Polyaldehyde microspheres, polyglutaraldehyde (PGL), and polyacrolein (PA) were synthesized by polymerizing glutaraldehyde and acrolein in the presence of an appropriate surfactant. The microspheres with average diameter of 0.2 micron were used for the specific labeling of human red blood cells (RBC) and mouse lymphocytes. The "naked" microspheres were encapsulated with agarose and formed agarose-polyaldehyde microsphere beads in sizes ranging from 50 microns up to 1 cm. The encapsulated beads, with diameters ranging from 50 to 150 microns were used as insoluble adsorbents for affinity purification of antibodies. Beads with diameters varied from 150 to 250 microns were used for cell fractionation purposes (mouse B splenocytes from T splenocytes). Uniform beads of 1 mm diameter were designed for hemoperfusion purposes. As a model, the removal in vitro of anti-BSA from immunized goat whole blood was studied.