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在某些实验中,由于样品来源的有限性,导致样品数量有限,因而有必要探讨少量样品中主次元素的测定方法。X射线荧光光谱法具有样品制备简单、分析速度快、重现性好、测量范围宽和多元素同时进行分析的特点,目前在众多领域中得到了广泛的应用。基于回归曲线法、经验系数法和康普顿散射线内标法求取了各待测元素的工作曲线常数、元素间效应的影响系数和谱重叠系数,并对4 g(32 mm内径,常规)和1 g(10 mm内径,少量)样品测量的精密度和准确度进行了比较分析。结果表明,4 g(32 mm内径,常规)样品测量平均精密度约为1%,1 g(10 mm内径,少量)样品的平均精密度约为3%。测定结果基本能够满足覆盖区多目标地球化学调查样品的质量要求。 相似文献
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对X射线衍射仪的工作原理、物相定性、定量分析方法进行了扼要介绍,同时详细论述了X射线衍射仪在盐湖地质(盐类矿物、盐湖粘土矿物、盐湖沉积矿物与古气候古环境关系)、盐湖化工(镁水泥、锂离子电池和晶须材料)和水盐体系相图研究中的应用。 相似文献
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拉果错盐湖位于西藏自治区阿里地区改则县麻米乡境内,盐湖水化学类型为硫酸钠亚型,氯化锂资源储量232×104t,是西藏重要锂盐湖之一。前人对拉果错盐湖的研究集中在锂元素来源、成矿规律,不同温度下盐类矿物析出序列等,对盐湖中含硼盐类矿物并未开展相关研究。对拉果错盐田中采集的5件样品进行X射线衍射实验和扫描电镜分析,发现盐田中盐类矿物组合为三方硼砂、石盐、钾石盐、钾芒硝、无水芒硝、硫酸锂钾。三方硼砂呈他形—半自形的短柱状集合体,长约36 μm,宽约30 μm,含量在5.94%~84.51%,为硼砂脱水的次生成因,属硫酸盐型盐湖中首次发现。 相似文献
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拉果错盐湖位于西藏阿里地区改则县麻米乡境内,盐湖水体类型为硫酸钠亚型地表卤水,氯化锂资源储量232万吨,是西藏重要锂盐湖之一。前人对拉果错盐湖的研究集中在锂元素来源、成矿规律,不同温度下盐类矿物析出序列等,对盐湖中含硼盐类矿物并未相关研究。本次工作对拉果错盐田中采集的5件样品进行X射线衍射实验和扫描电镜分析,发现盐田中盐类矿物组合为三方硼砂、石盐、钾石盐、钾芒硝、无水芒硝、硫酸锂钾。三方硼砂呈他形-半自形的短柱状集合体,长约36μm,宽约30μm,含量在5.94%-84.51%。三方硼砂为首次在硫酸盐型盐湖卤水盐类结晶矿物中被发现,由先析出的硼砂脱水形成,属次生三方硼砂。 相似文献
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扎布耶盐湖是全球最独特的自然结晶扎布耶石(Li2CO3)的盐湖。该盐湖正在开发利用中,2020年产富锂混盐4500吨。实验所采取的样品是通过“盐梯度太阳池”技术结晶出来的10件富锂混盐。通过对采集的样品进行X射线衍射、扫描电镜、电感耦合等离子质谱法、离子色谱法和滴定法的测试,得到了矿物组成的成分和化学元素组成含量数据,扎布耶盐湖太阳池富锂混盐中的物相组成有扎布耶石、钾石盐、石盐、氯碳钠镁石、天然碱、钾芒硝、菱锰矿、石英这8种,其中菱锰矿是首次从富锂混盐中发现的矿物,扎布耶石的含量为24.10%-88.27%,平均为62.89%,是该盐湖中含量最高的矿物。测试的样品中Li含量4.56%-16.70%,平均为11.90%;K+含量为0.14%-10.17%,平均为2.42%; KCl的含量为0.26%-20.44%,平均为4.63%(工业品位1%)。该混盐的结构和构造的形成受温度和水流的影响,温度越高碳酸锂的结晶速率越快,碳酸锂的晶核生长速率和晶粒大小与温度呈正相关。扎布耶盐湖二期工程预计年产20000吨碳酸锂,其中利用膜法生产12000吨;利用太阳池技术生产8000吨,预计年产出12700吨的富锂混盐,可以产出约600吨氯化钾,建议进行综合利用。 相似文献
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采集了15种荒漠地区常见植物的样品,基于X射线荧光光谱法对其元素含量进行了测定。结果表明:组成荒漠地区植物的常量元素主要有Cl、S、P、Ca、Si、Al、K、Na和Mg,微量元素主要有Sr、Rb、Br、Zn、Cu、Ni、V、Ti、Ba、Mn 和Fe。不同种类植物中各元素的含量不同,体现了植物因遗传生理特性的不同而对环境元素选择吸收的特点。15种荒漠植物的常量元素组成的典型特征是富Ca、K贫Na,表明生境对各类植物化学成分含量的统一影响。属于同科的植物化学元素组成比较接近,说明植物元素化学成分可作为植物分类的标志之一。 相似文献
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为了研究南极的植物与环境间的关系 ,探讨植物在南极环境监测中的作用 ,在无标样条件下 ,利用微束 X荧光分析法对南极菲尔德斯半岛的 6种藻类和地衣植物进行了元素分析。其中藻类植物有孔石莼 (Ulva pertusa)、海膜 (H alymenia sp.)和大型鞘丝藻 (Lyngbya major) ,地衣植物有筛石蕊 (Cladonia borealis)、喇叭石蕊 (C.fimbriata)和松萝 (Usnea sp.)。研究结果发现 ,不同的藻类植物对各种元素的吸收能力不同 ,在 XRF(X射线荧光 )谱中 ,孔石莼比海膜含有更多的元素 ,象 As、Br和 Rb,Cu和 Zn的含量也较高。在大型鞘丝藻中 ,K比 Ca少 ,Zn的含量较高。在 3种地衣植物中 ,其 XRF谱中的元素种类组成非常相似 ,只是 Mn、Fe、Cu和 Zn等元素的相对含量有些差异 相似文献
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对塞曼效应石墨炉原子吸收法对地质样中痕量银的测定进行了研究。简化了样品处理过程。对地质标样及实际样品分析获得了满意的结果加标回收率为96.2%-103.5%,相对标准偏差为3.04%-4.77%所采用的方法快速、简便,准确。 相似文献
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Johan Rydberg 《Journal of Paleolimnology》2014,52(3):265-276
X-ray fluorescence spectroscopy (XRF) has been used extensively to analyze many types of environmental samples, including lake sediments. In most cases, however, analyses have required either a relatively large sample mass or sample pretreatment, e.g. lithium borate fusion, and have not taken advantage of the potential of XRF analysis as a non-destructive technique. This paper describes the development of two completely non-destructive calibration methods that use small, i.e. 200- and 500-mg loose-powder sediment samples. Analytical performance of these methods was assessed using ten different certified reference materials and a previously analyzed sediment profile, and for both methods, accuracy and precision were less than ±10 % (or a few ppm) for 26 elements (Na, Mg, Al, Si, K, Ca, Sc, Ti, V, Mn, Fe, Ni, Cu, Zn, Ga, As, Br, Rb, Sr, Y, Zr, Sn, Sb, Ba, W and Pb). This shows that quantitative wavelength dispersive X-ray fluorescence analysis, using small loose-powder samples, can be a useful geochemical tool for many paleolimnological applications, especially because lack of pretreatment ensures that samples can be used for further analysis. 相似文献
