Recent experiments were performed in which return loss and insertion loss of waveguide test assemblies in the frequency range from 325 to 508 GHz were measured by use of a swept-frequency two-port vector network analyzer (VNA) test set. The experiments were part of a continuing effort to develop means of characterizing passive and active electronic components and systems operating at ever increasing frequencies. The waveguide test assemblies comprised WR-2.2 end sections collinear with WR-3.3 middle sections. The test set, assembled from commercially available components, included a 50-GHz VNA scatteringparameter test set and external signal synthesizers, augmented with recently developed frequency extenders, and further augmented with attenuators and amplifiers as needed to adjust radio-frequency and intermediate- frequency power levels between the aforementioned components.