We present some results on the content of metals determined in atmospheric aerosols sampled on a filter. The quality of the domestic (AFA-KhA and FPP) and foreign (Whatman-41) filters is compared and the recommendations for sampling atmospheric aerosols for their subsequent analysis by the X-ray spectrometry are given. The techniques of X-ray spectrometric determination of V, Mn, Fe, Ni, Zn, and Pb in urban and industrial aerosols are developed and studied from the standpoint of metrology.