铝灰及其浸出液中氟的测定

铝灰中的氟化物是铝灰中的环境危害因子.使用X射线荧光光谱(XRF)法、X射线衍射(XRD)法对15份铝灰样品进行了元素及物相组成检测,使用SPSS 25.0对数据进行因子分析和聚类分析,将15份样品分成四类,从每类中选择1～2个样品,共选取5份样品作为代表进行后续实验.使用离子色谱法和氟离子选择电极法对铝灰浸出液中氟离...     

X射线荧光光谱结合聚类分析对橡胶轮胎的检验

应用X射线荧光光谱结合系统聚类分析对30种不同的橡胶轮胎样本进行检验研究。利用X射线荧光光谱仪对橡胶轮胎中的主要元素及其含量进行测定,根据测定结果使用聚类分析对样本进行分类。选择最长距离法作为类与类之间距离的定义方法,采用平方欧式距离作为度量区间描述样品间亲疏程度进行系统聚类,最终将30个样本分为12类。该方法简单易行,分类结果可靠且无损轮胎样本,为实际案件的橡胶轮胎检验提供了一种检验思路。     

红外光谱结合X射线荧光光谱分析多种塑料袋组份的研究

为建立一种简便快捷、准确可靠的检验塑料袋样品的分析方法,利用傅立叶红外光谱仪(FTIR)结合能量色散型X射线荧光光谱仪(XRF),对43个不同品牌、不同规格的塑料袋样品进行测定。结果表明,依据样品的有机成分和样品中所含元素的种类及含量的不同,可以对样品进行区分,同时,利用SPSS聚类分析Ward法作为类间距离,对塑料袋样品进行分类,效果较好。并且该方法操作简便快速、结果准确可靠、样品无需特殊的前处理,且属于无损检验,该方法可以用于公安机关实际办案。     

X射线荧光光谱法对橡胶鞋底的分类

为建立案件现场常见橡胶鞋底物证的分类方法,利用X射线荧光光谱,对40个不同品牌、不同系列的橡胶鞋底样品中的无机元素进行了检验。并结合多元统计学,分别选用主成分分析法、k均值聚类法及判别分析法等对实验结果进行分析。结果表明,该方法简便快速、结果准确可靠且无损检材,对样品的分类效果较好。利用该方法可以对橡胶鞋底物证进行分类。     

基于聚类分析对易燃液体塑料容器盖的光谱检验

将光谱分析方法与聚类方法相结合,对38个模拟案件环境的纵火现场助燃剂塑料容器盖样本进行X射线荧光光谱分析,根据元素种类将38个样本分为6组,建立了一种无损快速检验纵火现场物证的光谱分析方法。使用最短距离聚类法,以欧氏距离作为度量区间表示样本间亲疏关系,进行系统聚类分析,同时使用K-Means快速聚类法与t检验验证聚类效果。结果表明,38个样本分为6组时效果最好。并将各类的样本观测点在Fisher判别空间中的分布和位置情况绘出,与使用元素种类进行分类结果一致,为确定火灾案件性质,侦破案件线索提供了理论依据。     

红外光谱结合X射线荧光光谱检验塑料 打包带(绳)的研究

建立简便快捷的检验塑料打包带(绳)的光谱分析方法。利用傅里叶变换红外光谱仪和X射线荧光光谱仪,对33个不同来源的塑料打包带(绳)样品进行检验分析。结合红外光谱成分填料分析与XRF元素比例分析,达到对塑料打包带(绳)样品准确区分的目的。该方法简便快速,准确可靠且无损检材,可应用于鉴定塑料打包带(绳)物证。     

便携式X射线荧光光谱法结合支持向量回归算法定量分析土壤中的砷含量

研究了基于统计学习理论的支持向量机（SVM）回归法在X射线荧光光谱定量分析中的应用。以39个农田土壤样品作为实验材料,以其中32个土壤样品作为校正集,选用SVM模型中Linear、Poly和RBF 3种核函数对As元素含量与荧光光谱数据进行回归建模。用3种不同模型对预测集中7个土壤样品的As元素含量进行预测分析,结果显示模型预测As元素含量与电感耦合等离子体发射光谱法测定的As元素含量之间的相关系数R2均大于0.99,相对分析误差RPD均大于3,表明所建立的SVM模型具有较好的使用价值。为了进一步考察SVM回归模型的预测效果,同应用较成熟的PLS回归模型的预测结果进行对比,结果显示SVM法的预测结果更好,表明SVM回归模型亦可用于便携式X射线荧光光谱法的定量预测分析。     

