We performed a detailed deconvolution analysis of ATR-FTIR peaks of a common diacetylene, 10,12-tricosadiynoic acid (TRCDA) during the polymerization and the blue-to-red transition. Based on the analysis and the solvent dependence on the IR signals, we found that the triple peak from CC stretching mode that has been previously suspected as a consequence of Fermi resonance is rather associated with the macromolecular assembly of TRCDA. Besides these CC triple peaks, we found that the background in the region increased during the UV exposure due to the CC signals from polymers. In addition, the anisotropic compression during polymerization was also detected, which supports the proposed interpretation of X-ray data reported previously. These results are the benefits from the deconvolution analysis.