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Radiochemical Processing Laboratory

Hydrogen Gas Measurements

Working with the high-sensitivity quadrupole mass spectrometer system
Quadrupole detector and vacuum enclosure.(Enlarge image)

Hydrogen is generated in reactor or accelerator materials by reactions which produce protons. Unlike helium, which accumulates at grain boundaries, it is generally thought that hydrogen easily diffuses out of metals at elevated temperatures, never reaching large concentrations. Under some irradiation conditions, however, it appears that relatively large hydrogen concentrations can be retained in a variety of microstructural trapping sites (e.g., voids or bubbles), some having large binding energies. It appears that hydrogen may be participating in the nucleation and growth of voids, producing swelling at lower-than-expected exposures. PNNL has developed a unique mass spectrometry system that provides sensitive measurements of hydrogen in very small samples of radioactive materials in order to study these effects. The sensitivity is up to three orders of magnitude higher than standard commercially available analysis instruments.

Hydrogen Measurement Services

A unique high-sensitivity quadrupole mass spectrometer system for measurement of low concentrations of hydrogen in very small solid materials is operational at PNNL. The system heats the samples without melting or vaporizing them, in a small-volume ceramic crucible. The samples are held in an evacuated carousel which allows for multiple analyses without breaking the system vacuum. Crucible temperature is adjusted up to ~ 1200°C depending on the analysis material. Hydrogen leak standards are used to calibrate the system. This new facility is capable of providing hydrogen analysis services for utilities and research laboratories in the United States, Europe, Japan, and elsewhere. The capabilities of the system include:

  • Analysis of both normal and radioactive samples.
  • A dynamic range from low atomic parts-per-million to percent levels, with an absolute accuracy of approximately 5%.
  • Analysis of samples ranging in mass from sub-milligram to several grams.
  • Measurement of total hydrogen content (by rapid heating) or hydrogen release as a function of time or temperature (for diffusion and/or kinetics measurements).
  • The system can also be used for the measurement of other gases such as helium, argon, krypton, that will diffuse at temperatures of 1200°C or below.

Point of Contact:
Ingrid Burgeson, Nuclear Chemistry & Engineering Team
Phone: (509) 375-5387

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