72 As, 74 As, 77 As / Radioactive arsenic / Germanium target / Radiochemical separation / Labelled antibodies Summary. Radioarsenic labelled radiopharmaceuticals could add special features to molecular imaging with positron emission tomography (PET). For example the long physical half-lives of 72 As (T 1/2 = 26 h) and 74 As (T 1/2 = 17.8 d) in conjunction with their high positron branching rates of 88% and 29%, respectively, allow the investigation of slow physiological or metabolical processes, like the enrichment and biodistribution of monoclonal antibodies in tumour tissue or the characterization of stem cell trafficking. A method for separation and purification of no-carrier-added (nca) arsenic from irradiated metallic germanium targets based on distillation and anion exchange is developed. It finally converts the arsenic into an * As(III) synthon in PBS buffer and pH 7 suitable for labelling of proteins via As−S bond formations. The method delivers radioarsenic in high purity with separation factors of 10 6 from germanium and an overall yield from target to labelling synthon of > 40%. In a proof-ofprinciple experiment, the monoclonal antibody Bevacizumab, directed against the human VEGF receptor, was labelled with a radiochemical yield > 90% within 1 h at room temperature with nca 72/74/77 As.