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TRITIUM ANALYSIS of SEAWATER. TRESIS Submitted for the Degree,Of TRITIUM ANALYSIS OF SEAWATER. TRESIS submitted for the degree,of DOCTOR OF PHILOSOPHY of the UNIVERSITY OF GLASGOW by H. MARK BLAUER Chemistry Department May, 1977 ProQuest Number: 13804114 All rights reserved INFORMATION TO ALL USERS The quality of this reproduction is dependent upon the quality of the copy submitted. In the unlikely event that the author did not send a com plete manuscript and there are missing pages, these will be noted. Also, if material had to be removed, a note will indicate the deletion. uest ProQuest 13804114 Published by ProQuest LLC(2018). Copyright of the Dissertation is held by the Author. All rights reserved. This work is protected against unauthorized copying under Title 17, United States C ode Microform Edition © ProQuest LLC. ProQuest LLC. 789 East Eisenhower Parkway P.O. Box 1346 Ann Arbor, Ml 48106- 1346 ACKNOWLEDGEMENTS'. The author is indebted to the Natural Environmental Research Council for financial support throughout this research project and to the University of Glasgow for laboratory and support facilities. Thanks are extended to A. Anderson and his staff for design and construction of the Constant Current Density Unit and maintenance of all electronic equipment; to A. Hislop and his staff for construction of the reaction vessels and other equipment; and to J. Connelly and his staff for glassblowing. Appreciation is extended to the crew of the U.S.N.S. Bartlett, Drs. W.S. Moore, M.S. Baxter and A.E. Fallick for collection of eastern tropical Pacific Ocean samples and supplementary hydrographic data. The same is extended to the crew of the U.S.N.S. Eltanin (Cruise 47) and Dr. J.M. Edmond for the Antarctic samples. The Inter­ national Atomic Energy Agency and Dr. C.B. Taylor supplied tritium standards and intercalibration facilities. The expertise of A. Ritchie for mass-spectrometric measurements of D/H ratios and the extended collection of tritium results by K. McKay are acknowledged. Thanks are also due to. Drs. A.E. Fallick and A.B. Mackenzie and Messrs. D. Swan and J. Campbell for providing the opportunity for many frank and illuminating discussions in the best of Scottish tradition. Appreciation for final preparation of this manuscri is extended to Messrs. C. Stuart, C, Cook s.nd M. Gray, and most especially to Miss.T. Collins. The author is especially grateful to Dr. M.S. Baxte for his diligent supervision, guidance and constructive criticism throughout the period of research. Without hi assistance this thesis would never have been possible. TABLE OF CONTENTS. Page. CHAPTER. I. INTRODUCTION . 1.1 Prolegomena ........... 1 1.2 Properties of tritium and tritium oxide .......................... 3 1.3^ Sources of tritium ............ 3 1.4 Tritium in the ocean .......... 10 1.5 Aims of research ..... 23 CHAPTER II. SAMPLING AND ANALYTICAL PROCEDURE II.1 Introduction .................. 25 .11.2 Methods of measurement of tritium 25 II. 3 Sampling ....................... 31 11.4 Distillation ................... 35 11.5 Electrolytic enrichment ....... 35 11.6 Methane synthesis ............. 47 11.7 Gas storage and counter filling sections ....................... 68 II. 8 Tritium counting system ....... 70 II.9 Counter characteristics ..... 76 CHAPTER III. CALIBRATION AND STANDARDISATION III.l Contamination and hlank values.. 88 III. 2 Storage ..... 106 III. 3 Enrichment factors .. 107 CHAPTER IV. DISCUSSION OF EASTERN TROPICAL PACIFIC OCEAN DATA IV. 1 Introduction ................... 123 IV.2 General oceanography ......... 125 IV. 3 Hydrographic features ..... 134 IV.4 Tritium features .............. 161 % IV.5 Summary ............... 181 TABLE OF CONTENTS (continued). Page. CHAPTER V. MEASUREMENTS FROM ANTARTIC. WATERS V.l Introduction ........ 184 V.2 General oceanography .......... 185 V.3 Hydrographic features ...... 194 ♦ .V.4 Tritium features ..... 206 APPENDIX 1 212 APPENDIX 2 ...... 213 APPENDIX 3 ... ... 214 REFERENCES 221 LIST OF FIONRES. Page. Cumulative tritium inventory . 8 11*1 Flow diagram for tritium assay 32 II-2 Atmospheric moisture condenser 33 II. 3. Distillation apparatus ..... 36 II-4 . Electrolysis cell and electrodes 37 II-5 Reservoir and feeding system ... 40 II.6 Probe placement versus current density in main electrodes ..... 43 II. 7 Perspex holding cage ........... 44 II;8 Current density, amperage and volume reduction versus electrolysis time ..... ;.................... 46 11.9 Distillation ampoule .......... 48 11.10 Final distillation apparatus ... 49 11.11 Flow system for methane synthesis 54 11.12 Vacuum line for routine methane purification ................... 56 11.13 Cross-section of reaction Vessel 37 11.14 Counter filling section ....... 65 11.15 ; Histogram of methane synthesis yields versus frequency ....... 