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1.
Further Characterisation of the 91500 Zircon Crystal   总被引：28，自引：2，他引：28  
This paper reports the results from a second characterisation of the 91500 zircon, including data from electron probe microanalysis, laser ablation inductively coupled plasma-mass spectrometry (LA-ICP-MS), secondary ion mass spectrometry (SIMS) and laser fluorination analyses. The focus of this initiative was to establish the suitability of this large single zircon crystal for calibrating in situ analyses of the rare earth elements and oxygen isotopes, as well as to provide working values for key geochemical systems. In addition to extensive testing of the chemical and structural homogeneity of this sample, the occurrence of banding in 91500 in both backscattered electron and cathodoluminescence images is described in detail. Blind intercomparison data reported by both LA-ICP-MS and SIMS laboratories indicate that only small systematic differences exist between the data sets provided by these two techniques. Furthermore, the use of NIST SRM 610 glass as the calibrant for SIMS analyses was found to introduce little or no systematic error into the results for zircon. Based on both laser fluorination and SIMS data, zircon 91500 seems to be very well suited for calibrating in situ oxygen isotopic analyses.  相似文献   

2.
Samples of glauconite, representing different stages of glauconitisation, as well as different formation environments, were analysed for rare earth elements (REE) and other trace elements using a combination of bulk sample and spatially-resolved in situ techniques. The results indicate that the high-sensitivity, spatially-resolved technique of laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) produces values up to two orders of magnitude lower than the bulk sample analyses. This suggests that submicroscopic rare earth element-bearing phases are distributed within the glauconite aggregates comprising the bulk samples. Analytical scanning electron microscopy (ASEM) revealed the presence of micrometre-sized grains of apatite and pore filling precipitates of an unidentified (REE, Ca)-phosphate (approximate composition Ca0.3–0.4(Ce0.4La0.1–0.2Nd0.1)PO4) in some glauconite grains.The inherent REE concentrations of the glauconite aggregates (i.e., glauconite crystallites without accidental mechanical inclusions or authigenic, not layer silicate mineral precipitates) was found to be relatively low (e.g., typically less than 100 ppm), and this value decreased with increasing glauconitisation (smectite–mica transformation through a series of recrystallisation processes). These results suggest that the REEs substitute for Ca in the interlayer space of the layer silicate structure and, therefore, the REE content decreases as Ca is progressively removed from the interlayer (smectite–mica transition).LA-ICP-MS, when combined with electron probe microanalysis (EPMA) or ASEM, offers an opportunity to exclude submicroscopic accessory minerals from glauconite trace element analyses, and so produces reliable trace element data for the respective minerals which host those elements.These results illustrate that accessory minerals are difficult to eliminate from clay samples, and that care needs to be taken in the interpretation of clay mineral REE distributions, irrespective of the aggregation state of the studied clay (i.e., whether finely dispersed within the sedimentary rock, or forming millimetre-sized aggregates). Model calculations showed that authigenic apatite associated with the studied green marine clays tends to have higher REE content than “bioapatites”, the total REE content being above 10 000 ppm.  相似文献   

