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1.
In this study, X‐ray diffraction (XRD) is applied to select ceramics, particularly dating to the Ayyoubid (A.D. 1174–1250) period from Tell Tuneinir in Syria. Because XRD has not been commonly applied to archaeological ceramics, a thorough background of the technique is given, with emphasis on quantitative measurements of quartz and calcite tempers. Several compositional groups based on raw materials and firing conditions emerge. While most ceramic samples are of local manufacture, Islamic stonepaste wares, and the “grenade” sample emerge as likely imports. We conclude that XRD is a powerful tool in characterizing archaeological ceramics and may be used to semi‐quantitatively gauge the amount of quartz, calcite, and feldspars in a sample. © 2001 John Wiley & Sons, Inc.  相似文献   

2.
Roman mortars were collected from the Villa dei Quintili in Rome, an archaeological site consisting of numerous edifices from nine construction phases dating from the 2nd century A.D. to modern times. A multianalytical approach was used on 34 mortar samples to infer the evolution of production techniques over time and to identify the source area of calcareous raw materials used in the preparation of the lime. Optical microscopy, scanning electron microscopy coupled with an energy‐dispersive system, and laser ablation inductively coupled plasma mass spectrometry were used to study the samples. The major and trace element data were compared with the compositions of two types of limestone samples (Calcare Massiccio and Calcare Maiolica) collected from the Cornicolani Mountains. The results suggest that the technological practices and the calcareous raw materials used for lime production remained unchanged over the time period considered (2nd century A.D. to 3rd century A.D.). The compositions of lime‐related particles in the mortars match those of Calcare Maiolica, which suggests its use as raw material for lime production. On the whole, the results are in agreement with data from existing literature regarding both the use by Roman builders of specific raw materials for the mortars’ production and the relative supply area.  相似文献   

3.
Recent transportation infrastructure works in Naples, Italy, provided important discoveries related to the production of pottery in the Hellenistic workshop area of Piazza Nicola Amore. A minero‐petrographic investigation was conducted on 35 samples belonging to the widespread Campana A ware and production indicators (clayey raw materials, unfired Graeco‐Italic amphorae, kiln wastes, workshop tools). Additional analysis was conducted on black‐glaze and common ware samples for comparison. The analyses reveal compositional and technological homogeneity of Campana A ware. Samples are characterized by low CaO content with evidence of both volcanic and sedimentary components, suggesting that different clay sources were properly mixed to prepare a standard recipe. Production indicators, black‐glaze and common wares, have a composition well consistent with the calcareous clays from the island of Ischia. Leucite‐ and garnet‐bearing temper from the Somma Volcano were used for the preparation of coarse‐grained pastes, unfired Graeco‐Italic amphorae, and clayey raw materials, thus suggesting that they represented the clay sources for amphorae production. Our results reveal new technological and socioeconomic aspects of Hellenistic pottery production in the Bay of Naples, in particular for the Campana A ware, now representing a new reference group: Neapolis.  相似文献   

4.
The creation of anthropic sediments, traditionally referred to under the blanket term midden, through the utilization of settlement waste materials in domestic settlement construction was first recognized during early excavations at the Orcadian Neolithic site of Skara Brae (V.G. Childe, 1931a; 1931b). Prior to the present study there has been no systematic attempt to identify the nature of these sediments at Skara Brae, whose likely occupation dates between ˜3100 and 2500 B.C., or to assess whether different materials were incorporated into construction or varied with different phases of site formation. The opportunity to begin addressing these issues arose with the location of undisturbed sediment samples held in storage since the last site excavations of 1972–1973 (D.V. Clarke, 1976). Ten thin sections were manufactured from these samples, representing earlier and later phases of Neolithic settlement at Skara Brae. Observations using thin‐section micromorphology, supported by total phosphorus and particle‐size distribution analyses, suggest that both earlier and later settlement phases show accumulation of household waste dominated by fuel residues. These wastes may have been used to help stabilize wind‐blown sand deposits during the later settlement phases. In addition, the use of clay material tempered with household waste is associated with wall construction. Animal manures are only evident in anthropic deposits on the edge of the main settlement site where composting may have been taking place, and there is no evidence for their use in site construction. The authors conclude by drawing attention to possible diverse uses of anthropic sediments in settlement construction at other Neolithic settlements in Orkney. © 2006 Wiley Periodicals, Inc.  相似文献   

