基本参数法在地面验证实验中的的应用

As the nearest celestial body to the earth, the moon has become a hot spot again in astronomy field recently. The element analysis is a much important subject in many lunar projects. Remote X-ray spectrometry plays an important role in the geochemical exploration of the solar bodies. Because of the quasi-vacuum atmosphere on the moon, which has no absorption of X-ray, the X-ray fluorescence analysis is an effective way to determine the elemental abundance of lunar surface. The CE-1 X-ray fluorescence spectrometer （CE-1/XFS） aims to map the major elemental compositions on the lunar surface. This paper describes a method for quantitative analysis of elemental compositions. A series of ground base experiments are done to examine the capability of XFS. The obtained results, which show a reasonable agreement with the certified values at a 30% uncertainty level for major elements, are presented.     

基于地面试验的嫦娥五号月球矿物光谱分析仪数据质量分析

探月工程三期项目将完成“绕、落、回”三个阶段中的采样返回任务,将在未来发射嫦娥五号(CE-5)探测器,执行月面着陆、采样并返回地球的任务。嫦娥五号月球矿物光谱分析仪(LMS)是探月工程三期重要的数据来源,通过LMS光谱数据分析识别月球表面物质的矿物组成,包括含水矿物,同时有助于判断岩石类型,辅助地层学分析。为月球的形成过程、月球地质演变及岩石-水交互作用的研究提供数据支撑。相比于嫦娥三号红外成像光谱仪,LMS将光谱范围从450～2 400 nm扩展到了480～3 200 nm,除了能探测月球表面主要矿物辉石、橄榄石等,还可以探测3 000 nm附近的羟基吸收峰特征,为月球表面是否存在“水”提供强有力的证据。此外,嫦娥五号月面工作任务将获取月表以下物质,LMS可以对月表采样前后的采样区域进行光谱探测,比较不同深度、不同风化程度下的月壤光谱特征,且与后期返回样品的实验室光谱对比分析。为保证LMS月面数据的可靠性,在探测器发射之前开展了LMS地面验证试验,采用多种矿物及矿物混合样品,在不同试验环境下获取LMS的探测数据,分析研究LMS的矿物成分探测能力,并结合标准比对仪器光谱进行光谱质量分析。计算了所有实验样品的光谱不确定度参数。除了具有低反射率的钛铁矿外,所有样品都具有高质量的光谱数据。同时,在相同条件下,LMS光谱特征与标准比对仪器得到的光谱数据相一致,表明LMS整体数据质量高。     

Prospective results of CHANG'E-2 X-ray spectrometer

The Chinese second lunar satellite CE-2, which carries an X-ray spectrometer （XRS）, will be launched at the end of 2010. In order to estimate the scientific results of XRS, we simulate the anticipated lunar X-ray spectra observed by XRS by using the expected mean solar X-ray flux in 2011. We also obtain the integration time and the spatial resolution required to achieve a certain significance level for the major lunar rock-forming elements in different solar activity conditions. It is expected that a spatial resolution of finer than 100 kilometers can be achieved for elements Mg, Al, Si, Ca, Ti, and Fe.     

Prospective results of CHANG'E-2 X-ray spectrometer

The Chinese second lunar satellite CE-2, which carries an X-ray spectrometer (XRS), will be launched at the end of 2010.In order to estimate the scientific results of XRS, we simulate the anticipated lunar X-ray spectra observed by XRS by using the expected mean solar X-ray flux in 2011.We also obtain the integration time and the spatial resolution required to achieve a certain significance level for the major lunar rock-forming elements in different solar activity conditions.It is expected that a spatial resolution of finer than 100 kilometers can be achieved for elements Mg, Al, Si, Ca, Ti, and Fe.     

The Usage of Fundamental Parameter Method in Ground-base Experiment for Quantitative Analysis

As the nearest celestial body to the earth, the moon has become a hot spot in astronomy researches again recently [1-3], while the resource exploration is of much importance for lunar project. For the quasi-vacuum atmosphere in the moon, X-ray quantitative analysis is a effective way to determine concentration of the element on lunar surface, especially for determination of Mg, Al and Si[1,4]. As one of the ChangE-1’s payloads, the X-ray spectrometer is aiming to map the global elements distribution on the lunar surface. The X-ray Spectro-graph is examined on ground for its usage for quantitative analysis in deep space mission, and the results are in accord with the certified values.     

