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1.
Anastassia Yu. Borisova Rémi Freydier Mireille Polvé Stefano Salvi Frederic Candaudap Thierry Aigouy 《Geostandards and Geoanalytical Research》2008,32(2):209-229
Microscopic melt inclusions found in magmatic minerals are undoubtedly one of the most important sources of information on the chemical composition of melts. This paper reports on the successful application of near-infrared (NIR) femtosecond laser ablation (LA) - inductively coupled plasma-mass spectrometry to in situ determination of incompatible trace elements (Li, Rb, Sr, Y, Zr, Nb, Cs, Ba, REE, Ta, Th, U) and ore metals (As, Mo, Pb) in individual melt inclusions hosted in quartz from the Mount Pinatubo dacites, Philippines. The determined elements cover a concentration range of five orders of magnitude. Femtosecond LA-ICP-MS analyses of twenty-eight individual melt inclusions demonstrate the efficiency of the microanalytical technique and suggests a spectacular homogeneity of the entrapped melt, at least with respect to the following incompatible trace elements: Rb, Sr, Nb, Cs, Ba, La, Ce, Pr, Nd, Pb, Th. The analytical precision (1s) for Na, Ca, Rb, Sr, Y, Nb, Ba and LREE ranged from 3 to 20%. Comparison of trace element concentrations in Mt. Pinatubo melt inclusions determined by femtosecond LA-ICP-MS with those of melt inclusions previously analysed by secondary ion mass spectrometry analysis (SIMS) and those of matrix glasses previously determined by nanosecond LA-ICP-MS showed an agreement typically within 30–40%. The homogeneity of trace element concentrations of the Mt. Pinatubo melt inclusions and the matrix glasses is consistent with the melt inclusion origin as homogeneous rhyolitic melt that was trapped in quartz phenocrysts at the final crystallisation stages of the host adakite (dacite) magma. 相似文献
2.
Masanori Kurosawa Kunihiro Shima Satoshi Ishii Kimikazu Sasa 《Geostandards and Geoanalytical Research》2006,30(1):17-30
The concentrations of fifty trace elements, including relatively volatile elements and transition metal elements, in fused glasses of Geological Survey of Japan rock reference materials GSJ JR-2, JA-1, JA-2, JB-1a, JB-3, JGb-1 and JF-1 were determined by particle (proton) induced X-ray emission (PIXE) and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS). The fused glasses were prepared by rapid fusion and subsequent quenching in welded platinum capsules and were found to be homogeneous for major elements and for trace elements with concentrations of more than 1 μg g-1 within the observed precision (± 10% mean) on a 70 μm sampling scale. The values obtained by PIXE and LA-ICP-MS for the transition elements (Cr, Mn, Fe, Ni and Cu), the relatively volatile elements (Zn, Ga, Rb and Pb) and the refractory elements (Y, Zr, Nb and Th) with concentrations greater than a few μg g-1 showed good agreement (within 10 % relative difference). The values for almost all the elements detected at concentrations higher than 1 μg g-1 as determined by LA-ICP-MS also agreed well with the reference values (mean relative difference < ± 10%), except for B and Cu. The good agreement confirmed the appropriateness of the NIST SRM 600 series glass calibration reference material for LA-ICP-MS analysis of glasses with variable major-element compositions for almost all elements. The concentrations of Cu in all the samples were lower than the reference values, which was attributed to adsorption of the transition metals onto the platinum capsule during preparation. 相似文献
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Determination of REE, Y, Nb, Zr, Hf, Ta, Th and U in Geological Reference Materials LSHC-1 and Amf-1 by Solution and Laser Ablation ICP-MS 总被引：1，自引：0，他引：1
Elena V. Smirnova Belinda Flem Elena A. Anchutina Irina N. Mysovskaya Valeriy I. Lozhkin Lev L. Petrov † 《Geostandards and Geoanalytical Research》2010,34(1):49-65
