A seven-crystal spectrometer for high-energy resolution X-ray spectroscopy at Shanghai Synchrotron Radiation Facility

A Johann-type X-ray spectrometer was successfully developed at the hard X-ray branch(in-vacuum undulator with a 24-mm periodic length)of the energy material beamline(E-line)at the Shanghai Synchrotron Radiation Facility(SSRF).This spectrometer was utilized to implement X-ray emission spectroscopy(XES),high-energy resolution fluorescence-detected X-ray absorption spectroscopy(HERFD-XAS),and resonant inelastic X-ray scattering.Seven spherically bent crystals were positioned on the respective vertical 500-mm-diameter Rowland circles,adopting an area detector to increase the solid angle to 1.75%of 4πsr,facilitating the study of low-concentrate systems under complex reaction conditions.Operated under the atmosphere pressure,the spectrometer covers the energy region from 3.5 to 18 keV,with the Bragg angle ranging from 73°to 86°during vertical scanning.It offers a promised energy resolution of sub-eV(XES)and super-eV(HERFD-XAS).Generally,these comprehensive core-level spectroscopy methods based on hard X-rays at the E-line with an extremely high photon flux can meet the crucial requirements of a green energy strategy.Moreover,they provide substantial support for scientific advances in fundamental research.

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.

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.

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.

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。

能量色散X射线荧光光谱仪在镁砂成分测定中的应用

能量色散X射线荧光光谱仪(X射线能谱仪)具有体积小、价格低、分析速度快等优点而被广泛应用于高分子、陶瓷、混凝土、生物等材料的成分和形态分析,但是在耐火材料行业没有相关方法标准的规定。为了实现X射线能谱仪对镁砂中SiO_(2)、Al_(2)O_(3)、Fe_(2)O_(3)、TiO_(2)、CaO、MgO含量的快速分析,通过优化仪器参数,优选样片制备方法,进行精密度和准确度试验,能谱法和波谱法比对试验。结果表明:以熔铸玻璃片法制取样片,采用X射线能谱仪,可以快速测试镁砂样品中SiO_(2)、Al_(2)O_(3)、Fe_(2)O_(3)、TiO_(2)、CaO、MgO的含量,其相对标准偏差为0.09%~1.85%,具有满意的精密度和准确度。能谱法与波谱法的检测差值满足现用标准GB/T 21114—2019规定的允许差要求,数据可靠。

扫描电镜/能谱法对粉底液的检测分类研究

为建立一种将扫描电镜/能谱法与多元统计学结合检测粉底液物证的方法。对收集到的50个粉底液样本进行前处理,利用扫描电镜/能谱仪对样本进行分析测试,将50个样本大致分成2大类;结合K-Means聚类对实验数据进行处理,将2大类样本细化分为4类;最后利用随机森林算法搭建分类模型,40个样本作为训练集,10个样本作为测试集,测试集的预测正确率达到86.6%,预测效果良好,可实现样本分类自动化。此方法操作简单,可实现无损检材、分类效果良好,可直接用于公安机关侦查破案,在法庭科学领域有广阔的应用前景。

矿物特征自动分析系统对碎屑矿物定量识别及与传统镜下鉴定的误差分析

碎屑矿物分析被广泛应用于沉积物物源和物质扩散研究中,对分析沉积动力环境和海洋动力特征方面具有重要意义,然而长期以来碎屑矿物数据的获取主要以光学显微镜为工具,依靠人工鉴定来完成,工作量大、效率低。为使科研人员及时获得科学有效的矿物鉴定数据,本文基于热场发射扫描电镜-X射线能谱仪,利用矿物特征自动定量分析系统(简称AMICS),运用矿物表面微形貌观察和化学成分分析技术,通过实测数据自主建立的一套碎屑矿物标准库为分类依据,实现了对碎屑矿物的定量识别。AMICS系统对第一个样品共识别出矿物种类25种,人工实体显微镜-偏光显微镜法鉴定出25种;AMICS系统对第二个样品共识别出矿物种类26种,人工实体显微镜-偏光显微镜法鉴定出27种,两种方法鉴定出的碎屑矿物种类基本相同,且每一种矿物含量的误差绝对值均小于5%。该系统识别氧化物(褐铁矿、铬铁矿等),磷酸盐(磷灰石等),硫酸盐(重晶石等),硫化物(黄铁矿等),碳酸盐(方解石、白云石等),部分硅酸盐(锆石、榍石、橄榄石、石英、钾长石、钠长石、石榴石族等)相对准确,但仅依靠矿物化学成分很难准确识别同质多象和类质同象系列碎屑矿物,层状硅酸盐矿物在制样时容易逐层脱落的问题需要进一步解决。

扫描电子显微镜和能谱仪在玻璃结石成分分析中的应用

玻璃中常见各种结石缺陷,利用透反偏光显微镜可以初步判定玻璃结石的种类,但无法分析结石的成分,且处理样品效率较低。以硅质析晶结石、铝质耐火材料结石、锆质耐火材料结石为例,利用扫描电子显微镜和能谱仪分析结石,可以快速测定结石成分,辨别结石种类,进而推断结石形成的原因。采用该方法可及时准确调整生产,解决玻璃生产中产生结石问题。

