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Applications of Raman Spectroscopy in Art and Archaeology
IF 2.4 3区 化学 Q2 SPECTROSCOPY Pub Date : 2024-12-02 DOI: 10.1002/jrs.6756
Anastasia Rousaki, Juan Manuel Madariaga
<p>Raman spectroscopy is considered as one of the most valued and important techniques in the art and archaeology analysis field. Its increasing importance when the technique is applied on cultural heritage objects is reflected on the number of <i>peer reviewed</i> papers published each year on a variety of journals regarding cultural heritage science, analytical chemistry and (vibrational) spectroscopy, among others. Moreover, the importance of the application Raman spectroscopy on works of art and archaeology together with its improvements and breakthroughs is underlined on dedicated international scientific conferences (and sessions) such as the International Conference on the Application of Raman Spectroscopy in Art and Archaeology (RAA).</p><p>The RAA conferences is a great gathering of scientists working on Raman spectroscopy and its instrumental developments and an excellent opportunity to be informed on the latest advances of the technique on Cultural Heritage studies. The first edition of the RAA conference was realized in London in 2001 [<span>1</span>], followed by Ghent (2003) [<span>2</span>] and then Paris (2005) [<span>3</span>], Modena (2007) [<span>4</span>], Bilbao (2009) [<span>5</span>], Parma (2011) [<span>6</span>], Ljubljana (2013) [<span>7</span>], Wroclaw (2015) [<span>8</span>], Évora (2017) [<span>9</span>] and Potsdam (2019) [<span>10</span>]. The 11<sup>th</sup> edition of the RAA conference (RAA2023, 6 to 9 September 2023) was hosted by the National Gallery-Alexandros Soutsos Museum, located in Athens, Greece in collaboration with Ghent University, Ghent, Belgium. For the first time, the RAA2023 conference included a <i>two-day</i> Raman spectroscopy training school (4 to 5 September 2023) on selected topics addressed to students and early career researchers.</p><p>As the previous editions, the scientific programme was focused on characterization of materials associated with cultural heritage research (natural and synthetic inorganic and organic materials including biological materials), degradation processes, conservation related themes and challenges, surface enhanced Raman spectroscopy (SERS), chemometrics, Raman spectroscopy related topics in paleontology, paleoenvironment and archaeology, the development and progresses of Raman techniques and the application, advantages and challenges of new Raman instrumentation. The aforementioned topics can be connected either to laboratory or in situ analysis, or both while Raman spectroscopy should act as a core technique in studies that include other analytical techniques. During the RAA2023, these type of studies were organized in 3 keynote and 1 plenary lectures, 30 oral presentations, 4 sponsor oral presentations and 37 poster presentations. The RAA2023 conference garnered 100 registries from 21 countries. There were 332 authors and co-authors in the studies of the conference's scientific programme.</p><p>This special issue includes 14 selected manuscripts reflecting th
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引用次数: 0
The Complementary Use of Raman, ATR-FTIR Spectroscopy, and Chemometrics for Investigating the Deterioration of Artificially Aged Parchment
IF 2.4 3区 化学 Q2 SPECTROSCOPY Pub Date : 2024-12-02 DOI: 10.1002/jrs.6755
Ekaterini Malea, Stamatis C. Boyatzis, Dimitris Karlis, Dimitrios Palles, Soghomon Boghosian, Spiros Zervos

Among the materials constituting our cultural heritage, parchment has a significant role as the substrate of many archival documents. The assessment of its state of preservation has an important benefit to conservation and delineates the adequate preventive measures that would lead to better-controlled storage and exhibition conditions in museums and libraries worldwide. In the framework of this project, artificial aging of 48 new goat parchment samples was performed to induce deterioration similar to naturally aged parchment exposed to atmospheric pollutants. Five factors have been examined: relative humidity; NO2; SO2; exposure time, and the order of sequential exposure to NO2 and SO2. Temperature was kept constant at 25°C, while the effect of the above-mentioned factors was examined at two levels (low and high). Statistics was involved in advance in the experimental design. Raman spectroscopy along with attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectroscopy were used to investigate the condition of collagen in parchment. The entire set of environmental factors along with detected changes in the spectra were investigated through a chemometrics scheme involving analysis of variance (ANOVA). According to the results, the onset of collagen's secondary structure decomposition was observed. Statistical elaboration of data reveals that the two analytical methods (Raman and ATR-FTIR) function in a complementary manner related to the molecular changes and the chemical reactions that happen. In conclusion, both methods can increase their impact on the investigation of parchment degradation if they are combined with other analytical methods and chemometric applications.

