Analysis Of Microsamples Research Articles

Upgrade of the ion beam analysis end-station with the wavelength dispersive X-ray spectrometer for use with the focused MeV ion beams

A novel modular end-station has been developed for use with focused MeV ion beams. It supports analysis of micro-samples using simultaneously several ion beam analysis (IBA) techniques, including wavelength dispersive (WD) and energy dispersive (ED) Particle Induced X-ray Emission (PIXE) spectrometry, Elastic Backscattering Spectrometry (EBS and RBS) and Nuclear Reaction Analysis (NRA). The end-station enables quantitative elemental analysis, including the creation of two-dimensional elemental maps based on the ED-PIXE and EBS/RBS/NRA measurements. The in-house developed wavelength dispersive X-ray (WDX) spectrometer can measure high energy resolution spectra on selected sample micro-regions. In this work the description of the modular end-station is presented, highlighting the features of the WDX spectrometer: i) in the complementary analysis of complex ED X-ray spectra with many overlapping peaks measured simultaneously and ii) in chemical speciation studies. An example is presented to demonstrate the capabilities of the modular system for simultaneous analytical measurements of selected heterogeneous micro-samples.

Miniaturized confocal Raman and Laser-induced breakdown spectroscopy imaging system based on micro-electro-mechanical mirror

Detection of the elemental and molecular structural distribution with high resolution and miniaturization of unknown minerals is a main bottleneck in deep space exploration and geology analysis. The aim is to enhance the accuracy of the chemical analysis of micro-samples by combining the distribution information from Raman spectroscopy and laser-induced breakdown spectroscopy (LIBS). The existing Raman-LIBS imaging methods are difficult to balance the imaging performance and system volume. There is an urgent need to develop a Raman-LIBS imaging method with miniaturization, and high imaging performance. A miniaturized Raman-LIBS imaging instrument based on the micro-electro-mechanical (MEMS) mirror has been developed to overcome these challenges. The instrument utilizes dual 2D MEMS mirror scanning technology to shorten the optical length of the system and improve the detection efficiency of hybrid spectral signals. The optical probe measures 94 mm × 66 mm, and has an axial focusing ability of approximately 40 nm, with a lateral resolution of approximately 700 nm for Raman maps and 9.5 μm for LIBS maps. As a proof experiment, 3D high-resolution Raman-LIBS hybrid spectral distribution maps of meteorite Tisserlitine 001 were obtained. The attainment of high imaging performance and miniaturization in hybrid spectral imaging is crucial for on-site chemical analysis. The proposed instrument enables in-situ spectrum and multispectral imaging with miniaturization, high spatial resolution, and high stability. The instrument is a powerful tool for composition and structural information characterization in the fields of space exploration and geological exploration.

Ultrasound-Induced Enrichment of Ultra-Trace miRNA Biosensing in Nanoliter Samples.

The rapid and accurate analysis of micro-samples is a crucial foundation for precision medicine, particularly for early screening and monitoring of cancer, where it holds significant importance. Ultrasound-based multifunctional biocompatible manipulation techniques have been extensively applied in a variety of biomedical fields, providing insights for the development of rapid, cost-effective, and accurate biomarker detection strategies. In this chapter, we combine ultrasound-based gradient pressure fields with functionalized microsphere enrichment to develop a biosensing method for ultra-trace miRNA enrichment in nanoliter samples without PCR. This system relies on inexpensive capillaries, enabling simultaneous visual imaging and trace sample detection.

