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1.
A broad suite of geological materials was studied a using a handheld laser‐induced breakdown spectroscopy (LIBS) instrument. Because LIBS is simultaneously sensitive to all elements, the full broadband emission spectrum recorded from a single laser shot provides a ‘chemical fingerprint’ of any material – solid, liquid or gas. The distinguishing chemical characteristics of the samples analysed were identified through principal component analysis (PCA), which demonstrates how this technique for statistical analysis can be used to identify spectral differences between similar sample types based on minor and trace constituents. Partial least squares discriminant analysis (PLSDA) was used to distinguish and classify the materials, with excellent discrimination achieved for all sample types. This study illustrates through four examples (carbonate minerals and rocks, the oxide mineral pair columbite–tantalite, the silicate mineral garnet and native gold) how portable, handheld LIBS analysers can be used for real‐time chemical analysis under simulated field conditions for element or mineral identification, plus such applications as stratigraphic correlation, provenance determination and natural resource exploration.  相似文献   

2.
Laser-induced breakdown spectroscopy (LIBS) is a simple atomic emission spectroscopy technique capable of real-time, essentially non-destructive determination of the elemental composition of any substance (solid, liquid, or gas). LIBS, which is presently undergoing rapid research and development as a technology for geochemical analysis, has attractive potential as a field tool for rapid man-portable and/or stand-off chemical analysis. In LIBS, a pulsed laser beam is focused such that energy absorption produces a high-temperature microplasma at the sample surface resulting in the dissociation and ionization of small amounts of material, with both continuum and atomic/ionic emission generated by the plasma during cooling. A broadband spectrometer-detector is used to spectrally and temporally resolve the light from the plasma and record the intensity of elemental emission lines. Because the technique is simultaneously sensitive to all elements, a single laser shot can be used to track the spectral intensity of specific elements or record the broadband LIBS emission spectra, which are unique chemical ‘fingerprints’ of a material. In this study, a broad spectrum of geological materials was analyzed using a commercial bench-top LIBS system with broadband detection from ∼200 to 965 nm, with multiple single-shot spectra acquired. The subsequent use of statistical signal processing approaches to rapidly identify and classify samples highlights the potential of LIBS for ‘geochemical fingerprinting’ in a variety of geochemical, mineralogical, and environmental applications that would benefit from either real-time or in-field chemical analysis.  相似文献   

3.
An innovative approach of double pulse laser‐induced breakdown spectroscopy (DP‐LIBS) coupled with optical microscopy was applied to the characterisation and quantitative analysis of the Agoudal iron meteorite in bulk sample and in petrographic thin section. Qualitative analysis identified the elements Ca, Co, Fe, Ga, Li and Ni in the thin section and the whole meteorite. Two different methods, calibration‐free LIBS and one‐point calibration LIBS, were used as complementary methodologies for quantitative LIBS analysis. The elemental composition data obtained by LIBS were in good agreement with the compositional analyses obtained by traditional methods generally applied for the analysis of meteorites, such as ICP‐MS and EDS‐SEM. Besides the recognised advantages of LIBS over traditional techniques, including versatility, minimal destructivity, lack of waste production, low operating costs, rapidity of analysis, availability of transportable or portable systems, etc., additional advantages of this technique in the analysis of meteorites are precision and accuracy, sensitivity to low atomic number elements such as Li and the capacity to detect and quantify Co contents that cannot be obtained by EDS‐SEM.  相似文献   

