Volatile fatty acids (C2-C7) analysis in wool scouring water and lanolin is presented. These substances are of major interest as malodorous compounds in urban and industrial wastewaters. In this work, they have been analysed in wool scouring water by headspace solid-phase microextraction followed by gas chromatography negative chemical ionisation mass spectrometry. Most of the volatile fatty acids have been identified at microg g(-1) levels. In addition, since lanolin is a major impurity of raw wool, volatile fatty acid patterns of wool scouring water and lanolin have been compared in order to establish the origin of these compounds in the wastewater. Finally, the efficiency of the deodorization step, mandatory to obtain commercial lanolin, has been assessed taking into account the decrease in volatile fatty acid content from the raw wool to the lanolin.