A novel adsorbent (ZnS:Mn nanoparticles loaded on activated carbon) was made. The competitive adsorption of Direct Yellow 12 (DY12) and Reactive Orange 12 (RO12) dyes in binary mixture onto this adsorbent was studied. DY12 and RO12 with severe spectra overlapping were chosen and analyzed simultaneously with high accuracy by first order derivative spectrophotometric method in binary solutions. The effect of multi-solute systems on the adsorption capacity was investigated. Because of the specific characteristics of ZnS:Mn-NP-AC was found to be efficient for the removal of the dyes studied. The adsorption capacities were investigated and described by the mono- and multi-component Langmuir and Freundlich isotherm models for both single and binary dye solutions. The isotherm constants for DY12 and RO12 were calculated. For single solution of DY12 and RO12 dyes, the adsorption capacities of the