Environmental pollution as a result of industrial activity is widespread in many urban areas including Chicago. In an effort to evaluate the heavy metal fraction originating from industrial activities, plant samples of Daucus Carota or wild carrot were collected at or adjacent to six sites located in two of Chicago's designated industrial corridors. Plants, especially herbaceous species, have been deemed suitable as environmental pollution monitors as they are able to provide information about the heavy metal fraction accessible to biota. The leaves of Daucus Carota were acid digested and analyzed with total reflection X‐ray fluorescence spectrometry TXRF. The results showed elevated heavy metal mass fractions for at least one collection site which is close to an operational railyard. Other studies investigating heavy metals in proximity to railroad operations found elevated mass fractions for several elements, but specifically manganese as well. This suggests that abrasion from shunting and breaking releases certain pollutants into the local environment. The data were compared with studies executed in Rome, Italy, and Pakistan, which used Daucus Carota to evaluate heavy metal pollution. It was found that the heavy metal mass fractions obtained for Chicago were higher for some elements indicating an increased pollutant burden for these elements. The same samples were also analyzed by graphite furnace atomic absorption spectrometry GFAAS for the elements copper and lead and the data compared. Those two elements were chosen as they were present at each location and GFAAS has proven to be highly sensitive for them. It was found that the two methods provided comparable results for copper, whereas for lead, TXRF overestimated the mass fractions most likely due to limitations of the spectra evaluation software. The analysis of a certified reference material ‘BCR 679 white cabbage’ showed that most data obtained by TXRF were in good agreement with the certified values, with the exception of lead, which was not certified. However, since GFAAS has high sensitivity toward lead and is considered reference method for that element by regulatory agencies, a comparison between GFAAS and TXRF data for lead in the same sample can serve as good indicator for TXRF performance.
{"title":"Biomonitoring of urban industrial pollution using total reflection X‐ray fluorescence","authors":"M. Schmeling, M. Gende, A. Tovar","doi":"10.1002/xrs.3439","DOIUrl":"https://doi.org/10.1002/xrs.3439","url":null,"abstract":"Environmental pollution as a result of industrial activity is widespread in many urban areas including Chicago. In an effort to evaluate the heavy metal fraction originating from industrial activities, plant samples of <jats:italic>Daucus Carota</jats:italic> or wild carrot were collected at or adjacent to six sites located in two of Chicago's designated industrial corridors. Plants, especially herbaceous species, have been deemed suitable as environmental pollution monitors as they are able to provide information about the heavy metal fraction accessible to biota. The leaves of <jats:italic>Daucus Carota</jats:italic> were acid digested and analyzed with total reflection X‐ray fluorescence spectrometry TXRF. The results showed elevated heavy metal mass fractions for at least one collection site which is close to an operational railyard. Other studies investigating heavy metals in proximity to railroad operations found elevated mass fractions for several elements, but specifically manganese as well. This suggests that abrasion from shunting and breaking releases certain pollutants into the local environment. The data were compared with studies executed in Rome, Italy, and Pakistan, which used <jats:italic>Daucus Carota</jats:italic> to evaluate heavy metal pollution. It was found that the heavy metal mass fractions obtained for Chicago were higher for some elements indicating an increased pollutant burden for these elements. The same samples were also analyzed by graphite furnace atomic absorption spectrometry GFAAS for the elements copper and lead and the data compared. Those two elements were chosen as they were present at each location and GFAAS has proven to be highly sensitive for them. It was found that the two methods provided comparable results for copper, whereas for lead, TXRF overestimated the mass fractions most likely due to limitations of the spectra evaluation software. The analysis of a certified reference material ‘BCR 679 white cabbage’ showed that most data obtained by TXRF were in good agreement with the certified values, with the exception of lead, which was not certified. However, since GFAAS has high sensitivity toward lead and is considered reference method for that element by regulatory agencies, a comparison between GFAAS and TXRF data for lead in the same sample can serve as good indicator for TXRF performance.","PeriodicalId":23867,"journal":{"name":"X-Ray Spectrometry","volume":"148 1","pages":""},"PeriodicalIF":1.2,"publicationDate":"2024-06-25","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141508116","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}