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引用次数: 0
Archaeometric Study of the Colorants in the Finds From the 4th Century BC Cist Tomb at Lakkoma, Chalcidice
IF 2.4 3区 化学 Q2 SPECTROSCOPY Pub Date : 2024-11-28 DOI: 10.1002/jrs.6754
Svetlana Vivdenko, Athina Vasileiadou, Maria Tsimbidou-Avlonitou, Alexandros Konstanta, Lydia Avlonitou, Nikolaos Zacharias

The analytical findings concerning the red pigments used on various decorative features originating from a Macedonian, as well as the purple dye from the deceased's attire, are presented. The cist tomb, discovered in 1987 at the area of Lakkoma Chalcidice (Macedonia, Greece), dated to the 4th century bc and featured a wooden funeral couch with intricate ornaments, such as clay “eyes,” colored plaster, and clay gorgoneions. Vermilion and red ochre served as the main pigments of these decorative features. The pigments were applied in various combinations to produce a range of red hues, from deep to bright red. Furthermore, the precious vermilion was also used in every element of the couch. The stucco on the decoration was gypsum, whereas the preparation layers over clay and stucco elements consisted of calcite and lead white, respectively. The cloth covering the deceased was dyed with the most expensive organic dye of antiquity, the Tyrian (shellfish) purple. In this research, the preliminary identification of the chromophoric minerals in the colors of the samples was carried out with the examination of their optical characteristics in thin sections using polarizing light microscope (PLM) and with portable XRF. Physicochemical techniques, Raman and HPLC, were also used to definitively identify the pigments. Portable Raman spectrometer was used for the in situ analysis of the inorganic colorants of the decorative materials, whereas laboratory Raman spectrometer served for the identification of inorganic and organic colorants of the grain samples and the dye. High-pressure liquid chromatography with diode array detector (HPLC-DAD) was applied for the identification of the coloring components of the purple organic dye from the deceased's clothes. The samples examined (0.5- to 1.5-mm diameter) were collected during the initial cleaning of the surface.

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引用次数: 0
Rapid and Accurate Identification of Dyes on Ancient Textiles by SERS With a Negligibly Invasive Approach
IF 2.4 3区 化学 Q2 SPECTROSCOPY Pub Date : 2024-10-01 DOI: 10.1002/jrs.6737
Xiao-Han Xi, Yun Zhang, Sen Yan, Ping-Shi Wang, Hao Ma, Meng Ren, Guo-Kun Liu, Yong Lei, Bin Ren, Xiang Wang

Nowadays, surface-enhanced Raman spectroscopy (SERS) has become a powerful tool for rapidly detecting and analyzing textile cultural relics due to its ability to provide chemical information with single-molecule sensitivity. However, preserving a high level of detection sensitivity while avoiding sample damage remains a persistent challenge. In this work, we developed a SERS approach with both microextraction and detection functions. The alcohol–water droplet with iodide-modified Au nanoparticles (AuIMNPs) is directly dropped on the textile, where dyes strongly bound on textiles can be extracted by ethanol (EtOH). As a result, the sample can be well preserved from being damaged. In particular, the volatility of EtOH allows the molecules to be captured in the hot spots through the capillary effect during droplet evaporation, resulting in a dramatic increase in Raman signal intensity. This highly sensitive strategy can be used to measure dyes in plant extracts and mock-up textiles. Furthermore, the capability of SERS to provide fingerprint information allows us to distinguish different dyes in overdyeing textiles. Eventually, this approach is successfully applied to identify dyes of authentic ancient Chinese textiles. This rapid, universal, and negligibly invasive approach provides a powerful way to study textile cultural relics.

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引用次数: 0
Microstructural Study of the Coloring Variation of Chinese Sauce Glaze Replications
IF 2.4 3区 化学 Q2 SPECTROSCOPY Pub Date : 2024-09-23 DOI: 10.1002/jrs.6736
Tian Wang, Senwei Xia, Zhao Ren, Clement Hole, Fen Wang, Jianfeng Zhu, Hongjie Luo, Qiang Li, Meihong Liao, Philippe Sciau

