ZIRCON SUB G8ttingen 7 r Illlllllllll

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1 Reviews in Mineralogy and Geochemistry Volume John M. Hanchar Paul W.O. Hoskin ZIRCON SUB G8ttingen 7 r Illlllllllll L 1Y / 2004 A The George Washington University Washington, D.C. Albert-Ludwigs-Universitat Freiburg Freiburg im Breisgau, Germany Front cover: Cathodoluminescence photomicrograph of zircon crystals from the Old Woman granodiorite, southeastern California. The crystals were mounted in epoxy and polished to reveal interiors of the crystal. The blue-luminescing central regions are inherited Proterozoic cores, and the fine-scale zoned yellow-luminescing rims are magmatic overgrowths of Mesozoic age. Similar zircon crystals from this sample have been dated using the Sensitive High Resolution Ion Micro Probe (SHRIMP) at the Australian National University. Ages of inherited cores range from Ga; magmatic overgrowths are -72 Ma (Foster et al. 1989, Miller et al. 1992). This image was recorded on Kodak Ektachrome 200 film. Conditions used: 12 kv, 0.7 ma with a cold-cathode PATCO ELM-3 Luminoscope; 180 s exposure. The field of view along the width of the photograph is approximately 770 um. Courtesy of J.M. Hanchar (The George Washington University) and C.F. Miller (Vanderbilt University). References: Foster DA, Harrison TM, Miller CF (1989) Age, inheritance, and uplift of the Old Woman-Piute batholith, California, and implications for K-feldspar age spectra. J Geol Miller CF, Hanchar JM, Wooden JL, Bennett VC, Harrison TM, Wark DA, Foster DA (1992) Source regions of a granite batholith: Evidence from lower crustal xenoliths and inherited accessory minerals. Trans Roy Soc Edinburgh: Earth Sci 83: [Also published in Geological Society of America Special Paper 272 (1992)]. Series Editors: PaulH. Ribbe & Jodi Rosso MINERALOGICAL SOCIETY OF AMERICA GEOCHEMICAL SOCIETY

2 Table of Contents Zircon Reviews in Mineralogy and Geochemistry, Vol Structure and Chemistry of Zircon and Zircon-Group Minerals Robert J. Finch, John M. Hanchar INTRODUCTION ; 1 STRUCTURE OF ZIRCON 2 Cation polyhedra 2 Interstitial sites 3 ZIRCON-GROUP MINERALS 4 Silicates 7 Actinide silicates 7 Phosphates 8 Borates 8 Vanadates 8 Arsenates 9 Chromates 10 Related structures 10 STRUCTURAL EFFECTS OF TEMPERATURE, PRESSURE AND COMPOSITION 13 Temperature 13 Pressure 14 Composition 19 ACKNOWLEDGMENTS, 20 REFERENCES 21 2 The Composition of Zircon and Igneous and Metamorphic Petrogenesis Paul W. O. Hoskin, Urs Schaltegger INTRODUCTION.: 27 Analytical techniques 28 ZIRCON AND IGNEOUS PETROGENESIS 29 Saturation, crystallization, occurrences and zoning of igneous zircon 29 Major-element composition of igneous zircon 32 Trace-element composition of igneous zircon 34 Zircon composition and investigations of igneous processes 42 Provenance-indicator studies using igneous zircon composition 43 ZIRCON AND METAMORPHIC PETROGENESIS 45 Textural characterization of metamorphic zircon ; 45 The growth of new zircon during metamorphism and its composition 46 Solid-state recrystallization and dissolution-reprecpitation of protolith zircon and compositional changes 48 HYDROTHERMAL ZIRCON 52 CONCLUSIONS AND OUTLOOK 54 ACKNOWLEDGMENTS 55 REFERENCES, 55 IX

