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How reliable is the X‐ray fluorescence‐based differentiation between glass wool and rock wool and the age classification of rock wool? 基于 X 射线荧光法区分玻璃棉和岩棉以及岩棉年龄分类的可靠性如何?
IF 1.2 4区 物理与天体物理 Q3 SPECTROSCOPY Pub Date : 2024-09-05 DOI: 10.1002/xrs.3451
Andrea Paul, Zoe Liestmann, Steffen Zaenker, Kristin Vogel, Tanja Broszies, Markus Ostermann
A prerequisite for the recycling of mineral wool is information about the type of material, that is, whether it is glass wool or rock wool. As mineral wool produced before the year 2000 can be potentially carcinogenic, it is furthermore important to distinguish between “old” and “new” wool when handling the material. Based on VDI 3492, it is possible to determine the material and, in the case of rock wool, the age by analyzing the mass fractions of eight oxides, which are the main components of mineral wool. This study presents the X‐ray fluorescence (XRF) analyses of 141 man‐made mineral fibers collected in Germany. Only in a few cases it was not possible to clearly assign the material type. In contrast, the identification of “old” and “new” rock wool posed a challenge as there were many borderline samples. Based on the available data, a chemometric model was developed that can classify “old” and “new” RW with a sensitivity of 93% and 89% and with a specificity of 100% in both cases. However, care must be taken when oxide contents are close to the specification limits. The reason for this mainly lies in the overlapping intervals of key oxides as suggested by VDI 3492, and, to a lesser extent, in the uncertainties typically occurring in the XRF‐based analysis of oxides. With this study, a comprehensive collection and evaluation of XRF data on mineral wool is made available, which can serve as a reference database for future users.
回收矿棉的一个先决条件是了解材料的类型,即是玻璃棉还是岩棉。由于 2000 年以前生产的矿棉可能会致癌,因此在处理这种材料时还必须区分 "旧 "矿棉和 "新 "矿棉。根据 VDI 3492 标准,可以通过分析矿棉的主要成分--八种氧化物的质量分数来确定矿棉的材质,如果是岩棉,则可以确定其使用年限。本研究介绍了在德国收集的 141 种人造矿物纤维的 X 射线荧光 (XRF) 分析结果。只有少数情况下无法明确确定材料类型。相比之下,"老 "岩棉和 "新 "岩棉的鉴别则是一项挑战,因为有许多样品都存在边界问题。根据现有的数据,我们建立了一个化学计量模型,该模型可以对 "老 "和 "新 "岩棉进行分类,灵敏度分别为 93% 和 89%,特异度均为 100%。不过,当氧化物含量接近规格限值时,必须小心谨慎。其原因主要在于 VDI 3492 所建议的关键氧化物的重叠区间,其次是基于 XRF 的氧化物分析中通常会出现的不确定性。本研究全面收集和评估了矿棉的 XRF 数据,可作为未来用户的参考数据库。
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引用次数: 0
Energy dependence of x‐ray beam size produced by polycapillary x‐ray optics 聚毛细管 X 射线光学器件产生的 X 射线束尺寸的能量依赖性
IF 1.2 4区 物理与天体物理 Q3 SPECTROSCOPY Pub Date : 2024-08-22 DOI: 10.1002/xrs.3450
Anusheela Das, Chris M. Heirwegh, Ning Gao, William T. Elam, Lawrence A. Wade, Benton C. Clark, Joel A. Hurowitz, Scott J. VanBommel, Michael W. M. Jones, Abigail C. Allwood
In this work, we studied the x‐ray energy dependence of x‐ray beam diameter focused by polycapillary optics. A quantitative beam diameter–energy relation enables more accurate estimation of the element‐specific interrogation area of a sample using the compositional maps produced by a micro‐XRF system. This improves upon our ability to visualize individual beam‐diameter sized mineral grains and in turn directly benefits Planetary Instrument for X‐ray Lithochemistry (PIXL) analyses of martian soil in addition to benefitting other micro‐focused x‐ray fluorescence (XRF) systems. The spatial distribution of an array of characteristic XRF emission lines was measured by sampling via a knife‐edge approach with small motor stepping of the beam across target edges. Data taken as part of this effort, from the Planetary Flight Model (PFM), were limited to only seven beam energies corresponding to the elements Ni, Cu, Se, Ta, Au, Ti and Ba. Hence, we conducted additional analysis using JPL's lab‐based breadboard (LBB) micro‐XRF system, a system that emulates PIXL's functionality where we measured beam diameter corresponding to 18 elements: Na, Mg, Al, Si, Cl, Ca, Ti, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, Se, Sr and Mo. The experimental results were also compared with Monte Carlo simulations. The beam diameter (y)–energy (x) relation that we obtained for LBB was y = 185.79 exp(−0.078x) whose exponential component was then used to get a more accurate relation for the PFM even with the limited data set: y = 227.53 exp(−0.078x). The difference in the two coefficients for the PFM and LBB stems mainly from the difference in the polycapillary optic design, and this work establishes x‐ray beam diameter versus energy relation quantitatively for both the systems.
