同步辐射X荧光法分析矿物流体包裹体若干问题的探讨

本实验的目的是研究北京同步辐射装置 (BSRF)的 XRF实验装置对地质样品中的元素、特别是对轻元素的检测能力 ,并探讨利用目前这套装置检测流体包裹体样品时的若干问题。样品是以国家标准物质GBW0 710 6为基体 ,加入一定量的 Na Cl、 KCl,混合均匀后压制成的厚样片。测量在 BSRF的 XRF实验站进行 ,储存环电流约为 40 m A。样品与 Si(L i)半导体探测器的距离为 2 cm,同步辐射源的束斑为 2 0× 2 0 μm2。实验在大气条件下进行 ,采谱时间为 2 0 0秒。计算了各元素的相对检出限、采样深度、采样量和绝对量检出限 (达 10 - 8～ 10 - 1 0 g) ;并讨论了现有条件下分析流体包裹体样品时的可测量元素范围、包裹体深度的测量方法及深度对元素 XRF强度的影响、实验设备的最佳几何配置等问题。     

The capabilities of an electrically cooled energy‐dispersive x‐ray detector for quantitative x‐ray fluorescence analysis

The capabilities of the Si PIN diode x‐ray detector were determined and compared with those of a standard Si(Li) detector. The x‐ray fluorescence (XRF) analysis systems assembled with these two detectors included annular radioisotope excitation sources of Cd‐109 and Fe‐55. The systems were calibrated for sensitivity and quantification was performed with fundamental parameters software. Based on the analysis of the standard reference material NIST 2710 (Montana soil), the elemental sensitivities and the limits of detection of both systems were obtained. The elemental sensitivities of the Si PIN detector for fluorescence x‐rays in the energy range up to 10 keV were comparable to those of the Si(Li) detector. At higher fluorescence x‐ray energies the sensitivity of the Si PIN detector gradually decreased and was smaller by a factor of ～4 at 20 keV. The reason was mainly the small thickness of the sensitive volume of the Si PIN diode (0.2 mm) and therefore the smaller relative efficiency of this detector. The assessed limits of detection (LODs) were comparable for the two detectors, which was mainly due to the lower spectral background of the Si PIN detector in excitation with the Cd‐109 source as a result of its smaller sensitive thickness. The accuracy of elemental determinations for the two detectors was comparable and within the limits of the assessed uncertainties, which were calculated considering all the steps of the analysis, i.e. spectrum measurement and analysis, sensitivity calibration and quantification. Copyright © 2004 John Wiley & Sons, Ltd.     

A Simple X-ray Spectrometer and PC-based Data Acquisition System for Newly Developed X-ray Source Based on Laser Compton Scattering

A simple X-ray spectrometer and a PC-Based Data Acquisition System(DAS) have been developed newly in Shanghai Institute of Applied Physics(SINAP),Chinese Academy of Sciences (CAS) for the measurement of the X-ray source generated using laser Compton scattering.The system consists of liquid nitrogen cooled high resolution Si(Li) detector,electronics and a DAQ.The Si(Li) detector was designed and made by Center of Advanced Instruments in SINAP,CAS,it allows us to measure X-rays with the energy up to 60 keV and the energy resolution(FWHM) of 184 eV at 5.9 keV.We measured the system uncertainty was 0.2 eV and time drifting of detector was 0.05% both at 5.9 keV.The DAQ was based on Object-Oriented software LabVIEW 7.1,it has data on-line analysis and original data saved functions.     

硬X光弯晶谱仪的定量化标定方法

介绍了具有定量化测量能力的硬X光弯晶谱仪的结构, 利用Mo靶X光管的K特征线作为标定源, 使用绝对标定过的Si(Li)探测器对X光管出射的特征线谱进行强度和谱测量。结合X光管空间分布均匀的特点, 计算进入弯晶谱仪的光子数目, 采取了特征谱扣去轫致谱的计数处理方法, 得到了17 keV和19 keV处弯晶谱仪的绝对效率, 分别为4.3210-4和3.9410-4。     

Measurement of X-ray production cross-sections of Ti,V, Cr,Mn, Fe,Co, Ni and Cu molecules

K shell X-ray production cross-sections in the Ti, V, Cr, Mn, Fe, Co, Ni, and Cu in the molecules were studied at 59.5 keV excitation energy by using a Si(Li) detector ( FWHM = 155 eV at 5.96 keV). The present results are compared with other theoretical values.     

