Although the bubble-floc agglomerate floated and formed the float layer on the surface of the water in the DAF process, after inducing in the thickening tank a part of the bubble-floc agglomerate come up again to the surface and the other is settled at the bottom of the tank. The bubble-floc agglomerate divided into two group as the scum on the surface and the sludge of the bottom gives rise to operational troubles for the thickening process. In order to find out the cause of break-up and the effective thickening method for sludge from the DAF process, the composition of the bubble-floc agglomerate was investigated and a series of flotation experiments carried out. There was no difference of composition between the scum on the surface and the sludge of the bottom in the thickening tank. The coagulation was not effective to improve the trouble that the bubble-floc agglomerate divided into the scum and the sludge. It was estimated that for the bubble-floc agglomerate of thickening tank the trouble was caused by not the change or the difference of chemical composition but whether the bubble-floc agglomerate hold bubbles. Furthermore, for the effective thickening of sludge from the DAF process, it is required an additional flotation applied the AS ratio depending upon the solid concentration of sludge as the operation parameter.