A technique for the estimation of time since discharge of a given class of spent shotgun shells is presented. The technique involved the use of SPME (Solid Phase Microextraction) sampling from the atmosphere inside spent shotgun shells. Compounds absorbed on the SPME fiber were desorbed and analyzed with GC-MS. The decrease in concentration of the combustion product naphthalene was monitored in all shells over a two-month period. Three conditions were examined to prevent naphthalene from escaping prior to testing the shells. A glass vial was successfully incorporated to halt the dissipation of naphthalene. At room temperature the naphthalene peak can be measured for several months and the curve-fitting data can lead to an estimation of time since discharge.