1：Experimental Design and Method Selection:

The study employed a heterogeneous photocatalytic ozonation process combining ozone with TiO2/CDs photocatalysts under simulated sunlight irradiation to degrade CIP. The design rationale was to enhance the degradation efficiency through synergistic effects between photocatalysis and ozonation, focusing on reactive species generation and electron transfer mechanisms. Theoretical models included pseudo-first-order kinetics for degradation rate analysis and mechanisms involving reactive species (?OH, O2?—, h+, etc.).

2：Sample Selection and Data Sources:

CIP aqueous solutions (10 ppm initial concentration) were prepared using ultrapure water. Secondary wastewater effluent from a Guangzhou wastewater treatment plant and Pearl River water were used as real water matrices for feasibility evaluation. Samples were collected at given time intervals during experiments.

3：List of Experimental Equipment and Materials:

Equipment included an XPA-7 rotary photochemical reactor, ozone generator (Quanju Technology), 350 W xenon lamp with 290 nm cut-off filters, HPLC (Waters e2695), HRAM LC-MS/MS (Q Exactive Orbitrap mass spectrometer with Ultimate 3000RSLC HPLC), XRD (Bruker-D8-Advanced), TEM (JEM-2100HR), SEM (JSM-6700), XPS (Thermo VG ESCALAB 250), FT-IR spectrophotometer (Nicolet 6700), and Milli-Q apparatus. Materials included CIP (TCI Reagent Co. Ltd.), TiO2 (commercial), CDs (synthesized from citric acid and urea), and various chemicals (e.g., NBD-Cl, tert-Butyl alcohol, benzoquinone) from suppliers like Aladdin and Taitan.

4：Experimental Procedures and Operational Workflow:

Photocatalysts (TiO2/CDs with varying CDs content) were prepared via hydrothermal-calcination method. For degradation experiments, 50 mg photocatalyst was added to 50 mL CIP solution in a quartz tube, stirred in dark for 30 min for adsorption equilibrium, then illuminated with xenon lamp while ozone was bubbled (flow rate 15 mL/min). Samples were withdrawn at intervals, quenched with Na2S2O3, filtered, and analyzed by HPLC. Control experiments included single photocatalysis, ozonation, and photolysis.

5：Data Analysis Methods:

CIP concentration was determined by HPLC with calibration curves (0.02-5.00 μg/mL). Degradation kinetics were fitted to pseudo-first-order model. Reactive species were quantified using quenching experiments with specific scavengers (e.g., TBA for ?OH, BQ for O2?—). Intermediates were identified by HRAM LC-MS/MS with a Hypersil GOLD C18 column. Characterization data (XRD, TEM, SEM, XPS, zeta potential) were analyzed to assess photocatalyst properties.