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1.
This review describes developments major and in trace element determination using atomic absorption spectroscopy (AAS), inductively coupled plasma-atomic emission spectrometry (ICP-AES), instrumental neutron activation analysis (INAA), and X-ray fluorescence (XRF) spectrometry that were reported in 2008 and 2009. Publication levels were comparable to those of previous years, except for XRF which showed an increase in the number of articles published in the past 2 years. In terms of number of publications and impact, the most active field was AAS, while INAA was the least active. As expected for well-established and mature methods, novel developments for all four analytical techniques were relatively sparse. For AAS, the most notable publications concerned developments in sample introduction, particularly focussing on solid samples, increasing analyte sensitivity, and higher sample throughput. For ICP-AES, publication of developments in sample introduction, remediation of matrix effects and calibration continues. Compared with past years, there was a clear focus on sample preconcentration methods, but very few publications reporting new hyphenated speciation methods. For INAA, there were several publications exploring the accuracy and robustness of the method, as well as the requirements for INAA to meet criteria for a primary method of measurement. Two other related techniques, delayed neutron activation analysis, and prompt gamma activation analysis, were also described. Hyphenated XRF techniques showed interesting developments in enabling XRF and XRD analysis on the same spot, and further work characterising and calibrating three-dimensional micro-XRF shows promising results for investigating sample heterogeneity.  相似文献   

2.
These technologically mature techniques occupied a stable to modestly increasing sector of the spectrum of analytical methods in Earth and environmental sciences in 2004–5. Despite this, several notable advances were reported in this two year period. In the field of X-ray fluorescence spectrometry, these included the development of portable synchrotron and total reflection instruments, the use of pyroelectric crystals as X-ray generators, introduction of high-purity Ge detector arrays, and the development of an XRF imaging spectrometer with the capability of mapping analytes and X-ray intensity ratio. Atomic absorption s spectrometry saw major work published on high-resolution continuum source AAS (HR-CS AAS) involving the development of a xenon short-arc lamp. Other advances included the use of laser wave mixing in a graphite furnace tube (with a claimed detection limit of 10–16 g g-1), solid sampling and ultrasound in sample preparation. Neutron activation analysis saw two innovations that may herald future growth in this technique, namely a neutron source free of a nuclear reactor and a detector operating at room temperature.  相似文献   

3.
《Applied Geochemistry》2005,20(9):1737-1745
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4.
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   

5.
Geological reference materials (RMs) with variable compositions and NIST SRM 612 were analysed by isotope dilution mass spectrometry for bulk rock concentrations of chalcogen elements (sulfur, selenium and tellurium), rhenium and platinum‐group elements (PGEs: Ru, Pd, Os, Ir and Pt), including the isotope amount ratios of 187Os/188Os. All concentrations were obtained from the same aliquot after HCl‐HNO3 digestion in a high pressure asher at 320 °C. Concentrations were determined after chemical separation by negative TIMS, ICP‐MS and hydride generation ICP‐MS (Se, Te). As in previous studies, concentrations of the PGEs in most RMs were found to be highly variable, which may be ascribed to sample heterogeneity at the < 1 g level. In contrast, S, Se and Te displayed good precision (RSD < 5%) in most RMs, suggesting that part of the PGE budget is controlled by different phases, compared with the chalcogen budget. The method may minimise losses of volatile chalcogens during the closed‐system digestion and indicates the different extent of heterogeneity of chalcogens, Re and PGEs in the same sample aliquot. OKUM, SCo‐1, MRG‐1, DR‐N and MAG‐1 are useful RMs for the chalcogens. NIST SRM 612 displays homogenous distribution of S, Se, Te, Pt and Pd in 30 mg aliquots, in contrast with micro‐scale heterogeneity of Se, Pd and Pt.  相似文献   

