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1.
This paper presents an analytical study of LateBronze andIronAge ceramics and natural clay deposits from the archaeological site ofPuig deSa Morisca in southwestMallorca,Spain. In our study, we combine petrographic, micropaleontological, mineralogical (X‐ray powder diffraction) and textural (laser particle size) analyses of sherds and local clays that may have been used as raw material in ceramic production. This approach allowed us to compare the ceramics’ formal characteristics with those observed in nearby plastic clays and assess raw clay procurement and paste preparation. The results indicate the use of local (<500 m distance) calcareous clays throughout theLateBronze andIron ages. This raw material was mixed with other coarser clays or crushed calcite, as well as other calcareous tempers, such as breccias or calcarenites, located close to the site. The results demonstrate that the same clay deposit was used to make ceramic vessels following different technological choices and recipes. Thus, local communities established a strong connection with the same raw materials through time that were located within the potters’ preferential range of exploitation.  相似文献   

2.
Research in 2006 and 2007 dealing with laser ablation‐(multicollector)‐inductively coupled plasma‐mass spectrometry, LA‐(MC)‐ICP‐MS, involved studies concerned with optimising the technique itself, as well as applying the method to a variety of problems in the Earth sciences. The causes of elemental and isotopic fractionation produced during laser ablation continues to be of considerable interest, with evidence mounting that processes occurring both at the ablation site and in the argon plasma of the ICP are culpable. There is growing excitement in the use of femtosecond lasers for LA‐(MC)‐ICP‐MS, with the hope that they reduce or eliminate melting and non‐congruent volatilisation at the ablation site and thus approach stoichiometric sampling. Ablation chamber design emerged as a serious concern, particularly with respect to achieving the rapid washout needed for fine‐scale compositional mapping of geological objects. LA‐MC‐ICP‐MS provided data for a wide range of isotopic systems, especially hafnium, but also B, S, Mg, Cu, Fe, Sr, Nd, Pb and U. Measurement uncertainties in LA‐ICP‐MS were discussed by several researchers, and are critically reviewed here ‐ total uncertainties for trace element concentration measurements of silicates including errors on the calibration values of common reference materials are ～10% (95% confidence limits), though the precision of individual spot measurements (50 to 100 μm) is much better, ～1% RSD, using a 193 nm laser and a sector field‐ICP‐MS. LA‐ICP‐MS U‐Pb ages for zircon and other U‐rich accessory phases are claimed by most geoanalysts to have 2s uncertainties of ～0.7 and 1.3% respectively but the actual accuracy of the method is probably only as good as ～2% (2s), when uncertainties associated with laser‐induced Pb/U fractionation are included.  相似文献   

3.
An efficient, clean procedure for the measurement of element mass fractions in bulk rock nanoparticulate pressed powder pellets (PPPs) by 193 nm laser ablation ICP‐MS is presented. Samples were pulverised by wet milling and pelletised with microcrystalline cellulose as a binder, allowing non‐cohesive materials such as quartz or ceramics to be processed. The LA‐ICP‐MS PPP analytical procedure was optimised and evaluated using six different geological reference materials (JP‐1, UB‐N, BCR‐2, GSP‐2, OKUM and MUH‐1), with rigorous procedural blank quantification employing synthetic quartz. Measurement trueness of the procedure was equivalent to that achieved by solution ICP‐MS and LA‐ICP‐MS analysis of glass. The measurement repeatability was as low as 0.5–2% (1s, n = 6) and, accordingly, PPP homogeneity could be demonstrated. Calibration based on the reference glasses NIST SRM 610, NIST SRM 612, BCR‐2G and GSD‐1G revealed matrix effects for glass and PPP measurement with NIST SRM 61×; using basalt glasses eliminated this problem. Most significantly, trace elements not commonly measured (flux elements Li, B; chalcophile elements As, Sb, Tl, In, Bi) could be quantified. The PPP‐LA‐ICP‐MS method overcomes common problems and limitations in analytical geochemistry and thus represents an efficient and accurate alternative for bulk rock analysis.  相似文献   