This paper presents data on REE and Y, Nb, Zr, Hf, Ta, Th and U abundances for two candidate reference materials (RMs), spinel lherzolite LSHC-1 and amphibole Amf-1, being currently developed at the Institute of Geochemistry SB RAS, Irkutsk. To determine the contents of these elements inductively coupled plasma-mass spectrometry was applied with: (i) solution nebulisation (solution ICP-MS) and (ii) laser ablation (LA-ICP-MS) of fused glass disks. The precision of results obtained by both techniques was better than 6% RSD for most elements. Accuracy was assessed by using the geochemical RMs JB-2, JGb-1 (GSJ) and MAG-1 (USGS). The trace element results by solution ICP-MS for JGb-1 and JB-2 agree with reference values presented by Imai et al. (1995, this Journal) within 1–10%. Significant differences were found for Nb and Ta determinations. The accuracy of LA-ICP-MS results evaluated by RM MAG-1 was within 4%, except for Eu (about 10%). The analytical results obtained for LSHC-1 and Amf-1 by solution ICP-MS and LA-ICP-MS were in good agreement with each other and with INAA and XRF data presented for the certification of these RMs. They can be considered as the indicative values for assigning certified values to the above-mentioned RMs. 相似文献
5.
Zongshou Yu Marc D. Norman Philip Robinson 《Geostandards and Geoanalytical Research》2003,27(1):67-89
Major and trace element compositions of fifteen silicate rock reference materials have been determined by a combined XRF and laser ablation ICP‐MS (LA‐ICP‐MS) technique on glasses prepared by fusing the sample with a lithium borate flux (sample:flux = 1:3). Advantages of this technique include the ability to measure major and trace element abundances on a single sample using a quick and simple preparation that attacks resistant phases such as zircon without the need for acid dissolution. The method is suitable for a wide variety of bulk compositions including mafic, intermediate and silicic rocks. Abundance‐normalized mass response patterns (the ratio of signal intensity to element concentration) of the LA‐ICP‐MS analyses vary systematically with major element composition, demonstrating the presence of a matrix effect that cannot be compensated by normalisation to a single internal standard element. Increasing the sampling distance between the ICP‐MS cone and the torch reduces the magnitude of this effect, suggesting that a mechanism related to residence time of ablated particles in the plasma may be at least partially responsible for the observed variations in mass response patterns. When using a matrix‐matched calibration, agreement of the LA‐ICP‐MS results with published reference values or those obtained by solution ICP‐MS is 10% relative. Analytical precision based on replicate analyses is typically 5% RSD. Procedural detection limits that include contributions from gas background and flux are 0.01‐0.1 μg g‐1 for the heavy mass trace elements (Rb‐U). Major element analyses by XRF show excellent agreement with results obtained using a conventional heavy element absorbing flux. High quality major and trace element data for silicate rocks can be achieved by a combined XRF and LA‐ICP‐MS analysis of Li2B4O7/LiBO2 fused glasses provided an appropriate matrix‐matched calibration is adopted. 相似文献
6.
Synthesis and Preliminary Characterisation of New Silicate, Phosphate and Titanite Reference Glasses 总被引：3，自引：0，他引：3
Stephan Klemme Stefan Prowatke Carsten Münker Charles W. Magee Yann Lahaye Thomas Zack Simone A. Kasemann E. Joan A. Cabato Benjamin Kaeser 《Geostandards and Geoanalytical Research》2008,32(1):39-54
Eleven synthetic silicate and phosphate glasses were prepared to serve as reference materials for in situ microanalysis of clinopyroxenes, apatite and titanite, and other phosphate and titanite phases. Analytical results using different micro-analytical techniques showed that the glass fragments were homogeneous in major and trace elements down to the micrometre scale. Trace element determinations using inductively coupled plasma-mass spectrometry (ICP-MS), multi-collector inductively coupled plasma-mass spectrometry (MC-ICP-MS), laser-ablation inductively coupled plasma-mass spectrometry (LA-ICP-MS) and secondary ionisation mass spectrometry (SIMS) showed good agreement for most elements (Li, Be, B, Cs, Rb, Ba, Sr, Ga, Pb, U, Th, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Er, Tm, Yb, Lu, Zr, Hf, Ta, Nb) studied and provide provisional recommended values. 相似文献
7.
