A seven-crystal spectrometer for high-energy resolution X-ray spectroscopy at Shanghai Synchrotron Radiation Facility

A Johann-type X-ray spectrometer was successfully developed at the hard X-ray branch(in-vacuum undulator with a 24-mm periodic length)of the energy material beamline(E-line)at the Shanghai Synchrotron Radiation Facility(SSRF).This spectrometer was utilized to implement X-ray emission spectroscopy(XES),high-energy resolution fluorescence-detected X-ray absorption spectroscopy(HERFD-XAS),and resonant inelastic X-ray scattering.Seven spherically bent crystals were positioned on the respective vertical 500-mm-diameter Rowland circles,adopting an area detector to increase the solid angle to 1.75%of 4πsr,facilitating the study of low-concentrate systems under complex reaction conditions.Operated under the atmosphere pressure,the spectrometer covers the energy region from 3.5 to 18 keV,with the Bragg angle ranging from 73°to 86°during vertical scanning.It offers a promised energy resolution of sub-eV(XES)and super-eV(HERFD-XAS).Generally,these comprehensive core-level spectroscopy methods based on hard X-rays at the E-line with an extremely high photon flux can meet the crucial requirements of a green energy strategy.Moreover,they provide substantial support for scientific advances in fundamental research.

Accuracy analysis of iron content of galvanized coating using an X-ray fluorescence spectrometer with an L-spectrum

The accuracy(repeatability and reproducibility) of the iron content analysis of galvanized coating using an X-ray fluorescence spectrometer with an L-spectrum is not better than that of flame atomic absorption spectrometry, sometimes it exceeds the quality control limit.Influences, such as current, voltage, equipment(internal circulating water, 10%CH4+90%Ar, and vacuum) checking, instrument monitoring, sample cleaning, and oper-ators, were investigated by means of 6-sigma and lean operations to improve accuracy.

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.

Potential Applications of X-ray Fluorescence Core Scanner in Elemental Analyses of the Muddy Sediments on the Coastal Shelves of China and in Ecological Study

Large areas of muddy sediments on the coastal shelves of China provide important samples for studying climate and ecological changes. Analysis of a large number of such samples, which is essential for systematic study on environmental information recorded in mud areas because of complicated sedimentary environment and variable sedimentary rate, requires a fast and economical method. In this study, we investigated the potential of X-ray fluorescence core scanner （XRFS）, a fast analytical instrument for measuring the elemental concentrations of muddy sediments, and observed a significant correlation between the element concentrations of muddy sediments determined by regular X-ray fluorescence spectrometer （XRF） and XRFS, respectively. The correlations are mainly determined by excitation energy of elements, but also influenced by solubility of element ions. Furthermore, we found a striking link between A1 concentrations and marine-originated organic carbon （MOC）, a proxy of marine primary productivity. This indicates that MOC is partly controlled by sedimentary characteristics. Therefore, XRFS method has a good potential in fast analysis of a large number of muddy sediment samples, and it can also be used to calibrate MOC in ecological study of coastal seas.

Application of a Portable XRF Spectrometer for <i>In-Situ</i>and Nondestructive Investigation of Pigments in Two 15th Century Icons

A simple portable X-Ray Fluorescence (XRF) spectrometer was successfully used for in-situ and nondestructive identification of the painting materials in two 15th century icons from the Onufri Museum in Beart, Albania. The spectrometer is based on a low power X-ray tube, a thermoelectrically cooled Si PIN detector and the spectrum acquisition system. It was assembled and adjusted at our laboratory for the investigation of the icons. A small number of pigments were clearly identified by X-Ray Fluorescence (XRF) measurements in both icons. This includes Lead white for the white color, gold and yellow ochre for the yellow color, red lead, cinnabar and red ochre for the red color, as well as cooper based pigments for the green color. At the same time, the investigation raised some new questions that need further investigations by the use of additional analytical techniques. The results show that in both icons are used similar pigments, which are in accordance with the Byzantine icon painting tradition.

Use of sampling based correction for non-radioactivity X-ray energy calibration

As the requirement of non-radioactivity measurement has increased in recent years,various energy cali- bration methods applied in portable X-ray fluorescence (XRF) spectrometers have been developed. In this paper,a sampling based correction energy calibration has been discussed. In this method both history information and current state of the instrument are considered and relative high precision and reliability can be obtained.

