Geochemical analysis of marine sediments using fused glass disc by X-ray fluorescence spectrometry

A method was developed for content determination of Na, Mg, A1, Si, P,S, C1, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Nb, Zr, Y, Sr, Rb, Ba, La and Ce etc. covering 26 major, minor, and trace elements in marine sediment samples using fused glass disc by X-ray Fluorescence spectrometry. Calibration was made using marine sediment certified reference materials and the synthetic standard samples prepared by mixing several marine sediments with stream sediment and carbonate standard samples in different proportions. The matrix effect was corrected using theoretical alpha coefficients, experience coefficients and the scattered radiation as the internal standard （for the trace elements）. The accuracy of the method was evaluated by analysis of certified reference materials GBW07314, GBW07334 and GSMS6. The results are in good agreement with the certified values of the standards with RSD less than 2.60%, except for Y, Cr, Ga, Ce, La, Nb, Rb, and V with RSD less than 9.0% （n=12）.

Scanning electron microscopy coupled with energydispersive X-ray spectrometry for quick detection of sulfuroxidizing bacteria in environmental water samples

Detection of sulfur-oxidizing bacteria has largely been dependent on targeted gene sequencing technology or traditional cell cultivation, which usually takes from days to months to carry out. This clearly does not meet the requirements of analysis for time-sensitive samples and/or complicated environmental samples. Since energy-dispersive X-ray spectrometry(EDS) can be used to simultaneously detect multiple elements in a sample, including sulfur, with minimal sample treatment, this technology was applied to detect sulfur-oxidizing bacteria using their high sulfur content within the cell. This article describes the application of scanning electron microscopy imaging coupled with EDS mapping for quick detection of sulfur oxidizers in contaminated environmental water samples, with minimal sample handling. Scanning electron microscopy imaging revealed the existence of dense granules within the bacterial cells, while EDS identified large amounts of sulfur within them. EDS mapping localized the sulfur to these granules. Subsequent 16S rRNA gene sequencing showed that the bacteria detected in our samples belonged to the genus Chromatium, which are sulfur oxidizers. Thus, EDS mapping made it possible to identify sulfur oxidizers in environmental samples based on localized sulfur within their cells, within a short time(within 24 h of sampling). This technique has wide ranging applications for detection of sulfur bacteria in environmental water samples.

X-ray fluorescence spectrometry determination of open-hearth furnace slag by pressed powder briquetting

A rapid analysis method of determining content of eight compounds of open-hearth furnace slag was developed using X-ray fluorescence spectrometry and pressed powder briquettes. Matrix effect was corrected using theoretical alpha coefficient. Grains-size effect was eliminated by optimized sample preparation technique parameters. Mineral effect was corrected with standard curve of specially made standard samples. The analysis results of TiO2, TFe, SiO2, MgO, Al2O3, CaO, MnO and P2O5 in slag samples showed that both precision and accuracy are comparable with that of chemical method.

Determination of Content of Eight Elements in Metal Coating Smeared on Waste Plastics by X-ray Fluorescence Spectrometry

X-ray fluorescence spectrometry was used to detect the content of eight elements in metal coating smeared on waste plastics,and effects of sample cups,elements in plastic substrate,and interaction of elements in metal coating on detection results were analyzed. The results show that the RSD of the method used to detect element content in the metal coating smeared on the waste plastics ranged from 0.008% to 0.044%; the determination range of the eight elements was 0.002%-52.0%,and their detection limit ranged from 0.0002% to 0.0008%. The determination results of X-ray fluorescence spectrometry were consistent with that of ICP-AES. The method can provide technical support for the determination of damage and pollution caused by metal coating smeared on waste plastics.

Quantitative Analysis of FeMo Alloys by X-Ray Fluorescence Spectrometry

A quantitative analysis method of molybdenum in FeMo alloys by X-ray spectrometry using borate fusion technique was compared with that with pressed pellet. The complete pre-oxidation of FeMo alloys for the preparation of homogeneous fused discs was achieved by employing an automated fusion machine equipped with specially designed O2-blowing nozzles, which used lithium tetra-borate as flux with the addition of lithium nitrate (LiNO3) as oxidizer. The calibration curves of Mo and Fe were used in the quantitative analysis of standard materials and unknown plant samples with satisfactory accuracy and precision, utilizing the corrections of the matrix effects and line overlap. It was confirmed that the newly proposed method of preparing fused glass discs of FeMo alloys can replace the conventional wet chemical analyses requiring the labor intensive and time consuming procedure.

