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Gas Chromatography of Hydrogen-Deuterium Mixtures

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Gas Chromatography of Hydrogen-Deuterium Mixtures University of Tennessee, Knoxville TRACE: Tennessee Research and Creative Exchange Doctoral Dissertations Graduate School 3-1960 Gas Chromatography of Hydrogen-Deuterium Mixtures Paul Payson Hunt University of Tennessee - Knoxville Follow this and additional works at: https://trace.tennessee.edu/utk_graddiss Part of the Chemistry Commons Recommended Citation Hunt, Paul Payson, "Gas Chromatography of Hydrogen-Deuterium Mixtures. " PhD diss., University of Tennessee, 1960. https://trace.tennessee.edu/utk_graddiss/2921 This Dissertation is brought to you for free and open access by the Graduate School at TRACE: Tennessee Research and Creative Exchange. It has been accepted for inclusion in Doctoral Dissertations by an authorized administrator of TRACE: Tennessee Research and Creative Exchange. For more information, please contact [email protected]. To the Graduate Council: I am submitting herewith a dissertation written by Paul Payson Hunt entitled "Gas Chromatography of Hydrogen-Deuterium Mixtures." I have examined the final electronic copy of this dissertation for form and content and recommend that it be accepted in partial fulfillment of the requirements for the degree of Doctor of Philosophy, with a major in Chemistry. Hilton A. Smith, Major Professor We have read this dissertation and recommend its acceptance: John W. Prados, Jerome F. Eastham, William E. Bull, John A. Dean Accepted for the Council: Carolyn R. Hodges Vice Provost and Dean of the Graduate School (Original signatures are on file with official studentecor r ds.) January 16, 1960 To the Graduate Council: I am submitting herewith a dissertation wr itten by Paul Payson Hunt entitled "Gas Chromatography of Hydrogen­ Deuterium Mixtures." I recommend that it be accepted in partial fulfillment of the requirements for the degree of Doctor of Philosophy , wi th a ma jor in Chemistry. We have read this dissertation and reccmmend its acceptance: Accepted for the Council: _ tl�uJ. __ Dean,i&l/ of th ){aue G� ool GAS CHROMATOGRAPHY OF HYDR OGEN-DEUTERIUM MIXTURES A Disser tation Pre sented to the Graduate Counc il of The University of Tenne ssee In Partial Fulfillment of the Requirements for the Degree Doctor of Philosophy by Paul Payson Hunt March 1960 ACKNOWLEDGMENT The author wishes to express hi s most sincere appre­ ciation to Dr. Hilton A. Smi th for his fri end ship and counsel during the cour se of this research. The work was made pos- sible through a research grant from the Un ited States Atomic Energy Commission for the period from September 1957 to Decembe r 1959 . The flint quartz employed in this work was donated by the Whittaker , Clark , and Daniels Company , Inc., and the Raney nickel and Rane y cobalt were contributed by the Raney Catalyst Company. The author also wi shes to thank his wife , Helen , for her patience , understanding , and encouragement toward the completion of the work . TABLE OF CONTENTS CHAPTER PAGE I. INTRODUCTION • • . 1 A. Scope . 1 B. His torical . 2 c. • . Chromatographic Techn iques • • . 5 1. Elution Development . • • • .•• 5 2. Frontal Analysis . • • . 6 3. Displacement Development •..•.... 6 D. Dis tribution Isotherms • . • . 7 E. Hydrogen and Deuterium • . 7 II. APPARATUS AND MATERIALS • . 12 A. General . 12 B. Carrier Gas System . • . • . • . 12 1. Carrier Gases 12 2. Flow Ra te Control . 16 3. Flow Rate Measurement . 17 4. Circulatory System . 17 c. Sample System . 19 • • • . D. Column Assembly . • 21 1. Column Preparation .•.••.. 21 2. Cooling System .••.• 31 3. Heating System . • . • • . • • . 32 iv CHAPTER PAGE II. (continued) E. Detection System . 33 1. General • • . • • . • . 33 2. Katharometer . • . • . 34 3. Measuring and Record ing Circuit . 36 III. EXPERIMENTAL PROCEDURES AND RESULTS . • . 38 A. Introduction. ....... .· ..••. 38 B. Elution Experiments . • . 39 1. Silica Gel Columns . • . 39 2. Molecular Sieve-5A Columns . 52 3. Charcoal Column . • • . 52 4. Raney Nickel Columns . 52 5. Raney Cobalt Columns . 60 6. Chromia-Alumina Columns ....•. 62 7. Chromia-Flint Quartz Column .•. 70 IV. DISCUSS ION OF THE RESULTS . • . 75 A. Retention Volumes 75 B. Separation Factor .... 77 C. Column Efficiency .•.. 81 . D. Analytical Application .. 83 E. Comparison with Previous Chromatographic Results . 86 v. SUMMARY . 88 BIBLIOGRAPHY . 91 LIST OF TABLES TABLE PAGE I. Percentage Composition of the Hydrogen Isotopes . 48 II . Retention Time for Hydrogen Gas on Raney Cobalt Column ..... 63 III . Isotopic Composition for Equilibrium '. Mixtures of Hydrogen Isotopes • • . • • . 73 IV. Experimental and Theoretical Composition of the Isotope s . 8? LIST OF FIGURES FIGURE PAGE 1. Distr ibution Isotherms and Corresponding Typical Elution Peaks • . 