能量色散X射线荧光光谱仪在镁砂成分测定中的应用

能量色散X射线荧光光谱仪(X射线能谱仪)具有体积小、价格低、分析速度快等优点而被广泛应用于高分子、陶瓷、混凝土、生物等材料的成分和形态分析,但是在耐火材料行业没有相关方法标准的规定。为了实现X射线能谱仪对镁砂中SiO_(2)、Al_(2)O_(3)、Fe_(2)O_(3)、TiO_(2)、CaO、MgO含量的快速分析,通过优化仪器参数,优选样片制备方法,进行精密度和准确度试验,能谱法和波谱法比对试验。结果表明:以熔铸玻璃片法制取样片,采用X射线能谱仪,可以快速测试镁砂样品中SiO_(2)、Al_(2)O_(3)、Fe_(2)O_(3)、TiO_(2)、CaO、MgO的含量,其相对标准偏差为0.09%~1.85%,具有满意的精密度和准确度。能谱法与波谱法的检测差值满足现用标准GB/T 21114—2019规定的允许差要求,数据可靠。

便携式单波长激发能量色散X射线荧光光谱法在土壤重金属速测中的应用

应用便携式单波长激发能量色散X射线荧光光谱(SW-PXRF)法测定国家土壤标准物质(GSS-1a~GSS-8a)及安徽铜陵农田重金属污染土壤中Cr、Ni、Cu、Zn、Pb、As和Cd 7种元素的含量,将农田污染土样的测试结果与电感耦合等离子体质谱(ICP-MS)法进行对比,分析该方法对各元素的检出限、精密度及准确度。进一步探究土壤含水量和粒径对测定结果的影响,并通过实验确定现场测试时的最佳前处理条件。结果表明:SW-PXRF法对土壤中各元素检出限均低于1.3 mg/kg,其中Cd的检出限可低至0.07 mg/kg。除Cd的精密度略差外,其余元素相对标准偏差基本小于5%。除As和Cd外,其余元素相对误差的平均值均可控制在-10%~10%。SW-PXRF法与ICP-MS法的测定结果相关性较好,除Cr、Ni外,其余元素决定系数均高于0.95。土壤含水量和粒径对测定结果存在一定影响,现场测试时只要将土样在200℃下烘干6 min并研磨60 s,就能在最短时间内削弱含水量和粒径的影响。

紧凑型Si-PIN探测器的低温制冷控制电路设计

针对便携式X荧光光谱仪,设计了紧凑型Si-PIN探头低温控制电路。低温制冷器采用微型半导体电制冷片,其恒流控制电路利用低噪声的线性稳压器来避免引入电子学噪声,并利用闭环控制保证温度的稳定性。前级供电采用高效率的DC-DC电路稳压,以降低探测器的整体热耗散。Si-PIN探测器安装在制冷片的陶瓷电路板上,并真空封装在TO-8管座内来维持低温制冷效果。实验测试结果表明,探测器可稳定保持在-35℃的低温工作环境,对59.5 keV能量获得的能量分辨率从常温下的2.70%提高到1.47%。

石油焦中微量元素含量的测定

采用能量色散X射线荧光光谱仪建立石油焦中微量元素含量的快速测定方法。考察制样方式、基质影响、定量曲线拟合方式等因素对测定结果的影响。石油焦中高含量的硫元素是最大的基质干扰因素,采用基本参数法和α经验系数法均可较好地进行基质校正,使所建方法可以在10 min内准确测定石油焦中S,Fe,Ni,V,Ca元素的含量。该方法对于各元素的定量曲线在相应的测试范围中均具有良好的线性相关性,决定系数R 2大于0.99。该方法对于S元素质量分数的定量限为0.040%,对于Fe,Ni,V,Ca元素质量分数的定量限分别为5.4,1.4,2.1,2.8μg g。