An Achaemenid God in Color

A limestone relief fragment with a figure in a winged disk from the fifth-century BCE Hall of 100 Columns at Persepolis in southwestern Iran that entered the Harvard Art Museums’ collections in 1943 preserves significant traces of its original coloration and has played a key role in the rediscovery of polychromy at the Achaemenid Persian capital. After tracing the fragment’s journey to Cambridge, MA, this article presents the results of recent technical studies of its pigment remains, including visible light-induced infrared luminescence (VIL) imaging, X-ray fluorescence (XRF) spectroscopy, and the analysis of micro samples by Raman spectroscopy, Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM), and polarizing light microscopy (PLM). The new scientific data is compared to the findings of ongoing investigations of polychromies at Persepolis and other Achaemenid Persian sites and evaluated for the information it can and cannot provide on the original appearance of the figure in the winged disk, likely the Zoroastrian god Ahuramazda. The article reviews past attempts at reconstructing the relief’s coloration and the assumptions that guided them, recounts the experience of creating a tangible three-dimensional color reconstruction for an exhibition, and concludes with some general thoughts on the valuation of colorfulness.

Abstract B019: RNA transcriptome profiling in microsamples of blood

Abstract Multi-omic analysis of microsamples of lancet-induced blood drops allows frequent capture and quantitation of numerous metabolites, lipids, cytokines, and proteins. Microsample-based transcriptome profiling would facilitate use of RNA biomarkers in diagnosis and treatment of immunotherapy patients, but a suitable method has not been available. We tested a targeted sequencing protocol for this purpose in human blood microsamples. We tested normal blood collected either by phlebotomy into standard vacutainer tubes or by absorption of 30 uL of blood onto a Mitra device pre-treated with an RNA-stabilization reagent. We tested detection of gene expression changes by incubating anti-coagulated blood for 18 hours with endotoxin followed by isolation of identical volumes of blood using a standard method (Qiagen kit) or from Mitra devices air dried for 24 h to mimic a home-use scenario. RNA was extracted from the microsamplers. After RNA purification, a panel of 274 immune/inflammatory genes was quantified by NGS after PCR using targeted primers following the Cellecta DriverMap protocol, which avoids counting of abundant rRNA and mitochondrial sequences. The targeted sequencing results were normalized to counts per million and used to compare results in standard vs microsamples. We found robust detection of gene expression and correlation using the two methods in both unstimulated (r = 0.94) and endotoxin-stimulated blood. The differentially expressed genes (DEGs) identified in both standard and microsample methods showed high overlap with DEGs reported in public datasets in similar experiments. We conclude that RNA transcriptome profiling using targeted sequencing allows sensitive detection of gene expression levels in normal and activated blood samples. Because microsamples can be air-dried and mailed in for analysis, this approach has great promise for simple and repeated monitoring of RNA biomarkers in immunotherapy. Citation Format: Alex Chenchik, Lester Kobzik, Mikhail Makhanov, Paul Diehl. RNA transcriptome profiling in microsamples of blood [abstract]. In: Proceedings of the AACR-NCI-EORTC Virtual International Conference on Molecular Targets and Cancer Therapeutics; 2023 Oct 11-15; Boston, MA. Philadelphia (PA): AACR; Mol Cancer Ther 2023;22(12 Suppl):Abstract nr B019.

Modern Mural Paintings. The Planisphere Painting of Almada Negreiros: Technical and Material Features of Plasters and Painting Technique

This paper presents the results of observations and analysis carried out in the modern mural painting of 54m2, known as Planisphere (or Mapa-mundi), made by Almada Negreiros in 1939 in the city of Lisbon. The painting is Almada’s first monumental painted work at fresco, and it is a striking, colourful composition inspired by early world maps of navigators. The aim is to ascertain how he built up this masterpiece and what artistic sources could have inspired him. The analytical setup comprised in-situ technical photography in the visible (Vis and Vis-Rak) and near infrared radiation (NIR), Vis-handled-Optical microscopy, complemented by laboratorial analysis of microsamples collected from paint layers with OM-Vis-UV and SEM-EDS. The data obtained was compared with the painting compendiums of Paul Bedouin’s La fresque. Sa Technique-ses applications (1914) and of Costin Petresco’s L’art de la fresque (1931), retrieved from the artist studio in 2019. The study reveals the first technical and material features found, such as the painting execution by large giornate, the use of different types of techniques to transfer the drawings to the wall, and the presence of paint layers made with buon and lime fresco. The results also reveal the likely strategies used by Almada to overcome the challenges imposed by a fresco execution, inspired by both eastern and western mural painting traditions.