66 11.16 Block diagram of counting electronics 72 11.17 Cross section of detector ...... 73 II.18A Background count rate versus external Cs-137 ratios .................. 79 II.18B Figure of merit versus external Cs- 137 ratios ..................... 80 II.18C Counting efficiency versus external Cs-137 ratios .......... 81 11.19 Plateaux of detector and guard .. 83 11.20 Distribution of counting rates in net a and net 6 channels 85 11.21 Pressure versus background count rates ............ '............... LIST OF FIGURES (continued.) Page. .111.1 Inert atmosphere dry box. ...... 91 111.2 Blank count rates during concurrent syntheses ....................... .95 111.3 Outgassing rate versus time .... 98 III. 4 Electrolytic enrichment curve .. 115 111.5 Electrolytic calibration curve . 117 111.6 Theoretical tritium recovery curve 119 IV.1 Station locations in eastern tropical Pacific Ocean ......... 124 IV.2 Surface currents of the Pacific ' _ Ocean ........................... 129 IV.3 Salinity versus depth at eastern tropical Pacific stations ..... 148 IV.4 Dissolved oxygen versus depth at eastern tropical Pacific Stations ........................ 149 IV.5 Temperature versus depth at eastern tropical Pacific Stations ..... 150 IV.6 Subsurface salinity profile ... at eastern tropical Pacific I . Stations ......................... 152 IV.7 , Subsurface temperature profile at eastern tropical Pacific Stations 153 IV.8 Subsurface dissolved oxygen profile for eastern tropical Pacific Stations 154 IV.9 Entire plot 0 -S for eastern tropical Pacific Stations ............... 156 IV.10 Q -S plot for eastern tropical Pacific deep water ............. 157 IV.11 0 -S for Bartlett Stations deep water .............. 160 IV.12 Potential temperature versus dissolved oxygen for Bartlett Stations deep water ............ 162 IV.13 South Tow tritium profiles .... 164 LIST ( FIGURES (continued,) Page. IV.14 . Tritium concentration versus depth for Bartlett Stations "3 and 12 ................. 166 IV.15 Tritium concentration along a surface of 25 168 IV.16 Tritium concentration along a surface of 26 ;.. 169 IV.17 Tritium concentration along a surface of 27 170 IV.18 Surface tritium concentrations in eastern tropical Pacific Ocean 172 IV.19 Average tritium distribution in surface seawater of the Pacific Ocean ....................... 173 IV.20 Temperature gradient versus tem­ perature for Bartlett Stations 3,5,7 and 9 174 IV.21 Approximate exponential subrange for Bartlett Stations 3,5,7 and 9 175 V.l Southern Ocean - surface circu­ lation and mean positions of the Antarctic and Subtropical Convergences 188 V.2 Schematic of vertical components of the circulation in the Southern Ocean and prominent hydrographic features 190 V.3 Temperature versus depth at Cruise 47 stations .................... 197 V.4 Salinity versus depth at Cruise 47 stations ......... 198 V.5 Dissolved oxygen distribution at Cruise 47 stations ............. 199 V.6 0 -S plot for complete water column 203 V.7 Subsurface ®-S plot of Cruise 47 stations ............ 204 V.8 0-S plot for Deep and Bottom Water 205 V.9 Surface tritium concentrations in T , U .......................... 209 V.10 Depth-tritium profiles at four Southern Latitudes ............ 210 LIST OF TABLES. Page. 1.1 Natural distribution of tritium 5 1.2 Thermonuclear energy yields of atmospheric tests in megatons .. 6 11.1 Ampoule vapour.losses-final distillation ; . 50 11.2 Comparison of volume reduction factors ................. 50 11.3 Gasket material - associated blank count rate .................... 59 11.4 Methane purification test - per­ centage recovery .............. 64 * II.5 Memory effect - reaction-vessels • 67 11.6 Determination c-f the presence of short-lived radionuclides ..... 69 11.7 Determination of the figure of merit .......................... 78 111.1 Background levels of tritium ... 89 111.2 Initial period blank determinations ~concurrent syntheses ........... 93 111.3 Final period blank determinations 94 111.4 Bakeout times for 2mm thick sheet steel .......................... 101 111.5 Outgassing rates for various metals 103 111.6 Measurement of the blank counting rate contamination throughout analytical procedure . .......... 105 111.7 Mass-spectrometry calibration for D/H measurement ........ Ill 111.8 Calibration of tritium enrichment and determination of the apparent fractionation factors ........ 114 111.9 Reproducibility - tritium recovery between cells ................. 120 III. 10 Tritium recovery between method:' 121 IV.1 Location of eastern tropical 'Pacific oceanographic stations . 136 LIST OF TABLES (continued.) Page. IV.2 Hydrographic properties at Bartlett Station 3 .... 137 IV. 3 Hydrographic properties at Bartlett Station 5 .... 138 IV.4 Hydrographic properties at • Bartlett Station 7 ...,. 139
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