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The degradation of poly(phenylacetylene), a typical autoxidatively degradable polymer of substituted acetylene, is shown to take place inside the SEC (size exclusion chromatography) columns during the polymer analysis carried out with eluent (THF) not protected from air. Three types of experimental evidence are given based on the comparison of results of SEC analyses carried out: (i) with the eluent kept under air or argon atmosphere; (ii) with different flow rates of the eluent; and (iii) with and without the interruption of the analysis for a few hours. Other degradable polymers of substituted acetylene are mentioned and recommendations for their SEC analyses are given.

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