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.

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.

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.

Method and portable facility for measurement of trace element concentration in prostate fluid samples using radionuclideinduced energy-dispersive X-ray fluorescent analysis

A facility and method for109 Cd radionuclide-induced energy-dispersive X-ray fluorescent(EDXRF) were developed to determine the Fe,Zn,Br,Rb,and Sr concentrations in the specimens of human prostatic fluid.Specimens of expressed prostatic fluid were obtained from 51 men(mean age 51 years,range 18–82 years) with apparently normal prostates using standard rectal massage procedure.Mean values(M ± SEL) for concentration of trace elements(mg L^(-1)) in human prostate fluid were:Fe 9.04 ±1.21,Zn 573 ± 35,Br 3.58 ± 0.59,Rb 1.10 ± 0.08,and Sr B 0.76.It was shown that the results of trace element analysis in the micro-samples(20 l L) are sufficiently representative for assessment of the Fe,Zn,Br,and Rb concentration in the prostate fluid.The facility for109 Cd radionuclide-induced EDXRF is comparatively compact and can be located in close proximity to the site of carrying out the massage procedure.The means of Zn and Rb concentration obtained for prostate fluid agree well with median of reported means.For the first time,the Fe and Br concentrations,as well as the upper limit of the Sr concentration,were determined in the human prostate fluid.

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.

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.

Analysis of precipitation in a Cu-Cr-Zr alloy

Precipites in Cu-0.42%Cr-0.21%Zr alloy were analyzed by using scanning electron microscope （SEM）, energy dispersive X-ray spectroscopy （EDXS） and transmission electron microscope （TEM）. After the solid solution was performed at 980℃ for 2 h, water-quenched and aged at 450℃ for 20 h, the precipite had a bimodal distribution of precipitate size. The coarse precipitates are pure Cr and Cu5Zr, the dispersed fine precipitate is CrCu2（Zr, Mg） and pure Cr ranging from 1 to 50 nm. The coarse phases formed during solidification and were left undissolved during solid solution. The fine precipitates are the hardening precipitates that form due to decomposition of the supersaturated solid solution during aging.

Elemental Analysis of Soil Phosphorus Neighborhoods Using SEM, Spectral Mapping and GIS

The utility of GIS （geographic information system） methods and spatial statistical analysis on spectral maps of sediment samples were examined. Detailed elemental maps are often constructed using energy dispersive X-ray techniques and SEM （scanning electron microscopy）. The elemental neighborhood associations of a single element, P （phosphorus）, were quantified at a magnification of 3,000 ×. For each of the 170,000 pixels on the images which displayed a strong P concentration, neighborhoods from 0.1μm^2 to 12 μm^2 were examined for associated elemental concentrations. PCA （principal component analysis） revealed two significant neighborhood types associated with P in samples of pH 4, and three neighborhood types at pH 8. These neighborhoods corresponded to Mg-P associations commonly found to be chemically prevalent in river sediments impacted by agricultural operations. Discriminant analysis showed that the greatest accuracy in predicting sample pH could be achieved by using a neighborhood size of 12 ~m2. Potassium at relatively large neighborhood sizes was the element most significant in predicting pH. While many of the chemical associations in close proximity to P could be predicted and explained through mineral solubility, spatial analysis provided some interesting insights into the structure of the samples. Results also indicted differences in the spatial scale associated with different processes.

Hematite, Biotite and Cinnabar on the Face of the Turin Shroud: Microscopy and SEM-EDX Analysis

The Turin Shroud, recently accessible for hands-on scientific research, is now extensively investigated. Its pinkish red blood stains that seem anomalous ones are studied by modern techniques (notably by resolute optical microscopy and scanning electron microscopy coupled with energy dispersive X-ray). Exploration by these techniques of a blood stain located on the face permits us to discover some red-colour particles (hematite, biotite and cinnabar) of exogenous material in this stain. We finally characterize these red-colour particles and try to explain their presences in the blood stain. Globally, all these red-colour particles cannot explain all of the reddish appearance of the area under study.