VISUALISATION OF HISTOLOGICAL SPECIMENS AND TASKS AS A TECHNIQUE TO IMPROVE KNOWLEDGE, SKILLS AND ABILITIES OF MEDICAL STUDENTS

The purpose of this study is to explore the role of visualization of histological tasks in improving the quality of knowledge, abilities, and skills of medical students by summarizing the work experience of the Department of Histology, Cytology, and Embryology.
 In the field of higher medical education, the discipline of "Histology, Cytology, and Embryology" is crucial as it forms the foundation of students' understanding of the microscopic and functional morphology, structure, development, and regeneration of human cellular, tissue, and organ systems. However, first-year medical students often struggle with the vast amount of information presented to them.
 To optimize the teaching of this discipline and enhance the quality of students' knowledge, modern teaching methods and technologies are employed, including the use of microscopes with video apps, multimedia projectors, and educational resources that take advantage of digital technologies. The staff of the Department of Histology, Cytology, and Embryology has also created educational resources that broaden the possibilities of digital technologies for visualization of microscopic structures: collections of photomicrographs of histological preparations and electronograms, multimedia presentations, educational films, animated videos and Internet resources (computer training programs, electronic atlases, etc.).
 Students complete visualized tasks for the diagnosis of histological preparations by establishing correspondence between digital markings of structures on images of micro-samples and proposed lists of histological structures, or by diagnosing drugs through determining their colour and histological structures. These visual tasks expand the possibilities of studying histology, cytology, and embryology, eliminating randomness in assessing students' knowledge, abilities, and skills.
 In practical histology classes, moulages of histological preparations, structures of human embryonic development, facial development, teeth, and their supporting apparatus, thematic stands, and wet preparations are used to enhance the visualization of histological structures.
 By visualizing histological samples and tasks in practical classes, students can better assimilate educational material and acquire the skills necessary for differential diagnosis based on the analysis of microsamples. The experiences of the Department of Histology, Cytology, and Embryology can serve as an example of the positive impact of this approach on the quality of medical education.

Analysis of microsamples by miniaturized magnetic-based pipette tip microextraction: determination of free cortisol in serum and urine from very low birth weight preterm newborns.

Miniaturized magnetic-based pipette tip microextraction is presented as a sample preparation approach for microsamples. It involves quick dispersion of a diminutive amount of a magnetic sorbent material in a low-volume sample (10 μL) to entrap the target analytes. Next, the dispersion is aspirated using a (semi)automatic pipette through a pipette tip with a small cubic neodymium magnet inside, which retrieves the magnetic sorbent containing the analytes. After discarding the rest of the sample, the sorbent is properly rinsed by aspirating/dispensing deionized water, and then, the analytes are eluted by aspirating/dispensing an appropriate solvent. This approach was employed for the determination of free cortisol in serum and urine from very low birth weight preterm newborns, a vulnerable patient group who present low availability for sampling biological fluids. A magnetic immunosorbent made of a cortisol antibody was employed for the selective extraction, followed by liquid chromatography-tandem mass spectrometry. Good analytical features were obtained, such as limits of detection and quantification of 0.08 and 0.27 ng mL-1, respectively, linearity up to 50 ng mL-1 (R2 > 0.999), RSD values under 15% and relative recoveries between 91 and 111%. The cross-reactivity with other glucocorticoids (i.e., cortisone and prednisolone) was evaluated to show the selectivity of the extraction. Finally, the method applicability was demonstrated towards the determination of free cortisol in the serum and urine samples from low birth weight preterm newborns.

