Micro-X-Ray Fluorescence and the Old Masters Non-destructive in situ characterisation of the varnish of historical Low Countries stringed musical ins…

2012

Applied Physics A, 107

Synthesis and spectroscopic studies (Mo¨ssbauer, IR and NMR) of [R2SnCl2bipym] (R = butyl or phenyl) and the crystal and molecular structure of [Ph2S…

1994

Abstract The complexes [R 2 SnCl 2 bipym] (R = phenyl or butyl, bipym = 2,2′,6,6′-bipyrimidine) were synthesized and studied in solution by 1 H- and 13 C-NMR spectroscopy and in the solid state by IR and Mo¨ssbauer spectroscopy. The latter was also performed in frozen ethanolic solution. The structure of the phenyl complex was determined by single crystal diffraction methods. The value obtained for the angle C-SN-C in the phenyl compound is 169.3(2)° (X-ray) and 151° (Mo¨ssbauer), but the assignment of an octahedral configuration by Mo¨ssbauer spectroscopy is consistent with the structure determined by diffraction. The butyl complex is also octahedral and the two techniques show better agre…

Determinazione di componenti della vernice e della colla del contrabbasso “Panormo” di Vincenzo Trusiano

2007

Synthesis, spectroscopic studies (Mössbauer and infrared), and the crystal and molecular structure of the organotin(IV)-pyrazine adducts [Sn(CH3)2Cl2…

1987

Two adducts [Sn(CH 3 ) 2 Cl 2 ] 2 pyz ( Ia ) and Sn- (CH 3 ) 2 Br 2 pyz] ( Ib ) (pyz = pyrazine) have been synthesized and characterized in the solid state. Infrared and Mossbauer spectroscopies suggest a five- coordinated species for the Ia complex with an angular CSnC bond and a six-coordinated compound with a linear CSnC bond for the Ib complex. X-ray diffraction studies confirm a distorted trigonal bipyramidal geometry with N, Cl axial atoms and Cl and methyls in the equatorial plane for Ia where the Cl ax SnN bond angle is the lowest one reported to date and the Cl eq Sn bond distance the longest one with regard to similar complexes. This molecule has a short contact of 3.47 A b…

Il degrado di manufatti ceramici archeologici: sistemi diagnostici e metodologie di intervento

2007

Gas chromatography-mass spectrometry characterization of the varnish and glue of an ancient 18th century double bass.

2007

A GC–MS investigation is conducted on the double bass “Panormus”, property of Conservatorio di Musica “Vincenzo Bellini” in Palermo. The most important components of the varnish (fatty acids) and of the glue (proteinaceous amino acids), with which the musical instrument was treated in the past, are determined. The analyses are carried out by prior derivatization of fatty acids by acidic methanol and of amino acids by acidic methanol and trifluoroacetic anhydride (TFAA). Analytes identification is achieved by direct comparison with several reference materials and the use of a digitized library.

Synchrotron Radiation-Based Micro-XANES and Micro-XRF Study of Unsuccessfully Produced Egyptian Blue from the Late Hellenistic Production Site of Kos…

2021

International audience; This paper examines the production technology of Egyptian blue, an ancient artificial pigment, through the investigation of an unsuccessfully produced pellet derived from the Hellenistic production site of Kos (Dodecanese, Greece). This heterogeneous material was investigated by a combination of laboratory and synchrotron radiation-based (SR) techniques: scanning electron microscopy coupled with energy-dispersive Xray spectrometry, micro-Raman spectroscopy, high-resolution SR micro-X-ray fluorescence spectroscopy, and SR micro-X-ray absorption near-edge structure spectroscopy (XANES), at the ID21 beamline of the European Synchrotron Radiation Facility. Principal comp…

Un protocollo scientifico per la desalinizzazione di materiali lapidei: caso studio dei mosaici della Villa del Casale (Sicilia)

