On-line Tritium Process Gas Analysis by Laser Raman Spectroscopy at TSTA

O’hira, Shigeru; Nakamura, Haruto; Konishi, Satoshi; Hayashi, T.; Okuno, Kenji; Naruse, Yuji; Sherman, R.H.; Taylor, David J.; King, M.; Bartlit, J.R.; Anderson, James L.

doi:10.13182/fst92-a29790

Cited by 27 publications

(6 citation statements)

References 7 publications

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“…These efforts evolved from off-line analysis of collected gas 17 to at-line measurements using specialized gas cells and free-beam lasers 18,19 , with subsequent use of fiber optics with external gas cells. [20][21][22] None of these approaches met one or more of the requirements for TCAP implementation, specifically contained laser energy, ease of use, a rugged on-line sampling interface, and minimal use of glove box space.…”

Section: Conventional Raman Measurementsmentioning

confidence: 99%

Isotopic hydrogen analysis via conventional and surface-enhanced fiber optic Raman spectroscopy

Lascola

Zeigler

McWhorter

et al. 2004

Advanced Environmental, Chemical, and Biological Sensing Technologies II

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This report describes laboratory development and process plant applications of Raman spectroscopy for detection of hydrogen isotopes in the Tritium Facilities at the Savannah River Site (SRS), a U.S. Department of Energy complex. Raman spectroscopy provides a lower-cost, in situ alternative to mass spectrometry techniques currently employed at SRS. Using conventional Raman and fiber optics, we have measured, in the production facility glove boxes, process mixtures of protium and deuterium at various compositions and total pressures ranging from 1000 -4000 torr, with detection limits ranging from 1-2% for as low as 3-second integration times. We are currently investigating fabrication techniques for SERS surfaces in order to measure trace (0.01-0.1%) amounts of one isotope in the presence of the other. These efforts have concentrated on surfaces containing palladium, which promotes hydrogen dissociation and forms metal hydride bonds, essentially providing a chemical enhancement mechanism.

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Section: Conventional Raman Measurementsmentioning

confidence: 99%

Isotopic hydrogen analysis via conventional and surface-enhanced fiber optic Raman spectroscopy

Lascola

Zeigler

McWhorter

et al. 2004

Advanced Environmental, Chemical, and Biological Sensing Technologies II

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“…The Material Science and Technology Division in the Tritium group at Los Alamos National Laboratory, along with a research group from the Japanese Atomic Energy Research Institute, designed a 4 cm 3 flow through cell for near-real time observation of hydrogen mixes 4,5 . They were able to analyze the isotopes in less than two minutes, with detection limits of 0.02%.…”

Section: Brief Review Of Literaturementioning

confidence: 99%

“…They were able to analyze the isotopes in less than two minutes, with detection limits of 0.02%. They also determined the first order time constants for hydrogen isotopic exchange rates 4,5 . Uda and coworkers 6 used Raman to analyze isotopic methanes in fusion fuel gas processing systems.…”

Section: Brief Review Of Literaturementioning

confidence: 99%

Fiber-Optic Laser Raman Spectroscopy Sensor

Ziegler¹

2003

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“…The Material Science and Technology Division in the Tritium group at Los Alamos National Laboratory, along with a research group from the Japanese Atomic Energy Research Institute, designed a 4 cm 3 flow through cell for near-real time observation of hydrogen mixes. [8,9] They were able to analyze the isotopes in less than two minutes, with detection limits of 0.02%. They also determined the first order time constants for hydrogen isotopic exchange rates.…”

Section: Introductionmentioning

confidence: 99%

“…They also determined the first order time constants for hydrogen isotopic exchange rates. [8,9] Uda and coworkers [10] used Raman to analyze isotopic methanes in fusion fuel gas processing systems. In addition to a flow cell, they used fiber-optics to deliver the laser energy to the cell.…”

Section: Introductionmentioning

confidence: 99%

Evaluation of Technologies to Complement/Replace Mass Spectrometers in the Tritium Facilities

Tovo¹,

Lascola²,

Spencer³

et al. 2005

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EXECUTIVE SUMMARYThe problem of the aging mass spectrometers coupled with lack of vendor support and no viable commercially available replacement presents risks for process control and monitoring in the Tritium Facilities. Therefore, several technologies were evaluated to maintain and, if possible, to enhance the current analytical capabilities provided by the existing mass spectrometers. These technologies included potential replacement/complement mass spectrometers as well as on-line sensors. Based on the results of this evaluation, the Savannah River National Laboratory (SRNL) makes the following recommendations.• Work should begin on implementation of the Quantra Fourier Transform-Ion CyclotronResonance (FT-ICR) as a complement to the existing mass spectrometers or as an on-line process analyzer. In its current configuration, the instrument can measure masses 12 or greater, with a resolution of 30,000 at mass 28, and 100 part per million detection limit using ion ejection of major ions. Thus, the 16-24 mass region that is not so easily separated by the existing Tritium Facility mass spectrometers could be resolved and measured using the FT-ICR. For the FT-ICR (Quantra) to be of even more benefit to the Tritium Facilities, it should be reengineered to provide analysis of masses 2-1000 in a single scan as well as other hardware and software improvements identified during our evaluation (i.e. long term stability, quantitative analysis of mixtures, etc.). In collaboration, SRS, LANL, and Y12 have secured funding for this project and the re-engineering effort will begin in FY06. Once the re-engineering effort is complete, funding will be required for performance testing and implementation in a tritiated environment as well as validation with the design agency.• The bench top magnetic sector mass spectrometer (GCMATE) technology closely matches that of the existing mass spectrometers in the Tritium Facilities. The initial work with the GCMATE indicates that its resolution and sensitivity meet the requirements of a replacement mass spectrometer for the Tritium Facilities. Although this instrument appears to be the most promising as a replacement for the existing mass spectrometers, delayed funding in FY05 precluded a complete evaluation. Therefore, evaluation of this instrument should continue in FY06.• Fiber optic Raman Spectroscopy has been demonstrated as a useful on-line technology for measurement of hydrogen isotopes at a concentration of greater than 1%. The method should be demonstrated on a process containing tritium. Upon successful demonstration in a tritium process, the method should then be implemented on the Hydrogen-Tritium Thermal Cycling Adsorption Process (HT-TCAP) and other processes that would require a detection limit of 1% or greater. Research and development to improve the detection limit of the fiber optic Raman method should continue as this would allow on-line analysis of other process points (i.e. HT-TCAP product and raffinate, Tritium Process Stripper, etc.).• The on-line vapochromic sens...

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On-line Tritium Process Gas Analysis by Laser Raman Spectroscopy at TSTA

Cited by 27 publications

References 7 publications

Isotopic hydrogen analysis via conventional and surface-enhanced fiber optic Raman spectroscopy

Isotopic hydrogen analysis via conventional and surface-enhanced fiber optic Raman spectroscopy

Fiber-Optic Laser Raman Spectroscopy Sensor

Evaluation of Technologies to Complement/Replace Mass Spectrometers in the Tritium Facilities

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