In this study a headspace spectrophotometric method is proposed for analysis of dichloromethane and isobutyl methyl keton (IBMK) residues in the ampicillin powder. Ampicillin is dissolved in 1 M NaOH in the vessel of an arsenic analyzer unit of an atomic absorption spectrophotometer. After 3-min stirring, the headspace has flowed by air into the flow-through cell and its absorbance is read at 196 nm, as emitted by a selenium hollow cathode lamp. The absorbance of the headspace is read in two cases (in the presence and absence of MnO4- ion). In the former case, the absorbance is only related to dichloromethane; in the latter, it is related to both solvents. By this method both solvents are determined in the ampicillin samples. The obtained results are compared with gas chromatography (GC) data. These results have good agreement. The proposed method is very rapid, selective and repeatable. Other solvents present, such as isopropyl alcohol, ethylacetate and triethylamine, are not interfering.