Magnesium Isotopic Compositions of International Geological Reference Materials

Magnesium isotopic compositions are reported for twenty‐four international geological reference materials including igneous, metamorphic and sedimentary rocks, as well as phlogopite and serpentine minerals. The long‐term reproducibility of Mg isotopic determination, based on 4‐year analyses of olivine and seawater samples, was ≤ 0.07‰ (2s) for δ²⁶Mg and ≤ 0.05‰ (2s) for δ²⁵Mg. Accuracy was tested by analysis of synthetic reference materials down to the quoted long‐term reproducibility. This comprehensive dataset, plus seawater data produced in the same laboratory, serves as a reference for quality assurance and inter‐laboratory comparison of high‐precision Mg isotopic data.     

Lead Isotopic Composition in Biogenic Certified Reference Materials Determined by Different ICP‐based Mass Spectrometric Techniques

This work presents data for the radiogenic Pb isotopic ratios (²⁰⁶Pb/²⁰⁷Pb and ²⁰⁸Pb/²⁰⁶Pb) in nine biogenic certified reference materials (NIST SRM 1515, 1566b, 1570a, 1573a, 1575a; BCR 100, BCR 101, BCR 670 and IAEA 359), which are suitable for analytical quality control in environmental research. The results were obtained using three different types of ICP‐based mass spectrometer (quadrupole‐based/magnetic sector field single‐collector ICP‐MS instruments and a multi‐collector ICP‐MS) and applying different mass bias correction procedures (calibrator‐sample bracketing and external Tl normalisation) with and without Pb separation from the matrix using ion exchange chromatography. In the majority of the samples, the measurements from all three of the ICP‐MS instruments were in agreement within ± 0.1%, despite the lower analytical precision of the single‐collector ICP‐MS instruments. We demonstrate that the presence of the sample matrix did not significantly influence the Pb isotopic ratios measured by magnetic sector field ICP‐MS, whereas the use of the two different mass bias corrections resulted in a systematic difference of 0.09% for the ²⁰⁸Pb/²⁰⁶Pb ratio.     

Correlation and characterisation of individual glass shards from tephra deposits using trace element laser ablation ICP‐MS analyses: current status and future potential

Laser ablation inductively coupled plasma mass spectrometry (LA‐ICP‐MS) is a high spatial resolution analytical method which has been applied to the analysis of silicic tephras. With current instrumentation, around 30 trace elements can be determined from single glass shards as small as ～ 40 µm, separated from tephra deposits. As a result of element fractionation during the ablation process using a 266 nm laser, a relatively complex calibration strategy is required. Nonetheless, such a strategy gives analyses which are accurate (typically within ±5%) and have an analytical precision which varies from ～ ±2% at 100 ppm, to ～ ±15% at 1 ppm. Detection limits for elements used in correlation and discrimination studies are well below 1 ppm. Examples of the application of trace element analysis by LA‐ICP‐MS in tephra studies are presented from the USA, New Zealand and the Mediterranean. Improvements in instrumental sensitivity in recent years have the potential to lower detection limits and improve analytical precision, thus allowing the analysis of smaller glass shards from more distal tephras. Laser systems operating at shorter wavelengths (e.g. 193 nm) are now more widely available, and produce a much more controllable ablation in glasses than 266 nm lasers. Crater sizes of <10 µm are easily achieved, and at 193 nm many of the elemental fractionation issues which mar longer wavelengths are overcome. By coupling a short wavelength laser to a modern ICP‐MS it should be possible to determine the trace element composition of glass shards as small as 20 µm and, providing sample preparation issues can be overcome, the determination of the more abundant trace elements in glass shards as small as 10 µm is within instrumental capabilities. This will make it possible to chemically fingerprint tephra deposits which are far from their sources, and will greatly extend the range over which geochemical correlation of tephras can be undertaken. Copyright © 2007 John Wiley & Sons, Ltd.     

Anomalous lead isotope ratios and provenance of offshore sediments,Gulf of Carpentaria,northern Australia

Anomalous Pb isotope ratios measured by Inductively Coupled Plasma Mass Spectrometry in terrigenous marine sediments (<63 μm fraction) from the Gulf of Carpentaria originated from depositional mixing of clay/silt with average modern crustal Pb isotope ratios and detrital monazite with high ²⁰⁸Pb/²⁰⁶Pb and low ²⁰⁷Pb/²⁰⁶Pb. This interpretation is supported by strong correlations between Pb isotope ratio and Th, U and light rare‐earth element concentrations in the sediments as well as by monazite compositional data. A likely source of the detrital monazite is the western portion of the Georgetown Inlier of mainly Proterozoic S‐type granitic rocks. A clear distinction between Pb isotope ratios in sediments deposited from the Norman and Bynoe Rivers in the southeast Gulf of Carpentaria and the persistence of catchment‐specific Pb isotope ratios 45 km offshore suggest that Pb isotope data are useful in tracing the provenance of terrigenous offshore sediments when the source rocks of catchments show sufficient chemical and/or mineralogical variation.     

Determination of Trace Elements in Geological Reference Materials G‐3, GSP‐2 and SGD‐1a by Low‐Dilution Glass Bead Digestion and ICP‐MS

We present a revised alkali fusion method for the determination of trace elements in geological samples. Our procedure is based on simple acid digestion of powdered low‐dilution (flux : sample ≈ 2 : 1) glass beads where large sample dilution demanded by high total dissolved solids, a main drawback of conventional alkali fusion, could be circumvented. Three geological reference materials (G‐3 granite, GSP‐2 granodiorite and SGD‐1a gabbro) decomposed by this technique and routine tabletop acid digestion were analysed for thirty trace elements using a quadrupole ICP‐MS. Results by conventional acid digestion distinctly showed poor recoveries of Zr, Hf and rare earth elements due to incomplete dissolution of resistant minerals. On the other hand, results obtained by our method were in reasonable agreement with reference data for most analytes, indicating that refractory minerals were efficiently dissolved and volatile loss was insignificant.     

