Gross alpha activity determination in drinking water is one of the radiological parameters that must be determined in order to decide whether further specific analyses of radionuclides in samples is required. This parameter can be determined by the co-precipitation method using a ZnS(Ag) scintillation detector or a proportional counter. The method consists of collecting all alpha emitters of interest using barium and iron as carriers as they provide more uniform and homogeneous residues than the evaporation method, especially for highly saline waters. In the course of our work, the efficiencies of the gas proportional and ZnS(Ag) detectors for alpha particle detection in water residues were studied in function of sample mass (precipitate) with residues ranging between 16.0 and 35.0mg. In addition, the structure and morphological composition of a residue collected by the co-precipitation method was studied with the aim of verifying whether the residue is a homogeneous mixture. The effect of alpha energy on the efficiency and stability of the calibration samples (mass and efficiency) was studied using (230)Th, natural uranium ((nat)U) and (241)Am radionuclides.