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1.
The geochemistry of Re-Os and the recent use of Re as a non-traditional stable isotope both need accurate and precise quantification of 187Re/185Re ratios. This paper reports rhenium isotopic data obtained from the analysis of a standard solution and geological samples by MC-ICP-MS. We show that measured isotopic ratios are modified by matrix effects that cannot be accounted for by the standard solution bracketing technique. The bias resulting from measurements on a spiked (185Re-enriched) sample is shown to alter the apparent Re concentration by several percent. When spiking samples and calibrators with tungsten, simultaneous measurement of tungsten and rhenium isotopes compensates for the matrix-induced modification of mass bias. Rhenium and tungsten are shown to have different fractionation factors. This may be due to the fact that the two elements fractionate in a different but systematic way, or that the reference isotopic ratios used for elemental Re and W are incoherent with one another. The consistency of fractionation through time can be used to obtain an empirical relationship between W and Re measured ratios from a standard solution to obtain a sample's fractionation-corrected 187Re/185Re spiked ratio on samples containing pg g−1 levels of Re, even if some matrix capable of affecting mass bias remains in the final solution.  相似文献   

2.
Application of Laser Ablation ICP-MS to U-Th-Pb Dating of Monazite   总被引：2，自引：1，他引：2  
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.  相似文献   

3.
An igneous zircon reference material (OG1) was characterised for U-Pb isotopes by ID-TIMS, and utilised to evaluate SIMS (SHRIMP) instrumental mass fractionation (IMF) of radiogenic Pb isotopes (207Pb*/206Pb*). The TIMS 207Pb*/206Pb* reference value for OG1 was 0.29907 ± 0.00011 (95% confidence limit), 3465.4 ± 0.6 Ma. The high 207Pb* (∼ 30 μg g−1), negligible common Pb, and isotopic homogeneity permitted precise (± 1–2‰) 207Pb*/206Pb* measurements within the analytical sessions. External reproducibility of mean 207Pb*/206Pb* ratios between sessions was demonstrated for one instrument, yielding a mean IMF of +0.87 ± 0.49‰. The mean 207Pb*/206Pb* ratios between instruments were dispersed beyond uncertainties, with session IMF values from +3.6 ± 1.7‰ to −2.4 ± 1.3‰, and a grand mean IMF value (twenty-six sessions) of +0.70 ± 0.52‰, indicating a tendency towards elevated 207Pb*/206Pb*. The specific causes of variability in IMF are unclear, but generally reflect subtle differences in analytical conditions. The common practice in SIMS of assuming that IMF for Pb+ is insignificant could result in systematic age biases and underestimated uncertainties, of critical importance for precise correlation of Precambrian events. Nevertheless, a zircon RM such as OG1 can be readily incorporated into routine dating to improve 207Pb*/206Pb* accuracy and external reproducibility.  相似文献   

4.
In this study, the Cd isotopic composition of various geological reference materials and anthropogenic samples was investigated. The measurements were made by multicollector ICP-MS and instrumental mass fractionation was controlled using a "sample-standard bracketing" technique. Cadmium isotopic data are reported relative to an internal Cd solution (Cd Spex) and expressed as the 114 Cd/110Cd delta value. Two other Cd solutions (Prolabo and JMC) were analysed and yielded the same 0% delta value. A fractionated Cd metal sample (Münster Cd) was used as a secondary reference material for Cd isotopic measurements and we obtained a 114 Cd/110 Cd delta value of 4.48% relative to Cd Spex solution. As opposed to multi-stage Cd purification previously published in the literature, a new one step anionic exchange purification using dilute HCl for the analysis of Cd isotopes in geological samples was developed. This method enabled a high recovery (> 95%) and effective separation of the sample matrix to be achieved. The long-term external reproducibility was evaluated at 0.12% (2 standard deviations) for the 114 Cd/110Cd ratio, based on reference solutions and replicated measurements of samples over one year. The variation of Cd isotopic composition of natural terrestrial samples is restricted to a small range of 0.4%, which is similar to previously reported results. In contrast, large variations of Cd isotopic composition were found for anthropogenic samples with values as low as −0.64% for a dust sample issued from a lead smelter and values as high as +0.50% for NIST SRM 2711 (metal-rich soil). These variations are 10 times larger than the reproducibility and suggest that Cd isotopes can be useful as tracers of anthropogenic sources of Cd in the environment.  相似文献   

