Sublimation from lactose and sucrose solutions has been monitored by temperature measurement, visual observation, heat flux sensing and manometric measurements. Estimates of energy transfer rates to the subliming mass made from visual observations and heat flux measurements are in broad agreement, demonstrating for the first time that heat flux sensors can be used to monitor the progress of lyophilization in individual vials with low sample volumes. Furthermore, it is shown that under identical lyophilization conditions the initial rate of drying for lactose solutions is low with little water sublimation for up to 150 minutes, which contrasts markedly with the much faster initial rate of drying for sucrose solutions. Measurement of the initial heat flux between shelf and vial indicated a lower flux to a 10% lactose solution than to a 10% sucrose solution.