The advantages of using digital signal processing in polarized x‐ray fluorescence analysis

Improving the specificity and productivity of XRF is of great relevance for the determination of trace elements in samples of diverse origin. The advantages of using digital signal processing in energy‐dispersive polarized x‐ray fluorescence analysis are demonstrated by comparing the instrumental sensitivities achieved with those obtained by using a conventional analogue signal processing‐based spectrometer. A compact geometry secondary target arrangement was designed to increase the effective solid angles and to reduce the distances between secondary target, sample and detector, thus achieving larger x‐ray fluxes for both the excitation and detection process, resulting in improved instrumental sensitivities. The performance of both spectrometers was evaluated for two different detectors: an Si(Li) detector and a thermoelectrically cooled passivated‐implanted planar silicon detector (X‐PIPS). The uncertainties achieved and accuracy are illustrated for the analysis of a group of sediment and organic‐origin certified reference materials using two different quantitative procedures. Copyright © 2006 John Wiley & Sons, Ltd.     

PGNAA-XRF联合检测水溶液中重金属的研究

重金属污染越来越受到人们的关注,迫切需要开发具有高精度的原位检测技术。瞬发伽玛中子活化分析（PGNAA）技术具有原位、无损、快速等优点而被广泛应用于重金属测量,但由于目前原位检测装置中使用的中子源通量相对较低,因此对一些重金属元素分析精度相对不高。为提高测量精度,直接利用PGNAA技术中的瞬发特征γ射线充当传统X荧光光谱分析的激发源,来激发重金属元素的特征X射线荧光（XRF）信息,提出了一种PGNAA-XRF联合检测水溶液中重金属元素的方法,并设计了一套由BGO和带铍窗的NaI组成的双探测器联合检测装置,分别用来探测PGNAA中瞬发特征γ射线和特征X荧光信息。通过MCNP分别模拟研究了Cr,Cd,Hg和Pb的浓度（ｃ_i）对瞬发特征γ射线强度（I_γ）和特征X荧光强度(I_X)的影响,模拟结果表明该装置中Cr,Cd,Hg和Pb元素的I_γ和I_X均与ｃ_i成良好的线性关系,并建立了联合检测方法的经验公式。比较重金属元素特征X射线荧光发现,该联合方法对Hg和Pb等高原子序数重金属的检测较灵敏,最后计算得到该装置对Hg和Pb等重金属元素的检测限分别为17.4和24.2 mg·kg-1。     

垂直氧化锌纳米线中的激射现象

通过水热的方法以退火0.5 h的ZnO薄膜作为籽晶,得到垂直的ZnO纳米线.在X射线衍射谱中,除了Si的(400)衍射峰以外,只观察到了ZnO的(002)衍射峰.室温光致发光谱中出现了强的紫外发射峰,同时也伴随着弱的缺陷相关的发射.这些数据表明垂直的ZnO纳米线序列有着较好的晶体质量.同时,通过光泵浦也观察到了ZnO纳...     

Molecular Emission Spectrohetry ih a Low Pressure Electrical Discharge

A low pressure electrical discharge for excitation of polycyclic aromatic hydrocarbons, PAHs, without fragmentation is described. The discharge characteristics as well as the plasma background spectra are given. The application of the discharge for the excitation of molecular spectra of PAHs is described. Difficulties with correction of the analyte emission spectrum for the background emission spectrum of the gas (He) are mentioned. Analytical use of the discharge for detection of PAH3 introduced by gas chromatography is described and is shown to be of marginal analytical use because of the rather poor detection limits of about 1 μg.

