraction, scanning electron microscopy, atomic force microscopy and X-ray photoelectron spectroscopy. NP degradation was conducted for 5 min using 10 films of <inline-formula><math display="inline"><semantics><mrow><mi>N</mi><mi>i</mi><msub><mi>O</mi><mrow><mo>(</mo><mi>F</mi><mo>)</mo></mrow></msub></mrow></semantics></math></inline-formula> comparing against ozonation using 100 mg/L <inline-formula><math display="inline"><semantics><mrow><mi>N</mi><mi>i</mi><mi>O</mi></mrow></semantics></math></inline-formula> powder in suspension (<inline-formula><math display="inline"><semantics><mrow><mi>N</mi><mi>i</mi><msub><mi>O</mi><mrow><mo>(</mo><mi>S</mi><mo>)</mo></mrow></msub></mrow></semantics></math></inline-formula>) and conventional ozonation (<inline-formula><math display="inline"><semantics><msub><mi>O</mi><mn>3</mn></msub></semantics></math></inline-formula>-conv). Total organic carbon analysis demonstrated a mineralization degree of 12% with <inline-formula><math display="inline"><semantics><msub><mi>O</mi><mn>3</mn></msub></semantics></math></inline-formula>-conv, 35% with <inline-formula><math display="inline"><semantics><mrow><mi>N</mi><mi>i</mi><mi>O</mi></mrow></semantics></math></inline-formula> as powder and 22% with <inline-formula><math display="inline"><semantics><mrow><mi>N</mi><mi>i</mi><msub><mi>O</mi><mrow><mo>(</mo><mi>F</mi><mo>)</mo></mrow></msub></mrow></semantics></math></inline-formula> after 60 min of reaction. The films of <inline-formula><math display="inline"><semantics><mrow><mi>N</mi><mi>i</mi><msub><mi>O</mi><mrow><mo>(</mo><mi>F</mi><mo>)</mo></mrow></msub></mrow></semantics></math></inline-formula> were sequentially used 4 times in ozonation demonstrating the stability of the synthesized material, as well as its properties as a catalyst for ozonation. A proposed modeling strategy using robust parametric identification techniques allows the comparison of NP decomposition pseudo-monomolecular reaction rates.