4.
Identifying the geological and geographical origin of lithic raw materials is critical to effectively address prehistoric forager raw material economies and mobility strategies. Currently, Paleolithic archaeology in Belgium lacks a systematic sourcing strategy to effectively substantiate detailed interpretations of prehistoric hunter‐gatherer behavioral change across time and space. This pilot study evaluates the potential to “fingerprint” flint from the Mons Basin, western Belgium, using the laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS) technique and a multivariate statistical analysis of 87 geological samples and 39 Gravettian period chipped stone artifacts. We reappraise two hypotheses raised by previous scholars based on visual raw material identification: (1) the Gravettian occupants of Maisières‐Canal supplied themselves with “black flint” from one single source; (2) the sites Rhens and Koblenz‐Metternich yielded artifacts indicative of long‐distance transfer of western Belgian flint into the German Rhineland, ca. 260 km from the primary source area. Our results demonstrate the validity of LA‐ICP‐MS data with flint and compositional data analysis for fingerprinting discrete geological formations from the Mons Basin. We suggest multiple source provisioning for Maisières‐Canal. Geochemical characterization of other potential flint sources is required to validate the long‐distance transfer hypothesis of western Belgian “black flint” into the German Rhineland.  相似文献   

5.
摘〓要：[HT5K]利用阴极发光和LA ICP MS微区定年分析方法,对甘肃天水地区百花岩浆杂岩中的辉长岩进行了单颗粒锆石U Pb同位素分析。百花岩浆杂岩体主要由辉石岩—辉长（闪长）岩—闪长岩—石英闪长岩组成,构成较完整的同源岩浆演化序列,地球化学研究表明其形成于岛弧构造环境。对百花岩浆杂岩中辉长岩的LA ICP MS锆石U Pb同位素定年结果表明,其同位素年龄为(449.7±3.1)Ma（MSWD=1.9）,形成于晚奥陶世,表明西秦岭北带岛弧型岩浆岩的形成时代为晚奥陶世,结合区域地质资料,揭示出以西秦岭北缘关子镇蛇绿岩为代表的古洋盆的俯冲作用及产生岛弧型岩浆活动的时限为中晚奥陶世。   相似文献   

6.
We report homogeneity tests on large natural apatite crystals to evaluate their potential as U reference materials for apatite fission‐track (AFT) thermochronology by laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS). The homogeneity tests include the measurements of major element concentrations by electron probe microanalysis (EPMA), whereas for U concentration, isotope dilution (ID) ICP‐MS and laser ablation (LA) ICP‐MS were employed. Two apatite crystals are potential reference materials for LA‐ICP‐MS analysis: a 1 cm3 fraction of a Durango crystal (7.5 μg g?1 U) and a 1 cm3 Mud Tank crystal (6.9 μg g?1 U). The relative standard deviation (1 RSD) of the U concentration determined by ID‐ICP‐MS of both apatite crystals was ≤ 1.5%, whereas 1 RSD for the LA‐ICP‐MS results was better than 4%, providing sufficient homogeneity for fission‐track dating. The results on the U homogeneity for two different apatite samples are an important step towards establishing in situ dating routines for AFT analysis by LA‐ICP‐MS.  相似文献   

7.
Normally, the use of clays as reference materials in chemical provenance studies of ancient ceramics is complicated due to the original clay paste processing. The primary mixing and/or refining of raw materials during pottery production makes a straightforward comparison of archaeological ceramics with extant geological materials difficult if not impossible in many cases. However, in the case of Pliocene clays from Aegina (Greece), which were examined chemically and mineralogically and compared with Bronze Age pottery produced on the island, a successful exception can be presented. The chemical composition of a large group of Aeginetan pottery resembles the chemical composition of clays from a deposit in close vicinity to the main Bronze Age settlement of the island. Clays from specific outcrops exhibit considerable chemical and mineralogical homogeneity, and the suitability of those clays for pottery production apparently made substantial clay paste processing unnecessary. © 2004 Wiley Periodicals, Inc.  相似文献   

8.
Seven ilmenite (FeTiO3) megacrysts derived from alnöite pipes (Island of Malaita, Solomon Islands) were characterised for their major and trace element compositions in relation to their potential use as secondary reference materials for in situ microanalysis. Abundances of thirteen trace elements obtained by laser ablation ICP‐MS analyses (using the NIST SRM 610 glass reference material) were compared with those determined by solution‐mode ICP‐MS measurements, and these indicated good agreement for most elements. The accuracy of the LA‐ICP‐MS protocol employed here was also assessed by repeated analysis of MPI‐DING international glass reference materials ML3B‐G and KL2‐G. Several of the Malaitan ilmenite megacrysts exhibited discrepancies between laser ablation and solution‐mode ICP‐MS analyses, primarily attributed to the presence of a titano‐magnetite exsolution phase (at the grain boundaries), which were incorporated solely in the solution‐mode runs. Element abundances obtained by LA‐ICP‐MS for three of the ilmenite megacrysts (CRN63E, CRN63H and CRN63K) investigated here had RSD (2s) values of < 20% and therefore can be considered as working values for reference purposes during routine LA‐ICP‐MS analyses of ilmenite.  相似文献   