6.
The JEB Tailings Management Facility (TMF) is central to reducing the environmental impact of the McClean Lake uranium mill facility that is operated by AREVA Resources Canada. This facility has been designed around the idea that elements of concern (e.g., U, As, Ni, Se, Mo) will be controlled through equilibrium with precipitants. Confirming the presence of calcium-containing carbonates in the JEB TMF is the first step in determining if gypsum (CaSO4·2H2O) controls the concentration of HCO3− (aq), limiting the formation of soluble uranyl bicarbonate complexes. A combination of X-ray diffraction (XRD), X-ray absorption near-edge spectroscopy (XANES), and microprobe X-ray fluorescence (XRF) mapping was used to analyze a series of tailings samples from the JEB TMF. Calcium carbonate in the form of calcite (CaCO3), aragonite (CaCO3), and dolomite (CaMg(CO3)2) were identified by analysing Ca K-edge μ-XANES spectra coupled with microprobe XRF mapping. This is the first observation of these phases in the JEB TMF. The combination of μ-XANES and XRF mapping provided a greater sensitivity to low concentration calcium species compared to the other techniques used, which were only sensitive to the major species present (e.g., gypsum).  相似文献   

7.
A comparison is made of elemental analyses of sediment samples (lake bottom sediments and sediments from the petroliferous Bazhenovka Formation) by five competitive methods (synchrotron radiation X-ray fluorescence (SR-XRF), INAA, ICP-MS, AAS and traditional XRF). The object of this study was to identify the most suitable analytical techniques for applications in sedimentary geochemistry. Advantages and shortcomings of the five techniques were considered with respect to applications related to studies of palaeo-climate changes recorded in sedimentary cores from Lake Baikal and the geochemical stratigraphy of the Bazhenovka Formation, which is rich in organic material. We have concluded that SR-XRF was the best technique for producing extensive analytical data series, from the point of view of its speed, ease of application, cost, non-destructive nature and sensitivity, which allowed for the simultaneous determination of more than twenty elements of geochemical interest in small samples of sediments. An additional benefit of the method was demonstrated when used for the independent certification of geological reference materials. International reference samples BIL-1 and SDO-1 were certified by means of this method without use of reference materials. Analyses were based on the physics of the theory of energy transport.  相似文献   

8.
This paper reports the results of pilot‐study efforts to develop methods to profile quartzite, a rock type to which geochemical and other sourcing techniques have only rarely been applied. The long‐term goal of the research is to fingerprint sources of quartzite in the Gunnison Basin, southwest Colorado, used by Paleoindian people ca. 11,500–8,000 years ago to make stone tools. Success would facilitate reconstruction of Paleoindian mobility in the Southern Rocky Mountains and potentially anywhere prehistoric people used quartzite. The goals of this paper are more modest: to demonstrate that a small‐scale exploration of sourcing techniques suggests reason for optimism that quartzites may be amenable to source discrimination. For the same twenty Gunnison Basin quartzite samples, this study evaluated petrography, ultraviolet fluorescence (UVF), wavelength dispersive X‐ray fluorescence (WD‐XRF), instrumental neutron activation analysis (INAA), and inductively coupled plasma mass spectrometry—both acid‐digestion (AD‐ICP‐MS) and laser ablation (LA‐ICP‐MS)—as means to differentiate among the specimens and the sources they represent. Although more testing is needed to verify and refine our results, the study suggests there is potential for petrography, INAA, and both versions of ICP‐MS to discriminate among quartzites from different source localities in the Gunnison Basin. The greatest potential for discriminating among different sources of quartzite in the Gunnison Basin may lie in a methodology combining petrographic analysis and LA‐ICPMS. Future testing is required to evaluate this two‐fold approach. © 2008 Wiley Periodicals, Inc.  相似文献   

9.
The articles that comprise this critical review serve to draw attention to research papers published in specific fields of interest during 2003, provide critical comment on the relevance and importance of individual publications in these fields, and offer an overview of the comparative importance of advances in particular areas. In this way, these articles aim to assist experts in the field by keeping them informed of relevant recent publications, as well as providing an important resource for students or early career researchers who are embarking on studies in an area new to them. This year, five papers provide summaries of developments in bulk sample determinations employing (1) ICP-AES and ICP-MS (trace elements), (2) XRF and atomic absorption spectrometry and INAA, (3) isotope ratio measurements (TIMS, MC-ICP-MS, ICP-MS, ToF), as well as in situ measurements conducted using (4) secondary ion mass spectrometry and (5) laser ablation ICP-MS (trace element and isotope ratio determinations).  相似文献   