在这项工作中,我们研究了聚毛细管光学系统聚焦的 X 射线束直径与 X 射线能量的关系。通过定量的光束直径-能量关系,可以利用微型 XRF 系统产生的成分图更准确地估计样品的特定元素探测区域。这提高了我们对单个光束直径大小的矿物颗粒进行可视化的能力,进而直接有益于行星 X 射线岩石化学仪器(PIXL)对火星土壤的分析,并有益于其他微聚焦 X 射线荧光(XRF)系统。通过在目标边缘使用小电机步进光束的刀刃取样方法,对特征 XRF 发射线阵列的空间分布进行了测量。作为这项工作的一部分,从行星飞行模型(PFM)中获取的数据仅限于与 Ni、Cu、Se、Ta、Au、Ti 和 Ba 元素相对应的七种光束能量。因此,我们使用 JPL 的实验室面包板 (LBB) micro-XRF 系统进行了额外的分析,该系统可模拟 PIXL 的功能,我们在该系统中测量了与 18 种元素相对应的光束直径:我们测量了 18 种元素对应的光束直径:Na、Mg、Al、Si、Cl、Ca、Ti、Cr、Mn、Fe、Ni、Cu、Zn、Ga、Ge、Se、Sr 和 Mo。实验结果还与蒙特卡洛模拟结果进行了比较。我们为 LBB 得到的光束直径(y)-能量(x)关系式为 y = 185.79 exp(-0.078x),然后利用其指数分量为 PFM 得到了更精确的关系式,即使数据集有限:y = 227.53 exp(-0.078x)。PFM 和 LBB 两个系数的差异主要源于聚毛细管光学设计的不同,这项工作为这两个系统定量地建立了 X 射线束直径与能量的关系。
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引用次数: 0
Total reflection x‐ray fluorescence analysis of trace elements in highly saline samples 高盐度样品中痕量元素的全反射 X 射线荧光分析
IF 1.2 4区 物理与天体物理 Q3 SPECTROSCOPY Pub Date : 2024-08-14 DOI: 10.1002/xrs.3448
Bastian Wiggershaus, Eric Franke, Carla Vogt
The reliable trace analysis of high‐purity chemicals and environmentally relevant samples is more important than ever and has led to the development of novel analytical methods. Total reflection x‐ray fluorescence (TXRF) analysis is an increasingly known method for the determination of heavy metals at low concentration levels in environmental and industrial sample systems. However, there is still a need for optimization to obtain fast and precise results, especially for highly saline samples like brines and salts used in battery production or sea water. In this study, multi‐element standard solutions containing analytes like Co, Cr, Cu, Fe, Mn, Ni, or Zn in a concentration range between 0.1 and 1 mg/L were analyzed in the matrices lithium carbonate (Li2CO3) and artificial seawater (ASW) containing 1000 mg/L Li and 24,000 mg/L NaCl, respectively, leading to matrix‐analyte ratios of up to 240,000:1. Different sample preparation methods were compared in order to achieve the highest possible repeatability (1) and signal‐to‐noise ratios (2) with the least amount of time (3). Various parameters such as sample volume, drying conditions, time, temperature and additive concentration were varied. The relative standard deviation (RSD%) was used as a measure of repeatability for three replicates per sample. For lithium carbonate, a method with a preparation time of only 2 min and a measurement time of 500 s could be developed, which allowed to obtain RSD% well below 5%, a high linearity (R2 > 0.99) and limits of detection (LOD) in the range of 30 μg/L to 60 μg/L for most elements. Seawater analysis could be optimized with respect to signal‐to‐noise ratio, whereby the Kα‐line of the internal standard (Ga) was used for evaluation and the use of a desiccator was found to yield the best results.
