This study investigated the impact of commonly used treatment chemicals on the morphology and molecular structure of microfibers (MFs) and microplastic films (MPFs) to determine whether significant changes could occur during wastewater treatment. MFs and MPFs were exposed to sodium hypochlorite (NaOCl), hydrogen peroxide (H2O2), calcium hydroxide (Ca(OH)2, pH 11), sodium hydroxide (NaOH, pH11), and hydrochloric acid (HCl, pH 3) at typical doses and exposure times used at wastewater treatment plants. Scanning electron microscopy (SEM) analysis and attenuated total reflectance-Fourier-transform infrared (ATR-FTIR) were used to examine any morphological or chemical changes after the treatment. Morphological changes were observed in the form of cracks, and increased roughness was revealed in the SEM and 3-D surface images. The results showed that MFs were more resistant to surface degradation than MPFs. Moreover, intensity peaks of ATR-FTIR revealed some partial dislodgement of the bonds in both MFs and MPFs after chemical treatment, but the overall polymer structure remained intact. The changes that occur on the surface of MFs and MPFs during chemical treatment can impact their fate, removal, and transportation behavior both at the treatment plant and after discharge to the environment.