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In situ oxygen isotope analysis of feldspar and quartz by Nd:YAG laser microprobe Nd:YAG激光微探针原位分析长石和石英的氧同位素
Pub Date : 1992-06-10 DOI: 10.1016/0009-2541(92)90200-O
Don Elsenheimer, John W. Valley

In situδ18O analyses have been reproducibly obtained±0.5‰ (1σ) on 400–1200-μm diameter spots of plagioclase using a Nd:YAG laser microprobe system and BrF5. Over 100 analyses if plagioclase megacrysts from a single sample of Marcy Anorthosite were made to determine the optimum analytical conditions. The best results are obtained on 400–800-μm-thick wafers; less accurate and less precise results were obtained on centimeter-thick slabs. Analyses on some individual wafers display very high precision (below±0.2‰, 1σ) that are nearly as good as the precision of conventional analyses. However, such high precision cannot yet be systematically obtained in situ, and it is certain whether it results from especially homogeneous domains within the sample or from differences in operating conditions. Oxygen-leaching and isotope fractionation along the edges of the laser-heated reaction pits may have a minor effect on precision.

The combination of sub-millimeter spatial resolution and±0.5‰ precision has not previously been ohbtained on feldspar, and provides the means to investigate fluid-rock interactions in a variety of geologic environments. The plagioclase in this study is the first sample for which oxygen isotope homogeneity has been evaluated in situ. The absence of isotopic zonation restricts theories on the roles of fluids associated with the Marcy Anorthosite Massif, New York, U.S.A. In contrast, replicateδ18O analyses in quartz, K-feldspar and plagioclase grains in granite from the Siljan Ring astrobleme, Sweden, vary by > 1‰, suggesting the existence of intragranular isotopic heterogeneity resulting from interaction with late meteoric fluids.

利用Nd:YAG激光微探针系统和BrF5对斜长石400-1200 μm直径的斑点进行了δ 18o分析,可重复性地得到±0.5‰(1σ)。为了确定最佳分析条件,对马西斜长岩单一样品的斜长石巨晶进行了100多次分析。在400 ~ 800 μm厚的硅片上效果最好;在厘米厚的平板上得到的结果不太准确和不太精确。对个别晶圆的分析显示出非常高的精度(低于±0.2‰,1σ),几乎与传统分析的精度一样好。然而,如此高的精度还不能在原位系统地获得,而且它是由样品内特别均匀的区域还是由操作条件的差异引起的,这是确定的。沿激光加热反应坑边缘的氧浸出和同位素分馏可能对精度有轻微影响。亚毫米空间分辨率和±0.5‰精度的组合在长石上是前所未有的,为研究各种地质环境下的流体-岩石相互作用提供了手段。本研究中的斜长石是第一个原位评价氧同位素均匀性的样品。同位素分带的缺失限制了与美国纽约马西斜长岩地块相关的流体作用的理论。相反,瑞典Siljan环星坑花岗岩中石英、钾长石和斜长石颗粒的复制δ 18o分析差异较大;1‰,表明存在与晚期大气流体相互作用的粒内同位素非均质性。
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引用次数: 58
Carbon isotope measurements on diamonds 钻石的碳同位素测量
Pub Date : 1992-06-10 DOI: 10.1016/0009-2541(92)90215-Q
B. Harte , M. Otter
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引用次数: 27
In situ laser microprobe techniques for stable isotope analysis 稳定同位素原位激光微探针分析技术
Pub Date : 1992-06-10 DOI: 10.1016/0009-2541(92)90199-F
Z.D. Sharp

In situ laser extraction techniques have been developed for determining the stable isotope ratios in carbonates, silicates, oxides and sulfides with high spatial resolution. All of these methods use the laser as a heat source to extract the appropriate gas. Carbonate analyses are made by decomposing the carbonate at elevated temperatures to liberate CO2. Oxygen is extracted from silicates by heating the sample surface in a halogen fluoride atmosphere, and sulfur is extracted from sulfides by heating in either an O2 or halogen fluoride atmosphere. The analytical precision for carbonate analyses isσ = ±0.2‰and±0.1‰ forδ18C andδ18O, respectively. Higher scatter in some samples is probably due to sample heterogeneities. In situ silicate analyses have a precision ofσ = ±0.1‰0.6‰ depending upon sample material and heterogeneity. The measured isotopic ratio may be different from the accepted value, but is insensitive to changing operating conditions. Published results for in situ analyses of sulfides have a precision of< ±0.3‰ (1σ). Theδ34S-values obtained with the laser method are less than accepted values, and vary according to the sulfide.

A new level of spatial resolution is possible with the in situ laser methods. Oxygen isotope variations of10‰ are found to exist at a scale of< 1mm in greenschist-grade quartz veins. Carbon and oxygen isotopic ratios may be quite heterogeneous in hydrothermal calcites and low-grade marbles. High-grade marbles are isotopically homogeneous. Determinations of isotopic variations at the sub-millimeter scale may be used as an indicator of fluid sources and mechanisms of isotopic exchange.

