Traces of vanadium, manganese, iron, cobalt, nickel, copper, and zinc were quantitatively extracted with diethyldithiocarbamate (DDTC) in benzene from a digested solution of biological materials and the metal-DDTC complexes were collected into a small amount of polystyrene foam produced by lyophilization of the benzene extract after addition of polystyrene. The polystyrene foam was dissolved in benzene and spread on Mylar film. After drying, a polystyrene film containing metal-DDTC complexes was produced on Mylar film, and then the polystyrene film was peeled from the Mylar film. This film was subjected to PIXE analysis. This method was applied to NBS SRM 1572 citrus leaves and a marine macroalgal sample, and 6 trace metals were simultaneously and accurately determined.