Energy-dispersive X-ray Spectroscopy for the Quantitative Analysis of Pyrite Thin Specimens

To explore ways to improve the accuracy of quantitative analysis of samples in the micrometer to nanometer range of magnitudes,we adopted analytical transmission electron microscopy(AEM/EDS)for qualitative and quantitative analysis of pyrite materials.Additionally,the k factor of pyrite is calculated experimentally.To develop an appropriate non-standard quantitative analysis model for pyrite materials,the experimentally calculated k factor is compared with that estimated from the non-standard quantitative analytical model of the instrument software.The experimental findings demonstrate that the EDS attached to a TEM can be employed for precise quantitative analysis of micro-and nanoscale regions of pyrite materials.Furthermore,it serves as a reference for improving the results of the EDS quantitative analysis of other sulfides.

Quantitative energy-dispersive X-ray fluorescence analysis for unknown samples using full-spectrum least-squares regression

The full-spectrum least-squares(FSLS) method is introduced to perform quantitative energy-dispersive X-ray fluorescence analysis for unknown solid samples.Based on the conventional least-squares principle, this spectrum evaluation method is able to obtain the background-corrected and interference-free net peaks, which is significant for quantization analyses. A variety of analytical parameters and functions to describe the features of the fluorescence spectra of pure elements are used and established, such as the mass absorption coefficient, the Gi factor, and fundamental fluorescence formulas. The FSLS iterative program was compiled in the C language. The content of each component should reach the convergence criterion at the end of the calculations. After a basic theory analysis and experimental preparation, 13 national standard soil samples were detected using a spectrometer to test the feasibility of using the algorithm. The results show that the calculated contents of Ti, Fe, Ni, Cu, and Zn have the same changing tendency as the corresponding standard content in the 13 reference samples. Accuracies of 0.35% and 14.03% are obtained, respectively, for Fe and Ti, whose standard concentrations are 8.82% and 0.578%, respectively. However, the calculated results of trace elements (only tens of lg/g) deviate from the standard values. This may be because of measurement accuracy and mutual effects between the elements.

Determination of Element Levels of Lagoon from Townships near Cocody City Abidjan Côte D’Ivoire Using Energy Dispersive X-Ray Fluorescence

Eight water bottles from Ebrie lagoon with pollution potency were studied using nuclear chemistry technique and Energy dispersive X-ray fluorescence. This pollution is characterized by pH and conductivity parameters, concentrations average in mg/L of metals such Fe (0.731), Mn (0.345), Cr (0.070), Cu (0.014) and concentrations of nutrients known to be pollutants and toxic for living or-ganisms. These heavy metals are dangerous to the lives, the local inhabitants and also a threat to aquatic life since this water is essential for the economical town, Abidjan. According to the Manganese concentration average (0.345 mg) values that higher than WHO (0.05 mg) value, the main likely source of pollu-tants is anthropogenic, industrial and agricultural. This study also shows the use of materials and lubricants near the lagoon that pollute this water.

Alpha-actinin expression at different differentiating time points from temporal lobe cerebral cortex neural stem cells to neuron-like cells using energy dispersive X-ray analysis

BACKGROUND： Alpha-actinin （ a -actinin） plays a key role in neuronal growth cone migration during directional differentiation from neural stem cells （NSCs） to neurons. OBJECTIVE： To detect in situ microdistribution and quantitative expression of a -actinin during directional differentiation of NSCs to neurons in the temporal lobe cerebral cortex of neonatal rats. DESIGN, TIME AND SETTING： Between January 2006 and December 2008, culture and directional differentiation of NSCs were performed at Department of Histology and Embryology, Preclinical Medical College, China Medical University. Immune electron microscopy was performed at Department of Histology and Embryology and Department of Electron Micrology, Preclinical Medical College, China Medical University. Spectrum analysis was performed at Laboratory of Electron Microscopy, Mental Research Institute, Chinese Academy of Sciences. MATERIALS： Basic fibroblast growth factor, epidermal growth factor, brain-derived nerve growth factor, type-1 insulin like growth factor, and a -actinin antibody were provided by Gibco BRL, USA; rabbit-anti-rat nestin monoclonal antibody, rabbit-anti-rat neuron specific enolase polyclonal antibody, and EDAX-9100 energy dispersive X-ray analysis were provided by PHILIPS Company, Netherlands. METHODS： NSCs, following primary and passage culture, were differentiated with serum culture medium （DMEM/F12 ＋ 10% fetal bovine serum ＋ 2 ng/mL brain-derived nerve growth factor ＋ 2 ng/mL type-1 insulin like growth factor）. MAIN OUTCOME MEASURES： Expression of a -actinin in neuron-like cells was quantitatively and qualitatively detected with immunocytochemistry using energy dispersive X-ray analysis. RESULTS： Immunocytochemistry, combined with electron microscopy, indicated that positive α -actinin expression was like a spheroid particle with high electron density. In addition, the expression was gradually concentrated from the nuclear edge to the cytoplasm and expanded into developing neurites, during differentiation of neural stem cells to neurons. Conversely, energy dispersive X-ray analysis indicated that the more mature the neural differentiation was, and the greater the expression of α -actinin. CONCLUSION： The gradual increase of α -actinin expression is related to growth, development, and maturity of differentiated neuron-like cells, in neonatal rat frontal lobe cortex, at different differentiating time points of NSCs to neurons.