Elemental and proximate analysis of coal by x-ray fluorescence assisted laser-induced breakdown spectroscopy

Although laser-induced breakdown spectroscopy(LIBS),as a fast on-line analysis technology,has great potential and competitiveness in the analysis of chemical composition and proximate analysis results of coal in thermal power plants,the measurement repeatability of LIBS needs to be further improved due to the difficulty in controlling the stability of the generated plasmas at present.In this paper,we propose a novel x-ray fluorescence(XRF) assisted LIBS method for high repeatability analysis of coal quality,which not only inherits the ability of LIBS to directly analyze organic elements such as C and H in coal,but also uses XRF to make up for the lack of stability of LIBS in determining other inorganic ash-forming elements.With the combination of elemental lines in LIBS and XRF spectra,the principal component analysis and the partial least squares are used to establish the prediction model and perform multi-elemental and proximate analysis of coal.Quantitative analysis results show that the relative standard deviation(RSD) of C is 0.15%,the RSDs of other elements are less than 4%,and the standard deviations of calorific value,ash content,sulfur content and volatile matter are 0.11 MJ kg,0.17%,0.79% and 0.41%respectively,indicating that the method has good repeatability in determination of coal quality.This work is helpful to accelerate the development of LIBS in the field of rapid measurement of coal entering the power plant and on-line monitoring of coal entering the furnace.

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.

氢化物发生-原子荧光法测定生活垃圾堆肥产品中砷

通过试验研究,建立了硝酸-高氯酸消解,原子荧光法测定生活垃圾堆肥产品中的砷。该方法的检出限为0.06mg/kg（按称取0.5g试样消解定容至50ml计算）,用于不同地域堆肥样品中砷的测定,其相对标准偏差（RSD）均在8.99%以下,加标回收率介于89.0%~107.0%之间。

原子荧光光谱法测定铜坑矿中的砷

建立了王水消解—原子荧光光谱法测定铜坑矿中砷的方法。讨论了矿石样品中金属元素对砷测定的干扰及消除方法;分析了影响测定结果准确性的因素,选择了合适的仪器条件、还原剂浓度、测定介质和载流酸度等,在最佳实验条件下,检出限为0.1μg/L,相对标准偏差为2.15%-4.61%,加标回收率为95.1%-102.7%,其操作快速、简便,结果准确、可靠。本法适用于闪锌矿、方铅矿、黄铁矿、黄铜矿、粘土矿物、毒砂、萤石、辉石、锡石、磁黄铁矿、铜坑矿等矿石中砷的测定。

程序控温石墨消解-顺序注射氢化物原子荧光光谱法测定豆类中总硒含量

本文建立了一种基于程序控温石墨消解-顺序注射氢化物原子荧光光谱法测定豆类中总硒含量的方法,并对消解体系、载气和屏蔽气流量、载流浓度、硼氢化钾浓度、酸度和铁氰化钾的影响等试验条件进行研究和优化,同时讨论了共存离子的干扰情况。在实验条件下,硒的测定范围为0～40μg/L,线性回归方程为:y=89.1449*C+26.4435,相关系数为0.9999,检出限为0.10μg/L,相对标准偏差为0.55%,加标回收率在97%～101%之间。该方法操作简单,准确度好,精密度高,可方便测定批量豆类样品中的总硒含量。

冷原子荧光法测定生活垃圾堆肥产品中汞

通过试验研究,建立了用王水消解、冷原子荧光法测定生活垃圾堆肥产品中汞的方法。本方法的检出限为0.006 mg/kg（按称取0.5 g试样消解定容至50 ml计算）,用于国内不同地域的堆肥样品测定,其相对标准偏差（RSD）在2.55%-10.7%之间,加标回收率介于91.0%-108.0%,可作为一种较理想的检验堆肥产品质量的方法。