Conductive cross-section preparation of non-conductive painting micro-samples for SEM analysis

Scanning electron microscopy (SEM) is a common method for the analysis of painting micro-samples. The high resolution of this technique offers precise surface analysis and can be coupled with an energy-dispersive spectrometer for the acquisition of the elemental composition. For light microscopy and SEM analysis, the painting micro-samples are commonly prepared as cross-sections, where the micro-sample positioned on the side is embedded in a resin. Therefore, the sequence of its layers is exposed after the cross-section is polished. In common cases outside of cultural heritage, a conductive layer is applied on the polished side, but in this field, the measurements are mostly done in low-vacuum SEM (LV-SEM). Although the charging effect is reduced in LV-SEM, it can still occur, and can hardly be prevented even with carbon tape or paint. This work presents two conductive cross-section preparation methods for non-conductive samples, which reduce charging effects without impairing the sample integrity.

Analysis of microsamples of biological fluids via inductively coupled plasma-tandem mass spectrometry using a micro-flow injection system coupled to a high-efficiency sample introduction setup

In many fields, the sample volume available is the limiting factor for ultra-trace elemental analysis, and thus, the development of novel methods that can extract more information from lower sample amounts is a topic that deserves attention. In this work, the performance of a micro-flow injection system coupled to either (1) a traditional or (2) a high-efficiency sample introduction system has been evaluated for the analysis of liquid microsamples using inductively coupled plasma-mass spectrometry (ICP-MS). The figures of merit with each sample introduction system have been studied in a wide range of sample volumes and sample uptake rates. The use of a high-efficiency low-volume sample introduction system provided a > 4-fold enhanced sensitivity as compared to the traditional one, while the former setup was demonstrated being capable of accurately delivering volumes as low as 5 or 10 μL to the ICP. Even for such low sample amounts, good linearity (>0.9998) and repeatability (RSD down to 0.2%) were experimentally demonstrated, while matrix effects were lower with the high-efficiency sample introduction system. The use of an internal standard adequately corrected for changes in sample introduction conditions, allowing quantitative results to be obtained by using a single set of calibration data obtained at fixed operating conditions (sample volume and sample uptake rate), with a bias <15% (typical acceptance criterion for clinical QC analysis). The set-up characterized was successfully applied to the analysis of microsamples of biological fluids (down to 0.4 μL of sample volume). Tandem ICP-MS (ICP-MS/MS) was used to overcome spectral overlap (chemical resolution with a mixture of NH3/He) affecting the determination of six clinically relevant metals (Co, Cr, Mn, Ni, Ti and V) at ultra-trace concentration levels. No significant differences were found between the results obtained in this work and the reference values, even when using different sample introduction conditions for the measurement of calibration standards and samples.

The development of NAD+-dependent dehydrogenase screen-printed biosensor based on enzyme and nanoporous gold co-catalytic strategy

Given the significance of dihydronicotinamide adenine dinucleotide (NADH) and nicotinamide adenine dinucleotide (NAD+) in numerous biochemical fields such as clinical diagnostics and fermentation monitoring, a synergistic strategy was proposed based on the co-catalysis of NAD+-dependent dehydrogenases and nanoporous gold (NPG) towards the oxidation of substrates and NADH, respectively. An NAD+-dependent dehydrogenase/NPG/SPE biosensing platform was developed by modifying screen-printed electrode (SPE) with NPG and NAD+-dependent dehydrogenase for the electrochemical detections of NADH, ethanol, and glucose. Owing to the exceptional oxidation activity of NPG towards NADH, the amperometric detection of NADH exhibited good linearity from 50 μM to 2.0 mM with a low detection limit (LOD) of 15.18–16.39 μM and a satisfactory sensitivity of 1.58–1.72 μA mM−1 within a wide pH range. With alcohol dehydrogenase (ADH) and glucose dehydrogenase (GDH) as model enzymes, ADH/NPG/SPE and GDH/NPG/SPE exhibited excellent analytic characteristics (sensitivity of 0.66 μA mM−1 and 2.04 μA mM−1, LOD of 40.72 μM and 14.83 μM) of ethanol and glucose detection in buffer solution as well as in human serum and fermentation broth. The sensitive micro-sample detections of ethanol and glucose in both real samples were achieved using the proposed biosensors with comparable accuracy (deviation rates of 0.85–7.92%) as automatic analyzers. The proposed biosensing platform elicited many advantageous properties in practical applications, including micro-sample analysis, cost-efficient, easy fabrication, and flexible adaptability, which made it a promising candidate for the clinical blood test, urinalysis, and fermentation monitoring.