10.
With increasing use of bismuth in industry, a better understanding of its environmental behaviour is required, including an improved knowledge of its background concentration range in (non‐saline) freshwaters. However, the poor analytical sensitivity of previous methods may lead to inaccurate measurement results for Bi3+ in environmental samples. In this work, cobalt ion‐assisted photochemical vapour generation (PVG) was developed for the detection of trace Bi with inductively coupled plasma‐mass spectrometry (ICP‐MS) measurement. The volatile species of Bi was found to be (CH3)3Bi generated under UV irradiation in the presence of formic acid, acetic acid and Co2+. The major parameters potentially influencing the detection of Bi were investigated. Under optimised conditions, the limit of detection (3s, n = 11) of the proposed method was 0.3 ng l?1. The analytical sensitivity was enhanced about 70‐fold for Bi3+ compared with that using classic pneumatic nebulisation of ICP‐MS. Furthermore, the proposed method showed better analytical sensitivity and anti‐interference ability towards co‐existing ions compared with ferric ion‐assisted PVG systems. The accuracy of the proposed method was evaluated by analysis of environmental water samples and certified reference materials with satisfactory results.  相似文献   

11.
样品经硝酸-氢氟酸混合酸溶解后,用标准加入-原子吸收光谱法测定钢渣中的铁。实验探讨了钢渣的均匀性等干扰因素对结果的影响,并提出基体高、浓度高的样品稀释倍数过高误差越大,建议采用如旋转燃烧头、选择次灵敏线等降低仪器灵敏度的方法或采用标准加入法。并将标准加入法与X射线荧光光谱、电感耦合等离子体发射光谱、原子吸收光谱直接测定法进行比较,铁的实验结果分别为51.6%、54.2%、46.2%、16.6%,相对标准偏差分别为2.8%、5.3%、2.0%、2.3%。标准加入-原子吸收光谱法用于测定基体高、浓度高的样品是准确可靠的。方法可用于环境类实验室用水剂标准溶液进行钢渣类样品中元素的分析。  相似文献   

12.
This paper suggests a new method for obtaining steady‐state solutions for ‘full‐flow’ penetrometers. The method is based on the numerical solution of the small strain plastic‐flow problem (i.e. rigid plastic material) with an inhomogeneous strength field, which is determined by converting changes of material properties over time in a stationary frame of reference into spatial distribution of strength in a moving frame of reference. Rather than building streamlines from back integration of soil element distortion, as previous methods have suggested, the method treats the domain as continuous with the associated field equations. The method employs an upstream weighting technique for the determination of information flow within the domain. The execution order for the calculation is based on topological ordering. This results in the calculation having a complexity of O(N), as compared with O(N1.5) for the strain path or streamline methods (N is the number of discretized points), which significantly reduces the calculation time. The formulation is presented for the cylindrical (T‐bar) penetrometer, and includes aspects of soil strength degradation, strain rate effects, strength anisotropy, and interface strength law. Comparison to previously published values, based on large displacement finite element simulations with remeshing, showed good agreement, indicating on the correctness of the suggested approach. Investigation into the soil rigid‐body rotation and the remolding effect on anisotropy characteristics showed an interesting behavior, where the decrease of strength anisotropy due to remolding has a greater influence when the soil strength is higher in the vertical direction. Copyright © 2009 John Wiley & Sons, Ltd.  相似文献   

13.
标准加入-原子吸收光谱法测定钢渣中的铁   总被引：1，自引：1，他引：0  
刘琳娟  张琪  陆培培 《岩矿测试》2010,29(6):699-702
样品经硝酸-氢氟酸混合酸溶解后,用标准加入-原子吸收光谱法测定钢渣中的铁.实验探讨了钢渣的均匀性等干扰因素对结果的影响,并提出基体高、浓度高的样品稀释倍数过高误差越大,建议采用如旋转燃烧头、选择次灵敏线等降低仪器灵敏度的方法或采用标准加入法.并将标准加入法与X射线荧光光谱、电感耦合等离子体发射光谱、原子吸收光谱直接测定法进行比较,铁的实验结果分别为51.6%、54.2%、46.2%、16.6%,相对标准偏差分别为2.8%、5.3%、2.0%、2.3%.标准加入-原子吸收光谱法用于测定基体高、浓度高的样品是准确可靠的.方法可用于环境类实验室用水剂标准溶液进行钢渣类样品中元素的分析.  相似文献   