原位激光提取技术已发展用于测定碳酸盐、硅酸盐、氧化物和硫化物的稳定同位素比率,具有高空间分辨率。所有这些方法都使用激光作为热源来提取适当的气体。碳酸盐分析是通过在高温下分解碳酸盐以释放二氧化碳来进行的。通过在氟化卤素气氛中加热样品表面从硅酸盐中提取氧,通过在O2或氟化卤素气氛中加热从硫化物中提取硫。碳酸盐岩δ 18c和δ 18o的分析精度分别为σ =±0.2‰和±0.1‰。在一些样品中较高的散射可能是由于样品的异质性。原位硅酸盐分析的精度为σ =±0.1‰0.6‰,具体取决于样品材料和非均质性。测量的同位素比率可能与接受值不同,但对变化的操作条件不敏感。已发表的硫化物原位分析结果的精度为<±0.3‰(1σ)。激光法得到的δ 34s值小于公认值,且随硫化物的不同而变化。使用原位激光方法可以达到一个新的空间分辨率水平。在<尺度上发现存在10‰的氧同位素变化;绿片岩级石英脉1mm。在水热方解石和低品位大理岩中,碳氧同位素比例可能相当不均匀。高品位大理岩同位素均质。亚毫米尺度上同位素变化的测定可作为流体来源和同位素交换机制的指标。
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引用次数: 117
Laser microprobe stable isotope measurements on geological materials: Some experimental considerations (with special reference toδ34S in sulphides) 地质物质的激光微探针稳定同位素测量:一些实验考虑(特别参考硫化物中的δ 34s)
Pub Date : 1992-06-10 DOI: 10.1016/0009-2541(92)90202-G
A.E. Fallick, P. McConville, A.J. Boyce, R. Burgess, S.P. Kelley

A laser, especially when focused through a petrographic microscope, can provide a localised heat source for extraction of light elements from solids prior to stable isotope ratio measurements by gas-source mass spectrometry. In certain cases, such as conversion of sulphides to SO2 by combustion in an oxygen atmosphere, it may be necessary to choose operating characteristics which allow the chemistry at the solid target surface to be controlled. Experimental considerations such as wavelength, laser mode and irradiance are discussed and it is shown that several successful system work at very similar irradiances of∼ 109W m−2. It is suggested, for those circumstances where high spatial resolution is required and where deep penetration into the surface cannot be tolerated, that a suitable modus operandi is to use a relatively low power but narrowly focused beam to excavate trenches perpendicular to the direction in which resolution is demanded. This allows a spatial resolution of< 100 μm even for porous pyrite witha poor quality of surface.

激光,特别是当通过岩石显微镜聚焦时,可以在气源质谱法测量稳定同位素比之前,为从固体中提取轻元素提供局部热源。在某些情况下,例如在氧气气氛中通过燃烧将硫化物转化为二氧化硫,可能有必要选择能够控制固体目标表面化学反应的操作特性。讨论了波长、激光模式和辐照度等实验考虑因素,并表明几个成功的系统工作在非常相似的辐照度为~ 109W m−2。建议,对于那些需要高空间分辨率和不能容忍深入地表的情况,合适的操作方法是使用相对低功率但窄聚焦的光束来挖掘垂直于需要分辨率的方向的沟槽。这允许空间分辨率为<对于表面质量较差的多孔黄铁矿,也可达到100 μm。
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引用次数: 54
Oxygen stable isotope measurements on a gravestone exposed to the Hiroshima A-bomb explosion and the “Dosimetry System 1986” 受广岛原子弹爆炸影响的墓碑的氧稳定同位素测量及“剂量测定系统1986”
Pub Date : 1992-06-10 DOI: 10.1016/0009-2541(92)90206-K
D. Blamart , W. Ru¨hm , W. Spiegel , K. Kato , G. Korschinek , H. Morinaga , G. Morteani , E. Nolte

The “Dosimetry System 1986”, DS86, established theoretical neutron spectra and fluences of the atomic-bomb explosions in Hiroshima and Nagasaki correlated with the radiation disease rate of survivors. The actual neutron fluence and spectrum from the Hiroshima explosion can be derived by use of different radioisotopes produced by neutron capture reactions due to different neutron capture cross-sections.

In a gravestone 107 m from the hypocentre of the explosion in Hiroshima, the radioisotopes36Cl,41Ca,60Co,152Eu and154Eu were already measured. From this a neutron spectrum can be derived which is much harder than the neutron spectrum used in DS86 provided the gravestone represents a closed system. To check this, petrographic and oxygen stable isotope investigations were performed on the gravestone as well as on a not-irradiated sample coming from the same quarry as the gravestone. The results of the petrographic and geochemical studies both negate the possibility of major isotopic exchange with rainwater.

