Abstract
Mn(iii)CyDTA [(trans-cyclohexane-1,2-diamine-N,N,N′,N′-tetraacetato) manganate(iii)] was generated electrochemically from Mn(ii)CyDTA (6–54 mm) in 0.1 m NaHCO3 at pH 9.0 and 10.5, respectively, 25 °C, for two CyDTA/Mn molar ratios (1/1 and 2/1). A divided batch electrochemical reactor was employed with anode current densities from 2.6 to 102 A m−2. Separate cyclic voltammetry experiments of Mn(iii)CyDTA in alkaline media showed a prepeak behaviour, indicating the adsorption of Mn(ii) species. The visible anodic deposit, formed during the electrosynthesis of Mn(iii)CyDTA at pH 10.5 and 1/1 CyDTA/Mn molar ratio on stainless steel and PbO2/Pb, reduces the current efficiency for Mn(iii). For a Mn(ii) concentration of 18 mm and at 13 A m−2, the graphite and platinized titanium anodes gave a current efficiency for Mn(iii) of 78% and 66%, respectively, without a visible deposit. A 2/1 CyDTA/Mn molar ratio, avoided a visible anodic deposit formation, but gave lower current efficiencies for Mn(iii) than in the case of a 1/1 ligand to metal ratio. The electrosynthesis of Mn(iii)CyDTA is recommended for routine preparation of the complex and is also suitable for in situ electrochemically mediated oxidations in alkaline media (up to pH 11).
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