Jean-Claude GERMANIQUE 《Geostandards and Geoanalytical Research》1994,18(1):91-100
Major and trace elements have been determined by wavelength dispersive X-ray fluorescence and by inductively coupled plasma optical emission spectroscopy (ICP-OES), in the Geological Survey of Japan Igneous rock series, using a routine sample preparation technique including lithium borate fusion. Samples were analysed for 10 majors elements and the following trace elements: Ba, Co, Cr, Ga, Nb, Sc, Sr, V, Y, Zn and Zr. The rare-earth elements were determined only by ICP-OES following separation by ion exchange. In most cases, results compared well with published values. 相似文献
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The paper presents preliminary results of the use of a high resolution double-focussing, magnetic sector inductively coupled plasma-mass spectrometer (HR-ICP-MS) with ultraviolet laser ablation (LA) for the bulk analysis of geological materials fused with Li2 B4 O7 . Detection limits are based on data from precision measurements of a fused SiO2 sample of high purity, and sensitivity data (cps/μg g-1 ) obtained on the Reference Material (RM) Syenite SY-2. For many trace elements, the detection limits are better than 0.05 μg g-1 using a sample to flux weight ratio of 1:7.
Calibration curves, which are based entirely on RMs, are established for Hf, Ta, Tb, Tm and Lu. They indicate that, even at this early stage in the development of the technique, data accurate to ˜ 25% can be collected. It is concluded that the method may prove to be a valuable supplement to XRF for low level element concentration measurements; it is also very practical, as the same sample discs can be used for both XRF and LA-ICP-MS analyses. 相似文献
Calibration curves, which are based entirely on RMs, are established for Hf, Ta, Tb, Tm and Lu. They indicate that, even at this early stage in the development of the technique, data accurate to ˜ 25% can be collected. It is concluded that the method may prove to be a valuable supplement to XRF for low level element concentration measurements; it is also very practical, as the same sample discs can be used for both XRF and LA-ICP-MS analyses. 相似文献
10.
Emelie Axelsson Jonas Pape Jasper Berndt Fernando Corfu Klaus Mezger Michael M. Raith 《Geostandards and Geoanalytical Research》2018,42(3):319-338
A new natural rutile reference material is presented, suitable for U‐Pb dating and Zr‐in‐rutile thermometry by microbeam methods. U‐Pb dating of rutile R632 using laser ablation ICP‐MS with both magnetic sector field and quadrupole instruments as well as isotope dilution‐thermal ionisation mass spectrometry yielded a concordia age of 496 ± 2 Ma. The high U content (> 300 μg g?1) enabled measurement of high‐precision U‐Pb ages despite its young age. The sample was found to have a Zr content of 4294 ± 196 μg g?1, which makes it an excellent complementary reference material for Zr‐in‐rutile thermometry. Individual rutile grains have homogeneous compositions of a number of other trace elements including V, Cr, Fe, Nb, Mo, Sn, Sb, Hf, Ta and W. This newly characterised material significantly expands the range of available rutile reference materials relevant for age and temperature determinations. 相似文献
11.
A critical evaluation of trace element data derived by energy dispersive X-ray fluorescence (ED-XRF) analysis of over 40 geochemic reference samples shows that results for Rb, Sr, Y, Zr, Nb, and Th can be at least as good in terms of precision (better than ± 2 ppm (2s) or ± 3 % (2s relative), accuracy, and 3s detection limits (2 to 4 ppm) as those obtainable by other routine multi-element analytical techniques. Data obtained simultaneously for Ni, Cu, Zn, Ga, Pb and U are less precise because excitation conditions are less well optimised (with 3s detection limits of 6 to 12 ppm). The quality of data and the efficiency of simultaneous analysis of both sets of elements is well-suited to most geological applications. Following a critical appraisal of calibration accuracy, new trace element data are presented for 15 reference samples from the Geological Survey of Japan. 相似文献
12.
