L-shell x-ray fluorescence relative intensities for elements with 62≤Z≤83 at 18 keV and 23 keV by synchrotron radiation

The relative intensities of L-subshell x-ray fluorescence(XRF)for elements with atomic numbers 62≤Z≤83 were measured at two excitation energies,18 keV and 23 keV,using a synchrotron radiation source at a beamline of the Synchrotron Light Center for Experimental Science and Applications in the Middle East(SESAME),Jordan.The experimentally measured results of the relative intensities were compared with the calculated results using the subshell fluorescence yield and the Coster-Kronig transition probabilities recommended by Campbell and the values based on the Dirac-Hartree-Slater model by Puri.The experimental and theoretical results are in agreement.In this work,L XRF relative intensities for the elements Sm,Gd,Tb,Er,Ta,W,Re,Hg,Pb and Bi at energies of 18 keV and 23 keV were measured.

Characterization of metal element distributions in the rat brain following ischemic stroke by synchrotron radiation microfluorescence analysis

Ischemic stroke is one of the leading causes of death worldwide,and effective treatment strategies in the chronic phase of this disease remain insufficient.Homeostasis of metals in the brain plays an important role in maintaining normal brain function.However,the dynamic spatial distributions of iron,zinc,calcium,potassium,and copper in a rat brain following ischemic stroke and the association between structural distribution and function remain to be elucidated.In this study,we used a synchrotron radiation-based micro-X-ray fluorescence technique to image element mapping changes in special rat brain regions after ischemic stroke,showing the distribution characteristics of iron,zinc,calcium,potassium,and copper.We demonstrated,for the first time,the consistent dynamic spatial distributions of metal elements at a series of time points(3 h,4.5 h,6 h,12 h,1 d,3 d,5 d,7 d,10 d,14 d,28 d)after brain ischemia,which revealed that the homeostasis of iron,zinc,calcium,potassium,and copper in the brain was disturbed with distinctive change trends,providing clear insights in understanding the underlying pathogenesis of stroke from a novel perspective,thus laying the foundation of further developing new drug targets for stroke treatment.

The Study Internal Structure of the Annual Layers in Lake Sediments Using Synchrotron Radiation with X-ray Focusing Optics

1 Introduction Annually laminated(varve)sedimentary deposits are considered as one of the most important archives,since they offer precise temporal information(years)in combination with high time resolutions.Bottom sediments of the lakes contain detailed geochemical information on

Scan system for arbitrary-shaped samples at the synchrotron radiation facility

X-ray fluorescence(XRF) scan methodology is important for elemental mapping of samples at a synchrotron radiation facility. To save the experiment time and improve the experiment efficiency, one should develop an efficient XRF scan method. In this paper, a new scan mode is presented. It can map arbitrary-shaped areas withou stopping the motors. The control and data acquisition system integrates motor controlling, detector triggering, and data acquisition and storage. The system realizes the arbitrary-shaped 2D-mapping and fluorescence data acquisition synchronously. SR-XRF mapping has been performed with a standard gold mask to verify the validity of this method a beamline BL15U1 of the Shanghai Synchrotron Radiation Facility. The results show that this method reduces the tota scan time and improves the experiment efficiency.

Analysis of nickel distribution by synchrotron radiation X-ray fluorescence in nickel-induced early- and late-phase allergic contact dermatitis in Hartley guinea pigs

Background: Nickel-induced allergic contact dermatitis (Ni-ACD) is a global health problem. More detailed knowledge on the skin uptake of haptens is required. This study aimed to investigate the penetration process and distribution of nickel in skin tissues with late phase and early phase of Ni-ACD to understand the mechanisms of metal allergy. Methods: Forty Hartley guinea pigs were divided into four groups according to the NiSO4 sensitizing concentration and the NiSO4 challenged concentration: the 5% NiSO4-group, 5% to 10%(sensitization-challenge;late phase group);10% NiSO4-group, 10% to 10%(sensitization-challenge;early-phase group);and the positive and negative controls. Pathological biopsies were performed on each group. The depth profile of nickel element concentration in the skin of guinea pigs was detected by synchrotron radiation micro X-ray fluorescence spectroscopy (SR-μ-XRF) and micro X-ray absorption near-edge spectroscopy (μ-XANES). Results: In each section, the nickel element concentration in both the 5% NiSO4-group and 10% NiSO4-group was significantly higher than that in the negative control group. In the upper 300-μm section of skin for the early phase group, the nickel element concentration was significantly higher than that in the lower section of skin. In deeper sections (>200 μm) of skin, the concentration of nickel in the early phase group was approximately equal to that in the late phase group. The curve of the late phase group was flat, which means that the nickel element concentration was distributed uniformly by SR-μ-XRF. According to the XANES data for the 10% NiSO4 metal salt solution, structural changes occurred in the skin model sample, indicating that nickel was not present in the Ni^2+ aqueous ionic state but in the nickel-binding protein. Conclusions: This study showed that the distribution of the nickel element concentration in ACD skin tissue was different between the early phase and late phase groups. The nickel element was not present in the Ni^2+ aqueous ionic state but bound with certain proteins to form a complex in the stratum corneum in ACD model tissue.