9.
Ilmenite (FeTiO3) is a common accessory mineral and has been used as a powerful petrogenetic indicator in many geological settings. Elemental fractionation and matrix effects in ilmenite (CRN63E‐K) and silicate glass (NIST SRM 610) were investigated using 193 nm ArF excimer nanosecond (ns) laser and 257 nm femtosecond (fs) laser ablation systems coupled to an inductively coupled plasma‐mass spectrometer. The concentration‐normalised 57Fe and 49Ti responses in ilmenite were higher than those in NIST SRM 610 by a factor of 1.8 using fs‐LA. Compared with the 193 nm excimer laser, smaller elemental fractionation was observed using the 257 nm fs laser. When using 193 nm excimer laser ablation, the selected range of the laser energy density had a significant effect on the elemental fractionation in ilmenite. Scanning electron microscopy images of ablation craters and the morphologies of the deposited aerosol materials showed more melting effects and an enlarged particle deposition area around the ablation site of the ns‐LA‐generated crater when compared with those using fs‐LA. The ejected material around the ns crater predominantly consisted of large droplets of resolidified molten material; however, the ejected material around the fs crater consisted of agglomerates of fine particles with ‘rough' shapes. These observations are a result of the different ablation mechanisms for ns‐ and fs‐LAs. Non‐matrix‐matched calibration was applied for the analysis of ilmenite samples using NIST SRM 610 as a reference material for both 193 nm excimer LA‐ICP‐MS and fs‐LA‐ICP‐MS. Similar analytical results for most elements in ilmenite samples were obtained using both 193 nm excimer LA‐ICP‐MS at a high laser energy density of 12.7 J cm?2 and fs‐LA‐ICP‐MS.  相似文献   

10.
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   

11.
We performed petrophysical analyses on 34 clayey samples of different geological origin within the Campania region of Italy in order to determine possible sources of raw materials used to produce ancient pottery. Possible raw material sources can be grouped into high‐CaO clays (HCC) and low‐CaO clays (LCC). HCC are mainly represented by more recent (Miocene‐Pleistocene) basinal sediments whereas LCC tend to be associated with basinal, alluvial, and pyroclastic deposits. A chemical comparison between clayey raw materials, modern ceramic replicas, and Campanian archaeological ceramics of several typologies (common ware, cooking ware, fine tableware, amphorae, and bricks) from 8th century B.C. to the Middle Ages (a total of 350 ceramic samples) indicates that HCC were extensively used for common wares and that these were either mixed with temper or levigated. In contrast, most of the LCC were used for the production of cookware. We also analyzed the technological potential of the sampled raw materials, taking into consideration their actual and possible uses. We observed that most HCC deposits were well suited for tableware and amphorae, whereas LCC were better for cookware and some fine tableware.  相似文献   

12.
A range of independently characterised reference materials (RMs) for LA‐ICP‐MS, used for the determination of the platinum‐group elements (PGE) and Au in a sulfide matrix, were analysed and compared: 8b, PGE‐A, NiS‐3, Po727‐T1, Po724‐T and the Lombard meteorite. The newly developed RM NiS‐3 was used as the RM for the calibration of all LA‐ICP‐MS analyses and the measured concentrations of the other RMs compared against their published concentrations. This data were also used to assess the consistency of concentrations calibrated against the different RMs. It was found that Po727‐T1 and 8b produced results that were comparable, within uncertainty, for all elements. Po727‐T1 also produced consistent results with NiS‐3 for all elements. All other RMs showed differences for some elements, especially Ru in Po724‐T, and Os, Ir and Au in PGE‐A. The homogeneity of the PGE and Au in each RM was assessed, by comparing the precision of multiple LA‐ICP‐MS spot analyses with the average uncertainty of the signal. Po724‐T, Po727‐T1 and the Lombard meteorite were found to be homogeneous for all elements, but 8b, PGE‐A and NiS‐3 were heterogeneous for some elements. This is the first direct comparison between a range of independently characterised PGE and Au LA‐ICP‐MS RMs.  相似文献   