A Hybrid Angular/Energy Dispersive Method to Improve Some Characteristics of Laboratory X-Ray Diffraction

The Energy Dispersive X-ray Diffraction, generally referred as EDXD, has shown to be a valid alternative to the conventional Angular Dispersive X-ray Diffraction, the ADXD. EDXD exhibits several advantages to its AD counterpart, mainly related to the properties of the polychromatic X-ray beam utilized for diffracting, such as higher signal intensities, a wider accessible region of the reciprocal space, a greater transparency of samples, and a parallel data collection of the q-points in the diffraction pattern acquisition. However, the main drawback of poly-chromaticity lays in the fact that the quantities that modulate the scattered intensity in a diffraction measurement depend on the energy. These quantities are the primary X-ray beam spectrum, polarization, and X-ray absorption, the last producing by far the most critical effect because it rapidly changes as a function of energy. Therefore, a detailed knowledge of the energy dependence of all these quantities is required in EDXD in order to process the data correctly and prevent systematic errors. The difficulty in handling the energy-dependent factors complicates the experimental procedure and may make the measurements unreliable. In the present paper, a hybrid method between the ED and AD X-ray Diffraction is proposed to maintain the advantages of the polychromatic nature of the radiation utilized in EDXD, while preventing the problems produced by the energy-dependent quantities.

Energy Dispersive X-Ray Spectroscopy of the Sohnari Member of Laki Formation from Southern Indus Basin of Pakistan

This study determines the geochemical and depositional environment analysis of the sediments of the Sohnari Member of the Laki Formation, Northern Kirthar Fold Belt of Pakistan. The Energy-Dispersive-X-Ray Spectroscopy (EDS) technique is used for the detection of major elements and the effects of shifting depositional climatic conditions of six representative samples which were acquired from the Sohnari Member of the Laki Formation at Lakhra area, Sindh, Pakistan. The sedimentological studies clarify that the sediments the Sonahri Member are relatively immature and most migrated in clastic mode. The availability of Silica shows that the Member was formed due to biochemical precipitation and detrital mode and was deposited at a fast rate of sediment deposition under the fluvio-deltaic depositional system. This is also deduced that the rapid rate of sediment deposition might be created a reducing atmosphere and allowing for the mineralization of sulphur.

Research of CdZnTe detector based portable energy dispersive spectrometer

A kind of excellent CdZnTe crystal has been grown in Yinnel Tech, Inc. in recent years. Based on these CdZnTe crystals and some new techniques, a portable energy-dispersive spectrometer has been constructed which has yielded good results. CdZnTe detector has a 3% relative resolution in high-energy field and can detect gamma rays at room temperature. An integrated circuit based on preamplifier and shaping amplifier chips is connected to the detector. Voltage pulses are transformed into digital signals in MCA (multichannel analyzer) and are then transmitted to com- puter via USB bus. Data process algorithms are improved in this spectrometer. Fast Fourier transform (FFT) and nu- merical differentiation (ND) are used in energy peak’s searching program. Sampling-based correction technique is used in X-ray energy calibration. Modified Gaussian-Newton algorithm is a classical method to solve nonlinear curve fitting problems, and it is used to compute absolute intensity of each detected characteristic line.

Monte Carlo simulation for bremsstrahlung and photoneutron yields in high-energy x-ray radiography

This paper reports on the results of calculations using a Monte Carlo code （MCNP5） to study the properties of photons, electrons and photoneutrons obtained in the converted target and their transportations in x-ray radiography. A comparison between measurements and calculations for bremsstrahlung and photoneutrons is presented. The radiographic rule and the effect of the collimator on the image are studied with the experimental model. The results provide exact parameters for the optimal design of radiographic layout and shielding systems.

