The occurrence of Pt in environmental matrices is increasing since the introduction of automobile catalytic converters. Given that Pt is bioavailable and causes biological effects in plants and animals, respective biomonitoring programs are in high demand. But the analytical methods for conducting such programs have not yet been sufficiently established. Therefore, a study was carried out to develop a microwave digestion of biological samples, which allows a rapid determination of Pt by adsorptive cathodic stripping voltammetry. A high pressure microwave system was used and the digestion was performed in HNO3 and HCl. After digestion the HNO3 was evaporated with a microwave assisted vacuum concentration set. The study resulted in a procedural detection limit of 37.5 ng L−1 and a relative standard deviation of 18%. A recovery study resulted in a Pt loss below5%. The microwave assisted evaporation ofHNO3 performed satisfactorily and up to 500mL of the sample solution could be used for the voltammetric measurements without any effect on the peak heights. A direct comparison of Pt concentrations conducted after microwave digestion and digestion by high pressure ashing showed similar values. However, these promising results were not persistent throughout the repeated analysis using the same Teflon vessels. The vessels did not endure the harsh conditions and due to aging processes the Pt loss consistently increased until Pt determination in environmental relevant concentrations became impossible. Quartz vessels could not be employed as an alternative to the Teflon vessels, due to a lack of compatibility with the vacuum concentration system. Consequently, the results of this paper showthat there is a need for further development of more resistant Teflon materials.