It is well-known that entrainment of particles into the froth is a key factor in the selectivity and performance of the flotation process, especially for fine particle recovery. Since flotation is a continuous process, in this work, the effects of operating parameters on the entrainment of ash materials in a sample coal flotation is investigated from a time-sequence viewpoint. The effects of the pulp solid content, collector concentration, frother concentration, impeller speed, and particle size on the entrainment factor and water recovery at different flotation times are evaluated using a D-optimal response surface experimental design. The experimental work carried out shows that some parameters, especially particle size and pulp density, can yield completely different responses from those reported in the literature. The observed unusual behaviours can be attributed to the entrainment mechanisms and verified by the experimental results. It is also shown that the dominant entrainment mechanism can be varied by time. In addition, the statistical analyses of the experimental design show that the effects of some parameters change during time from the initial to the final stages of the flotation process. The results obtained indicate that the particle size and pulp density are the most important parameters influencing the entrainment rate and water recovery. The effects of the collector and frother concentrations are less on the entrainment and water recovery. In addition, the interaction between the solid percentage and particle size is the only significant mixed effect.