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1.
We introduce and propose zircon M257 as a future reference material for the determination of zircon U‐Pb ages by means of secondary ion mass spectrometry. This light brownish, flawless, cut gemstone specimen from Sri Lanka weighed 5.14 g (25.7 carats). Zircon M257 has TIMS‐determined, mean isotopic ratios (2s uncertainties) of 0.09100 ± 0.00003 for 206pb/238U and 0.7392 ± 0.0003 for 207pb/235U. Its 206pb/238U age is 561.3 ± 0.3 Ma (unweighted mean, uncertainty quoted at the 95% confidence level); the U‐Pb system is concordant within uncertainty of decay constants. Zircon M257 contains ~ 840 μg g?1 U (Th/U ~ 0.27). The material exhibits remarkably low heterogeneity, with a virtual absence of any internal textures even in cathodoluminescence images. The uniform, moderate degree of radiation damage (estimated from the expansion of unit‐cell parameters, broadening of Raman spectral parameters and density) corresponds well, within the “Sri Lankan trends”, with actinide concentrations, U‐Pb age, and the calculated alpha fluence of 1.66 × 1018 g?1. This, and a (U+Th)/He age of 419 ± 9 Ma (2s), enables us to exclude any unusual thermal history or heat treatment, which could potentially have affected the retention of radiogenic Pb. The oxygen isotope ratio of this zircon is 13.9%o VSMOW suggesting a metamorphic genesis in a marble or calc‐silicate skarn.  相似文献   
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In this article, we document a detailed analytical characterisation of zircon M127, a homogeneous 12.7 carat gemstone from Ratnapura, Sri Lanka. Zircon M127 has TIMS‐determined mean U–Pb radiogenic isotopic ratios of 0.084743 ± 0.000027 for 206Pb/238U and 0.67676 ± 0.00023 for 207Pb/235U (weighted means, 2s uncertainties). Its 206Pb/238U age of 524.36 ± 0.16 Ma (95% confidence uncertainty) is concordant within the uncertainties of decay constants. The δ18O value (determined by laser fluorination) is 8.26 ± 0.06‰ VSMOW (2s), and the mean 176Hf/177Hf ratio (determined by solution ICP‐MS) is 0.282396 ± 0.000004 (2s). The SIMS‐determined δ7Li value is ?0.6 ± 0.9‰ (2s), with a mean mass fraction of 1.0 ± 0.1 μg g?1 Li (2s). Zircon M127 contains ~ 923 μg g?1 U. The moderate degree of radiation damage corresponds well with the time‐integrated self‐irradiation dose of 1.82 × 1018 alpha events per gram. This observation, and the (U–Th)/He age of 426 ± 7 Ma (2s), which is typical of unheated Sri Lankan zircon, enable us to exclude any thermal treatment. Zircon M127 is proposed as a reference material for the determination of zircon U–Pb ages by means of SIMS in combination with hafnium and stable isotope (oxygen and potentially also lithium) determination.  相似文献   
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This study is an attempt to unravel the tectono-metamorphic history of high-grade metamorphic rocks in the Eastern Erzgebirge region. Metamorphism has strongly disturbed the primary petrological genetic characteristics of the rocks. We compare geological, geochemical, and petrological data, and zircon populations as well as isotope and geochronological data for the major gneiss units of the Eastern Erzgebirge; (1) coarse- to medium-grained “Inner Grey Gneiss”, (2) fine-grained “Outer Grey Gneiss”, and (3) “Red Gneiss”. The Inner and Outer Grey Gneiss units (MP–MT overprinted) have very similar geochemical and mineralogical compositions, but they contain different zircon populations. The Inner Grey Gneiss is found to be of primary igneous origin as documented by the presence of long-prismatic, oscillatory zoned zircons (540 Ma) and relics of granitic textures. Geochemical and isotope data classify the igneous precursor as a S-type granite. In contrast, Outer Grey Gneiss samples are free of long-prismatic zircons and contain zircons with signs of mechanical rounding through sedimentary transport. Geochemical data indicate greywackes as main previous precursor. The most euhedral zircons are zoned and document Neoproterozoic (ca. 575 Ma) source rocks eroded to form these greywackes. U–Pb-SHRIMP measurements revealed three further ancient sources, which zircons survived in both the Inner and Outer Grey Gneiss: Neoproterozoic (600–700 Ma), Paleoproterozoic (2100–2200 Ma), and Archaean (2700–2800 Ma). These results point to absence of Grenvillian