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In the Variscan Bohemian Massif, (ultra-)potassic plutons are conspicuously associated with the high-grade, lower crustal/upper mantle Gfohl Unit (Moldanubian Zone). They can be subdivided into two contrasting groups: (1) coarse amphibole–biotite melagranite to quartz syenite with conspicuous K-feldspar phenocrysts (the ‘durbachite suite’), and (2) essentially equigranular biotite–two-pyroxene quartz syenites to melagranites (the ‘syenitoid suite’). The latter suite, represented by the Tabor and Jihlava plutons, is characterized by an originally ‘drier’ mineral assemblage orthopyroxene + clinopyroxene + Mg-biotite + plagioclase + K-feldspar + quartz, with accessory zircon, apatite, ilmenite, monazite and/or rutile + chromite. The rich assemblage of both rock-forming and accessory minerals allows testing of numerous geothermobarometers. The resulting P–T data are mutually consistent; they document emplacement of the parental magmas at mid-crustal levels (~5 kbar/19 km for Tabor and 7–8 kbar/26–30 km for Jihlava) and record near-isobaric crystallization from at least 1170 °C to the solidus. New Isotope-Dilution Thermal Ionization Mass-Spectrometry (ID-TIMS) U–Pb ages for zircon (336.9 + 0.6 Ma) and rutile (336.8 + 0.8 Ma) from the Tabor Pluton, together with previously published ages from the Jihlava Pluton, provide temporal constraints for the emplacement and rapid cooling of the syenitoids below c. 600 °C. This supports the hypothesis of post-tectonic emplacement of a hot and dry melt (>1200 °C?) into an essentially consolidated orogenic crust. The two syenitoid plutons have comparable, crust-like radiogenic isotope signatures (87Sr/86Sr337 = 0.7114–0.7133, e337Nd = −6.8 to −8.0). This, in context of whole-rock geochemical variation and K-feldspar Pb isotopic compositions, is consistent with generation from a strongly enriched lithospheric mantle source. Shortly before melting, the local orogenic mantle was most likely modified by deep subduction and relamination of felsic crustal material of the Saxothuringian provenance, transformed to the felsic high-pressure granulites common in the Moldanubian Zone. In the subsequent evolution of the two-pyroxene syenitoid plutons, crystal fractionation and accumulation played a key role, unlike in the durbachite suite itself, where magma mixing with leucogranitic melts was much more important. Structural relations inside and around the (ultra-)potassic plutons (~343–335 Ma) suggest that – besides different depths and specific processes of magma emplacement – these plutons track different kinematic histories and evolutions of regional strain fields in their high-grade country rocks in this crucial period of the Variscan Orogeny.

Garnet and zircon geochronology combined with trace element partitioning and petrological studies provide tight constraints on evolution of the UHT-(U)HP terrain of the Orlica-Śnieznik Dome (OSD) in the NE Bohemian massif. Lu-Hf dating of peritectic garnet from two mesocratic granulites constrained the time of its initial growth at 346.9 ± 1.2 and 348.3 ± 2.0 Ma recording peak 2.5 GPa pressure and 950 °C temperature. In situ, U-Pb SHRIMP dating of zircon from the same granulite gave a younger age of 341.9 ± 3.4 Ma. Ti-in-zircon thermometry indicates crystallization at 810–860 °C pointing to zircon formation on the retrograde path. Lu partitioning between garnet rim and zircon suggest equilibrium growth and thus U-Pb zircon age constrain the terminal phase of garnet crystallization which lasted about 6 Ma. All Sm-Nd garnet ages obtained for mesocratic and mafic granulites are identical and consistently younger than the corresponding Lu-Hf dates. They are interpreted as reflecting cooling of granulites through the Sm-Nd closure temperature at about 337 Ma. The estimated PTt path documents the ca. 10 Ma evolution cycle of the OSD characterized by two distinct periods: (1) 347 - > 342 Ma period corresponds to nearly isothermal decompression resulting from crustal scale folding and vertical extrusion of granulites, and (2) at > 342–337 Ma which corresponds to a fast, nearly isobaric cooling.

A new data set of ca. 500 LA–ICP-MS U–Pb detrital zircon ages for six metasedimentary units from the Tuscan basement (Apuan Alps, Monti Pisani, Monticiano-Roccastrada), along with a precise SHRIMP U–Pb crystallization age of a metavolcanic unit (Apuan Alps) have been collected to determine their depositional ages and provenance. These results have been integrated with the recently published ca. 900 U–Pb detrital zircon ages from Elba Island to draw a complete picture of the Paleozoic journey of the Tuscan basement. A major change in the sources supplying sediments to the Tuscan basins is shown to occur during this journey. Detrital zircon ages of early Cambrian to middle Ordovician metasediments mirror those of coeval northern Africa sediments: most samples were sourced in western Africa, while one sample is derived material from central northern Africa. The Tuscan block was therefore located at the peri-Gondwana margin, close to central northern Africa. The prominent mid-Ordovician magmatic arc activity (ca. 460 Ma) at the northern Gondwana margin and its detritus, characterise the zircon age distribution of Ordovician and Silurian volcano-sedimentary rocks, that were therefore generated at the northernmost Gondwana margin during subduction and subsequent initial Paleotethys rifting. The Carboniferous–Permian metasediments are dominated by populations of Ordovician and Variscan-age zircons, with a minor occurrence of Neoarchean and Paleoproterozoic zircons that is best explained by recycling of European Neoproterozoic–Cambrian metasediments. In summary, the main sources supplying the Tuscan basins were located in northern Africa throughout Cambrian–Ordovician times, shifting to the volcanic arc active at the northern Gondwana margin during the middle Ordovician. During Variscan and post-Variscan times, detrital zircon sources were mostly located in European terrains, witnessing the shift of Tuscany from Africa to Europe.

The LA-ICP-MS U-(Th-)Pb geochronology international community has defined new standards for the determination of U-(Th-)Pb ages. A new workflow defines the appropriate propagation of uncertainties for these data, identifying random and systematic components. Only data with uncertainties relating to random error should be used in weighted mean calculations of population ages; uncertainty components for systematic errors are propagated after this stage, preventing their erroneous reduction. Following this improved uncertainty propagation protocol, data can be compared at different uncertainty levels to better resolve age differences. New reference values for commonly used zircon, monazite and titanite reference materials are defined (based on ID-TIMS) after removing corrections for common lead and the effects of excess 230Th. These values more accurately reflect the material sampled during the determination of calibration factors by LA-ICP-MS analysis. Recommendations are made to graphically represent data only with uncertainty ellipses at 2s and to submit or cite validation data with sample data when submitting data for publication. New data-reporting standards are defined to help improve the peer-review process. With these improvements, LA-ICP-MS U-(Th-)Pb data can be considered more robust, accurate, better documented and quantified, directly contributing to their improved scientific interpretation. La communauté internationale de la géochronologie LA-ICP-MS U-(Th-)Pb a défini les nouvelles normes pour la détermination des âges U-(Th-)Pb. Un nouveau flux de travail définit la propagation adéquate des incertitudes pour ces données, en identifiant les composants aléatoires et systématiques. Seules les données avec des incertitudes relatives à l'erreur aléatoire devraient être utilisées dans les calculs des moyennes pondérées des âges de la population; les composantes de l'incertitude pour les erreurs systématiques sont propagées après cette étape, empêchant leur réduction erronée. En suivant ce protocole amélioré pour la propagation de l'incertitude, les données peuvent être comparées à différents niveaux d'incertitude pour mieux résoudre les différences d’âge. Les nouvelles valeurs pour les matériaux de référence zircon, monazite et titanite sont définies (basée sur ID-TIMS) après les corrections du plomb commun et les effets de l'excès en 230Th. Ces valeurs reflètent plus fidèlement le matériau échantillonné lors de la détermination des facteurs d’étalonnage par analyse LA-ICP-MS. Des recommandations sont faites pour représenter graphiquement des données avec seulement des ellipses d'incertitude à 2s et pour soumettre ou pour citer des données de validation avec les données de l’échantillon lors de la soumission des données pour publication. Les nouvelles normes de déclaration des données sont définies pour améliorer le processus d'évaluation par les pairs. Grâce à ces améliorations, les données LA-ICP-MS U-(Th)-Pb peuvent être considérés comme plus solides, exactes, mieux documentées et quantifiées, contribuant ainsi à une meilleure interprétation scientifique.