3 3 Melt Inclusions in Zircon J. B. Thomas, R. J. Bodnar, N. Shimizu, C. A. Chesner INTRODUCTION 63 PREVIOUS INVESTIGATIONS 65 METHODOLOGY 66 Petrography of melt inclusions hosted in zircon 67 Heating and homogenization of crystalline melt inclusions in zircon 69 Major and trace element compositions of melt inclusions in zircon 69 DETERMINING ZIRCON/MELT TRACE ELEMENT PARTITION COEFFICIENTS USING MELT INCLUSIONS IN ZIRCON 72 Trace element partitioning data and interpretations 72 Petrogenetic implications 77 Summary of trace element partitioning by the MIM technique 78 ARE MI COMPOSITIONS REPRESENTATIVE OF THE BULK MELT? 79 Boundary layer effects 79 Re-equilibration of melt inclusions 81 Potential errors during homogenization and analysis 82 FUTURE DIRECTIONS 82 ACKNOWLEDGMENTS 83 REFERENCES 83 4 Zircon Saturation Thermometry John M. Hanchar, E. Bruce Watson INTRODUCTION 89 ZIRCON SATURATION THERMOMETRY 90 Historical development 90 APPLICATIONS OF ZIRCON SATURATION THERMOMETRY 96 Background 96 Selected examples of studies that used zircon saturation thermometry 97 CALCULATION OF ZIRCON SATURATION TEMPERATURES 102 Considerations for using zircon saturation thermometry with plutonic rocks 102 Bulk sample or in situ analyses? 103 Calculation of M for geologic samples 104 Worked example to determine M and Zr content and zircon saturation temperature 105 SUMMARY : 109 ACKNOWLEDGMENTS 110 REFERENCES Diffusion in Zircon Daniele J. Cherniak, E. Bruce Watson INTRODUCTION 113 HISTORY A BRIEF REVIEW OF BULK-RELEASE AND EARLY LOWER-RESOLUTION DIFFUSION MEASUREMENTS 113

4 CATIONS 114 Pb 115 Substitutional processes involving Pb 118 Diffusion systematics of trivalent cations 119 Substitutional processes for trivalent cations 122 Tetravalent cations 123 Cation diffusion in zircon a general summary 125 OXYGEN DIFFUSION...~' 126 Experimental results 126 Diffusion mechanisms 128 IMPLICATIONS AND APPLICATIONS OF DIFFUSION FINDINGS 129 Diffusive fractionation 129 Closure temperatures 129 The preservation of zoning in zircon 130 Pbloss 132 Preservation of oxygen isotope signatures Q/16Q retention in zircon cores and rims 135 Retention at rim and core centers during cooling 138 FUTURE DIRECTIONS 139 ACKNOWLEDGMENTS 139 REFERENCES Historical Development of Zircon Geochronology Donald W. Davis, Ian S. Williams, Thomas E. Krogh INTRODUCTION ". 145 PRELUDE.' 146 ISOTOPIC DATING OF ZIRCON 1955 TO ADVANCES IN TECHNIQUE 1973 TO RESOLUTION OF THE PB LOSS PROBLEM 1982 TO THE PRESENT 159 Further advances in ID-TIMS methods 159 The Sensitive High-Resolution Ion Micro-Probe (SHRIMP) 164 The zircon evaporation method 171 Other developments 171 THE LEGACY OF ZIRCON DATING 171 ACKNOWLEDGMENTS 173 REFERENCES Zircon U-Th-Pb Geochronology by Isotope Dilution Thermal Ionization Mass Spectrometry (ID-TIMS) Randall R. Parrish, Stephen R. Noble INTRODUCTION ; 183 METHODS AND DATA PRESENTATION 184 Background 184 Evolution of analytical methods 184 Mass spectrometry 187 XI

5 CATIONS 114 Pb, 115 Substitutional processes involving Pb 118 Diffusion systematics of trivalent cations 119 Substitutional processes for trivalent cations 122 Tetravalent cations 123 Cation diffusion in zircon a general summary 125 OXYGEN DIFFUSION...~ 126 Experimental results 126 Diffusion mechanisms 128 IMPLICATIONS AND APPLICATIONS OF DIFFUSION FINDINGS 129 Diffusive fractionation 129 Closure temperatures 129 The preservation of zoning in zircon 130 Pbloss 132 Preservation of oxygen isotope signatures O/' 6 O retention in zircon cores and rims 135 Retention at rim and core centers during cooling 138 FUTURE DIRECTIONS 139 ACKNOWLEDGMENTS 139 REFERENCES Historical Development of Zircon Geochronology Donald W. Davis, Ian S. Williams, Thomas E. Krogh INTRODUCTION '. 145 PRELUDE.' 146 ISOTOPIC DATING OF ZIRCON 1955 TO ADVANCES IN TECHNIQUE 1973 TO RESOLUTION OF THE PB LOSS PROBLEM 1982 TO THE PRESENT 159 Further advances in ID-TIMS methods 159 The Sensitive High-Resolution Ion Micro-Probe (SHRIMP) 164 The. zircon evaporation method 171 Other developments 171 THE LEGACY OF ZIRCON DATING 171 ACKNOWLEDGMENTS,, 173 REFERENCES Zircon U-Th-Pb Geochronology by Isotope Dilution Thermal Ionization Mass Spectrometry (ID-TIMS) Randall R. Parrish, Stephen R. Noble INTRODUCTION 183 METHODS AND DATA PRESENTATION 184 Background 184 Evolution of analytical methods 184 Mass spectrometry 187 XI