In situ analysis of trace elements in metalloproteins of human liver by synchrotron radiation X-ray fluorescence

A method using synchrotron radiation X-ray fluorescence analysis toin situ determine trace elements during protein electrophoretically separating process was established. The distribution of elements in protein bands for human liver cytosolic sample separated by SDS-PAGE was analyzed along polyacrylamide gel. The results showed that the protein fraction of peak III in cytosol was mainly composed of metal ion Zn-associated proteins, being in agreement with that given by atomic absorption spectrometry. Thus, it demonstrated the feasibility of this novel technique forin situ analysis of trace elements in protein bands.

Influence of crystal materials on the synchrotron X-ray fluorescence analysis:a study of crystal and amorphous clinopyroxene

Synchrotron X-ray fluorescence analyses of crystal and amorphous clinopyroxene were compared. The results showed that using the synchrotron X-ray as a source of energy, the diffraction X-ray of crystal materials will seriously affect the X-ray fluorescence analysis. In order to avoid the influence of diffraction, the best way to solve it is to use the monochromatic source, or to have a collimating slit between sample and Si(Li) detector.

First X-ray fluorescence CT experimental results at the SSRF X-ray imaging beamline

X-ray fluorescence CT is a non-destructive technique for detecting elemental composition and distribution inside a specimen. In this paper, the first experimental results of X-ray fluorescence CT obtained at the SSRF X-ray imaging beamline （BL13W1） are described. The test samples were investigated and the 2D elemental image was reconstructed using a filtered back-projection algorithm. In the sample the element Cd was observed. Up to now, the X-ray fluorescence CT could be carried out at the SSRF X-ray imaging beamline.

Synchrotron radiation XRF microprobe investigation of elemental distribution in femoral head slice with osteoporosis

This note deals with the scanning of femoral head slices from both normal and osteoporosis subjects using synchrotron radiation X-ray fluorescence (SRXRF) microprobe technique. The sample preparation and experimental apparatus are described in detail. The quantitative computerized tomography (QCT) of elemental distribution, such as Ca, P, K, Fe, Zn, Sr and Pb in bone slice tissue including cartilage, substantial compact and substantial spongy, is investigated. Combined with the correlation between P, K, Zn, Sr and Ca, the loss way of minerals and the physiological functions of some metal elements in bone are also discussed.

Sulfur speciation and bioaccumulation in camphor tree leaves as atmospheric sulfur indicator analyzed by synchrotron radiation XRF and XANES

Analyzing and understanding the effects of ambient pollution on plants is getting more and more attention as a topic of environmental biology.A method based on synchrotron radiation X-ray fluorescence and X-ray absorption near edge structure spectroscopy was established to analyze the sulfur concentration and speciation in mature camphor tree leaves （CTLs）,which were sampled from 5 local fields in Shanghai,China.Annual SO2 concentration,SO42-concentration in atmospheric particulate,SO42-and sulfur concentration in soil were also analyzed to explore the relationship between ambient sulfur sources and the sulfur nutrient cycling in CTLs.Total sulfur concentration in mature camphor tree leaves was 766-1704 mg/kg.The mainly detected sulfur states and their corresponding compounds were ＋6 （sulfate,include inorganic sulfate and organic sulfate）,＋5.2 （sulfonate）,＋2.2 （suloxides）,＋0.6 （thiols and thiothers）,＋0.2 （organic sulfides）.Total sulfur concentration was strongly correlated with sulfate proportion with a linear correlation coefficient up to 0.977,which suggested that sulfur accumulated in CTLs as sulfate form.Reduced sulfur compounds （organic sulfides,thiols,thioethers,sulfoxide and sulfonate） assimilation was sufficed to meet the nutrient requirement for growth at a balanced level around 526 mg/kg.The sulfate accumulation mainly caused by atmospheric sulfur pollution such as SO2 and airborne sulfate particulate instead of soil contamination.From urban to suburb place,sulfate in mature CTLs decreased as the atmospheric sulfur pollution reduced,but a dramatic increase presented near the seashore,where the marine sulfate emission and maritime activity pollution were significant.The sulfur concentration and speciation in mature CTLs effectively represented the long-term biological accumulation of atmospheric sulfur pollution in local environment.