5.
Resin‐impregnated sediment blocks are a by‐product of micromorphological sample processing. These blocks can be further studied using a variety of destructive, nondestructive, and minimally destructive geochemical techniques. X‐ray fluorescence microanalyses conducted on sediment blocks yield semiquantitative major and trace elemental abundances that can be used to generate compositional maps, and to illustrate compositional change within or between archaeological strata and features. Sediment blocks can also be drilled to obtain small sediment samples for stable oxygen and carbon isotopic analyses. Both elemental and isotopic analyses can be conducted in conjunction with micromorphological analyses to yield a holistic picture of archaeological sediment composition, source, and depositional processes. The integration of micromorphological, compositional, and isotopic analyses is used here to aid in the differentiation of calcareous ash and lime plasters from the Neolithic site of Asıklı Höyük, Turkey.  相似文献   

6.
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   

7.
An integrated petrographic and spectroscopic (X‐ray diffraction, phosphor imaging and synchrotron X‐ray absorption spectroscopy) study of tufas from the Miocene Barstow Formation, California, relates sample morphology, mineralogy and geochemical composition. The tufas, composed mainly of calcite that formed at the interface between an ancient alkaline lake and ground or spring waters, have textures similar to those of microbially mediated terrestrial stromatolites and travertines. The tufas have elevated concentrations of a number of trace elements including Mn, Fe, Sr and U. Synchrotron X‐ray fluorescence analyses show that U concentrations can exceed 500 p.p.m. X‐ray absorption spectroscopy indicates that the U in these samples is incorporated as U(IV). It is suggested here that alkaline lake waters had a high U/Ca ratio and tufa calcite formed where groundwater or (possibly epithermal) springs brought in Ca and trace elements such as Sr. The rapid, and possibly microbially mediated, precipitation of calcite allowed for incorporation of high concentrations of trace metals as either structural substitutes or extremely fine‐scale inclusions.  相似文献   

8.
炼锌废渣中重金属 Pb、Zn的矿物学特征   总被引：8，自引：1，他引：8  
利用X射线衍射（XRD）和带能谱的电子显微镜（TEM／SEM）等方法研究土法炼锌固体废物的矿物组成，特别是重金属Pb和Zn的矿物学赋存特征。结果表明：固体废物是一种高度不均匀的复杂集合体。废渣主要是由石英、长石、碳酸盐矿物、铁质和铝质的非晶质玻璃以及少量风化次生矿物相组成。Pb在废渣中主要以金属Pb形式存在，或呈纳米金属Pb颗粒包裹或吸附于其它矿物表面及玻璃质集合体中。废渣中Zn的存在形式比Pb复杂得多，有硅锌矿、 锰硅锌矿、丝锌铝石等矿物存在形式，在其它矿物表面或玻璃质集体体中也能见到少量纳米级金属Zn。  相似文献   

