By studying on the material composition, texture and structure of ores of Shapinggou molybdenum deposit, Anhui Province, it is found that molybdenites in the ores often present as small scale-like and disseminated minerals distributed in veinlets. As the associated elements in the ores show no interference with the determination of Mo-content, in the conditions of no addition of Fe2O3 carrier, melting ore with corundum crucible-Na2O2, reducing blank values and strict quality supervisory control, the method of thiocyanate spectrophotometric analysis for determination of Mo-content gave stable and reliable results.