Abstract: The technological process of preparing 1400 cm2 α-spectrometric source and method of determination of α-nuclides in samples are described. This process includes the pretreatment of samples, the grounding of samples to near colloidal solution by supersonic breaker and the sticking of the sample micro-particles on aluminized polyester film in vacuum drying oven. The wet particle size is 1μm, the non-evenness--9.5%.The source is firm enough to meet therequirement. The resolution is 70 keV (for 70 μg/cm2, 241Am) . One sample can be prepared in 8 hours. This process is low in cost.The procedure of determination of samples containing α-nuclides is givenThe recovery of the whole procedure is 99.1%. The detection llmit of the method is 7×10-4 Bq/g (solid). The spectrogram and specific activity of seven kinds of samples have been determinated. The results of the standard soil material of IAEA analyzed are in agreement with the data.