Monoaromatic hydrocarbons (MAHs) monitoring is of environmental interest since these chemical pollutants are omnipresent. While waiting for robust sensors able to detect hydrocarbons at very low levels, the present study shows how each compound from pure BTEX mixtures can be identified fast and quantified thanks to Raman spectrometry and data processing based on the SIMPLISMA algorithm. A preprocessing module has been created to remove background contributions and a postprocessing program has been added to achieve matching and calibration. A wide range of BTEX concentrations and relative proportions has been investigated in order to determine the limitations of the processing. Output results achieved an accuracy of up to 95%. This method could be extended to other important pollutants such as polyaromatic hydrocarbons (PAHs) and chlorinated hydrocarbon derivatives.