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A modified method for biogenic silica determination 总被引:1,自引:0,他引:1
We describe a modified method for the determination of biogenic silica (BSi) in lacustrine sediment samples with BSi concentrations
>0.5% SiO2 (detection limit). To speed up the leaching procedure (48 samples per day), we suggest the use of Teflon autoclaves that
can be left unattended (no stirring of the solution) for 3 h at 100°C in an oven. We suggest a volume correction by Na measurement
to account for volume errors during pipetting off a hot solution. We also propose to carry out a correction for minerogenic
silica by the simultaneous determination of Al in the leachate. Analytical precision and accuracy of the proposed method are
2.4% (relative standard deviation) and 70–110% recovery (relative to the mean of four international reference sediment samples),
respectively. Additionally, we demonstrate that pre-treatment of the samples with H2O2 and/or HCl prior to alkaline leaching is not necessary for all samples. Due to the great diversity of lacustrine and marine
sediments, however, the pre-treatment procedure should be tailored for samples from different sites. 相似文献
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John F. Boyle 《Journal of Paleolimnology》2000,23(2):213-221
Energy dispersive isotope-source X-ray fluorescence (XRF) analysers are little used in academic environmental research, in spite of being ideally suited to a number of tasks. In this paper an XRF method is tested by measuring a wide range of environmental materials of known elemental composition. Precision, accuracy and detection limits are presented.Using isotope-source X-ray fluorescence analysis, the total concentrations of Si, Ti, Ca, K, Fe, Mn, Cl, S, Nb, Ni, Pb, Rb, Sr, Zn and Zr can be determined in soils and sediments at a rate of >70 samples per day. The combination of speed and accuracy makes the technique ideal for three classes of application within environmental research. First, in sediments and soils that are highly heterogeneous, reliable characterisation is more dependent upon the number of samples measured than on measurement precision or accuracy. Under these circumstances the method is sufficiently accurate to be used alone. This is also the case where there is high and wide ranging contamination of sediment or soil by Pb and Zn. Second, major elements (Si, Ti, Fe, Ca, K and S) can be measured with sufficient accuracy in sediments and soils to aid the interpretation of other sediment chemical analyses. Third, the technique is ideal for the rapid screening of sediment or soil, allowing effective targeting of samples for more time consuming or expensive analyses. The XRF method presented here offers rapid, non-destructive total elemental analysis of sediments and soils that is sufficiently accurate to be useful in environmental research. 相似文献
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Braden R. B. Gregory Eduard G. Reinhardt Andrew L. Macumber Nawaf A. Nasser R. Timothy Patterson Shawn E. Kovacs Jennifer M. Galloway 《Journal of Paleolimnology》2017,57(3):287-293