3.
《Applied Geochemistry》2004,19(3):289-322
The accurate recognition of tephra deposits is of great value to Earth scientists because they facilitate stratigraphic correlation. The most useful tephra deposits form from violent volcanic eruptions; they are isochronous and widespread. Most are dacitic and rhyolitic in composition, and can be difficult to identify unequivocally using major element chemistry alone. Distal tephras are typically thin and are prone to contamination and thus are awkward to analyse by bulk methods. Here, the authors review their previous work in the development of analytical techniques for the analysis of small volumes of glass separates from tephra deposits, both by solution nebulisation and by laser ablation (LA) inductively coupled plasma mass spectrometry (ICP-MS), placing particular emphasis on the precision and accuracy of the various methods. In solution nebulisation ICP-MS, accurate data can be obtained from samples as small as 0.025 g. LA-ICP-MS methods are described for the analysis of small bulk samples and single glass shards as small as 40 μm in diameter. Accurate and reproducible analyses can be achieved by ICP-MS by both solution and laser ablation methods on homogeneous materials. Solution analyses are normally accurate to ±5% and have typical precisions (1 σ) of around ±4% for abundant trace elements (e.g. Zr, Rb) but this can deteriorate to about ±20% for rare elements in small samples (e.g. HREE in a 25 mg sample). Laser ablation methods are slightly less accurate (typically ±5–10%) and precision decreases from about ±3% at concentrations of a few hundred ppm, to about ±10% at 1 ppm and about ±30% at 0.05 ppm. An apparent lack of precision in the bulk analysis of small volumes of glass shards by LA-ICP-MS often represents within sample heterogeneity (and not analytical error), inter-shard variation becoming abundantly clear in some tephra deposits when individual glass shards are analysed. Single grain analysis on shards as small as 40 μm can provide an accurate analysis of the pure glass phase, which may not be achieved in solution or bulk sample LA-ICP-MS methods. Analyses affected by micro-phenocryst phases, such as feldspar or zircon can be easily removed following careful inspection of the data. Single shard LA-ICP-MS also allows any compositional variation within the parental magma to be defined.  相似文献   

4.
We report a study of the oxygen isotope ratios of chondrules and their constituent mineral grains from the Mokoia, oxidized CV3 chondrite. Bulk oxygen isotope ratios of 23 individual chondrules were determined by laser ablation fluorination, and oxygen isotope ratios of individual grains, mostly olivine, were obtained in situ on polished mounts using secondary ion mass spectrometry (SIMS). Our results can be compared with data obtained previously for the oxidized CV3 chondrite, Allende. Bulk oxygen isotope ratios of Mokoia chondrules form an array on an oxygen three-isotope plot that is subparallel to, and slightly displaced from, the CCAM (carbonaceous chondrite anhydrous minerals) line. The best-fit line for all CV3 chondrite chondrules has a slope of 0.99, and is displaced significantly (by δ17O ∼ −2.5‰) from the Young and Russell slope-one line for unaltered calcium-aluminum-rich inclusion (CAI) minerals. Oxygen isotope ratios of many bulk CAIs also lie on the CV-chondrule line, which is the most relevant oxygen isotope array for most CV chondrite components. Bulk oxygen isotope ratios of most chondrules in Mokoia have δ18O values around 0‰, and olivine grains in these chondrules have similar oxygen isotope ratios to their bulk values. In general, it appears that chondrule mesostases have higher δ18O values than olivines in the same chondrules. Our bulk chondrule data spread to lower δ18O values than any ferromagnesian chondrules that have been measured previously. Two chondrules with the lowest bulk δ18O values (−7.5‰ and −11.7‰) contain olivine grains that display an extremely wide range of oxygen isotope ratios, down to δ17O, δ18O around -50‰ in one chondrule. In these chondrules, there are no apparent relict grains, and essentially no relationships between olivine compositions, which are homogeneous, and oxygen isotopic compositions of individual grains. Heterogeneity of oxygen isotope ratios within these chondrules may be the result of incorporation of relict grains from objects such as amoeboid olivine aggregates, followed by solid-state chemical diffusion without concomitant oxygen equilibration. Alternatively, oxygen isotope exchange between an 16O-rich precursor and an 16O-poor gas may have taken place during chondrule formation, and these chondrules may represent partially equilibrated systems in which isotopic heterogeneities became frozen into the crystallizing olivine grains. If this is the case, we can infer that the earliest nebular solids from which chondrules formed had δ17O and δ18O values around -50‰, similar to those observed in refractory inclusions.  相似文献   