4.
This study demonstrates the application of laser‐induced breakdown spectroscopy (LIBS) and hyperspectral imaging to the investigation of coprolite and fossil samples. Solid samples from the Permian (seven coprolites and one fossil), Cretaceous (one coprolite) and Oligo‐Miocene (two coprolites) periods were directly analysed, and emission spectra from 186 to 1042 nm were obtained in several areas covering coprolite/fossil and rock material. Initial exploratory analyses were performed using principal component analysis with the data set normalised by the norm (Euclidean norm = 1). After identification and selection of emission lines of eleven elements (Al, Ca, Cr, Fe, K, Mg, Mn, Na, Ni, P and Si), the signals were normalised again by the relative intensity of the selected element. Phosphorus was identified mainly in the coprolites, while K and Na were primarily found in the rock material. In several cases, there was a positive correlation between Ca and P. A sample from the Oligo‐Miocene series was also analysed using inductively coupled plasma‐optical emission spectrometry (ICP‐OES) (rock and coprolites were analysed separately). Based on the quantitative results from ICP‐OES, it was confirmed that the tendency was the same as that observed with the results obtained from LIBS directly in the solid sample.  相似文献   

5.
Geochronology is a fundamental measurement for planetary samples, providing global and solar system context for the conditions prevailing on the planet at the time of major geological events. The potassium (K)‐Argon (Ar) laser experiment (KArLE) will make in situ noble gas geochronology measurements aboard planetary robotic missions such as rovers and landers. Laser‐induced breakdown spectroscopy (LIBS) is used to measure the K abundance in a sample and to release its noble gases; the evolved Ar is measured by mass spectrometry, and relative K content is related to absolute Ar abundance by sample mass, determined by optical measurement of the ablated volume. This approach allows K and Ar to be measured on identical volumes multiple times to create an isochron, which improves the age determination and reveals irregularities in the rock if they exist. The KArLE technique measures a whole‐rock K‐Ar age with 10% uncertainty or better for rocks 2 Ga or older, sufficient to resolve the absolute age of many planetary samples. The LIBS–mass spectrometry approach is attractive because the analytical components have been flight‐proven, do not require further technical development and provide essential measurements (complete elemental abundance, evolved volatile analysis, micro‐imaging) as well as in situ geochronology.  相似文献   

6.
《Applied Geochemistry》2006,21(5):730-747
Laser induced breakdown spectroscopy (LIBS) is a simple spark spectrochemical sensor technology in which a laser beam is directed at a sample surface to create a high-temperature microplasma and a detector used to collect the spectrum of light emission and record its intensity at specific wavelengths. LIBS is an emerging chemical sensor technology undergoing rapid advancement in instrumentation capability and in areas of application. Attributes of a LIBS sensor system include: (i) small size and weight; (ii) technologically mature, inherently rugged, and affordable components; (iii) real-time response; (iv) in situ analysis with no sample preparation required; (v) a high sensitivity to low atomic weight elements which are difficult to determine by other field-portable sensor techniques, and (vi) point sensing or standoff detection. Recent developments in broadband LIBS provide the capability for detection at very high resolution (0.1 nm) of all elements in any unknown target material because all chemical elements emit in the 200–980 nm spectral region. This progress portends a unique potential for the development of a rugged and reliable field-portable chemical sensor that has the potential to be utilized in variety of geochemical, mineralogical, and environmental applications.  相似文献   

7.
Due to matrix interference and sample particle size effects, some of the most important and difficult issues in laser‐induced breakdown spectroscopy (LIBS) analysis are the calibration and quantitative measurement of a complex matrix. This study proposes the use of borate fusion as an alternative sample preparation procedure for the quantitative measurement of Al, Fe, Si and Ti in bauxite by LIBS. Analytical calibration curves were made using bauxite certified reference materials (CRM), and the precision and accuracy of the methods were evaluated by analysing an additional bauxite CRM, using two different approaches: pressed powder pellets and fused glass beads. The borate fusion method was the most suitable sample preparation technique, since particle size effects and matrix interference could be minimised, obtaining better linearity on the analytical calibration curves (r2), and more accurate and more precise results for bauxite analysis.  相似文献   

