Abstract
The internal precision of Pb isotope analyses using single-zircon evaporation in a double-filament solid source mass spectrometer (Kober 1986) can be improved combining the evaporation of Pb directly from the single grain with a suitable Pb+ emitter-bedding technique. This is most easily done by step-wise evaporating the investigated grain at temperatures of 1700–1800 K generating on the ‘cold’ ionization filament a deposit of radiogenic Pb together with further elements and compounds derived directly from the crystal. The heating of the deposit on the ionization filament to 1400–1500 K results in long-lived and stable Pb+ ion beams. The ‘activating reagents’ in the deposit are HfO2 and SiO2. Their release from the zircon grain together with the radiogenic Pb, which presumably is sited in the crystalline zircon domains as Pb4+, is probably due to disintegration reactions of trace-element silicates hosted in the grain.
In the bedding deposited on the ionization filament thermally stable Pb/Hf/SiO2 compounds are formed (PbHfSiO5(?)). They retain the Pb isotopes on the (Re) filament up to 1400 K–1500 K and are highly efficient Pb+ ion emitters similar to the ‘Si-gel’-method (Cameron et al. 1969).
The combined evaporation/emitter-bedding technique has been applied to natural zircons of different genesis and to isotope standards. Routinely, a Pb+ ion yield of 2*10−4-1*10−3 and a relative standard deviation of the 207Pb/206Pb ratio in the order of 1% have been obtained for sub-ng- to ng-amounts of Pb from standards and samples. The method rapidly can yield Pb isotope information on the ‘concordant’ zircon phases with a standard deviation of ±15–20 Ma of the derived ages also in the case of Paleozoic zircon populations.
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References
Akhmanova MV, Leonova LL (1961) Investigation of metamictization of zircons with the aid of infrared absorption spectra. Geochem Int, pp 416–431
Akishin PA, Nikitin OT, Panchenkov GM (1957) A new effective ion emitter for the isotopic lead analysis. Geochem Int, pp 500–505
Butterman WC, Foster WR (1967) Zircon stability and the ZrO2-SiO2 phase diagram. Am Mineralogist 52:880–885
Cameron AE, Smith DE, Walker RL (1969) Mass spectrometry of nanogram size samples of lead. Anal Chem 41:525–526
Catanzaro EJ, Murphy TJ, Shields WR, Garner EL (1968) Absolute isotopic abundance ratios of common, equal-atom and radiogenic lead isotope standards. J Res NBS A 72:261–267
Chukhonin AP (1978) A mass spectrometric study of the forms taken by lead in zircon. Geochim Int 15:186–189
Compston W, Williams IS, Meyer C (1984) U-Pb geochronology of zircons from lunar breccia 73217 using a sensitive high massresolution ion microprobe. J Geophys Res Suppl 89:B525-B534
Curtis CE, Sowman HG (1953) Investigation of the thermal dissociation, reassociation, and synthesis of zircon. J Am Ceram Soc 36:190–198
Drach V von (1978) Mineralalter im Schwarzwald. Unpubl thesis, Heidelberg
Fleischer M (1955) Hf content and Hf-Zr ratio in minerals and rocks. US Geol Survey Bull 1021A:1–13
Froude DO, Ireland TR, Kinny PD, Williams IS, Compston W (1983) Ion microprobe identification of 4100–4200 Myr old terrestrial zircons. Nature 304:616–618
Gentry RV, Sworski TJ, McKown HS, Smith DH, Eby RE, Christie WH (1982) Differential lead retention in zircons: implications for nuclear waste containment. Science 216:296–297
Görz H (1974) Microprobe studies of inclusions in zircons and compilation of minor and trace elements from the literature. Chem Erde 33:326–357
Gottfried D, Senftle FE, Waring CL (1956) Age determination of zircon crystals from Ceylon. Am Mineral 41:157–161
Henderson GH, Bateson S (1934) A quantitative study of pleochroitic haloes. 1st Proc R Soc London Ser A 145:563–581
Hinthorne JR, Anderson CA, Conrad RL, Lovering JF (1979) Single-grain 207Pb/206Pb and U/Pb age determinations with a 10 μm spatial resolution using the ion microprobe mass analyser (IMMA). Chem Geol 25:271–303
Hofmann A, Köhler H (1973) Whole rock Rb-Sr ages of anatectic gneisses from the Schwarzwald, SW-Germany. N Jahrb Mineral Abh 119:163–187
Hoppe G (1963) Die Verwendbarkeit morphologischer Erscheinungen an akzessorischen Zirkonen für petrologische Auswertungen. Abh Dtsch Akad Wiss Berlin 1
Kober B (1985) Radiogenblei-Evaporation aus Zirkon-Einzelkristallen in einer Zweiband-Thermionenquelle zur Bestimmung von 207Pb/206Pb-Altern. Fortschr Mineral 63:117
Kober B (1986) Whole-grain evaporation for 207Pb/206Pb-age investigations on single zircons using a double-filament thermal ion source. Contrib Mineral Petrol 93:482–490
Kober B, Hradetzky H, Lippolt HJ (1986) Radiogenblei-Evaporationsstudien an einzelnen Zirkonkristallen zur präherzynischen Entwicklung des Grundgebirges im Zentralschwarzwald, SWDeutschland. Fortschr Mineral 64:81
Köhler H (1970) Die Änderung der Zirkonmorphologie mit dem Differentiationsgrad eines Granits. N Jahrb Mineral Mh 9:405–420
