EDXRF无标样分析未知样品含量的算法研究

针对未知样品能量色散X射线荧光分析(energy dispersive X-ray fluorescence analysis,EDXRFA)方法开展无标样分析,通过测量Ti、Fe、Ni、Cu、Zn、Sr、Sn、Pb单元素标样,得到Rh靶材原级谱中Kα峰的相干与非相干散射峰强度比值R,并建立R与对应单元素标样有效原子序数的关系,得到Zeff-R的拟合曲线。求解未知样品基体时,测量未知样,得到其R,将R代入Zeff-R拟合曲线得到未知样有效原子序数,再通过基本参数法迭代计算其质量衰减系数。利用Ti、Fe、Ni、Cu、Zn、Sr、Sn、Pb单元素标样刻度仪器获取Gi参数,求解未知样品基体时用于相应元素的基本参数迭代。为验证算法可靠性,采用本算法分析15个国家土壤标准样品,结果表明,Ti、Fe、Ni、Cu、Zn元素的计算含量与标准含量接近,部分低含量元素受到散射本底等因素影响,含量误差较大。结果表明,该方法能够用于现场能量色散X射线荧光分析。     

黄饼标准分析流程建立研究

正四家核取证研究实验室进行了黄饼样品的核取证特征属性比对分析,分析的特征属性包括微观形貌,化学成分,铀含量,铀同位素丰度,杂质元素含量(Al、Cr、Fe、Pb、Ti、Zn、Mo、Nb、Sb、Sn、Ru、Ta、Th、Ni、Mn等),Pb、Sr、Nd同位素丰度等。通过黄饼的比对分析,希望建立黄饼样品的     

波长色散X荧光光谱法检测室内PM_(2.5)无机元素组份

介绍用波长色散X荧光光谱法(WDXRF)对室内PM2.5样品进行无机元素检测的测试方法。该方法以在同一房间每天只采集一个PM2.5样品的方式,利用自行搭建的大气颗粒物采集平台,将PM2.5样品收集在滤膜上,运用WDXRF检测滤膜试样中的无机元素。结果表明:(1)室内PM2.5样品的无机元素成份复杂,主要存在Na、Mg、Al、Si、S、Cl、K、Ca、Ti、Fe、Zn等元素,以及极少量的As、Rb、Sr、Zr、Sb、Ta、Pb等元素;(2)对Fe、Ni、Cu、Zn、As、Pb等15种无机元素的定量分析结果表明,室内PM2.5中Ca元素的含量最高,平均浓度达3.381μg/m3;其次是K、Zn、Fe,平均浓度分别为1.316、1.114、0.517μg/m3;Ti、Mn、Cu、As、Pb等无机元素平均浓度均在0.500μg/m3以下。确定室内PM2.5中无机元素组份,可为室内PM2.5的污染物溯源和污染防治措施提供科学依据。     

GSD水系沉积物标准参考样中一些元素的仪器光子活化分析

本文首次用仪器光子活化法测定了GSD-2、GSD-5和GSD-6三种标准参考样中的Ce、Cs、Fe、Mg、Mn、Na、Nb、Nd、Ni、Pb、Rb、Sr、Ti、Y、Zn、Zr等16种元素的含量。其中Nb、Ph、Ti、Y、Zr等5种元素中子活化法还未曾提供数据。测定采用相对法,利用Cu箔活化产生的~(64)Cu校正不同照射位置处光子通量。分析周期3—5天。结果表明69％以     

基于SRXRF的单个流体包裹体无损分析及其在石油地质中的应用

本文叙述了同步辐射X射线荧光微探针用于单个流体包裹体无损分析研究的实验装置和方法，通过测定NIST612标样，计算了目前实验条件下部分元素的检出限，对取自我国西部含油气盆地的典型有机包裹体作无损成分分析，给出了K，Ti,V,Cr,Mn,Fe,Co,Ni,Cu,Zn,Rb,Sr,Y,Zr,Ba,Pb等元素的半定量测试结果，并对分析结果在石地质中的应用进行了初步研究。     

发射光谱法测定二氧化碲中的杂质元素

采用发射光谱粉末法同时测定二氧化碲Pb、Mn、Ba、Sn、Fe、Co、Ti、Cd、Cr、Al、Ca、Si、B、Bi、V、Ni、Sb、Zn、Ag、Mg、Cu18个金属元素，选择石墨作载体，直接压样于石墨电极中，简单，快速而准确。其回收率在80%-120%范围内，相对标准偏差小于8%，用于样品的测定取得了满意的结果。     

X射线荧光光谱分析法同时测定化探样品中多组分的含量

采用粉末压片制样法,利用PANalytical Axios型波长色散X荧光光谱仪同时对化探样品中的Fe2 O3、Al2 O3、Cr、Co、Ni、Cu、Zn、Pb等36种主、次和痕量组分进行测定.采用基本参数法,结合PH模式的经验系数法校正光谱干扰和集体效应.用国家标准物质做检验,测量结果与标样认定值吻合,用国家一级标准...     