Accepted manuscript version. Published version available at https://doi.org/10.1016/j.precamres.2017.06.017. Detrital zircon provenance study of a metamorphosed sedimentary succession in the eastern part of the Kaoko Belt in Namibia has revealed two distinct sources for the Neoproterozoic sedimentation along the southwestern Congo Craton margin. The lower part of the succession shows detrital zircon ages consistent with erosion of Paleoproterozoic basement of the Congo Craton with an inferred Mesoproterozoic volcano-sedimentary cover. Within the middle part of the succession, which includes glaciogenic sediments correlated with the Sturtian (717–660 Ma) glaciation, the Mesoproterozoic zircon grains disappear and the signal is dominated by ages known from the Congo Craton basement. The sedimentation in these parts of the succession is interpreted as related to the early Neoproterozoic rifting. The sedimentary rocks in the top part of the profile contain only subordinate proportion of the Paleoproterozoic–Archaean zircon grains and the populations are dominated by three age groups of ca. 1.0–1.2 Ga, ca. 800–750 Ma and ca. 650 Ma, consistent with erosion of the Punta del Este–Coastal Terrane exposed in the centre of the Kaoko–Dom Feliciano–Gariep orogen. An associated glaciogenic horizon interpreted as reflecting the Marinoan (645–635 Ma) glaciation constrains the sedimentation in the upper part of the succession and suggests a short time span between the high-grade metamorphism/magmatism in the Punta del Este–Coastal Terrane and its exhumation. Sedimentary rocks with such detrital zircon pattern appear also in the Damara and Gariep belts. Their source in the western part of the Kaoko–Dom Feliciano–Gariep orogen suggests that they represent an early orogenic flysch that originated during early collision in the western part of the orogen. The short time span between the metamorphism/magmatism in the Punta del Este–Coastal Terrane and deposition of the early orogenic flysch derived from it suggests that the Coastal Terrane was never separated from the Congo Craton by an oceanic domain. The estimated time span between the end of lithospheric stretching and sedimentation of the early flysch suggests that the hypothetical Adamastor Ocean separating the western and eastern forelands of the Kaoko–Dom Feliciano–Gariep orogen must have been small.

Distinctly different crustal blocks converge in southern Tanzania which are thought to belong to the Paleoproterozoic Usagaran/Ubendian Belt, the Mesoproterozoic Irumide Belt and the Neoproterozoic East African Orogen. Zircons from thirteen samples were dated by LA-SC/MC-ICPMS in order to assign the different crystalline basement rocks to one of the above mentioned geological units based on the age of metamorphism and formation of the igneous precursor rocks. The mainly migmatic gneissic samples were taken along a traverse from Mbamba Bay, Lake Malawi to Masasi, S-Tanzania. Zircon cores and rims trace magmatic protoliths between 1000 ± 9 and 1055 ± 6 Ma and metamorphism between 563 ± 10 and 616 ± 12 Ma. Ages belonging to the Usagaran/Ubendian event as well as the 640 Ma EAO event were only found in the westernmost and easternmost part of the transsect, respectively. Magmatic ages of 724 ± 6 and 764 ± 4 Ma were determined in locally confined undeformed granitoid bodies. Mostly similar ages as well as lithological units can be found in the Unango and Marrupa Complexes in N-Mozambique which are considered as part of the Southern Irumide Belt. The exact location of terrane boundary between the Southern Irumide Belt and the Western/Eastern Granulites and the Usagaran/Ubendien Belts in southern Tanzania remains uncertain. With aid of digital elevation data, satellite images and airborne geophysical data we suggest that a combination of fault systems is responsible for the distribution of the different units. The northeastern limit of the Southern Irumide Belt (Unango and Marrupa Complexes) can be traced along a major tectonic boundary, the Mwembesi Fault system, that extends from Malawi to the south of the Mahenge Mountains in Tanzania.

The Eger Complex in the northwestern Bohemian Massif consists mainly of amphibolite facies granitic gneisses containing a subordinate volume of felsic granulites. Microstructural changes and modelling of metamorphic conditions for both rock types suggest a short-lived static heating from ~760 to ~850 °C at a constant pressure of ~16 kbar, which led to the partial granulitization of the granitoid rocks. Detailed study of the protolith zircon modifications and modelling of the Zr re-distribution during the transition from amphibolite to granulite facies suggests that the development of c. 340 Ma old zircon rims in the granulite facies sample is the result of recrystallization of older (c. 475 Ma) protolith zircon. This study suggests that the partial granulitization is a result of a short exposure of the Eger Complex metagranitoids to a temperature of ~850 °C at the base of an arc/fore-arc domain and their subsequent rapid exhumation during the Lower Carboniferous collision along the western margin of the Bohemian Massif.

Inter-laboratory comparison of laser ablation ICP-MS and SIMS U-Pb dating of synthetic detrital zircon samples provides an insight into the state-of-the art of sedimentary provenance studies. Here, we report results obtained from ten laboratories that routinely perform this type of work. The achieved level of bias was mostly within ± 2% relative to the ID-TIMS U-Pb ages of zircons in the detrital sample, and the variation is likely to be attributed to variable Pb/U elemental fractionation due to zircon matrix differences between the samples and the reference materials used for standardisation. It has been determined that ~ 5% age difference between adjacent age peaks is currently at the limit of what can be routinely resolved by the in situ dating of detrital zircon samples. Precision of individual zircon age determination mostly reflects the data reduction and procedures of measurement uncertainty propagation, and it is largely independent of the instrumentation, analytical technique and reference samples used for standardisation. All laboratories showed a bias towards selection of larger zircon grains for analysis. The experiment confirms the previously published estimates of the minimum number of grains that have to be analysed in order to detect minor zircon age populations in detrital samples. Une comparaison inter-laboratoires de datation U-Pb d'echantillons de zircons detritiques de synthese par les methodes d'ablation laser ICP-MS et SIMS donne un apercu de l'etat de l'art des etudes de provenance sedimentaire. Nous presentons ici les resultats obtenus par dix laboratoires qui effectuent regulierement ce type de travail. Le niveau de biais atteint etait compris dans l'intervalle ± 2% par rapport aux âges U-Pb ID-TIMS des zircons de l'echantillon detritique et la variation peut certainement etre attribue a un fractionnement elementaire Pb/U variable relie a des differences de matrices entre les zircons des echantillons et les zircons de reference utilises pour la normalisation. Il a ete determine qu'environ 5% de difference d'âge entre les pics d'âge adjacents est actuellement a la limite de ce qui peut etre resolu en mode routine par la datation in situ d'echantillons de zircons detritiques. La precision de la determination de l'âge de zircon individuel reflete principalement la reduction des donnees et les procedures de mesure de la propagation de l'incertitude, et elle est largement independante de l'instrumentation, de la technique d'analyse et des echantillons de reference utilises pour la standardisation. Tous les laboratoires ont montre un biais vers la selection des plus gros grains de zircon pour l'analyse. L'experience confirme les estimations precedemment publiees sur le nombre minimum de grains qui doivent etre analyses afin de detecter les populations mineures d'âge de zircons dans les echantillons detritiques.

Accepted manuscript version. Published version at http://doi.org/10.1016/j.precamres.2016.05.011. License CC BY-NC-ND 4.0. The match of geological units of the dissected Kaoko-Dom Feliciano-Gariep orogenic system exposed along the coasts of the South Atlantic is poorly understood. Two suites of intrusive rocks crop out in the Angra Fria Bay area, a part of the Coastal Terrane of the Kaoko Belt in Namibia. U–Pb zircon dating of three samples from the younger suite provided ages of 574 ± 6, 586 ± 3 and 584 ± 7 Ma, similar to the ages of the oldest syn-collisional granitoids in the area. Three samples of the older suite gave ages of 626 ± 5, 622 ± 5 and 620 ± 6 Ma respectively, which have not previously been recorded in intrusive rocks of the Kaoko Belt, but which coincide with those from the Florianópolis Batholith in the Dom Feliciano Belt in Brazil. Zircon ages, Sr–Nd isotopic composition and tectonic position of these granitoids suggest that this magmatic complex could be a continuation of the Florianópolis Batholith on the African side of the Atlantic Ocean. Consequently, the Angra Fria intrusions and the Florianópolis Batholith may represent suitable localities for spatial reconstruction of the Gondwana supercontinent in the area, where the robust pre-Mesozoic connecting points are scarce.

