Analytical procedures for the determination of selected speciation forms of sulphur have been proposed. The method for conversion of sulphur sols into homogeneous solutions sols allowing simultaneous determination of sulphur either in model solutions or in sols environmental samples has been described. The methods for determination of sulphur sols, elemental sulphur, soluble and insoluble sulphides, sulphates and total sulphur have been optimized. Selected speciation forms of sulphur were determined in the same samples of water and bottom sediments from the eutrophic lakes Lipno and Kiekrz, lying close to Poznan. The speciation analysis proposed is based on the catalytic, chromatographic, ion-selective methods and absorption spectrometry. The concentrations of the speciation forms of sulphur determined ranged from micrograms to milligrams per litre.