新疆西昆仑中太古界古陆核的确定及地质意义

原赫罗斯坦岩群为一套无序变质核杂岩,岩性为混合岩化花岗质片麻岩、紫苏辉石麻粒岩等。岩石组合及地球化学特征都具TTG岩石特征。采用LA-ICP-MS方法测定锆石U-Pb年龄值3137.3±4.1Ma,反映其时代为中太古代,代表赫罗斯坦杂岩原岩生成年龄。由此说明,塔里木南缘铁克里克地区存在太古宙大陆核,为新疆境内所发现的最古老岩系之一。     

Geochronologies of the Huaixi copper-gold deposit and the Caomen alkaline granite,SE China: implications for tectonic evolution

The Huaixi copper-gold polymetallic deposit of SE Zhejiang Province, China, is a typical hydrothermal-vein ore body. The Caomen K-feldspar granite porphyry, the dominant intrusion in the mining district, has been dated by laser ablation inductively coupled plasma mass spectrometry (LA–ICP–MS) analyses of zircon, which yielded a weighted mean ²⁰⁶Pb/²³⁸U age of 101.6 ± 0.9 Ma (MSDW?=?1.3). Rb-Sr dating of fluid inclusions in auriferous quartz from ore bodies yielded an isochron age of 101 ± 2 Ma. These results indicate that intrusion of the Caomen pluton and Cu-Au mineralization was contemporaneous and corresponds to the third episode of Mesozoic magmatism and metallogenesis in South China. Calculated δ¹⁸O values of fluid inclusions from ore-bearing quartz range from??0.89 to??1.98‰ and δD from??42.60 to??60.20‰, suggesting that the ore-forming fluids are derived from a mixed source of magmatic and meteoric waters. δ¹⁸S values of 8 pyrites range from??2.14 to?+4.14‰ with a mean of?+1.67‰, similar to magmatic sulphur. These isotope data support a genetic relationship between the Huaixi copper-gold deposit and the Caomen alkaline granite and probably indicate a common deep source. Petrography and chemical compositions show that the Caomen alkaline granite crystallized from shoshonitic magmas characterized by high SiO₂ (75.64–78.00%) and alkali (K₂O?+?Na₂O?=?7.96–8.82%) but low FeO^T (1.34–3.31%), P₂O₅ (0.05–0.13%) and TiO₂ (0.12–0.18%). The granitic rocks are enriched in Ga, Rb, Th, U, and Pb but depleted in Ba, Nb, Sr, P, and Ti. REEs are characterized by marked negative Eu anomalies (Eu/Eu*?=?0.06–0.13) and exhibit right-dipping ‘V’ patterns with LREE enrichment. These are similar to the Late Cretaceous alkaline granites in the coastal areas of Zhejiang and Fujian provinces, implying that the Caomen granite formed in a post-collisional extensional tectonic setting. Combined with previous studies, we interpret the Huaixi copper-gold deposit and the associated Caomen alkaline granite as related to back-arc extension due to high-angle subduction of the palaeo-Pacific plate, caused by northward movement of the Indian plate.     

西昆仑慕士塔格岩体的LA ICP MS锆石U Pb定年:对古特提斯碰撞时限的制约

慕士塔格岩体是西昆仑造山带出露面积最大的侵入体,主要由黑云母二长花岗岩、似斑状黑云母二长花岗岩和花岗闪长岩组成,其中发育大量的暗色微细粒包体和基性岩浆条带。根据锆石的阴极发光图像以及Th、U、REE元素等特征,所测试的锆石均为典型的岩浆结晶锆石,利用LA-ICP-MS锆石U-Pb定年,测得岩体东西部分的加权平均206Pb/238U年龄分别为229.6±0.8Ma(MSWD=0.44)、232.8±1.5Ma(MSWD=0.21),两者在误差范围内一致,综合获得该岩体年龄为231.4±0.7Ma(MSWD=1.5),属于中三叠世晚期。根据岩石学、锆石内部结构及其REE元素特征,结合前人地球化学资料,该岩体应为壳幔岩浆混合成因。结合区域地质资料,慕士塔格岩体应是从挤压的主碰撞期向伸展后碰撞期转换的产物,表明古特提斯主碰撞作用发生在中三叠世晚期之前,之后开始进入古特提斯后碰撞阶段。     

GGR Biennial Critical Review: Analytical Developments Since 2010

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.     

Determination of Total Sulfur in Fifteen Geological Materials Using Inductively Coupled Plasma‐Optical Emission Spectrometry (ICP‐OES) and Combustion/Infrared Spectrometry

A method for the determination of total sulfur in geological materials by inductively coupled plasma‐optical emission spectrometry (ICP‐OES) is described. We show that good results were obtained using this method even for sample types with very low (< 20 μg g^?1) sulfur concentration (e.g., peridotite). Sulfur was determined in fifteen geological reference materials with different sulfur contents. For reference materials with certified sulfur contents, the ICP‐OES method gave results in excellent agreement with certified values, and uncertainties better than 4% RSD. ICP‐OES results for sulfur in other reference materials yielded RSDs better than 10%, where S concentrations were > 100 μg g^?1 (except for diabase W‐2a, 16% RSD). Reference materials with lower sulfur contents (< 40 μg g^?1) showed much higher RSDs (17–18%). Except for RMs with certified values for sulfur, most data obtained by the combustion infrared detection method generally showed higher concentrations than those measured by ICP‐OES and a better RSD (≤ 8% for all materials except DTS‐2b).