8.
This study illustrates how decoupling of quartz and zircon can be used advantageously in provenance research. Thirty‐eight fine‐grained to coarse‐grained arkose samples of the Early Triassic intracontinental Buntsandstein Group from the Central European Basin in Germany were analysed for their petrography and 1200 grains in 23 of these for their detrital quartz cathodoluminescence characteristics. The samples represent the Hessian and Thuringian sub‐basins and the Eichsfeld–Altmark Swell separating them. The Hessian Sub‐basin includes more metamorphic lithoclasts with a larger content of plutonic grains than are found further east in the Thuringian Sub‐basin. More than 90% of the detrital quartz from the eastern Thuringian Sub‐basin produce medium to bright blue cathodoluminescence colours and corresponding spectra that are typical for igneous or high‐temperature metamorphic origin. Differently, the quartz from the Hessian Sub‐basin mostly luminesces brown and dark to medium blue, typical for a low‐temperature metamorphic origin. Quartz from the Eichsfeld–Altmark Swell and the western Thuringian Sub‐basin is a mixture between these origins. The quartz indicates different catchments for the sub‐basins, possibly the Bohemian Massif and the Massif Central, with converging transport routes on and close to the eastern fringe of the swell. Taking published zircon data from the same samples into account, light mineral‐zircon grain‐size shifts are up to 2 Φ units. That can be explained by mineral decoupling due to different transport modes for quartz and zircon and different zircon‐size availability in the source areas, exaggerated by combined aqueous–aeolian transport, as well as sample preparation‐induced sorting. This study concludes that submerged highs significantly can influence continental sediment transport. Hence, vast, flat continental areas with submerged morphological highs and a seemingly straightforward transportation pattern may be more complex than expected. The results also illustrate that analysis of detritus that has been affected by different dominating transport modes, and further sorting during sampling and preparation can reveal additional source information.  相似文献   

9.
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10.
The Asmari Formation deposited in the Zagros foreland basin during the OligoceneMiocene. Lithologically, the Asmari Formation consists of limestone, dolomitic limestone, dolomite, argillaceous limestone, some anhydrite(Kalhur Member) and sandstones(Ahwaz Member). This study is based on the analysis of core samples from four subsurface sections(wells Mn-68, Mn-281, Mn-292 and Mn-312) in the Marun Oilfield in the Dezful embayment subzone in order to infer their provenance and tectonic setting of the Ahwaz Sandstone Member. Petrographical data reveal that the Ahwaz Sandstone comprises 97.5% quartz, 1.6% feldspar, and 0.9% rock fragments and all samples are classified as quartz arenites. The provenance and tectonic setting of the Ahwaz Sandstone have been assessed using integrated petrographic and geochemical studies. Petrographic analysis reveals that mono- and poly-crystalline quartz grains from metamorphic and igneous rocks of a craton interior setting were the dominant sources. Chemically, major and trace element concentrations in the rocks of the Ahwaz Sandstone indicate deposition in a passive continental margin setting. As indicated by the CIW′ index(chemical index of weathering) of the Ahwaz Sandstone(average value of 82) their source area underwent "intense" recycling but "moderate to high" degree of chemical weathering. The petrography and geochemistry results are consistent with a tropical, humid climate and low-relief highlands.  相似文献   

11.
This contribution presents the first results of compositional tomography of a geological sample. The volume render of 6 × 8 × 1 mm3 was constructed by assembling 63 compositional maps acquired in 21 min (19.5 s/layer) by laser‐induced breakdown spectroscopy (LIBS), which determines the chemical composition of the analysed spot from the light emitted by a plasma produced by the laser. This technique is, therefore, able to directly reveal the 3D distribution of chemical elements in a sample. As an example, the spatial distribution and 3D geometry of visible gold in an ultramafic schist are presented. Inasmuch as this newly developed portable LIBS instrument is able to the rapidly characterize the 3D geometry of any geological materials, it has a high potential to be useful for the mining industry and for a wide range of geosciences, such as structural geology, petrology, sedimentology and economic geology.  相似文献   

