According to the trend of the heavy crudes and high demand of fuels, it is projected a considerable increase in the production of vacuum residues. With the purpose of taking advantage of these loads, the refineries have been improving conversion processes for the production of better quality distillates. However, as increasing the severity conditions and the species content of resins and asphaltenes high concentrations of coke are obtained. To provide an insight into the quality and cokes properties, in this study fifty (50) coke samples obtained from vacuum residues processed under conditions of thermal cracking and hydroconversion were selected. Each coke was analysed in detail with properties such as fixed carbon, volatile material, ash, and calorific value. Subsequently, a characterization methodology was developed to predict the properties of cokes, by using partial least squares regression, and infrared spectroscopy (FTIR-ATR) in the spectral range from 4000 to 500cm-1. The models obtained by chemometrics allowed to predict the quality of the coke produced from vacuum residues with reliable responses in short periods of time.