一款紧凑型磁谱仪的特性参数分析与实验刻度研究

超短脉冲激光与靶相互作用可产生高能电子以及质子、离子、X/γ射线等次级粒子和射线,这些粒子和射线在惯性约束聚变、激光核物理、实验室天体物理、生物、医学以及材料科学等领域具有广泛的应用前景。高能电子的特征参数测量对理清激光等离子体相互作用过程、优化粒子参数和拓展其应用具有重要意义。本文研究设计了一款紧凑型矩形结构磁谱仪,在永磁铁均匀场中采用前、侧、后三面IP板布局,满足了几十keV到10 MeV的电子能谱测量需求,并对磁谱仪的特征参数如能量色散、能量色散梯度、能量分辨率、斜入射效应等进行详细分析。基于北京大学DC-SRF-Ⅱ射频超导光阴极电子枪开展了磁谱仪能量刻度实验,在真空条件下实验测量了0.7~1.8 MeV区间内多个能量的电子能谱,结果显示,磁谱仪的能量测量与监测系统结果基本符合。电子能谱的能量分辨率主要决定于磁谱仪自身分辨能力,为提高能量分辨率,需通过准直系统进一步减小入射孔径和电子发散角。

Establishment of Energy Dispersive X-ray Diffraction Experimental System With Synchrotron Radiation Under High Pressure

Because the interactions between molecules and atoms in mediums can be dramatically changed by compression, high pressure studies on materials can provide much information on fundamental properties including phase transition and

Quantum interference in laser-assisted photo-ionization excited by a femtosecond x-ray pulse

The photoelectron energy spectra （PESs） excited by monochromatic femtosecond x-ray pulses in the presence of a femtosecond laser are investigated. APES is composed of a set of separate peaks, showing interesting comb-like structures. These structures result from the quantum interferences between photoelectron wave packets generated at different times. The width and the localization of each peak as well as the number of peaks are determined by all the laser and x-ray parameters. Most of peak heights of the PES are higher than the classical predictions.

Wood Moisture Content Measurement by X-Ray Exposure Method

Although quite a numer of papers can be found up to now dealing with the subject of the measurement ofwood density by using the X-ray exposure methods, direet scanning or radiographic photography, the following two aspects,which are very important from both theorctical and engineering application points of view, have not yet been properly handled. One is that the elementary analyses or the experimental measurement on the mass attenuation coefficients were notspecified in regard to spectnun energv distridutions [1]. In this connection, the ambiguities in the specification of the coeffiecients and in turn for thc results among studies arise when only one of the two parameters, namely wave length and applied voltage, of detining the energy spectrum of X-ray is given. The oher is that the relationships between the relative intensity and the sample thickness as well the wood moisture content [2], which are the critical factors for the design and theselection of X-ray apparatus, were not sufficiently examined. In addition, the knowledge of the measurelnent of woodmiosture content by using the direct X-ray scanning method is also almost unavaible now. In the study, the direct X-rayscanning method of measuring wood moisture content was at first investigated theoretically with respect to the relationshipbetween the mass attenuation coefficients of wood (beech, Fagus Sylvatica) and the maximum spectrum energy of X-ray.Secondly, the dependence of the relative intensity on the sample thickness and on the wood moisture content was analysed.The main advantage of the method is on-site nondestructive measuring of wood moisture content in the processes such asdrying, impregnation and unsteady mass diffusion. Specifically for the application in the area of biomechanics, the methodcan also bc used for understanding the water pathway within wood, for example, the water around the knots and the relation between the stress distribution and the local moisture content of wood.

X-Ray and Mössbauer Study of Magnetic Black Sand from Mayotte Island

Natural magnetic black sands are known from several sites often located in areas of volcanic origin. Their elemental and mineral composition provides information on the geology of their territory and depends on several factors occurred during their formation. A sample of black sand was collected on the seashore of the island of Mayotte in the Indian Ocean and its magnetic part was investigated by means of energy dispersive X-ray spectroscopy (EDS), powder X-ray diffraction (XRD), and MÖssbauer spectroscopy at room temperature. The mineral composition is dominantly magnetite, in good agreement with samples collected in other sites of volcanic origin. Contrary to pure magnetite, a relevant fraction of Ti was detected by EDS. The 16% Ti and 1% Mn content increase the magnetite lattice parameter to 8.4312 (25) Å. The broadening of XRD lines pointed towards a significant degree of disorder. This was confirmed by MÖssbauer spectroscopy and is attributed to the presence of Ti replacing Fe in the magnetite lattice. The presence of Ti modifies the local magnetic field on the Fe sites, leading to a broader and more complex MÖssbauer transmission spectrum with respect to the one of pure magnetite. To study the effect of temperature, samples were heated for 12 hours to 600°C and 800°C in argon and to 1000°C in air. Annealing in argon did not improve the crystallinity while annealing in air caused a complete decomposition of magnetite into hematite and pseudobrookite.

