High temperature condensed phase mass spectrometric analysis. 1998 annual progress report

Technical Report · Mon Jun 01 04:00:00 EDT 1998

DOI:https://doi.org/10.2172/13466· OSTI ID:13466

Delmore, J E

'The purposes of this program are to design and construct a mass spectrometer for the analysis of high temperature condensed phase materials, and to use this instrument to investigate the high temperature chemistry of waste form materials. Individual mass spectrometric techniques can provide windows through which to view selected properties of materials at high temperatures, but information from several sources must be combined to obtain the larger picture. This instrument is designed to provide several types of interlaced mass spectrometric analyses from a single specimen, eliminating the uncertainties associated with combining data from several different samples analyzed in different instruments. The features that are being combined in this instrument are: (1) miniaturized sample mounting and control of sample temperature to 1,300 C; (2) electron impact (EI) ionization of volatilized neutrals; (3) surface ionization, positive and negative ions; (4) secondary ion mass spectrometry (SIMS), positive and negative ions; (5) ultrahigh vacuum combined with sputtering to allow surface analyses to be related to bulk composition; (6) a single mass analyzer able to sequentially analyze ions from each of the ionization modes. These features will allow the following types of information to be obtained: (1) Atomic and molecular species vaporizing from the surface, both neutral and ionic. Neutrals will predominate in almost all systems, but the positive and negative ions which do volatize give valuable insights into the condensed phase chemistry. (2) SIMS interrogation of the surface composition, with ions sputtered from the surface analyzed by mass spectrometry. A high intensity sputter ion gun will be used to clean the surface, while a lower intensity ion gun will be used for the SIMS analysis. The ultrahigh vacuum will allow the surface to be maintained in a clean configuration until the analysis can be completed. This in turn gives information concerning the bulk composition of the material. (3) This information is obtained as a function of temperature from a single sample, so the interpretation of events will be more straight forward than merging data from different instruments. There currently are two instruments operating in the laboratory that perform these functions; one for SIMS and surface ionization on high temperature samples, and the other for EI and surface ionization. These have provided valuable insights into the properties of materials at high temperatures, but there is uncertainty from the perspective that all analyses cannot be performed on the same sample and from the fact that neither can guarantee a clean surface.'

• Research Organization: Lockheed Martin Idaho Technologies Co., Idaho National Engineering and Environmental Lab.,Idaho Falls, ID (US)
• Sponsoring Organization: USDOE Office of Environmental Management (EM), Office of Science and Risk Policy
• OSTI ID: 13466
• Report Number(s): EMSP-60424--98; ON: DE00013466
• Country of Publication: United States
• Language: English

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54 ENVIRONMENTAL SCIENCES
CHEMICAL REACTIONS
CHEMICAL WASTES
Chemical Reactions
Chemical Wastes
DECOMMISSIONING
DECONTAMINATION
Decommissioning
Decontamination
HIGH-LEVEL RADIOACTIVE WASTES
High-Level Radioactive Wastes
MASS SPECTROSCOPY
Mass Spectroscopy
PROGRESS REPORT
Progress Report
RADIOACTIVE WASTES
REMEDIAL ACTION
Radioactive Wastes
Remedial Action
SEPARATION PROCESSES
Separation Processes
TECHNETIUM
Technetium