type sources and derivation of the crust from the West African Craton. The granite magma of the Inner Grey Gneiss was probably derived through in situ melting of the Outer Grey Gneiss sedimentary protolith as indicated by geological relationships, similar geochemical composition, similar Nd model ages, and inherited zircon ages. Red Gneiss occurs as separate bodies within fine- and medium-grained grey gneisses of the gneiss–eclogite zone (HP–HT overprinted). In comparison to Grey Gneisses, the Red Gneiss clearly differs in geochemical composition by lower contents of refractory elements. Rocks contain long-prismatic zircons (480–500 Ma) with oscillatory zonation indicating an igneous precursor for Red Gneiss protoliths. Geochemical data display obvious characteristics of S-type granites derived through partial melting from deeper crustal source rocks. The obtained time marks of magmatic activity (ca. 575 Ma, ca. 540 Ma, ca. 500–480 Ma) of the Eastern Erzgebirge are compared with adjacent units of the Saxothuringian zone. In all these units, similar time marks and geochemical pattern of igneous rocks prove a similar tectono-metamorphic evolution during Neoproterozoic–Ordovician time.  相似文献   
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Summary We report results of a combined SHRIMP ion microprobe and Raman microprobe study of the correlation between metamictization and U-Pb isotopic discordance of zircon. The spatial resolution of the SHRIMP and Raman probe used are about 200 m3 and 80 m3, respectively. This allows a direct comparison of U-Pb isotopic discordance and metamictization of small areas within zircon crystals. We show that the impact of the oxygen ion beam on the zircon during the SHRIMP analysis does not cause significant amorphization or recrystallization in the remaining zircon on a scale of 1 m. Consequently, it is possible to determine the initial degree of metamictization of zircon within and adjacent to a SHRIMP analytical spot by Raman microprobe measurements after performing SHRIMP analyses. A combination of the two microprobe techniques gives information on the concentration and distribution of radionuclides as well as the degree of metamictization and its heterogeneity and the lateral age distribution within the grain. We found that the degree of U-Pb isotopic discordance correlates closely with the degree of metamictization within single zircon grains, on a scale of 15 m, which is consistent with previous results on the scale of single and multiple zircon grains showing that metamictization enhances the relative potential for secondary loss of radiogenic lead in zircon.
Metamiktisierung und U-Pb-Isotopendiskordanz in Einzelzirkonen: eine komplexe Untersuchung mittels Ramanmikrosonde und SHRIMP Ionensonde
Zusammenfassung Wir präsentieren die Ergebnisse einer Untersuchung des Zussammenhangs von Metamiktisierung und U-Pb Isotopendiskordanz in Zirkonen mittles kombinierter SHRIMP-Ionenmikrosonden- und Ramanmikrosondenanalysen. Die räumliche Auflösung der verwendeten Analysensysteme, experimentell mit 200 m3 (SHRIMP) und 80 m3 (Ramansonde) bestimmt, gestattet den direkten Vergleich der in Mikrobereichen innerhalb von Zirkon-Einkristallen gemessenen Isotopendiskordanzen und Metamiktisierungsgrade. Wir zeigen, daß der während der SHRIMP-Analyse auf den Zirkon einwirkende Sauerstoffionenstrahl weder signifikante Amorphisierung noch Rekristallisation des benachbarten Zirkonmaterials im 1 m-Bereich hervorruft. Es ist deshalb möglich, den Grad der Metamiktisierung eines Zirkon-Mikrobereiches auch in den SHRIMP-Analysengrübchen, d.h. erst nach dem Analysieren dieses Bereiches mit der Ionensonde, mittels hochauflösender Ramanmessungen unverfälscht zu bestimmen. Der Einsatz beider Mikromethoden liefert kombinierte Informationen zu den Gehalten und Verteilungen radioaktiver Elemente, zum Grad der Metamiktisierung und seiner Heterogenität und zur lateralen Altersverteilung innerhalb von Einzelkörnern. Wir weisen eine deutliche Korrelation des Grades der U-Pb-Isotopendiskordanz mit dem Grad der Metamiktisierung im Mikrobereich (15 m Auflösung) nach. Dies stimmt mit früheren, an Einzelzirkonen und Populationen getätigten Beobachtungen überein, daß die Metamiktisierung von Zirkon dessen Potential zu sekundären Bleiverlusten erhöht.
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7.
