1：Experimental Design and Method Selection:

The study involved the synthesis of HNA/OS-LRH composites via ion exchange reactions using a hydrothermal process. The rationale was to intercalate HNA and OS into LRH layers to study luminescence properties and ion recognition. Theoretical models included energy transfer mechanisms and intramolecular charge transfer inhibition.

2：Sample Selection and Data Sources:

Samples included HNAxOS1?x-LTbH and HNAyOS1?y-LYH composites with varying HNA/OS ratios. Precursors were NO3-LTbH and NO3-LYH prepared hydrothermally. Data sources included synthesized composites and metal ion solutions for recognition experiments.

3：List of Experimental Equipment and Materials:

Equipment: PANalytical X’Pert PRO MPD diffractometer (XRD), Nicolet-360 Fourier transform infrared spectrometer (FT-IR), Hitachi S-4800 FESEM, Hitachi S-8010 and Bruker XFlash 6160 for EDS, Cary Eclipse spectrofluorimeter, Edinburgh FS5 spectrofluorimeter, FLS980 spectrofluorimeter, Edinburgh FLS-980 with integrating sphere, Jarrel-ASH ICAP-9000 ICP-AES, Elementar vario EL elemental analyzer. Materials: HNA, OS, NaOH, formamide, metal nitrate salts, deionized water, KBr pellets.

4：Experimental Procedures and Operational Workflow:

Preparation of NO3-LRH precursors via hydrothermal reaction. Intercalation of HNA/OS into LRH by ion exchange at 70°C for 24 h, followed by filtration, washing, and drying. Delamination in formamide with mechanical shaking. Recognition experiments by mixing composite colloid with metal ion solutions and measuring luminescence. Characterization using XRD, FT-IR, SEM, EDS, luminescence spectra, lifetimes, quantum yields, ICP-AES, and elemental analysis.

5：Data Analysis Methods:

XRD patterns analyzed for basal spacing. FT-IR spectra for functional groups. Luminescence spectra for emission wavelengths and intensities. Fluorescence lifetimes fitted with single-exponential equation. Quantum yields measured with integrating sphere. Detection limit calculated using 3σ/S method.