应用同步辐射微束X射线荧光光谱法研究单个大气PM_(2.5)颗粒物的源特征

将高灵敏度的同步辐射微束X射线荧光光谱分析方法与计算机模式识别技术相结合,用于上海市大气PM2.5单颗粒物的源识别。分析了污染排放源的PM2.5单颗粒物,结果表明,来自不同污染排放源的颗粒物具有不同的能谱特征。同时分析了环境空气监测样品PM2.5单颗粒物,结果表明,在上海市中心区大气PM2.5的污染源主要以机动车尾气为主,而在吴淞工业区大气PM2.5的污染源主要以钢铁工业尘和燃煤烟尘为主。

斯里兰卡曼泰遗址出土青花瓷的化学成分分析及产地初探

利用X射线荧光光谱、同步辐射X射线荧光光谱、中子活化、电感耦合等离子体原子发射光谱等多种技术手段分析了斯里兰卡曼泰遗址出土的7枚青花瓷残片的结构和成分。通过遗址出土部分青花瓷样品和中国各地瓷器样品的瓷胎元素含量聚类分析,初步判断其中的4枚青花瓷残片产自中国景德镇,而其余3枚样品的出处尚不能确定,需作进一步研究。

X射线荧光光谱原位微区分析的地学应用评介

原位微区分析是微观物质研究的重要手段,是现代分析技术的重要发展方向。以扫描核探针(SNM)、同步辐射X射线微探针(SR-XRMP)、二次离子质谱(SIMS)和激光剥蚀-电感耦合等离子体质谱(LA-ICP-MS)为主的微区痕量分析技术是一类新的微区分析手段,它从根本上解决了以电子探针分析技术(EMPA)和各类电镜(扫描电子显微镜(SEM)、透射电子显微镜(TEM)、分析电子显微镜(AEM))为主的电子微束技术(发展较早,已相当成熟)难以分析痕量元素的弱点,使原位微区分析成为一种能测定包括主、次、痕量元素和同位素在内的完整分析体系。文章收集了20世纪80年代以来原位微区X射线荧光分析地质应用探索的文献,首先介绍了相关专著、XRF专著中的相关内容及这方面的重要评述,随后从SR-XRMP、SNM、微束X射线荧光光谱(M-XRF)和多功能X射线荧光光谱仪器等方面评介其地学应用,涉及矿物微区元素分布、地质包裹体、陨石分析、从海洋矿物层状结构和韵律特征进行的成因矿物学研究及海洋环境变化、通过石笋类环带结构和湖泊沉积进行的古环境古气候研究的时间分辨率提高到季节尺度、恐龙蛋化石的铂族元素分布研究生物绝灭事件等。最后从技术特点和应用领域讨论了原位微区XRF分析的分类问题。引文187篇。

关于研制X射线荧光微分析标准物质的探讨

将经过高温处理的土壤样品进行反复研磨后,用于X射线荧光微分析标准物质的研制,当99%的粉末粒径≤30μm时,用仪器中子活化和同步辐射X射线荧光进行元素分布均匀性和最少取样量分析,结果表明24个元素的最少取样量可以降到约1mg。

用同步辐射X射线荧光分析技术测定石油地质样品中的微量元素

简述了进行同步辐射Ｘ射线荧光（ＳＲＸＲＦ）分析的原理，利用北京正负电子对撞机国家实验室（ＢＥＰＣＮＬ）的同步辐射装置（ＢＳＲＦ）提供的实验条件，根据石油地质样品的特点，设计了实验配套装置和样品制备方法；进行了改善测试检测限、提高测试精度等的实验研究。系统测定了２００多个原油、生油岩、油田水样品，测出的微量元素的种类可达２０～３０种，最小检测限可达ｐｐｍ量级．利用原油样品中微量元素的含量分布特征可以区分不同类型的原油。

高温高压下元素配分的原位实验与计算模拟研究进展

地球内部元素的配分行为具有重要意义,有助于揭示地球内部物质循环、元素成矿、超临界流体性质等基础地质问题。同步辐射微聚焦X射线荧光光谱(SR-μXRF)结合金刚石压腔(DAC)技术,可以在高温高压条件下实现高准确度和高分辨率的原位(in situ)测试元素在不同物相间的浓度,并获取配分系数。而基于地球化学热力学的理论计算模拟,可以获得元素在不同物相间的赋存形式,有助于揭示元素配分机制。本文综述了SR-μXRF结合DAC技术和地球化学热力学计算模拟原位测定高温高压下元素配分的研究方法,及其在地球内部元素迁移、成矿作用和地球早期形成过程等领域中的应用进展,认为利用该套方法研究高温高压下元素配分行为的体系将变得更加复杂,对温度、压力条件则要求更高。本文旨在更新和丰富高温高压下元素配分系数数据,深化对地球内部物质循环等问题的认知。

