Toluene swell or equilibrium swelling is universally used by rubber factories to measure the degree of crosslink of their compounded or prevulcanized latices at different stages of production. To apply near infrared spectroscopy for rapid and accurate quality control, spectral acquisition of prevulcanized latex, thin film and thick film was performed using a Fourier transform near infrared spectrometer in diffuse reflection mode across the wavenumber range of 12,500-3600 cm À1. For prevulcanized latex an effective model was developed using partial least squares regression with preprocessing (first derivative þ straight line subtraction method). The coefficient of determination (r 2), root mean square error of cross validation and bias of the validation set were 0.71, 3.93% and À0.005%, respectively. For the thin film model the r 2 , root mean square error of cross validation and bias were 0.65, 4.01% and À0.028%, respectively. Whereas for the thick film model the r 2 , root mean square error of cross validation and bias were 0.70, 4.00% and À0.006%, respectively. Three models including prevulcanized latex, thin film and thick film were validated by 23 unknown samples, providing standard error of prediction and bias of 5.357 and 2.494, 4.565 and 1.001 and 3.641 and À0.961%, respectively, for prevulcanized latex, thin film and thick film. The model developed for the thick film spectra gave the best results.