The composition profile across a lamellar phase obtained in a multicomponent blend of saturated poly(butadiene) and poly(isobutylene), stabilized by a saturated poly(butadiene) copolymer serving as a surfactant, was quantified by transmission electron microscopy (TEM) and self-consistent field theory (SCFT). The liquidlike nature of this system at room temperature makes traditional staining methods for the enhancement of contrast ineffective. Instead, we take advantage of the large inelastic scattering cross-section of soft materials to generate contrast in zero-loss TEM images. Independent spatially resolved thickness measurements enable quantification of electron scattering. This enabled a comparison between the TEM data and predictions based on SCFT without any adjustable parameters. © 2008 American Chemical Society.