Samples of a fly ash and a bottom ash, each before and after ignition, have been investigated by X-ray diffraction and Mössbauer spectroscopy in order to explain the observed negative loss of ignition (LOI). It is shown that the ashes after ignition contain more maghemite resulting from newly formed magnetite. Moreover, the fly ash which contained already magnetite exhibited an increase of hematite after ignition. Both oxidation processes can be responsible for a weight gain which compensates the loss due to the burning of the remaining carbon. The magnetite and the alpha-iron formed after ignition is originated by an unidentified compound represented by a Fe2+ doublet in the Mössbauer spectrum.