Detection of canines are well-known to be valuable in the location of contraband, such as explosives or narcotics. More recently, canines have been trained and utilized in the detection of concealed mass storage devices that might contain evidence of illegal activity such as child pornography. To lay the analytical foundation for this detection work, research was carried out to determine the volatile organic compounds associated with mass storage devices (MSD) that could be used by trained canines for detection. Headspace analysis of a variety of electronic devices was performed using solid phase microextraction (SPME) with gas chromatography/mass spectrometry (GC/MS). Analyses found several volatile compounds common to SIM and SD cards, as well as USB drives, including 2-propenenitrile, styrene, isophorone, hydroxycyclohexyl phenyl ketone, and 2-furanmethanol, tetrahydro. Results indicated that mass storage devices do have a characteristic odor profile making detection with minimal false alerts feasible for trained canines.