The working of loop seal is one of the least understood aspects of a circulating fluidized bed boiler although this component is critical to the operation of such boilers. The present work is an experimental study of the flow of solids; through the recycle chamber of a loop seal in a circulating fluidized bed (CFB). The effect of different parameters on the velocity of solid overflow through the recycle chamber is investigated. The sharp-crested weir theory of free surface water flow was used to analyze the solid flow through the loop seal. The analysis gives a good indication of the validity of the above theory for solids overflow over a weir. The results show that the solid flow rate increases with increase in bed height above the weir and the particle size had no effect on the value of the weir coefficient.