6 Advances in chemical procedures and tracers 187 Standards, reproducibility, corrections, errors, and presentation 190 OTHER METHODS OF ID OR TIMS 191 Pb evaporation (TIMS but no ID) 191 ID-PIMMS (ID but no TIMS) 191 THE MAPPING OF U-TH-PB DATA ONTO DIAGRAMS 192 Age equations 192 Wetherill Concordia diagram 192 Tera-Wasserburg diagram : 194 Isochron diagram 194 The interpreted age of crystallization 194 ZIRCON DATING APPLICATIONS AND U-TH-PB SYSTEMATICS 195 High precision dating of igneous zircon across the scope of geological time 195 Difficulties with igneous U-Pb zircon geochronology 199 Dating of metamorphic zircon 200 Baddeleyite-zircon reactions in coronitic gabbro 200 Growth of zircon in granulites and upper amphibolite facies rocks 200 Metamorphic growth of zircon in amphibolite facies 201 The dating of zircon in eclogite and other UHP rocks 203 Th and Pa chemical partitioning in zircon and its implications 204 Other examples where ID-TIMS data has proved effective 207 SUMMARY 210 ACKNOWLEDGMENTS 210 REFERENCES ; Considerations in Zircon Geochronology by SIMS Trevor R. Ireland, Ian S. Williams INTRODUCTION 215 SELECTED APPLICATIONS 216 Oldest zircon in the solar system 216 Development of fractionated lunar crust 217 The oldest-known terrestrial rocks 218 Detrital-zircon age spectra 218 Analysis of thin rims and near-surface concentration gradients (depth profiles) 219 The youngest zircons.7..'. :. 219 Timescale 219 INSTRUMENTAL AND ANALYTICAL APPROACHES 220 SHRIMP 221 Cameca Operational comparison 222 ZIRCON ANALYSIS, 222 Pb isotopes...; r. 223 Correction for common Pb 224 U/Pb calibration 225 OTHER MINERALS 227 Monazite... ; 227 Xenotime 227 Apatite (+whitlockite) 227 XII

7 Titanite 228 Baddeleyite '. 228 Rutile 228 Perovskite., 228 Allanite * 228 DATA ANALYSIS 229 Analytical uncertainties Pb/ 206 Pb ratio 230. U-Pb ratio 230 Standards.' 231 Data assessment 233 COMPARISON OF DIFFERENT ANALYTICAL SESSIONS 234 FUTURE DEVELOPMENTS 236 ACKNOWLEDGMENTS 238 REFERENCES, Present Trends and the Future of Zircon in Geochronology: Laser Ablation ICPMS Jan Kosler, Paul J. Sylvester INTRODUCTION 243 LASER ABLATION : 244 Laser principles 244 Laser ablation system Interaction of laser radiation with solid samples 246 Choice of laser ablation parameters 247 INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY 249 Inductively coupled plasma as ion source 249 Quadrupole ICPMS 250 Magnetic sector ICPMS 251 Time-of-flight ICPMS 252 Mass discrimination (bias) and fractionation of isotopes and elements 252 DATING OF ZIRCON BY LASER ABLATION ICPMS : 253 Past studies of U-Pb zircon dating by laser ablation ICPMS 254 Elemental fractionation of Pb and U and methods of correction 254 Sampling strategies 256 Spatial resolution 257 Correction for instrument mass bias (standardization) 258 Correction for initial common-pb 260 Precision and accuracy 261 Strategies for data acquisition and reduction 262 LASER ABLATION ICPMS DATING IN PRACTICE 264 Laser ablation ICPMS dating of zircon for sedimentary provenance studies 264 Dating magmatic events by laser ablation ICPMS 265 Application of laser ablation ICPMS to fission track dating of zircon 266 In situ dating of accessory minerals by laser ablation ICPMS 268 FUTURE PROSPECTS OF LASER ABLATION ICPMS DATING 269 Quadrupole vs. magnetic sector and single- vs. multi-collector comparisons 270 New applications in laser ablation ICPMS dating of zircon 271 XIII

