The labelling of a water-soluble synthetic polyelectrolyte, having anticoagulant activity, has been studied. The polyelectrolyte is derived from cis-1,4-polyisoprene and contains N-sulfate and carboxylate groups. [125I]-Iodination of the polyelectrolyte, using the Chloramine-T method and an electrolytic method, resulted in a [125I]-labelled polyelectrolyte from which release of the label occurred. Resulfation of a partially desulfated polyelectrolyte with a [35S]-sulfur trioxide trimethylamine complex resulted in a [35S]-labelled polyelectrolyte which showed no release of the label