便携式单波长激发能量色散X射线荧光光谱法在土壤重金属速测中的应用

应用便携式单波长激发能量色散X射线荧光光谱(SW-PXRF)法测定国家土壤标准物质(GSS-1a~GSS-8a)及安徽铜陵农田重金属污染土壤中Cr、Ni、Cu、Zn、Pb、As和Cd 7种元素的含量,将农田污染土样的测试结果与电感耦合等离子体质谱(ICP-MS)法进行对比,分析该方法对各元素的检出限、精密度及准确度。进一步探究土壤含水量和粒径对测定结果的影响,并通过实验确定现场测试时的最佳前处理条件。结果表明:SW-PXRF法对土壤中各元素检出限均低于1.3 mg/kg,其中Cd的检出限可低至0.07 mg/kg。除Cd的精密度略差外,其余元素相对标准偏差基本小于5%。除As和Cd外,其余元素相对误差的平均值均可控制在-10%~10%。SW-PXRF法与ICP-MS法的测定结果相关性较好,除Cr、Ni外,其余元素决定系数均高于0.95。土壤含水量和粒径对测定结果存在一定影响,现场测试时只要将土样在200℃下烘干6 min并研磨60 s,就能在最短时间内削弱含水量和粒径的影响。

35CrMoA螺栓失效分析和改进措施

汽轮机运行时,转子上连接联轴器的高强度螺栓如果发生断裂,轻则需要停机维修,重则造成较大事故。为了找出某汽轮机35CrMoA钢制螺栓断裂失效的原因,对失效件的宏观断口形貌进行了观察,并采用光学显微镜、扫描电镜、X射线能谱仪、硬度计设备等对失效件的微观断口形貌、显微组织、硬度和化学成分等进行了理化试验和分析,结果表明早期淬火裂纹导致了该螺栓发生沿晶脆性断裂。杆部转接处在冷镦变形过程中形成了非正常组织,硬度为430~500 HV,远高于标准硬度,其经过淬火后扩展成淬火裂纹,最终导致螺栓断裂。提出了改进冷镦工艺并增加冷镦后的热处理的建议。研究成果可为冷镦工序后硬度异常问题的处理提供参考。

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

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.

南海海泥中甲烷水合物的形貌及赋存特性

水合物表观形貌受水合物的生长方式影响,能够反映水合物在沉积物中的分布以及与沉积物的空间关系,进而对含水合物沉积物的物理特性产生影响。本文通过在实际钻采的南海神狐海域水深2713m的海泥中生成甲烷水合物,利用冷冻扫描电子显微镜(Cryo-SEM)和能谱仪(EDS)对合成水合物的微观形貌、元素组成进行表征。结果表明,与冰相比,纯水体系下的甲烷水合物形貌单一且容易分解。纯水体系生成的水合物与海泥体系生成的水合物形貌相似,均呈颗粒胶结状,微量纳米级别的颗粒冰分布在表面。元素分析表明相较于纯水体系,海泥中生成的水合物C元素含量更高,水合物笼子占有率也越高。海泥中含有微量的C元素,通过C元素含量增加及C、Si比提高确定了表面颗粒胶结状为水合物。本研究为辨别沉积物中的水合物提供了新思路,为研究水合物的表观形貌及赋存提供了重要方法。

基于扫描电镜-能谱仪的矿物定量分析——以AMICS为例

近年来,矿物自动定量分析系统被广泛应用于矿业、冶金、石油和地质等领域。该系统以扫描电镜-能谱仪(SEM-EDS)为基础,具有高放大倍数、高分辨率、高效和无损等优点,适用于矿石样品选冶和元素赋存状态等方面的研究,对优化选矿工艺流程,提高矿石元素利用率,深入认识元素赋存机制等具有重要意义。目前,基于此类定量分析系统的应用研究居多,而对其定量结果的准确性相关研究较少。以AMICS系统为例,对自制的已知含量的矿物组合样品进行了定量分析测试,探究了其最佳分析测试条件,同时对定量结果的准确性进行了分析,结果表明:AMICS系统最佳定量分析条件为电压20 kV、工作距离10 mm、束流5 nA,单点X-ray采集时间8 ms;其次,样品中不同种类、不同含量矿物的定量结果与参考值较为一致,相对误差小,定量结果可信度高,表明该系统适用于岩矿样品的高效、高质量的定量分析,对微细粒、低含量的矿物研究有着重要意义。

基于扫描电镜和能谱仪的薄膜表面形貌和厚度同时测量研究

扫描电子显微镜通过电子束轰击样品产生的二次电子、背散射电子等实现对样品表面形貌的观测,通过对样品横断面的观测来获得薄膜厚度信息,但难以实现对薄膜表面形貌和厚度的同时观测。通过能谱仪研究各种厚度的薄膜同其激发的特征X射线计数率之间的关系,实现了通过特征X射线计数率来测量薄膜厚度的方法。对于激光吹气系统所需的钨薄膜而言,结果表明,计数率随薄膜厚度的增加先线性增加后趋于稳定,利用该曲线的直线部分作为刻度曲线,可实现对5~19μm范围内钨薄膜表面形貌和厚度的同时测量,精度约为10%,通过增加电子能量可实现对更厚样品的测量。该方法可推广到其他种类的薄膜研究,有助于推动薄膜物理研究的开展。