8 Titanite 228 Baddeleyite 228 Rutile 228 Perovskite..., 228 Allanite?. 228 DATA ANALYSIS 229 Analytical uncertainties ; Pb/ 206 Pb ratio 230 U-Pb ratio 230 Standards.' 231 Data assessment 233 COMPARISON OF DIFFERENT ANALYTICAL SESSIONS 234 FUTURE DEVELOPMENTS 236 ACKNOWLEDGMENTS ; 238 REFERENCES ; Present Trends and the Future of Zircon in Geochronology: Laser Ablation ICPMS Jan Kosler, Paul J. Sylvester INTRODUCTION 243 LASER ABLATION 244 Laser principles 244 Laser ablation system Interaction of laser radiation with solid samples 246 Choice of laser ablation parameters : INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY 249 Inductively coupled plasma as ion source.249 Quadrupole ICPMS 250 Magnetic sector ICPMS 251 Time-of-flight ICPMS 252 Mass discrimination (bias) and fractionation of isotopes and elements 252 DATING OF ZIRCON BY LASER ABLATION ICPMS 253 Past studies of U-Pb zircon dating by laser ablation ICPMS 254 Elemental fractionation of Pb and U and methods of correction 254 Sampling strategies 256 Spatial resolution 257 Correction for instrument mass bias (standardization) 258 Correction for initial common-pb 260 Precision and accuracy 261 Strategies for data acquisition and reduction 262 LASER ABLATION ICPMS DATING IN PRACTICE 264 Laser ablation ICPMS dating of zircon for sedimentary provenance studies 264 Dating magmatic events by laser ablation ICPMS 265 Application of laser ablation ICPMS to fission track dating of zircon 266 In situ dating of accessory minerals by laser ablation ICPMS 268 FUTURE PROSPECTS OF LASER ABLATION ICPMS DATING 269 Quadrupole vs. magnetic sector and single- vs. multi-collector comparisons 270 New applications in laser ablation ICPMS dating of zircon 271 XIII

9 ACKNOWLEDGMENTS ; 271 REFERENCES Detrital Zircon Analysis of the Sedimentary Record Christopher M. Fedo, Keith N. Sircombe, Robert H. Rainbird INTRODUCTION 277 STATISTICS AND METHODOLOGY OF SAMPLING 278 Sampling 278 Sample preparation 279 Analysis 280 Data display 281 Interpretation. 282 AGE OF STRATIGRAPHIC SUCCESSIONS 284 Maximum age and age bracketing 284 Direct depositional ages 286 Disconformity recognition 287 PROVENANCE ANALYSIS 288 Petrographic and petrologic 288 Geochemistry 288 Fission track (FT) 289 Geochronology 289 PALEOGEOGRAPHIC AND TECTONIC RECONSTRUCTIONS 293 Introduction 293 Initial studies Shaler Supergroup 294 Regional studies northern Cordillera 294 Regional studies central Cordillera 294 Siberia 295 Scotland.' 295 A cryptic Grenvillian foreland basin in the U.S. mid-continent 296 Rodinian paleogeography 296 IMPLICATIONS FOR EARLIEST EARTH HISTORY 297 SUMMARY '..'. 297 ACKNOWLEDGMENTS 298 REFERENCES High-Precision U-Pb Zircon Geochronology and the Stratigraphic Record Samuel A. Bowring, Mark D. Schmitz INTRODUCTION 305 THE GEOLOGIC'TIME SCALE 307 Proxies for radiometric geochronology: chemostratigraphy 307 GEOCHRONOLOGICAL TECHNIQUES 308 Measurement uncertainty 310 Common Pb correction.:? 311 Tracer calibration and interlaboratory comparison 312 U decay constants 312 XIV

10 INTERMEDIATE DAUGHTER PRODUCT DISEQUILIBRIA 313 GEOLOGICAL COMPLEXITY AND OPEN SYSTEM BEHAVIOR 313 Crystal inheritance and Pb-loss 313 Resolving a geological "age" from a large population of zircon dates 314 Sample selection and analytical strategies THE NEOPROTEROZOIC-CAMBRIAN TRANSITION 316 Triassic-Jurassic boundary 318 THE END-PERMIAN EXTINCTION 320 SUMMARY ; 322 ACKNOWLEDGMENTS 323 REFERENCES Lu-Hf and Sm-Nd isotope systems in zircon Peter D. Kinny, Roland Maas INTRODUCTION 327 THE Lu-Hf ISOTOPE SYSTEM IN NATURE 327 Hafnium as a geochemical tracer 328 HF ISOTOPES IN ZIRCON '. 329 Measurement techniques 331 Studies of magmatic zircons 331 Studies of detrital zircon 332 Studies of metamorphic zircon 334 Studies of mantle zircons 334 Concluding remarks: Lu-Hf isotopes and zircon 335 Sm-Nd ISOTOPE STUDIES OF ZIRCON '. 335 REE patterns of zircon 336 Sm-Nd mineral dating of zircon 336 Inherited Nd 338 Concluding remarks: Sm-Nd isotopes and zircon 338 OUTLOOK 339 ACKNOWLEDGMENTS 339 REFERENCES Oxygen Isotopes in Zircon John W. Valley INTRODUCTION 343 ANALYSIS OF 5 18 O IN ZIRCON 343 Laser fluorination 343 Ion microprobe 343 Standards 344 ZIRCON SAMPLE PREPARATION 345 Mechanical separation of zircons 346 Selection of zircons 346 Imaging zircons 348 OXYGEN ISOTOPE FRACTIONATION IN ZIRCON. 348 OXYGEN DIFFUSION RATE IN ZIRCON 349 ASSIMILATION VS. FRACTIONAL CRYSTALLIZATION 352 XV