Köppel V (1974) Isotopic U-Pb ages of monazites and zircons from the crust-mantle transition and adjacent units of the Ivrea and Ceneri zones (Southern Alps, Italy). Contrib Mineral Petrol 43:55–70
Köppel V, Sommerauer J (1974) Trace elements and the behaviour of the U-Pb system in inherited and newly formed zircons. Contrib Mineral Petrol 43:71–82
Kosztolanyi C (1965) Nouvelle methode d'analyse isotopique des zircons a l'etat naturel apres attaque directe sur le filament. C R Acad Sci 261:5849–5851
Krasnobayev AA, Polezhayev YM, Yunikov BA, Novoselov BK (1974) Genetic nature of metamict zircon. Geochim Int 9:195–207
Krogh TE (1973) A low-contamination method for hydrothermal decomposition of zircon and extraction of U and Pb for isotopic age determinations. Geochim Cosmochim Acta 37:485–494
Krogh TE (1982) Improved accuracy of U-Pb zircon ages by the creation of more concordant systems using air abrasion technique. Geochim Cosmochim Acta 46:637–649
Lancelot J, Vitrac A, Allegre CJ (1976) Uranium and lead isotope dating with grain by grain zircon analysis: a study of complex geological history with a single rock. Earth Planet Sci Lett 29:357–366
Levskiy LK, Murin AN, Zaslavskiy VG (1969) Use of thermionic emission in isotope analysis of lead and lithium. Geochem Int 6:601–605
Lipova IM, Mayeva MM (1971) The relation of Zr/Hf ratio in zircon to crystal morphology. Geochem Int 8:785–791
Lipova IM, Kuznetsova GA, Makarov ES (1965) An investigation of the metamict state in zircons and cyrtolites. Geochem Int 2:513–525
Nekrasova RA, Rozhdestvenskaya IV (1970) The ZrO2/HfO2 ratio in zircons from kimberlites and alluvial sediments. Geochem Int 7:536–543
Oosthuyzen EJ, Burger AJ (1973) The suitability of apatite as an age indicator by the uranium-lead method. Earth Planet Sci Lett 18:29–36
Pavlenko AS, Vainshtein EE, Shevaleevskii ID (1957) On the Hafnium-Zirkonium ratio in zircon of igneous and metasomatic rocks. Geochem Int, pp 411–430
Pidgeon RT, O'Neil JR, Silver LT (1966) Uranium and lead isotopic stability in a metamict zircon under experimental hydrothermal conditions. Science 154:1538–1540
Poldervaart A (1950) Statistical studies of zircon as a criterion in granitization. Nature 165:574–575
Poldervaart A (1955) Zircon in rocks. 1. Sedimentary rocks. Am J Sci 253:433–461
Poldervaart A (1956) Zircon in rocks. 2. Igneous rocks. Am J Sci 254:521–554
Polezhayev YM (1974) On mechanism of metamictization of minerals under the action of autoradiation. Geochim Int 11:1157–1161
Pupin JP (1980) Zircon and granite petrology. Contrib Mineral Petrol 73:207–220
Pupin JP, Turco G (1981) Le zircon, mineral commun significatif des roches endogenes et exogenes. Bull Mineral 104:724–731
Pyatenko YA (1965) Isomorphism of atoms and its mineralogical consequences. Geochem Int 2:268
Pyatenko YA (1970) Behavior of metamict minerals on heating and the general problem of metamictization. Geochem Int 7:758–763
Ruh R, Garrett HJ, Domagala RF, Tallan NM (1968) The system Zirconia-Hafnia. J Am Ceram Soc 51:23–27
Shannon RD, Prewitt CT (1969) Effective ionic radii in oxydes and fluorides. Acta Cryst 625:925–946
Shevaleevskii ID, Pavlenko AS, Vainshtein EE (1960) Dependence of the behavior of zirconium and hafnium on the petrochemical characteristics of igneous and alkalic metasomatic rocks. Geochem Int, pp 262–272
Silver LT (1963) The relation between radioactivity and discordance in zircons. Nucl Sci Ser 38, Nat Acad Sci Publ 1075, Washington, pp 34–42
Smirnova EV (1967) In: Gmelin (1970) Handbuch der anorganischen Chemie: Blei, C3, p 851
Sommerauer J (1976) Die chemisch-physikalische Stabilität natürlicher Zirkone und ihr U-(Th)-Pb System. Unpubl thesis, ETH Zürich, No. 5755, p 151
Steiger RH, Bär MT, Büsch W (1973) The zircon age of an anatectic rock in the Central Schwarzwald. Fortschr Mineral 50:131–132
Sunin LV, Malyshev VI (1983) The thermoisochron method of determining Pb-Pb ages. Geochem Int 20:34–45
Tera F, Wasserburg GJ (1975) Precise isotopic analyses of lead in picomole and subpicomole quantities. Anal Chem 47:2214–2220
Tilton GR, Aldrich LT (1955) The reliability of zircon as age indicator. Trans Am Geophys Union 36:531–536
Vainshtein EE, Ginzburg AI, Shevaleevskii ID (1959) The Hf/Zr ratio in zircons from granite pegmatites. Geochem Int, pp 151–157
Williams IS, Compston W, Black LP, Ireland TR, Foster JJ (1984) Unsupported radiogenic lead in zircon: a cause of anomalously high Pb-Pb, U-Pb and Th-Pb ages. Contrib Mineral Petrol 88:322–327
Wollen GM (1963) Diffusionless phase transformations in zirconia and hafnia. J Am Ceram Soc 46:418–422
Zykov SI, Stupnikova NI (1957) Isotopic analysis of lead not requiring any preliminary chemical preparation of the mineral. Geochem Int, pp 506–510
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Kober, B. Single-zircon evaporation combined with Pb+ emitter bedding for 207Pb/206Pb-age investigations using thermal ion mass spectrometry, and implications to zirconology. Contr. Mineral. and Petrol. 96, 63–71 (1987). https://doi.org/10.1007/BF00375526
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DOI: https://doi.org/10.1007/BF00375526