In this study, empirical and semiempirical K-shell fluorescence yields (omega(K)) and K beta/K alpha intensity ratios from the available experimental data for elements with 23 <= Z <= 30 were calculated to compare them with elements in different alloys. The experimental data are fitted using the quantity [omega(K)/(1 -omega(K))](1/4) vs Z to deduce the empirical K-shell fluorescence yields and K beta/K alpha intensity ratios. The empirical and semiempirical K-shell fluorescence yield values were used to calculate the K x-ray-production cross-section values for pure Co and Zn elements. Also, sigma(K alpha), sigma(K beta) production cross sections and K beta/K alpha intensity ratios of Co and Zn have been measured in pure metals and in different alloy compositions which have different pH values. The samples were excited by 59.5-keV. rays from a Am-241 annular radioactive source. K x rays emitted by samples were counted by an Ultra-LEGe detector with a resolution of 150 eV at 5.9 keV. The effect of pH values on alloy compositions and the effect of alloying on the fluorescence parameters of Co and Zn were investigated. The x-ray fluorescence parameters of Co and Zn in the alloying system indicate significant differences with respect to the pure metals. These differences are attributed to the reorganization of valence shell electrons and/or charge transfer phenomena.