11 MANTLE ZIRCONS 354 PRE-CAMBRIAN ZIRCONS, 355 Archean granitoids 355 Volcanogenic massive sulfide deposits 357 Hadean detrital zircons 358 Mid-Proterozoic 359 CRUSTAL GROWTH AND MATURATION 363 Superior vs. Grenville province : 363 Evolution of magmatic 8 18 O through time 364 ULTRA-HIGH PRESSURE ECLOGITES, DABIE AND SULU 365 FELSIC. VOLCANISM, WESTERN UNITED STATES 365 Low S 18 O-rhyolites, Yellowstone 365 Timber Mountain / Oasis Valley Caldera Complex 368 Bishop Tuff, Long Valley caldera 370 PHANEROZOIC GRANITES 371 British Tertiary Igneous Province 371 Mesozoic and Cenozoic granites of the western United States 374 A-type granites, northeastern China 377 Cenozoic granitoids of the Antarctic Peninsula 377 Fe-oxide melt in syenitic xenoliths 378 Magmatic epidote-bearing granitoids 378 ACKNOWLEDGMENTS 380 REFERENCES Radiation Effects in Zircon Rodney C. Ewing, Alkiviathes Meldrum, LuMin Wang, William J. Weber, L. Rene Corrales INTRODUCTION 387 EXPERIMENTAL RESULTS 389 Bulk properties 390 Long range order 392 Short-range order : 398 Recovery of radiation damage ; 400 MODELS OF DAMAGE ACCUMULATION 405 Temperature "' Ion mass'and energy 410 COMPUTER SIMULATION OF DEFECT FORMATION AND RADIATION DAMAGE 411 Intrinsic and extrinsic defect energies 412 Threshold displacement energies 413 Collision cascades '. 414 UNRESOLVED RESEARCH ISSUES 418 ACKNOWLEDGMENTS 420 REFERENCES : 420 XVI

12 15 Spectroscopic methods applied to zircon Lutz Nasdala, Ming Zhang, Ulf Kempe, Gerard Panczer, Michael Gaft, Michael Andrut, Michael Plotze INTRODUCTION 427 LUMINESCENCE SPECTROSCOPY OF ZIRCON 428 Cathodoluminescence of zircon 428 Laser-induced time-resolved photoluminescence of zircon 435 VIBRATIONAL SPECTROSCOPY OF ZIRCON 438 Infrared absorption spectroscopy of zircon 438 Raman spectroscopy of zircon 443 OTHER SPECTROSCOPIC TECHNIQUES 449 Electronic absorption spectroscopy 449 Mbssbauer spectroscopy 455 Electron paramagnetic resonance 455 Other spectroscopic methods 459 ACKNOWLEDGMENTS 460 REFERENCES Atlas of Zircon Textures Fernando Corfu, John M. Hanchar, Paul W.O. Hoskin, Peter Kinny INTRODUCTION 469 ZIRCON IMAGING 470 MORPHOLOGY OF ZIRCON 472 ZONING TEXTURES IN IGNEOUS ZIRCON 476 XENOCRYSTIC CORES 478 SUBSOLIDUS MODIFICATIONS AND GROWTH OF ZIRCON 480 Late-magmatic phenomena 480 Medium to high temperature metamorphism 481 High-pressure metamorphism :. 486 HYDROTHERMAL ZIRCON 487 KIMBERLITIC AND MANTLE-RELATED ZIRCON 488 IMPACT-RELATED TEXTURES 489 FRACTURING 489 ALTERATION 491 INCLUSIONS, INTERGROWTHS AND OVERGROWTHS OF ZIRCON AND OTHER MINERALS 493 CONCLUDING REMARKS 494 ACKNOWLEDGMENTS 495 REFERENCES 495 XVII

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