Jurgensen and Winefordner¹ have reviewed both reduced pressure and atmospheric pressure nitrogen discharges for detection of atomic and molecular species. The same authors² have also described an active nitrogen-induced chemiluminescence system for detection of polycyclic aromatic hydrocarbons, PAHs, and achieved detection limits in the range of 0.01 - 2000 ng. The intriguing aspect of the active nitrogen—induced chemiluminescence approach² for detection of PAHs was that the discharge was gentle resulting in little fragmentation of the PAHs and in the appearance of emission spectra characteristic of the parent molecules. Because of the poor understanding of the mechanism of excitation of the large organic molecules and the minimal fragmentation and because of the lack of control of the direct discharge as opposed to the afterglow in the studies of Jurgensen and Winefordner², the present authors began a careful study of the physical and analytical characteristics of this discharge in the fall of 1984. The physical characteristics were reported by Yu and Winefordner³ and indicated that the previous workers², were using the direct discharge plasma as a result of llpoorlv grounding. In addition, the same workers³ showed that the active nitrogen afterglow was not capable of exciting PAHs. In this note, we report on the analytical capabilities of an improved active gas (nitrogen or helium) electrical discharge system for gaseous PAHs.     

Al窗Ag靶微型透射式X射线管模拟与性能分析

微型透射式X射线管广泛应用于能量色散X射线荧光分析领域,具有体积小、功耗低、X射线发射效率高等特点,可作为手持式X射线荧光分析仪器的激发源。目前常用铍(Be)作为出射窗材料,成本高,而且有毒性。同时为减少低能散射射线,在射线管前端放置铝(Al)作为过滤窗。本文拟采用Al为微型透射式X射线管出射窗材料,透射高能射线,屏蔽低能散射射线,降低制作成本和难度。文中采用蒙特卡洛模拟软件MCNP5模拟计算不同银(Ag)靶厚度和Al窗厚度的X射线管输出谱。结果表明,Al窗对低能射线的屏蔽作用强于对高能射线的屏蔽作用,在Al窗厚度超过1.5 mm时,低能射线完全被屏蔽,高能射线有部分透射。通过和已有研究成果[1,5]对比分析,在Ag靶厚度为2 μm,Al窗厚度为0.8 mm时,低能射线所占的比例仅为0.087 8%,高能射线产生率为0.002 73%,既能有效屏蔽低能射线,又能保证高能射线较高的出射率,能够满足野外现场能量色散 X射线荧光分析的需要。     

Determination of phosphorus and other elements in atmospheric aerosols using synchrotron total‐reflection X‐ray fluorescence

In this study, P and other low Z elements were determined in aerosol particulates from ambient air using synchrotron radiation‐induced total‐reflection X‐ray fluorescence analysis. Atmospheric transport of nutrients such as P or Si to the oceans is a key factor to marine plankton growth. Concentration of these elements in marine air masses is generally low (P < 10 ng/m³). Therefore, analytical procedures enabling for low detection limits are of interest. Because particle size is strongly correlated to its origin and sedimentation, the aerosols were collected with the aid of a low‐pressure Berner impactor, which separates the aerosol particulates in nine size fractions with the smallest fraction from 15 to 30 nm. To be able to determine low Z elements, measurements were performed under vacuum conditions at the FLUO beamline at the ANKA synchrotron. An excitation energy of 3.5 keV near the P K‐edge but below the Ca K absorption edge was chosen to avoid interferences of the P K‐line with the detector escape artifact of the Ca‐Kα line. The result showed P was present in concentration from 2 to 180 ng/m³. Detection limits were found to be generally 0.2–0.3 ng/m³ for a collecting time of 1 h for the aerosols, which is an improvement to detection limits reported in other studies. Other elements such as S, Cl, and Si were determined as well. Si like P is a nutrient for marine plankton (diatoms). S and Cl play an important role in cloud formation, e.g. polar stratospheric clouds. Copyright © 2013 John Wiley & Sons, Ltd.     

