Electromagnetic properties of doped perovskites depend sensitively on the doping level. Both the superconducting transition temperature of Bi2Sr2Ca(Pr)Cu2O8+d compounds and the magnetic and electronic transport properties of La(Sr)Co(Fe)O3 perovskites change dramatically with the doping level. Apart from doping, oxygen deficiency is influenced by the details of preparation processes such as calcination and sintering. Simultaneous determination of constituents is of crucial importance from sample characterization point of view. Quantitative analysis of perovskite oxides can be performed by Secondary Neutral Mass Spectrometry (SNMS) which is a suitable technique to measure the chemical composition of almost any sample because the flux of atoms sputtered from the sample is representative of the stoichiometry of the top-most layers. The composition and oxygen content of Bi2Sr2Ca0.86Pr0.14Cu2O8.4 and La1-xSrxCo0.975Fe0.025O3-d, where 0