5.
This paper reports an investigation into the suitability of the neutron-activation method, by use of the reaction 238 U(n,γ) 239 U with detection of the gamma-rays from the daughter 239 Np, for the determination of uranium in 10 proposed reference materials. 182 Ta was used to monitor the neutron flux. The precision of measurement varied from 0.92 to 2.7 per cent. Results compare favourably with those obtained by other analytical procedures, and show that this established method can be used to yield useful and independent results in the preparation of uranium reference materials.  相似文献   

6.
A new method has been developed for the simultaneous determination of Pb abundance and Pb isotopic composition with high precision and accuracy for small test portion masses by thermal ionisation mass spectrometry. In this method, a 205pb-204pb double spike is added to samples prior to the chemical separation of Pb, and the isotopic composition of the spike-sample mixture is determined rigorously by the double spike technique using a 207Pb-204Pb spike. The isotopic composition and concentration of Pb in the sample are then obtained by utilising the principle of isotope dilution. Using this technique, replicate determinations of Pb from NIST SRM 981 and GSJ JP-1 (peridotite; 0.07 μg g−1 Pb) were performed. The measured concentration and isotopic data were identical, within uncertainty, to published data or to data that were determined independently in this study. The application of this method to U-Pb dating and the determination of the "initial" Pb isotopic composition was also tested. Lead isotopic compositions and the concentrations of Pb, Th and U were determined for a single batch of samples, through the addition of 205pb-204pb, 230Th and 235U spikes to samples prior to chemical separation. Also in these experiments, we confirmed that this routine gives accurate data for Pb, Th and U concentrations and Pb isotopic compositions.  相似文献   

7.
For studies of mass-dependent fractionation of calcium isotopes in natural materials, the 48Ca/42Ca ratio is a superior choice to the conventionally measured 44Ca/40Ca ratio for two important reasons. These are (1) mass-dependent fractionation can be determined free from the effects of inherited or ingrown radiogenic 40Ca and (2) this ratio increases the spread of measured isotopic masses by 50%, resulting in statistically better resolution of fractionation, assuming similar precision. A third, though strictly technical, advantage is the inherent ability of a mass spectrometer to measure ratios close to unity (48Ca/42Ca) more precisely than very small or large ratios (44Ca/40Ca). However, because of the very low natural abundance of both 48Ca and 42Ca, their ratio has been very difficult to measure, the only attempt so far being on a high mass resolution MC-ICP-MS with a precision of 0.33%. We report here determination of the 48Ca/42Ca ratio by the more commonly available and user-friendly multi-collector TIMS using a 43Ca-46Ca double-spike, with a significantly better precision of 0.18% (2s). The 48Ca/40Ca or 44Ca/40Ca ratio can also be measured in the same mass spectrometer run to provide complementary information on any radiogenic component.  相似文献   

8.
Liqiang Yang    Jun Deng    Chunying Guo    Jing Zhang    Shaoqing Jiang    Bangfei Gao    Qingjie Gong    Qingfei Wang 《Resource Geology》2009,59(2):181-193
The Dayingezhuang gold deposit is located in the central part of the Zhaoping Fault Zone, which is one of the most important gold-hosting faults in the Jiaodong gold province of China. Dayingezhuang is a typical large-scale shear zone-hosted disseminated gold deposit with superimposed silver mineralization. Fluid inclusion (FI) petrography and microthermometry, and analysis of oxygen and hydrogen isotopes for fluid inclusions were conducted to determine the characteristics of the ore-forming fluids and the processes of silver mineralization. Microthermometry data of FI indicated that ore-forming fluids are characterized by low salinity and low density. Homogenization pressures of FI are estimated at 20 × 105–220 × 105 Pa. The change in ore-forming fluids from K2SO4 type to NaCl type indicates the superposition of two hydrothermal mineralizing events. Ore-forming fluids were dominated by magmatic components in the early mineralization period, and affected by meteoric waters in the late period. Gold may have been transported as Au-S or Au-Cl complexes, whereas silver was transported as Ag-Cl complexes. Early fluid boiling and later fluid mixing are thought to be two of the main factors causing the deposition and superimposing of gold and silver to form the large deposit.  相似文献   