Geochemical analysis of sediment samples can be used to characterize between- and within-lake variability and provide insights into lake chemistry, depositional processes and contamination sources. The number of samples for geochemical studies is restricted by cost, sample volume required, and the destructive nature of inductively coupled plasma mass spectrometry, instrumental neutron activation analysis, or wavelength dispersive x-ray fluorescence. Core scanners that incorporate energy dispersive x-ray fluorescence spectrometry, such as the Cox Itrax-XRF core scanner, have high through-put and can be used to produce high-quality geochemical datasets at low cost without destroying sample material. Here we describe a new analysis vessel that enables rapid, non-destructive Itrax-XRF analysis of discrete sediment samples. 相似文献
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INVESTIGATING MORPHOLOGICAL CHARACTERISTICS AND CHEMICAL COMPOSITION OF NAFTLIGE MUD VOLCANO IN GOLESTAN PROVINCE,EASTERN PART OF THE CASPIAN SEA
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SAMAD FOTOOHI HOSSEIN NEGARESH 《Geografiska Annaler: Series A, Physical Geography》2016,98(3):207-219
Mud volcanoes are geomorphological phenomena and there is a limited volume of knowledge about them. Output of a composition of water, mud, and gas forms the mud volcano phenomenon. Geographical distribution of mud volcanoes indicates their relationship with pressured, rapid and thick sedimentation, which is seen in both tectonically active and inactive zones. Naftlige mud volcano is located in the southwest of the Caspian Sea and west of Gomishan Wetland in Golestan Province, Iran. Since no study has ever been conducted with a specific focus on mud volcanoes, field and laboratory studies were carried out for the first time to overcome the shortage of library resources. The objective was to determine the composition of emerging mud and study its morphometric and geomorphic features so that there would be a method for identifying and introducing some unknown aspects of this mud volcano. Therefore, three samples of this mud volcano which were taken on 27 Apr., 2012 were tested and analyzed using X‐ray diffraction and X‐ray fluorescence techniques to determine the mineral and chemical composition. The results of this analysis showed that, in these three samples, silicon oxide with the chemical formula SiO2 had 40.88% volatile materials, 19.15% H2O Loss on Ignition (LOI) and 13.97% calcium oxide. Quartz, calcite and albite formed the three main phases of minerals. 相似文献
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Estimation of grain size variability with micro X-ray fluorescence in laminated lacustrine sediments,Cape Bounty,Canadian High Arctic 总被引:4,自引:0,他引:4
Finely laminated sediment cores from two Arctic lakes were investigated using the Itrax™ Core Scanner that provides micro
X-ray fluorescence (μ-XRF) measurements with a spatial resolution of 100 μm. We compared these chemical measurements with
standard geochemical methods using, at the macroscopic scale, inductively coupled plasma–atomic emission spectrometry (ICP-AES)
and, at the microscopic scale, energy dispersive spectroscopy (EDS). We also investigated the relationship between the chemical
profiles and the grain size of sediments at macro-scale using laser particle-size analysis, and at microscopic scale, using
thin section image analysis techniques. Results show a link between grain size and the relative abundance of several elements.
