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The analysis of cleaning solutions is difficult, especially if a chemical reaction occurs in the mixed solution. Such chemical reactions lead to real‐time changes in the vibrations of the molecules due to changes in the binding forces. Thus, techniques for analyzing mixed solutions are required to determine the processes that occur during the cleaning process. A real‐time intermolecular vibrational analysis method employing Raman spectroscopy is used herein for quantitative analysis of organic and inorganic residues in TFD4 cleaning solution (TFD4 comprises a mixture of anionic and nonionic surfactant agents, potassium hydroxide, and stabilizing agents). This study also identifies the development of a new peak, indicative of Al‐bonding in TFD4 solution during the cleaning process, and demonstrates that a change in the bonding occurs in the solution. The result of Raman intensity measurement by changing the bonding strength in solution can be applied to make predictive models and analytical techniques that can indicate the relationship of mixed solution.