9.
We have developed a new chemical procedure for the quantitative separation of molybdenum (Mo) and rhenium (Re) from a wide variety of geological samples. A single pass anion exchange separation provided complete recovery of pure Mo and Re in a form that was ideal for subsequent isotope and abundance determination by multi-collector inductively coupled plasma-mass spectroscopy (MC-ICP-MS). An enriched 100Mo-97Mo solution, mixed with the sample before digestion, enabled natural mass-dependant isotopic fractionation of Mo to be determined with an external reproducibility of < 0.12‰ (δ98Mo/95Mo, 2 s ). Determination of the concentration of Mo and Re in the same sample was achieved by isotope dilution, with instrumental mass-fractionation of Re being corrected by the simultaneous measurement of the 191Ir/193Ir ratio. We have applied the new procedure to a variety of samples, including seawater, basalt and organic-rich mudrock. The procedure is ideally suited to palaeoredox studies requiring the precise determination of the Mo isotope composition and the Re/Mo ratio from the same sample.  相似文献   

10.
Oxygen and carbon isotopes were measured to a high depth resolution in a nannoplankton carbonate sequence spanning the Cretaceous-Tertiary boundary at Koshak Hill, Mangyshlak Peninsula, Kazakhstan. The boundary is characterized by the presence of a ∼ 1 cm thick clay layer having a sharp peak in iridium concentration with a maximum value of 3.7 ng g-1. The δ18O data reveal rapid (∼103 years) excursion of sea-surface temperature at the boundary where an initial cold pulse is followed by a persistent warm period. The δ13C data, in contrast, indicate only a gradual change in productivity across the boundary. The observations suggest a biogeochemical scenario for the boundary event pertaining to shallow epicontinental seas.  相似文献   

11.
砂岩铀矿成矿过程与氧化还原分带: 铀系不平衡证据   总被引：3，自引：0，他引：3  
铀系不平衡技术被用来研究新疆伊犁盆地库捷尔太砂岩型铀矿床的氧化还原分带和成矿过程.取自该矿床的26个样品的铀、钍含量以及234 U/ 238U, 230 Th/ 234 U和230 Th/ 238U活度比值分别用ICP -MS和α能谱仪进行了测量.不同氧化还原带岩石的铀、钍含量和钍/铀比明显不同: 强氧化带岩石的U、Th含量和Th/U比分别为12.4 μg/g, 4.5 μg/g和0.48; 弱氧化带分别为20.4 μg/g, 5.0 μg/g和0.38; 过渡带(矿化带)分别为169.7μg/g, 4.7μg/g和0.07; 还原带(未蚀变带)分别为6.8μg/g, 3.7μg/g和0.87.其同位素特征亦有明显差异: 氧化带岩石234 U/ 238U大多大于1, 过渡带(矿化带)岩石部分大于或等于1, 部分小于1, 还原带(未蚀变带)岩石大多大于1; 氧化带岩石230 Th/ 234 U和230 Th/ 238U大多大于1, 过渡带(矿化带)岩石大多小于或等于1, 还原带(未蚀变带)岩石大多大于1.这可作为砂岩型铀矿床矿体定位的指示剂.铀系不平衡特征还示踪了该矿床的成矿作用过程.   相似文献   

12.
This paper presents an adapted anion exchange column chemistry protocol which allowed separation of high-purity fractions of Cu and Zn from geological materials. Isobaric and non-spectral interferences were virtually eliminated for consequent multiple-collector ICP-MS analysis of the isotopic composition of these metals. The procedure achieved ∼ 100% recoveries, thus ensuring the absence of column-induced isotopic fractionation. By employing these techniques, we report isotopic analyses for Cu and Zn from five geological reference materials: BCR-027 blende ore (BCR), δ65Cu = 0.52 ± 0.15‰ (n = 10) and δ66Zn = 0.33 ± 0.07‰ (n = 8); BCR-030 calcined calamine ore (BCR), δ66Zn = -0.06 ± 0.09‰ (n = 8); BCR-1 basalt (USGS), δ66Zn = 0.29 ± 0.12‰ (n = 8); NOD-P-1 manganese nodule (USGS), δ65Cu = 0.46 ± 0.08‰ (n = 10) and δ66Zn = 0.78 ± 0.09‰ (n = 9); SU-1 Cu-Co ore (CCRMP), δ65Cu = -0.018 ± 0.08‰ (n = 10) and δ66Zn = 0.13 ± 0.17‰ (n = 6). All uncertainties are ± 2s; copper isotope ratios are reported relative to NIST SRM-976, and zinc isotope ratios relative to the Lyon-group Johnson Matthey metal (batch 3-0749 L) solution, JMC Zn. These values agree well with the limited data previously published, and with results reported for similar natural sample types. Samples were measured using a GVi IsoProbe MC-ICP-MS, based at the Natural History Museum, London. Long-term measurement reproducibility has been assessed by repeat analyses of both single element and complex matrix samples, and was commonly better than ± 0.07‰ for both δ66Zn and δ65Cu.  相似文献   

