The crystallochemical features of Co in Co-substituted goethite solid-solutions prepared by two different procedures have been studied using infrared, X-ray photoelectron and electron energy loss spectroscopies. It was found that the path followed for the synthesis of Co-substituted goethite determines the oxidation state of Co in the goethite structure. Thus, in the solid-solution prepared by precipitation with Na2CO3 of an Fe(II) aqueous solution containing Co(II) cations, followed by the aerial oxidation of the precipitate, the Co cations were found to be divalent, whereas trivalent Co was incorporated into the goethite obtained by ageing a solution containing Fe(III) and Co(II) cations precipitated by the addition of KOH. This different behavior is explained by the higher pH of goethite formation in the latter case, which favors the oxidation of the Co(II) cations.

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