14.
X‐ray fluorescence (XRF) core scanning has become widely available for geological studies during the last decade. The data obtained from XRF core scanning, however, may be strongly influenced by the amount of organic matter, water content, density and porosity of the sediment matrix. In this study we discuss the usefulness of XRF core scanning to distinguish different kinds of organic‐rich sediments and peat based on examples from tropical Lakes Kumphawapi and Nong Leng Sai in Thailand. We examined how sedimentary factors influence XRF core scanning analyses by comparing elemental and scattering ratios to lithological changes and quantitative LOI, TOC, biogenic silica (BSi) and grain‐size values. Our comparison suggests that the (inc/coh) scattering ratio is of limited use as an indicator for variations in LOI and TOC in peaty gyttja or peat. In Lake Kumphawapi's sediments, Si/Ti ratios reflect clastic input associated with grain‐size variations rather than BSi contents. The Ti‐normalized ratios of Si, Zr, Sr, K and Rb are linked to mineral input and associated grain‐size variations. We conclude that XRF core scanning of organic‐rich tropical lake sediments and peat is useful to infer palaeoenvironmental conditions. However, XRF core scanning data does not stand‐alone and needs to be underpinned by additional proxies.  相似文献   

15.
目前土壤中Se主要采用原子荧光光谱法测定,存在用酸量大、前处理相对复杂等缺点,对于高含量Se的测定则需要高倍稀释,无疑会扩大分析误差.本文采用粉末压片波谱-能谱复合X射线荧光光谱法测定湖北富硒土壤样品中的Se等17个主次量元素,波谱分析10个元素的同时,能谱分析As、Cu、Rb、Sr、Zr、Ba、Ni等7个元素,大幅节...  相似文献   

16.
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17.
Concentration data obtained by instrumental neutron activation analysis (INAA) are presented for up to 36 chemical elements in 93 geochemical reference samples, including some for which there are little previous data. Because all data are based on at least three independent analyses, and for many of the data the uncertainty associated with counting is an insignificant source of error, the values presented here are considered of higher precision than generally reported by INAA. Information on subsampling error (sample heterogeneity) is also presented.  相似文献   

18.
镓的原子吸收光谱分析进展   总被引：2，自引：1，他引：2  
米瑞华 《岩矿测试》1996,15(1):53-57
文章对近年来用原子吸收光谱法测定镓进行了总结评述。重点介绍了用电热原子吸收法测Ｇａ时，基体改进剂、进样方式以及预富集技术对提高方法灵敏度的作用。引用主要文献３８篇。  相似文献   

19.
We evaluate the potential of a hand‐held energy dispersive XRF spectrometer for the preliminary classification of non‐chondritic differentiated meteorites. The studied achondrites include nine lunar meteorites, seventeen Martian meteorites, five angrites and eighteen meteorites from asteroid 4 Vesta. Analytical precision and accuracy was tested on thirty‐nine terrestrial igneous rock slabs with a wide range of composition. Replicate analyses, performed on the studied meteorites, show that Fe/Mn values together with Si and Ca/K ratio can be used in the discrimination of different achondrite groups. Fusion crust's Fe/Mn values of meteorites from Vesta and Mars are indistinguishable from those of the interior implying that even measurements on the fusion‐crusted external surface could be sufficient to pigeonhole non‐chondritic meteorites. Hand‐held energy dispersive XRF spectrometer is a non‐destructive but very effective technique for preliminary classification of achondrites in the field and in laboratory and for the identification of mislabelled meteorites in museum collections.  相似文献   

20.
The purpose of this study is to investigate the enrichment level and dispersion patterns of Se and associated elements in rocks, soils and crops which were collected in the Dukpyung and the Chubu areas covered with black shales of the Okchon Group in Korea. Rock and soil samples were analyzed for Se including multiple elements by ICP, ICP-MS and INAA, and crop samples by INAA. Soil pH and loss-on-ignition (LOI) were also measured.  相似文献   

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