13.
A direct method for the determination of lead isotopic ratios by laser ablation-inductively coupled plasma-quadrupole mass spectrometry (LA-ICP-QMS) is presented. Samples of lake sediments were ground and pressed as pellets before being analysed. Mass bias was corrected by analysing an external calibration sample manufactured with pure silica doped with NIST SRM 981 solution. The efficiency of the mass bias correction was checked by comparing the ICP-MS data with lead isotopic ratios determined by thermal ionisation mass spectrometry (TIMS). The average long term reproducibilities were 0.40%, 0.40%, 0.20% and 0.30% (RSD) respectively for the 206Pb/204Pb, 207Pb/204Pb, 206Pb/207Pb and 208Pb/206Pb ratios. The method was applied to the study of lake sediment samples, in order to determine the amount and origin of historical contamination by lead.  相似文献   

14.
We present boron isotope and concentration data from magmatic (komatiitic to rhyolitic) and sedimentary geological silicate and artificial glass reference materials that cover a wide spectrum of boron isotope compositions and boron concentrations. Boron isotope compositions were determined by TIMS (Cs2BO2+ -graphite and BO2- method) and boron concentrations by ICP-AES. Boron concentrations ranged from 7 to 159μ g-1 and agree within 14% with published values. Based on replicate analyses of individually prepared sample aliquots an overall external reproducibility of better than 10% was determined. The obtained δ11B values ranged from -12.6 to +13.6% and were reproducible within 1.1 % (2 RSD; excluding NTIMS) on the basis of individually prepared sample aliquots. The δ11B values of JA-1 (+5.3%), JB-3 (+5.9%) and JR-2 (+2.9%) overlap the published data within analytical uncertainty. For the first time δ11B values for the TB (-12.6%) and the MPI-DING glasses GOR-128-G (+13.6%), GOR-132-G (+7.1 %) and StHs6/80-G (-4.5%) are reported. The δ11B values obtained by the Cs2BO2+ -graphite and the BO2- method as well as the majority of δ11B values obtained using different sample preparation methods agree within analytical uncertainty. Therefore, we conclude that none of these analytical methods introduce any systematic error on the obtained δ11B values.  相似文献   

15.
In this paper we address the question of how to determine the period of activity (sedimentation) of fossil (Holocene) fluvial systems in vertically aggrading environments. Our data base consists of almost 100 14C ages (partly AMS) from the Rhine–Meuse delta in the central Netherlands. Radiocarbon samples from the tops of lithostratigraphically correlative organic beds underneath overbank deposits (sample type 1) yield consistent ages, indicating a synchronous onset of overbank deposition over distances of at least up to 20 km along channel belts. Similarly, 14C ages from the base of organic residual channel fills (sample type 3) generally indicate a clear termination of within-channel sedimentation. In contrast, 14C ages from the base of organic beds overlying overbank deposits (sample type 2), commonly assumed to represent the end of fluvial sedimentation, show a large scatter reaching up to 1000 14C years. This setting usually produces 14C ages significantly younger than residual channels of the same fluvial system, indicating the presence of non-depositional unconformities. These usually occur on top of slightly elevated sediment bodies (especially natural levee deposits), which often contain palaeosols. Such hiatuses appear to be much more abundant than hitherto supposed. We conclude that a combination of sample types 1 and 3 generally yields a satisfactory delimitation of the period of activity of a fossil fluvial system. The problems associated with 14C samples of type 2 may also be present in coastal areas with an alternation of tidal deposits and organic beds.  相似文献   

16.
Thirteen geochemical reference standards have been analysed for lithium by a technique originally developed for assay of lithium in biological materials. The technique consists of thermal neutron irradiation, then measurement of 3He from decay of 3H produced via the reaction 6Li(n, α)3H. The results are compared with literature values.  相似文献   