9.
Micro‐X‐ray fluorescence scanning spectroscopy of marine and lake sedimentary sequences can provide detailed palaeoenvironmental records through element intensity proxy data. However, problems with the effects of interstitial pore water on the micro‐X‐ray fluorescence intensities have been pointed out. This is because the X‐ray fluorescence intensities are measured directly at the surfaces of split wet sediment core samples. This study developed a new method for correcting X‐ray fluorescence data to compensate for the effects of pore water using a scanning X‐ray analytical microscope. This involved simultaneous use of micro‐X‐ray fluorescence scanning spectroscopy and an X‐ray transmission detector. To evaluate the interstitial pore water content from the X‐ray transmission intensities, a fine‐grained sediment core retrieved from Lake Baikal (VER99‐G12) was used to prepare resin‐embedded samples with smooth surfaces and uniform thickness. Simple linear regression between the linear absorption coefficients of the samples and their porosity, based on the Lambert–Beer law, enabled calculation of the interstitial pore spaces and their resin content with high reproducibility. The X‐ray fluorescence intensities of resin‐embedded samples were reduced compared with those of dry sediment samples because of: (i) the X‐ray fluorescence absorption of resin within sediment; and (ii) the sediment dilution effects by resin. An improved micro‐X‐ray fluorescence correction equation based on X‐ray fluorescence emission theory considers the instrument's sensitivity to each element, which provides a reasonable explanation of these two effects. The resin‐corrected X‐ray fluorescence intensity was then successfully converted to elemental concentrations using simple linear regression between the data from micro‐X‐ray fluorescence scanning spectroscopy and from the conventional analyzer. In particular, the calculated concentration of SiO2 over the depth of the core, reflecting diatom/biogenic silica concentration, was significantly changed by the calibrations, from a progressively decreasing trend to an increasing trend towards the top of the core.  相似文献   

10.
New trace element analyses are reported for 25 samples of basalt taken from a vertical traverse in an 11 m thick single flow of Icelandic tholeiite. Compositional variations among the samples substantially exceed those expected from analytical uncertainties and are random with respect to height in the flow. These variations in an undifferentiated single flow suggest a short-range segregation model in which the proportions of phenocrysts. groundmass minerals and residual liquid vary randomly among different samples of the flow. A least-squares mixing model is used to determine whether the compositional variations reflect different proportions of crystallizing phases and residual liquid. Most elements (alkalis and alkaline earths excepted) are fit to within their analytical uncertainties, supporting the short-range segregation model. A Monte-Carlo calculation is used to model the phase modes and compositions of various samples of a hypothetical basalt. Most compositional and interelement variations for the Icelandic basalt resemble those of the hypothetical basalt. The calculations show that short-range segregation produces inhomogeneity as large as interflow compositional differences and results in incoherence among elements with different geochemical behaviors while preserving coherence among elements of similar behavior.  相似文献   

11.
Over the last ninety years or so, archaeological field work on outcrops of raw materials in western France has allowed researchers to identify the use of a large number of deformed rock types in lithic industries. These materials include Armorican phtanites, which are cherts that were widely exploited during the Mesolithic, principally during its final phase (5500–5000 yrs cal. B.C.). Because of variations in the mineralogical composition and physical properties of phtanites, different mechanical properties are exhibited by samples from the four main geological formations containing this rock type in the Armorican Massif of western France. These geological and mechanical parameters influenced the quantity of rock used and the knapping methods employed. They also influenced the tool types produced and their transfer, as recorded in archaeological sequences. The types of raw materials used are also controlled by the distance to sources of coastal flint pebbles or other autochthonous siliceous rocks. Therefore, the role of raw material properties in the creation and persistence of techno‐cultural or economic characteristics is different for each type of phtanite and yields fundamental information on the interaction of society with the geological environment. © 2010 Wiley Periodicals, Inc.  相似文献   

