A method for rapid determination of the contents of lignin, monosaccharides and organic acids in the process solutions of sulfite pulping. Accordingly, any non-ionized compounds that disturbs the measurement of these concentrations are separated from the lignin material by an ion-exclusion technique. The measurements of concentrations are carried out by means of the UV-method, refractive-index method, and/or by means of the polarimetric method. The method of the present invention is usable for the controlling of sulfite cooking or other pulping or by-product production processes as well as for the characterization of the spent liquor.