Mossbauer,X-Ray and Magnetic Studies of Black Sand from the Italian Mediterranean Sea

The study of natural magnetic sands is instrumental to investigate the geological aspects of their formation and of the origin of their territory. In particular, Mossbauer spectroscopy provides unique information on their iron content and on the oxidation state of iron in their mineral composition. The Italian coast on the Mediterranean Sea near Rome is known for the presence of highly magnetic black sands of volcanic origin. A study of the room temperature Mossbauer spectrum, powder X-ray diffraction, energy dispersive X-ray spectroscopy, and magnetic measurements of a sample of black magnetic sand collected on the seashore of the town of Ladispoli is performed. This study reveals magnetite as main constituent with iron in both tetrahedral and octahedral sites. Minor constituents are the iron minerals hematite and ilmenite, the iron containing minerals diopsite, gossular, and allanite, as well as ubiquitous sanidine, quartz, and calcite.

具有梯度静应力的红砂岩应力波衰减特性试验研究

地下工程围岩体承受梯度应力,导致围岩体在梯度空间上的孔隙度不同,影响应力波在其传播的衰减特性。为研究梯度应力对岩石应力波传播衰减特性的影响,利用改进的SHPB试验装置,对红砂岩试件进行不同静应力梯度工况下的应力波传播试验。将采集得到的波形时域数据分别进行傅里叶变换和小波包分解重构。分析应力波质心频率和频带能量分布与静应力梯度的关系,构建频域特征参数的演化经验模型,表征梯度静应力下岩石中应力波的衰减与频散特性。研究结果表明:应力波频谱幅值和应力波信号能量都主要集中于低频带,其中,频带0~7.81 kHz的能量占总能量的80%左右。梯度静应力作用时,岩石中的应力波质心频率随传播距离增加呈线性增加,在同一测点处,应力波质心频率随应力梯度的增加呈“先增加后减小”的变化趋势;在梯度静应力作用下,岩石应力波的频谱峰值衰减呈先快速下降再平稳发展的趋势;岩石应力波总能量与传播距离的幂函数呈线性变化;在梯度静应力作用下,应力波的频带能量和质心频率随传播距离的增加由低频带向较高频带偏移。研究结果阐释了梯度应力的围岩体中应力波的传播衰减规律,从频域的角度指出了应力波在具有梯度应力环境下的传播衰减特性。

应用同源自校正EDXRF分析法测定三元正极材料中Mn、Co、Ni的含量

锂离子电池在新能源开发与应用中具有重要作用。三元正极材料成分配比对锂离子电池产品性能与质量产生很大影响,生产控制需要及时、精确地掌握混料的成分变化。能量色散型X射线荧光(EDXRF)技术在该领域的快速分析中具有较好的应用前景,但目前商品仪器的分析精度尚不能满足生产需求。为了解决三元正极材料成分Mn、Co、Ni的高精度EDXRF分析的技术难题,提出了一种基于同源激发的自校正式EDXRF分析技术,采用钨靶X射线管(25 kV/400μA)和两个能量分辨率均为135 eV(@5.9 keV)的电致冷SDD探测器组成双路X荧光同步激发-探测装置,将X射线管发射的原级X射线经双路准直器分束后,分别激发校准样品和待测样品,两个探测器同时测量两个样品的荧光计数,采用标准样品的能谱数据对待测样品的能谱数据进行“归一化”处理实现同步校正,从而降低分析仪器中X射线管不稳定性的影响。通过8小时内的140次重复性测试,从计数衰减率、计数波动和整体效果等方面分析了该装置的稳定性,并与单光路的稳定性进行比较,以相对标准偏差和最大相对偏差作为评价指标来评估该装置的稳定性。计数衰减率从单光路的-0.0493%·h^(-1)降低到0.0010%·h^(-1),对于11个波动较大的数据点,相对标准偏差从单光路的0.1514%降到0.0326%,表明同源激发的自校正式EDXRF分析技术可有效降低计数衰减、初级X射线能谱波动的影响。从综合效果来看,经同步数据校正后,Mn、Co、Ni的相对标准偏差和最大相对偏差分别为0.076%、0.170%,稳定性较单光路提高了1倍。建立了基于双光路EDXRF分析的定量分析数学模型,经实验检验,分析粉末压样品中Mn(17.361%~20.016%)、Co(12.991%~14.965%)、Ni(29.653%~33.065%)的绝对误差分别不超过-0.072%、-0.061%、0.098%,单样品的分析时间为200 s,表明采用同源激发的自校正式EDXRF分析技术能有效改善仪器分析精度,实现快速、准确的测量要求。

