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Real-time monitoring of the corona-poling process that is used to create a bulk second-order nonlinear-optical susceptibility was accomplished by observing electrochromic shifts and intensity decreases of charge-transfer absorption bands in both dye-doped and covalently functionalized polymer films. By measuring small changes in the refractive-index anisotropy, the optical waveguiding technique was demonstrated to be a sensitive measure of the poling-induced order and its relaxation. The guest–host systems were formed from the dyes N,N-dimethylaminonitrostilbene, N,N-dimethylindoaniline (Phenol Blue), and 4-(N-(2-hydroxyethyl)-N-ethyl)-amino-4^′-nitroazobenzene (Disperse Red 1), each dissolved in a poly(methyl methacrylate) matrix. The covalently functionalized polymers contained pendant para-nitroaniline (PNA) moieties. The first, poly(N-(4-nitrophenyl)allylamine), was formed from a poly …