During the spherical agglomeration process, a suspended solid is agglomerated by adding a binding liquid. First, micro-agglomerates or flocs are produced, which are compacted in the course of the process. Agglomerate size was evaluated by laser diffraction spectrometry, image analysis was used to determine the size and some adequately defined shape parameters calculated by Fourier analysis of the particle contour. The shape analysis confirms the visual observations; the compaction of the flocs is expressed by the corresponding change of the shape parameters. The influence of several process parameters on changes in agglomerate shape can be described quantitatively and help to gain an insight into agglomeration mechanisms. The particle size distributions determined by image analysis and laser diffraction spectrometry hardly differ for fairly spherical flocs or agglomerates. Concerning the size distribution of the irregular flocs, laser diffraction spectrometry measures larger particles than image analysis.