Sauce glazed wares of Yaozhou kilns are famous for their high gloss and distinctive glaze color palette varying from yellowish-brown to reddish-brown. In this work, sauce glazes were successfully replicated using the traditional technology of Yaozhou kilns. Micro-Raman spectroscopy, combined with optical microscopy, scanning electron microscopy, x-ray fluorescence, and reflective spectroscopy, was systematically applied to analyze the chemical composition, nature and distribution of crystals, and the coloration of the glazes. The results show that the yellowish-brown glaze is mainly original from dendritic ε-Fe2O3 crystals, whereas the reddish-brown color is mainly derived from dendritic hematite crystals. Such dendritic structure could account for slightly color variations of the glaze surface observed in different angles, which also reported in Japanese Bizen ceramics. The principal component analysis (PCA) was further applied to study the Raman spectra of these iron oxides. The PCA results effectively indicates the structural disorders of these crystals introduced by ion substitutions. These substitutions could not only stabilize the crystals but also darken the crystals color. Besides, high Mg in the raw materials was found to benefit the growth of magnesioferrite crystals. The relative low level of Fe2O3, high level of SiO2, and CaO may relate to the formation of ε-Fe2O3 crystals.

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引用次数: 0
A Novel Incident Circular Polarized Light Raman Optical Activity (ICP‐ROA) Spectrometer With Advanced Polarization Control 具有先进偏振控制功能的新型入射圆偏振光拉曼光学活性 (ICP-ROA) 光谱仪
IF 2.5 3区 化学 Q2 SPECTROSCOPY Pub Date : 2024-09-18 DOI: 10.1002/jrs.6733
Klaus Hofmann, Luisa Martin, Ingo Fischer
The design and setup of a novel and simple backscatter Raman optical activity (ROA) spectrometer with incident light circular polarization (ICP) is presented, constructed from commercially available components. Incident light polarization is controlled using a combination of waveplates, compensating for unwanted birefringence and beam offsets. Realignment of the spectra in post‐processing reduced artifacts caused by spatial offsets. Spurious signals from achiral solvents like toluene and water are almost completely removed. The setup was validated by measuring references samples, including α‐pinene, carvone, and glucose in aqueous solution. The spectra show very good agreement with previously published results.
本文介绍了一种新颖而简单的入射光圆偏振(ICP)反向散射拉曼光学活动(ROA)光谱仪的设计和设置。入射光偏振通过波板组合进行控制,以补偿不必要的双折射和光束偏移。在后处理中重新调整光谱,减少了空间偏移造成的伪影。几乎完全消除了来自甲苯和水等非手性溶剂的杂散信号。通过测量参考样品,包括水溶液中的α-蒎烯、香芹酮和葡萄糖,对该装置进行了验证。光谱结果与之前公布的结果非常吻合。
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引用次数: 0
Sensitivity of the C–H Stretching Band in Raman Spectra to Phospholipid Order 拉曼光谱中的 C-H 伸展带对磷脂阶次的敏感性
IF 2.4 3区 化学 Q2 SPECTROSCOPY Pub Date : 2024-09-18 DOI: 10.1002/jrs.6731
Yulia V. Zaytseva, Konstantin A. Okotrub, Nikolai V. Surovtsev

Phospholipid bilayers, which are a major component of cellular membranes and some drug delivery vehicles, can be in different states of order depending on the conformations of the hydrocarbon tails and their mutual arrangement. The important task of experimental characterization of phospholipid order is often addressed using Raman spectra of the C–H stretching bands. Such characterization uses some empirical relationships for apparent maxima in the spectra, although the origin of the sensitivity of the C–H band to phospholipid order and its model description remain unclear. Surely, a correct description of the sensitivity of the C–H band to phospholipid order is critical for its proper application. Here, we provide a description of the ordering sensitivity of the C–H stretching band using a polarized Raman experiment with hydrated aligned multibilayers of a saturated phospholipid. By this way, Raman contributions from symmetric and antisymmetric vibrations of CH2 were obtained in a model-free manner. Experiments in a wide temperature range and the use of isotopic isolation helped us to consider separately the effects of conformational and lateral order of chains. The conformational sensitivity of the spectrum of antisymmetric vibrations was confirmed by DFT modeling. The outcomes of the study allowed us to provide recommendations for the use of the Raman spectrum of the C–H stretching band to characterize the conformational and lateral order of phospholipid-containing materials.