5.
一个新的矿物面扫描分析方法开发和地质学应用   总被引：22，自引：10，他引：12  
LA-ICP-MS面扫描分析近些年来发展的新兴技术,相对于其他面扫描仪器,其具有样品制样流程简单、仪器购置和分析成本低、分析时间短、检测限低、多元素表面分析(5μm)、近乎无损等分析优势,在地球科学和生物学领域有着大量的应用。本文系统介绍了作者应用Photon Machines激光剥蚀系统与安捷伦ICP-MS新开发矿物元素面扫描分析方法。该方法基于近些年来开发的双室样品仓技术和Matlab软件,通过自主开发的LaIcpMsSoftware(LIMS)进行数据处理来完成的。本次研究开发的激光面扫描分析技术可以在短时间内(2小时)分析3mm×3mm区域,并同时给出多组元素(包括稀土元素等)在二维平面的分布特征。论文详细描述了LIMS工作原理和特点,相对于国外同类型软件,LIMS具有操作简单,并具有多种数据显示模式和剖面切割展示,元素比值面分布分析等优势,便于后期数据分析与解译。同时,还展示了对斜长石、白钨矿和石榴子石进行面扫描分析的初步结果。研究表明,通过LA-ICP-MS面扫描,可以获得比点分析更为准确的元素分布特征,并能够更为直观的展示不同元素在矿物分布特征和相关关系,更好的开展矿物地球化学研究。  相似文献   

6.
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  
罗彦  刘勇胜  胡圣虹  高山 《地球科学》2001,26(5):508-512
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   

7.
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   

8.
Partitioning behavior of Sc, Ti, V, Mn, Sr, Y, Zr, Nb, Ba, La, Nd, Sm, Eu, Gd, Dy, Ho, Yb, Hf, and Pb between dacitic silicate melt and clinopyroxene, orthopyroxene, and plagioclase has been determined based on laser ablation-inductively coupled plasma mass spectrometric (LA-ICPMS) analysis of melt inclusions and the immediately adjacent host mineral. Samples from the 1988 eruption of White Island, New Zealand were selected because petrographic evidence suggests that all three mineral phases are in equilibrium with each other and with the melt inclusions. All three phenocryst types are found as mineral inclusions within each of the other phases, and mineral inclusions often coexist with melt inclusions in growth-zone assemblages. Compositions of melt inclusions do not vary between the different host minerals, suggesting that boundary layer processes did not affect compositions of melt inclusions and that post-trapping modifications have not occurred.Partition coefficients were calculated from the host and melt inclusion compositions and results were compared to published values. All trace elements examined in this study except Sr are incompatible in plagioclase, and all measured trace elements except for Mn are incompatible in orthopyroxene. In clinopyroxene, Sc, V, and Mn are compatible, and Y, Ti, HREE, and the MREE are only slightly incompatible. Most partition coefficients overlap the wide range of values reported in the literature, but the White Island data are consistently at the lower end of the range in published values. Results from the literature obtained using modern microanalytical techniques such as secondary ion mass spectrometry (SIMS) or proton induced X-ray emission spectroscopy (PIXE) also fall at the lower end of the published values, whereas partition coefficients determined from bulk analysis of glass and crystals separated from volcanic rocks typically extend to higher values. Rapid crystal growth-rates, crystal zonation, or the presence of accessory mineral inclusions in phenocrysts likely accounts for the wide range and generally higher partition coefficients obtained using bulk sampling techniques. The results for 3+ cations from this study are consistent with theoretical predictions based on a lattice strain model for site occupancy. The results also confirm that the melt inclusion-mineral (MIM) technique is a reliable method for determining partition coefficients, as long as the melt inclusions have not experienced post-entrapment reequilibration.  相似文献   

9.
矿物包裹体的化学成分研究在地质学、矿床学和油气勘探等方面具有重要意义。目前对包裹体化学成分分析的主要分析方法有激光烧蚀电感耦合等离子体质谱(LA-ICP-MS)、电子探针(EPMA)、显微激光拉曼光谱(LRS)、傅里叶变换红外光谱(FTIR)、质子诱发X射线光谱分析(PIXE)、同步辐射X射线荧光光谱(SXRF)和(传统的)二次离子质谱分析(SIMS)等。本文在对上述方法的分析特点进行简单介绍的基础上,重点阐述了对于矿床学样品表征具有广泛应用潜力的飞行时间二次离子质谱(TOF-SIMS)的原理、特点和技术优势,总结了国内外学者应用TOF-SIMS对矿物包裹体化学成分分析的研究进展与存在问题,并做了相关领域的展望。  相似文献   

