波长色散X射线荧光光谱仪的检定

介绍波长色散X射线荧光光谱仪的检定方法。以ZSX PrimusⅡ型波长色散X射线荧光光谱仪为实例,对仪器性能测试和计量检定流程进行了详细说明。波长色散X射线荧光光谱仪的总不确定度分别由精密度测量不确定度,稳定性测量不确定度,X射线计数率测量不确定度,检测器能量分辨率不确定度,仪器计数线性的不确定度组成。对仪器的各不确定度分量进行评定。在置信水平95%,扩展因子为k=2的条件下,计算得此波长色散X射线荧光光谱仪的标准扩展不确定度为1.45 kcps。该方法为检定该类仪器和计量标准的考核提供了参考。     

发射光谱仪检定规程的探讨和应用

《发射光谱仪检定规程》是计量部门检定/校准电感耦合等离子体发射光谱仪、直读光谱仪及摄谱仪的重要依据,对规程进行了探讨,包括检定前的准备、测量数据的判断、标准物质的选择及计量性能的要求,提出了直读光谱仪应用于其它非冶金材料时的计量性能指标,如铜及铜合金、铝及铝合金、锌及锌合金等的成分分析。发射光谱仪检定规程也可以应用于油液分析用原子发射光谱仪、辉光放电发射光谱仪、金属原位分析仪、手持式合金分析仪、激光诱导击穿光谱仪等仪器的检定/校准,可作为计量人员的参考依据。     

X-射线荧光光谱分析技术的发展

归纳了X-射线荧光光谱分析技术发展的进程。从现代控制技术的改善、仪器检测性能的提高、元素检测范围的扩大等8方面阐述了波长色散X-射线荧光光谱技术的进展,还就能量色散X-射线荧光光谱仪的X射线管和探测器技术的快速发展及近10年来我国在X-射线荧光光谱分析方法方面的论文发表情况进行了总结,对近年来X-射线荧光光谱仪的发展趋势———手持式、偏振、微束分析等进行了评述,并对其技术的发展方向进行了展望。     

能量色散X射线荧光光谱评议报告

管激发X射线荧光光谱仪大致分为二类:一类为波长色散X射线荧光光谱仪(以下简称WDXRF或TWDXRF);另一类为能量色散X射线荧光光谱仪(以下简称EDXRF或TEDXRF)。WDXRF产生于50年代,经历了几十年的发展,现已逐步完善。最新生产的WDXRF谱仪可测元素从硼到铀,测定轻     

能量色散偏振X射线荧光光谱法测定生铁中锰和钛

探讨了应用能量色散偏振X射线荧光光谱仪测定生铁中锰和钛进行炉前快速分析的方法.对测定锰及钛时仪器的工作条件,试样的制备以及工作曲线的制作等因素作了较系统的试验,该方法所得测定结果与化学法测定结果或标样标准值相吻合,相对标准偏差小于1.5%,与化学法相比,锰和钛的测定时间由50 min缩短到2 min.     

X荧光光谱技术在油品硫分析中的应用

选择校正曲线法定量，在能量色散X荧光光谱仪上建立汽油、柴油和重油中硫分析方法。方法重复性、再现性符合国家标准要求，分析效率高。     

能量色散X射线光谱分析

本文介绍能量色散X射线荧光光谱分析的基本原理、仪器特征、Si(Li)探测器特性以及它的多种应用等。文中着重对能量色散与波长色散技术的不同特点进行了比较,并讨论了能量色散方法所具有的优点和它的适用范围。     

RoHS检测用X荧光光谱仪校准方法的初探

对RoHS检测用X荧光光谱仪提出了计量性能要求及校准方法,并验证了方法的可行性,为今后规程的制定提供参考。     

能量色散型X荧光分析仪测定生铁样品

目前 ,国内钢铁企业生铁样品分析大多采用传统的化学分析方法 ,分析速度慢 ,难以满足生产需要 ,部分企业采用进口的波长色散型X荧光分析仪 ,但因其价格昂贵 ,很多企业难以接受。而采用能量色散型X荧光分析仪 (简称EDXRF)测定生铁样品 ,国内还未见报道。本文试验了国产X荧光仪分析生铁样品的方法 ,成功地应用于炼铁化验室生产分析 ,为国内炼铁化验手段的更新换代作了有益的探索。1　试验部分1.1　仪器及性能WISDOM 80 0 0型能量色散X荧光分析仪 (上海精谱仪器有限公司 )分析范围 :同时分析元素周期表中由钠到铀之间的全部元素。高压发…     

一种快速半定量检测烟花爆竹用烟火药盲样中汞含量的方法

本发明公开一种快速半定量检测烟花爆竹用烟火药盲样中汞含量的方法,属于分析测试技术领域。将烟火药样品从烟花爆竹产品中解剖出来,研磨,过筛,干燥,冷却至室温,以能量色散型X射线荧光光谱仪为检测仪器,采用强度法建立分析方法,将样品装入仪器样品杯中,再将待测样品置于检测仪器测试舱内,记录仪器上显示的汞元素特征谱线的荧光强度值,估算汞元素在样品中的含量,再进一步选择适当的分析仪器准确定量分析烟花爆竹用烟火药中的汞含量。本发明方法操作简单,效率高,所估算样品中的汞含量与其实际含量相差较小,且能为进一步选择准确定量分析样品中汞含量的方法提供依据。     

Soil characterization by energy dispersive X-ray fluorescence: sampling strategy for in situ analysis.

