Poly(phenylacetylene)s are a family of dynamic helical polymers where the elongation and the helical sense of the double helix can be easily tuned in a controlled way using the proper external stimuli. Since there is a direct relationship between the secondary structure of the polymer and its potential applications, the structural elucidation of these polymers is nowadays a challenge in polymer chemistry.

These polymers are characterised using the combination of different techniques such as CD, UV-Vis, Raman, DSC… However, the interpretation of the data is time consuming and in occasions difficult, madding necessary appeal to AFM. Due these obstacles, we focus on the light-driven cyclization of PPAs as a fast and easy-going alternative approach to decipher the configuration of the polyene backbone.

Several parameters should be considered to achieve acceptable values of reproducibility and repeatability on this technique. On this work, we evaluate the influence of the relation between volume/concentration of sample and photoabsorption on PPAs when monitoring results by circular dichroism, resulting in and easy and controlled way to tune the light-driven characterization of PPAs.