13.
Sphalerite (ZnS) is an abundant ore mineral and an important carrier of elements such as Ge, Ga and In used in high‐technology applications. In situ measurements of trace elements in natural sphalerite samples using LA‐ICP‐MS are hampered by a lack of homogenous matrix‐matched sulfide reference materials available for calibration. The preparation of the MUL‐ZnS1 calibration material containing the trace elements V, Cr, Mn, Co, Ni, Cu, Ga, Ge, As, Se, Mo, Ag, Cd, In, Sn, Sb, Tl and Pb besides Zn, Fe and S is reported. Commercially available ZnS, FeS, CdS products were used as the major components, whereas the trace elements were added by doping with single‐element ICP‐MS standard solutions and natural mineral powders. The resulting powder mixture was pressed to pellets and sintered at 400 °C for 100 h using argon as an inert gas. To confirm the homogeneity of major and trace element distributions within the MUL‐ZnS1 calibration material, measurements were performed using EPMA, solution ICP‐MS, ICP‐OES and LA‐ICP‐MS. The results show that MUL‐ZnS‐1 is an appropriate material for calibrating trace element determination in sphalerite using LA‐ICP‐MS.  相似文献   

14.
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   

15.
LA-(MC)-ICP-MS锡石U-Pb定年研究进展   总被引：4，自引：0，他引：4  
随着锡石U-Pb定年方法的不断进步,利用锡石微区原位U-Pb定年直接测定锡多金属矿床的成矿(锡矿化)时代已经具备了相对成熟的技术条件,成为锡矿床成矿年代学研究最直接和最有效的途径之一。本文结合近几年本实验室开展的相关研究工作,总结了LA-(MC)-ICP-MS锡石U-Pb定年方法的研究进展,简要评述了多接收器LA-MC-ICP-MS和单接收器LA-ICP-MS两种方法的优缺点。此外,文章还介绍利用LA-(MC)-ICP-MS锡石U-Pb定年方法在湖南芙蓉、云南个旧和广西大厂等超大型锡矿成矿年代学研究中取得的重要进展,指出这一方法目前存在的主要问题和技术难点在于普通铅的准确校正和理想标样的研制,选择合理的普通铅扣除方法和实验外标,有利于提高测定结果的精确度和准确性。同时本文提出通过进一步优化这一测年技术,可以获得锡多金属矿床准确的成矿年代学信息,为全面认识相关矿床的生成和演化历史提供技术支持。  相似文献   

16.
The potters' quarter of the ancient city of Sagalassos, southwest Turkey, was one of the largest and most enduring ceramic‐producing manufactories in the eastern Mediterranean. The objective of our study was to determine environmental circumstances that favored development of different clay resources in the territory of Sagalassos and to assess utilization of these resources in the local pottery manufactory. The potters' quarter was established where, owing to favorable geological circumstances, a large clay body had developed. The bedrock in the potters' quarter, a tectonized ophiolite sequence, has synclinal structure; hence, surface runoff and groundwater tend to accumulate in its center. The weathering of the basic rock formed a smectite‐rich clay with vertic properties. This clay was mined in antiquity, and mineralogical and chemical analyses indicate that it was used for the production of local ceramics from Hellenistic to Byzantine times. It is likely that colluvium on top of the ophiolitic clay at the potters' quarter is related to deforestation and slope processes after the potters' quarter was abandoned. In sum, environmental circumstances determined the location of the artisanal quarter of Sagalassos, with its clay quarrying operation and ceramic manufactory. However, for the local mass‐produced Sagalassos red slip ware, the results of our chemical and mineralogical analyses indicate that a different, more suitable clay was used: detrital lake sediments, rich in chlorite and chlorite/smectite mixed layers, located about 8 km from the original artisanal quarter. The choice for this clay was determined both by the presence of a suitable clay deposit, as well as socio‐economic circumstances such as land ownership. The site of Sagalassos yielded unique evidence of mining of clay at a ceramic production site, as well as import of nearby clays. The local and imported clays were used side‐by‐side, but one for the production of common wares and building ceramics, and the other for the manufacturing of luxury fine tablewares. © 2003 Wiley Periodicals, Inc.  相似文献   

