Lowering of the detection limits of the alkali elements in Bi-containing superconductors was achieved by optimization of the carrier gas flow rate in ICP-AES. The contents of the alkali metals in the final superconducting products, obtained on the basis of the Li, Na, K, Rb and Cs doped Bi-containing materials, were investigated. A significant decrease of their concentrations after the synthesis was found. The limits of detection with respect to the dissolved solid were as follows: 1.0×10-4% Li, 1.0×10-3% Na, 7.7×10-4% K and 9.7×10-4% Rb. The relative standard deviation was not more than 0.6 % for Li, 1% for Na and 2% for K and Rb. © 1995 Springer-Verlag.