PIXE Analysis of Ancient Egyptian Pigments (Case Study)

Particle Proton–Induced X-Ray Emission (PIXE) is one of the most sensitive analytical methods which can be used in the study of ancient mural paintings - especially pigments. It requires small samples or tiny fragments of the paint layer. It is a non-destructive technique and provides data on elemental concentrations. Analysis can be performed in vacuum or in air. The major advantage of this technique is the ability to analyze simultaneously both elements and trace elements present in the sample. Another advantage is the short data acquisition time. This research studies red, yellow, blue and green pigments used in the tomb of Ramesses III (N.11 - 1198 BC), the tomb of Tohthmous III- (N.34 - 1504 BC), both located at the Valley of the Kings Luxor, and also, Medinet Habu temple of Ramesses II (1198 -1166 BC) located at the West Bank of Luxor. The study was performed by using light Optical Microscope (LOM) and Particle Proton–Induced X-Ray Emission (PIXE).

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An Ancient Egyptian Multilayered Polychrome Wooden Sculpture Belonging to the Museo Egizio of Torino: Characterization of Painting Materials and Design of Cleaning Processes by Means of Highly Retentive Hydrogels

Coatings ◽

10.3390/coatings11111335 ◽

2021 ◽

Vol 11 (11) ◽

pp. 1335

Author(s):

Nicole Manfredda ◽

Paola Buscaglia ◽

Paolo Gallo ◽

Matilde Borla ◽

Sara Aicardi ◽

...

Keyword(s):

Uv Light ◽

Optical Microscope ◽

Mechanical Action ◽

Light Sources ◽

Pyrolysis Gas ◽

X Ray ◽

Painting Materials ◽

Ancient Egyptian ◽

Multispectral Analysis

This contribution focuses on the conservation of an Egyptian wooden sculpture (Inventory Number Cat. 745) belonging to the Museo Egizio of Torino in northwest Italy. A preliminary and interdisciplinary study of constituent painting materials and their layering is here provided. It was conducted by means of a multi-technique approach starting from non-invasive multispectral analysis on the whole object, and subsequently, on selected micro-samples. In particular, visible fluorescence induced by ultraviolet radiation (UVF), infrared reflectography (IRR) and visible--induced infrared luminescence were used on the whole object. The micro-samples were analysed by means of an optical microscope with visible and UV light sources, a scanning electron microscope (SEM) with an energy-dispersive X-ray spectrometer (EDX), Fourier transform infrared (FT-IR) spectrometer, pyrolysis-gas chromatography/mass spectrometer (Py-GC/MS) and micro-particle induced X-ray emission (PIXE). The characterization of the painting materials allowed the detection of Egyptian blue and Egyptian green, and also confirmed the pertinence of the top brown layer to the original materials, which is a key point to design a suitable surface treatment. In fact, due to the water sensitiveness of the original materials, only few options were available to perform cleaning operations on this artwork. To setup the cleaning procedure, we performed several preliminary tests on mockups using dry cleaning materials, commonly used to treat reactive surfaces, and innovative highly water retentive hydrogels, which can potentially limit the mechanical action on the original surface while proving excellent cleaning results. Overall, this study has proved fundamental to increase our knowledge on ancient Egyptian artistic techniques and contribute to hypothesize the possible provenance of the artefact. It also demonstrated that polyvinyl alcohol-based retentive gels allow for the safe and efficient cleaning of extremely water sensitive painted surfaces, as those typical of ancient Egyptian artefacts.

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Multi-technique characterization and conservation of an ancient Egyptian fabric from King Khufu first solar ship

10.21203/rs.3.rs-202536/v1 ◽

2021 ◽

Author(s):

Eman Nabil ◽

Tawfik A. Khattab ◽

samir kamel

Keyword(s):

Electron Microscopy ◽

Optical Microscope ◽

Elemental Content ◽

Infrared Analysis ◽

X Ray ◽

Ancient Egyptian ◽

The World ◽

Ft Ir ◽

Great Discovery ◽

Scanning Electron

Abstract Textiles are among the most fragile artefacts in the world. They have been difficult to preserve even in the best circumstances. Herein, we studied an artefact fabric of a special nature in terms of usage. Despite the multiple applications of textiles, the piece understudy is one of the unique pieces that the ancient Egyptian used as fenders for King Khufu first solar boat which is the second-largest discovery in Egypt history. The boat was discovered inside a limestone pit. It was disassembled and arranged in several layers. Four pillows of wrapped fabric were found in the first layer, which were used as boat fenders. This use is in itself a great discovery of the role played by textiles in the manufacture of ancient boats. Thus, we conducted tests and analytical studies of those fenders using a scanning electron microscopy (SEM) and an optical microscope to identify the type and nature of fibers, spinning method and aspects of damage. Both energy-dispersive X-ray (EDX) analysis and infrared analysis (FT-IR) were employed to explore the elemental content of the sample and to study the functional groups of the fabric. These analytical processes were useful in carrying out the restoration and preservation work necessary for the artefact under study.

