The aims of this article are therefore: (i) to use SPME in a static headspace mode to trap and concentrate volatile compounds present at high and low concentrations in two grades of natural rubber and that are released in the atmosphere under certain conditions, (ii) to identify these compounds by gas chromatography coupled with mass spectrometry, (iii) to determine their sensory impact and level using Gas Chromatography coupled with Olfactometry (GC-O), and (iv) to establish a correlation between volatile compounds emitted and curing process.