The Pinjarra Orogen, stretching along the western coast of Western Australia, is one of the least understood orogens on the continent. Exposure is limited to fault-bound basement blocks within the Phanerozoic Perth Basin, which have been interpreted as either remnants of a Mesoproterozoic orogen or as allochthonous blocks within a Neoproterozoic orogen. Thus even the timing of orogenesis is controversial. However, since the orogen is in a critical position for reconstructions of both Rodinia and Gondwana, a better understanding is highly desirable. New U–Pb ages of detrital zircon cores, metamorphic zircon rims and metamorphic monazites from the Northampton Complex, the northernmost and largest of the exposed basement blocks, provide better insights into the sedimentary provenance and metamorphic history of the metasediments exposed in this part of the orogen. Both the monazite ages and the youngest metamorphic zircon rims constrain metamorphism in the Northampton Complex to 1090–1020 Ma. Additionally, a large number of older metamorphic zircon rims pre-date this event and were inherited from the Albany-Fraser Orogen in southwestern Australia, which is also identified as the main source region for the detrital zircon cores. Additional sources of detrital zircons are the Mawson Continent (the South Australian Craton and parts of East Antarctica) and possibly the North Australian Craton, as well as synsedimentary volcanic rocks. However, the combination of ages from the cores and inherited metamorphic rims shows that zircons from the Mawson Continent/North Australian Craton were not directly transported to the Northampton Complex but arrived there after being incorporated into the Albany-Fraser Orogen and then eroded from there. The dataset records therefore two orogenic cycles: (1) erosion of the Mawson Continent/North Australian Craton, deposition along the craton margins, collision between the Mawson Continent and North-West Australian Craton and metamorphism in the Albany-Fraser Orogen and (2) erosion of the Albany-Fraser Orogen, deposition along Australia's western margin and metamorphism during the Pinjarra Orogeny. This highlights the care that must be taken in detrital zircon studies, since many of the detrital cores record a second-order provenance. It also explains how zircons from the Mawson Continent could be transported across the Albany-Fraser Orogen that should normally have been a barrier to northwest-directed sediment transport. Finally, in light of these new and previously published data, we support the interpretation that the Pinjarra Orogen is a Mesoproterozoic orogen formed along Australia's western margin.

Detrital zircon grains in coarse-grained sedimentary rocks of the Noisy formation, (traditionally considered as the H6 unit of the uppermost Hooggenoeg Formation) in the Paleoarchean Barberton Greenstone Belt (BGB) South Africa, are investigated by laser ablation (LA)-ICP-MS to constrain their U–Pb and 207Pb/206Pb ages for depositional age and provenance determination. Drill core and field observations indicate that these rocks are clastic polymictitic diamictites and sandstones. A wide range in 207Pb/206Pb ages between ca. 3600 and 3430 Ma is reported. The youngest detrital zircon grain identified has an age of 3432 ± 10 Ma, constraining the maximum depositional age of the sedimentary sequence and the formation of a major underlying erosional unconformity. The youngest grains correspond in age to the ca. 3460–3430 Ma tonalite–trondjemite–granodiorite (TTG) gneisses of the Stoltzburg terrane and felsic intrusions of the uppermost Hooggenoeg Formation that constitute most of the Songimvelo Block of the BGB on the Kaapvaal craton. The 207Pb/206Pb ages of the oldest grains identified corresponds to plutonic sources identified in older proto-continental blocks of the Kaapvaal craton, namely the ca. 3509 Ma Steynsdorp Block and ca. 3667–3223 Ma Ancient Gneiss Complex (AGC). This new data indicates provenancial linkage between the Songimvelo Block and older proto-continental blocks exposed on the Kaapvaal craton at ca. 3432 Ma. It is argued here, that the Noisy formation is a remnant of the earliest tectonic basin in the BGB, that developed during major tectonic accretion and uplift at ca. 3432 Ma that lead to formation of the erosional unconformity. In conjunction with new drill core and field observations, the geochronological constraints presented here support plate-tectonic processes operating in the proto-Kaapvaal craton that resulted in its formation as a stable continental landmass as early as ca. 3432 Ma.

Geochemical and petrologic studies on Paleogene basanites from the Carpatho-Pannonian region (Poiana Rusca, Romania) and associated peridotite xenoliths provide information about the composition of the underlying lithosphere, the petrogenetic evolution of the magma and its mantle source, as well as the geodynamic significance of the igneous activity in a regional context. Major and trace elements as well as Sr–Nd isotopic ratios reveal an ocean–island basalt signature, interpreted as the derivation from an upper mantle source chemically similar to the European Asthenospheric Reservoir after low fraction partial melting. Due to estimated average mantle source temperatures and the absence of any subduction-related geochemical features, the igneous activity in Poiana Rusca was apparently triggered by adiabatic decompression melting, as postulated for similar and nearly coeval alkaline rocks in eastern Serbia. Differentiation processes within the Poiana Rusca magmatic suite initially resulted from removal of mainly olivine, followed by olivine + clinopyroxene fractional crystallization. The spinel-lherzolitic to harzburgitic composition of the mantle fragments point to 2–30% fractional melting at a depth of approx. 70 km. Petrographic and geochemical investigations indicate both cryptic and modal metasomatism related to the influence of both alkaline-rich silicate and alkaline-rich hydrous silicate melts rather than subduction-related fluids/melts.

Annual growth rings of a common hardwood species, Picea abies L., were investigated as a potential archive of past atmospheric Pb pollution. Wide distribution of trees in terrestrial settings and straightforward chronology are two advantages of this potential geochemical archive, but several processes described in the literature may obscure the trends in past Pb deposition. These confounding factors include, e.g., radial post-depositional mobility of Pb in xylem, and ecosystem acidification leading to higher bioavailability of Pb. One- to five-year annual wood increments were analyzed for Pb concentrations and 206Pb/207Pb ratios at Jezeri (JEZ), Uhlirska (UHL) and Na Lizu (LIZ), three sites in the Czech Republic, differing in atmospheric Pb loads. Three to four trees per site were included in the study. Distinct Pb concentration maxima between 1960 and 1990 at the two heavily polluted sites (JEZ and UHL) coincided with historical Pb emissions known from inventories of industrial production. No Pb concentration maxima were found at one site, LIZ, situated in a national park 150 km from major pollution sources. Spruce tree rings from JEZ, located just 5 km from coal-burning power stations, contained a large proportion of coal-derived Pb (a high-206Pb/207Pb ratio of 1.19). A coal-related maximum in 206Pb/207Pb in JEZ tree rings was found using two different analytical techniques, laser-ablation multi-collector ICP MS, and single-collector sector-field ICP MS. In a three-isotope graph (206Pb/207Pb vs. 208Pb/207Pb), tree-ring data plotted into the field of ombrotrophic (i.e., rain-fed) peat bogs, suggesting negligible contribution of bedrock-derived Pb in the xylem. We concluded that none of the potential confounding factors played a major role at our sites. Annual growth rings of P. abies in Central Europe faithfully recorded historical changes in atmospheric Pb depositions.

We studied primary ore samples from Kalmakyr, a giant Cu–Au–Mo porphyry deposit in eastern Uzbekistan. Disseminated and stockwork-type high-grade Cu–Au–Mo mineralization showed average concentrations of 55 ppb Pd, 5.5 ppb Pt, 0.95 ppb Rh, 0.49 ppb Ir, and 4.1 ppm Au (n = 8). This type of mineralization is characterized by the presence of pyrite, chalcopyrite, molybdenite, and gold. A peak Pd content of 292 ppb was determined in a base-metal-rich quartz vein in granodiorite porphyry, which contains galena, sphalerite, chalcopyrite, tetrahedrite, and gold. Palladium correlates with Cu, Ag, Se, and S. Mineralogical and laser ablation ICP-MS study confirmed that Pd is homogeneously distributed in chalcopyrite, which contains up to 110 ppm Pd, and tetrahedrite, containing up to 20 ppm Pd. An assessment of the Pd and Pt budget at Kalmakyr showed the potential of approximately 17 t of Pd and 1.7 t of Pt.