车载台式能量色散X射线荧光光谱仪在地球化学勘查现场分析中的应用

充分发挥小型实验室设备的功能以提高现场快速分析的能力。在内蒙和新疆两地覆盖区的钻探现场,采用车载化台式偏振能量色散X射线荧光光谱仪,对由轻便钻采集的覆盖层和基岩样品进行了贱金属分析。共采集、制备和分析了约400件钻探样品,采用能量色散X射线荧光光谱法、波长色散X射线荧光光谱法和电感耦合等离子体质谱法对这些样品进行比对分析。现场分析数据与实验室分析数据(各方法的平均值)的比对结果表明,K、Ca、Ti、V、Cr、Mn、Fe、Ni、Cu、Zn、Ga、As、Rb、Sr、Y、Zr、Nb、Ba、Pb、Th等20余种元素的分析数据的一致性良好;含量超过10μg/g时,除了V和Ba外,其他元素的平均相对偏差均小于25%。在现场作为质控样品分析4个地质标准物质GBW07301～GBW07304,测定结果表明,除了低含量的Cu和Ga外,上述其他18种元素均符合地质行业标准地质矿产实验室测试质量管理规范(1∶20万)规定的误差要求。应用研究表明,设计的仪器车载化方案可行,现场分析方法快速、准确,适用于野外钻探、化探等急需现场数据支持的工作。

高能偏振能量色散-X射线荧光光谱法测定PM_(10)大气颗粒物的组成

为配合X射线衍射分析(XRD)方法对可吸入大气颗粒悬浮物(PM10)的结晶物相进行定性和定量分析的研究工作,本文应用高能偏振能量色散X射线荧光光谱(HE-P-EDXRF)对Whatman玻璃纤维滤膜采集的PM10颗粒物中主、次量元素进行定量分析,着重研究了空气滤膜空白值对测定PM10颗粒物中组成的影响。结果表明,当玻璃纤维滤膜空白值中元素的面密度大于0.1μg/cm2时,需使用玻璃纤维滤膜为载体的标准样品;元素的面密度小于0.1μg/cm2时,可用聚碳酸脂膜为载体的标准样品。对HE-P-EDXRF谱仪测定PM10颗粒物中痕量重元素进行探讨,将测定元素范围扩展到62个元素,其中Na、Mg、S、Y、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu的检岀限>0.1μg/cm2;Ca、Cr、Mn、Fe、Co、Ni、Cu、Zn、Br和Rb的检岀限<0.01μg/cm2;Cl、Al、Si、P、K、Sc、Ti、V、Ge、As、Br、Se、Sr、Zr、Mo、Pd、Rh、In、Nb、Ag、Cd、Te、Sb、Sn、Ba、Cs、La、Ce、Pr、Au、Pt、W、Tl、Pb、Bi、Th和U等元素检出限为0.1～0.01μg/cm2。

Minipal4便携式能量色散X射线荧光光谱仪在勘查地球化学中的应用

使用粉末样品压片制样,用Minipal 4便携式能量色散X射线荧光光谱仪测定化探样品中的Na2O、MgO、Al2O3、SiO2、CaO、Fe2O3、K2O、As、Ba、Br、Ce、Co、Cr、Cu、Ga、La、Mn、Nb、Ni、P、Pb、Rb、Sr、Th、V、Y、Zn、Zr、Ti、Mo等30种组分。方法简便、快速,分析结果的精度和准确度能满足野外现场分析的要求。

X荧光光谱仪在实验室-调查船测定海洋沉积物元素的对比研究

运用Epsilon3系列小型能量色散X射线荧光光谱仪,选取水系沉积物、海洋沉积物等标准物质31个,采用压片法制样,建立了该仪器对海洋沉积物中34种元素定量测试的分析方法,该方法检出限低,精密度高,准确性好。在海上调查期间运用该仪器与方法,对深海沉积物样品进行了现场测试,调查船上的测定值与陆上实验室内的测定值基本一致,两者平均相对偏差基本小于10%,结果表明运用该分析方法,Epsilon3系列小型能量色散X射线荧光光谱仪能快速、准确测定沉积物中多种元素,为及时判断现场资源分布情况提供依据,减少取样的盲目性,这将为我国海洋地质调查工作提供新的技术支持。

X射线荧光光谱仪在RoHS分析上的应用

介绍欧盟的RoHS/WEEE/ELV/EuP指令,综述X射线荧光法在检测RoHS成分上的应用现状,比较能量色散仪与波长色散仪的特点,讨论几项先进技术在能量色散X荧光光谱仪上的应用。