12.
Four outcrops of Lower Cretaceous (Barremian) karst bauxites located in Teruel (NE Spain) were analysed to determine their mineral associations and genesis related to climatic palaeoweathering events and late superimposed kaolinization processes. The materials comprise metric‐sized pisolitic blocks embedded in a clay‐rich red groundmass. Fourteen samples were examined by X‐ray diffraction, optical microscopy, scanning and transmission electron microscopy and the major elements were analysed by inductively‐coupled plasma mass spectroscopy (ICPMS). The samples are composed of kaolinite, gibbsite, goethite, and hematite as the main phases, with diaspore, boehmite, anatase, and rutile as accessory minerals. The results show a complex sequence of mineralogical and geochemical processes that transformed the parent rock into the current bauxite materials. The clay‐rich groundmass constitutes the lateritic parent material of the pisolitic bauxites. In the parent material authigenic kaolinite (e.g. vermicular kaolinite and kaolinite between cleavage sheets of pre‐existing mica) has been observed; Fe oxides formed subsequent to kaolinite. In the pisolitic bauxites, mineralogical and textural evidence indicates that bauxitization took place at the expense of previous kaolinite, with gibbsite post‐dating the other Al hydroxides. The pisolitic bauxites also show a more homogeneous chemical composition and a relative Ti, Al and Zr enrichment. The data are consistent with an intense palaeoweathering event during the Lower Cretaceous (Barremian) under tropical climatic conditions (warm and humid). Several stages probably took place during the bauxitization process, suggesting variations in water saturation conditions. Subsequent karst reactivation stages and related collapses were responsible for the present lithostructure of the deposits and allowed late kaolinization not related to climate to take place. Copyright © 2014 John Wiley & Sons, Ltd.  相似文献   

13.
Quantification of discrete pressure–temperature domains in deformed chlorite + white mica‐bearing metapelites was undertaken on mineral compositions derived by two‐dimensional microprobe compositional mapping of selected areas of rock thin sections. In order to achieve compositional information at sufficient analytical precision, spatial resolution and sample coverage within a typical analysis time of 1 day, an optimization of measurement methods was necessary. The method presented here allows collection of raw counts for eight different element concentrations at an analytical precision of ～1–2 wt%. X‐ray intensity multiplane maps (one map per measured chemical element) are translated into concentration multiplane maps, utilizing selected conventionally measured spot analyses combined with the Castaing approximation for each mineral. As this step requires identification of the different minerals present in the mapped area, a statistical clustering technique to identify different groups of composition was developed, guided by simple petrographic inspection of the thin section, to delineate the important minerals in the mapped area. Finally, the compositions of each pixel are translated into a mineral structural formula thus yielding a new kind of image with a high content of petrological information. The reliability of the mineral composition images was emphasized by carrying out precision tests on the analytical data. The possible use of chemical maps to infer the P–T–deformation history of metamorphic rocks is illustrated with two samples from the Spitzbergen and the Sambagawa blueschist facies belts. In both samples, a strong correlation between structures and chemistry is observed. Qualitative estimates of P–T conditions from the Si‐content of mica and chlorite are in good agreement with their location in microstructures that formed at different times. Therefore, the combination of chemical maps with microstructural observations is a very powerful approach to understand both the evolution of complex metamorphic rocks and the control by deformation of mineral reactivity.  相似文献   

14.
Speciation of Cr in geochemical reference materials was characterised by sequential extraction and X‐ray absorption near‐edge structure (XANES) spectroscopy to identify Cr(III) resulting from the reduction of pollutant Cr(VI). Sequential extraction suggested that the amount of Cr associated with an acetic acid soluble fraction was low; Cr associated with a reducible phase and an oxidisable phase was extracted at 5–10% of the total Cr concentration, and the residual phase was found to be the dominant Cr‐containing fraction. Cr speciation in soil artificially doped with Cr(VI) and sediment samples collected from highly populated and industrialised areas was different from that in naturally occurring materials. Substantial Cr was extracted as a reducible phase (15–30%) and an oxidisable phase (30–60%) for these samples. Through subsequent XANES spectroscopy analysis, the reducible phase was explained by Cr bound to Fe hydroxide, while the oxidisable phase was a mixture of Cr bound to humic substances and Cr hydroxides. That is, Cr(VI) present as a contaminant in sediments and soils was reduced to Cr(III), which then bound to Fe hydroxide and humic substances, precipitating as a hydroxide. Thus, a combination of sequential extraction and XANES spectroscopy allows for effective identification and quantification of the chemical forms of Cr in sediments and soils.  相似文献   