“1986年剂量测定系统”(DS86)建立了理论中子谱和广岛和长崎原子弹爆炸的影响与幸存者的辐射发病率之间的关系。广岛爆炸的实际中子通量和谱可通过利用中子俘获反应产生的不同放射性同位素推导出来,因为中子俘获截面不同。在距广岛爆炸震源中心107米的一块墓碑上,已经测量了放射性同位素36cl、41Ca、60Co、152Eu和154eu。由此可以推导出比DS86中使用的中子谱要难得多的中子谱,前提是墓碑代表一个封闭系统。为了验证这一点,岩石学和氧稳定同位素研究对墓碑以及来自同一采石场的未辐照样本进行了研究。岩石学和地球化学研究的结果都否定了与雨水进行主要同位素交换的可能性。
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引用次数: 6
LASSIE (laser ablation sampler for stable isotope extraction) applied to carbonate minerals 用于碳酸盐矿物稳定同位素提取的激光烧蚀取样器
Pub Date : 1992-06-10 DOI: 10.1016/0009-2541(92)90201-F
P.C. Smalley, C.N. Maile, M.L. Coleman, J.E. Rouse

LASSIE is an instrument that enables rapid (∼ 30 min) stable isotope analysis of extremely small (∼ 35-μm diameter) areas of carbonates, selected by the operator from a colour TV image of a thin rock slice. This allowspractical routine integration of petrography with isotopic analysis.

The main technical problem—isotopic fractionation during laser ablation—has been overcome by generating correction factors based on analyses of standards (for calcite, correction factors are +1.2‰ forδ18O, —0.8‰ forδ13C. Accuracy is determined by the uncertainty (σ) in these correction factors:±0.4‰ forδ18O andδ13C. Reprocducibility of replicate analyses is also∼ ±0.4‰ (σ) forδ18O and ∼±0.2‰ forδ13C.

An example in which LASSIE analyses were performed on carbonate-cemented sandstones, demonstrated the ability of LASSIE to resolve the various components of a complex carbonate mixture. The study further demonstrated how conventional bulk analyses can give uninterpretable or, worse, misleading results.

LASSIE是一种能够快速(~ 30分钟)稳定同位素分析极小(~ 35 μm直径)碳酸盐区域的仪器,由操作员从薄岩片的彩色电视图像中选择。这使得岩石学与同位素分析的常规结合成为可能。激光烧蚀过程中主要的技术问题——同位素分馏——已经通过对标准物(方解石)的分析产生校正因子(δ 18o校正因子为+1.2‰,δ 13c校正因子为-0.8‰)解决。精度由这些校正因子的不确定度(σ)决定:δ 18o和δ 13c的不确定度为±0.4‰。δ 18o和δ 13c的重复分析的可重复性也分别为~±0.4‰和~±0.2‰。在对碳酸盐胶结砂岩进行LASSIE分析的实例中,证明了LASSIE能够分解复杂碳酸盐混合物的各种成分。该研究进一步证明了传统的批量分析是如何给出不可解释的,或者更糟的是,误导性的结果。
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引用次数: 21
Oxygen isotope measurement of magnetites 磁铁矿氧同位素测定
Pub Date : 1992-06-10 DOI: 10.1016/0009-2541(92)90214-P
J.W. Valley , C.M. Graham
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引用次数: 4
Application of high-sensitivity carbon isotope techniques— a question of blanks 高灵敏度碳同位素技术的应用——一个空白问题
Pub Date : 1992-06-10 DOI: 10.1016/0009-2541(92)90205-J
P.D. Yates, I.P. Wright, C.T. Pillinger

The performance of a new carbon stable isotope static mass spectrometer over the sample size range 10 pmol to 1 nmol is reviewed with reference to standard data gathered over a year of operation. Specimens of known isotopic composition and zero enrichment tests suggest that the instrument is accurate to within±0.5‰ over the entire sample size range, with precision only becoming worse than∼±;1‰at< 80pmol. Efforts to obtain “blanks” compatible with the above performance are also reviewed. A procedure is available which controls the total blank in a stepped combustion, from room temperature to 1200°C, to 1 nmol; in the temperature range of most inserest for extraterrestrial samples (600–1200°C),⩽50pmol can be achieved. However, a real benefit of the new instrument is that isotopic compositions of the blanks can be accurately obtained, so allowing a proper assessment of its causes and a correction of sample data if desired.

在10 pmol到1 nmol的样品尺寸范围内,对一种新型碳稳定同位素静态质谱仪的性能进行了评价,并参考了一年以上运行中收集的标准数据。已知同位素组成的标本和零富集试验表明,该仪器在整个样本量范围内的精度在±0.5‰以内,精度仅低于±1‰。80 pmol。还审查了获得与上述性能兼容的“空白”的努力。有一种程序可以控制分步燃烧的总空白量,从室温到1200℃,到1nmol;在最适合地外样品的温度范围(600-1200℃),可达到≥50pmol。然而,新仪器的一个真正好处是可以准确地获得空白的同位素组成,因此可以对其原因进行适当的评估,并在需要时对样品数据进行校正。
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引用次数: 13
Oxygen-isotope analysis on the Came´ca® ims-300 come´ca®ims-300的氧同位素分析
Pub Date : 1992-06-10 DOI: 10.1016/0009-2541(92)90218-T
J.C. Lorin
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引用次数: 11
The Isolab®54 ion microprobe Isolab®54离子微探针
Pub Date : 1992-06-10 DOI: 10.1016/0009-2541(92)90219-U
I. Lyon, G. Turner
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引用次数: 2
期刊
Chemical Geology: Isotope Geoscience section
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