2009

PHYSICO-CHEMICAL CHARACTERIZATION OF THE ACQUALADRONE ROSTRUM

2011

The archaeological discovery of the Acqualadrone rostrum (an offensive naval weapon mounted on the prow at the waterline), off the Italian coast near Messina in 2008, has led to the need for scientific research in order to plan the conservation treatment of this artefact. The discovery is exceptional because of the presence of a wooden section from the original ship. This paper describes the physico-chemical characterization of a metallic and two wooden samples by inductively coupled plasma – optical emission spectroscopy, inductively coupled plasma – mass spectrometry, Fourier transform infrared spectroscopy, 13 C{ 1 H} cross-polarization magic angle spinning NMR spectroscopy, energy-dispe…

Recovering bronze metallurgy from archaeological artefacts for the production of reference materials in conservation science

2007

The production of reference Cu-based alloys is the first step of an original experimental protocol to be used in the field of conservation and restoration of metal artefacts. The production of these synthetic alloys has a double value. They can be used both as suitable substitutes of unique archaeological pieces for testing new materials and methods for conservation, and as guidelines for contemporary metal production. We report on a research activity focused on the recovery of the ancient production techniques from the investigation of archaeological copper-based artefacts. The chemical, physical and metallurgical characterization of several Cu-based artefacts, found in different Italian a…

Caratterizzazione delle vernici da antichi strumenti musicali.

2011

Solid state NMR investigation of the roman Acqualadroni rostrum: tenth year assessment of the consolidation treatment of the wooden part

2020

Abstract: This work follows a previous one dealing with the state of conservation study of the wooden part of the roman Acqualadroni rostrum soon after its finding in the seabed of Acqualadroni (Messina, Italy). The archaeological survey and recovery were particularly relevant since this artefact is one of the two rostrums, nowadays known,found together with its wooden part. Following the recovery, it was consolidated by immersion in a melamine-formaldehyde resin (Kauramin) aqueous solution for eight months at the “Centro di Restauro del Legno Bagnato” (Pisa, Italy). The present investigation is aimed to determine at microscopic scale the wood state of conservation and to highlight interact…

Ancient wood of the Acqualadrone rostrum: Materials history through gas chromatography/mass spectrometry and sulfur X-ray absorption spectroscopy

2012

In 2008 the rostrum from an ancient warship was recovered from the Mediterranean near Acqualadrone, Sicily. To establish its provenance and condition, samples of black and brown rostrum wood were examined using sulfur K-edge X-ray absorption spectroscopy (XAS) and gas chromatography/mass spectrometry (GC/MS). GC/MS of pyrolytic volatiles yielded only guaiacyl derivatives, indicating construction from pinewood. A derivatized extract of black wood yielded forms of abietic acid and sandaracopimaric acid consistent with pine pitch waterproofing. Numerical fits to the sulfur K-edge XAS spectra showed that about 65% of the endogenous sulfur consisted of thiols and disulfides. Elemental sulfur was…

X-ray Fluorescence Spectroscopy applied to the study of three sicilian painted artworks

2009

This paper reports on three X-Ray Fluorescence (XRF) studies of ancient Sicilian painted materials: a 13th century canvas from Cerami (Enna, Italy), the Muqarnas wood ceiling of the 12th century Palatine Chapel (Palermo, Italy) and a delicate early 20th century viola d’amore, the property of the Conservatorio di Musica “Vincenzo Bellini” in Palermo. Information about the pigments and preparation layer mixtures used as well as inferences regarding various past painting techniques emerged from the interpretation of spectra and data analyses.