15.
In this study, we employ wavelength‐dispersive X‐ray fluorescence (WDXRF) to characterize construction materials from Formative civic architecture (1000 B.C.E.–C.E. 400), ethnographic mudbricks, and off‐site controls from the Taraco Peninsula, Bolivia. The preparation of earthen construction materials for civic buildings can shed light on aspects of community development such as labor organization, resource management, and architectural technologies. We apply geochemical results to reconstructing how public buildings were made as communities moved toward socio‐political complexity in this region. However, there are few geochemical studies in the Andes, and little prior scientific analysis of earthen architecture. We therefore tested the efficacy of WDXRF for this region, and developed control materials. Our archaeological samples were selected from two Formative villages, Chiripa and Kala Uyuni. In this study, we performed WDXRF analyses on 63 archaeological and control samples including archaeological floors, walling, plasters, and mortars, as well as contemporary ethnographic walling and topsoils. Elemental signatures for 28 elements clearly distinguished the archaeological flooring, walling, plaster, and mortars from ethnographic and off‐site controls. More subtle variations were detected that distinguish study sites and the different material types. Laboratory‐calibrated multi‐element XRF effectively supports efforts to reconstruct the pathways to social complexity in the Titicaca Basin.  相似文献   

16.
Compared with solution ICP‐MS, LA‐ICP‐MS studies have thus far reported comparatively few external reference data for accuracy estimates of experiments. This is largely the result of a paucity of available reference materials of natural composition. Here, we report an evaluation of natural glass (obsidian) as an inexpensive and widely available external reference material. The homogeneity of over forty elements in six different obsidian samples was assessed by LA‐ICP‐MS. Accuracy was tested with two obsidian samples that were fully characterised by electron probe microanalysis and solution ICP‐MS. Laser ablation experiments were performed with a variety of ablation parameters (fluence, spot sizes, ablation repetition rates) and calibration approaches (natural vs. synthetic reference materials, and different internal standard elements) to determine the best practice for obsidian analysis. Furthermore, the samples were analysed using two different laser wavelengths (193 nm and 213 nm) to compare the effect of potential ablation‐related phenomena (e.g., fractionation). Our data indicate that ablation with fluences larger than 6 J cm?2 and repetition rates of 5 or 10 Hz resulted in the most accurate results. Furthermore, synthetic NIST SRM 611 and 612 glasses worked better as reference materials compared with lower SiO2 content reference materials (e.g., BHVO‐2G or GOR128‐G). The very similar SiO2 content of the NIST SRM glasses and obsidian (i.e., matrix and compositional match) seems to be the first‐order control on the ablation behaviour and, hence, the accuracy of the data. The use of different internal standard elements for the quantification of the obsidian data showed that Si and Na yielded accurate results for most elements. Nevertheless, for the analysis of samples with high SiO2 concentrations, it is recommended to use Si as the internal standard because it can be more precisely determined by electron probe microanalysis. At the scale of typical LA analyses, the six obsidian samples proved to be surprisingly homogenous. Analyses with a spot size of 80 μm resulted in relative standard deviations (% RSD) better than 8% for all but the most depleted elements (e.g., Sc, V, Ni, Cr, Cu, Cd) in these evolved glasses. The combined characteristics render obsidian a suitable, inexpensive and widely available, external quality‐control material in LA‐ICP‐MS analysis for many applications. Moreover, obsidian glass is suited for tuning purposes, and well‐characterised obsidian could even be used as a matrix‐matched reference material for a considerable number of elements in studies of samples with high SiO2 contents.  相似文献   