Review of the diagnosis of gastrointestinal lanthanum deposition

Lanthanum carbonate is used for treatment of hyperphosphatemia mostly in patients with chronic renal failure.Although lanthanum carbonate is safe,recently,lanthanum deposition in the gastrointestinal mucosa of patients has been reported in the literature.This review provides an overview of gastroduodenal lanthanum deposition and focuses on disease's endoscopic,radiological,and histological features,prevalence,and outcome,by reviewing relevant clinical studies,case reports,and basic research findings,to better understand the endoscopic manifestation of gastrointestinal lanthanum deposition.The possible relationship between gastric lanthanum deposition pattern and gastric mucosal atrophy is also illustrated;in patients without gastric mucosal atrophy,gastric lanthanum deposition appears as diffuse white lesions in the posterior wall and lesser curvature of the gastric body.In the gastric mucosa with atrophy,lanthanum-related lesions likely appear as annular or granular whitish lesions.Moreover,these white lesions are probably more frequently observed in the lower part of the stomach,where intestinal metaplasia begins.

Nano-tribological characteristics of lanthanum-based thin films on sulfonated self-assembled monolayer of 3-mercaptopropyl trimethoxysilane

Silane coupling reagent （3-mercaptopropyl trimethoxysilane （MPTS）） was prepared on silicon substrate to form two-dimensional Self-Assembled Monolayer （SAM） and the terminal -SH group in the film was in situ oxidized to -SO3H group to endow the film with good chemisorption ability. Thus, lanthanum-based thin films were deposited on oxidized MPTS-SAM to form rare earth composite thin films （RE thin films）, making use of the chemisorption ability of the -SO3H group. Atomic Force Microscope （AFM）, X-ray Photoelectron Spectrometry （XPS）, and contact angle measurements were used to characterize the RE thin films. Adhesive force and friction force of the RE thin films and silicon substrate were measured under various applied normal loads and scanning speed of AFM tip. The results showed that the friction force increased with applied normal loads and scanning speed of AFM tip. To study the effect of capillary force, tests were performed in various relative humidities. The results showed that the adhesive force of silicon substrate increased with relative humidity and the adhesive force of RE thin films only increased slightly with relative humidity. Research showed that surfaces with higher hydrophobic property reveal lowered adhesive and friction forces.

Growth of Fluorocarbon Films by Low-Pressure Dielectric Barrier Discharge

Plasma polymerized fluorocarbon （FC） films have been deposited on silicon substrates from dielectric barrier discharge （DBD） plasma of C4Fs at room temperature under a pressure of 25～125 Pa. The effects of the discharge pressure and frequency of power supply on the films have been systematically investigated. FC films with a less cross linked structure may be formed at a relatively high pressure. Increase in the frequency of power supply leads to a significant increase in the deposition rate. Static contact angle measurements show that deposited FC films have a stable, hydrophobic surface property. All deposited films show smooth surfaces with an atomic surface roughness. The relationship between plasma parameters and the properties of the deposited FC films are discussed.

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.

Dealloying-induced dual-scale nanoporous indium-antimony anode for sodium/potassium ion batteries

InSb alloy is a promising candidate for sodium/potassium ion batteries(SIBs/PIBs)but challenged with achieving high performance by dramatic volumetric changes.Herein,nanoporous(np)-InSb with dualscale phases(cubic/hexagonal(C/H)-InSb)was fabricated by chemical dealloying of ternary Mg-In-Sb precursor.Operando X-ray diffraction(XRD)and ex-situ characterizations well rationalize the dealloying/alloying mechanisms and the formation of dual-scale microstructures/phases.As an anode for SIB/PIBs,the np-InSb electrode exhibits superior reversible capacities and lifespan compared with the monometallic porous(p)-In electrode,stemming from the dealloying-induced dual-scale nanoporous architecture and alloying strategy with proper composition.The operando XRD results demonstrate that the(de)sodiated mechanism of the np-InSb electrode involves a two-step(de)alloying process,while the(de)potassiated mechanism is associated with a full electrochemically-driven amorphization upon cycling.Additionally,the gas evolution during the(dis)charge process was monitored by on-line mass spectrometry.