Neutron Activation Analysis and Scanning Electron Microscopy of Phytoplankton in the Coastal Zone of Crimea (The Black Sea)

The physiology and ecology of planktonic organisms are influenced by the concentration, chemical speciation and resulting bioavailability of some trace metals. The determination of the elemental structure of phytoplankton is important for interpretation of physiological and functional states of coastal ecosystems. The present study is focused on the structure and elemental composition of the phytoplankton assemblages from the different coastal zones by instrumental neutron activation analysis (INAA), scanning electron microscopy (SEM) and energy-dispersive X-ray spectrometry (EDS). For the first time these complementary techniques were simultaneously applied to study the Black Sea phytoplankton. The concentrations of 45 elements in the coastal phytoplankton communities used as bioindicator of inorganic contamination of the Black Sea coastal area near Sevastopol, Ukraine, were determined. Phytoplankton samples were collected by total tows of the plankton net with 35 μm pore size at 3 stations situated in polluted and relatively pristine water areas of the Sevastopol coastal zone during autumn period of the phytoplankton growth. The concentration of Mg, Al, Sc, Ti, V, Mn, As, Rb, Ba, Th and Fe, Cr increases exponentially from relatively pristine station to more polluted station and 10-times and 3-times greater, respectively, in the phytoplankton of the Sevastopol Bay. The rare-earth elements have relatively the same concentration values less than 1 μg/g and tend to accumulate in the phytoplankton from the polluted station in the Sevastopol Bay. The obtained results are in a good agreement with the elemental concentration data in the oceanic plankton, plankton communities from the White Sea and the Black Sea. Using energy-dispersive X-ray spectrometry the mineral particles of unknown origin and impurities of copper (0.42% by weight) in the phytoplankton at the polluted station and zinc (0.57% by weight) at the relatively pristine station were determined.

物相定性分析的综合实验设计与实践

物相定性分析主要用来判定物质组成及其存在状态,是材料、化工和地质等学科专业学生必须掌握的综合性实验技能。为培养学生对材料的物相分析测试能力,设计了未知粉末物相定性分析的综合实验。以氧钼矿、黑铜矿、斜锆石和六方软锰矿的混合粉末作为盲样,依据X射线衍射和能谱元素结果,通过实验数据和综合解析推导,撰写实验分析报告,全面提高学生的仪器操作和数据分析能力。

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。

Frost Resistance of Pervious Concrete Mixed with Waste Glass Powder

The contents of waste glass powder(WGP)(0%,10%,15%,20%,25%)and water-binder ratio(W/C)(0.24,0.26,0.28)were used as influencing factors,and the quality loss rate(Δm)and compressive strength loss rate(Δfc)were used as characterization parameters.The Ca/Si ratio and main element contents of C-S-H gels with different WGP content were investigated by energy dispersive spectrometry(EDS).The pore structure evolution characteristics of WGP composite cementing materials were investigated by low field nuclear magnetic resonance(NMR).UsingΔfc as the index of frost resistance degradation and Weibull function,the frost resistance degradation of glass doped pervious concrete(WGP-PC)was modeled.The results show that,with WGP,for the same number of cycles,Δm andΔfc decrease and increase with the increase of WGP.Under the same WGP content,Δm andΔfc decrease first and then increase with the increase of W/C.After 100 freeze-thaw cycles,the samples with WGP content of 20%and W/C of 0.26 have the best freeze-resistance.Microscopic tests show that with the increase of WGP content,the Ca/Si ratio of C-S-H gel decreases at first and then increases with the increase of WGP content.The extreme value of Ca/Si is 2.36 when WGP is added by 20%.The pore volume of hardened paste with 20%WGP content decreased by 18.6%compared with that of cement system without WGP.The overall compactness of the specimen was improved.On the basis of the test data,a life prediction model was established according to Weibull function.The experiment showed thatΔfc could be used as a durability degradation index,and the slope of the reliability curve became gentle after WGP was added,which reduced the damage degradation rate of PC.W/C was 0.26.It's about 5000 hours.

