EBE and BEB triblock copolymers were prepared and characterized. Microphase separation in the melt state was studied, and the results combined with those for EB and BEB copolymers reported previously. The microphase separation temperature (MST) was determined from the temperature dependence of SAXS. There was a large difference in MST between the diblock and triblock copolymers as expected from theory. The Flory-Huggins parameter (chi) was independent of block architecture for all three series provided that the E block lengths in the EBE copolymers exceeded 65.