磷脂双分子层是细胞膜和某些药物输送载体的主要成分,根据碳氢化合物尾部的构象及其相互排列,磷脂双分子层可以处于不同的有序状态。磷脂秩的实验表征这一重要任务通常使用 C-H 伸展带的拉曼光谱来完成。尽管 C-H 带对磷脂秩的敏感性的来源及其模型描述仍不清楚,但这种表征使用了光谱中明显最大值的一些经验关系。当然,正确描述 C-H 带对磷脂阶次的敏感性对其正确应用至关重要。在此,我们利用饱和磷脂水合排列多层的偏振拉曼实验,对 C-H 伸展带的有序敏感性进行了描述。通过这种方法,以无模型的方式获得了来自 CH2 对称和非对称振动的拉曼贡献。宽温度范围内的实验和同位素隔离的使用帮助我们分别考虑了链的构象和横向顺序的影响。DFT 建模证实了反对称振动谱的构象敏感性。研究结果使我们能够为使用 C-H 伸展带的拉曼光谱来表征含磷脂材料的构象和横向顺序提供建议。
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引用次数: 0
Noninvasive Multitechnique Analysis of Baroque Amber Artworks From Gdansk: The Benefits of Using Raman Spectroscopy 对来自格但斯克的巴洛克琥珀艺术品进行非侵入式多技术分析:使用拉曼光谱的好处
IF 2.4 3区 化学 Q2 SPECTROSCOPY Pub Date : 2024-09-10 DOI: 10.1002/jrs.6727
Anna Rygula, Anna Klisińska-Kopacz, Marta Matosz, Tomasz Wilkosz, Michał Obarzanowski, Paulina Krupska-Wolas, Karolina Skóra, Aldona Kopyciak, Joanna Harasim-Grym, Julio M. del Hoyo-Meléndez

The multidisciplinary, noninvasive analysis of baroque amber artworks is part of a research project that deals with the most valuable objects from the Museum of Gdansk (Poland). The two most interesting objects will be presented here: a Baroque Gdansk wardrobe-shaped amber cabinet (made by Johann Georg Zernebach, Gdansk, 1724) and a crucifix (Gdansk, 17th century). Macro- (UV, IR, and X-radiography) and micro- (XRF and Raman spectroscopy) analytical methods were applied to reveal traces of old conservation treatments and uncover the techniques of the 17th and 18th century amber masters. UV photography shows the differences between the amber plates that are not so easily detected under visible light, while XRF spectrometry detects elements atypical for amber objects, suggesting previous conservation treatments. Confocal Raman measurements, especially Raman depth profiling, were performed for the amber artworks and allowed to detect areas of previous conservation treatments. Single-point scans were collected from the surface (0 μm) to a depth of −200 μm, with a step of 50 μm. The results allowed us to identify three different types of zones: where the amber was preserved without any protective layer, places where the amber was covered with a thin layer of a protective substance, and places where amber elements were compensated for loss using a binding agent and filler. The presented project allowed the development of a comprehensive methodology for the analysis of amber objects, especially to optimize the capabilities of confocal Raman microscopy. The combination of macro- and microanalytical techniques made it possible to obtain a broad overview of such complex artworks while optimizing the time and effort spent on the investigations.

对巴洛克琥珀艺术品的多学科、非侵入性分析是格但斯克博物馆(波兰)最珍贵文物研究项目的一部分。这里将介绍两件最有趣的物品:一个巴洛克时期格但斯克衣橱形琥珀柜(由约翰-乔治-泽内巴赫制作,格但斯克,1724 年)和一个十字架(格但斯克,17 世纪)。应用宏观(紫外线、红外线和 X 射线)和微观(XRF 和拉曼光谱)分析方法揭示了旧的保存处理痕迹,并揭示了 17 和 18 世纪琥珀大师的技艺。紫外线摄影显示了在可见光下不易察觉的琥珀板之间的差异,而 XRF 光谱法则检测出了琥珀物品的非典型元素,表明了以前的保护处理。对琥珀艺术品进行共焦拉曼测量,特别是拉曼深度剖面测量,可以检测出曾经进行过保护处理的区域。从表面(0 μm)到-200 μm的深度进行了单点扫描,扫描步长为50 μm。结果使我们确定了三种不同类型的区域:没有任何保护层的琥珀保存区、琥珀被一层薄薄的保护层覆盖的地方,以及使用粘合剂和填充物补偿琥珀元素损失的地方。该项目为分析琥珀物品开发了一套全面的方法,尤其是优化了共焦拉曼显微镜的功能。宏观和微观分析技术的结合使我们有可能对此类复杂的艺术品进行全面的了解,同时优化了调查所花费的时间和精力。
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引用次数: 0
Micro-Raman Spectroscopy for the Identification of Drawing Materials Used Throughout the 17th and 20th Centuries 利用微拉曼光谱鉴定 17 世纪和 20 世纪使用的绘画材料
IF 2.4 3区 化学 Q2 SPECTROSCOPY Pub Date : 2024-09-09 DOI: 10.1002/jrs.6728
Anna Klisińska-Kopacz, Anna Ryguła, Julio M. del Hoyo Meléndez