Direct Inlet Py-GC-MS analysis of cultural heritage materials

Pyrolysis-gas chromatography-mass spectrometry (Py-GC-MS) is an invaluable tool in the analysis of cultural heritage materials, particularly those containing complex polymerised components, whether natural or synthetic in origin. As the field embraces non-destructive and micro-sampling analysis, it is not always possible to perform traditional flash Py-GC-MS due to the sample size requirements of the technique, which are typically in the range of 50–100 µg. The development of a pyrolysis method using a Thermal Separation Probe (Agilent Technologies Inc.) has allowed for splitless Py-GC-MS analysis to be carried out on much smaller samples. This technique makes use of a multi-mode inlet that is capable of rapidly heating to 450 °C. Because pyrolysis takes place within the inlet, the methodology has been designated Direct Inlet Pyrolysis (DIP). Examples of synthetic reference materials, as well as case studies of archaeological residues and a varnish from the 1960 s were employed to demonstrate this adapted analytical technique. The results obtained using DIP-GC-MS were compared to published thermal degradation data and higher-temperature flash Py-GC-MS chromatograms. The results indicate that DIP-GC-MS can characterise the organic fraction of complex polymeric samples. Differences in pyrolysate formation and relative abundance occur for some polymers which are caused by lower and prolonged pyrolysis conditions. The technique can be performed in splitless mode with just a few micrograms of precious sample from cultural heritage objects, or by employing a low split if desired for more abundant reference materials. Like other Py-GC-MS methods, the on-line use of a reagent such as tetramethylammonium hydroxide (TMAH) allows for the derivatisation of polar functional groups.

Strontium isotopic analysis of environmental microsamples by inductively coupled plasma – tandem mass spectrometry

A method for direct (without chromatographic Rb/Sr separation) Sr isotopic analysis using tandem ICP-MS has been optimized for small-size environmental samples and applied to Antarctic PM10 and soil samples from South America and Australia as proof-of-concept.

Evaluation of electrothermal vaporization for sample introduction aiming at Cu isotopic analysis via multicollector-inductively coupled plasma mass spectrometry

A new method for Cu isotopic analysis was developed using a commercially available electrothermal vaporization (ETV) device coupled to multicollector-inductively coupled plasma mass spectrometry (MC-ICP-MS).The method demonstrated potential for the isotopic analysis of microsamples (e.g., 5 μL) in a biological context. For example, Cu isotopic analysis of NIST 3114 (diluted to 1 mg L−1 Cu) using self-bracketing provided average δ65Cu values of 0.00 ± 0.17‰ (2SD, n = 10) and internal precision values of 712 ppm. In order to achieve this level of accuracy and precision, it is critical to properly deal with the short transient signals generated by the ETV-MC-ICP-MS, which implies using point by point calculations and time lag detector correction (TDC), as well as a criterion to reject potential outliers.The results of this technique were compared with the results obtained via femtosecond-laser ablation-MC-ICP-MS using the same pre-treated serum samples. No significant differences were observed among the results obtained in both cases, while external precision was 0.26‰ for ETV-MC-ICP-MS and 0.24‰ for fs-LA-MC-ICP-MS, expressed as median value of 2SD (n = 27), further proving the usefulness of the approach proposed in this context, as the use of ETV results in a more straightforward approach.

Adherence to cardiovascular pharmacotherapy by patients in Iraq: A mixed methods assessment using quantitative dried blood spot analysis and the 8-item Morisky Medication Adherence Scale.