10.
The analytical capabilities of laser ablation (LA)-ICP-MS in determining Li, Be and B at trace levels in geological samples have been tested on a series of glass reference materials and natural samples. The LA-ICP-MS instrument used consisted of a sector-field ICP-MS coupled with a laser ablation microprobe operating at either 266 or 213 nm wavelength. Reference glasses from NIST (SRM 612, 614 and 616) and MPI-DING (KL2-G, ML3B-G, StHs6/80-G, GOR128-G, GOR132-G, T1-G and ATHO-G) were selected to develop the analytical method and to assess the best instrumental configuration. A series of calcic amphiboles with different Li, Be and B concentrations were also analysed using both LA-ICP-MS and SIMS to test the applicability of the method to natural minerals. Results indicated that with a spot size of 40 μm the agreement between measured and reference values of Li, Be and B is generally better than 10% for NIST SRM 612 and 20% for NIST SRM 614. Average reproducibility at the 2s level was 10% for Li, 20% for Be and 15% for B. Limits of detection were approximately 100 ng g-1 for Be and B and 200 ng g-1 for Li. These results were confirmed by analyses carried out on natural amphiboles and compared well in terms of precision and accuracy with those commonly achieved by SIMS.  相似文献   

11.
The USGS reference glasses GSA-1G, GSC-1G, GSD-1G, GSE-1G, BCR-2G, BHVO-2G and BIR-1G were investigated by different analytical techniques. All these materials have a geological (basaltic) matrix and are therefore useful in igneous geochemistry as matrix-matched reference materials for microanalytical techniques. The new GS glasses have trace elements in groups at concentration levels of about < 0.01, 5, 50 and 500 μg g-1. Their major element compositions have been determined by EPMA, and trace elements have been analysed by LA-ICP-MS and two isotope dilution techniques using TIMS and ICP-MS. EPMA and LA-ICP-MS analyses indicated that the USGS reference glasses are homogeneous at the μm to mm scale with respect to major (variations < 1-2%) and most trace elements (variations 1-4%). Trace element data obtained from the different analytical techniques agreed within an uncertainty of 1-5%, indicating that between method results are comparable. Therefore, the preliminary working values for the four USGS GS glasses calculated from these data have a low level of uncertainty.  相似文献   

12.
碳酸盐岩研究中存在多种微量元素、同位素测试方法,为进一步探究各测试手段实际获取地化信息之间是否存在差异?能否进行比对?以川中下寒武统龙王庙组碳酸盐岩样品为例,通过对比研究中常用的主微量元素测试(电子探针[EPMA]、激光剥蚀—等离子质谱[LA-ICP-MS]、溶液法微量[ICP-OES])、氧同位素测定(原位离子探针[in-situ SIMS]、酸溶粉末)结果,揭示讨论各测试结果的差异性,旨在为降低地化信息的多解性提供经验依据。研究发现: (1)各测试手段(EPMA、LA-ICP-MS、ICP-OES)之间的差异性客观存在,但测试结果偏差整体随着所测元素实际浓度的增高而降低。对于主量元素(>10%)各测试结果偏差小于2%;富集元素(>1000 μg/g)各测试结果处于测试误差之内,结果偏差小于6%;微量元素浓度区间(100~1000 μg/g)各测试结果偏差显著增大,并且LA-ICP-MS与ICP-OES结果偏差要小于LA-ICP-MS与EPMA结果偏差,前者偏差幅度由6%增至45%,后者偏差幅度由9.1%增至151%;在低于100 μg/g元素浓度区间,受矿物内非均质性影响LA-ICP-MS与ICP-OES的测试结果可相差几倍。(2)微区原位限定下,EPMA测试结果在邻近检测线区间(100~300 μg/g)与LA-ICP-MS结果偏差逐渐加大,推测此偏差变化是由EPMA结果矫正过程中对低含量元素的矫正补偿机制所造成。(3)in-situ SIMS氧同位素值揭示了矿物微区尺度上的 δ18O 值差异,但其整体测试结果与传统酸溶法测试的结果存在0.5‰~2.5‰ V-PDB的负偏偏差,推测此偏差可能来自于标样矫正转换误差。(4)实例样品中可见阴极发光特征与Fe、Mn含量无关的现象,故成岩流体判定更需结合岩石学、地化证据探讨。  相似文献   

