Oxidation of organic matter with H2O2 produced substantial amounts of NH3 which was then fixed by vermiculite, causing partial or complete collapse and converting the mineral to a mica-like product. The collapse of the mineral was indicated by shifts in the 001 spacing from 1.476 to 1.030 nm and the appearance of a well-defined band at 1430 cm−1 in the IR spectrum, indicative of the presence of NH4+ in the interlayer positions of the clay. Our data suggest that: (a) the transformation of vermiculite to mica during H2O2 oxidation may result in underestimation of the vermiculite content of soils by XRD, and (b) the wide occurrence of mixed-layer minerals in soils may in part have resulted from the fixation of NH3 liberated from the microbial mineralization of organically bound N. Key words: Ammonia, X-ray diffraction, IR spectrophotometry, mixed-layer minerals, H2O2 pretreatment