This study evaluated the adherence to prescribed cardiovascular therapy medications among cardiovascular disease patients attending clinics in Misan, Amara, Iraq. Mixed methods were used to assess medication adherence comprising the Arabic version of the eight-item Morisky Medication Adherence Scale (MMAS-8) and determination of drug concentrations in patient dried blood spot (DBS) samples by liquid chromatography-high resolution mass spectrometry. Three hundred and three Iraqi patients (median age 53 years, 50.5% female) who had been taking one or more of the nine commonly prescribed cardiovascular medications (amlodipine, atenolol, atorvastatin, bisoprolol, diltiazem, lisinopril, losartan, simvastatin and valsartan) for at least six months were enrolled. For each patient MMAS-8 scores were determined alongside drug concentrations in their dried blood spot samples. Results from the standardized questionnaire showed that adherence was 81.8% in comparison with 50.8% obtained using the laboratory-based microsample analysis. The agreement between the indirect (MMAS-8) and direct (DBS analysis) assessment approaches to assessing medication adherence showed significantly poor agreement (kappa = 0.28, P = 0.001). The indirect and direct assessment approaches showed no significant correlation between nonadherence to prescribed cardiovascular pharmacotherapy and age and gender, but were significantly associated with the number of medications in the patient’s treatment regimen (MMAS-8: Odds Ratio (OR) 1.947, 95% CI, P = 0.001; DBS analysis: OR 2.164, 95% CI, P = 0.001). The MMAS-8 results highlighted reasons for nonadherence to prescribed cardiovascular pharmacotherapy in this patient population whilst the objective DBS analysis approach gave valuable information about nonadherence to each medication in the patient’s treatment regimen. DBS sampling, due its minimally invasive nature, convenience and ease of transport is a useful alternative matrix to monitor adherence objectively in Iraq to cardiovascular pharmacotherapy. This information combined with MMAS-8 can provide clinicians with an evidence-based novel approach to implement intervention strategies to optimise and personalise cardiovascular pharmacotherapy in the Iraqi population and thereby improve patient health outcomes.

Characterization of contemporary artworks made on photosensitized canvas by means of optical microscopy and micro-Raman spectroscopy techniques

Contemporary artists experimented with a wide range of techniques as it is photography, combined with other materials so as to create images on various surfaces. Nikos Kessanlis (1930–2004), an eminent Greek artist, used photographic and mechanical techniques, involving the application of a photosensitive emulsion on different supports for his artistic creations. This photomechanical technique is called alternative printing.The present study examines a series made by Kessanlis in 1999–2000, composed of eleven panels of photosensitized canvases with the scope to identify the materials used by the artist (canvas, primer, photographic emulsion, protective layer), to understand the artist’s technique and to document the panels overall condition. The series is examined using non-invasive techniques (portable digital optical microscope) and analysis of micro-samples by–micro-Raman spectrometry.Micro-Raman analysis results identified the support, as canvas made by cotton and jute, the primer layer as a combination of titanium white and calcium carbonate and finally the photosensitized layer, as a gelatin silver chloride emulsion. Also further compounds are detected such is silver sulfide, related to the photosensitized emulsion deterioration and soot and lignin, related to the impure environment (air flow inside the metro station) where the series are on display for the last twenty years (Athens metro station).Finally, measurements of air temperature and relative humidity are also performed for a short period near the panels so as to evaluate the environmental conditions of the area. The results have shown extreme daily fluctuations of both factors, characterized by “cycling” that could be related to mechanical and chemical deterioration factors affecting the artwork condition.

Laser ablation of microdroplets for copper isotopic analysis via MC-ICP-MS. Analysis of serum microsamples for the diagnosis and follow-up treatment of Wilson's disease

The deposition of microdroplets onto silicon wafers followed by drying and fsLA is evaluated by MC-ICP-MS Cu isotopic analysis.

