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The physical properties of cyclic polymers can be perturbed by the presence of architectural impurities, even in trace amounts. As a result, it is important to develop techniques for quantifying and improving the purity of cyclic polymer samples. The zwitterionic ring-expansion polymerization (ZREP) of glycidyl phenyl ether (GPE) with B(C₆F₅)₃ is a convenient, one-step method to generate cyclic polyethers in large amounts. However, the obtained cyclic samples are inherently contaminated by architectural impurities, which in this study are detected, identified, quantified, and successfully removed by a “click-scavenging” approach. The analytical techniques employed included matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI–TOF MS), quantitative Fourier transform infrared spectroscopy (FTIR), and gel permeation chromatography/multiangle light scattering (GPC–MALS). The end …