We have used dynamic oscillatory measurements to locate the temperatur
e of the microphase separation transition (T-MST) for a series of near
ly monodisperse styrene-isoprene diblock (SI) and triblock (SIS) copol
ymers, all containing 13 wt % styrene and ranging in molecular weight
from 48K to 149K. The microphase-separated morphology in all cases is
a disordered (liquidlike) arrangement of polystyrene spheres in a poly
isoprene matrix, as determined by small-angle X-ray scattering. Values
of T-MST were obtained from isochronal plots of the storage modulus v
ersus temperature. The marked change in slope at the MST demonstrates
that even materials with a disordered microdomain structure can experi
ence significant property changes when the MST is traversed. The diblo
ck and triblock T-MST values are consistent with a single chi(T) relat
ion, indicating that targe-scale polymer architecture has little effec
t on chi.