This work studied the at-line Raman spectroscopy monitoring for the inverse miniemulsion polymerization of acrylamide. The conversion,. was determined from the Raman spectra without previous. calibration :using the peaks corresponding to -CH2- and C=C functional groups of acrylamide. Gravimetric data: was used to validate the results of conversion obtained with the Raman spectra,: Dynamic light scattering was used to measure the particle size. The results show that high energy in the homogenization step increases the surface area of the droplets and generates a lack of surfactant, which results in larger diameters. It is possible to make at-line monitoring of monorner conversion diredly from, the Raman spectra without using calibration models. The data obtained show an incomplete conversion that is also confirmed by gravimetric analysis.