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Technical Study of Polychrome Arhat Figures Dated From the Song Dynasty(960-1279 CE) From the Lingyan Temple, Changqing, Shandong, China

10.21203/rs.3.rs-662279/v1 ◽

2021 ◽

Author(s):

Yongdong Tong ◽

Youzhen Cai ◽

Xuening Wang ◽

Zhimin Li ◽

Austin Nevin ◽

...

Keyword(s):

Song Dynasty ◽

Paint Layer ◽

Optical Microscope ◽

Green Is ◽

X Ray ◽

The Song Dynasty ◽

Scientific Analysis ◽

Golden Yellow ◽

Solid Foundation ◽

Technical Study

Abstract Scientific analysis revealed the materials and techniques used in the process of making the polychrome sculptures providing a solid foundation for the protection and restoration of the painted statues. In addition analysis revealed changes in colour schemes applied to the sculptures can provide the basis for the virtual restoration of the painted statues. In order carry out scientifically-informed protection and restoration of the Bodhidharma statue from the Lingyan Temple, Changqinq, Shandong, several analytical methods such as optical microscope (OM), Micro-Raman spectroscopy (μ-RS), scanning electron microscopy coupled with energy dispersive X-ray analysis (SEM-EDS) and Fourier transform infrared spectroscopy (FTIR) were employed. Analysis clearly reveal the information including the stratigraphic structure and the composition of pigment. The use of silver foils and golden yellow pyrophyllite mineral to replace gold foils were found in the gilding paint layer in the later repainting after the Song Dynasty. This work reports the coexistence of emerald green (Cu(C2H3O2)2·3Cu(AsO2)2) and the degradation product lavendulan (NaCaCu5(AsO4)4Cl·5H2O) in large areas of the paint stratigraphy and on the surface confirming that the degradation of emerald green is related to the thickness of the paint layer; in thinner paint layers emerald green is transformed in lavendulan, while thicker layers of contain both lavendulan and emerald green, suggesting an environmental source of chlorides.

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Polychrome arhat figures dated from the Song Dynasty (960–1279 CE) at the Lingyan Temple, Changqing, Shandong, China

Heritage Science ◽

10.1186/s40494-021-00592-3 ◽

2021 ◽

Vol 9 (1) ◽

Author(s):

Yongdong Tong ◽

Youzhen Cai ◽

Xuening Wang ◽

Zhimin Li ◽

Austin Nevin ◽

...

Keyword(s):

Song Dynasty ◽

Paint Layer ◽

Optical Microscope ◽

Green Is ◽

X Ray ◽

The Song Dynasty ◽

Micro Raman Spectroscopy ◽

Scientific Analysis ◽

Golden Yellow ◽

Solid Foundation

AbstractScientific analysis revealed the materials and techniques used in the process of making polychrome sculptures providing a solid foundation for the protection and restoration of the painted statues. In addition, the analyses revealed changes in colour schemes applied to the sculptures can provide the basis for the virtual restoration of the painted statues. In order to carry out scientifically-informed protection and restoration of the Bodhidharma statue from the Lingyan Temple, Changqinq, Shandong, several analytical methods such as optical microscope (OM), Micro-Raman spectroscopy (μ-RS), scanning electron microscopy coupled with energy dispersive X-ray analysis (SEM–EDS) and Fourier transform infrared spectroscopy (FTIR) were employed. Analyses clearly reveal the information including the stratigraphic structure and the composition of pigment. The use of silver foils and golden yellow pyrophyllite mineral to replace gold foils were found in the gilding paint layer in the later repainting after the Song Dynasty. This work reports the coexistence of emerald green (Cu(C2H3O2)2·3Cu(AsO2)2) and the degradation product lavendulan (NaCaCu5(AsO4)4Cl·5H2O) in large areas of the paint stratigraphy and on the surface confirming that the degradation of emerald green is related to the thickness of the paint layer; in thinner paint layers emerald green is transformed in lavendulan, while thicker layers of contain both lavendulan and emerald green, suggesting an environmental source of chlorides.