拉曼光谱法结合X射线荧光光谱法检验一次性塑料鞋套的研究

为建立简便快速、准确无损的检验一次性塑料鞋套的方法,利用RT2000便携式拉曼光谱仪和X-MET7000能量色散型荧光光谱仪对27个不同品牌的一次性塑料鞋套进行检验分析。根据鞋套样品的有机成分、元素组成,可对一次性塑料鞋套样品进行很好的区分。同时,利用spss软件和K-Means聚类法对鞋套样品中的元素含量进行分析研究,实验效果较好。该方法简单快速、结果准确可靠,可用于公安机关实际办案。     

波长色散X射线荧光光谱法分析小麦籽粒中矿质元素

采用波长色散X射线荧光光谱法(WDXRF)对小麦籽粒中Mn,Fe,Cu,Zn,Ca,Mg,P,K和S含量进行测定,讨论了不同产地小麦籽粒中矿质元素含量。运用主成分分析提取2个主成分、建立了主成分方程,利用聚类分析对小麦产地进行识别。结果表明,不同产地小麦籽粒中矿质元素含量差异明显。前2个主成分累积方差贡献率达到82.0%,黑龙江和内蒙古产地的小麦籽粒样品品质较优。在阈值为3.5的水平上将小麦籽粒样品聚为6类,可以实现小麦籽粒样品产地的初步鉴别。用WDXRF法结合化学计量学方法可揭示小麦籽粒样品中矿质元素含量差异及进行产地识别。     

能量色散X射线荧光光谱法测定中草药中的Cd元素

利用能量散射X射线荧光光谱（ED-XRF）法快速测定中草药中的Cd元素.方法对中草药进行简单预处理（粉碎）,使用X射线荧光光谱法建立中草药中Cd元素含量与相对强度的校正工作曲线,分析中草药样品中的Cd元素.Cd元素的检出限为0.083 mg/kg,定量限为0.207 mg/kg,定量限低于国家控制标准0.3 mg/kg.测量定量限以上的中草药样品时,其准确性与化学分析结果相当,重复性和稳定性等结果完全满足GB/T 4889-2008数据的统计处理标准.方法预处理时间不超过5 min,完成一个样品的检测时间不超过15 min,可应用于中草药生产企业中的重金属监控.     

X-ray fluorescence analysis of obsidian objects from Catamarca,Argentina

The concentrations of five trace elements (Rb, Zr, Sr, Ti and Mn) and one major (Fe) element have been determined in groups of obsidian samples by wavelength dispersive X-ray fluorescence spectrometry. Two methods were used for different elements on the basis of different excitation conditions and sample preparation procedures. Synthetic standards with compositions similar to those of the igneous stone were prepared into which the analytes were incorporated in solution. The method was used to establish the provenance of a number of prehistoric obsidian artifacts. The results ascertained in these analyses are discussed in this paper.     

豫产桔梗的土壤与药材中部分微量元素含量与分析

为了解桔梗中微量元素含量特征,研究土壤中微量元素对桔梗药材道地性的影响,采用原子吸收光谱法、冷原子荧光法、双道原子荧光法对不同产地的桔梗药材及生境土壤中8种微量元素含量进行了测定,所得数据用SPSS 11.0软件进行分析比较。结果表明,不同产地的桔梗微量元素含量有差异;药材与土壤中微量元素之间具有相关性。桔梗对土壤中微量元素是主动与被动相结合的有选择吸收。     

Identification of glass and ceramics by X-ray fluorescence analysis with a pyroelectric X-ray generator.

Applications of X-ray fluorescence (XRF) analysis with a pyroelectric X-ray generator are presented. Glass and ceramics were analyzed with this novel X-ray generator to examine its capability for analyzing nonmetallic inorganic material. Although the power of X-ray output was a few orders of magnitude lower than conventional X-ray tubes, many elements such as Si, K, Ca, Ti, Cr, Fe, Zn, Sr, Ba, and Pb were detected in glass and ceramic samples. Light elements such as Na, Mg, and Al were not detected because of the low fluorescence yield and the absorption of fluorescent X-rays in air. The elements detected or the relative peak intensities of the elements were different from each other, and the samples analyzed were identified by the XRF spectrum, notwithstanding the low power of the X-ray output. This novel device showed the sufficient capability for preliminary screening before strict identification of analytes. The pyroelectric X-ray generator can also be used to analyze large samples that cannot be put into ordinary XRF spectrometers because the device has no dimensional limitation of analytes.     

