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The alternating copolymer of divinyl ether and maleic anhydride (DIVEMA) possesses diverse biological activity and uses for production of drug delivery systems. DIVEMA's biological effects are determined by molecular mass, therefore it is necessary to have information about copolymer molecular mass and its distribution. A direct method for gel permeation chromatography analysis of DIVEMA molecular mass characteristics in aqua solution without any preliminary modification was developed. The effect of a number of factors (the concentration of monomers and their ratios, the concentration of initiator, the nature of the solvents) on DIVEMA's solution properties and molecular mass distribution was studied by gel permeation chromatography and viscometry. The approach to synthesis of DIVEMA with narrow molecular mass distribution was designed. The substantial influence of water on DIVEMA molecular mass characteristics was determined. The proposal was made that water may play a part in the formation of charge‐transfer complexes playing a significant role in copolymerization. Copyright © 2003 John Wiley & Sons, Ltd.