12.
Provenance studies of stone artifacts often rely heavily upon chemical techniques such as neutron activation analysis. However, stone specimens with very similar chemical composition can have different mineralogies (distinctive crystalline structures as well as variations within the same mineral) that are not revealed by multielemental techniques. Because mineralogical techniques are often cheap and usually nondestructive, beginning with mineralogy allows the researcher to gain valuable information and then to be selective about how many samples are submitted for expensive and somewhat destructive chemical analysis, thus conserving both valuable samples and funds. Our University of Illinois team of archaeologists and geologists employs Portable Infrared Mineral Analyzer (PIMA) spectroscopy, X‐ray diffraction (XRD), and Sequential acid dissolution/XRD/Inductively coupled plasma (SAD‐XRD‐ICP) analyses. Two case studies of Hopewellian pipes and Mississippian figurines illustrate this mineralogical approach. The results for both studies identify sources relatively close to the sites where the artifacts were recovered: Sterling, Illinois (rather than Ohio) for the (Hopewell) pipes and Missouri (rather than Arkansas or Oklahoma) for the Cahokia figurines. © 2002 Wiley Periodicals, Inc.  相似文献   

13.
Lithium is an important geochemical tracer for fluids or solids. However, because the electron microprobe cannot detect Li, variations of Li abundance at the micrometric scale are most often estimated from bulk analyses. In this study, the Li intense emission line at 670.706 nm in optical emission spectroscopy was used to perfect the analysis of Li at the micrometric scale by means of laser-induced breakdown spectroscopy (LIBS). To estimate lithium content for different geological materials, LIBS calibration of the emission line at 670.706 nm was achieved by use of synthetic glasses and natural minerals. The detection limit for this method is ∼5 ppm Li. Three applications to geological materials show the potential of LIBS for lithium determination, namely for Li-bearing minerals, melt inclusions, quartz, and associated fluid inclusions.For spodumene and petalite from granite pegmatite dikes (Portugal), the Li2O concentrations are 7.6 ± 1.6 wt% and 6.3 ± 1.3 wt%, respectively, by use of LIBS. These values agree with ion microprobe analyses, bulk analyses, or both. For eucryptite crystals, the Li concentrations are scattered because grain size is smaller than the LIBS spatial resolution (6 to 8 μm). Lithium concentrations of melt inclusions from the Streltsovka U deposit (Siberia) are in the range of 2 to 6.2 wt% (Li2O) for Li-rich daughter minerals. Lithium estimations on silicate glasses display values between 90 and 400 ppm.Lithium was also analyzed as a trace element in quartz. Transverse profiles were performed in hydrothermal barren quartz veins from the Spanish Central System (Sierra de Guadarrama). The highest Li concentrations (250 to 370 ppm) were found in specific growth bands in conjunction with the observed variation in optical cathodoluminescence intensity. Considering the fluid inclusion analysis, the source of fluid responsible to the Li enrichment in quartz is probably high-salinity fluids derived from sedimentary basins.  相似文献   

14.
The Western Irish Namurian Basin (WINB) preserves classic examples of basin floor sequences through to slope deposits and deltaic cyclothems. Despite over 50 years of research into the WINB, its sediment provenance remains highly contested. Sedimentological arguments, including palaeocurrent vectors and palaeoslope indicators have been invoked to propose a sediment source from the NW or the west (i.e. from within Laurentia). These same indicators have been subsequently reinterpreted to reflect a southern provenance. It is not clear from sedimentological arguments alone which interpretation more accurately reflects the infilling of the WINB. Regional‐scale constraints on WINB provenance may be obtained with detrital zircon U–Pb geochronology. U–Pb LA‐ICP‐MS detrital zircon analysis was undertaken on samples from three sandstone units at different stratigraphic levels within the WINB siliciclastic sedimentary fill (Ross Formation, Tullig Sandstone, Doonlicky Sandstone). The samples are dominated by 500–700 Ma zircons, which can be correlated with Cadomian–Avalonian orogenic activity within terranes to the south of the WINB (Avalonia/Ganderia, Armorica and Iberia). In contrast, Eastern Laurentia, to the north of the WINB, was devoid of orogenic activity at this time. WINB samples also yield age populations younger than 500 Ma, and older than 700 Ma. These are not diagnostic of a particular source terrane and thus could be derived from terranes north and/or south of the WINB. WINB detrital zircon age spectra can be reconciled by an Avalonian or combined Avalonian–Laurentian provenance for WINB sedimentary strata. Further research is required in order to distinguish between these two possibilities. Copyright © 2011 John Wiley & Sons, Ltd.  相似文献   