对高纯度化学品和环境相关样品进行可靠的痕量分析比以往任何时候都更加重要,这也促使了新型分析方法的开发。全反射 X 射线荧光 (TXRF) 分析是一种日益为人所知的方法,可用于测定环境和工业样品系统中低浓度水平的重金属。然而,该方法仍需优化,以获得快速、精确的结果,尤其是对于电池生产中使用的盐水或海水等高盐度样品。本研究在碳酸锂(Li2CO3)和人工海水(ASW)(分别含 1000 mg/L Li 和 24,000 mg/L NaCl)基质中分析了浓度范围在 0.1 至 1 mg/L 之间的钴 (Co)、铬 (Cr)、铜 (Cu)、铁 (Fe)、锰 (Mn)、镍 (Ni) 或锌 (Zn) 等多元素标准溶液,基质与分析物的比率高达 240,000:1 。为了用最少的时间(3)获得尽可能高的重复性(1)和信噪比(2),对不同的样品制备方法进行了比较。样品体积、干燥条件、时间、温度和添加剂浓度等各种参数均有不同。用相对标准偏差(RSD%)来衡量每个样品三次重复的可重复性。对于碳酸锂,所开发的方法制备时间仅为 2 分钟,测量时间为 500 秒,可获得远低于 5%的 RSD%,线性度高(R2 > 0.99),大多数元素的检测限(LOD)在 30 μg/L 至 60 μg/L 之间。海水分析可根据信噪比进行优化,使用内标(Ga)的 Kα 线进行评估,并发现使用干燥器可获得最佳结果。
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引用次数: 0
X‐ray microanalysis and mapping for white ceramics unearthed from Gangguantun Kiln of Liaoyang, Liaoning province, China 中国辽宁省辽阳市岗官屯窑出土白瓷的 X 射线显微分析与绘图
IF 1.2 4区 物理与天体物理 Q3 SPECTROSCOPY Pub Date : 2024-08-14 DOI: 10.1002/xrs.3449
Guiyun Shen, Jinyu Yu, Baolong Zhang, Yuanyuan Wu, Jun Zhou, Naisheng Li, Jian Zhu
In this case, electron probe microanalyzer (EPMA) and micro x‐ray fluorescence (μ‐XRF) techniques were employed to the analysis of white porcelain species artifacts unearthed from the Gangguantun Kiln (10–13th century) and investigate for its production processes' details by microanalysis. Microscopic observation reveals the presence of inclusions in the ceramic bodies across different historical periods, with notable disparities in the form and quantity of these inclusions between samples from distinct periods. By employing EPMA mapping and particle analysis, it was discerned that the inclusions in the late‐period white porcelain are primarily composed of calcium‐rich materials, exhibiting a uniform composition and structure. The uniformity in particle size distribution strongly suggests that these inclusions are temper with certain purpose, deliberately and intentionally introduced by skilled artisans following a controlled processing method. This discovery rectifies the previously held notion that the white porcelain products from the Gangguantun Kiln were rustic and coarse, with the “black iron spots” or other inclusion being viewed as impurities. Furthermore, these temper materials, likely treated before incorporation, may have played a role in enhancing the firing process of ceramics. This revelation sheds light on the distinctive technological aspects of ceramic craftsmanship during the Liao and Jin dynasty periods. It serves as a crucial reference for delving into the technical choices and integration within the handicraft industry of northern China during the Liao‐Jin era, as well as the unique regional characteristics and stylistic features of the period. This significantly enriches our comprehension of this historical era.