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A microstratigraphic investigation of iron ion migration in some ancient Egyptian wall paintings using PIXE Analysis

Canadian Journal of Chemistry ◽

10.1139/v91-044 ◽

1991 ◽

Vol 69 (2) ◽

pp. 286-292 ◽

Cited By ~ 2

Author(s):

George Burns ◽

K.M. Wilson-Yang

Keyword(s):

Surface Layer ◽

Paint Layer ◽

Arid Environment ◽

Layer Formation ◽

Ion Migration ◽

Pixe Analysis ◽

Depth Profiles ◽

Apparent Diffusion Coefficients ◽

Ancient Egyptian ◽

Surface Layer Formation

The painted murals in the tombs at Beni Hasan (circa 2100 B.C.) are obscured by a rock-like grey surface layer. Its formation involves subsurface removal of slightly soluble calcite (CaCO3) under the action of surface-condensed water. To study the mechanism of surface layer formation and the effect of mural cleaning during recent restorations, the PIXE microprobe was used. Iron depth profiles in red-painted samples taken from the murals, both uncleaned and cleaned, have been obtained over depths of 80 μm (the cleaned sample) and 100 μm (the uncleaned sample). It has been found that the uncleaned sample has more Fe at all depths than does the cleaned sample and that portions of the uncleaned pigment appear to be pure Fe2O3. The shapes of depth profiles of Fe in the cleaned and uncleaned samples are similar to the shapes of diffusion curves; this finding is in agreement with the mechanism of surface layer formation proposed in our earlier papers. Apparent diffusion coefficients for the ion migration of Fe, DFe, in the limestone painting substrate have been determined, assuming constant temperature diffusion over 4 000 years: DFe(u) = (1.4 ± 0.5) × 10−16 cm2/s for the uncleaned sample and DFe(c) = (0.7 ± 0.4) × 10−16 cm2/s for the cleaned sample, where errors are given as the 95% C.I. based on standard deviations of the slope of the fitted curve. These coefficients are consistent with the mechanism of slow migration of Fe in the painting substrate in an arid environment. The difference between DFe values secured for the cleaned and uncleaned samples is attributed to a partial removal of the paint layer in the cleaned sample during the restoration efforts. Thus, if it is assumed that either 20 or 40 μm of paint layer was removed during HCl-cleaning of murals, DFe(c) = (1.0 ± 0.4) × 10−16 and DFe(c) = (1.4 ± 0.6) × 10−16 cm2/s, respectively, are obtained. Removal of the top 40 μm of the mural corresponds to elimination, during the restoration, of the order of 60% of the uncleaned paint layer. Key words: Egypt, PIXE, ancient murals deterioration.

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Microanalysis of Cuprate Superconductors Using the Color of Polarization

MRS Proceedings ◽

10.1557/proc-169-361 ◽

1989 ◽

Vol 169 ◽

Cited By ~ 1

Author(s):

H.A. Hoff ◽

W.L. Lechter ◽

M.S. Osofsky ◽

G.A. Candela

Keyword(s):

Strong Correlation ◽

Cuprate Superconductors ◽

Optical Microscope ◽

Energy Dispersive ◽

Apparent Lack ◽

Superconducting Cuprates ◽

X Ray ◽

Grain Color ◽

Light Optical Microscope ◽

Selection Of

AbstractA technique for the identification of individual anisotropic grains in a heterogeneous and opaque material involves the observation of grain color in a reflecting light optical microscope. Such colors are generally characteristic of particular phases. We have studied the presence of color in many superconducting cuprates and found a strong correlation between color and the existence of superconductivity. The change in color from insulator to superconductor facilitates the selection of grains for microanalysis. Color variations in a Tl-Sr-Ca-Cu-O material are investigated using quantitative energy dispersive x-ray spect-roscopy. Cation concentrations are found not to correlate with the changes in color. This apparent lack of correlation of color with composition is discussed.

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XRF and PIXE Analysis of light and Dark Adapted Ocular Tissue

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100053619 ◽

1982 ◽

Vol 40 ◽

pp. 190-191

Author(s):

B. J. Panessa ◽

H. W. Kraner ◽

J. B. Warren ◽

K. W. Jones

Keyword(s):

Trace Metals ◽

Pigment Epithelium ◽

Nerve Impulse ◽

Light Response ◽

Ocular Tissue ◽

Emission Spectrometry ◽

Retinol Dehydrogenase ◽

Pixe Analysis ◽

X Ray ◽

Optimal Function

During photoexcitation the retina requires specific electrolytes and trace metals for optimal function (Na, Mg, Cl, K, Ca, S, P, Cu and Zn). According to Hagins (1981), photoexcitation and generation of a nerve impulse involves the movement of Ca from the rhodopsin-ladened membranes of the rod outer segment (ROS) to the plasmalemma, which in turn decreases the in-flow of Na into the photoreceptor, resulting in hyperpolarization. In toad isolated retinas, the presence of Ba has been found to increase the amplitude and prolong the delay of the light response (Brown and Flaming, 1978). Trace metals such as Cu, Zn and Se are essential for the activity of the metalloenzymes of the retina and retina pigment epithelium (RPE) (i.e. carbonic anhydrase, retinol dehydrogenase, tyrosinase, glutathione peroxidase, superoxide dismutase...). Therefore the content and fluctuations of these elements in the retina and choroid are of fundamental importance for the maintenance of vision. This paper presents elemental data from light and dark adapted frog ocular tissues examined by electron beam induced x-ray microanalysis, x-ray fluorescence spectrometry (XRF) and proton induced x-ray emission spectrometry (PIXE).