This work describes a sampling strategy that will allow the use of portable EDXRF (energy dispersive X-ray fluorescence) instruments for "in situ" soil analysis. The methodology covers a general approach to planning field investigations for any type of environmental studies and it was applied for a soil characterization study in the zone of Campana, Argentina, by evaluating data coming from an EDXRF spectrometer with a radioisotope excitation source. Simulating non-treated sampled as "in situ" samples and a soil characterization for Campana area was intended. "In situ" EDXRF methodology is a powerful analytical modality with the advantage of providing data immediately, allowing a fast general screening of the soil composition.     

Particle analysis for a strengthened safeguards system: Use of a scanning electron microscope equipped with EDXRF and WDXRF spectrometers

The purpose of this study was twofold: the identification of some uranium compounds and a measurement of mixed U/Pu particles with different ratios of these elements. We used a Philips XL-30 scanning electron microscope equipped with an EDAX energy dispersive spectrometer with a Si(Li) detector and a super ultra-thin polymer window and with a Microspec wavelength dispersive spectrometer. A number of WDXRF and EDXRF spectra of U and Pu containing particles were accumulated and evaluated. The software package provided by the manufacturer was used for EDXRF spectra evaluation and calculation of the weight and atomic composition. Eight different U compounds were identified with a different degree of confidence. Several different types of U and Pu particles were measured using the WDXRF spectrometer and the results of the measurements are discussed. The measurement of mixed U-Pu particles showing large differences in the concentration of both elements can best be carried out with the use of WDXRF because the deconvolution of the M lines of U and Pu in the energy dispersive spectra is only possible over a relatively small concentration range. The results of particle analysis are very useful for verifying the absence of undeclared nuclear activities.     

Minimate EDXRF谱仪在水泥工业分析中的应用

Minimate EDXRF谱仪是由低功率X射线管、封闭式正比计数管和2048道分析器组成,可分析原子序数11以上的元素(其中钠和镁需通氦气).作者用该仪器分析了粉末状水泥中MgO、Al_2O_3、SiO_2、SO_3、K_2O、CaO和Fe_2O_3等组成,并对水泥生料的取样误差作了估计.结果表明,该仪器可满足水泥制品的控制分析.     

EDXRF analysis of some samples of cigarette paper

The effects of tobacco on human health have been widely investigated and documented However, there are not too many specific reports on the potential risk associated to the presence of metals in the paper employed for cigarettes fabrication Even more, there is a lack of national and international norms in this respect. Otherwise, in the literature INAA appears as the unique method for wrapping paper analysis. Therefore, without a nuclear reactor available at the National University of Mexico (UNAM), EDXRF was selected with the aim to explore the possibility to apply this method, instead of INAA, to the analysis of wrapping paper assuming this task, at the beginning, as a supplement to a previous research which was recently presented (2005).¹ The analytical work was developed on the wrapping paper of eight of the most known marks of cigarettes in Mexico, in two non-destructive stages: a first survey, by the classical technique of energy dispersive X-ray fluorescence (EDXRF), used a 1 11 GB qradiation source of ²³⁸Pu and a SiLi detector. In the absence of standard reference materials for cigarette’s paper, the SRM-1832 and 1833 were required for calibration, a fiberglass air filter was used as a secondary standard. The second stage was performed in a spectrometer TX-2000, anode of Mo, quantification software EDXRF32 (fundamental parameters). This paper presents a comparison of the obtained values with those found in the literature. The results show that the EDXRF method, in the Mo tube version, has the adequate precision and detection limits for the analysis of wrapping paper.     

Energy dispersive X-ray fluorescence as a tool in biomedical analysis

Summary The energy dispersive X-ray fluorescence spectrometer (EDXRF) developped together with the Siemens Company (FRG) allows to perform rapid multi-elemental analysis of biological fluids without pretreatment of the samples. The performance of this technique and its features are reported in two different fields: blood analysis and pulmonary investigations. Blood and plasma analysis were performed for more than 2500 patients and a statistical treatment of the data lead to the normal concentrations of trace elements Se, Rb, Cu, Zn, Fe, Ca, Br, K. Toxic elements such as Hg or Pb and also drugs like Au and Pt compounds can be detected even after a long period after treatment. To illustrate the performance of the spectrometer we report the influence of Cis-Pt treatment on the trace element concentrations in plasma of patients with anemia.The EDXRF spectrometry was also used to investigate the inorganic composition of the broncho-alveolar lavage fluids. After determination of the normal concentration range, it was possible to characterize some typical pulmonary diseases due to occupational exposure. Some examples of detected pneumoconiosis and for some patients the presence in the alveoli of elements due to special medication (Amiodarone, Aurothiopropanol-sulfonate) are mentioned.Other fields are being investigated such as: follow-up of Mn dependent enzymes in neuronal and glial cells in culture; origin of lead in dental tissues or composition of lyophilized food powders. They will be briefly discussed.