Synthesis, spectroscopic (Mössbauer, IR and NMR) and X-ray structural studies of diorganotin complexes of 2,2′-bipyrimidine and further NMR studies o…

1996

Abstract The ligand 2,2′-bipyrimidine (bipym) was reacted with diorganotins R 2 SnCl 2 (R = methyl, ethyl) and complexes of the types R 2 SnCl 2 bipym, R 2 SnCl 2 bipym · bipym and (R 2 SnCl 2 ) 2 bipym were synthesized and studied by 1 H and 13 C NMR spectroscopy in solution, and by IR and Mossbauer spectroscopy in the solid state and frozen solutions. The complexes Et 2 SnCl 2 bipym · bipym and (Et 2 SnCl 2 ) 2 bipym were characterized by X-ray diffraction methods. In both complexes the tin environment is octahedral with chloro atoms in a cis disposition, the ethyl groups in a trans disposition and two N atoms from the ligand bipym. the second complex is a centrosymmetric binuclear specie…

A novel scientific approach to the conservation of archaeological copper alloys artefacts

2007

A novel research approach focused on innovative materials and methods to assure the long-term stability of bronze archaeological artefacts during exhibition and storage is reported. The work deals with the application of advanced analytical techniques and the development, characterisation and testing of materials and procedures for the conservation, protection and restoration of ancient Cu-based alloy artefacts. Our first aim was the selection of Cu-based alloy artefacts from different archaeological sites in Southern Italy with respect of chemical composition, metallurgical features and corrosion products. This step allowed the identification of the ancient alloys, the study of natural pat…

Precursors of aza-macrocycles: Characterization of substituted phenanthrolines and related bases. Crystal and molecular structure of dichloro-d i-n-b…

1993

The synthesis, characterization and 1~ NMR spectra of some substituted 1,lO-phenantrolines are described. These are precursors of azacyclophanes which are, along with their metal complexes, insoluble in polar solvents. It is suggested that the use of substituted 2,2’, 6,6’ -bipyrimidines as precursors would lead to soluble macrocycles. The crystal and molecular structure of dichloro-di-n-butyl(2,2’,6,6’-bipyr

A New Procedure for the Lightning Experiment: Mn2O7 and Ethanol

2010

Formation of Mn2O7 and its reaction with ethanol is commonly referred to as “underwater lightnings”. Classic procedures are reviewed, along with their weak points, and physical and chemical properties of dimanganese heptaoxide are shown. A new improved approach is finally presented, safer and easier, and suited for lecturehall activities.

Adducts of tin(IV) and organotin(IV) derivatives with 2,2′-azopyridine II. Crystal and molecular structure of SnMe2Br2AZP and further mössbauer and p…

1990

Abstract A series of adducts of tin(IV) derivatives with 2,2′-azopyridine, AZP, has been studied by Mossbauer and X-ray photoelectronic spectroscopies and the crystal and molecular structure of SnMe2Br2- AZP has been determined. The linear correlation of the Mossbauer parameter isomer shift with partial atomic charge on tin suggests the occurrence of a single homologous series of isostructural adducts. The correlation of the Mossbauer parameter quadrupole splitting and C-Sn-C bond angle permits their calculation in SnMe2X2AZP adducts (X = Cl, Br). The N1s binding energies, obtained by XPS data, pointed out two slightly different values for both pyridinic and azo-group nitrogens. The crystal…

Micro-analytical identification of the components of varnishes from South Italian historical musical instruments by PLM, ESEM-EDX, microFTIR, GC-MS, …

2014

Abstract A multi-analytical investigation was carried out to study varnish micro-samples from historical stringed musical instruments from the collection of the “Vincenzo Bellini” Conservatory in Palermo (Italy). This paper reports on the results of the application of five micro-destructive techniques: optical microscopy analysis of cross-sections, micro-Fourier transform infrared spectroscopy, gas chromatography coupled with mass spectrometry, pyrolysis gas chromatography coupled with mass spectrometry with thermochemolysis, and environmental scanning electron microscopy with X-ray microanalysis. The study provides microchemical information about the composition of the varnishes of the ins…

Geomorphological environment: dunes in Agrigento coast

2008

[ITA] La fascia costiera di San Leone (Agrigento-Siclia). è costituita da una spiaggia sabbiosa delimítala verso terra da un complesso dunale di particolare pregio. L'assetto geomorfologico di questo litorale è stato inlluenzato dal forte grado di antropizzazione del luogo. La fascia costiera nel tempo ha súbito degli avanzamenti e arreiramenti. Sono stati quindi analizzati e proposti alcuni rimedi. mirali alia ricostruzione. al mantenimenlo e alia diíesa della duna.

