Abrasive stripping voltammetry was applied to the investigation of the reductive dissolution of some iron(III) oxides and hydroxy-oxides, particularly goethite (α-FeOOH), in acid media. The electrode reaction directly involves the solid phase, and the reaction pathway depends on the phase composition and particle shape. This can be used for a qualitative and quantitative characterization of goethite. The results of a quantitative analysis of a mixture of goethite (α-FeOOH) and lepidocrocite (γ-FeOOH) are compared with those of IR and Moessbauer spectroscopic examination. The effects of the particle appearance (shape, crystal intergrowth) on the results of the voltammetric and chronoamperometric measurements are discussed.Direct analysis of powdered solids by electrochemical methods complements nicely conventional phase analysis methods such as powder X-ray analysis, IR spectroscopy and, for iron compounds, Moessbauer spectroscopy. In fact, each of the methods places some specific requirements on the phase crystallinity and particle size and the procedures are instrumentally demanding and time consuming and so that the possibility of resorting to alternative analytical methods is very appealing.A method which does not place very high demands on instrumentation, is well suited to routine phase analysis, and moreover, can be used on a micro scale, has been suggested by Scholz and coworkers 1,2 . The method is based on voltammetric measurement with a carbon electrode to which analyte particles are fixed by rubbing against sample, the authors named the technique "abrasive stripping voltammetry" (henceforth AbrSV). The method is useful for the analysis and characterization of metal alloys 1 , minerals 2 , various inorganic binary mixtures 3 , pigments 4 , for the study of high-temperature superconductors 5 , for the calculation of thermodynamic constants of low soluble compounds 6,7 , etc. (a survey of applications has been presented in ref. 8 ). Since electrode processes can generally involve higher order electrochemical reactions, diffusion, adsorption, and chemical reactions of the substance in the surroundings of the electrode, the overall reaction pathway is very complex 8 and interpretation of the voltammograms requires prior understanding of the conversion mechanism of the substance on the electrode and/or in its surroundings.
950Grygar, Subrt, Bohacek: