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.

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.

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.

L-shell x-ray fluorescence relative intensities for elements with 62≤Z≤83 at 18 keV and 23 keV by synchrotron radiation

The relative intensities of L-subshell x-ray fluorescence(XRF)for elements with atomic numbers 62≤Z≤83 were measured at two excitation energies,18 keV and 23 keV,using a synchrotron radiation source at a beamline of the Synchrotron Light Center for Experimental Science and Applications in the Middle East(SESAME),Jordan.The experimentally measured results of the relative intensities were compared with the calculated results using the subshell fluorescence yield and the Coster-Kronig transition probabilities recommended by Campbell and the values based on the Dirac-Hartree-Slater model by Puri.The experimental and theoretical results are in agreement.In this work,L XRF relative intensities for the elements Sm,Gd,Tb,Er,Ta,W,Re,Hg,Pb and Bi at energies of 18 keV and 23 keV were measured.

X-RAY FLUORESCENCE SPECTRA ANALYSIS ON THE STRUCTURE AROUND Ti^(4+) OF BaO-SiO_2-B_2O_3-TiO_2 SYSTEM GLASSES

The structure around Ti^(4+) in Bao-SiO_2 -B_2O_3-TiO_2 had been studied by X-ray fluorescence spectra. The results show that the Ti^(4+) mainly exists in the [TiO_4] and enters the network of [SiO_4]. [TiO_4] has the tendency to change to [TiO_6] with the increase of TiO_2 con-tent. When the TiO_2 content increases to about 20mol% the tendency reaches its maximum.

手持式XRF在土壤调查修复项目中应用的可靠性分析

为确定手持式X射线荧光光谱仪(XRF)测量精度和准确度是否能够满足土壤环境快速检测要求,以山东省济宁市某地块土壤污染状况调查项目为背景,分别采用XRF快速检测仪检测和实验室检测方法对浅层土层(0.2~0.5 m)和深层土层(1.5~2.0 m)样品中砷(As)、铜(Cu)、铅(Pb)、锌(Zn)和镍(Ni)5种元素浓度进行检测。结果表明:浅层土层重金属As的XRF检测值普遍高于实验室检测值,Cu、Pb、Zn、Ni的XRF检测值普遍低于实验室检测值,误差普遍在±30%以内;浅层土层的重金属元素XRF检测值与实验室检测值普遍相对偏差(RD为−33.82%~23.53%)及总体相对偏差标准差(6.79~19.52)小于深层土层(分别为−30.26%~98.36%、9.53~49.77),相对偏差的离散程度小于深层土层;浅层土层的重金属的决定系数(R^(2)为0.7762~0.9549)普遍高于深层土层(R^(2)为0.7762~0.9549),相关性高于深层土层。野外使用XRF对土壤样品中重金属进行检测时,所取的土壤样品尽量避免大颗粒,对样品待测面进行压实、压平处理,对于含水率高的样品应适当进行干燥处理,以降低检测误差。虽然手持式XRF检测存在一定误差,但在土壤污染状况调查项目中可以较好地反映土壤元素浓度范围,具有较高的可靠性,可以满足项目土壤快速检测需求。

Soil Clay Mineralogical Phase Analysis of Ganges Floodplain Soils by XRD and XRF

Soil minerals study is vital in terms of investigating the major soil forming compounds and to find out the fate of minor and trace elements in soils. It is also essential for the soil-plant interaction purpose. To identify soil mineral phases especially clay minerals, X-ray diffraction (XRD) has been a popular technique. The clay mineralogical information of soils in Bangladesh is limited, especially in Ganges flood plain region (Agro Ecological Zone (AEZ) 12 and 13). Therefore, to overcome this limitation, in this study, we performed XRD analysis of <2 mm fractions soil samples of AEX 12 and 13. However, identifying mineralogical phases by XRD in <2 mm fractions soils is not so straight-forward due to many practical problems. We fully matched only two mineralogical phases in all the soil samples which is quartz and potassium-Aluminum-Silicate. However, the full XRD peaks indicate that more minerals are also present, but due to heterogeneity of soils samples, it is difficult to find other minerals phases by only XRD peak of <2 mm fractions. Therefore, to find more information about mineralogical phases, we performed XRF analysis that provides the elemental composition of minerals phase as oxide. XRF analysis indicated the presence of secondary minerals like illite and chlorite. The presence of high percentage Fe oxide not only indicated the iron mineral phase (goethite and ferrihydrite) but also indicated iron rich high charge smectite minerals (beidellite). The presence of iron rich smectite minerals in the Ganges sediments reported in several previous studies. Thus, we concluded that only XRD in <2 mm fractions of soils is not adequate to identify the mineralogical phases of soil samples. Others analyses like XRF, XRD in <2 μm fractions will be necessary to locate an entire image of soil mineralogical phases.

XRF Standardless Comparison of Mining Head and Tail Grades to Screen and Display Ore Processing Recoveries

Separation of target elements or minerals from their host rock or ore is essential to successful mining operation. The inevitable loss of a portion of the desired material that accompanies each step in the extraction process must be documented to develop the operational protocol. Superposition of the characteristic X-ray fluorescence spectra of head (crushed rock ore particles, pre-processing) and tail (post-processing particles) samples provides a direct visual comparison of relative peak sizes, and thereby the relative concentrations, of elements of interest. If the head and tail peaks are identical, none of the element was recovered in the extraction process. At the other extreme if the tail peak “flat lines”, i.e., there is no peak, there was 100% recovery of that element. Standardless visual comparison is valid if the same mass of identical starting material is incorporated into the head and tail sample analysis pucks, and XRF analytical conditions are identical. The considerable time and expense of acquiring and calibrating the standards associated with XRF analysis of 75 or more elements are avoided, a significant advantage during initial broad screening of an experimental extraction procedure. Full quantitation by XRF or an alternate technique can proceed at a later project stage, if desired. The approach retains and presents all features of the original data, thus eliminating questions about data quality, standards and their calibration, and data manipulation in processing from raw counts to concentrations in printout tables. This form of display is ideal for both the mining professional and such less technical groups as corporate staff, investors, regulators, and the public. Examples presented herein are for heap leaching;the protocol can be applied as well to any of the other traditional ore processing and beneficiation procedures, e.g., gravity concentration, magnetic and electrical separation, froth flotation, and ore sorting.

垂直电镀挂具对TO封装陶瓷外壳表面镀镍层厚度均匀性的影响

针对封装陶瓷外壳表面镀层厚度均匀性方面的重要性,利用定制的TO封装陶瓷外壳垂直电镀专用挂具,通过电沉积的方式在TO封装陶瓷外壳的表面电镀镍层。利用X射线荧光(XRF)光谱仪测量研究了TO封装陶瓷外壳相对阳极所在平面与阳极平面间的夹角(θ)对镀镍层厚度均匀性的影响。结果表明,当θ为30°时,在键合指与引线端表面电镀镍层能够实现较好的均匀性,此时的镀层厚度变异系数为24.42%,相比θ为0°和45°时,明显降低了镀镍层厚度的波动范围,有效提升了镀镍层厚度的均匀性。

X射线荧光光谱法对硅砂中主要成分的检测

建立了一种对硅砂中成分进行快速测定的方法。样品经过碳化钨的研磨,制成能通过200目(筛孔径0.075 mm)标准筛的粉末,经1000℃灼烧2 h,去除里面含有的碳以及有机物。按照特定的比例在1050℃的高频熔样炉中制成玻璃片。标准物质采用日本耐火材料技术协会系列标准物质,按照说明书800℃灼烧后,按照和样品同样的熔样方法制作玻璃标片,在XRF光谱仪中选定待测元素的2θ角以及PHD能级范围,进行测定。标准曲线制作完毕后,用国家标准物质进行检测,经检测,该方法检测精确度高,误差小,能够满足化学分析的要求,结果令人满意。该方法适用于硅质砂岩以及铸造用砂。

多通道波长色散X射线荧光光谱仪的升级改造

采用面向对象、开放式、功能模块化结构设计原理及X射线荧光光谱分析数据处理和信息共享等方面的新技术,研究开发了多通道波长色散X射线荧光光谱仪仪器控制和分析应用软件,在中文Windows XP/2000平台运行。操作界面全部中文显示,具有定量、半定量、定性分析等多种X射线荧光光谱分析的整体解决方案,功能完善,操作方便,分析效率高,易于维护和移植,具有较好的推广应用前景。

微束X射线荧光光谱仪测定射击残留物特征元素分布图的应用研究

通过优化定距射击样本采集条件,考察了六四手枪在不同距离(0,2,5,10,15,20,25,30,35,40,45,50,60,80,100,120,140,170,200,300,500,1 000 cm)垂直射击PU布块靶体时相关元素(氯、钾、硫、锑、锡、钡、铅、汞、砷、铁、铜、锌、钛、钙、铑)的区域扫描图,建立了微束X射线荧光光谱(μ-XRF)面扫描技术分析射击样本的方法,并建立了六四手枪射击残留物特征元素分布图形随射击距离而变化的数据模型,同时对所得数据进行了归一化处理。本方法可协助推断射击距离,为涉枪案件的侦查与诉讼提供科学证据。

蒙古国东南部钨多金属靶区的快速圈定与成矿分析

复杂地表条件下矿产勘探一直是个难题,国外区块更是如此,首次利用XLT-592WZ型便携式XRF分析仪在蒙古国苏赫巴托尔省(额尔德尼查干苏木)13451X草原覆盖地区系统采集数据,分析研究并圈定成矿靶区。初期利用X荧光仪进行扫面勘探,发现有W、As、Pb、Zn、Cu、Fe等元素异常,经过异常查证优选了一个钨多金属找矿远景区。在钨多金属找矿远景区内通过23条探槽和钻探工程进一步揭露发现一条黑钨矿体;钨矿主要以脉状、团块状或是角砾状形式出现,成矿围岩为花岗斑岩,矿石以黑钨矿为主,白钨矿极少,可见硅化、萤石,推测该区成矿类型为高温热液型黑钨矿。综合来看,在野外利用便携式X荧光光谱仪进行定性与半定量分析是有效的,该方法可在同类地区推广应用。

X射线荧光光谱仪及其分析技术的发展

按照获得和分辨特征X射线荧光光谱的方式,X射线荧光光谱仪可以分为波长色散X射线荧光光谱仪(WDXRF)和能量色散X射线荧光光谱仪(EDXRF)两大类。依照这一分类,论述了X射线荧光光谱仪在设备装置和配套方法方面的新状况。X射线荧光光谱仪整机现在向着小型化、智能化、多功能方面发展,仪器各部件也随着研究的深入而得到了更进一步地改进,在这一基础上,仪器可分析元素的含量范围得到了拓展,方法也得到了丰富。目前,X荧光光谱仪开发了微区面分布的元素成像分析方法、高级次谱线分析方法、薄膜分析方法等新的方法,对这些新方法作以介绍,同时也对基本参数法(FP法)的新近发展作了说明。

手持式X-射线荧光光谱仪在金属材料检测中的应用

系统评述手持式X-射线荧光光谱仪的发展过程,详细比较、分析其辐射情况,探讨金属材料状态对检测的影响。综合基本参数法、自动选择模式测试金属材料的数据,提取检测结果,与认定值或其他方法的分析结果基本吻合。

Suitability of Some Selected Clay Deposit from Edo, Ogun, Ondo and Ekiti State of Nigeria for Ceramic Water Filters Production

This study is designed to investigate the suitability of selected Nigeria clay deposit for clay based ceramic water filters (CWFs). Clay samples were taken from five randomly selected locations in Nigeria Namely: Okpella (Edo1) and Ojirami (Edo2) in Edo;Ikere in Ekiti state;FUTA in Ondo state and Onibode in Ogun to determine their suitability for clay based ceramic water filters (CWFs). Experimental analysis for linear shrinkage, water absorption, bulk density, compressive strength X-ray diffraction (XRD) and X-ray Fluorescence (XRF) was carried out on each of the clay samples. Test results reveal that all the clays contain high contents of alumina (Al2O3) and silica (SiO2) with minor contents of P2O5, Fe2O3, MgO, K2O, MnO and TiO2. The average crystal sizes of the clay were between 15 and 27 nm. Lattice structure indicates that the sample is Monoclinic and Anorthic. Ceramic water filters (CWFs) were made from a mixture of clay and sawdust at different volume ratios, and processed into test samples. Water absorption, linear shrinkage and compressive strength of the clay based ceramic filters (CWFs), reveal that as the volume ratio of sawdust increases these properties decrease. Flow rate analysis indicates that Edo and Ekiti ceramic water filters (CWFs) have higher flow rates. The research indicates that Edo and Ekiti Clay with specification of some industrial clays shows that the samples can be recommended for use in clay based ceramic water filters production.

Palaeodiet of Miocene Producers and Depositional Environments:Inferences from the First Evidence of Microcoprolites from India

This paper reviews research on coprolites from India,providing the first evidence of microcoprolites from the early Miocene(Aquitanian)Khari Nadi Formation sedimentary succession,exposed about 1.5 km northeast of the village of Kotada,Kachchh(Kutch)District,Gujarat State,western India.Morphometric and size comparisons(in a statistical framework)with known coprolites from the Mesozoic-Cenozoic successions of India(including those recorded herein)and globally suggest that fishes were the likely producers of the Kotada coprolites.Scanning electron microscopy confirms the presence of fish dental remains within the coprolites,while both Scanning Electron Microscopy(SEM)and Energy Dispersive X-ray Spectroscopy(EDS)reveal the phosphatic nature of the microscopic coprolite specimens(recorded herein)hinting that the producer(s)were predominantly carnivorous(ichthyophagous)in their diet.Furthermore,X-Ray Fluorescence(XRF)analysis of the host and associated lithologies allows us to deduce that the Kotada coprolites were deposited in a shallow marine environment,with possible aerial exposure of the host lithology occurring at some point after deposition.To the best of our knowledge,the present report is the first record of microscopic fish coprolites from India,as well as being the first from the Aquitanian of India and the oldest Neogene record from India.

福建紫金山铜金矿床铜矿体中As元素分布规律及其在配矿中的应用研究

通过光学显微镜、电子探针和手持式X射线荧光光谱分析仪(p-XRF)等方法对紫金山铜金矿床的铜矿体中As元素的赋存状态和分布特征进行了研究。结果表明,矿石中As元素主要赋存于含As的铜矿物,且与其他铜矿物共生,极少以单独相产出;少量As元素以类质同象赋存于蓝辉铜矿、铜蓝、黄铜矿和黄铁矿等矿物中;As元素在选矿过程中难以单独选别,造成铜精矿中As含量普遍超标。为了降低铜精矿中As元素含量,采用手持式X射线荧光光谱分析仪对钻孔副样进行分析,建立As/Cu比值的三维模型,划分矿石类型,进行科学配矿,有效减少浮选精矿中的As元素含量,提高经济效益。研究成果可为同类型矿山的配矿提供参考。

长江三角洲平原湖沼沉积物XRF岩芯扫描结果的可靠性分析

对长江三角洲顶部湖沼相沉积为主的XJ02孔(32°19′57″N,119°16′22″E)进行XRF全岩芯扫描(XRF-cps)分析,同时选取70个样品利用X射线荧光光谱仪(XRF-ppm)进行元素含量测定。通过对两种测试方法所获结果的对比及相关性分析,探讨了XRF岩芯扫描方法测定元素含量的可靠性及其影响因素。结果表明:两种方法所测得的6种元素Ti,Zn,Rb,Sr,Fe和Ca的相关系数很高,XRF扫描强度变化可以很好地反映其含量的变化;XRF扫描强度受含水量的影响,尤其对原子量较小的元素Si等影响比较明显;对于含量较低的元素P和Pb,XRF扫描强度不能真实的反映沉积物中的元素含量。