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Macroprobe Mode for the Study of Segregation in Steels

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100134909 ◽

1990 ◽

Vol 48 (2) ◽

pp. 260-261

Author(s):

Auclair Gilles ◽

Benoit Danièle

Keyword(s):

Mechanical Properties ◽

Spatial Distribution ◽

High Performance ◽

Volume Fraction ◽

Sheet Steel ◽

Acquisition Time ◽

Chemical Information ◽

X Ray ◽

Accurate Quantitative Analysis ◽

Optical Micrographs

During these last 10 years, high performance correction procedures have been developed for classical EPMA, and it is nowadays possible to obtain accurate quantitative analysis even for soft X-ray radiations. It is also possible to perform EPMA by adapting this accurate quantitative procedures to unusual applications such as the measurement of the segregation on wide areas in as-cast and sheet steel products.The main objection for analysis of segregation in steel by means of a line-scan mode is that it requires a very heavy sampling plan to make sure that the most significant points are analyzed. Moreover only local chemical information is obtained whereas mechanical properties are also dependant on the volume fraction and the spatial distribution of highly segregated zones. For these reasons we have chosen to systematically acquire X-ray calibrated mappings which give pictures similar to optical micrographs. Although mapping requires lengthy acquisition time there is a corresponding increase in the information given by image anlysis.

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Crystallization Behavior and Mechanical Properties of Poly(ε-caprolactone) Reinforced with Barium Sulfate Submicron Particles

Materials ◽

10.3390/ma14092368 ◽

2021 ◽

Vol 14 (9) ◽

pp. 2368

Author(s):

Hegoi Amestoy ◽

Paul Diego ◽

Emilio Meaurio ◽

Jone Muñoz ◽

Jose-Ramon Sarasua

Keyword(s):

Barium Sulfate ◽

Thermal Studies ◽

Polarized Light ◽

Optical Microscope ◽

Submicron Particles ◽

Degree Of Crystallinity ◽

Scanning Calorimetry ◽

Nucleation Effect ◽

Crystal Fraction ◽

Light Optical Microscope

Poly(ε-caprolactone) (PCL) was mixed with submicron particles of barium sulfate to obtain biodegradable radiopaque composites. X-ray images comparing with aluminum samples show that 15 wt.% barium sulfate (BaSO4) is sufficient to present radiopacity. Thermal studies by differential scanning calorimetry (DSC) show a statistically significant increase in PCL degree of crystallinity from 46% to 52% for 25 wt.% BaSO4. Non-isothermal crystallization tests were performed at different cooling rates to evaluate crystallization kinetics. The nucleation effect of BaSO4 was found to change the morphology and quantity of the primary crystals of PCL, which was also corroborated by the use of a polarized light optical microscope (PLOM). These results fit well with Avrami–Ozawa–Jeziorny model and show a secondary crystallization that contributes to an increase in crystal fraction with internal structure reorganization. The addition of barium sulfate particles in composite formulations with PCL improves stiffness but not strength for all compositions due to possible cavitation effects induced by debonding of reinforcement interphase.

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Integrated quantitative PIXE analysis and EDX spectroscopy using a laser-driven particle source

Science Advances ◽

10.1126/sciadv.abc8660 ◽

2021 ◽

Vol 7 (3) ◽

pp. eabc8660

Author(s):

F. Mirani ◽

A. Maffini ◽

F. Casamichiela ◽

A. Pazzaglia ◽

A. Formenti ◽

...

Keyword(s):

Experimental Investigation ◽

Materials Science ◽

Quantitative Information ◽

Pixe Analysis ◽

Materials Analysis ◽

Particle Source ◽

X Ray ◽

Analysis Techniques ◽

Sample Structure ◽

Elemental Characterization

Among the existing elemental characterization techniques, particle-induced x-ray emission (PIXE) and energy-dispersive x-ray (EDX) spectroscopy are two of the most widely used in different scientific and technological fields. Here, we present the first quantitative laser-driven PIXE and laser-driven EDX experimental investigation performed at the Centro de Láseres Pulsados in Salamanca. Thanks to their potential for compactness and portability, laser-driven particle sources are very appealing for materials science applications, especially for materials analysis techniques. We demonstrate the possibility to exploit the x-ray signal produced by the co-irradiation with both electrons and protons to identify the elements in the sample. We show that, using the proton beam only, we can successfully obtain quantitative information about the sample structure through laser-driven PIXE analysis. These results pave the way toward the development of a compact and multifunctional apparatus for the elemental analysis of materials based on a laser-driven particle source.

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