13.
碳酸盐岩研究中存在多种微量元素、同位素测试方法,为进一步探究各测试手段实际获取地化信息之间是否存在差异?能否进行比对?以川中下寒武统龙王庙组碳酸盐岩样品为例,通过对比研究中常用的主微量元素测试(电子探针[EPMA]、激光剥蚀—等离子质谱[LA-ICP-MS]、溶液法微量[ICP-OES])、氧同位素测定(原位离子探针[in-situ SIMS]、酸溶粉末)结果,揭示讨论各测试结果的差异性,旨在为降低地化信息的多解性提供经验依据。研究发现: (1)各测试手段(EPMA、LA-ICP-MS、ICP-OES)之间的差异性客观存在,但测试结果偏差整体随着所测元素实际浓度的增高而降低。对于主量元素(>10%)各测试结果偏差小于2%;富集元素(>1000 μg/g)各测试结果处于测试误差之内,结果偏差小于6%;微量元素浓度区间(100~1000 μg/g)各测试结果偏差显著增大,并且LA-ICP-MS与ICP-OES结果偏差要小于LA-ICP-MS与EPMA结果偏差,前者偏差幅度由6%增至45%,后者偏差幅度由9.1%增至151%;在低于100 μg/g元素浓度区间,受矿物内非均质性影响LA-ICP-MS与ICP-OES的测试结果可相差几倍。(2)微区原位限定下,EPMA测试结果在邻近检测线区间(100~300 μg/g)与LA-ICP-MS结果偏差逐渐加大,推测此偏差变化是由EPMA结果矫正过程中对低含量元素的矫正补偿机制所造成。(3)in-situ SIMS氧同位素值揭示了矿物微区尺度上的 δ18O 值差异,但其整体测试结果与传统酸溶法测试的结果存在0.5‰~2.5‰ V-PDB的负偏偏差,推测此偏差可能来自于标样矫正转换误差。(4)实例样品中可见阴极发光特征与Fe、Mn含量无关的现象,故成岩流体判定更需结合岩石学、地化证据探讨。  相似文献   

14.
白钨矿是各类矿床中较为常见的副矿物,通过分析白钨矿的稀土元素质量分数及其标准化配分模式图,可为矿床成矿流体特征及演化提供重要的判别依据。本文对东北地区羊鼻山矽卡岩型矿床和杨金沟热液脉型矿床两个典型钨矿床的白钨矿样品中的稀土元素进行了激光剥蚀-电感耦合等离子体质谱（LA-ICP-MS）原位分析。其中：羊鼻山矽卡岩型矿床白钨矿LA-ICP-MS分析方法所获得的稀土元素配分曲线模式与前人用传统的溶液-ICP-MS分析方法所获得的结果完全吻合,表明采用剥蚀束斑44 μm和剥蚀频率7 Hz的193 nm ArF激光器,NIST 610作外部标样,Ca作内标元素,对基体效应影响最小,所获数据可靠,方法可行;而杨金沟热液脉型矿床白钨矿溶液-ICP-MS分析方法与LA-ICP-MS分析法所获得结果既具有相似性又具有差异性。原因在于羊鼻山白钨矿的成因类型为矽卡岩型、粒度较小且形成时间短,因此不同矿物颗粒间、同一矿物不同部位间稀土元素的配分模式一致;而杨金沟白钨矿的成因类型属于热液脉型、粒度较大、沉淀结晶时间长,因此同一矿物不同部位的稀土元素的配分模式因成矿流体早晚阶段不同而不同。基于以上对比研究发现,无论是在取样和测试过程方面,还是数据准确度方面,相比传统溶液-ICP-MS分析法,LA-ICP-MS原位分析法均具有明显的优势,主要表现在样品形式简单、粒度和质量分数要求低、测试周期短、费用低且结果精确度高;同时其可对不同成矿阶段或白钨矿不同部位成分进行精细测定,从而得出不同成矿阶段或白钨矿不同部位的稀土元素质量分数,以及在更高的空间分辨率下获得更详细准确的数据信息。此外,对白钨矿（尤其是无明显环带者）进行LA-ICP-MS原位分析时,既可采用电子探针微量分析（EPMA）准确测定Ca的质量分数,也可直接采用标准化学式计算Ca的质量分数,分析所得数据同样可以获得合理的地质解释。  相似文献   

