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Sonication in a 1:1 mixture (volume ratio) of water and concentrated H(2)O(2) (30%) is a soft method for particle size reduction of phyllosilicate minerals like vermiculites. Repeated sonication causes a particle size reduction to about 70 nm for the Santa Olalla and to 45 nm for the Ojén-vermiculite. In this context the question arises whether the strong oxidising effect of the hydrogen peroxide affects the oxidation state of the iron in the vermiculites. Therefore, the Fe(3+)/Fe(total) ratio before and after sonication was determined by means of Mössbauer spectroscopy. Whereas this ratio was found to remain almost constant in the Santa Olalla vermiculite, it increased from 0.79 to 0.85 in case of the Ojén sample. In the latter case, the oxidation is accompanied by a decrease of the layer charge. Surprisingly, sonication in pure water leads to a decrease of the Fe(3+)/Fe(total) ratio in the case of the Ojén-vermiculite, i.e., to an increase of the Fe(2+) fraction to roughly twice the value before sonication. Again the Fe(3+)/Fe(total) ratio of the Santa Olalla vermiculite remains unchanged. The surface area S(BET) of the reduced Ojén-vermiculite amounts to 50 m(2)/g, which is close to the value obtained in the presence of hydrogen peroxide. The results presented should be taken as a warning that particle size reduction by sonication may be accompanied by a change of the redox state and the layer charge of the material.