本次研究采用电子探针显微分析仪(EPMA)和微X射线荧光(μ-XRF)技术,对江官屯窑(10-13世纪)出土的白瓷器物进行分析,并通过显微分析研究其生产工艺细节。显微镜观察发现,不同历史时期的瓷器胎体中都存在夹杂物,不同时期的样品在夹杂物的形态和数量上存在明显差异。通过 EPMA 制图和颗粒分析,发现晚期白瓷中的夹杂物主要由富含钙质的物质组成,呈现出均匀的成分和结构。颗粒大小分布的均匀性有力地表明,这些夹杂物是由能工巧匠按照可控的加工方法有意识、有目的地加入的。这一发现纠正了以往认为江官屯窑的白瓷产品质朴粗糙,"黑铁点 "或其他夹杂物被视为杂质的观点。此外,这些回火材料很可能是在加入之前经过处理的,可能在提高陶瓷烧制工艺方面发挥了作用。这一发现揭示了辽金时期陶瓷工艺的独特技术。它为研究辽金时期中国北方手工业的技术选择和整合,以及该时期独特的地域特征和风格特征提供了重要参考。这极大地丰富了我们对这一历史时代的理解。
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引用次数: 0
Calendar article 条款日历
IF 1.2 4区 物理与天体物理 Q3 SPECTROSCOPY Pub Date : 2024-08-08 DOI: 10.1002/xrs.3446
Kenji Sakurai
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引用次数: 0
News Article 新闻报道
IF 1.2 4区 物理与天体物理 Q3 SPECTROSCOPY Pub Date : 2024-08-08 DOI: 10.1002/xrs.3445
Kenji Sakurai
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引用次数: 0
Study of the chemical composition of coal and coal ash by X‐ray fluorescence method: A review 用 X 射线荧光法研究煤和煤灰的化学成分:综述
IF 1.2 4区 物理与天体物理 Q3 SPECTROSCOPY Pub Date : 2024-07-26 DOI: 10.1002/xrs.3444
Anatoly G. Revenko, Galina V. Pashkova
Information about the elemental compositions of coal and coal ash is very important to solve some issues related to both technological processes and the control of environmental pollution. It is known that the coal and coal ash samples often contain significant amounts of valuable as well as toxic components (e.g., V, Cr, Со, Ni, Cu, Zn, As, Sr, Ba, Pb, Ga, and Ge) that can be successfully determined by X‐ray fluorescence (XRF) spectrometry. This review briefly discusses the development of XRF equipment, elements of interest determined by XRF, and common sample preparation procedures. The calculation of relative intensities of analytical lines of some elements and scattered radiation is presented to demonstrate possible matrix effects in XRF analysis. Possibilities and drawbacks of total reflection XRF (TXRF) are described in detail as the coal and ash analysis is a relatively new area of application of TXRF method. The review also presents examples of the application of the XRF method for analysis of waste from coal preparation plants and thermal power plants to assess their prospects and to choose a method for extracting individual elements. Among the reviewed publications, several works are devoted to the study of the element distributions, especially rare earth elements, in coals, coal ash, and coal waste.
煤和煤灰的元素组成信息对于解决一些与技术工艺和环境污染控制有关的问题非常重要。众所周知,煤和煤灰样品中通常含有大量有价值和有毒的成分(如钒、铬、Со、镍、铜、锌、砷、锶、钡、铅、镓和锗),这些成分可通过 X 射线荧光 (XRF) 光谱法成功测定。本综述简要讨论了 XRF 设备的发展、通过 XRF 测定的相关元素以及常见的样品制备程序。介绍了一些元素分析线和散射辐射相对强度的计算方法,以说明 XRF 分析中可能存在的基体效应。详细介绍了全反射 XRF (TXRF) 的可能性和缺点,因为煤和灰分析是 TXRF 方法的一个相对较新的应用领域。综述还介绍了应用 XRF 方法分析选煤厂和热电厂废物的实例,以评估其前景并选择提取个别元素的方法。在审查的出版物中,有几部作品专门研究了煤炭、煤灰和煤炭废料中的元素分布,特别是稀土元素。
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引用次数: 0
Determination of macro‐ and microelements concentrations by wavelength‐dispersive X‐ray fluorescence spectrometry in the objects of the technogenic ecosystem 用波长色散 X 射线荧光光谱法测定技术生态系统物体中的宏量和微量元素浓度
IF 1.2 4区 物理与天体物理 Q3 SPECTROSCOPY Pub Date : 2024-07-24 DOI: 10.1002/xrs.3443
Svetlana I. Shtel'makh, Alena N. Zhilicheva, Irina E. Vasil'eva
The wavelength‐dispersive X‐ray fluorescence (WDXRF) spectrometry was applied to determine Na, Mg, Al, P, S, K, Ca, Cr, Mn, Fe, Ni, Cu, Zn, Sr, Ba, and Pb concentrations in the needles of dwarfish spruce Picea canadensis conica and the blue prickly spruce Picea pungens glauca, as well in technogenic soil of Irkutsk city, in which these spruce species grow. All measurements were performed in vacuum using WDXRF spectrometer S8 TIGER produced by Bruker AXS, Germany. The calculated values of instrumental limit of detection (ILD) ranged from 0.5 for Ni to 67 mg/kg for Al for soil certified reference materials (CRMs) such as OOKO151 (light chestnut soil) and from 0.2 for Cu and Ni to 18–24 mg/kg for Na for the plant CRMs such as LB‐1 (birch leaf) and EC‐1 (Canadian waterweed). The repeatability is satisfactory. The values of relative standard deviations (RSDs) do not exceed 15% for soils and available plant material. With calculated T‐statistics, it was found that the WDXRF data do not contain systematic errors. The values of relative discrepancy for WDXRF, total reflection X‐ray fluorescence (TXRF) spectrometry, and atomic emission spectrometry with arc discharge (d.c. arc‐AES) results do not exceed 30% for studied elements.