8 2. Func tional Diagram of Gas Chromatography Apparatus Employed with Argon, Helium, and Hydrogen Carriers • . • • . • • . • • 13 3. Photograph of Gas Chromatography Apparatus . • 14 4. Functional Diagram of Gas Chromatography Apparatus Employed with Neon Carrier . • 15 5. Circulatory Pump . 18 6. Pyrex Glass Column Packed with Raney Nickel • . 24 7. Katharome ter Block . • . 35 8. Complete Circuit for Detection System . • . 37 9. Effect of Sample Magnitude on the Shape of Hydrogen Peak . 40 10. Typical Elution Peak for Deuterium with Hyd rogen Carrier on Silica Gel Column . 42 11. Recorder Trace for Hydrogen-Deuterium Sample Passed Through Palladium and Silica Gel Columns • . • . 43 12. Typical Elution Curve for Hydrogen , Deuterium, and Hydrogen Deuteride Sample on Silica Gel Column • 0 • • • • • • • • • • • • • • 44 vii FIGURE PAGE 13 . Calibration Curve for the Determination of Deuterium . • • . • • . 46 14 . Typical Elution Curve for Hydrogen and Deuterium at the Temperature of Boiling MethBile . • . • . • . 49 15. Typical Elution Curve for Hydrogen, Deute­ rium, and Hydrogen Deuteride at the Temperature of Boiling Methane . • . 50 16. Typical Elution Peak for Hydrogen and Deute- rium Sample with Neon Carrier at -161° •. • • 51 17 . Typical Elution Trace with Hydrogen, Deute­ rium, and Hydrogen Deuteride Sample on Charcoal Column . • • . • • . • 53 18 . Typical Recorder Trace for the Elution of Hydrogen or Deuterium from Raney Nickel Column . 55 19 . Elution Peak for Hydrogen-Deuterium Sample after Elevating the Raney Nickel Column Temperature • • • . • . • • • . 56 20. Elution Trace Obtained after Cooling and Reheating the Raney Nickel Column . • . • • . • 58 21. Elution Peak Obtained with Deuterium Sample on 6-ft. Raney Nickel Column . ' . 59 viii FIGURE PAGE 22. Typical Elution Curve for Hydrogen or Deute- rium Sample on Raney Cobalt Column 61 23. Effect of Time between Runs upon the Reten- tion Time of Hydrogen on Raney Cobalt . o • • • 64 24. Typical Elution Curve for Hydrogen Sample on Activated Chromia-Alumina Column . 65 25. Typical Elution Curve for Hydrogen and Deuterium Sample on Partially Poisoned Chromi a-Alumina Column . • . 67 26. Typical Elution Curve for Hydrogen , Hydrogen Deuteride , and Deuterium Sample on Par­ tially Po isoned Ch romia-Alumina Column 68 27. Elution Trace Obtained with Highly Deacti- vated Chr omia-Alumina Column •.•. 69 28 . Typical Elution Curve for Hydrogen , Hydrogen Deuteride , and Deuterium Samp le on Par­ tially Poisoned 8-ft . Chromia-Alumina Column 71 29. Calibration Curves for the Determination of Hydrogen and Deuterium . 72 CHAPTER I INTRODUCTION A. Scope In recent years the gas chromatographic method has found widespread applications, chiefly for analytical pur­ poses. This method is principally employed for the separa­ tion, identification, and quantitative determination of vola­ tile compounds. It is potentially of great value for the quantitative determination of mixtures of the hydrogen iso­ topes. The development of a rapid, convenient, and inexpen­ sive method for the analysis of the hydrogen isotopes would be a valuable addition to many laboratories, especially those where a mass spectrograph is unavailable. This problem was undertaken in an attempt to develop further the chromato­ graphic method for the separation and quantitative determina­ tion of hydrogen and deuterium mixtures. The term "gas chromatography" describes all chromato­ graphic methods in which the moving phase is a gas. The sub­ ject may be subdivided into gas-liquid chromatography and gas-solid chromatography. The former is employed to describe all gas chromatographic methods in which the fixed phase is a liquid, and the latter refers to those methods in which the fixed phase is a solid. 2 The ma jor difference between liquid chromatography and gas chromatography is the nature of the mobile phase . The former employs an incompressible liquid as the mobile phase , but in the latter the mobile phase is a compressible gas. The chromatographic me thods depend on the distribution of the samp le between tw o phases and the subsequent se paration of these two phases. Gas-solid chromatography consists of a solid with a large surface area as a stationary bed , and a gas which percolates through the stationary bed. B o Historical Credit for the introduction of the chromatographic me thod is given to Tswe tt. 1 This investigator employed liquid-solid chromatography for separating components of plant pigments . During the years which followed the original papers, this method went practically unnoticed until Kuhn and Lederer2,3 resolved the carotenes on a pr eparative scale . Li quid-liquid chromatography was introduced by Martin and Synge4 in 194lo Wa ter-saturated silica gel was employed as the stationary phase for separating some amino acids. In the same paper these investigators
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