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Abstract This study presents a novel analytical method for the quantitative and qualitative analysis of microplastics (MPs) in deionized (DI) water using Raman spectroscopy. Raman peak area ratios of 1295 cm−1 for polyethylene (PE) and 637 cm−1 for polyvinylchloride (PVC) to the broad H2O peak were utilized to establish a calibration model for the concentration of MPs dispersed in DI water at 0.1 wt% to 1.0 wt%. The calibration model demonstrated R2 values of 0.98537 for PE and 0.99511 for PVC, indicating high linearity between the peak area ratio and concentration. The calibration model was validated using mixed PE and PVC samples to confirm its applicability to real-world water bodies, where multiple types of MPs are present. The calculated standard error of calibration (SEC) and relative standard error of calibration (%RSEC) values further confirmed the accuracy of the predictions, providing a robust approach for detecting and quantifying MPs in aquatic environments.