The molecular weight dependence of lamellar domain spacing of styrene—2-vinylpyridine diblock copolymers in bulk was measured by means of small-angle X-ray scattering and compared with theories of microphase-separated structure. It was found that the lamellar domain spacing-molecular weight relationship of the diblock copolymer in bulk is given by D = O.337M0·64 over the molecular weight range from 38K to 740K. The experimental result is in good agreement with the theories on the basis of Gaussian chain statistics in a confined space, particularly the theory of Helfand-Wasserman. © 1990, American Chemical Society. All rights reserved.