The investigation of Bi1.8Pb0.4Sr2Ca2.2Cu3.2O10-y material sputtering in hollow cathode discharge is presented. The ICP-OES analysis is used for quantitative analysis of the cathode sample and the deposit on a substrate, situated in front to the cathode hole. We suggest using spectral coefficients, which connect the relative spectral intensity with the relative concentration of the deposited elements. These coefficients, once obtained, are typical for every element in the multi-component material and for its chosen spectral line. The above-mentioned spectral coefficients can be used for relative concentration obtaining and for “in-situ” concentration, control during the sputtering of this kind of ceramics.