CE-1干涉成像光谱仪数据光度校正与反射率计算

干涉成像光谱仪(interference imaging spectrometer,IIS)是嫦娥1号探月卫星(chang'e-1,CE-1)搭载的有效载荷,具有图谱合一的特点,用于实现月表重要元素及矿物类型的分布与含量分析的科学目标.由于观测条件的不一致,IIS获取的不同区域的月表数据明暗差异显著,因此,必须要进行光度校正,以消除由于观测条件不一致而引起的目标辐射特性的不均一性.文章在分析IIS数据特点的基础上,利用改进的Lommel-Seeliger模型对辐射定标后的IIS辐亮度数据进行逐像素光度校正;选定距离Apollo16着陆点最近的一块区域作为定标区,利用实验室测得的62231月壤样品双向反射率作为校正标准进行辐亮度到反射率的计算,得到CE-1 IIS反射率数据,并选择71501月壤样品对反射率计算结果进行精度评价.该工作对于月表矿物类型识别和信息提取、不同类型月表矿物与岩石的分布图绘制等具有重要意义.     

一种毛细管聚焦的便携式微束X射线荧光谱仪

基于毛细管X光透镜技术的便携式能量色散X射线荧光分析因其无损分析等优点成为分析文物样品的有利工具。但由于文物样品的表面不平整或弧度以及毛细管X光透镜聚焦X射线的特点，导致在测量过程中样品测量点与毛细管X光透镜出端之间的距离产生变化，引起照射样品的X射线束斑大小发生改变，从而影响测量结果的准确性和元素区域扫描的分辨率。介绍了本实验室自行研发的一种新型便携式微束X射线荧光谱仪，此谱仪主要是由SDD X射线探测器、30 W低功率X射线管、毛细管X光透镜、CCD和一个新型闭环控制系统构成。该闭环控制系统是在激光位移传感器能够精确控制样品测量点到毛细管X光透镜出端距离的基础上，结合LabVIEW语言环境下开发的计算机控制程序以及步进电机、样品台等器件组成。基于此系统，该实验室研发的便携式微束X射线荧光谱仪在测量过程中可以时刻保证照射样品的X射线光斑大小固定不变。同时，该谱仪还可以通过调整样品测量点到透镜出端的距离来选择不同尺寸的X射线照射光斑。为了验证设备的可行性，使用该便携式微束X射线荧光谱仪在激活激光位移传感器和关闭激光位移传感器两种情况下测量了一块表面不平整古陶瓷样品釉彩层中K，Ca，Zn和Fe等元素的含量及分布，并将测量结果进行了对比。结果显示，在激活激光位移传感器的情况下测得的样品微区元素含量与真实值较接近，扫描区域元素分布图的分辨率更好，表明本谱仪基于激光位移传感器开发的自动调整样品测量点到透镜出口端距离的闭环控制系统能有效的减少由于样品表面不平整或弧度带来的测量误差，弥补了现有微束X射线荧光谱仪在此方面的不足。因此，本便携式微束X射线荧光谱仪在无损分析检测文物方面具有潜在的应用前景。     

Confocal three-dimensional micro X-ray fluorescence based on synchrotron radiation for mineral analysis

The confocal three-dimensional micro X-ray fluorescence using polycapillary optics and a synchrotron radiation was applied to nondestructively analyze elemental compositions of minerals, and thereby obtain the three-dimensional distributions of elements in the minerals. Such confocal micro X-ray fluorescence had potential applications in the mineral prospecting, identification of jades, differentiation of stones.     

古代多色硅酸盐制品的光谱学分析及方法学研究

采用自主搭建的多光谱成像系统、便携式X射线荧光光谱仪(X-ray fluorescence spectrometer, XRF)、激光拉曼光谱仪(laser Raman spectrometer, LRS)对5件战国时期多色硅酸盐制品的表面物质的光谱特性、化学成分和物相结构进行了无损分析。根据多光谱图像中的光谱响应情况,对样品表面物质进行了区域划分,并发现样品表面的多数蓝、绿、紫色系区域出现荧光现象。XRF检测结果表明不同区域的化学成分存在明显差异,但多数区域均以SiO₂,PbO,BaO为主要化学成分,5件样品基本属于铅钡硅酸盐体系,而且出现荧光区域皆是铜离子致色。LRS精确检测出各个区域中的玻璃相、中国蓝、中国紫、石英、赤铁矿、铅白、无定形碳等物相,并发现产生可见发光二极管致近红外荧光的物质为中国蓝和中国紫。利用X射线衍射技术(X-ray diffraction, XRD)验证了LRS检测结果的正确性。本研究将多用于书画分析的多光谱成像面检测技术与常用于硅酸盐文物成分分析的XRF和LRS技术进行有效结合,提出了一套更为高效的无损的分析古代多色硅酸盐制品的研究方法。光谱图像与X射线荧光光谱、激光拉曼光谱数据的结合,将样品的光谱特性与化学构成联系起来,有助于提高硅酸盐文物的分析效率,加强对硅酸盐文物的整体认识,和降低硅酸盐文物的受损风险。     