Possible Relevance of the Allende Meteorite Conditions in Prebiotic Chemistry: An Insight into the Chondrules and Organic Compounds

The study of the mineral and organic content of the Allende meteorite is important for our understanding of the molecular evolution of the universe as well as the ancient Earth. Previous studies have characterized the magnetic minerals present in ordinary and carbonaceous chondrites, providing information on the evolution of magnetic fields. The interaction of organic compounds with magnetic minerals is a possible source of chemical diversity, which is crucial for molecular evolution. Carbon compounds in meteorites are of great scientific interest for a variety of reasons, such as their relevance to the origins of chirality in living organisms. This study presents the characterization of organic and mineral compounds in the Allende meteorite. The structural and physicochemical characterization of the Allende meteorite was accomplished through light microscopy, powder X-ray diffraction with complementary Rietveld refinement, Raman and infrared spectroscopy, mass spectrometry, scanning electron microscopy, and atomic force microscopy using magnetic signal methods to determine the complex structure and the interaction of organic compounds with magnetic Ni-Fe minerals. The presence of Liesegang-like patterns of chondrules in fragments of the Allende structure may also be relevant to understanding how the meteorite was formed. Other observations include the presence of magnetic materials and nanorod-like solids with relatively similar sizes as well as the heterogeneous distribution of carbon in chondrules. Signals observed in the Raman and infrared spectra resemble organic compounds such as carbon nanotubes and peptide-like molecules that have been previously reported in other meteorites, making the Mexican Allende meteorite a feasible sample for the study of the early Earth and exoplanetary bodies.

粉煤灰表面形貌和组成的电子显微镜/能量色散谱、聚焦离子束分析

用超级场发射电子显微镜 (FE SEM) ,扫描电子显微镜 /能量色散谱 (SEM/EDS)和聚焦离子束测试仪(FIB)等 ,对粉煤灰进行了表面形貌和元素组成分析。FIB显示粉煤灰大多为 0 .3～ 0 .5 μm的球状微粒 ;FE SEM则显示约有 88%的粉煤灰为 0 .3～1 μm的球状微粒 ,表面凹凸不平 ,主要为铝、硅、铁等元素的氧化物 ,其中铝、硅、铁和氧的质量分数分别为 2 0 .5 %、2 3 .6%、1 .4%和 5 0 .9%。

砚石的X射线能谱分析

用 X射线能谱仪对一系列砚石样品进行成分分析得知砚石主要含铝、硅、钙、铁、钾等元素 ,为砚石的成因研究打下基础 ,指出砚石成因研究有助于某些地球课题的深化。

复合绝缘子粉化伞裙的微观结构与憎水性的关联研究

为研究粉化硅橡胶伞裙的憎水性与其微观结构的关系,针对现场取回的3支粉化的110kV复合绝缘子,通过红外光谱、扫描电镜、能谱分析等方法开展研究。首先,利用静态接触角和喷水分级法测试样本的憎水性,粉化层表面的憎水性相比新样本略有下降,去掉表面的粉化层后,其憎水性明显下降。然后,通过红外光谱测试发现样本的主链和侧链基团(Si-O和Si-CH_3)发生了断裂,侧链甲基含量减少;扫描电镜发现去粉化层后硅橡胶表面存在大量微孔和裂纹,因而导致去粉化层后的硅橡胶伞裙表面憎水性明显降低。最后,通过能谱分析发现,粉化层中的硅含量明显高于去粉化层后硅橡胶表面和材料内部值,同时粉化层表面的粗糙度增加,说明粗糙度和硅氧烷小分子的迁移同时导致粉化层表面的憎水性优于去掉粉化层后的表面。研究结果表明,粉化与硅橡胶伞裙的憎水性关联密切,但仍需深入研究粉化复合绝缘子的运行可靠性和使用寿命。