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Energie-dispersive Röntgenfluorescenz in der biomedizinischen Analyse

     

Integrated sorption–energy-dispersive X-ray fluorescence detection for automatic determination of lead and cadmium in low-concentration solutions

Sorbent material packed in a PTFE laboratory-made flow cell located in the specimen holder of an energy-dispersive X-ray fluorescence (EDXRF) detector has been used for in situ solid-phase extraction (SPE) preconcentration–detection of metals. The flow cell was connected to a single-channel flow-injection (FI) manifold (for full automation of the steps and proper development of the method) by two PTFE tubes of 0.5-mm inner diameter introduced into the spectrometer specimen holder by a small orifice without distortion or modification of the instrument. The optical window open in the PTFE flow cell was adjusted to the X-ray irradiation zone of the spectrometer and fixed to it. The approach was tested by using both Pb and Cd aqueous solutions and a Dowex 50 cation-exchange resin as a sorbent, and flushing the sample through the flow cell for EDXRF measurements after removal of the sample matrix. The limits of detection and the limits of quantification (LOQs) thus obtained were 0.15 and 0.5 μg for Pb and 0.3 and 0.8 μg for Cd, respectively, values that allow the approach to be used for the analysis of drinking water by injecting a 100-mL sample into the FI manifold, taking into account the EC drinking water directives. The linear dynamic ranges are between the LOQ and 600 μg for both analytes. The method was validated by the standard addition method using tap-water samples. In addition, the integrated SPE–EDXRF approach enables the study of the variables influencing the sorption step–namely the effects of the volume of sample flushed through the column, concentrations of the analytes in the sample, breakthrough volume of the resin, elution profiles, sample pH and retention and elution flow rates–in an automatic, cheap, fast and precise way.     

Standardless energy-dispersive X-ray fluorescence analysis using primary radiation monochromatized with LiF(200) crystal

Energy-dispersive X-ray fluorescence spectrometer (EDXRF) with primary radiation monochromatized by LiF(200) crystal was developed. In the constructed spectrometer, the radiation from the Ag target X-ray tube operated at 50 kV and 40 mA excites the secondary target (Cu, Se, Zr or Mo). The characteristic radiation (Cu K_α, Se K_α, Zr K_α or Mo K_α) of the target is monochromatized with LiF(200) crystal and excites elements in the analyzed sample. The X-ray spectra are collected by thermoelectrically cooled Si-PIN detector with resolution of 145 eV at 5.9 keV. The pinhole collimator placed in front of the X-ray detector allows reducing size of the analyzed area. Quantitative analysis is performed using standardless fundamental parameters (FP) method. Because sample is excited using highly monochromatized radiation, the calculations are much simpler and analysis error resulting from uncertainty of X-ray tube spectral distribution is completely eliminated. Moreover, EDXRF system allows obtaining very low background and appropriate secondary target can be selected for the best excitation of the determined elements and to avoid overlapping of the analyte peaks with characteristic radiation originating from the secondary target. The FP calculations were verified using several certified reference materials of stainless steel. The spectrometer was used for nondestructive analysis of mono- and polycrystals of selenide spinels of general formula M_xN_yCr_zSe₄ (where M, N are Cu²⁺, Zn²⁺, Cd²⁺, Mn²⁺, Ge²⁺, Ni²⁺, V³⁺, Sb³⁺, Ga³⁺). The results from EDXRF were compared with those obtained by means of the wavelength-dispersive X-ray fluorescence spectrometry (WDXRF).     

Determination of Cr,Fe, Co,Ni, Cu,Zn, As and Pb in liquid chemical waste by energy dispersive X-ray fluorescence

A method for simultaneous determination of Cr, Fe, Co, Ni, Cu, Zn, As e Pb in liquid chemical waste using Energy Dispersive X-Ray Fluorescence (EDXRF) technique was evaluated. A small sample amount (200 μL) was dried on a 6.35 μm thickness Mylar film at 60 °C and the analyses were carried out using an EDXRF spectrometer operated with an X-ray Mo tube (Zr filter) at 30 kV/20 mA. The acquisition time was 300 s and the Ga element was utilized as internal standard at 25 mg/L for quantitative analysis. The method trueness was assessed by spiking and the detection limit for those elements ranged from 0.39 to 1.7 mg/L. This method is notable because it assists the choice of the more appropriated waste treatment procedure, in which inter elemental interference is a matter of importance. In addition, this inexpensive method allows a non-destructive determination of the elements from ₁₉K to ₉₂U simultaneously.     

光谱实验室的建设和管理

阐述冶金、铸造等行业用于金属成分分析的直读发射光谱仪实验室的建设和管理。从仪器的调研、选型，实验室选址，基础设施设备的准备，仪器的安装、调试、验收、日常分析，实验室管理等几个方面，分别作了介绍。