Paula Silveira, Hugo Marcelo Veit, Johnny Dias, Tiago Falcade
Historical heritage pieces allow a better comprehension of the characteristics of different civilizations over time. The characterization of such pieces is of paramount importance for their preservation. Energy‐dispersive X‐ray fluorescence (EDXRF) is recommended for this application, mostly because it is non‐destructive and the equipment is portable. However, one of its limitations is the difficulty in separating the signal from the substrate and the coating of multilayered samples, as it does not provide depth resolution. This project investigates the application of EDXRF in the characterization of metallic coatings, in the context of historical heritage. The elemental concentration of electrodeposited Ni coatings onto carbon steel substrates was obtained from EDXRF analyses. The relationship between the layer thickness and the variation of the Kα/Kβ intensity ratio of nickel peaks was exploited and the thicknesses of the coatings were estimated through EDXRF measurements. For comparison, particle‐induced x‐ray emission spectroscopy and scanning electron microscopy of the cross‐section were employed, providing a depth profile of the coatings. The estimated thicknesses from EDXRF analysis were comparable to those observed in the microscopy images for thinner films (up to 8 μm). On the other hand, for thicker films, the thicknesses were underestimated, due to the technique's depth limit and matrix effects, as secondary absorption. Despite these limitations, EDXRF remains valuable for evaluating cultural heritage pieces, often providing sufficient information to address authenticity concerns or to guide restoration processes. A case study was also performed to apply the methodology discussed on historical metallic pieces.
历史遗产可以让人们更好地了解不同文明在不同时期的特征。对这些文物进行鉴定对其保护至关重要。能量色散 X 射线荧光 (EDXRF) 被推荐用于这种应用,主要是因为它是非破坏性的,而且设备便于携带。然而,其局限性之一是难以将信号从多层样品的基底和涂层中分离出来,因为它无法提供深度分辨率。本项目以历史遗产为背景,研究了电离辐射 X 射线荧光光谱在金属涂层表征中的应用。通过 EDXRF 分析获得了碳钢基底上电解沉积镍涂层的元素浓度。利用镀层厚度与镍峰 Kα/Kβ 强度比值变化之间的关系,通过 EDXRF 测量估算了镀层厚度。为了进行比较,还使用了粒子诱导 X 射线发射光谱和横截面扫描电子显微镜,以提供涂层的深度剖面图。对于较薄的薄膜(最厚 8 μm),EDXRF 分析得出的估计厚度与显微镜图像中观察到的厚度相当。另一方面,对于较厚的薄膜,由于该技术的深度限制和基质效应(二次吸收),厚度被低估了。尽管存在这些局限性,EDXRF 对于评估文化遗产仍然很有价值,通常可以提供足够的信息来解决真实性问题或指导修复过程。我们还进行了一项案例研究,将所讨论的方法应用于历史上的金属文物。
{"title":"Investigation of the X‐ray fluorescence technique in the characterization of Ni coatings applied to historical heritage studies","authors":"Paula Silveira, Hugo Marcelo Veit, Johnny Dias, Tiago Falcade","doi":"10.1002/xrs.3429","DOIUrl":"https://doi.org/10.1002/xrs.3429","url":null,"abstract":"Historical heritage pieces allow a better comprehension of the characteristics of different civilizations over time. The characterization of such pieces is of paramount importance for their preservation. Energy‐dispersive X‐ray fluorescence (EDXRF) is recommended for this application, mostly because it is non‐destructive and the equipment is portable. However, one of its limitations is the difficulty in separating the signal from the substrate and the coating of multilayered samples, as it does not provide depth resolution. This project investigates the application of EDXRF in the characterization of metallic coatings, in the context of historical heritage. The elemental concentration of electrodeposited Ni coatings onto carbon steel substrates was obtained from EDXRF analyses. The relationship between the layer thickness and the variation of the Kα/Kβ intensity ratio of nickel peaks was exploited and the thicknesses of the coatings were estimated through EDXRF measurements. For comparison, particle‐induced x‐ray emission spectroscopy and scanning electron microscopy of the cross‐section were employed, providing a depth profile of the coatings. The estimated thicknesses from EDXRF analysis were comparable to those observed in the microscopy images for thinner films (up to 8 μm). On the other hand, for thicker films, the thicknesses were underestimated, due to the technique's depth limit and matrix effects, as secondary absorption. Despite these limitations, EDXRF remains valuable for evaluating cultural heritage pieces, often providing sufficient information to address authenticity concerns or to guide restoration processes. A case study was also performed to apply the methodology discussed on historical metallic pieces.","PeriodicalId":23867,"journal":{"name":"X-Ray Spectrometry","volume":"1 1","pages":""},"PeriodicalIF":1.2,"publicationDate":"2024-05-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140841815","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}