17.
The start of the Upper Würmian in the Alps was marked by massive fluvioglacial aggradation prior to the arrival of the Central Alpine glaciers. In 1984, the Subcommission on European Quaternary Stratigraphy defined the clay pit of Baumkirchen (in the foreland of the Inn Valley, Austria) as the stratotype for the Middle to Upper Würmian boundary in the Alps. Key for the selection of this site was its radiocarbon chronology, which still ranks among the most important datasets of this time interval in the Alps. In this study we re‐sampled all available original plant specimens and established an accelerator mass spectrometry chronology which supersedes the published 40‐year‐old chronology. The new data show a much smaller scatter and yielded slightly older conventional radiocarbon dates clustering at ca. 31 14C ka BP. When calibrated using INTCAL13 the new data suggest that the sampled interval of 653–681 m in the clay pit was deposited 34–36 cal ka BP. Using two new radiocarbon dates of bone fragments found in the fluvioglacial gravel above the banded clays allows us to constrain the timing of the marked change from lacustrine to fluvioglacial sedimentation to ca. 32–33 cal ka BP, which suggests a possible link to the Heinrich 3 event in the North Atlantic. Copyright © 2013 John Wiley & Sons, Ltd.  相似文献   

18.
This paper presents a morphological and hydrogeological reconstruction of the Murcia Valley at the location of the great Roman stadium Circus Maximus in Rome. We reconstruct a valley segment using ERT (electrical resistivity tomography) and geoarchaeological drilling data that identified three main layers. The basal layer, with high resistivity values and convex shapes, is correlated to alluvial gravel and lithified silt‐clay sediments. The middle layer shows low‐to‐medium resistivity values extending to concavities between the basal convex shapes. The very low resistivity values of this middle layer characterize elliptical to circular morphologies and have been ascribed to the presence of water‐saturated clay‐silt and peaty sediments. The surface layer is characterized by widespread lateral inhomogeneity interpreted as anthropogenic fill. The data indicate a pre‐Roman anastomosed alluvial plain subsequently modified by human intervention. In an effort to reclaim the valley for construction of the Circus, the Romans utilized the natural topography and created a central embankment, later becoming the Spina, by filling depressions with sand taken from adjacent bars. Our study contributes to (1) knowledge of the pre‐Roman landscape, (2) understanding anthropogenic modification of the Murcia Valley flood plain, and (3) archaeological interpretation of the monument.  相似文献   

19.
In both nature and synthetic experiments, the common iron oxide haematite (α‐Fe2O3) can incorporate significant amounts of U into its crystal structure and retain radiogenic Pb over geological time. Haematite is a ubiquitous component of many ore deposit types and, therefore, represents a valuable hydrothermal mineral geochronometer, allowing direct constraints to be placed on the timing of ore formation and upgrading. However, to date, no suitable natural haematite reference material has been identified. Here, a synthetic haematite U‐Pb reference material (MR‐HFO) is characterised using LA‐ICP‐MS and ID‐TIMS. Centimetre‐scale ‘chips’ of synthesised α‐Fe2O3 were randomly microsampled via laser ablation‐extraction and analysed using ID‐TIMS. Reproducible U/Pb and Pb/Pb measurements were obtained across four separate chips (n = 13). Subsequently, an evaluation of the suitability MR‐HFO in constraining U‐Pb data via LA‐ICP‐MS is presented using a selection of natural samples ranging from Cenozoic to Proterozoic in age. The MR‐HFO normalised U‐Pb ratios are more concordant and ages more accurate versus the same LA‐ICP‐MS spot analyses normalised to zircon reference material, when compared with independently acquired ID‐TIMS data from the same natural haematite grains. Results establish MR‐HFO as a suitable reference material for LA‐ICP‐MS haematite U‐Pb geochronology.  相似文献   

20.
This paper contains the results of an extensive isotopic study of United States Geological Survey GSD‐1G and MPI‐DING reference glasses. Thirteen different laboratories were involved using high‐precision bulk (TIMS, MC‐ICP‐MS) and microanalytical (LA‐MC‐ICP‐MS, LA‐ICP‐MS) techniques. Detailed studies were performed to demonstrate the large‐scale and small‐scale homogeneity of the reference glasses. Together with previously published isotopic data from ten other laboratories, preliminary reference and information values as well as their uncertainties at the 95% confidence level were determined for H, O, Li, B, Si, Ca, Sr, Nd, Hf, Pb, Th and U isotopes using the recommendations of the International Association of Geoanalysts for certification of reference materials. Our results indicate that GSD‐1G and the MPI‐DING glasses are suitable reference materials for microanalytical and bulk analytical purposes.  相似文献   

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