Poly(styrene/divinylbenzene) has found use only recently as a high-performance reversed-phase material. There has been relatively little detailed investigation of the properties of poly(styrene/divinylbenzene) in gradient separation of peptides. It was recently found that both the selectivity and peak capacity of poly(styrene/divinylbenzene) are comparable to those of alkyl bonded phases in tryptic mapping. The present work demonstrates that increasing the temperature and flow rate of the mobile phase at constant column inlet pressure increases the efficiency of a poly(styrene/divinylbenzene) column, permitting rapid separations.