Khalil Hassebi, Nicolas Rividi, Michel Fialin, Anne Verlaguet, Gaston Godard, Jürgen Probst, Heike Löchel, Thomas Krist, Christoph Braig, Christian Seifert, Rabah Benbalagh, Régis Vacheresse, Vita Ilakovac, Karine Le Guen, Philippe Jonnard
Implementing a newly developed spectrometer for the soft x‐ray range of (35–130) eV based on reflection zone plates was successfully accomplished on an electron probe microanalyzer. In this context, we present the first spectra acquired using this setup, including those of elements such as Be (Kα), C (Kα), Mg (L2,3), Al (L2,3), and Si (L2,3). We have also conducted an analysis of several lithium compounds and measured the emission of Li Kα from metallic Li, LiF, and LiNbO3. Some of the results were compared with density functional theory calculations. The spectrum obtained for the lithium‐bearing mineral amblygonite Li0.75Na0.25Al(PO4)F0.75(OH)0.25 is chosen to discuss some of the challenges faced.
在电子探针显微分析仪上成功实现了基于反射区板的新开发的 (35-130) eV 软 X 射线范围光谱仪。在此背景下,我们展示了利用该装置获得的第一批光谱,包括 Be (Kα)、C (Kα)、Mg (L2,3)、Al (L2,3) 和 Si (L2,3) 等元素的光谱。我们还对几种锂化合物进行了分析,并测量了金属锂、LiF 和 LiNbO3 的 Li Kα 发射。其中一些结果与密度泛函理论计算结果进行了比较。我们选择了含锂矿物伏锂辉石 Li0.75Na0.25Al(PO4)F0.75(OH)0.25 的光谱来讨论所面临的一些挑战。
{"title":"High‐resolution x‐ray emission spectrometry in the lithium K range with a reflection zone plate spectrometer","authors":"Khalil Hassebi, Nicolas Rividi, Michel Fialin, Anne Verlaguet, Gaston Godard, Jürgen Probst, Heike Löchel, Thomas Krist, Christoph Braig, Christian Seifert, Rabah Benbalagh, Régis Vacheresse, Vita Ilakovac, Karine Le Guen, Philippe Jonnard","doi":"10.1002/xrs.3427","DOIUrl":"https://doi.org/10.1002/xrs.3427","url":null,"abstract":"Implementing a newly developed spectrometer for the soft x‐ray range of (35–130) eV based on reflection zone plates was successfully accomplished on an electron probe microanalyzer. In this context, we present the first spectra acquired using this setup, including those of elements such as Be (Kα), C (Kα), Mg (L<jats:sub>2,3</jats:sub>), Al (L<jats:sub>2,3</jats:sub>), and Si (L<jats:sub>2,3</jats:sub>). We have also conducted an analysis of several lithium compounds and measured the emission of Li Kα from metallic Li, LiF, and LiNbO<jats:sub>3</jats:sub>. Some of the results were compared with density functional theory calculations. The spectrum obtained for the lithium‐bearing mineral amblygonite Li<jats:sub>0.75</jats:sub>Na<jats:sub>0.25</jats:sub>Al(PO<jats:sub>4</jats:sub>)F<jats:sub>0.75</jats:sub>(OH)<jats:sub>0.25</jats:sub> is chosen to discuss some of the challenges faced.","PeriodicalId":23867,"journal":{"name":"X-Ray Spectrometry","volume":"212 1","pages":""},"PeriodicalIF":1.2,"publicationDate":"2024-04-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140629450","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}
Olga Yu. Belozerova, Victor S. Antipin, Larisa V. Kushch, D. Odgerel
The multicomponent technique of x‐ray electron probe microanalysis for rock‐forming and minor minerals of granites, pegmatites, and metasomatites was developed using the scanning electron microscopy (SEM) and x‐ray electron probe microanalysis (EPMA) methods. The conditions for excitation and recording of elements analytical lines were chosen taking into account the properties of the investigated material. The distortion of analytical signal due to the effect of mutual overlapping of determined elements analytical lines was corrected using overlap coefficients, previously determined on the samples that did not contain the determined element. An assessment of metrological characteristics of EPMA technique showed, that it satisfies the requirements for the second category of quality of quantitative determinations and the second category of analyses adopted in the International Program for Professional Testing of Geoanalytical Laboratories (GeoPT). This developed technique was used for studying rare‐metal granites, pegmatites, and metasomatites of Central Mongolia (multiphase Baga Gazriin massif).
