This paper reports an attenuated total reflection-ultraviolet-visible spectroscopy technique assisted With multivariate data analysis for real-time determination of the content: of dissolved cellulose during pulp xanthation. During xanthation, the dissolved cellulose fractions in the viscose dope were directly measured by this spectroscopy technique without any extra sample pretreatment. The results showed that by using orthogonal signal correction and partial least-squares regression (PLSR) techniques, a robust and accurate calibration: model has been developed in which the R-2, root mean squared error cross validation, and relative prediction errors are 0:99,85, 0.2208, and 0.34%, respectively, The results of the dissolved cellulose content in viscose determined by this PLSR method were in good agreement with:results of the iodometric titration method; that is, the relative difference is less than 3.00%. The present method is robust and suitable for the application of real-time monitoring of the content of dissolved cellulose in viscose in laboratory or industrial applications.