15.
微区原位分析是地球科学研究的重要手段,但这些分析技术在华南热液铀矿床中的应用相对较少,限制了对铀矿床成矿机理的深入认识。沙子江铀矿床是华南著名的花岗岩型热液铀矿床。本文利用电子探针(EMPA)、激光电感耦合等离子体质谱(LA-ICPMS)以及二次离子探针(SIMS)等微区原位分析技术,对沙子江铀矿床中的沥青铀矿开展了U-Pb同位素年代学及元素组成研究,确定了沥青铀矿的形成时代及成分特征,并探讨了蚀变作用对沥青铀矿成分及其表面年龄或化学年龄的影响。电子探针分析结果显示,该沥青铀矿以富铀和钙、极低含量的ThO_2和稀土元素为特征,揭示其为低温热液成因,成矿热液富含Ca。LA-ICP-MS分析结果显示,沥青铀矿的稀土元素总量较低,其配分模式呈轻稀土富集型,具有明显的负Eu异常,与赋矿围岩豆乍山花岗岩的稀土元素组成相似,暗示其铀源可能与豆乍山岩体有密切的关系。蚀变和未蚀变沥青铀矿成分的对比研究显示,蚀变作用会导致硅元素大量进入沥青铀矿晶格,造成铀和铅的丢失,从而影响沥青铀矿的表观年龄或化学年龄,但沥青铀矿的稀土元素配分模式不会受到蚀变的影响。未蚀变沥青铀矿的SIMS微区原位分析获得的U-Pb年龄为101. 3±4. 5Ma,表明沙子江铀矿床存在100Ma左右的铀成矿事件。受岩石圈伸展控制形成的富CO流体与富铀花岗岩相互作用浸取出花岗岩中的铀,并在合适的构造部位沉淀形成了沙子江铀矿床。  相似文献   

16.
In this study we evaluated the capability of a 213 nm laser ablation system coupled to a quadrupole-based ICP-MS in delivering accurate and precise U-Pb ages on zircons and monazites. Four zircon samples ( ca. 50 Ma to ca. 600 Ma) and four monazite samples ( ca. 30 Ma to ca. 1390 Ma) of known ages were analysed utilising laser ablation pits with diameters of 20 μm and 60 μm. Instrument mass bias and laser induced time-dependent elemental fractionation were corrected for by calibration against a matrix-matched reference material. Tera-Wasserburg plots of the calculated U-Pb data were employed to assess, and correct for, common Pb contributions. The results indicated that the LA-ICP-MS technique employed in this study allowed precise and accurate U-Pb isotope dating of zircon and monazite on sample areas 20 μm in diameter. At this spot size, the precisions achieved for single spot 206Pb/238U ages, were better than 5% (2s) for monazites and zircons with ages down to 30 Ma and 50 Ma, respectively. The precisions reported are comparable to those generally reported in SIMS and LA-MC-ICP-MS U-Pb isotope determinations.  相似文献   

