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Imploveients in METHODS of EXTRACTION, PURIFICATION, A1D 1ASUREIENT of EADIO

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Imploveients in METHODS of EXTRACTION, PURIFICATION, A1D 1ASUREIENT of EADIO IMPLOVEiENTS IN METHODS OF EXTRACTION, PURIFICATION, A1D 1ASUREIENT OF EADIO GENIC ARGON IN MINEAiLS by LAWRENCE STRICKLLND S.B., Massachusetts Institute of Technology (1952) SUBMITTED IN PARTIAL FULFILLIENT OF THE REQUIREIENTS FOR THE DEGREE OF DOCTOR OF PHILOSOPHY at the MASSACHUSETTS INSTITUTE OF TECHNOLOGY June, 1956 Signature of Author. ...... *0.-.. *a *.. , .... Department 4f Geology and Geophysics / X, Of .I Septe;nber p3, 1955 Certified Thepc SupgrvAsor Accepted by.\......... 4.................. .... Chairman, Departmental Committee on Gradua Students -Ming== A CINOWLEDGEMvENTS The author is indebted to the many people who helped in the completion of this research. He wishes to thank Dr. Leonard Herzog, who was always available for consultation when problems arose involving mass spectrometry and who was an invaluable help in the early stages of this re- search. Professor Patrick Hurley, who suggested the author undertake this research and who was always willing to take time from his busy schedule to help. He was a source of inspiration whenever forward progress was slow. The author will remember his association with Professor Hurley for many years. Mr. Milo Backus, whose companion- ship made the many hours spent on this research seem short. The typist, Joan Whitehouse, for her untiring efforts to complete this manuscriot in a tight schedule. His wife, Shirley, without her unlimited confidence in the author, and unselfish devotion, the successful completion of this research would have been impossible. The entire staff of the Geology Department. The research presented in this thesis was a part of a program supported by the Atomic Energy Commission urAer Contract AT(30-1)-1381. ABSTRACT Title: Improvements in methods of extraction, purification, and measurement of radio genic argon in minerals. Author: Lawrence Strickland Submitted in partial fulfillment of the requirements of the degree of Doctor of Philosophy at Massachu- setts Institute of Technology Age measurements by the A 40 /K4 0 method have shown promising results in recent tests. It is important that the possibility of small errors in analysis be investigated and that the techniques of analysis be simplified and shortened. In this investigation new instruments and facilities were constructed and tested to these ends. It was planned that isotope dilution analysis would be used to monitor experiments leading toward a possible re- liable volumetric method of analysis. For this purpose a mass spectrometer was constructed, after Nier's design, with a 60 magnet sector and 6 inch radius, and with changes made in the method of collection and measurement. The method of measuring the isotopes of argon was a dynamic one, in order to allow most of the sample to be used during an analysis. Molecular flow conditions exist throughout the entire gas-flow sheet. The isotope ratios measured at time intervals were then extrapolated to the time the sample started to flow into the ionization chamber. Experimentation showed that argon could be lost if the sample was absorbed on charcoal at too low temoeratures for too long a time. It was also found that quantities of gas containing argon c8uld be purified by selective adsorption on charcoal at -78 c. The mass spectrometric procedures were checked for discriminatio]0and reproducibility by measuring the atmos- pheric argon ratio and the radiogenic argon content of a sample of llpidolite of known age. Results of these tests were as follows: A T1OSPHERIC 36 ARGON 40 / Fractionation and (measured) Nier (1950) Discrimination 310 2 96+l 1.047 311 1.050 308 1.042 or approximately 2 percent discrimination per mass unit. This value is different for each spectrometer. The value obtained is reasonable. LEPIDOLITE SAIIPLE A4 0 / gm sample (x103 cm3 ) age (m. y. ) .79 + .08 This work Aldrich (1954) .74 + .03 1710 + 90 1610 .73 + .03 The volumetric analysis apparatus was checked by analyzing air for its argon content with .993 percent, .990 percent, and .992 percent the values obtained. This is to be comoared with a value of .993 percent obtained by Paneth. 'BLE OF CONTENTS .page Acknowledgements......*00 ............ * ......... 00 Abstract.......................... * ** o.*eoo .0 000 ...... 0 i11 Section I. Introduction.................0.0......00.0. 1 Methods of Determining Geologic Age Lead Strontium-Rubidium Argon-Potassium Comparison of age Methods Research Problems Section II. Mass Spectrometer........................... 7 Introduction Isotope Analysis of Argon Theory of Mass Spectrometer Refocusing of Divergent Beams Causes of Ion Beam Spread Resolution Physical Arrangement of the Equipment Section III. Vacuum Techniques and Gas Flow Conditions in the Mass Spectrometer.................. 45 Introduction Gas Flow Through the Mass Spectrometer Cold Traps Background Mass Spectre Gas Flow into the Mass Soectrometer Section IV. Production of Positive Ions................ 59 Introduction Methods and Workmanship The Orthodox Source Mass Discrimination of Ion Source Emission Regulator Sensitivity Stability Section V. Collection and Measurement of Ion Beams..... 