能量色散X射线荧光光谱仪和简化的基体效应校正模型测定土壤、沉积物中重金属元素

用于测定土壤、沉积物样品中无机元素的波长色散X射线荧光光谱法(WD-XRF)基体效应校正经验模型中,通常需要Mg、Al、Si、Ti、K、Fe、Ca等常量元素测定结果。针对能量色散X射线荧光光谱法(ED-XRF)应用方案,如果能将参与基体效应校正的元素个数压缩,不考虑Mg、Al、Si等轻元素,其分析成本和时间将明显得到优化。实验探讨了简化基体效应校正模型的可能性。基于康普顿散射和简化的基体效应校正模型,建立了土壤、沉积物样品中As、Cr、Cu、Ni、Pb、Zn、Mn、V等重金属元素的ED-XRF测定方法。用5个土壤、9个沉积物标样认定值和3个土壤考核样品WD-XRF测定结果为基准,以HJ 780—2015质控要求为依据,评估了方法的准确度和精密度。目标元素分析结果准确度合格率94.1%~100%,精密度合格率100%。基于经典的背景计数法和重复测定法评估了方法检出限。各项实验结果表明,ED-XRF可用于土壤重金属污染状况详查检测实验室质控工作。

高能偏振能量色散X射线荧光光谱仪应用现状和进展

对高能偏振能量色散X射线荧光光谱仪基本特点及其用于环境、生物、地质样品中痕量元素的分析和RoSH检测等领域的应用现状予以介绍,并对二次靶与滤光片在痕量元素分析中的应用作了探讨。

便携式能量色散X射线荧光光谱仪在新疆东天山浅钻化探异常查证中的应用

便携式能量色散X射线荧光光谱仪(EDXRF)具有大型XRF光谱仪的分析性能,在矿产资源勘查中具有广阔的应用前景,特别是在勘查难度大、找矿工作周期长的覆盖区的现场快速分析具有重要意义,但在野外快速分析方面亟需进一步开发。本文采用手工压制样片,建立了Minipal 4便携式能量色散XRF光谱仪现场测定新疆东天山浅覆盖区浅钻化探样品中的铜铅锌砷钴镍锰7种元素的野外快速分析方法,各元素的检出限分别为2、2、1.5、2、2、2、6μg/g,精密度(RSD,n=12)小于4.7%。本方法能在浅覆盖区实施有效的地球化学样品分析,数据成图效果与实验室分析数据成图效果接近,可快速指导浅钻化探扫面和异常查证工作,缩短了工作周期,提高了矿产资源勘查效率。

偏振激发能量色散X射线荧光光谱仪在野外矿区现场实验室的应用探讨

为提高野外找矿人员工作效率,探索测试设备直接在野外现场服务地质找矿事业的问题,项目组在辽宁丹东野外Fe-Cu-Co矿区以集装箱改造房作为实验测试场所,以小型偏振激发能量色散X射线荧光光谱仪(P-EDXRF)为测试手段,配备相应的电力供应系统、碎样系统以及配套相应的野外测试方法和样品前处理方法,建立了可独立工作的野外现场分析实验室。利用该矿区两个样品,现场进行精密度实验,Fe、Cu、Co 3种元素相对标准偏差(RSD)都在6%以下;利用标准样品GBW07233、GBW07296、GBW07306进行正确度实验,3种元素相对误差在10%以下。将野外现场分析实验室测试数据与找矿单位提供的30件矿区样品中Fe、Cu、Co 3个元素的室内实验室测试数据进行比较,Fe、Cu符合度较高,可以进行定量测试,Co的测试效果相对较差,建议只提供半定量数据,但均可以对其异常区进行准确圈定。研究表明,该类型实验室可以在野外条件下独立承担多种元素的测试工作,达到快速圈定元素异常区的目的,为野外找矿工作发挥现场技术支撑作用。

能量色散X射线荧光光谱仪研究现状

归纳了能量色散X射线荧光(EDXRF)光谱仪的主要部件及能谱处理算法的研究进展及现状,通过分别对比不同类型高压电源、X射线激发源和探测器在光谱仪上的使用,总结了X射线激发电压、X射线强度和探测器分辨率等对仪器灵敏度和分辨率等指标的影响。通过分别对比不同算法在能谱去噪、本底扣除、谱峰分解及荧光强度提取等方面的应用,分析了各种算法的适用范围,并比较了小波变换、人工神经网络和偏最小二乘法等在能谱分析中的独特优势。阐述了为提高仪器性能亟待解决的问题,并指出了EDXRF仪器的发展趋势及进一步研究该课题的必要性。