用同步辐射X荧光分析血浆蛋白质的微量元素

用同步辐射X荧光(SRXRF)分析技术与凝胶色谱生化分离相结合，分析了用抗肿瘤药物顺铂处理过的和未处理过的小鼠血浆的大分子蛋白质。对以轻元素为基体的小量样品，用X荧光谱中的康普顿散射强度作为质量的因子，获得了在大于22ku分子量的蛋白质中Pt、S、Ca、Fe、Ni、Cu、Zn、Se、Br和Sr等元素含量在不同样品问的相对变化。由此推测，经顺铂处理后，Pt元素可与血浆中的大分子蛋白结合，含CM和S的大分子蛋白含量明显升高，而含Zn的减少。     

PIXE用于北京市新镇地区大气颗粒物污染特征和来源解析研究

为研究北京市新镇地区大气颗粒物的污染特征及其来源,于2015年12月～2017年12月间以每周两次的频率采集颗粒物样品。利用质子激发X射线荧光分析(Proton Induced X-ray Emission, PIXE)测定了140个样品中的Mg、Al、Si、S、Cl、K、Ca、Sc、Ti、Mn、Fe、Ni、Cu、Zn、As、Pb共16种元素的含量,并对主要的污染元素进行特征分析。结果表明:S、Cl、Cu、Zn、Pb在细颗粒物中占比较大且相关性较强,Mg、Al、Si、Ca、Ti、Fe则主要存在于粗颗粒物中并存在强相关性;污染时期细颗粒物中S、Cl、K、黑碳(Black Carbon,BC)和粗颗粒物中Si、Ca、Fe上升明显。正矩阵因子分析(Positive Matrix Factor Analysis, PMF)得到该地区存在的6种主要污染源:次级硫(34.70%)、建筑工业(24.39%)、含氯工业(13.05%)、土壤扬尘(12.81%)、交通排放(11.63%)和其他污染(3.42%)。     

手持式XRF分析仪快速检测大气颗粒物中Cu、Zn、Pb含量

介绍了用手持式X射线荧光光谱(XRF)分析仪对大气颗粒物PM2.5中的Cu、Zn和Pb含量进行快速检测的方法。该方法用ICP-MS对滤膜样品的分析结果作为标样,建立XRF法被测元素含量——特征谱线强度工作曲线,利用此工作曲线测定大气颗粒物PM2.5中Cu、Zn和Pb的含量。该方法对大气颗粒物中Cu、Zn和Pb含量测量结果的相对标准偏差依次为5.50%、1.56%、4.71%。通过实验比对,该方法测试结果能与成都地区3月上旬浮尘天气现象相吻合。     

白血病患者头发中钙及微量元素的初步研究

应用放射性核素~(238)Pu源激发X射线荧光法测定了63例白血病患者头发中钙及锶、铅、锌、铜、镍、铁、锰、铬、钛等9种微量元素的含量。与同期苏州地区115名正常成人头发微量元素相比,发现男女患者发中Zn、Cu和Ca含量均明显下降,而Pb含量均显著上升(p≤0.05或p<0.001)。此外男性患者发中Ni、Fe、Mn、Cr亦明显上升,而女性患者发中Sr明显下降(p<0.05或p<0.001)。男性白血病发病率高于女性,可能同男性患者发中Mn、Fe、Ni、Cr含量显著升高有关。     

Quantitative energy-dispersive X-ray fluorescence analysis for unknown samples using full-spectrum least-squares regression

The full-spectrum least-squares(FSLS) method is introduced to perform quantitative energy-dispersive X-ray fluorescence analysis for unknown solid samples.Based on the conventional least-squares principle, this spectrum evaluation method is able to obtain the background-corrected and interference-free net peaks, which is significant for quantization analyses. A variety of analytical parameters and functions to describe the features of the fluorescence spectra of pure elements are used and established, such as the mass absorption coefficient, the Gi factor, and fundamental fluorescence formulas. The FSLS iterative program was compiled in the C language. The content of each component should reach the convergence criterion at the end of the calculations. After a basic theory analysis and experimental preparation, 13 national standard soil samples were detected using a spectrometer to test the feasibility of using the algorithm. The results show that the calculated contents of Ti, Fe, Ni, Cu, and Zn have the same changing tendency as the corresponding standard content in the 13 reference samples. Accuracies of 0.35% and 14.03% are obtained, respectively, for Fe and Ti, whose standard concentrations are 8.82% and 0.578%, respectively. However, the calculated results of trace elements (only tens of lg/g) deviate from the standard values. This may be because of measurement accuracy and mutual effects between the elements.     

