A Method for Measuring Total Protium and Total Deuterium …
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can be used by the scientific community to generate rapid and accurate data are
needed.
A novel analytical technique has been developed that measures both total protium
(H) and total deuterium (D) in a gas mixture containing protium (H 2 ), molecular
deuterium(D 2 ), and protium-deuterium (HD) using a relatively inexpensive microgas chromatograph (uGC) with thermal conductivity detectors. This technique uses
two molecular sieve columns. One column uses molecular deuterium (D 2 ) as the
carrier gas and the other uses protium (H 2 ) as the carrier gas.
Experimental
Materials and Instrumentation
The micro-gas chromatograph used for testing the Thermal Cycling Absorption
Process and subsequently to develop this new analytical technique is a model
fusion gas chromatograph from Inficon. This model micro-gas chromatograph can
be configured with two columns and two different carrier gases, which made it well
suited for testing and developing this new analytical technique. Samples injected
into the micro-gas chromatograph are analyzed simultaneously by the two columns.
Analysis time is approximately 45–60 s. A model M200 micro-gas chromatograph
was configured with two molecular sieve columns. One column was supplied with
molecular hydrogen carrier gas and the other column supplied with molecular
deuterium carrier. Both columns were equipped with thermal conductivity detectors.
Gas mixtures containing (25% protium, 75% molecular deuterium), (50% molecular
hydrogen, 50% molecular deuterium), and (75% protium, 25% molecular deuterium)
were prepared and analyzed with the gas chromatograph.
As anticipated, each gas chromatograph column displayed only one peak and this
peak amplitude varied as predicted. The maximum area of the peak for the gas chromatograph column with molecular hydrogen carrier gas was with the (25% molecular
hydrogen, 75% molecular deuterium) mixture and the minimum peak height was
produced by (75% molecular hydrogen, 25%molecular deuterium) mixture. This
data meant that the peak area represented molecular deuterium concentration. The
maximum peak area for the gas chromatograph column with molecular deuterium
carrier gas was produced by the (75% protium, 25% molecular deuterium) mixture
and the minimum peak area was with the (25% protium, 75% molecular deuterium)
mixture. This data meant that the peak area represented protium concentration. A
three-point calibration curve was generated for each gas chromatograph column
based on the area under the curve for each analysis.
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