Protection by extra virgin olive oil against oxidative stress in vitro and in vivo. Chemical and biological studies on the health benefits due to a m…

2017

Abstract We report the results of in vivo studies in Caenorhabditis elegans nematodes in which addition of extra virgin olive oil (EVOO) to their diet significantly increased their life span with respect to the control group. Furthermore, when nematodes were exposed to the pesticide paraquat, they started to die after two days, but after the addition of EVOO to their diet, both survival percentage and lifespans of paraquat-exposed nematodes increased. Since paraquat is associated with superoxide radical production, a test for scavenging this radical was performed using cyclovoltammetry and the EVOO efficiently scavenged the superoxide. Thus, a linear correlation (y = -0.0838x +19.73, regres…

5-Amino-1-phenyl-3-trifluoromethyl-1H-pyrazole-4-carboxylic acid

2009

In the title compound, C11H8F3N3O2, there are two molecules in the asymmetric unit wherein the phenyl rings make dihedral angles of 65.3 (2) and 85.6 (2)° with the pyrazole rings. In the crystal, pairs of molecules are held together by O—H...O hydrogen bonds between the carboxyl groups, forming a centrosymmetric dimer with an R22(8) motif. Intramolecular N—H...O interactions are also present.

Tin( II ) and Lead( II ) 4‐Acyl‐5‐pyrazolonates: Synthesis, Spectroscopic and X‐ray Structural Characterization

2004

Novel tin(II) β-diketonate Sn(Q)2 complexes [HQ = 1-R1-3-R3-4-R4(C=O)-pyrazol-5-one; HQC: R1 = Ph, R3 = Me, R4 = Cy; HQS: R1 = Ph, R3 = Me, R4 = CHPh2; HQL: R1 = Ph, R3 = Me, R4 = CH2Ph; HQT: R1 = Ph, R3 = Me, R4 = CH2tBu; HQE: R1 = Ph, R3 = Me, R4 = Et; HQB: R1 = Ph, R3 = Me, R4 = tBu; HQW: R1 = Ph, R3 = Me, R4 = p-(tBu)Ph; HQR: R1 = Ph, R3 = Me, R4 = p-[(CH2)5CH3]Ph; HQN: R1 = p-NO2Ph, R3 = Me, R4 = Ph; HQM: R1 = Me, R3 = Me, R4 = Ph; HQD: R1 = Me, R3 = Me, R4 = Me; HQP: R1 = Ph, R3 = Ph, R4 = Ph; HQG: R1 = Ph, R3 = Ph, R4 = Me; HQF: R1 = p-CF3Ph, R3 = Me, R4 = Ph; HQH: R1 = p-CF3Ph, R3 = Me, R4 = Me] have been isolated and characterized by single-crystal X-ray diffraction analyses, IR, 1…

Il Progetto ATENA: Applicazione di metodologie innovative per la conservazione di manufatti metallici e ceramici da scavo archeologico e per il recup…

2007

Qui di seguito viene illustrato il progetto scientifico ATENA, svolto presso l'Istituto per lo Studio dei Materiali Nanostrutturati (ISMN) del Consiglio Nazionale delle Ricerche (CNR) e co-finanziato dal MIUR con Decreto Direttoriale 9-10-2002, n. 1105/2002. Il progetto si propone di applicare avanzate tecniche diagnostiche strumentali al fine di acquisire la dettagliata conoscenza microchimica e microstrutturale di manufatti metallici e ceramici antichi, di definirne il meccanismo di alterazione e/o degrado e di progettare, sintetizzare e validare opportuni prodotti e formulazioni per il restauro conservativo di tali manufatti. Le conoscenze acquisite sono utilizzabili anche per il recuper…