SEPARATION OF HYDROGEN ISOTOPES BY GAS CHROMATOGRAPHY

Thesis/Dissertation · Mon Jan 01 00:00:00 EST 1962

OSTI ID:4756553

Carter, Jr, E H

Apparatus and procedures for the transfer, dilution, and separation of samples used in studies of the hydrogentritium-tritnum hydride, deuterium-tritium- tritium deuteride, and hydrogen-deuterium-hydrogen deuteride systenas by gas- solid elution chromatography were developed. Various elution experiments were conducted with palladium on flint quartz, silica gel, chromia-alumina, ferric oxide-alumina, and activated-alumina columns. Separation of hydrogen, tritium, and tritium hydride with palladium on flint quartz was not evidenced by elution analysis with argon carrier at column temperatures between 150-175 deg . The results, however, corfirmed the observation that pailadium can be used to concentrate tritium from hydrogen-tritium mixtures at elevated temperatures by displacement methods. Complete separation of tritium hydride and tritium was obtained on silica gel with hydrogen carrier at 77 deg K. Neon and helium failed to elute adequately the isotopes from the column at 77 deg K and inadequate resolution of tritium, tritium deuteride, and tritium hydride was observed with hydrogen carrier. An analytical determination of hydrogen, tritium, and tritium hydride in equilibrating mixtures of the isotopes was made. Under proper conditions of deactivation, resolution of hydrogen, tritium, and tritium hydride was effected on an 8-ft. chromiaalumina column at 77 deg K with both helium and neon carriers. Partial parahydrogen-orthohydrogen resolution was also observed. An analytical determinati on of the molar composition of hydrogen, tritium, and tritium hydride in equilibrating mixtures was made. A comparison between theoretically determined isotopic compositions at equilibrium (1200 deg K) in the H/sub 2/ + T/sub 2/ in equilibrium 2HT system and chromatographically determined compositions for equilibrium mixtures was also made. An 8-ft. ferric oxide-alumina column gave similar results in the 1-esolution of hydrogen, tritium hydride, and tritium. However, under the deactivationreactivation conditions employed, essentially complete equilibration of orthohydrogen and parahydrogen was observed with helium carrier at 77 deg K. Several activatedalumina columns were employed with hydrogen, helium, and neon carriers at 77 deg K. Various mixtures of hydrogen, deuterium, tritium, tritium hydride, tritium deuteride, and hydrogen deuteride were adequately resolved on the columns. Absolute resolution of hydrogen, tritium, and tritium hydride and of deuternum, tritium deuteride, and tritium was efiected on an 8-ft. activated (370 deg , 8-20 hrs.) alumina column at 77 deg K with helium carrier. An investigation of the effect of varying degrees of column activation on the relative separation factors for various isotopic species was made. In general, higher degrees of column activation (alumina-dehydration) were found to produce most effective resolution ployed. Adequate separation of hydrogen, tritium hydride, deuterium, tritium deuteride, and tritnum was also obtained with neon carrier at 77 deg K. A 6-ft. activated-alumina column was effective in the resolution of hytdrogen, tritium hydride, and tritium with neon carrier. With an increased number of components, less separation of the various isotopes was observed. Increased activation (340 deg , 53 hrs.) and increased column length (12 ft.) in general produced better resolutions of the various isotopes with hydrogen carrier at 77 deg K than were obtained on the shorter less-highly-activated columns. Helium and neon failed to elute the various isotopes from the highly-activated and/or longer columns in reasonable retention times. Simultaneous ionization chamber (50-ml.) and katharometer detection of hydrogen spin isomers and deuterium were also observed. (Dissertation Abstr., 23: No. 4, 1962)

• Research Organization: Originating Research Org. not identified
• NSA Number: NSA-17-004875
• OSTI ID: 4756553
• Resource Relation: Other Information: Thesis. Orig. Receipt Date: 31-DEC-63
• Country of Publication: Country unknown/Code not available
• Language: English

Related Subjects

ISOTOPE SEPARATION
ACTIVATION
ALUMINUM OXIDES
CHROMATOGRAPHY
CHROMIUM OXIDES
COLLOIDS
DETECTION
DEUTERIUM
DIFFUSION
EFFICIENCY
GASES
HELIUM
HYDROGEN
IONIZATION CHAMBERS
IRON OXIDES
ISOMERS
KATHAROMETERS
LABORATORY EQUIPMENT
MEASURED VALUES
NEON
PALLADIUM
QUALITATIVE ANALYSIS
QUARTZ
SILICON OXIDES
SOLIDS
SOLUTIONS
SPIN
TEMPERATURE
THERMAL CONDUCTIVITY
TRITIUM