Various physical and chemical parameters of interest to the pharmaceutical industry were determined by NIR spectroscopy with a view to assessing the potential of this technique as an effective, expeditious alternative to conventional methods for this purpose. To this end, the following two steps in the production process of tablets containing 1 g of paracetamol were studied: (1) intermediate granulation, which was characterized in terms of Active Principle Ingredient (API) content, average particle size and particle size distribution and (2) manufactured tablet, which was examined in relation to compaction pressure and API content of the tablets. The ultimate aim was to identify critical attributes of the process influencing the quality of the end-product. Based on the results, a new method for determining the API in the end-product was developed and validated for its quality control. © 2009 Elsevier B.V. All rights reserved.