It is demonstrated that during suspension polymerizations it is possible to monitor morphological characteristics of PVC resins such as bulk density, cold plasticizer absorption and average particle diameter in‐line and in real time using NIR spectroscopy. NIR spectra are obtained at different experimental conditions, showing that the spectra are sensitive to changes in the PVC properties. Standard mathematical procedures (partial least squares regression) are used to build empirical models and correlate the morphological properties with the obtained NIR spectra, allowing for monitoring of the PVC morphology in‐line and in real time.