The XRD patterns were directly recorded on Pt support for the film obtained after 10 successive electrodepositions, using a Philips X’Pert Pro diffractometer with a Cu Kα Bay 36-7620 (λ = 0.15415 nm) in the 2°–70° 2θ range, in steps of 0.0334°, with a counting time per step of 650 s.
The chemical compositions of LDH films, obtained by electrodeposition, were investigated by SEM/EDS analysis, using an EVO 50 Series Instrument (LEO ZEISS) equipped with an INCA Energy 350 EDS microanalysis system and INCA SmartMap for imaging the spatial variation of the elements in a sample (Oxford Instruments Analytical). The accelerating voltage was 25 or 10 kV, the beam current 1.5 nA and the spectra collection time 100 s. FEG-SEM images were acquired with a Zeiss Supra 55 FEG- VP operating at 3 keV.
The apparatus for the flow injection analysis (FIA) consisted of a sperm HPLC pump (LabFlow 1000), a six-way injection valve equipped with a 50 μL loop, an electrochemical detector (Metrohm, VA 641 Model) interfaced with a personal computer. The electrochemical detector was constituted of 1 μL wall-jet cell (Metrohm, 656 Model) in the three-electrode configuration (Ag/AgCl/ KCl 3.0 M as the reference, 2 mm diameter Au as the counter, and the working electrode) and a potentiostat for the amperometric measurements. In the HPLC configuration, the METROSEPCARB1 column (Metrohm) was inserted between the injection system and the detector. The eluent was a 0.1 M NaOH solution prepared starting from a 50 % (w/w) solution, previously-decarbonated, and, DD water. The flow rate was set at 1 mL?min−1.