17.
There is currently a lack of well‐characterised matrix‐matched reference materials (RMs) for forensic analysis of U‐rich materials at high spatial resolution. This study reports a detailed characterisation of uraninite (nominally UO2+x) from the Happy Jack Mine (UT, USA). The Happy Jack uraninite can be used as a RM for the determination of rare earth element (REE) mass fractions in nuclear materials, which provide critical information for source attribution purposes. This investigation includes powder X‐ray diffraction (pXRD) data, as well as major, minor and trace element abundances determined using a variety of micro‐analytical techniques. The chemical signature of the uraninite was investigated at the macro (cm)‐scale with micro‐X‐ray fluorescence (µXRF) mapping and at high spatial resolution (tens of micrometre scale) using electron probe microanalysis (EPMA) and laser ablation‐inductively coupled plasma‐mass spectrometry (LA‐ICP‐MS) analyses. Based on EPMA results, the uraninite is characterised by homogeneous UO2 and CaO contents of 91.57 ± 1.49% m/m (2s uncertainty) and 2.70 ± 0.38% m/m (2s), respectively. Therefore, CaO abundances were used as the internal standard when conducting LA‐ICP‐MS analyses. Overall, the major element and REE compositions are homogeneous at both the centimetre and micrometre scales, allowing this material to be used as a RM for high spatial resolution analysis of U‐rich samples.  相似文献   

18.
The preparation and characterisation of three nickel ores and two nickel concentrate certified reference materials are described in this paper. The samples of nickel ore and nickel concentrate were collected from the Hongqiling nickel deposit in Jilin province. The raw materials were crushed and passed through a 2.0‐mm sieve. The rough samples were then ground for 48 hr in a high‐alumina ball mill to a final size of < 0.074 mm. Homogeneity of the samples was tested by X‐ray fluorescence spectrometry (WD‐XRF) and inductively coupled plasma‐atomic emission spectrometry (ICP‐AES). The relative standard deviations (RSD) of results on mass fraction measurements by WD‐XRF were < 1.0% m/m for eighteen components. F‐tests showed that all five samples were homogeneous. Nineteen laboratories contributed with measurement results (2127 in total) for the certification of mass fractions for twenty‐three elements and compounds. Twenty‐three components in the nickel ores and twenty components in the nickel concentrates were characterised as certified values, while the Ni mass fractions ranges from 0.1 to 9.02% m/m in these certified reference materials. These five samples were approved as national certified reference materials by the National Organisation of Reference Materials of China in 2012.  相似文献   

19.
Coal‐based graphene quantum dots (GQDs) were successfully produced via a one‐step chemical synthesis from six different coal ranks, from which two superhigh organic sulfur (SHOS) coals were selected as natural S‐doped carbon sources for the preparation of S‐doped GQDs. The effects of coal properties on coal‐based GQDs were analyzed by means of high‐resolution transmission electron microscopy (HRTEM), X‐ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, X‐ray photoelectron spectroscopy (XPS), ultraviolet‐visible (UV‐Vis) absorption spectroscopy, and fluorescence emission spectra. It was shown that all coal samples can be used to prepare GQDs, which emit blue‐green and blue fluorescence under ultraviolet light. Anthracite‐based GQDs have a hexagonal crystal structure without defects, the largest size, and densely arranged carbon rings in their lamellae; the high‐rank bituminous coal‐based GQDs are relatively reduced in size, with their hexagonal crystal structure being only faintly visible; the low‐rank bituminous coal‐based GQDs are the smallest, with sparse lattice fringes and visible internal defects. As the metamorphism of raw coals increases, the yield decreases and the fluorescence quantum yield (QY) initially increases and then decreases. Additionally, the surface of GQDs that were prepared using high‐rank SHOS coal (high‐rank bituminous coal) preserves rich sulfur content even after strong oxidation, which effectively adjusts the bandgap and improves the fluorescence QY. Thus, high‐rank bituminous coal with SHOS content can be used as a natural S‐doped carbon source to prepare S‐doped GQDs, extending the clean utilization of low‐grade coal.  相似文献   

20.
采用X射线荧光光谱法测定高氟地质样品中氟、钙等元素,对样品进行熔融制样前处理,理论α系数和经验系数法校正基体效应。应用此方法分析国家一级标准物质和代表性样品,所测元素的精密度(RSD)均小于5%(除含量较低元素);分析不参加回归的标准物质和人工配制的标准样品,测量结果与标准值基本一致。通过实验数据可知,该方法可以满足高氟硅酸盐样品、萤石、萤石型铀矿、磷矿石等样品的测定要求。  相似文献   

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