An overview to the results from the application of various spectrometric (atomic absorption spectrometry, AAS; inductively coupled plasma -atomic emission spectrometry, ICP-AES; and inductively coupled plasma -mass spectrometry, ICP-MS) and radioanalytical (neutron activation analysis, NAA) techniques in environmental pollution studies in the Republic of Macedonia are presented. The results from the surveys of the pollution with heavy metals of soil, air and food are reported. The pollution with heavy metals in the particular regions was additionally investigated using moss, lichens, attic dust, soil, water and sediment samples. The results from the study of the pollution in the cities of Veles (lead and zinc smelter plant), Kavadarci (ferronickel smelter plant), Radoviš (copper mine and flotation), Probištip, Makedonska Kamenica and Kriva Palanka (lead and zinc mines and flotation plants) and Bitola and Kičevo (thermoelectric power plants) are presented.