X射线荧光微区分析结合电感耦合等离子体质谱法进行保健食品中元素含量的测定

X射线荧光光谱微区分析法既有X射线荧光光谱法快速、简便、无损检测等特点,又可对保健食品表面的元素分布进行检测,电感耦合等离子体质谱法具有检出限低、线性范围宽、多元素同时测定等优点,旨在建立一种X射线荧光光谱微区分析法和电感耦合等离子体质谱法联合测定保健食品中元素种类、分布及含量的方法。利用Ｘ射线荧光光谱微区分析技术对一种保健食品进行了元素种类及元素在样品表面的分析,并对元素含量进行了半定量分析,确定保健品中含有钙（Ca）、铁（Fe）、钌（Ru）、钼（Mo）元素。利用微波消解-电感耦合等离子体质谱法对其中含有的主要元素Ca和Fe进行了定量分析。微波消解-电感耦合等离子体质谱法测定结果Ca元素平均值为6.23%,相对标准偏差1.78%;Fe元素平均值3.82%,相对标准偏差 2.14%。与X射线荧光光谱微区分析法半定量测试结果的样品中含有的Ca元素含量在6.0%～10.0%之间,样品中含有的Fe元素含量在2.0%～4.0%之间的结论一致。且通过X射线荧光光谱微区分析法得知保健食品表面的各元素分布不均匀。结果表明：X射线荧光光谱微区分析方法既可利用微量样品快速无损测得保健食品中的元素半定量含量,又可测得保健食品中的元素分布情况。结合电感耦合等离子体质谱法,还可以对样品中感兴趣的元素含量进一步检测,得到定量分析结果。     

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...     

Orbit determination for Chang’E-2 lunar probe and evaluation of lunar gravity models

The Unified S-Band (USB) ranging/Doppler system and the Very Long Baseline Interferometry (VLBI) system as the ground tracking system jointly supported the lunar orbit capture of both Chang’E-2 (CE-2) and Chang’E-1 (CE-1) missions. The tracking system is also responsible for providing precise orbits for scientific data processing. New VLBI equipment and data processing strategies have been proposed based on CE-1 experiences and implemented for CE-2. In this work the role VLBI tracking data played was reassessed through precision orbit determination (POD) experiments for CE-2. Significant improvement in terms of both VLBI delay and delay rate data accuracy was achieved with the noise level of X-band band-width synthesis delay data reaching 0.2–0.3 ns. Short-arc orbit determination experiments showed that the combination of only 15 min’s range and VLBI data was able to improve the accuracy of 3 h’s orbit using range data only by a 1–1.5 order of magnitude, confirming a similar conclusion for CE-1. Moreover, because of the accuracy improvement, VLBI data was able to contribute to CE-2’s long-arc POD especially in the along-track and orbital normal directions. Orbital accuracy was assessed through the orbital overlapping analysis (2 h arc overlapping for 18 h POD arc). Compared with about 100 m position error of CE-1’s 200 km×200 km lunar orbit, for CE-2’s 100 km×100 km lunar orbit, the position errors were better than 31 and 6 m in the radial direction, and for CE-2’s 15 km×100 km orbit, the position errors were better than 45 and 12 m in the radial direction. In addition, in trying to analyze the Delta Differential One-Way Ranging (ΔDOR) experiments data we concluded that the accuracy of ΔDOR delay was dramatically improved with the noise level better than 0.1 ns and systematic errors better calibrated, and the Short-arc POD tests with ΔDOR data showed excellent results. Although unable to support the development of an independent lunar gravity model, the tracking data of CE-2 provided evaluations of different lunar gravity models through POD. It is found that for the 100 km×100 km lunar orbit, with a degree and order expansion up to 165, JPL’s gravity model LP165P did not show noticeable improvement over Japan’s SGM series models (100×100), but for the 15 km×100 km lunar orbit, a higher degree-order model can significantly improve the orbit accuracy.

     

X射线光谱在文物无损分析中的研究进展

文物遗存是人们认识历史发展的重要依据,通过对它们的相关研究可以了解古人的生存方式、生产技能、人与自然的关系等。X射线光谱（X射线荧光光谱和X射线吸收精细结构谱）作为重要的无损分析方法,可以用来研究物质内部元素组成和特定元素近邻结构等信息,为文物的保护研究和价值认知等提供支撑,目前被广泛应用于各种古代物质遗存的研究工作中。对近些年X射线光谱在不同类型文物研究中的应用情况进行简要的总结和介绍。总的来看,X射线荧光光谱技术在古陶瓷、油画、青铜器的断源断代研究方面发挥了重要作用,而基于X射线荧光光谱的成分数据库建设和X射线吸收精细结构谱在文物研究相关问题的深度介入是应用实践中的难点,也应是未来研究工作中的重要课题。     