15.
The depositional and metamorphic ages and provenances of the Ailaoshan(ALS) Group in the Ailaoshan-Red River(ALS-RR) shear zone, southwestern South China Block(SCB), were investigated to constrain the tectonic history of the southwestern SCB. In this study, we use petrology, geochemical analysis, zircon cathodoluminescence imaging and UPb geochronology to analyse samples of quartzite, garnet-bearing two-mica schist and metapelite. The age spectra of detrital zircon grains from these metasediments show two dominant age peaks at 550–424 Ma and 876–730 Ma and two subordinate peaks at 970–955 Ma and ～2450 Ma. The youngest peak, corresponding to the early Palaeozoic, accounts for more than 20% of the total dates and constrains the deposition of the ALS Group to the Palaeozoic rather than the Palaeoproterozoic as traditionally thought. Moreover, two peaks of metamorphic ages corresponding to the Permo-Triassic and Cenozoic were also identified, and these ages document the tectonothermal events associated with the Indosinian collision between the Indochina Block and the SCB and the Himalayan collision between the Indian and Asian plates. Geochemical data suggest that the provenances of the ALS Group were dominated by continental arc and recycled metasedimentary rocks. The comparison of probability density distribution plots of the detrital zircon U-Pb age data indicates that the Neoproterozoic detritus in the ALS Group was probably derived from the arc-related Neoproterozoic intrusive bodies in the northwestern and southwestern SCB. Furthermore, the early Palaeozoic detritus might have been sourced from eroded early Palaeozoic strata and magmatic plutons in Cathaysia and volcanic rocks in the western Indochina Block.  相似文献   

16.
Inter‐laboratory comparison of laser ablation ICP‐MS and SIMS U‐Pb dating of synthetic detrital zircon samples provides an insight into the state‐of‐the art of sedimentary provenance studies. Here, we report results obtained from ten laboratories that routinely perform this type of work. The achieved level of bias was mostly within ± 2% relative to the ID‐TIMS U‐Pb ages of zircons in the detrital sample, and the variation is likely to be attributed to variable Pb/U elemental fractionation due to zircon matrix differences between the samples and the reference materials used for standardisation. It has been determined that ~ 5% age difference between adjacent age peaks is currently at the limit of what can be routinely resolved by the in situ dating of detrital zircon samples. Precision of individual zircon age determination mostly reflects the data reduction and procedures of measurement uncertainty propagation, and it is largely independent of the instrumentation, analytical technique and reference samples used for standardisation. All laboratories showed a bias towards selection of larger zircon grains for analysis. The experiment confirms the previously published estimates of the minimum number of grains that have to be analysed in order to detect minor zircon age populations in detrital samples.  相似文献   

17.
Manganese oxide ore from the Bonai‐Keonjhar belt of Odisha, India, has been qualitatively assessed through Raman and FTIR spectroscopy, and X‐ray diffraction. Three categories of ore, namely, high‐grade (MnO2: >72%), medium‐grade (MnO2: 55‐72%) and low‐grade (MnO2:40‐55%) from four mine profiles, Purnapani, Joda West, Khandbandh and Bamebariwere, were collected and subjected to vibrational spectroscopic studies. The use of Raman analysis in the microscopic configuration allowed the spectra to be taken at different points on the polished ore. Besides the Raman features of the ß‐MnO2(Pyrolusite) phases, other signals were assigned to isolated FeO ions accommodated in vacancies and to some aluminium silicates. The three grades of ore show different Raman spectra. The FTIR spectra also exhibit contrasting pattern in different grade sample and support these findings. This study demonstrates the use of vibrational spectroscopy to assess the quality of Mn‐oxide ore that could provide a substitute to cumbersome wet chemical analysis  相似文献   