17.
C.J. Eastoe  & T. Peryt 《地学学报》1999,11(2-3):118-131
Routine trace-element geochemistry suggests that components in putative marine halite evaporites may be partly of nonmarine origin, but such interpretations are commonly ambiguous. Stable chlorine isotopes may provide a less-ambiguous marker of chloride origin where δ37Cl departs from the range predicted for evaporite formation from seawater. Bedded halite with primary sedimentary textures preserves original δ37Cl values. Measurable change in δ37Cl can be generated by incongruent dissolution of halite, but only if less than half the original halite remains. Badenian (middle Miocene) halite from the Forecarpathian and from the East Slovakian and Transcarpathian basins has a δ37Cl range of – 0.2 to 0.8‰. Two phenomena cannot be explained by simple evaporation of 0.0‰ seawater. At Wieliczka, the Shaft Salt has distinctive δ37Cl values (– 0.2 to 0.0‰) relative to neighbouring salt beds (0.2 to  0.6‰), requiring a large, abrupt input of brine with negative δ37Cl. Halite with high (0.6 – 0.8‰) δ37Cl near the base of the East Slovakian and Transcarpathian evaporites requires a large input of chloride with positive δ37Cl into the basins. Expulsion of basin brine with non-0‰δ37Cl into the evaporite basins may account for the nonmarine chloride sources.  相似文献   

18.
We report silicon isotopic determinations for USGS rock reference materials BHVO-1 and BHVO-2 using a Nu Plasma multi-collector (MC)-ICP-MS, upgraded with a new adjustable entrance slit, to obtain medium resolution, as well as a stronger primary pump and newly designed sampler and skimmer cones ("B" cones). These settings, combined with the use of collector slits, allowed a resolution to be reached that was sufficient to overcome the 14N16O and 14N2 interferences overlying the 30Si and the 28Si peaks, respectively, in an earlier set-up. This enabled accurate measurement of both δ30Si and δ29Si. The δ value is expressed in per mil variation relative to the NBS 28 quartz reference material. Based on data acquired from numerous sessions spread over a period of six months, we propose a recommended average δ30Si of −0.33 ± 0.05‰ and −0.29 ± 0.11‰ (2se) for BHVO-1 and BHVO-2, respectively. Our BHVO grand mean silicon isotope composition (δ30Si =−0.31 ± 0.06‰) is significantly more negative than the only published value for BHVO-2, but is in very good agreement with the recently established average value of ocean island basalts (OIB), confirming the conclusion that the OIB reservoir has a distinct isotopic composition from the solar reservoir as sampled by chondrites.  相似文献   

19.
We report here a newly developed method for measurement of Li isotopes by use of multi-collector ICP-MS (Neptune) allowing rapid and high precision determination of Li isotope ratios at low levels of lithium (15–20 ng). The lithium reference sample solution IRMM-016 was analysed over a period of ten months with an external reproducibility of 0.24% (2s, n = 52). Chemical separation of Li from matrix was performed on the seawater sample IRMM BCR-403, for which a mean δ7Li value of + 31.0 ± 0.1 % (2s/√n, n = 31) was obtained. This mean value is in good agreement with those previously published for other seawater samples. BCR-403 seawater being readily available, we propose that this seawater sample be used as a reference sample for Li isotope measurements.  相似文献   

20.
Calcium Isotopic Composition of Various Reference Materials and Seawater   总被引：1，自引：0，他引：1  
A compilation of δ44/40Ca (δ44/40Ca) data sets of different calcium reference materials is presented, based on measurements in three different laboratories (Institute of Geological Sciences, Bern; Centre de Géochimie de la Surface, Strasbourg; GEOMAR, Kiel) to support the establishment of a calcium isotope reference standard. Samples include a series of international and internal Ca reference materials, including NIST SRM 915a, seawater, two calcium carbonates and a CaF2 reference sample. The deviations in δ44/40Ca for selected pairs of reference samples have been defined and are consistent within statistical uncertainties in all three laboratories. Emphasis has been placed on characterising both NIST SRM 915a as an internationally available high purity Ca reference sample and seawater as representative of an important and widely available geological reservoir. The difference between δ44/40Ca of NIST SRM 915a and seawater is defined as -1.88 O.O4%o (δ44/42CaNISTSRM915a/Sw= -0.94 0.07%o). The conversion of values referenced to NIST SRM 915a to seawater can be described by the simplified equation δ44/40CaSa/Sw=δ44/40CaSa/NIST SRM 915a - 1.88 (δ44/42CaSa/Sw=δ44/42CaSa/NIST SRM 915a - 0.94). We propose the use of NIST SRM 915a as general Ca isotope reference standard, with seawater being defined as the major reservoir with respect to oceanographic studies.  相似文献   

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