Development of an online X-ray fluorescence analysis system for heavy metals measurement in cement raw meal

ABSTRACT

Particulate matters, gaseous chemicals, and heavy metals emitted from industrial processes into the environment could be directly transmitted to humans through air inhalation. In order to accurately estimate health risk and control the source of pollution caused by cement raw meal, an online X-ray fluorescence analyzer system, consisting of an X-ray fluorescence analyzer with data acquisition software and a laser rangefinder, was developed to carry out the measurement of heavy metals in cement raw meal. The X-ray fluorescence analyzer was mounted on a sled, which can effectively smooth the surface of cement raw meal and reduce the impact of surface roughness during online measurement. The laser rangefinder was mounted over the sled for measuring the distance between cement raw meal sample and the analyzer. Several heavy metals and other elements in cement raw meal were online measured by the X-ray fluorescence analyzer directly above a conveyor belt. The limits of detection for Pb, Cr, Fe, Ti, Ca, and S by the analyzer were 47 ± 1, 33 ± 1, 37 ± 1, 44 ± 1, 246 ± 4, and 118 ± 1 mg kg^?1, respectively. The relative standard deviation (RSD) for the elements mentioned was less than 10.7%. By comparison with the results by inductively coupled plasma mass spectrometry (ICP-MS) and CHNS/O elemental analyzer, relative deviation (D) of the online X-ray fluorescence analyzer was less than 7.4% for Fe, Ti, Ca, and S, between 1.71% and 12.10% for Pb and Cr.     

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.     

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.     

蛛丝和蚕丝化学元素X射线荧光光谱分析及其应用

采用X射线荧光光谱(XRF)方法研究蛛丝和蚕丝的化学元素组成,探讨成丝机制中金属离子的作用及生物丝性能优良的元素基础。XRF分析蚕丝中C含量是47.10%、O为29.92%、N是16.52%;金属元素包括：Ca含量0.166 2%、Mg含量0.104 0%和K含量0.039 5%,而Na,Zn,Ni,Fe和Cr是微量元素。Ca和Mg元素含量高,在桑蚕吐丝机制中起着重要的作用。在蛛丝中,主要的非金属元素是：C含量44.09%、O含量26.64%和N含量22.34%。高含量的N元素可能是蛛丝优异的刚性和韧性性能的元素基础。在蛛丝中,Na含量0.268 0%、K含量0.081 4%和Mg含量0.011 6%,而Ca,Zn,Fe,Cu和Cr则是微量元素。蛛丝中Na和K元素含量高,在蜘蛛吐丝机制中可能起重要作用。运用数学统计方法研究生物丝元素组成与XRF元素分析结果吻合。     

河南宝丰和新郑出土硅酸盐制品的无损分析研究

无损分析是文物样品研究的重要内容,研究中采用便携式能量色散型X射线荧光光谱仪(pXRF)和激光拉曼光谱仪(LRS),对河南宝丰和新郑出土的21件战国晚期到汉代的硅酸盐制品进行了化学成分分析和微区物相分析。依据化学成分分析结果,将样品划分为铅钡硅酸盐玻璃、钾硅酸盐玻璃、釉砂和铅钡釉砂四类分别进行讨论,并对样品的着色机理进行了初步探讨;利用激光拉曼光谱在部分蜻蜓眼和圆环珠蓝色颜料中检测到了中国蓝(BaCuSi₄O₁₀)、中国紫(BaCuSi₂O₆)和中国深蓝(BaCu₂Si₂O₇),同时成功确定了部分样品中存在石英、方解石、碳酸铅、煅棕土、绿土等多种物相;结合考古研究资料,对这些样品的来源进行了简要讨论,其中本实验铅钡硅酸盐玻璃、钾硅酸盐玻璃耳珰和铅钡釉砂为我国自制,而另外1件釉砂可能属于舶来品,反映了我国古代中原各地区间,以及中原与西域间有着广泛的文化技术交流。便携式能量色散型X射线荧光光谱仪和激光拉曼光谱仪的相互结合,能够提供硅酸盐制品的有效化学成分和结构信息,在文物科学分析中显示出特有的优势,为其考古研究提供有益的信息。     

薄膜特性的掠发射X射线荧光分析

掠射X射线荧光分析技术是实验室分析薄膜特性的一种重要工具。文章简述了利用掠出射X射线荧光技术分析薄膜厚度的原理和方法,介绍了一种可在实验室里实现薄膜特性测试的掠发射X射线荧光分析装置,该装置采用波长色散方式结合超薄窗流气正比计数管,可实现对轻元素的探测。最后从理论上计算了Si片上不同厚度的几种单层薄膜的X射线荧光强度和掠出射角的依赖关系。证明了掠发射X射线荧光分析是一种精确的分析薄膜厚度等特性的方法。