三江北段贡觉三叠纪火山岩是金沙江古特提斯洋向西俯冲消减及随后的弧陆碰撞造山作用的产物,主要由玄武岩、安山质熔结凝灰岩和安山岩等组成,对探讨金沙江古特提斯构造-岩浆演化过程具有重要意义.对贡觉火山岩进行了LA-ICP-MS锆石U-Pb定年和全岩主、微量元素研究.其中代表性样品安山质熔结凝灰岩的LA-ICP-MS锆石U-Pb定年结果显示,锆石23个分析点的206Pb/238U年龄为243~233 Ma,206Pb/238U加权平均年龄为238.3±1.3 Ma（MSWD=1.7,n=23）,代表了岩浆的结晶年龄为中-晚三叠世.地球化学分析表明,火山岩以低钛（0.52%~0.91%）、中镁（3.38%~7.22%）、富钠（3.63%~4.66%）、贫钾（0.09%~4.05%）、富集轻稀土元素（LREE/HREE=4.09~13.27）和大离子亲石元素（Th、U、La、Sm）、亏损高场强元素Nb和Ta（Nb=2.51×10-6~24.5×10-6、Ta=0.22×10-6~1.89×10-6）为特征,La/Nb值（2.13~2.89）较高、Nb/Th值（1.12~1.62）相对较低,具有与岛弧型或晚碰撞造山型火山岩相似的主-微量元素组成特征.贡觉中-晚三叠世火山岩代表了金沙江古特提斯演化过程中晚碰撞造山阶段的岩浆响应,推测是晚碰撞过程中残留的金沙江洋壳物质与岩石圈地幔物质相互作用的结果. 相似文献
13.
甘肃北山小西弓金矿区石英正长斑岩LA-ICP-MS锆石U-Pb年龄和地球化学特征 总被引：1，自引：0，他引：1
通过高精度的LA-ICP-MS锆石U-Pb测年,获得北山南带小西弓金矿区石英正长斑岩的形成年龄为247.5±2.2Ma,属中三叠世。地球化学分析表明,该岩体为准铝质、钾玄岩系列,主量元素高硅(Si O_2=65.8%~66.2%)、富碱(Na_2O+K_2O=8.99%~9.41%)、低钙(Ca O=1.72%~2.19%)、贫镁(Mg O=0.63%~0.70%);轻稀土元素富集,重稀土元素亏损,弱负Eu异常。大离子亲石元素Rb、Th、U、K和Pb富集,同时Ba、Sr、P、Ti和Eu亏损,并具高104*Ga/Al值和高Zr+Nb+Ce+Y含量,表现出A型花岗岩的特征。北山南带三叠纪岩浆活动强烈,高分异I型-A型花岗岩大量发育,暗示区域内三叠纪处于造山后伸展环境。 相似文献
14.
激光剥蚀电感耦合等离子体质谱测定岩石样品中稀土元素 总被引：10，自引：0，他引：10
以NIST612玻璃标准为外标校正物质, 采用42Ca为内标校正灵敏度漂移、基体效应、剥蚀效率及进样量的变化.将LSX-2 0 0激光剥蚀进样系统与POEMSIII电感耦合等离子体质谱仪联用, 对国际标准物质BCR-2 (玄武岩) 及国内标准物质GSR-11 (花岗岩) 玻璃熔饼进行了稀土元素的测定, 建立了LA -ICP -MS整体分析岩石样品中稀土元素的方法.结果表明, 绝大多数稀土元素准确度优于15 %, 测定精度(RSD) 小于10 %.稀土元素的检出限(LOD) 在21.4×10-9~23 1.6×10-9之间, 样品分析速度为2 0样品/h.在Excel软件下用VBA语言编制宏, 实现了脱机数据处理的自动化, 极大提高了工作效率. 相似文献
15.
