This study investigates the determination of the critical micelle concentration (CMC) and cloud point of synthesized surfactants, which are key parameters governing their physicochemical behavior in aqueous solutions. Surfactants, due to their amphiphilic nature, exhibit the ability to reduce surface tension and form micelles beyond a certain concentration threshold. The CMC was determined using surface tension measurements via the Du Noüy ring method, while the cloud point was established through controlled heating of surfactant solutions. Experimental results showed a decrease in surface tension with increasing concentration until a plateau region corresponding to micelle formation was reached. The synthesized surfactants demonstrated varying CMC and cloud point values, indicating differences in molecular structure and hydrophilic–lipophilic balance (HLB). Among the samples, PAVMS exhibited the highest surface activity, while PAVKM showed favorable characteristics for applications at lower temperatures due to its low CMC and cloud point. The findings highlight the importance of molecular structure in surfactant performance and provide a basis for selecting efficient and environmentally sustainable surfactants for industrial applications.