Andrea Paul, Zoe Liestmann, Steffen Zaenker, Kristin Vogel, Tanja Broszies, Markus Ostermann
{"title":"How reliable is the X‐ray fluorescence‐based differentiation between glass wool and rock wool and the age classification of rock wool?","authors":"Andrea Paul, Zoe Liestmann, Steffen Zaenker, Kristin Vogel, Tanja Broszies, Markus Ostermann","doi":"10.1002/xrs.3451","DOIUrl":"https://doi.org/10.1002/xrs.3451","url":null,"abstract":"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.","PeriodicalId":23867,"journal":{"name":"X-Ray Spectrometry","volume":null,"pages":null},"PeriodicalIF":1.2,"publicationDate":"2024-09-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142183583","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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
{"title":"Energy dependence of x‐ray beam size produced by polycapillary x‐ray optics","authors":"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","doi":"10.1002/xrs.3450","DOIUrl":"https://doi.org/10.1002/xrs.3450","url":null,"abstract":"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 (<jats:italic>y</jats:italic>)–energy (<jats:italic>x</jats:italic>) relation that we obtained for LBB was <jats:italic>y</jats:italic> = 185.79 exp(−0.078<jats:italic>x</jats:italic>) whose exponential component was then used to get a more accurate relation for the PFM even with the limited data set: <jats:italic>y</jats:italic> = 227.53 exp(−0.078<jats:italic>x</jats:italic>). 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.","PeriodicalId":23867,"journal":{"name":"X-Ray Spectrometry","volume":null,"pages":null},"PeriodicalIF":1.2,"publicationDate":"2024-08-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142183584","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Total reflection x‐ray fluorescence analysis of trace elements in highly saline samples","authors":"Bastian Wiggershaus, Eric Franke, Carla Vogt","doi":"10.1002/xrs.3448","DOIUrl":"https://doi.org/10.1002/xrs.3448","url":null,"abstract":"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 (Li<jats:sub>2</jats:sub>CO<jats:sub>3</jats:sub>) 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 (<jats:italic>R</jats:italic><jats:sup>2</jats:sup> > 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 <jats:italic>K</jats:italic><jats:sub><jats:italic>α</jats:italic></jats:sub>‐line of the internal standard (Ga) was used for evaluation and the use of a desiccator was found to yield the best results.","PeriodicalId":23867,"journal":{"name":"X-Ray Spectrometry","volume":null,"pages":null},"PeriodicalIF":1.2,"publicationDate":"2024-08-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142183585","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"X‐ray microanalysis and mapping for white ceramics unearthed from Gangguantun Kiln of Liaoyang, Liaoning province, China","authors":"Guiyun Shen, Jinyu Yu, Baolong Zhang, Yuanyuan Wu, Jun Zhou, Naisheng Li, Jian Zhu","doi":"10.1002/xrs.3449","DOIUrl":"https://doi.org/10.1002/xrs.3449","url":null,"abstract":"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.","PeriodicalId":23867,"journal":{"name":"X-Ray Spectrometry","volume":null,"pages":null},"PeriodicalIF":1.2,"publicationDate":"2024-08-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142183586","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
K. Hassebi, N. Rividi, Omar Boudouma, Michel Fialin, K. Le Guen, Philippe Jonnard
{"title":"X‐ray spectroscopy and quantification of an AlCuLi quasi‐crystal: A step forward for combination of reflection zone plate and crystal spectrometers","authors":"K. Hassebi, N. Rividi, Omar Boudouma, Michel Fialin, K. Le Guen, Philippe Jonnard","doi":"10.1002/xrs.3447","DOIUrl":"https://doi.org/10.1002/xrs.3447","url":null,"abstract":"We present the analysis of an AlCuLi quasi‐crystal on an electron probe microanalyser equipped with spectrometers working both in the soft and ultra‐soft x‐ray ranges. This original combination enables obtaining the Li Kα and Al L2,3 emissions with a reflection plate spectrometer and the Al Kβ and Cu Lα emissions with a curved‐crystal spectrometer. All these emissions are emission bands, sensitive to the chemical state of the emitting element. From the observation of the valence band shapes, it is confirmed that the electronic structure of the quasi‐crystal is quite different from that of the corresponding pure metals. From the measured intensities, quantification is performed using the PAP model. The weight fractions calculated from the ultra‐soft x‐ray emission intensities are very dependent on the chosen database of mass attenuation coefficients. Comparison with fractions calculated with small uncertainty in the soft x‐ray range enables choosing which databases are the most relevant for the ultra‐soft x‐ray range. Both quantifications performed from ultra‐soft and soft x‐ray emissions are compatible, leading to the Al60Cu24Li16 weight concentration of the quasi‐crystal.","PeriodicalId":23867,"journal":{"name":"X-Ray Spectrometry","volume":null,"pages":null},"PeriodicalIF":1.5,"publicationDate":"2024-08-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141927211","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Study of the chemical composition of coal and coal ash by X‐ray fluorescence method: A review","authors":"Anatoly G. Revenko, Galina V. Pashkova","doi":"10.1002/xrs.3444","DOIUrl":"https://doi.org/10.1002/xrs.3444","url":null,"abstract":"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.","PeriodicalId":23867,"journal":{"name":"X-Ray Spectrometry","volume":null,"pages":null},"PeriodicalIF":1.2,"publicationDate":"2024-07-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141777683","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Svetlana I. Shtel'makh, Alena N. Zhilicheva, Irina E. Vasil'eva
{"title":"Determination of macro‐ and microelements concentrations by wavelength‐dispersive X‐ray fluorescence spectrometry in the objects of the technogenic ecosystem","authors":"Svetlana I. Shtel'makh, Alena N. Zhilicheva, Irina E. Vasil'eva","doi":"10.1002/xrs.3443","DOIUrl":"https://doi.org/10.1002/xrs.3443","url":null,"abstract":"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 <jats:italic>Picea canadensis conica</jats:italic> and the blue prickly spruce <jats:italic>Picea pungens glauca</jats:italic>, 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.","PeriodicalId":23867,"journal":{"name":"X-Ray Spectrometry","volume":null,"pages":null},"PeriodicalIF":1.2,"publicationDate":"2024-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141777684","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
B. P. E. Tee, B. Ganly, J. D. Mcllquham, P. Giang, Y. Van Haarlem
{"title":"Fitting Compton peaks from first principles in x‐ray fluorescence spectra","authors":"B. P. E. Tee, B. Ganly, J. D. Mcllquham, P. Giang, Y. Van Haarlem","doi":"10.1002/xrs.3441","DOIUrl":"https://doi.org/10.1002/xrs.3441","url":null,"abstract":"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.","PeriodicalId":23867,"journal":{"name":"X-Ray Spectrometry","volume":null,"pages":null},"PeriodicalIF":1.2,"publicationDate":"2024-07-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141577723","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"物理与天体物理","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}