EDXRF analysis of red and white wines from Brazil

Several wines produced in different regions in southern Brazil and commercially available in Rio de Janeiro were analyzed for their contents of elements such as V, Fe, Ni, Cu, Zn, Mo and Pb. Multielement analysis was carried out with simple sample preparation and subsequent analysis by EDXRF spectrometry. The liquid residue was pre‐concentrated with the use of a chelating agent (ammonium pyrrolidinedithiocarbamate) and filtered through a Millipore filter (0.45 µm) by a vacuum pump. The experimental setup is based on a low‐power (2.25 W) miniaturized x‐ray tube and an Si(Li) detector. The levels of the various elements in the Brazilian wines are lower than those generally found in the literature, with the exception of Mo. The present study indicates the capability of multielement analysis for determining the contents of various elements present in wines by using a simple, sensitive and precise method. Copyright © 2004 John Wiley & Sons, Ltd.     

Synthesis of SiC/graphene nanosheet composites by helicon wave plasma

We report an approach to the rapid, one-step, preparation of a variety of wide-bandgap silicon carbide/graphene nanosheet(Si C/GNSs) composites by using a high-density helicon wave plasma(HWP) source. The microstructure and morphology of the Si C/GNSs are characterized by using scanning electron microscopy(SEM), Raman spectroscopy, x-ray diffraction(XRD), x-ray photoelectron spectroscopy(XPS), and fluorescence(PL). The nucleation mechanism and the growth model are discussed. The existence of Si C and graphene structure are confirmed by XRD and Raman spectra.The electron excitation temperature is calculated by the intensity ratio method of optical emission spectroscopy. The main peak in the PL test is observed at 420 nm, with a corresponding bandgap of 2.95 e V that indicates the potential for broad application in blue light emission and ultraviolet light emission, field electron emission, and display devices.     

Experimental evaluation of X‐ray optics applied for microanalysis

The performance of x‐ray capillary lenses has been evaluated. The tests were carried out using an x‐ray tube set‐up. A single glass capillary with tapered inner channel, a monolithic glass polycapillary, and an in‐house manufactured single metallic capillary with parabolic inner channel were characterized in terms of gain, spatial resolution, and element detection limits. The spatial resolution of a confocal set‐up utilizing a monolithic glass polycapillary and a polycapillary conical collimator has also been measured. The highest gain of about 2500 was observed for the glass polycapillary. The maximum gain achieved with the single glass capillary was equal to about 25, and the gain of the metallic capillary was only slightly greater than 1. For the glass capillary and polycapillary lenses, significant filtering of the higher‐energy photons (energy > 8 keV) was observed. The lowest relative detection limits were obtained with an ordinary cylindrical collimator and the polycapillary lens. Similar absolute detection limits were achieved with the use of the polycapillary and single capillary lenses. A relation between the ratios of the detection limits of elements achieved with different x‐ray lenses and the lens parameters (spatial resolution and gain) has been proposed and was verified experimentally. The monolithic polycapillary lens was found to be an optimum focusing device for an x‐ray tube‐based scanning spectrometer. This type of x‐ray lens can be coupled with a polycapillary conical collimator or a polycapillary half‐lens to make a confocal x‐ray microscope capable of depth profiling with a spatial resolution equal to about 30 micrometers. Copyright © 2008 John Wiley & Sons, Ltd.     

ELECTROHYDRODYNAMIC ENHANCEMENT OF HEAT TRANSFER IN A SHELL-AND TUBE HEAT EXCHANGER

Enhancement of heat transfer in a heat exchanger via a DC corona discharge was studied experimentally using a single-tube shell-and-tube heat exchanger. Air was the working fluid in both the tube and shell sides. Excitation of the tube side was via a single wire electrode, while that of the shell side was via four rod electrodes oriented symmetrically at 90^° intervals. Three series of experiments were performed: (1) excitation of the tube side only, (2) excitation of the shell side only, and (3) simultaneous excitation of the tube and shell sides. Both heat transfer and pressure drop measurements were performed, with Reynolds number and electric field potential as parametric quantities in the tube and shell sides. It was found that highest enhancements take place when the tube and shell sides are excited simultaneously, yielding a 322% increase in the overall heat transfer coefficient. Study of the heat transfer enhancements per unit pumping power indicates that for the range of parameters studied, the technique is most efficient at moderate Reynolds numbers and at electrode potentials in the midrange between threshold and sparkover limits.     

