By combining the offline static and dynamic laser light scattering (LLS) and gel permeation chromatography (GPC) results of a broadly distributed polymer sample, we were able to characterize a series of chiral binaphthyl-based polyarylenes and poly(aryleneethnylene)s in THF at 25 degrees C. For each of the samples, we obtained not only the weight-average molar mass M-w, the second virial coefficient A(2) and the z-average translational diffusion coefficient , but also two calibrations : V = A + Blog(M) and D = k(D) M-alpha D, where V, D, and M are the elution volume, the translational diffusion coefficient and the molar mass for monodisperse polymer chains, respectively, and A, B, k(D), and alpha(D) are four calibration constants. Using these calibrations, we estimated the molar mass distributions of these novel polymers. We showed that using polystyrene to calibrate the GPC columns could lead to a smaller M,. Our results indicate that all the polymers studied have a rigid chain conformation in THF at 25 degrees C and the introduction of the -NO2 groups into the monomer can greatly promote the polymer solubility in THF.