The metamorphic evolution of micaschists in the north-eastern part of the Saxothuringian Domain in the Central European Variscides is characterized by the early high-pressure M1 assemblage with chloritoid in cores of large garnet porphyroblasts and a Grt–Chl–Phe–Qtz ± Pg M2 assemblage in the matrix. Minerals of the M1–M2 stage were overprinted by the low-pressure M3 assemblage Ab–Chl–Ms–Qtz ± Ep. Samples with the best-preserved M1–M2 mineralogy mostly appear in domains dominated by the earlier D1 deformation phase and are only weakly affected by subsequent D2 overprint. Thermodynamic modelling suggests that mineral assemblages record peak-pressure conditions of ≥18–19 kbar at 460–520 °C (M1) followed by isothermal decompression 10.5–13.5 kbar (M2) and final decompression to

Northeast Africa 003 (NEA 003) is a lunar meteorite found as a two paired stones (6 and 118 g) in Libya, 2000 and 2001. The main portion (∼75 vol%) of the 118 g meteorite, used for this study, (NEA 003-A) consists of mare-basalt and a smaller adjacent portion (∼25 vol%) is a basaltic breccia (NEA 003-B). NEA 003-A has a coarse-grained magmatic texture consisting mainly of olivine, pyroxene and plagioclase. The late-stage mineral association is composed mainly of elongated plagioclase, ilmenite, troilite, fayalite, Si–K-rich glass, apatite, and a rare SiO2 phase. Other accessory minerals include ulvospinel, chromite, and trace Fe–Ni metal. Olivine and pyroxene contain shock-induced fractures, and plagioclase is completely converted into maskelynite. The Fe/Mn values of the whole rock, olivines and pyroxenes, and the bulk-rock oxygen isotopic composition provide evidence for the lunar origin of NEA 003-A meteorite. This is further supported by the presence of Fe–Ni metal and the anhydrous mineral association. NEA 003-A is geochemically and petrographically distinct from previously described mare-basalt meteorites and is not paired with any of them. The petrography and major element composition of NEA 003-A is similar to the composition of low-Ti olivine mare basalts from Apollo 12 and olivine-normative basalts from Apollo 15. The NEA 003-A meteorite shows obvious geochemical similarities in trace elements contents with Apollo 15 olivine-normative basalts and could represent a yet unknown geochemically primitive member of the olivine-normative basalt series. The meteorite is depleted in rare earth elements (REE) and incompatible trace elements indicating a primitive character of the parental magma. The bulk-rock chemical composition demonstrates that the parent melt of NEA 003-A was not contaminated with KREEP components as a result of magma mixing or assimilation processes. Results of crystallization modelling and low minimum cooling rate estimates (∼0.07 °C/h) suggest that the parent melt of NEA 003-A crystallized in the lower part of a lava flow containing cumulate olivine (∼10%) and was probably derived from more primitive picritic magma by fractional crystallization processes. Sm–Nd dating yields an age of 3.09 ± 0.06 Ga which corresponds to the period of lower Eratosthenian lunar volcanic activity, and the near-chondritic eNd value of −0.4 ± 0.3 indicates that the meteorite could be derived from a slightly enriched mantle source similar to the Apollo 15 green glasses. Ar–Ar step release results are inconsistent with Sm–Nd ages suggesting that NEA 003-A was exposed to one or more impact events. The most extensive event took place at 1.8 Ga and the shock intensity was likely between 28 and 45 GPa. The absence of solar Ar suggests that NEA 003-A has not been directly exposed at the lunar surface but the cosmic ray exposure age of 209 ± 6 Ma suggests that NEA 003-A resided in the upper regolith for part of its history.

(Fe–Zn–Mg)-spinel-bearing assemblages in the high-grade rocks from three localities in the Moldanubian domain of the Bohemian Massif (Variscan belt of Central Europe) have been studied to monitor the partition behaviour of zinc along the pressure–temperature path followed by the host rock and to discuss the role of Zn in spinel stabilization. Spinels in two studied samples are characterized by low gahnite content (max. 0.09 Zn p.f.u), they crystallized only under silica-undersaturated conditions and the presence of zinc is thus assumed to be insignificant for their stabilization. One sample contains spinels that are gahnite-rich (up to 0.58 Zn p.f.u) leading to their stabilization within a quartz-bearing matrix. All spinel-bearing domains reflect late re-equilibration corresponding to decompression. However, in samples with preserved relics of a high-pressure mineral assemblage, changes in the zinc content attributed to prograde garnet growth were observed in the garnet cores. In order to monitor the distribution of zinc along the pressure-temperature path, textural observations have been combined with electron-microprobe and laser ablation ICP-MS data. The results point to preferential partitioning of zinc into biotite during the spinel-absent early stages of decompression and suggest that biotite was the main source of zinc for spinel crystallizing at low pressures.

Using a state-of-the-art 193 nm-LA-MC-ICP-MS system and with careful control of analytical procedures, the long term external reproducibility and accuracy of the ages Phanerozoic zircons measured over a period of months using calibrator bracketing for the 206Pb/238U and 207Pb/206Pb ages were ca. 1% (2 RSD) if a single reference zircon was used for the matrix-matched calibration. When different reference zircons were used for the calibration, suspicious systematic shifts in the obtained ages were observed and thus a reduction in the overall accuracy of the dating method became obvious. Such shifts were within a few percent range of the U-Pb and Pb/Pb ages and seemed to vary independently of zircon age and composition. A “test of accuracy” experiment was conducted reducing instrumental effects as far as possible by analysing five different reference zircons mounted on a single mount eight times during the same session. An identical protocol was used for all analyses, with unchanged instrument parameters and with ion beam intensities kept as identical as possible. For data reduction, every zircon served consecutively as the reference zircon for calibration, with the others in the batch treated as unknowns. The known reference age and the four calculated ages obtained using the four other RMs for calibration were then compared. Even using such a strict analytical protocol, shifts in 206Pb/238U, 207Pb/235U and 207Pb/206Pb ratios were still present. They varied non-systematically and ranged from −4.35% to 3.08% for the investigated age range (1065 Ma to 226 Ma). Assuming the absence of instrumental effects (i.e., memory, dead-time correction, non-linearity of ion counters and interdetector calibration, crystallographic orientation, ablation cell geometry and setup, gas flows), the observed shifts were attributed to matrix and/or ablation related effects. It is proposed that non-spectral matrix effects in the Ar plasma torch resulted in non-uniform signal enhancement (or depression?) leading to shifts both in elemental and Pb isotopic ratios. Additionally, the ablated particle size distribution could be an important factor controlling plasma conditions and thus mass bias and fractionation. Until such effects are well understood and controlled, it would seem that any LA-ICP-MS zircon U-Pb and 207Pb/206Pb age determination cannot be meaningfully interpreted at below a ca. 3% to 4% (2 RSD) confidence level. Ce travail repose sur l'utilisation d'un systeme de 193 nm-LA-MC-ICP-MS de derniere generation, avec un controle minutieux des procedures analytiques. La reproductibilite externe et la justesse des mesures d'âges 206Pb/238U et 207Pb/206Pb effectuees par la methode de l'encadrement par des calibrateurs sur des zircons d'âge phanerozoique, ont ete testees sur plusieurs mois et sont de l'ordre de 1% (2 RSD) si un seul zircon de reference etait utilise pour effectuer la calibration de matrice identique. Quand differents zircons etaient utilises pour la calibration, des biais systematiques suspects etaient obtenus sur les âges mesures entrainant une moins bonne justesse globale de cette methode de datation. Ces biais etaient de l'ordre de quelques pourcents sur les âges U-Pb et Pb/Pb et semblaient varier independamment de l'âge du zircon ou de sa composition. Un test de justesse a ete realise, afin de reduire au maximum les effets instrumentaux, en analysant 8 fois durant une meme session, 5 zircons de reference differents, montes dans la meme pastille. Le meme protocole analytique a ete utilise pour toutes ces analyses, sans modification des parametres instrumentaux et avec des intensites des signaux emis conserves aussi proches que possible. Lors du traitement des donnees, chaque zircon a servi de zircon de reference pour la calibration, les autres etant traites comme des inconnus. Les âges recommandes et les âges mesures des 4 zircons ainsi traites en inconnus ont ete compares. Les biais sur les rapports 206Pb/238U, 207Pb/235U et 207Pb/206Pb etaient encore presents, malgre l'application d'un tel protocole. Ils montraient des variations aleatoires, de l'ordre de −4.35%a 3.08% pour la gamme d'âge consideree (1065 Ma a 226 Ma). Nous avons suppose l'absence d'effets instrumentaux tels que: effet de memoire, correction du temps mort, non linearite des compteurs d'ions, probleme d'inter calibration des detecteurs, orientation cristallographique, geometrie de la cellule d'ablation, flux des gaz. En consequence, les biais observes ont ete attribues a des effets de matrice ou des effets lies au processus d'ablation. Des effets de matrice, non spectraux, au niveau de la torche a plasma d'argon pourraient entrainer des amplifications (ou attenuations) du signal, conduisant a des biais, a la fois entre elements et entre isotopes du Pb. De plus la distribution de la taille des particules ablatees pourrait etre un facteur important dans le controle des conditions du plasma, donc des biais de masse et des fractionnements. Tant que de tels effets ne sont pas compris et controles, il semble que l'intervalle de confiance de toute determination d'âge U-Pb ou 207Pb/206Pb par LA-ICP-MS ne peut pas etre inferieur a 3 ou 4% (2 RSD).