Simulation of jet-noise excitation in an acoustic progressive wave tube facility

Acoustic excitation produced by jet-engine effluxes was simulated in a progressive wave tube (APWT) facility with a computer-based control system. The APWT siren is driven by a signal generated numerically in a PC and then converted into analog form. Characteristics of the acoustic pressure measured by a microphone are analyzed in digital form and compared with those prescribed for simulation. Divergence is compensated by immediate modification of the driving signal and this action is repeated in the form of iterative process until the test specification is attained. Typical power spectral density (PSD) shapes with maxima at low and high frequencies were simulated. A "tailoring" approach has been also achieved when a test specification was determined directly from field measurements for the particular aircraft under consideration. Since acoustic pressure signals of high level differ from the Gaussian random process model, particularly in terms of asymmetric probability density function, a method has been developed to make the driving signal also non-Gaussian by simulating skewness and kurtosis parameters of the APWT acoustic excitation simultaneously with PSD control. Experimental results with Gaussian and non-Gaussian characteristics obtained for various PSD specifications including sharp and narrow peaks are presented in the paper.     

Determination of elements in some lichens growing in Giresun and Ordu province (Turkey) using energy dispersive X-ray fluorescence spectrometry

The concentration of five different elements in six lichens species of different regions in Giresun and Ordu (Turkey) was determined using the energy dispersive X-ray fluorescence method. A radioisotope excited X-ray fluorescence analysis using the method of multiple standard addition is applied to the elemental analysis of lichens. An annular 50 mCi ²⁴¹Am radioactive source and an annular 50 mCi ⁵⁵Fe radioactive source were used for excitation of characteristic K X-rays. An Si(Li)detector which has a 147 eV full-width at half-maximum for 5.9 keV photons was used for intensity measurements. A qualitative analysis of spectral peaks showed that the samples contained potassium, calcium, titanium, iron, and barium.     

A perspective view to hard-X-ray astronomy

Summary The present observational and instrumental status of hard-X-ray astronomy ((10÷200) keV) is discussed. The relevance of observations in this energy range is stressed and a few examples of unsolved observational problems in galactic and in extragalactic astronomy are discussed. In these examples we focus on the possibility to solve the problems with observations using detectors of the current generation. In this framework, the performances of the most sensitive hard-X-ray detectors are discussed with particular emphasis on the control of systematic errors. Quite simple but unavoidable considerations on limits of the present generation of hard-X-ray detectors (supported by results of simple simulations) lead to the conclusion that a decisive breakthrough can be achieved only using optics with a sufficiently good concentration power. In particular we discuss the feasibility of hard-X-ray telescopes (with a concentration power ≫1), using either grazing incidence or Bragg diffraction. The use of concentrators in this energy band can also make feasible polarimetric measures of a substantial sample of X-ray sources, up to now severely limited by the very low detection efficiency of the devices used in polarimetry. Paper presented at the V Cosmic Physics National Conference, S. Miniato, November 27–30, 1990.     

Determination of experimental K-shell fluorescence yield for potassium and calcium compounds

K-shell fluorescence yields were experimentally determined for potassium and calcium compounds using a Si(Li) X-ray detector system (FWHM=5.96 keV at 160 eV). The samples were excited by 5.96 keV photons produced by a ⁵⁵Fe radioisotope source. The experimental values are systematically lower than the theoretical values.      

MEASUREMENT OF L-SHELL IONIZATION CROSS SECTIONS FOR NIOBIUM BY ELECTRON IMPACT

L-shell ionization cross sections of Nb by electron impact in the energy range from 3 to 40 keV have been determined with a Si(Li) X-ray detector. Influence of reflected electrons from backing on the measurement was corrected using an electron transport model. The experimental results are compared with theoretical calculations of Gryzinski and McGuire.