利用扫描电子显微镜(SEM)和 X 射线电子探针显微分析(EPMA)方法,开发了针对花岗岩、伟晶岩和变质岩的成岩矿物和次要矿物的多组分 X 射线电子探针显微分析技术。在选择元素分析线的激发和记录条件时,考虑了所研究材料的特性。由于测定的元素分析线相互重叠而造成的分析信号失真,使用重叠系数进行了校正,重叠系数是之前在不含测定元素的样品上测定的。对 EPMA 技术计量特性的评估表明,该技术符合《国际地质分析实验室专业测试计划》(GeoPT)采用的第二类定量测定质量要求和第二类分析要求。所开发的这一技术被用于研究蒙古中部(多相 Baga Gazriin 地块)的稀有金属花岗岩、伟晶岩和变质岩。
{"title":"Investigation of rare‐metal granites, pegmatites, and metasomatites minerals of Mongolia by scanning electron microscopy and x‐ray electron probe microanalysis methods","authors":"Olga Yu. Belozerova, Victor S. Antipin, Larisa V. Kushch, D. Odgerel","doi":"10.1002/xrs.3428","DOIUrl":"https://doi.org/10.1002/xrs.3428","url":null,"abstract":"The multicomponent technique of x‐ray electron probe microanalysis for rock‐forming and minor minerals of granites, pegmatites, and metasomatites was developed using the scanning electron microscopy (SEM) and x‐ray electron probe microanalysis (EPMA) methods. The conditions for excitation and recording of elements analytical lines were chosen taking into account the properties of the investigated material. The distortion of analytical signal due to the effect of mutual overlapping of determined elements analytical lines was corrected using overlap coefficients, previously determined on the samples that did not contain the determined element. An assessment of metrological characteristics of EPMA technique showed, that it satisfies the requirements for the second category of quality of quantitative determinations and the second category of analyses adopted in the International Program for Professional Testing of Geoanalytical Laboratories (GeoPT). This developed technique was used for studying rare‐metal granites, pegmatites, and metasomatites of Central Mongolia (multiphase Baga Gazriin massif).","PeriodicalId":23867,"journal":{"name":"X-Ray Spectrometry","volume":"12 1","pages":""},"PeriodicalIF":1.2,"publicationDate":"2024-04-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140614883","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}
Yasuto Isozumi, Jun Kawai, Takeshi Mukoyama, Fumitaka Nishiyama, Takashi Yamada
{"title":"Escape peaks of Ge detector in X‐ray fluorescence (XRF)","authors":"Yasuto Isozumi, Jun Kawai, Takeshi Mukoyama, Fumitaka Nishiyama, Takashi Yamada","doi":"10.1002/xrs.3426","DOIUrl":"https://doi.org/10.1002/xrs.3426","url":null,"abstract":"","PeriodicalId":23867,"journal":{"name":"X-Ray Spectrometry","volume":"149 1","pages":""},"PeriodicalIF":1.2,"publicationDate":"2024-04-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140572745","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}