Comparison of 14 MeV-NAA, k0-NAA and ED-XRF for air pollution bio-monitoring

In this paper the performances and the limitations of three multi-elementary analysis techniques are compared applied to a study of air pollution biomonitoring in Morocco. These techniques are: (1) 14 MeV neutron activation analysis (14 MeV-NAA), (2) thermal neutron activation analysis using the k ₀ quasi-absolute method (k ₀-NAA) and (3) energy dispersive X-ray fluorescence analysis (ED-XRF). The experimental procedures and the control of the analytical results using certified reference materials are described and discussed. The three methods were confronted for the analysis of lichens, mosses and tree-barks. The complementarity of these methods enabled us to determine 43 elements in different samples. The most suitable method for each element was selected according to the sensitivity and selectivity necessitating the minimum corrections of the matrix effects and/or the interfering reactions.     

Application of radioisotope-excited X-ray fluorescence to the determination of trace elements in blood

A radioisotope-excited energy-dispersive X-ray fluorescence system has been constructed and used for the analysis of blood samples for trace elements. The possibility of determination of trace elements in blood by X-ray fluorescence based on comparison with standard reference materials has been outlined and the applicability of the method demonstrated by the analysis of blood samples. The method enables fast, non-destructive direct analyses to be carried out without lengthy sample pretreatment on a routine basis.     

A correction method of matrix,density and thickness effects in thin samples analysed by X-ray fluorescence spectrometry

This paper deals with X-ray fluorescence spectrometry of powdered materials deposited on collection filters. The general applicability of this method is limited because the spectral response is affected by sample density and thickness and interelement effects may occur due to the specimen composition.The present work is aimed at contributing to the solution of the above mentioned problems, and reports a mathematical correction method which changes fluorescence intensity measurement data into fluorescence intensity values free from density and thickness effects. The correction of the thickness effect was obtained by overlapping the powder sample with a standard pellet containing some reference elements.The method allows the evaluation of the thickness of the unknown samples by measuring the intensity decrease of the X-ray fluorescence radiation coming from the reference pellet and passing through the unknown sample. These data are used to correct the intensity fluorescence values of the unknown samples.A computer program to elaborate spectral data by means of different and selected mathematical algorithms was set up.     

粉末压片-X-射线荧光光谱法分析砂岩型铀矿制样中粘结剂用量的探讨

由于砂岩型铀矿的成矿特性,样品粉末的内聚力小,采用直接压片法有时难以成型,样片表面常见裂纹,上机测量易碎裂。混合压片法适应性强,制样成功率高,但常见的问题是样品经粘结剂稀释会影响元素的检出限及结果的准确性。本文对粉末压片-X射线荧光光谱法测定砂岩型铀矿地质样品时,前期制样中添加粘结剂的比例进行了研究。试验按照不同比例在铀矿石标准物质GBW04101、GBW04102中添加粘结剂,在扫描电镜下观察到随着粘结剂用量的增加样片表面的光滑度及致密度都呈上升趋势,在X-射线荧光光谱仪上对主量元素进行测定后发现X射线强度在粘结剂添加量大于0.2 g时明显下降,经与GBW04101、GBW04102标准值进行对比后优选出粘结剂与样品的最佳比例为1：20,在此比例下制成的样片光滑平整,不易碎裂,用粉末压片-X射线荧光光谱法进行测定,标准物质测定结果的相对误差为0.56%～6.76 %,相对标准偏差(RSD,n=12)为0.013 %～7.68 %,均达到了《地质矿产实验室测试质量管理规范》DZ/T 0130-2006的要求。本文为粉末压片-X射线荧光光谱法分析砂岩型铀矿地质样品提供了可靠的实验参考依据。     

Semiempirical model for X-ray fluorescence analysis combining concentration correction equations and backscatter radiation method

The basic equations for a new semiempirical multielement calibration model for X-ray fluorescence analysis of thick samples are derived. Two main cases are considered: determination of all elements in the sample and determination of only a few selected elements. Advantages and disadvantages of the described calibration method are discussed. The method was applied to real samples and its results were compared to those obtained by multiple regression methods.     

Identification of steel by X-ray fluorescence analysis with a pyroelectric X-ray generator

An application of X-ray fluorescence analysis with a pyroelectric X-ray generator is presented. Steel standard samples were identified by X-ray fluorescence analysis with this novel X-ray generator to check its capability for performing qualitative and quantitative analysis as an X-ray source for X-ray fluorescence spectrometers. Cr, Ni, V, Co, and W were detected in steel standard samples. V and Cr can be detected even when the content is below 1%. Although it is difficult to detect minor elements because of the low power of the excitation X-rays, it is possible to identify the analyzed samples on the basis of major elements at the percentage level. The pyroelectric X-ray generator is very suitable for portable X-ray fluorescence spectrometers.