Abstract: A process and apparatus are provided that permits a sample to be cooled below the glass transition temperatures of the components of the sample without forming objectionable frost on the surface of the sample. In accordance with the invention, the sample is confined within a freeze box that is hermetically-sealed from the ambient atmosphere. The freeze box is purged with a dry inert gas until essentially all moisture is removed from the freeze box. The sample then is rapidly cooled to a temperature below the glass transition temperature of the components of the sample before being transferred to an analysis instrument without exposing the sample to ambient atmosphere.