X射线荧光光谱在石油炼制元素分析中的应用进展

石油原料中微量杂质元素在炼制过程会造成设备的腐蚀以及产品质量的下降,产品中的添加元素又是提升产品性能的关键,因此元素组成分析贯穿了整个石油炼制过程。伴随着硬件、软件上取得的显著技术进步,X射线荧光光谱(XRF)具备了快速、便捷、无损、覆盖元素多的特点,成为了石油化工领域元素分析应用中低碳、环保、最具有前景的普适性测试技术之一。介绍了近年来XRF技术的主要应用进展,综述了XRF在原油、汽油、柴油、润滑油、石油焦和催化剂等各个领域应用特点和问题,并总结了相关的标准方法及标准制订的变化趋势,对XRF在石油化工领域未来的应用发展趋势进行了展望。

透射槽波技术在煤田勘探中的应用研究

槽波地震勘探技术可以有效探查煤层中小断层、陷落柱等地质异常体,在探测精度和距离上明显优于其他煤矿井下勘探方法。透射法作为基本的槽波地震探测方法,具有简单灵活、探测范围大、准确率高等优势。采用透射槽波方法对实际煤矿工作面内断层构造进行探测研究,通过滤波、频散分析、波场及速度分析、能量分析以及透射CT成像等关键技术对实际透射槽波数据进行精细处理,获得准确的透射槽波成像剖面。根据槽波在煤层中受到断层阻断或遇到煤层破碎时其能量将急剧降低的特征,利用透射槽波能量CT剖面,并结合实际揭露情况,解释出12条可靠断层。通过实际煤层工作面透射槽波勘探方法测试,验证了透射槽波方法的有效性以及在煤田断层等构造探测中的实用价值。

航空发动机球轴承剥落故障模式分析

为研究航空发动机球轴承的剥落故障模式,利用原子发射光谱技术、自动磨粒分析技术、铁谱技术及能谱分析技术对球轴承加速等效试验滑油中磨粒的数量、大小、形貌及成分等信息进行分析。结果表明:金属颗粒污染物导致轴承出现初始疲劳剥落;球轴承剥落的特征磨粒为滚动疲劳磨粒和球形磨粒,内衬套微动磨损的特征磨粒为铁的黑色氧化物和红色氧化铁磨粒;临近轴承失效时,滑油中Fe元素质量分数由7.49×10-6增大至21.74×10-6,特征磨粒数量也由48.9个/mL急剧增加至1433.8个/mL,且特征磨粒直径主要分布在25~50μm。金属颗粒污染物的存在使轴承承力内半圈滚道加速出现接触疲劳剥落,滚道剥落到一定程度后,在轴向力、摩擦力及预紧力等综合作用下在内衬套与承力内半圈接触处发生微动磨损,进一步加剧了滚道的疲劳剥落,最终导致球轴承失效。

广州市某综合医院燃气蒸汽锅炉节能改造及效益分析

以广州市某综合医院为例,基于医院燃气蒸汽锅炉现状,采用高效热泵、蒸汽发生器、电热水锅炉等就近分散置换方式对燃气蒸汽锅炉进行节能改造。改造后,医院在安全、绿色、清洁、高效、智慧用能等方面均有提升,医院热水、蒸汽及供暖的安全可靠性也大大提升;能源系统调节智能灵活,供需实时互动,能源利用效率大幅提升;年节约标准煤1248.3 t,助力“双碳”目标的实现;NO_(x)年均减少排放量1.78 t,显著改善周边环境。本文针对医院燃气蒸汽锅炉的节能改造和效益分析可为类似项目提供参考。

荧光法测定铝溶胶中铝含量、氯含量分析方法探讨

对能量色散荧光光谱法测定铝溶胶中铝含量、氯含量进行研究。正确选择测试条件,考察温度对测定铝溶胶中元素的影响,并对准确性、重复性进行了验证。结果表明,该分析方法样品制备简单、分析速度快、操作简便、准确性较高、重复性较好,能满足铝溶胶中铝含量、氯含量的测定。