17.
An updated REE measurement of Gabbro GOG-1 was carried out by means of secondary ion mass spectrometry (SIMS). The availability of high amount of rock powder allowed the sample to be well ground and homogenized before analysis. Fused glass pellets were employed for SIMS investigations. REE data were compared with new ICP-AES and NAA analyses. REE results from all employed analytical techniques show good agreement and are consistent with in-situ SIMS measurements of REE in major mineral phases forming GOG-1. Extensive homogeneity tests seem to confirm the possibility to using this rock as a reference material for earth sciences.  相似文献   

18.
A simple, rapid and precise method is described for determining trace elements by laser ablation (LA)-ICP-MS analysis in bulk geological materials that have been prepared as lithium borate glasses following standard procedures for XRF analysis. This approach reliably achieves complete sample digestion and provides for complementary XRF and LA-ICP-MS analysis of a full suite of major and trace elements from a single sample preparation. Highly precise analysis is enabled by rastering an ArF excimer laser (λ= 193nm) across fused samples to deliver a constant sample yield to the mass spectrometer without inter-element fractionation effects during each analysis. Capabilities of the method are demonstrated by determination of twenty five trace elements (Sc, Ti, V, Ga, Rb, Sr, Y, Zr, Nb, Cs, Ba, REE, Hf, Ta, Pb, Th and U) in a diverse range of geological reference materials that includes peridotites, basalts, granites, metamorphic rocks and sediments. More than 90% of determinations are indistinguishable from published reference values at the 95% confidence level. Systematic bias greater than 5% is observed for only a handful of elements (Zr, Nb and U) and may be attributed in part to inaccurate calibration values used for the NIST SRM 612 glass in the case of Zr and Nb. Detection limits for several elements, most notably La, are compromised at ultra-trace levels by impurities in the lithium borate flux but can be corrected for by subtracting appropriate procedural blanks. Reliable Pb analysis has proved problematic due to variable degrees of contamination introduced during sample polishing prior to analysis and from Pt-crucibles previously used to fuse Pb-rich samples. Scope exists for extending the method to include internal standard element/isotope spiking, particularly where integrated XRF analysis is not available to characterise major and trace elements in the fused lithium borate glasses prior to LA-ICP-MS analysis.  相似文献   

19.
碳酸盐岩中碳酸盐矿物稀土元素分析方法进展   总被引：1，自引：0，他引：1  
碳酸盐岩中测定碳酸盐矿物的稀土元素主要有酸溶-ICP-MS和LA-ICP-MS方法.酸溶-ICP-MS方法用盐酸、硝酸溶解碳酸盐矿物,但也能溶解部分非碳酸盐矿物,而影响分析结果;用醋酸溶样可避免非碳酸盐矿物的干扰,但可能没有溶样完全,同样影响分析结果.LA-ICP-MS是应用激光对碳酸盐矿物进行原位剥蚀,将蒸发物导入ICP-MS进行分析,对不合粘土等的碳酸盐矿物最有效,由于激光束光斑较大,且碳酸盐岩中普遍含有微小的粘土矿物,可能也存在不确定性.总体而言,酸溶-ICP-MS和LA-ICP-MS获得的稀土元素页岩标准化配分模式及主要参数相似,均可用于沉积环境的示踪.  相似文献   

20.
Secondary ion mass spectrometry (SIMS) requires matrix‐matched reference materials to calibrate mass fractionation during oxygen isotope measurement. Over one thousand SIMS oxygen isotope measurements were conducted on eleven natural mineral samples (five olivines, three clinopyroxenes and three orthopyroxenes) in nineteen sessions using CAMECA IMS 1280 SIMS instruments to evaluate their potential as SIMS reference materials. The obtained results reveal oxygen isotope homogeneity of these samples. No matrix effect was measured for the same variety of mineral samples with limited Mg‐number variations (89.6–94.2, 90–91.9 and 90.1–92.1 for olivine, clinopyroxene and orthopyroxene, respectively). The recommended oxygen isotope compositions of these samples were determined using laser fluorination. These samples are therefore suitable to be used as reference materials for in situ oxygen isotope microanalysis.  相似文献   

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