Silicon and zirconium are associated with very coarse silt and sand deposits, K and Fe with clay-rich layers, and Ti with
silty facies. Four sedimentary facies are characterised based on sedimentary structure and texture, and interpreted in terms
of known seasonal hydroclimatic processes. We show that is possible to identify these sedimentary facies using μ-XRF element
abundance or ratio variations. The K/Ti ratio is the best marker of the upper varve boundary, and it might be used for varve
identification and counting of Cape Bounty sediments in future. More generally, this study demonstrates new applications for
paleohydrological reconstructions from laminated sediments. 相似文献
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Preliminary investigation of mercury in bone tissues of skua and penguin in Antarctica using AFS and Synchrotron Radiation X-ray Fluorescence(SR-XRF)
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<正> Mercury(Hg)was investigated in bone tissues of skua(Catharacta mac-cormick)and penguin(Pygoscelis adeliae)collected in the maritime Antarctic usingatomic fluorescence spectrometry(AFS)and synchrotron radiation X-ray fluorescence(SR-XRF)method.The total levels of mercury in bone tissues of penguin and skuaare much lower than those in other organs(e.g.,kidney,liver).The toxic effects ofmercury in bone tissues of seabirds in polar region are not known.We have used SR-XRF method to map the distribution of trace levels of mercury in bones.The levels ofmercury are found to be enriched somewhere near the periosteal surface and/or endos-teal surface.The distribution of mercury shows strongly correlation with that of someessential elements and probably poses negative effect on the bone metabolism inferringfrom the relationship of mercury with the other elements.These studies represent afirst step toward understanding the toxic effects of mercury on bone of polar animals bysuggesting the possible microscopic investigation. 相似文献
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Xiuju Liu Steven M. Colman Erik T. Brown Elizabeth C. Minor Hongyu Li 《Journal of Paleolimnology》2013,50(3):387-398
Major components of lacustrine sediments, such as carbonates, organic matter, and biogenic silica, provide significant paleoenvironmental information about lake systems. Fourier transform infrared spectroscopy (FTIR) and scanning X-ray fluorescence (XRF) techniques are fast, cost effective, efficient methods to determine the relative abundances of these components. We investigate the potential of these techniques using sediments from two large lakes, Lake Malawi in Africa and Lake Qinghai in China. Our results show statistically significant correlations of conventionally measured concentrations of carbonate (%CaCO3), total organic carbon (%TOC), and biogenic silica (%BSi), with absorbance in the corresponding FTIR spectral regions and with XRF elemental ratios including calcium:titanium (Ca/Ti), incoherent:coherent X-ray scatter intensities (Inc/Coh), and silicon:titanium (Si/Ti), respectively. The correlation coefficients (R) range from 0.66 to 0.96 for comparisons of FTIR results and conventional measurements, and from 0.70 to 0.90 for XRF results and conventional measurements. Both FTIR and XRF techniques exhibit great potential for rapid assessment of inorganic and organic contents of lacustrine sediments. However, the relationship between XRF-ratios or FTIR-absorbances and abundances of corresponding sedimentary components can vary with sediment source and lithology. 相似文献