The study explores drawing materials from the 17th century to the present using noninvasive techniques like Raman spectroscopy in selected cases supplemented by x-ray fluorescence (XRF) spectroscopy. This publication is an effort to expand knowledge across diverse periods and materials. A collection of six drawings spanning from 1700 to 1899 from the National Museum in Krakow and a 20th-century birch bark artifact were analyzed. Noninvasive techniques facilitated the systematic analysis of drawing materials, providing insights into diverse substances over centuries. Identified materials include hematite, calcite, graphite, bister, sepia, iron gall ink, and crystal violet dye. Understanding the chemical composition aids conservation and is a reference for future art history and preservation studies.

这项研究利用拉曼光谱等非侵入性技术,并辅以 X 射线荧光 (XRF) 光谱法,对 17 世纪至今的绘画材料进行了探索。该出版物旨在扩展不同时期和不同材料的知识。我们分析了克拉科夫国家博物馆收藏的 1700 年至 1899 年的六幅图画和一件 20 世纪的桦树皮工艺品。非侵入式技术有助于对绘画材料进行系统分析,从而深入了解几个世纪以来的各种物质。经鉴定的材料包括赤铁矿、方解石、石墨、铋剂、棕褐色、铁胆墨水和水晶紫染料。了解化学成分有助于保存,并为今后的艺术史和保存研究提供参考。
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引用次数: 0
Quantitative Raman Spectroscopy of Urea and Thiourea in the Reaction Mixtures of Allantoin and 4,5-Dihydroxyimidazolidine-2-Tione Formation 尿囊素和 4,5-二羟基咪唑烷-2-硫酮反应混合物中尿素和硫脲的定量拉曼光谱分析
IF 2.4 3区 化学 Q2 SPECTROSCOPY Pub Date : 2024-09-01 DOI: 10.1002/jrs.6729
L. E. Kalichkina, P. K. Krivolapenko, V. P. Tuguldurova

The present work introduces a new approach to quantitative determine the reagent concentrations (thiourea and urea) using in situ Raman spectroscopy in the reaction mixture exemplified by the reactions of formation of allantoin and 4,5-dihydroxyimidazolidine-2-thione. The approach comprises the use of a commercially available immersion probe (MarqMetrix Process Elite BallProbe with sapphire lens) as a standard for the immersion probe band at 790 cm−1 of optical glass. This leads to a linear dependence of the ratio of the intensity of non-overlapping analyte bands at 1003 cm−1 of -C-N- vibrations in urea to the one of the 790 cm−1 immersion probe band on the concentration of urea in the test solution. The definable method parameters such as precision (repeatability and reproducibility), linearity, limit of detection (LoD), limit of quantitation (LoQ), and accuracy were determined. The quantitative Raman spectroscopy method is linear, precise within the range of determined concentrations from 0.75 to 2.00 M and can be used to calculate the kinetics of allantoin formation. Using thiourea as an example, it is shown that despite the partial overlap of the analyte band at 730 cm−1 of the -C=S vibrations of thiourea with the immersion probe band at 790 cm−1, the method to determine thiourea in the reaction of 4,5-dihydroxyimidazolidine-2-thione preparation is also linear and precise in the range of determined concentrations from 0.10 to 1.57 M.

本研究以尿囊素和 4,5-二羟基咪唑烷-2-硫酮的生成反应为例,介绍了一种利用反应混合物中的原位拉曼光谱定量测定试剂浓度(硫脲和尿素)的新方法。该方法包括使用市售的浸入式探针(带蓝宝石透镜的 MarqMetrix Process Elite BallProbe)作为光学玻璃 790 cm-1 处浸入式探针带的标准。因此,尿素中 -C-N- 振动 1003 cm-1 处非重叠分析带的强度与 790 cm-1 浸入探针带的强度之比,与测试溶液中尿素的浓度呈线性关系。测定了方法的精密度(重复性和再现性)、线性度、检出限(LoD)、定量限(LoQ)和准确度等可定义的参数。定量拉曼光谱法线性好,在 0.75 至 2.00 M 的测定浓度范围内精确度高,可用于计算尿囊素的形成动力学。以硫脲为例,尽管硫脲的 -C=S 振荡的 730 cm-1 分析带与 790 cm-1 的浸入探针带有部分重叠,但在 4,5-二羟基咪唑烷-2-硫酮制备反应中测定硫脲的方法在 0.10 至 1.57 M 的测定浓度范围内也是线性和精确的。
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引用次数: 0
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Journal of Raman Spectroscopy
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