README

This file contains all the raw data presented in "Electron Paramagnetic Resonance for the Detection of Electrochemically Generated Hydroxyl Radicals: Issues Associated with Electrochemical Oxidation of the Spin Trap" and has been downloaded from: http://wrap.warwick.ac.uk/168380

Archive Created: 17/07/2022
Archive Last Modified: 29/09/2022

As per the original article the data in this archive is provided under a creative commons CC BY-NC-ND license.

Corresponding Authors:
Julie V. Macpherson - julie.macpherson@warwick.ac.uk

The file has been divided into two sections:

1 - Main Article Data 
	Figure 1 - CVs recording the electrochemical response of 0.10 M HClO4 and 10 mM DMPO in 0.10 M HClO4 at 0.1 V s–1; Consecutive CVs of 30 mM DMPO in 0.30 M HClO4 at 0.1 V s–1. All data were recorded using a 1 mm diameter BDD disk electrode.
	Figure 2 - LSV data for DMPO oxidation over the DMPO concentration range of 1 to 30 mM in 0.10 M HClO4 at 0.5 V s–1, the current magnitude (recorded at Ep = +1.90 V vs SCE) with respect to the concentration over this range; LSV data for 1 mM DMPO in 0.10 M HClO4 at different scan rates.  All data were recorded using a 1 mm-diameter BDD disk electrode.
	Figure 3 - EPR spectra for 5 min electrolysis of 10 mM DMPO in 0.10 M HClO4 at constant potentials using a 1 × 7 cm double-sided rectangle BDD electrode with an immersion depth of ca. 5 cm;  Plot of double integrated intensity and concentration of DMPO-OH· extracted from EPR spectra vs the applied potential.
	Figure 4 - EPR spectra for 5 min electrolysis of different DMPO concentrations in 0.10 M HClO4 at a constant potential of +1.90 V vs SCE using a 7 by 1 cm double-sided BDD electrode with an immersion depth of ca. 5 cm; Plot of corresponding double integrated intensity and concentration of DMPO-OH·.
	Figure 5 - Simulated spectra of DMPO-CH(OH)CH3· and DMPO-OCH2CH3·; EPR spectra for 5 min electrolysis of 10 mM DMPO and 5 M ethanol in 0.10 M HClO4 at a range of constant potentials using a double-sided 1 × 7 cm rectangle BDD electrode with an immersion depth of ca. 5 cm; Plot of corresponding double integrated intensity, concentrations of DMPO-OH· and DMPO-CH(OH)CH3· extracted from EPR spectra vs the applied potential.
	Figure 6 - Oxidative windows for 10 mM MNP dimer; PBN, and; POBN in 0.10 M HClO4 at a scan rate of 0.1 V s–1 on a 1 mm BDD electrode.

2 - Supporting Information Data
	Figure S1 - CVs for the electrochemical response of 0.10 M HClO4 and 10 mM DMPO in 0.10 M HClO4 on 2 mm Pt disk and 3 mm disk GC electrode at 0.1 V s-1
	Figure S2 - White light interferometry of the surface of the 1 x 1.5 cm mechanically polished BDD electrode 5 min at +1.70 V vs SCE and 5 min at +2.50 V vs SCE and corresponding line profiles across the white light interferometry image
	Figure S3 - White light interferometry of the surface of the 1 x 7 cm BDD electrode (nucleation face) after deposition scratching to remove any film formed with corresponding line profiles across the white light interferometry image
	Figure S4 - CVs of 10 mM DMPO in 0.10 M HClO4 recorded on a 7 by 1 cm BDD electrode at 0.1 V s-1 before and after a 5 min electrolysis +1.90 V vs SCE electrolysis and after one of four cleaning steps. 
	Figure S5 - EPR spectra of 500 nM, 1 μM, 10 μM and 100 μM 4-hydroxy TEMPO.
	Figure S6 - DigiElch simulations of the oxidation of DMPO, assuming an ECsol process of varying solution rate constants alongside a reversible E only response.
	Figure S8 - EPR spectra for 5 min electrolysis of 10 mM DMPO in 0.10 M HClO4 atpotentials of +3.00 V, +3.50 V, +4.00 V, +4.50 V and +5.00 V vs SCE, using a 7 by 1 cm BDD electrode immersed to a depth of ca. 5 cm. (b) Double integrated intensity of DMPO-OH˙ as a function of potential. Values at the potentials of +0.90 V to +2.90 V vs SCE are taken fromFigure 3 (main text). New data points at +3.00, +3.50, +4.00, +4.50 and +5.00 V vs SCE are highlighted in red.
	Figure S9 - First scan CV of 0.10 M TBAB in ethanol on a 1 mm diameter disk BDD macroelectrode at 0.1 V s-1 vs SCE.