Brigitte Stoll Klaus Peter Jochum Kirstin Herwig Marghaleray Amini Michael Flanz Berthold Kreuzburg Dmitry Kuzmin Matthias Willbold Jacinta Enzweiler 《Geostandards and Geoanalytical Research》2008,32(1):5-26
In this paper we describe a flux‐free fusion technique for the highly precise LA‐ICP‐MS bulk analysis of geological samples. For this purpose we have developed an automated iridium‐strip heater with temperature and melt time control. To optimise the homogeneity of the fused glasses and to reduce possible depletion of volatile elements during melting, we undertook experiments with basaltic rock and glass powders using different melting temperatures (1300–1700 °C) and melting times (5‐80 s). Major and trace element microanalysis was performed using EPMA and LA‐ICP‐MS. Homogeneous glasses were obtained for temperatures ≥ 1500 °C and melting times ≥ 10 s. High loss (20‐90%) of highly volatile elements (e.g., Cs, Ge, Sn, Pb) was observed for high melting temperatures (≥ 1600 °C) and long melting times (80 s). Standard melting conditions (1600 °C, 10 s) represent a compromise, as the glasses were homogeneous with respect to major and trace elements and, at the same time, were not depleted in elements with condensation temperatures (at a pressure of 10?4 bar) higher than about 900 K (e.g., Zr, Hf, Ba, Sr, REE, U, Mo, Ni, Rb, Ga). Several international geological reference materials with SiO2 ranging between 47% m/m and 59% m/m were prepared using our standard melting conditions (1600 °C, 10 s) and subsequently analysed by LA‐ICP‐MS. These samples also include the new Brazilian basaltic reference material BRP‐1. Matrix‐matched calibration of the LA‐ICP‐MS data was performed using the basaltic reference glasses KL2‐G, ML3B‐G, BCR‐2G and BHVO‐2G. Most analytical data agreed within uncertainty at the 95% confidence level with the GeoReM preferred values published in the GeoReM database for reference materials of geological and environmental interest. To demonstrate routine bulk LA‐ICP‐MS analyses of geochemical and cosmochemical samples using the whole rock fusion technique, we also present trace element data for ocean island basalts from Lanai (Hawaii) and of Martian meteorites. 相似文献
16.
Luo Yan Liu Yongsheng Hu Shenghong Gao Shan Open Laboratory of Constitution Interaction Dynamics of the Crust Mantle System Ministry of National Lands Resources China University of Geosciences Wuhan Lin Shoulin Faculty of Material Sc 《中国地质大学学报(英文版)》2001,12(3)
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17.
本文研究了以粉末样品直接压片,铑靶X光管的康普顿散射线作内标和背景的扣除,测定地质样品中微量铌、锆、钇、铷、锶、铀、铜和锌等元素的X射线光谱分析方法。本法具有制备样品简便快速、扣除背景简易准确以及能较好地克服基体效应、方法检测限较低(<2ppm)等优点。方法的精密度与准确度符合分析误差要求。因而本法是测定岩石样品中微量元素的一种简便快速且又较为准确的分析方法。 相似文献
18.