We present a comprehensive geochemical data set for a suite of back-arc alkaline volcanic rocks from James Ross Island Volcanic Group (JRIVG), Antarctic Peninsula. The elemental and isotopic (Sr, Nd, Pb and Li) composition of these Cenozoic basalts emplaced east of the Antarctic Peninsula is different from the compositions of the fore-arc alkaline volcanic rocks in Southern Shetlands and nearby Bransfield Strait. The variability in elemental and isotopic composition is not consistent with the JRIVG derivation from a single mantle source but rather it suggests that the magma was mainly derived from a depleted mantle with subordinate OIB-like enriched mantle component (EM II). The isotopic data are consistent with mantle melting during extension and possible roll-back of the subducted lithosphere of the Antarctic plate. Magma contamination by Triassic–Early Tertiary clastic sediments deposited in the back-arc basin was only localized and affected Li isotopic composition in two of the samples, while most of the basalts show very little variation in δ 7 Li values, as anticipated for “mantle-driven” Li isotopic composition. These variations are difficult to resolve with radiogenic isotope systematics but Li isotopes may prove sensitive in tracking complex geochemical processes acting through the oceanic crust pile, including hydrothermal leaching and seawater equilibration.

Hf isotopic data of minerals in a mafic pyroxene granulite from the southern Bohemian Massif, together with their major and trace element composition and petrological observations were used to decipher the metamorphic history and behaviour of zircon in the granulite. The Hf isotopic composition in the minerals was used to estimate whether the decompression reaction, namely the consumption of garnet and rutile, could have provided Zr for the formation of newly grown metamorphic zircon. The age of the decompression reaction indicated by the evolution of Hf isotopes in garnet and orthopyroxene is between 333 and 331 Ma, i.e. ca. 7 Ma younger than the available U–Pb zircon ages from the Moldanubian granulites and than the newly obtained 343 ± 2 Ma laser ablation ICP-MS U–Pb age of zircons. The combination of bulk and in-situ Hf isotopic data, major and trace element composition and petrological modeling of P–T evolution revealed that the formation of zircons can not be related to the decompression phase of the evolution of the mafic granulites.

The rocks of the crystalline basement of the East European Craton in southern Estonia show effects of partial melting under granulite facies conditions. Zircons extracted from partial melting products (tonalite from the Tapa Zone – 1824 ± 26, tonalite from the South Estonian Zone – 1788 ± 16 Ma and charnockite from the Tapa Zone – 1761 ± 11 Ma) yield U–Pb crystallisation ages that span over approximately 80 Ma, suggesting a prolonged high-grade metamorphism or several separate events. U–Pb zircon age of one sample of charnockite is concordant with the Nd model age of partial melting of its host mafic granulite facies gneiss (intercept at 1.76 Ga). Linear geochemical trends and similar initial Nd isotopic compositions of mafic granulites and charnockites suggest their possible genetic relationship. From our new and previously published data it follows that the peak granulite metamorphic conditions and formation of tonalites and charnockites (850 °C and 6 kbar) in the Estonian basement occurred at 1788–1778 Ma. Then, the rocks cooled down, passing through the garnet closure temperature of approximately 650–700 °C at 1728 ± 24 Ma. The age of metamorphism of the Estonian granulites is lower than the metamorphic ages known from southern Finland, but it is similar to the age of metamorphism reported from the Belarus-Baltic Granulite Belt in Latvia.

U-Pb isotopic data obtained by laser ablation ICPMS analysis of nine zircons with centre to margin oscillatory growth zones from a K-feldspar-rich augen gneiss in the allochthonous Lower Crystalline Nappe of the Erzgebirge domain of the western part of the Bohemian Massif yield a concordia age of 524 ± 10 Ma (2 sigma). This Early Cambrian age represents the time of magmatic crystallization of the protolith of a representative, from near Měděnec, of the allochthonous “Red gneiss” whose igneous nature is shown by the presence of (deformed) xenoliths. Data from TIMS analysis of zircons with variable proportions of unzoned xenocrystic cores surrounded by oscillatory-zoned overgrowths point to magma derivation from upper Proterozoic, or older, rocks. Data obtained for five zircon grains from another “Red gneiss” in the Lower Crystalline Nappe (in the Klinovec anticline) plot below the concordia with the age of the one point that is near concordant being 519 ± 26 Ma (2 sigma). These data, together with internal features of the zircons, are consistent with Early Cambrian granitic plutonism also in this part of the Erzgebirge but with later Pb loss, possibly associated with considerable fluid movement during thrust nappe development. Another sample of a coarse-grained orthogneiss from the autochthonous St Catherine9s dome yielded a significantly younger Early Ordovician age of 480 ± 10 Ma (2 sigma) calculated from eight zircon analyses. However, three zircon grains from the same sample gave a significantly older near-concordant Late Proterozoic age of ca. 620 Ma. Provided that the age difference of ca . 40 Ma between orthogneisses from Měděnec - Klinovec and St Catherine9s dome holds also for other orthogneisses in the Erzgebirge, zircon U-Pb age data could be used to discriminate between allochthonous and autochthonous units in this region. The ca. 25 Ma difference between the Early Cambrian protolith age of the augen gneiss from near Měděnec determined by the laser ablation ICPMS technique and a previously reported older age of 550 ± 9 Ma for a nearby sample determined by the Pb-Pb evaporation technique is accounted for on the basis of the latter not being adequate for dating zircons with a small xenocrystic component. This study demonstrates the importance of high spatial resolution dating techniques, such as SHRIMP or laser ablation ICPMS, in dating zircons with complex growth history that are common in crustally-derived melts.