Quantifying strain birefringence halos around inclusions in diamond   总被引:1,自引:0,他引:1  
The pressure and temperature conditions of formation of natural diamond can be estimated by measuring the residual stress that an inclusion remains under within a diamond. Raman spectroscopy has been the most commonly used technique for determining this stress by utilising pressure-sensitive peak shifts in the Raman spectrum of both the inclusion and the diamond host. Here, we present a new approach to measure the residual stress using quantitative analysis of the birefringence induced in the diamond. As the analysis of stress-induced birefringence is very different from that of normal birefringence, an analytical model is developed that relates the spherical inclusion size, R i, host diamond thickness, L, and measured value of birefringence at the edge of the inclusion, \Updelta n(R\texti )\textav \Updelta n(R_{\text{i}} )_{\text{av}} , to the peak value of birefringence that has been encountered; to first order \Updelta n\textpk = (3/4)(L/R\texti )  \Updelta n(R\texti )\textav \Updelta n_{\text{pk}} = (3/4)(L/R_{\text{i}} ) \, \Updelta n(R_{\text{i}} )_{\text{av}} . From this birefringence, the remnant pressure (P i) can be calculated using the photoelastic relationship \Updelta n\textpk = - (3/4)n3 q\textiso P\texti \Updelta n_{\text{pk}} = - (3/4)n^{3} q_{\text{iso}} P_{\text{i}} , where q iso is a piezo-optical coefficient, which can be assumed to be independent of crystallographic orientation, and n is the refractive index of the diamond. This model has been used in combination with quantitative birefringence analysis with a MetriPol system and compared to the results from both Raman point and 2D mapping analysis for a garnet inclusion in a diamond from the Udachnaya mine (Russia) and coesite inclusions in a diamond from the Finsch mine (South Africa). The birefringence model and analysis gave a remnant pressure of 0.53 ± 0.01 GPa for the garnet inclusion, from which a source pressure was calculated as 5.7 GPa at 1,175°C (temperature obtained from IR analysis of the diamond host). The Raman techniques could not be applied quantitatively to this sample to support the birefringence model; they were, however, applied to the largest coesite inclusion in the Finsch sample. The remnant pressure values obtained were 2.5 ± 0.1 GPa (birefringence), 2.5 ± 0.3 GPa (2D Raman map), and 2.5–2.6 GPa (Raman point analysis from all four inclusions). However, although the remnant pressures from the three methods were self-consistent, they led to anomalously low source pressure of 2.9 GPa at 1,150°C (temperature obtained from IR analysis) raising serious concerns about the use of the coesite-in-diamond geobarometer.  相似文献   
8.
Zircon samples without and with secondary chemical alteration from diverse sources were subjected to heat treatment at 1400 °C for 96 h. Resulting new phases and textures suggest that decomposition of zircon into component oxides occurred in all experiments to various degrees. The crucible material was found to have a strong influence on the extent of breakdown, especially in the case of altered starting materials. In this study the progressive stages of the breakdown of zircon grains are described. The factors that may govern the decomposition are discussed, including radiation damage, secondary alteration and external reaction conditions (sample container, atmosphere). Alumina crucibles should generally be avoided in dry annealing of zircon, to minimise uncontrolled breakdown into oxides.  相似文献   
9.
This study addresses whether Raman spectra can be used to estimate the degree of accumulated radiation damage in monazite-(Ce) samples whose chemical composition was previously determined. Our results indicate that the degree of disorder in monazite–(Ce), as observed from increasing Raman band broadening, generally depends on both the structural state (i.e., radiation damage) and the chemical composition (i.e., incorporation of non-formula elements). The chemical effects were studied on synthetic orthophosphates grown using the Li-Mo flux method, and non radiation-damaged analogues of the naturally radiation-damaged monazite–(Ce) samples, produced by dry annealing. We found that the “chemical” Raman-band broadening of natural monazite–(Ce) can be predicted by the empirical formula, $$ {\hbox{FWHM}} {\hbox{[c}}{{\hbox{m}}^{ - {1}}}{]} = {3}{.95} + {26}{.66} \times {\hbox{(Th}} + {\hbox{U}} + {\hbox{Ca}} + {\hbox{Pb)}} {\hbox{[apfu]}} $$ where, FWHM = full width at half maximum of the main Raman band of monazite–(Ce) (i.e., the symmetric PO4 stretching near 970?cm?1), and (Th+U+Ca+Pb) = sum of the four elements in apfu (atoms per formula unit). Provided the chemical composition of a natural monazite–(Ce) is known, this “chemical band broadening” can be used to estimate the degree of structural radiation damage from the observed FWHM of the ν1(PO4) band of that particular sample using Raman spectroscopy. Our annealing studies on a wide range of monazite–(Ce) reference materials and other monazite–(Ce) samples confirmed that this mineral virtually never becomes highly radiation damaged. Potential advantages and the practical use of the proposed method in the Earth sciences are discussed.  相似文献   
10.
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