A quantitative analysis of degree of transformation from a softwood sulphite dissolving pulp to alkalised material and the yield of this transformation as a function of the simultaneous variation of the NaOH concentration, denoted [NaOH], reaction time and temperature was performed. Samples were analysed with Raman spectroscopy in combination with multivariate data analysis and these results were confirmed by X-ray diffraction. Gravimetry was used to measure the yield. The resulting data were related to the processing conditions in a Partial Least Square regression model, which made it possible to explore the relevance of the three studied variables on the responses. The detailed predictions for the interactive effects of the measured parameters made it possible to determine optimal conditions for both yield and degree of transformation in viscose manufacturing. The yield was positively correlated to the temperature from room temperature up to 45 °C, after which the relation was negative. Temperature was found to be important for the degree of transformation and yield. The time to reach a certain degree of transformation (i.e. mercerisation) depended on both temperature and [NaOH]. At low temperatures and high [NaOH], mercerisation was instantaneous. It was concluded that the size of fibre particles (mesh range 0.25–1 mm) had no influence on degree of transformation in viscose processing conditions, apparently due to the quick reaction with the excess of NaOH.