Volcanics of the Skinner Cove Formation of western Newfoundland carry a primary remanence acquired at 550 Ma at a paleolatitude of 19°S. There has been doubt that this represents the latitude of the Laurentian margin at 550 Ma, because the Skinner Cove Formation is allochthonous. We present new evidence from inherited zircons in the volcanics that should remove this doubt. Zircon crystals extracted from an ankaramite flow and a trachyte flow were dated individually by measuring U–Th–Pb isotopes for ∼ 30 μm ×30 μm areas using a laser ablation microprobe (LAM) linked to an inductively coupled plasma mass spectrometer (ICP-MS). Most of the zircons from the ankaramite are concordant and yield a 550±5 Ma date indistinguishable from the 550+3/−2 Ma date previously reported using multi-grain thermal ionisation mass spectrometry. About half of the zircons from the trachyte are also concordant yielding an overlapping date of 556±5 Ma. The other half clustered at ∼1000 and 1500–1600 Ma, which are characteristic ages of the Grenvillian basement exposed nearby in the Long Range Inlier. These zircon xenocrysts were very likely picked up as the Skinner Cove magma ascended through Grenvillian basement of the Laurentian margin. There can now be little doubt that the ∼19°S Skinner Cove paleolatitude represents Laurentia’s southern margin at 550 Ma. This makes it unlikely that Laurentia changed from south polar at ∼523 Ma to equatorial at ∼508 Ma due to a rapid ∼90° change in the Earth’s rotation axis. Such an inertial interchange true polar wander (IITPW) event has been proposed as a trigger for the Cambrian faunal explosion. An IITPW event may have occurred in the Vendian, mostly between 577 and 565 Ma, judging by paleomagnetic results from Laurentia. However, it is more likely that the paleomagnetic results suggesting high latitude for Laurentia at 577 Ma or low latitude at 565 Ma are flawed. We suggest that Laurentia remained at low latitude throughout the Vendian (from the ∼600 Ma start of near-equatorial glaciations). This is supported by magmatic evidence suggesting that Laurentia’s incipient Iapetus margin was stationary over a mantle plume throughout the Vendian. Laurentia at low latitude throughout the Vendian also helps provide the predominance of low latitude continents needed to account for the Vendian’s near-equatorial glaciations, according to the snowball Earth hypothesis.

Nous avons acquis des donnees geochronologiques (systeme U-Th-Pb) par ablation au laser avec un plasma a couplage inductif et spectrometrie de masse (LAM-ICP-MS) afin de preciser in situ l'âge de l'allanite et du zircon dans une seule lame mince polie du granite de October Harbour, au Labrador. C'est la premiere fois que l'allanite est ainsi etudiee pour datation Th-Pb par methode LAM-ICP-MS, avec verification des resultats par datation du zircon dans le meme echantillon. Des cristaux atteignant a peine 20 X 20 μm ont meme pu etre analyses dans une lame mince polie d'une epaisseur de 100 μm. Au prealable, les cristaux de zircon ont ete examines avec des images d'electrons retrodiffuses afin d'evaluer la presence de coeurs herites, de surcroissances, et de croissance oscillatoire. Nous avons effectue 45 analyses LAM-ICP-MS de 35 cristaux de zircon. Selon les donnees U-Th-Pb obtenues sur zircon, l'âge du granite serait 1657 ′ 10 Ma (MSWD = 0.77, moyenne ponderee des âges 2 0 7 Pb/ 2 0 6 Pb telle que determinee avec 25 points concordants). Les donnees indiquent la presence de zircon herite ayant un âge de 1800-1850 Ma, et des signes de pertes repetees de plomb dans plusieurs grains. L'allanite se presente en gros cristaux idiomorphes. Elle fait preuve de teneurs elevees en U et en Th. Vingt-six analyses de deux cristaux d'allanite ont donne seize points concordants, provenant surtout du noyau a faible teneur en Th d'un seul cristal, et une moyenne ponderee de l'âge 2 0 8 Pb/ 2 3 2 Th de 1635 ′ 17 Ma (MSWD = 2.1). Quoique les signes d'une perte complexe de plomb sont aussi presents dans certaines portions de l'allanite, il n'y a aucun signe d'un coeur herite. L'âge du granite de October Harbour serait d'environ 1640-1660 Ma, ce qui est passablement plus jeune que ce que l'on avait propose anterieurement suite a une analyse conventionelle U-Pb de plusieurs grains de zircon pris de la suite intrusive de Strawberry, soupconnee d'etre liee genetiquement, ce qui avait donne un âge de 1719 ′ 3 Ma. La suite de Strawberry pourrait donc etre plus complexe qu'une simple suite de roches mise en place il y a environ 1720 Ma, et contenir des roches d'âges tres differents.

Laser-ablation quadrupole ICP-MS analyses of molybdenite samples from Preissac, Quebec, and Mokrsko, Belcice and Kasperske Hory gold deposits in the Bohemian Massif, Czech Republic, for Re and radiogenic 187 Os suggest the presence of strong zoning in Re and in 187 Os/ 187 Re values within grains. The zoning patterns indicate decoupling of daughter 187 Os from parent 187 Re after molybdenite crystallization. Whereas Re is not homogeneously distributed in the molybdenite grains studied, the lack of correlation between the calculated 187 Os/ 187 Re value and the Re content also reflects the mobility of 187 Os within individual grains of molybdenite. Such decoupling of Re and Os could affect the accuracy of Re-Os ages if disturbed portions of molybdenite are sampled for dating by conventional isotope-dilution N-TIMS or ICP-MS techniques. The results re-emphasize the critical need for homogenization of quantities of molybdenite sufficiently large to capture the bulk Os/Re of the sample to be dated by these methods. Laser-ablation sampling, when used with a multicollector magnetic-sector ICP-MS instrument, is able to produce Re-Os ages with a precision better than 2% (1 � m) from single spots in certain old and Re-rich molybdenite grains, but would be difficult to use as a dating tool given the extreme 187 Os/ 187 Re heterogeneity seen in individual grains.

In situ U-Th-Pb geochronology was born some two decades ago with the introduction and development of high-resolution secondary ion mass spectrometry (SIMS or SHRIMP [Sensitive High Mass Resolution Ion MicroProbe]; Compston et al. 1984, Williams 1998, Compston 1999, Davis et al.; this volume, Ireland and Williams, this volume). This technique clearly demonstrated the existence of age heterogeneities within the single crystals of zircon and other accessory phases and therefore the need for high-spatial resolution (tens to hundreds of cubic micrometers) geochronological data. In situ dating by ion probe is capable of achieving an analytical precision that is only an order of magnitude worse than the conventional isotope dilution-thermal ionization mass spectrometry (ID-TIMS) dating technique. It has the advantage, however, of more readily identifying concordant portions of grains, does not require chemical treatment of samples prior to the analysis, is essentially nondestructive, and can achieve greater sample throughputs. A major obstacle to the wider use of ion probe dating has always been the high cost of instrumentation and hence relative scarcity of suitably equipped geologic laboratories. Laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS) emerged in 1985 and rapidly became an important analytical tool for trace element determinations in geological samples (Jackson et al. 1992). It was soon realized that the large variations in radiogenic Pb and Pb/ U isotopic ratios found in nature could be resolved by ICPMS techniques and, when coupled to a laser, ICPMS could be used as a dating tool similar to the ion probe. The pioneering work of Feng et al. (1993), Fryer et al. (1993), Hirata and Nesbitt (1995) and Jackson et al. (1996) illustrated the potential usefulness of laser sampling for in situ dating by ICPMS particularly well. However, these studies and others that followed also revealed the major …

In the Saint-Aubin-des-Châteaux deposit (Massif Armoricain, France), the Ordovician Gres Armoricain sandstones have undergone several fluid-rock interaction events, including diagenetic cementation and orogenic base metal-As-Sb-Au mineralisation. Ironstone layers interbedded in the sandstones contain several generations of spectacular authigenic xenotime overgrowths that formed around detrital zircon grains in response to successive hydrothermal events. Textural and chemical characterisations allow to distinguish three generations of xenotime overgrowths, differing notably in their REE characteristics. In-situ U-Pb data obtained on these xenotime overgrowths show that their U-Pb systematics were largely disturbed by successive hydrothermal events over about 90 Ma between ~ 330 and ~ 420 Ma, a time interval encompassing most phases of the construction of the Variscan orogen in France. The younger dates cluster around ~ 330–340 Ma and likely correspond to the age of the deposition of massive sulphides and base-metals in the Saint-Aubin-des-Châteaux deposits, which is consistent with the structural contexts where they formed. Finally, this study shows that similarly to monazite, another phosphate widely used for U-Pb and Th-Pb dating studies, the U-Pb chronometric system in xenotime appears to be highly sensitive to fluid circulations.