70 Collector Design Preamxolifier D-C Current Amplifier Measurement of Ion Beams Treatment of Data Section VI. Isotope Dilution Techniques................ 77 Tracer Introduction System Calibration of the Tracer Possible Errors in Tracer Calibration Isotope Dilution Measurements Possible Errors in the Determination of Radiogenic Argon Section VII. Volumetric Analysis of Argon.............. 85 Introduction Separation Procedure (Introductory Remarks) Description of Equipment Calibration of Volumes Problems to be Solved Loss of Argon Extraction of Small Quantities of Argon from Min- erals Atmospheric Argon Contamination Hydrogen Removal Operation of the Barium Furnace Gas Circulation System Results of Volumetric Analyses Section VIII. Standardized Procedures.................. 104 Volumetric-Analysis Isotope Dilution Analysis Section IX.Measurement of Age by the Potassium-Argon Method................. .......... ... .. *. 110 Section X. Recommendations for Future Research......... 115 Appendix I. Use of Radio Frequency Induction Heater Appendix II. Condensed Procedure Sheet Biographical Sketch I __:i LIST OF ILLUSTRATIONS Figure 1. Refocusing properties of magnet sector. 11. 2. Effect on refocusing by shifting magnet .1 inch upward from correct position. 13. 3. Effect on refocusing by shifting magnet .2 inch down and .1 inch towards source from correct oosition. 14. 4. Bean spread due to various aberrations. 17. 5. Gas inlet system. 19. 6. Magnet poles. 21. 7. Right side view of mass spectrometer. 23. 8. Left side view of mass spectrometer. 24. 9. Schematic diagram of high voltage supply . 25. 10. Front panel view of high voltage supply. 2. 11. Bottom view of high voltage supply. 27. 12. Rear view of high voltage supply. 28. 13. Schematic diagram of ion current amplifier. 29. 14. Front panel view of ion current amolifier. 30. 15. Bottom view of ion current amplifier. 31. 16. Rear view of ion current amplifier. 32. 17. Schematic diagram of magnet current supply. 33. 18. Schematic diagram of balancing panel. 34. 19. Front panel view of balancing panel. 35. 20. Rear view of balancing panel. 36. 21. Schematic diagram of regulated D.C. power supply. 37. 22. Front panel view of regulated D.C. power supply. 38. Figure 23. Bottom view of regulated D.C. power supply. 319. 24. Rear view of regulated D.C. power supply. 40, 25. Schematic diagram of emission regulator. 41. 26. Front panel view of emission regulator. 42. 27. Rear view of emission regulator. 43. 28. Diagram of mass spectrometer tube. 44. 29. Schematic diagram of mass spectrometer with possible appropriate pressures. 47, 30. Residual spectra using solid carbon dioxide as coolant. 50. 31. Residual spectra using liquid nitrogen as coolant. 51. 32. Increase of background spectra with time. 52. 33. Variation in 4 ratio with time. 56. 40 34. Variation in 40 ratio with time. 57. 35. Schematic diagram of ion source. 61. 36. Schematic diagram of electron gun. 66. 37. Schematic diagram of ion gun. 67. 38. Peak height vs. electron accelerating voltage. 69. 39. Design of collector. 72. 40. Characteristics of CK5886 tube. 75. 41. Typical recorded ion beams. 76. 42. Percent error in Qh for 1 percent error in Rmn. 83. 43. Furnace for extraction of gases. 87. Figure 44. Gas separation system. 89. 45. Adsorption of argon on charcoal at liquid nitrogen temperature. 93. 46. Clean up of sma 1 quantities o gas in presence of 1.20 x 10-3 and cm argon. 100. 40 47. Decay scheme of K . 112. LIST OF TABLES Table Ak Comparison of Argon ratios (mass discrimination) 64. Table B Calibration of spike 79. Table C Percent error in volume of pure tracer determined per E percent error in ratio or quantity 79. Table D Percent error in the determination of radio- genic argon for a given percent error in ratio and quantity 81. Table E Results of volumetric analysis 103. Table F Branching ratio 111. Table G Comparison of ages 113. Section I INTRODUCTION It was the purpose of this research to construct and calibrate equipment and techniques for the extraction and quantitative separation and isotopic measurement of the argon from potassium bearing minerals, the ultimate objective being to contribute data toward the establishment of the potassium-argon method of age determination. It was also the purpose of this research to determine if it is possible to make contamination-free volumetric analysis of argon in min- erals. The section that follows will acquaint the reader with the recent developments which prompted the present research, and will present an introductory statement of the research problems. Methods of Determining the Geological Age of Rocks and Minerals Natural radioactivities have provided a means of studying absolute time in earth history. The more important of these are the breakdowns of 28 25 232 87 40 U2 3 8 , U , Th23, Rb and K Several excellent reviews of the methods of age determination have appeared in recent years. A detailed account of the historical develop- ment of the potassium-argon decay has been published in a paper by Birch (1951), while Faul (1954) has an excellent review of all methods of age determination.
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