60 years of street art: A comparative study of the artists’ materials through spectroscopic and mass spectrometric approaches

Abstract Street art murals are an artistic expression strictly interwoven in the urban landscape, and in recent years have received increasing attention as cultural heritage at risk. Today there is intense debate regarding the value assessment and choices related to the conservation of urban art; however, the evaluation of the stability of modern paint materials in outdoor environment is preliminary to any possible preservation strategy. In particular, the identification of the materials constituting a street artwork is critical for the preservation of these non-permanent heritage elements and to define the best restoration approaches. In this work, we performed a set of analyses of microsamples based on spectroscopy, analytical pyrolysis, gas and liquid chromatography, and mass spectrometry to identify paint materials (binders, pigments, additives, degradation products and conservation/restoration materials) of a selection of mural paintings, covering 60 years of history (1953–2014). The goal of this work was to identify the materials used to produce different mural paintings and to relate and compare their different compositions with previous studies in order to describe the evolution of the materials during the last 60 years. The collected knowledge and the limited data available in literature were exploited to increase the scientific background on the materials used by street artists, and to fill the lack of knowledge on this emerging topic.

New Orientation: A Downward-pointing Vertical Inductively Coupled Plasma Mass Spectrometer for the Analysis of Microsamples

We present a prototype of a vertical-downward configuration of an inductively coupled plasma mass spectrometer (ICPMS) allowing the sample introduction from the top. With this novel approach to orient the ICP downward, we aim to expand the sample transport capabilities in ICPMS especially for the transport of droplets or particles with a final goal to analyze individual cells. Because of this gravity-assisted sampling approach, the transport of larger sized droplets, that is, droplets that would be difficult to transport into a horizontally oriented ICPMS, becomes possible and, furthermore, becomes independent of the droplets' size or size distribution. We demonstrate that droplets of an initial size of 70 μm can be successfully transported into the plasma at dispensing frequencies up to 1 kHz without the need for a desolvation device. In addition, we observed that the implementation of a desolvation device, that is, a gas-exchange device (GED), can improve the detection efficiencies (DEs). Compared to operating conditions that are commonly reported for ICPMS experiments, significantly different optimization parameters (radio frequency power and gas flow rates) were tested in the presented experiments here while instrument type-specific DEs were obtained.

Identifying the Unknown Content of an Ancient Egyptian Sealed Alabaster Vase from Kha and Merit’s Tomb Using Multiple Techniques and Multicomponent Sample Analysis in an Interdisciplinary Applied Chemistry Course

This article highlights the multianalytical study of exuded liquid from an ancient Egyptian sealed alabaster vase by Master’s students in an applied chemistry for cultural heritage course. Master students are introduced to the field of Archaeometry that see the collaboration of experts in different areas of research such as conservators, curators of museums, physicists, chemists, etc. The sample is a residue exuded on the linen strip sealing an ancient Egyptian alabaster vase (inventory number S.8448) from the collection of the Museo Egizio in Turin (Italy). The students start to plan the noninvasive investigation by X-ray fluorescence (XRF), transmission electron microscopy (TEM), and energy-dispersive X-ray spectroscopy (EDS) for the inorganic compounds characterization, followed by the extraction of the organic components (such as oils, fats, and waxes) to be analyzed by high-resolution 1H and 13C nuclear magnetic resonance (NMR) spectroscopy and 2D NMR correlation spectroscopy (COSY), heteronuclear single quantum coherence (HSQC), and long-range heteronuclear correlation (HMBC) techniques and by gas chromatography coupled with mass spectrometry (GC/MS). Reference standards, spectral databases, and published data on similar artifacts served as the basis for the interpretation of the instrumental results. The approach was introduced in the course of Applied Chemistry for Cultural Heritage for Master students in Archaeology (University of Palermo, Italy), where the need is to know how to approach the scientific investigation together with the conservation scientists and how to manage with a very low amount of sample. Pedagogically, the approach introduces students to the main techniques currently used in the field of Archaeometry while reinforcing fundamental concepts in sample collecting and multicomponent microsample analysis. This interdisciplinary approach provides a unique experience that demonstrates chemistry’s broad applicability outside of the traditional laboratory. Students are guided to identify the inorganic and organic components of the exudate liquid: the first one is ascribable to clay minerals iron oxides, which could impart the brown color to the sample; the second one is ascribed to triglycerides of various kinds, which probably comes from vegetable oil.