钙,微量元素与妊娠关系的初步研究

用X射线荧光分析法(XRF)测定了1023例孕妇发中的Ca以及9种微量元素含量,与270例对照组相比,孕妇发中Sr、Mn、Ca含量显著降低(p<0.01),Zn、Cu、Fe含量也有不同程度的降低,特别是在妊娠晚期。     

乳腺癌和乳腺增生症患者头发中钙及其他微量元素的初步研究

用２３８Ｐｕ源激发Ｘ射线荧法测定３２例乳腺癌和１０５例乳腺增生症女性患者头发中Ｃａ及Ｓｒ，Ｐｂ、Ｚｎ、Ｃｕ、Ｎｉ、Ｆｅ、Ｍｎ、Ｃｒ、Ｔｉ等９种微量元素含量。与５５例正常成年女性头发中微量元素相比，发现乳腺增生症组中的Ｓｒ、Ｚｎ、Ｃｕ、Ｍｎ和Ｃａ含量显著下降（ｐ＜０．００１），其他元素无显著差异；乳腺增生症组中的Ｓｒ、Ｍｎ、和Ｃａ含量明显下降（Ｐ＜０．０１），而Ｚｎ、Ｎｉ、Ｃｒ含量显著升高（Ｐ＜０．０５）；乳腺增生症组中的Ｓｒ、Ｚｎ、Ｃｕ、Ｎｉ、Ｍｎ、Ｃｒ和Ｔｉ含量明显下降而（Ｐ＜０．０５－Ｐ＜０．００１）。     

Elemental analysis of mining wastes by energy dispersive X-ray fluorescence (EDXRF)

An energy dispersive X-ray fluorescence (EDXRF) tri-axial geometry experimental spectrometer has been employed to determine the concentrations of 13 different elements (K, Ca, Ti, Cr, Mn, Fe, Co, Ni, Cu, Zn, Rb, Sr and Pb) in mine wastes from different depths of two mine tailings from the Cartagena-La Union (Spain) mining district. The elements were determined and quantified using the fundamental parameters method. The concentrations of Cr, Ni, Cu, Zn and Pb were compared to the values from the European and Spanish legislation to evaluate the environmental risk and to classify the wastes as inert wastes or as wastes that have to be control land-filled. The results obtained demonstrate that these wastes can be considered as inert for the considered elements, apart from the concentration levels of Zn and Pb. Whilst Zn slightly overpasses the regulatory levels, Pb mean value exceeds three to six times the value to be considered as Class I potential land-filling material.     

上海市长寿老人的头发微量元素谱特征

微量元素与人体健康和疾病有着密切的联系,特别是一些必需微量元素,它们通过参与酶、激素、蛋白质、核酸等的合成及代谢功能,对人体的生长、发育、衰老、死亡起着至关重要的作用。近年来,微量元素对人类寿命的影响已引起人们的注意。头发是一种化学组成均匀而稳定的物质,金属微量元素一旦与毛囊中的硫基(-SH)结合就被固定而不易被机体重新吸收或脱落。头发也和皮肤一样参与机体的代谢过程,是代谢的最终产物,头发中的元素浓度可反映人体内存在的元素的平均浓度。因而测定头发中的微量元素含量可为生长、发育和衰老研究提供重要信息。本工作的目的在于通过测定九十岁以上长寿老人发中的十种必需元素含量,探讨长寿老人的微量元素谱特征。     

Thick target PIXE analyses of the elemental distributions across the surface and inside human fingernails

The energy dispersive spectrometry of thick target proton-induced X-ray emission (thick target PIXE) was used to determine the distributions of 11 elements (S, Cl, K, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn) across the surface and at a certain depth inside human fingernails. The respective profiles are discussed and preliminary interpretations are given. The results are compared with data from other authors.     

中医虚证与长寿老人发中微量元素相关关系探索

对于中医虚证的本质,国内外已进行了多方面的研究,获得了若干生理功能和生化代谢方面的各种客观指标的数据。由于微量元素在人体生长、发育和衰老中起着重要作用,近年来我国亦有人从这一角度对虚证本质进行了探索。     

Trace elements in lake sediments measured by the PIXE technique

Lakes are ecosystems where there is a great potential of metal accumulation in sediments due to their depositional characteristics. Total concentration of trace elements was measured on a 50 cm long sediment core from the Infernão Lake, that is an oxbow lake of the Moji-Guaçu River basin, in the state of São Paulo, Brazil. Dating of the core shows up to 180 yrs old sediment layers. The use of the PIXE technique for elemental analysis avoids the traditional acid digestion procedure common in other techniques. The multielemental characteristic of PIXE allows a simultaneous determination of about 20 elements in the sediment samples, such as, Al, Si, P, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Rb, Sr, Zr, Ba, and Pb. Average values for the elemental composition were found to be similar to the bulk crustal composition. The lake flooding pattern strongly influences the time series of the elemental profiles. Factor analysis of the elemental variability shows five factors. Two of the factors represent the mineralogical matrix, and others represent the organic component, a factor with lead, and another loaded with chromium. The mineralogical component consists of elements such as, Fe, Al, V, Ti, Mn, Ni, K, Zr, Sr, Cu and Zn. The variability of Si is explained by two distinct factors, because it is influenced by two different sources, aluminum-silicates and quartz, and the effect of inundation are different for each other. The organic matter is strongly associated with calcium, and also bounded with S, Zn, Cu and P. Lead and chromium appears as separated factors, although it is not clear the evidences for their anthropogenic origin. The techniques developed for sample preparation and PIXE analysis was proven as advantageous and provided very good reproducibility and accuracy.