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The determination of actinides in small concentrations of natural thorium, uranium, radium, lead and polonium in environmental samples has been subject of several investigations. Also, analyses of actinides nuclides in environmental materials are important for control measurements associated with discharge of these radio-nuclides from nuclear facilities and uranium mills. For that purpose, alpha spectroscopy is a convenient method that has been applied to various investigations in nuclear science and technology. Principally, radiochemical determination of alpha emitters consists of three main steps [2]:(1) sample pretreatment,(2) chemical separation of the nuclides of interest and (3) preparation of a source suitable for alpha counting. Therefore, after a good sample pretreatment step, chemical separations of the nuclides of interest have to be done carefully. Usually, separation techniques for alpha emitters …