同步辐射X射线荧光光谱国内外研究进展

同步辐射光源是带电粒子在加速器储存环中以接近光速的速度运动时,沿轨道切线方向发射出的辐射,同步辐射X射线荧光分析(SR-XRF)是以同步辐射X射线作为激发光源的X荧光光谱分析技术。同步辐射X射线荧光分析包括了用于微区及微量元素分析的同步辐射XRF、用于表面及薄膜分析的同步辐射全反射X射线荧光(SR-TXRF)以及用于三维无损分析的同步辐射X射线荧光扫描和成像方法(如X射线荧光CT、X射线荧光全场成像、共聚焦X射线荧光和掠出射X射线荧光等)。X射线荧光光谱法通过测量元素的特征X射线发射波长或能量,识别元素,该方法首先通过测量发射的特征线强度,然后将该强度与元素浓度联系起来,对给定元素进行量化分析。X射线荧光光谱技术可以进行多元素同时分析,同步辐射X射线荧光谱亮度高,可调谐,相干性、准直性及偏振性好,可以用于分析样品元素的含量和空间分布。近些年来随着新光源技术的使用、分析软件的更新换代和定量分析方法的发展,对同步X射线荧光光谱分析产生了极大促进,采用新型X射线光学元件和探测器,能极大提升分辨率和探测效率,促进相关学科应用的发展。介绍了近几年来国内外同步辐射X射线荧光光谱分析技术及其应用发展状况,给出了国内外比较典型的同步辐射X射线荧光光谱分析光束线站最新技术方面的发展概况,并列举了一些典型应用成果,例如在生物医学、环境科学、地质考古、材料科学和物理及化学等领域的应用。对于本领域及相关领域的专家学者了解国内外同步辐射技术发展现状、应用研究成果具有一定的参考意义。

Using X-ray computed tomography and micro-Raman spectrometry to measure individual particle surface area, volume, and morphology towards investigating atmospheric heterogeneous reactions

Heterogeneous reactions on the aerosol particle surface in the atmosphere play important roles in air pollution, climate change, and global biogeochemical cycles. However, the reported uptake coefficients of heterogeneous reactions usually have large variations and may not be relevant to real atmospheric conditions. One of the major reasons for this is the use of bulk samples in laboratory experiments, while particles in the atmosphere are suspended individually. A number of technologies have been developed recently to study heterogeneous reactions on the surfaces of individual particles. Precise measurements on the reactive surface area, volume, and morphology of individual particles are necessary for calculating the uptake coefficient, quantifying reactants and products, and understanding the reaction mechanism better. In this study, for the first time we used synchrotron radiation X-ray computed tomography（XCT） and micro-Raman spectrometry to measure individual CaCO_3 particle morphology, with sizes ranging from 3.5–6.5 μm. Particle surface area and volume were calculated using a reconstruction method based on software threedimensional（3-D） rendering. The XCT was first validated with high-resolution fieldemission scanning electron microscopy（FE-SEM） to acquire accurate CaCO_3 particle surface area and volume estimates. Our results showed an average difference of only 6.1% in surface area and 3.2% in volume measured either by micro-Raman spectrometry or X-ray tomography. X-ray tomography and FE-SEM can provide more morphological details of individual Ca CO3 particles than micro-Raman spectrometry. This study demonstrated that X-ray computed tomography and micro-Raman spectrometry can precisely measure the surface area, volume, and morphology of an individual particle.

Compositional Distribution and Growth Mode of Garnet Porphyroblasts during Deformation and Metamorphism

Although porphyroblast microstructures play an important role in structural and metamorphic studies, there are still controversies in the interpretation. The focus is how porphyroblasts grow during deformation and metamorphism. In this paper, we introduce a new approach, the Synchrotron Radiation X-Ray Fluorescence, to a hemi-quantitative interpretation of the growth mode of porphyroblasts. The analysis was done at the Beijing Synchrotron Radiation Facility. The specimens were sampled from metapelite of the Baoyintu Group, northern Urad Middle Banner, Inner Mongolia. The new method is successful for determining the microscopic distribution of trace elements in porphybroblasts. The results support the theory of deformation partition, which has been brought forth by Bell and his colleagues, and demonstrate the existence of porphyroblast growth phases and the growth mode of porphyroblasts by hemi-quantitative mineral chemical analysis. The porphyroblast grows stage by stage in the manner of the distribution of a roseleaf and is controlled by deformation. We call the growth stage of porphyroblast a growth phase.

生物样品中硒的形态分析方法研究进展

对近年来关于生物样品中微量元素硒的形态分析方法的研究成果进行了综述,总结了高硒生物样品(>10 mg Se/kg)和低硒生物样品(<1 mg Se/kg)的硒形态组分提取方法,以及利用液相色谱-原子荧光光谱(LC-AFS)、高效液相色谱与电感耦合等离子质谱(HPLC-ICP-MS)等仪器联用的方法分离、检测硒的形态组分。此外,对利用同步辐射X射线微区分析方法(STXM)原位微区分析微生物样品的硒形态及其分布进行了综述与展望。