SummaryThis program (EMSP Project #60424) was funded by the EM Science Program for the development of an integrated mass spectrometric analysis system (see Figure 1.) capable of analyzing materials from room up to high temperatures, with the practical upper temperature limit to be experimentally determined. A primary objective of the program was the development of techniques to analyze waste materials during vitrification processing to produce waste forms.The sample is heated in the ion formation region of the mass spectrometer. This instrument geometry allows the atoms and molecules that volatilize from the sample as neutrals to be ionized before they have a chance to condense on surfaces that generally are cooler that the sample. In addition, this geometry facilitates more efficient focussing of SIMS and thermal ions into the quadrupole mass analyzer. Instrumental capabilities include the detection of volatilizing neutral species by electron bombardment, ions forming on the surface by surface ionization, and surface species by static SIMS. In addition, the instrument has elemental analysis capability (by dynamic SIMS).It was also initially proposed that during the concluding year the instrument would be used for a series of demonstration analyses; however, the program was funded at just 69% of the requested level, which proved adequate to complete the major aspects of the instrument development but was insufficient for the complete development of the dynamic SIMS capability and the completion of the demonstration analyses. The demonstration analyses are being performed with the support of other programs in our laboratory, and a dynamic SIMS gun, which was made available from another of our programs, is installed on the instrument (but has not yet been tested). Demonstration analyses have proven the concept of the instrument; all of the capabilities, other than the dynamic SIMS capability, have been successfully deployed. The dynamic SIMS capability will be more fully developed when another program has a demonstrated need and funds that activity.The practical upper temperature limit for analyses is proving to be limited by mechanical stability of the sample support hardware at high temperatures and by chemical reactions between the material to be analyzed and the supporting filament or cup. The practical upper temperature limit for mechanical stability for the filament mode is proving to be about 1700°C, while for the refractory metal cup mode the limit is about 1300°C. When chemical reactions occur between the material and the cup or filament, which is often the case, the temperature limit can be lower, although systems have been studied at above 1000°C. In general, the cup assembly is proving to be more resistant to failure due to chemical reactions since the sample is not in contact with the delicate filament (that can be eroded through chemical reactions with the sample). The ability to study chemical interactions between the sample and the holder is turning out to be a significant advantage offered by the ...