采用波长色散 X 射线荧光 (WDXRF) 光谱法测定了矮云杉 Picea canadensis conica 和蓝刺云杉 Picea pungens glauca 的针叶中 Na、Mg、Al、P、S、K、Ca、Cr、Mn、Fe、Ni、Cu、Zn、Sr、Ba 和 Pb 的浓度,以及生长这些云杉的伊尔库茨克市技术土壤中的浓度。所有测量均在真空条件下使用德国布鲁克 AXS 公司生产的 S8 TIGER 型 WDXRF 光谱仪进行。对于土壤有证标准物质(CRMs),如 OOKO151(轻栗土壤),仪器检测限 (ILD) 的计算值从 0.5(镍)到 67 mg/kg(铝)不等;对于植物有证标准物质,如 LB-1(桦树叶)和 EC-1(加拿大水草),仪器检测限 (ILD) 的计算值从 0.2(铜和镍)到 18-24 mg/kg(钠)不等。重复性令人满意。土壤和可用植物材料的相对标准偏差 (RSD) 值不超过 15%。通过计算 T 统计量,发现 WDXRF 数据不包含系统误差。对于所研究的元素,WDXRF、全反射 X 射线荧光光谱法(TXRF)和电弧放电原子发射光谱法(d.c. arc-AES)结果的相对偏差值不超过 30%。
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引用次数: 0
Fitting Compton peaks from first principles in x‐ray fluorescence spectra 从第一原理拟合 X 射线荧光光谱中的康普顿峰
IF 1.2 4区 物理与天体物理 Q3 SPECTROSCOPY Pub Date : 2024-07-05 DOI: 10.1002/xrs.3441
B. P. E. Tee, B. Ganly, J. D. Mcllquham, P. Giang, Y. Van Haarlem
A method to fit Compton profiles in x‐ray fluorescence (XRF) spectroscopy using a line shape calculated from first principles is proposed. The fitting procedure incorporates the Compton profile calculations and the double Compton scattering line shape algorithm. The results demonstrate the effectiveness of the fitting approach in accurately describing the measured scattering spectra, with good agreement observed between the fit and experimental data. The findings of this study can be used for more accurate characterization of the scattering peaks in XRF spectroscopy.
本文提出了一种利用第一原理计算出的线形拟合 X 射线荧光 (XRF) 光谱中康普顿剖面的方法。拟合程序结合了康普顿剖面计算和双康普顿散射线形算法。结果表明,拟合方法能有效准确地描述测量到的散射光谱,拟合结果与实验数据之间具有良好的一致性。这项研究的结果可用于更准确地描述 XRF 光谱中的散射峰。
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引用次数: 0
Analysis of lichen and moss samples by the EDXRF method 用电离辐射X射线荧光法分析地衣和苔藓样品
IF 1.2 4区 物理与天体物理 Q3 SPECTROSCOPY Pub Date : 2024-07-04 DOI: 10.1002/xrs.3442
P. Zuzaan, Z. Batsuren, O. Enkhtuya, E. Sosorburam, Bolortuya Damdinsuren
This research presents the contents of K, Ca, Ti, Mn, Fe, Ni, Cu, Zn, Rb, Sr, and Pb in lichen and moss samples used as biomonitors of air pollution collected in Ulaanbaatar city. X‐ray fluorescence (XRF) methods were used, employing for excitation a Pd X‐ray tube with a molybdenum secondary target. Matrix effects were corrected by the use of normalization for the coherent and incoherent scattered peak, in this way the determination is more efficient. For quality control of the results, comparisons were made with results from other certified laboratories. No significant differences were found between the different techniques. The elemental distribution patterns obtained for each metal were associated with different pollution sources, thus contributing to the assessment of air pollution in Ulaanbaatar.
本研究介绍了在乌兰巴托市采集的作为空气污染生物监测器的地衣和苔藓样本中 K、Ca、Ti、Mn、Fe、Ni、Cu、Zn、Rb、Sr 和 Pb 的含量。采用 X 射线荧光 (XRF) 方法,使用带有钼二级靶的钯 X 射线管进行激发。通过对相干和非相干散射峰进行归一化处理,校正了基质效应,从而提高了测定效率。为了对结果进行质量控制,与其他认证实验室的结果进行了比较。不同技术之间没有发现明显差异。所获得的每种金属的元素分布模式都与不同的污染源有关,因此有助于评估乌兰巴托的空气污染情况。
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引用次数: 0
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X-Ray Spectrometry
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