New developments in U–Pb dating of zircons by laser ablation (LA) ICPMS are described and, for the first time, a direct comparison of detrital zircons dated by LA ICPMS and SIMS methods is presented. True real-time mass bias correction is made by aspirating a Tl/U tracer at the same time as laser ablation. The method is similar to that described in Horn et al. (2000) , except that enriched 233U rather than 235U is used in the tracer solution. Correction for laser-induced Pb/U elemental fractionation is based on a mathematical treatment of time-resolved data that is independent of laser ablation characteristics and does not require external standardisation. Internal corrections for mass bias and elemental fractionation eliminate the effects of variable sample matrix on isotopic ratios and improve the accuracy of U–Pb dating by laser ablation ICPMS. With the proper error propagation, the precision of U–Pb age determinations is only slightly worse than SIMS-based ion probe dating. However, LA ICPMS is capable of much more rapid analysis of the large number of zircons required for sediment provenance studies. There is excellent agreement between concordant laser ablation ICPMS and SIMS analyses of detrital zircons extracted from lower Silurian metasandstone from the Ulven Group (Skarfjell Formation) in the west Norwegian Caledonian nappes. Both LA ICPMS and SIMS U–Pb zircon ages indicate that sedimentary detritus of the Ulven Group was supplied from a terrain containing zircons of Archean, Proterozoic and early Ordovician age.

Recent advances in laser ablation ICP-MS techniques allow accurate U-Th-Pb age dating of monazites that are as young as several tens of million years to a precision better than 2%. Accuracy of the age determinations has been improved by true real-time mass bias correction via nebulisation of a solution containing enriched 233U and natural Tl isotopes. The Tl-U tracer solution eliminates possible effects of variable sample matrices on the precision and accuracy of measured isotopic ratios. Mass bias corrections based on measured 205Tl/233U ratios in the tracer solution allow direct measurement of 235U in monazite. Combined with high-sensitivity laser ablation ICP-MS measurements, direct measurement of 235U particularly improves the precision of U-Pb dating of young monazites. Correction for laser-induced Pb/U and Pb/Th elemental fractionation is based on a mathematical treatment of time resolved count-rate data that is independent of laser ablation characteristics, does not require external standardisation and allows variable laser pit size or raster patterns for each measurement. The new procedures make the LA ICP-MS technique more flexible for in situ U-Th-Pb analysis. Des avancees recentes dans les techniques LA ICP-MS permettent d'obtenir des âges U-Th-Pb de monazites de quelques dizaines de millions d'annees avec une precision superieure a 2%. L'exactitude de la determination des âges a ete amelioree par une correction du biais massique en temps reel grâce a la nebulisation d'une solution enrichie en 233U et en isotopes du Tl. La solution-traceur Tl-U evite les effets de matrices d'echantillons sur la precision et l'exactitude des rapports isotopiques mesures. Les corrections de biais massique basees sur les rapports 205Tl/233U dans la solution-traceur permettent la mesure directe de 235U de la monazite. Combinee avec la haute sensibilite des mesures par LA ICP-MS, l'analyse directe de 235U ameliore particulierement la precision de la datation U-Pb de monazites jeunes. La correction du fractionnement des elements Pb/U et Pb/Th dua l'ablation laser est basee sur un traitement mathematique du signal independant des caracteristiques de l'ablation laser, ne requiert pas de standard externe et permet d'utiliser des tailles variables de point ou d'aire balayee au laser pour chaque mesure. Les nouvelles procedures rendent la technique LA ICP-MS plus facile a adapter pour l'analyse U-Th-Pb in situ.

Precise measurements of the isotopic composition of Li in low-concentration natural carbonate samples is demonstrated for quadrupole ICPMS. Cool plasma conditions result in high sample/background ratios for the measured Li signals even for low concentrations. Quantitative chemical separation of Li prior to the measurement on ICPMS is necessary to avoid the matrix-induced isotopic fractionation and the results have to be externally corrected for mass bias and instrumental fractionation. The isotopic composition of lithium can be measured in samples containing only 5–10 ng Li with a within-run precision better than 0.5‰ (2 standard errors of the mean), and a long term reproducibility that is better that 2.1‰ (2 standard deviations). The method has been successfully used to measure Li isotopic composition of 1–10 mg samples of calcium carbonate tests of Pulleniatina obliquiloculata and Globorotalia tumida that were collected from the sediment–seawater interface and have Li concentrations of about 1 ppm. The isotopic composition of Li in studied calcium carbonate tests of P. obliquiloculata is independent of the size of tests and resembles the lithium isotopic composition of modern seawater, suggesting that this species may provide a record of Li isotope variations in past oceans.

High-precision garnet chronometry using the Sm–Nd, U–Pb, Rb–Sr or Lu–Hf isotope systems is gaining widespread application for constraining the prograde and high-temperature history of metamorphic belts. However, due to the low concentrations of the chronometrically important elements, garnet analyses are often susceptible to incorporation of small quantities of accessory phases such as zircon, monazite and allanite. Here we assess the extent to which such inclusions affect garnet analyses by comparing in situ analyses of Sm and Nd concentrations in the crystal lattice, obtained by laser ablation inductively coupled mass spectrometry (LA-ICP-MS), with those obtained by isotope dilution (ID) on separates of the same garnets. The results show that the garnets studied here are largely free from inclusions. In general, however, the low concentrations of Sm and Nd in the garnet lattice mean that the incorporation of even very small quantities of accessory phases will result in a significant change in the measured garnet Sm and Nd concentration. Simple modelling of the effect of such inclusions on age information shows that garnet inclusion disequilibrium and the extent to which inclusions decrease the apparent parent–daughter ratio are critical. Such modelling demonstrates that the incorporation of old LREE-enriched minerals such as monazite will yield an apparently lower age than the true garnet age. However, this study indicates that erroneous age information can be identified if duplicate garnet analyses are performed. In addition, LA-ICP-MS is shown to be a useful technique in verifying the purity of samples for isotope analysis.

Xenotime overgrowths on detrital zircon in siliciclastic sediments have been reported in numerous studies. However, in natural samples, solid solution of zircon and xenotime is limited to near-end-member compositions. In order to characterize the interface region between both minerals and to draw inferences on the growth mechanisms of authigenic xenotime, we studied xenotime overgrowths on detrital zircon grains from two Phanerozoic sandstone samples with contrasting post-depositional histories. In one sample, the small (≤10 μm), pyramidal xenotime overgrowths are of diagenetic origin and grew without major discontinuity on the detrital zircon grain. The second sample shows up to >50-μm-wide, porous and inclusion-rich, hydrothermal xenotime overgrowths on detrital zircon, whereas the transition zone between both minerals is accompanied by large pore volume. Chemical compositions of the xenotime precipitates from the two samples differ particularly in Y, REE, Th and Sc concentrations, whereas high MREE availability in the diagenetic sample and the presence of Sc in the hydrothermal sample, respectively, appear to have promoted xenotime growth. Transmission electron microscopy on electron-transparent foils cut from the interface region shows that both the diagenetic xenotime and the hydrothermal xenotime are crystalline and grew in optical and crystallographic continuity to their detrital zircon substrata. Only a narrow transition zone (≤90 nm—diagenetic sample, 200–300 nm—hydrothermal sample) between zircon and xenotime is in part made up of nanometre-scale crystalline domains that are slightly distorted and may have formed from dissolution–re-precipitation processes at the zircon rim along with precipitation from the respective fluid.

[1] We investigated some of the sampling and mineral separation biases that affect the accuracy of detrital zircon provenance studies. The study has been carried on a natural catchment in the Scottish Highlands that represents a simple two-component source system and on samples of synthetic sediment prepared for this study to test the effects of heavy mineral separation on the resulting zircon age spectra. The results suggest that zircon fertility of the source rocks and physical properties of zircon represent the most important factors affecting the distribution of zircon age populations in the stream sediments. The sample preparation and selection of zircons for analysis may result in preferential loss of information from small zircon grains. Together with the preference for larger crystals during handpicking, it can result in several-fold difference compared to the real age distribution in the sediment sample. These factors appear to be more important for the reproducibility of zircon age spectra than is the number of zircon grains analyzed per sample.