ICP-MS测定地质样品中37个元素的准确度和长期稳定性分析 总被引：8，自引：10，他引：8
对Elan6100DRC型ICP-MS近五年来所测得的国际地质标样BHVO-1(玄武岩)和AGV-1(安山岩)中的37个元素的测定值以及仪器灵敏度的长期漂移情况进行了统计分析(共计146次)。结果表明,几年来ICP-MS所测数据的长期稳定性和准确度都较好,除个别元素Li(BHVO-1)、Be(BHVO-1))、Cr(AGV-1)、Cs(BHVO-1)和Pb(BHVO-1)的相对误差(与参考值比较)接近或略大于10%外,绝大多数元素的相对误差和相对标准偏差(RSD,测定值之间,n=146)都在5%以内;仪器灵敏度并不是随着时间一直往下漂,有的是往上漂的,也有上下漂的,即使是在同一时间内,有的元素灵敏度往上漂,而有的往下漂。常用的内标法无法较好校正这种漂移,而需要采用内外标相结合的校正方法。不同批次,210个各种地质样品中Rb、Sr、Zr和Nb的XRF和ICP-MS分析结果对比情况表明,绝大多数样品中Rb、Sr、Zr和Nb的ICP-MS和XRF的测定值的相对误差小于10%。以上的分析结果表明,我们实验室所建立的以密闭高温高压消解技术为样品前处理方法,以模拟地壳样品中元素天然丰度比的基体匹配校正标准溶液为外标和以Rh为内标结合外标校正的ICP-MS多元素分析方法具有非常好的准确度和长期稳定性。 相似文献
19.
A Comparison of In Situ Analytical Methods for Trace Element Measurement in Gold Samples from Various South African Gold Deposits 
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下载免费PDF全文 Christoph Gauert Mathias Schannor Lutz Hecht Martin Radtke Uwe Reinholz 《Geostandards and Geoanalytical Research》2016,40(2):267-289
Trace element concentrations in gold grains from various geological units in South Africa were measured in situ by field emission‐electron probe microanalysis (FE‐EPMA), laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS) and synchrotron micro X‐ray fluorescence spectroscopy (SR‐μ‐XRF). This study assesses the accuracy, precision and detection limits of these mostly non‐destructive analytical methods using certified reference materials and discusses their application in natural sample measurement. FE‐EPMA point analyses yielded reproducible and discernible concentrations for Au and trace concentrations of S, Cu, Ti, Hg, Fe and Ni, with detection limits well below the actual concentrations in the gold. LA‐ICP‐MS analyses required larger gold particles (> 60 μm) to avoid contamination during measurement. Elements that measured above detection limits included Ag, Cu, Ti, Fe, Pt, Pd, Mn, Cr, Ni, Sn, Hg, Pb, As and Te, which can be used for geochemical characterisation and gold fingerprinting. Although LA‐ICP‐MS measurements had lower detection limits, precision was lower than FE‐EPMA and SR‐μ‐XRF. The higher variability in absolute values measured by LA‐ICP‐MS, possibly due to micro‐inclusions, had to be critically assessed. Non‐destructive point analyses of gold alloys by SR‐μ‐XRF revealed Ag, Fe, Cu, Ni, Pb, Ti, Sb, U, Cr, Co, As, Y and Zr in the various gold samples. Detection limits were mostly lower than those for elements measured by FE‐EPMA, but higher than those for elements measured by LA‐ICP‐MS. 相似文献
20.
Paul J. Sylvester 《Geostandards and Geoanalytical Research》2005,29(1):41-52
This annual review of laser-ablation inductively coupled plasma-mass spectrometry (LA-ICP-MS) covers the year 2003. Significant advances were made in understanding laser-sample interactions. In particular, research defined the distribution of particle sizes produced by the interplay of laser wavelength, laser pulse width and the gas environment of ablation. A link between particle sizes and elemental and isotopic fractionation at both the ablation site and in the ICP was established. Experimental 15 7 nm and femtosecond laser systems were tested with promising results. The number of applications of LA-ICP-MS in geology and environmental Earth science continued to grow with particular interest in element concentration and isotope ratio profiling of materials, linking composition to time scales. In situ isotopic ratio measurements were increasingly made using multicollector magnetic sector ICP-MS instruments. Other applications of wide interest included bulk sampling of rocks and ores prepared as lithium borate glasses; low level analysis of platinum-group elements, rhenium and gold in sulfides, metal and silicates; in situ uranium-lead zircon geochronology; and melt and fluid inclusion analysis. 相似文献