18.
Photo‐induced force microscopy (PiFM) is a new‐frontier technique that combines the advantages of atomic force microscopy with infrared spectroscopy and allows for the simultaneous acquisition of 3D topographic data with molecular chemical information at high spatial (~ 5 nm) and spectral (~ 1 cm?1) resolution at the nanoscale. This non‐destructive technique is time efficient as it requires only conventional mirror‐polishing and has fast mapping rates on the order of a few minutes that allow the study of dynamic processes via time series. Here, we review the method’s historical development, working principle, data acquisition, and evaluation, and provide a comparison with traditional geochemical methods. We review PiFM studies in the areas of materials science, chemistry and biology. In addition, we provide the first applications for geochemical samples including the visualization of faint growth zonation in zircons, the identification of fluid speciation in high‐pressure experimental samples, and of nanoscale organic phases in biominerals. We demonstrate that PiFM analysis is a time‐ and cost‐efficient technique combining high‐resolution surface imaging with molecular chemical information at the nanoscale and, thus, complements and expands traditional geochemical methods.  相似文献   

19.
Determining sediment provenance allows a better understanding of fluvial palaeo-dynamics, and identifying involved watersheds, at broad spatio-temporal scales. Conventional approaches for source identification are usually based on the physical, mineralogical, geochemical, magnetic or isotopic properties of sediments. Rapid, non-destructive and, in well-established contexts, highly accurate, mid-infrared spectroscopy is an alternative method for investigating sediment sources. The present research objectives are: (i) to use the mid-infrared spectroscopy method to discriminate the provenance of fine sediments, by applying discriminant analysis on a large set of reference samples from three different watersheds in the Upper Rhine area (associated with the Rhine, Ill and Vosges tributaries); (ii) to clarify whether the provenance spectra signatures are influenced by riverine depositional contexts (bars versus banks) and, to some extent, by grain size and/or high organic matter content; and (iii) to apply the mid-infrared spectroscopy – discriminant analysis method to a study of fluvial palaeo-dynamics and determine the provenance of palaeo-channel infillings. Three main sedimentary sources, divided into eight sub-categories, have been characterized by 196 modern reference samples from 78 collecting sites. Discriminant analysis displayed a strong separating power by classifying correctly the origin of samples without any inter-group overlap, independently from the geomorphological context (bar or bank) and associated slight changes in organic matter contents or grain size. Mid-infrared spectroscopy – discriminant analysis investigations of the palaeo-channel infill, complemented by radiocarbon dates and mineralogical data, allowed reconstructing general trends for the local morpho-sedimentary dynamics over the last ca 12 millennia.  相似文献   

20.
Volcanic rocks, mainly of intermediate composition, occupy several basins within the rift zone along which the Yangtze River flows in its lower reaches. Potassium‐argon (K‐Ar) age measurements on minerals and whole rock samples from lavas and syenitic intrusives in the Lujiang‐Tzungyang volcanic basin range from 131 to 123 m.y., and biotites from two lavas in the Nanjing‐Wuhu basin have measured ages of 127 and 130 m.y. Incremental heating experiments by the 40Ar/39Ar method on biotite from two volcanic rocks, one from each basin, yield simple age spectra with plateau ages of 129 to 130 m.y. These data provide evidence that the two biotites have remained undisturbed since crystallisation. The combined results show that volcanism was contemporaneous within the two basins in the Early Cretaceous. Vol‐canism in the Yangtze Volcanic Zone is thought to be related to adjustments within the Eurasian plate as a consequence of collision between the earlier Pacific (Kula) plate and the Eurasian plate.  相似文献   

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