A sealed rigid ‘‘purgebox’’ makes it possible to load air‐ and/or moisture‐sensitive solids into the solids probe inlet of a Fourier transform ion cyclotron resonance (FT/ICR) mass spectrometer. A pelletized sample is transferred (in a sealed canister) from a commercial drybox to a Lucite(R)purgebox. After the box is purged with inert gas, an attached glove manipulator is used to transfer the sample from the canister to the solids probe of the mass spectrometer. Once sealed inside the inlet, the sample is pre‐evacuated and then passed into the high vacuum region of the instrument at ∼10−7Torr. The purgebox is transparent, portable, and readily assembled/disassembled. Laser desorption FT/ICR mass spectra of the air‐ and moisture‐sensitive solids, NbCl5. NbCl2(C5H5)2, and Zr(CH3)2(C5H5)2are obtained without significant oxidation. The residual water vapor concentration inside the purgebox was measured as 100±20 ppm after a 90‐min purge with dry nitrogen gas. High‐resolution laser desorption/ionization mass spectrometry of air‐sensitive solids becomes feasible with the present purgebox interface. With minor modification of the purgebox geometry, the present method could be adapted to any mass spectrometer equipped with a solid sample inlet.