A biocatalyst was prepared by immobilization of Saccharomyces cerevisiae strain AXAZ-1 on delignified cellulosic material (DCM). Repeated batch fermentations were conducted using these biocatalysts and free cells, separately, at temperatures of 20, 15, and 10 degrees C. Solid phase microextraction (SPME) was used in monitoring the formation of volatile alcohols, acetate esters, and ethyl esters of fatty acids. The kinetics of volatile production were similar for free and immobilized cells. In all cases immobilized cells showed a better rate of volatile production, which was directly connected to sugar consumption. The main difference observed was in propanol production, which increased with temperature decrease for the immobilized cells, whereas it remained constant for the free ones. In the case of immobilized cells significant amounts of esters were also produced. It is well-known that esters contribute to the fruity aroma of wine. It was also established that SPME is a very sensitive, accurate, and reliable technique and can be used without any reservation in the characterization of volatile constituents of wine.