Lithospheric thickening during protracted Ediacaran supercontinent assembly was dissipated in various ways along the “Pan-African” East African–Antarctic Orogen. In NE Mozambique, late-tectonic extension and plutonism south of the Lurio Belt has been modelled in terms of lithosphere delamination, although rigorous testing of the hypothesis by structural analysis has not yet been undertaken. This study presents the first analyses of late-tectonic structures in both the Mesoproterozoic basement and the Cambrian cover sequences in the Nampula Complex, NE Mozambique, supported by, and integrated with, new geochronological data. Both late compressional and extensional fabrics overprint the main Pan-African collisional structures to a variable degree in identified structural domains. The long-lived northern boundary of the Nampula Complex, the Lurio Belt high-strain zone, initiated in the Ediacaran, was reactivated and segmented during these later phases, with boundary-parallel shortening. U–Pb SIMS ages from selected latest-tectonic units in the Nampula Complex and the Lurio Belt give consistent ages between 518 ± 2 and 514 ± 5 Ma. They are coeval with migmatisation and granitoid plutonism in the Nampula Complex. U–Pb titanite (471 ± 9 Ma) and 40 Ar/ 39 Ar biotite (431 ± 3 Ma) data suggest subsequent slow cooling rates in the Nampula Complex, consistent with basal heating by asthenosphere uprise following lithosphere delamination. Consequently, we believe the new data suggest that the observed intense late polyphase deformation has preferentially occurred where the delaminated lithosphere was doubly weakened by loss of the mantle root and the resulting long-lived elevated temperature regime.

Advances in the chemical and isotopic characterisation of geological and environmental materials can often be ascribed to technological improvements in analytical hardware. Equally, the creation of novel methods of data acquisition and interpretation, including access to better reference materials, can also be crucial components enabling important breakthroughs. This biennial review highlights key advances in either instrumentation or data acquisition and treatment, which have appeared since January 2010. This review is based on the assessments by scientists prominent in each of the given analytical fields; it is not intended as an exhaustive summary, but rather provides insight from experts of the most significant advances and trends in their given field of expertise. In contrast to earlier reviews, this presentation has been formulated into a unified work, providing a single source covering a broad spectrum of geoanalytical techniques. Additionally, some themes that were not previously emphasised, in particular thermal ionisation mass spectrometry, accelerator-based methods and vibrational spectroscopy, are also presented in detail.

Subvolcanic pyroxenite-hornblendite-kentallenite-diorite-granodiorite masses of the appinite suite that are spatially and temporally associated with the much more voluminous granitic plutons of the British Caledonides have major element proportions and REE patterns indicative of shoshonitic affinities. Hornblendite-monzonite-syenogabbro-pyroxene melasyenite-durbachite-biotite-rich syenite-biotite-rich granite masses of the plutonic durbachite suite of the Bohemian Massif of the Central European Hercynides, that also are spatially and temporally associated with much more voluminous granitic plutons, have geochemical characteristics that generally correspond with those of the appinite suite. Compositionally both suites resemble lamprophyres emplaced during the latter parts of the respective episodes. Both the appinite and durbachite suites show independence of K/Rb and SiO2 with the two suites having mainly different but somewhat overlapping K/Rb ratios. Other geochemical characters, as shown by fields and trends on K vs Rb, AFM and other plots, point to the durbachite suite representing generally more evolved products of shoshonitic magma than members of the appinite suite. However, there are different geochemical characteristics, including higher Cr/Ni ratios in the durbachite suite and Co present in lower proportions in the appinite suite. These differences are the result of different histories of freezing, remelting and partial separation and remixing of fractionation products and reflect the explosive subvolcanic vs plutonic regimes of the appinitic and durbachitic suites, respectively. Support for this petrogenesis is provided by mineral compositions and comparison of compositions of mineral phases and the rocks in which they occur.

Microbial activity in volcanic glass within the oceanic crust can produce micron sized pits and tunnels. Such biogenic textures have been described from the recent oceanic crust and mineralized equivalents in pillow lavas as old as 3.47–3.45 Ga from the Barberton Greenstone Belt (BGB) of South Africa. In meta-volcanic glasses these microbial traces are preserved by titanite mineralization (CaTiSiO5) and on the basis of morphological, textural and geochemical evidence have been argued to represent Earth's oldest trace fossils. Here we report the results of in-situ U–Pb dating of titanite that infills trace fossils from the Hooggenoeg Complex of the BGB using laser ablation MC-ICP-MS (multi-collector inductively coupled, plasma mass spectrometry). This yields a titanite age of 3.342 ± 0.068 Ga demonstrating the antiquity of the BGB trace fossils. This radiometric age confirms that a sub-seafloor biosphere was already established in the PaleoArchean and that it likely represented an important habitat for the emergence and evolution of early microbial life on the Earth.

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. Nous presentons et proposons a la communaute le zircon M257 qui pourrait devenir un materiau de reference pour la determination des âges U-Pb sur zircon par spectrometrie de masse a ions secondaires (SIMS). Ce specimen scie d'une gemme brun clair, sans defauts, provenant du Sri Lanka, pese 5.14 g (25.7 carats). Les moyennes des rapports isotopiques (et les incertitudes associees 2s) mesurees par TIMS sur ce zircon M257 sont 0.09100 ± 0.00003 en 206pb/238U et 0.7392 ± 0.0003 en 207pb/235U. Son âge 206pb/238U est de 561.3 ± 0.3 Ma (moyenne non ponderee, incertitude: 95% intervalle de confiance); le systeme U-Pb y est concordant, aux erreurs sur les constantes de desintegration pres. Le zircon M257 contient ∼ 840 μg g−1 U (Th/U ∼ 0.27). Ce materiel montre de tres faibles heterogeneites, avec une quasi absence de textures internes, meme a I'examen par cathodoluminescence. Le degre de dommage lie aux radiations (estime par I'expansion des parametres de la cellule unitaire, I'elargissement des parametres des spectres Raman et la densite) est modere et uniforme. II se correle bien, (sur I'alignement “Sri Lanka”) avec les concentrations en actinides, I'âge U-Pb et la fluence calculee de 1.66 × 1018 g−1 Ceci, couplea son âge (U+Th)/He de 419 ± 9 Ma (2s), nous permet d'exclure I'existence d'evenement thermique passe, ou de traitement par la chaleur, qui aurait potentiellement pu affecter le processus de retention de Pb radiogenique. Le rapport isotopique de I'oxygene de ce zircon est 13.9%o VSMOW, suggerant une genese par metamorphisme, au sein d'un marbre ou d'un skarn calco-silicate.

Matrix-matched calibration by natural zircon standards and analysis of natural materials as a reference are the principle methods for achieving accurate results in inicrobeam U-Pb dating and Hf isotopic analysis. We describe a new potential zircon reference material for laser ablation ICP-MS that was extracted from a potassic granulite facies rock collected in the southern part of the Bohemian Massif (Plesovice, Czech Republic). Data from different techniques (ID-TIMS, SIMS and LA ICP-MS) and several laboratories suggest that this zircon has a concordant U-Pb age with a weighted mean (206)Pb/(238)U date of 337.13 +/- 0.37 Ma (ID-TIMS, 95% confidence limits, including tracer calibration uncertainty) and U-Pb age homogeneity on the scale used in LA ICP-MS dating. Inhomogeneities in trace element composition due to primary growth zoning prevent its use as a calibration standard for trace element analysis. The content of U varies from 465 ppm in pristine parts of the grains to similar to 3000 ppm in actinide-rich sectors that correspond to pyramidal faces with a high degree of metamictization (present in ca. 30% of the grains). These domains are easily recognized from high intensities on BSE images and should be avoided during the analysis. Hf isotopic composition of the Plesovice zircon (>0.9 wt.% Hf) is homogenous within and between the grains with a mean (176)Hf/(177)Hf value of 0.282492 +/- 0.000013 (2SD). The age and Hf isotopic homogeneity of the Plesovice zircon together with its relatively high U and Pb contents make it an ideal calibration and reference material for laser ablation ICP-MS measurements, especially when using low laser energies and/or small diameters of laser beam required for improved spatial resolution.