Chemical Characterization of Auriferous Ores from the Brazilian State of Paraiba

One of the most important problems facing the gold industry is that the placer and free milling gold ores are almost terminating. Hence, the use of refractory ores has been increased during the recent years. In general, gold refractory ores occurs in various types of deposits associated with a range of minerals. Among the refractory ores, the sulfide type is the most common. The methodology employed in the mining process depends on the mode of occurrence of the ore and on the particle size, shape and degree of purity of the auriferous species. We have undertaken a mineralogical investigation of a representative sample of a complex gold mining ore collected in the municipality of Princesa Isabel, Paraiba, Brazil, using X-ray fluorescence spectrometry, X-ray diffractometry, infrared spectroscopy, inductively coupled plasma-atomic emission spectrometry and the Fire Assay. The results showed that the arsenic content of the ore was closely related to the gold content, and that the occurrence of “invisible gold” was associated primarily with pyrite and secondarily with arsenopyrite. The sulfur content of the ore was directly related to its refractoriness. It is concluded that gold mineralization in the study area is mainly of the gold-quartz-sulfide veins (lode gold), while the gold found in the mini-fractures of the deposits is probably associated with the hydrothermal processes that occurred in the region.

Geochemical Characterization and Mineralogy of Babouri-Figuil Oil Shale,North-Cameroon

Organic geochemistry methods such as high temperature combustion, Rock-Eval pyrolysis and gas analysis were used to analyze oil shale from Babouri-Figuil Basin. Results show that the average content of organic matter is 36.25 %wt, while that of mineral matter is 63.75 %wt. The total organic carbon (TOC) is between 15.93 %wt and 26.82 %wt. The HI vs. Tmax diagram indicates an immature Type I kerogen. The average value of the oil potential (S2b) is 149.95 mg HC/g rock. The gases obtained by retort process are H2, CO2, CO and CnH2n, CnH2n+2. Finally, it emerges that, the organic matter of Babouri-Figuil shales was immature or has just reached the beginning of the oil window. The mineralogical study of Babouri-Figuil oil shale has been carried out by means of XRD (X-Ray Diffractometry) and XRF (X-Ray Fluorescence spectrometry). The results show that mineral matrix contains silica, carbonates, sulphates, oxides and clay minerals. Besides, compounds contain metals and metalloids like Fe, In, Ca. The main oxides are SiO2 (majority), CaO, Fe2O3, Al2O3, SO3, and K2O.

国内食品分析中氢化物发生——原子荧光分析法的应用探讨

本文首先对食品分析领域中原子荧光光谱法的应用进展作一分析,分别从金属污染物汞、砷、铅等方面,探讨了原子荧光技术的分析方法及相关技术,望能为此领域应用研究有所借鉴。

Modulus and Hardness Change of Silicon and Sapphire Substrates by TiC/VC Multilayer Coatings

The nanohardness H of multilayer specimens TiC/VC@Si and TiC/VC@Sapphire prepared by Pulsed-Laser-Deposition is investigated to check the existence of a superlattice effect as known from TiN/VN multilayers. In the present work the multilayer period thickness λ varies between 1.34 nm and 24.8 nm (total layer thickness t ≈ 200 nm). Unlike Young’s modulus E, H is enhanced, regardless of t, by covering Si as well as sapphire with a TiC/VC multilayer;the relative load carrying capacity being larger for Si. The maximum value of H obtained is 38 GPa for TiC/VC@Sapphire. It is observed for a multilayer thickness of λ ≈ 10 nm. Hardness of TiC/VC@Sapphire obeys, after annealing, a Hall-Petch relation H = 35.25 + 6.945 λ–0.5 (H in GPa und λ≥ 10 nm). From orientation dependent X-ray absorption fine structure and X-ray reflection records, short-range order and layer geometry are derived. These analyses reveal a continuous approach of interatomic distances Ti-C and V-C for deceasing multilayer periods. High-resolution transmission electron microscopy shows that multilayers are nanostructured, i.e., not only TiC/VC phase boundaries but also subgrains represent obstacles against plastic deformation. Dislocations play a major role as sources of internal stress and vehicles of plasticity.