Papers by Alberto Spinella
The aim of this work is to define the conservation state and to ascertain the provenance of raw m... more The aim of this work is to define the conservation state and to ascertain the provenance of raw materials used in the construction of the Acqualadrone Rostrum. In 2008 the rostrum (an offensive naval weapon mounted on the prow at the waterline), from an ancient warship was recovered from the Mediterranean near Acqualadrone, Messina, Sicily. The archaeological discovery 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. The physical-chemical investigation, by using some complementary spectroscopic techniques, was focused on the characterization of both the metal alloy and the wooden fragments. The results reveal the use of leaded bronze (Cu, 70%; Pb, 20%; Sn, 10%) in the manufacturing process of the alloy and the use of lead whose isotopic composition is referable to either Spanish or Cypriot mines. The analysis of the results relating to the wooden samples indicates construction from pinewood. A derivatized extract of black wood yielded forms of abietic acid and sandaracopimaric acid consistent with pine pitch waterproofing. In summary, the rostrum was manufactured of pine wood and subsequently waterproofed with pine pitch. The subsequent 2300 years included battle, foundering, and marine burial followed by anoxia, bacterial colonization, sulfate reduction, and mobilization of transition metals, which produced pyrite and copious appended sulfur functionality. Furthermore a quantitative determination and the cristallinity degree evaluation of the holocellulose were performed through solid state NMR on a wooden sample obtained by coring. Finally results obtained by solid state NMR relaxometric experiments and 2D heterocorrelated analyses will be the subject of a forthcoming work
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Environmental Science and Pollution Research, 2021
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Cellulose, 2020
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Frontiers in Chemistry, 2020
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Beilstein Journal of Organic Chemistry, 2019
Two mixtures of polyaminoazides were synthesized by a nucleophilic displacement strategy providin... more Two mixtures of polyaminoazides were synthesized by a nucleophilic displacement strategy providing no separation of the components. The mixtures were adequately characterized by means of combined HR-ESIMS, FTIR and NMR techniques and, despite their complexity, they were successfully used to accomplish the subsequent preparation of pH-sensitive calixarene hyper-reticulated nanosponge materials. The desired responsivity to pH variations of the nanosponges obtained was verified by means of absorption tests on a set of organic pollutant model molecules.
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Beilstein journal of organic chemistry, 2018
New calixarene-based nanosponges (NSs), i.e., hyper-reticulated polymers constituted by calixaren... more New calixarene-based nanosponges (NSs), i.e., hyper-reticulated polymers constituted by calixarene monomer units joined by means of bis(1,2,3-trialzolyl)alkyl linkers, were synthesized, characterized and subjected to preliminary tests to assess their supramolecular absorption abilities towards a set of suitable organic guests, selected as pollutant models. The synthesis was accomplished by means of a CuAAC reaction between a tetrakis(propargyloxy)calix[4]arene and an alkyl diazide. The formation of the polymeric network was assessed by means of FTIR and C{H} CP-MAS solid-state NMR techniques, whereas morphological characterization was provided by SEM microghaphy. The materials were proved to possess pH-dependent sequestration abilities, due to the presence of the weakly basic triazole linkers. Sequestration efficiency indeed depends on the effective occurrence of both electrostatic and hydrophobic interactions between the guest and the polymer lattice. Thus, our NS nanosponges can b...
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Microchemical Journal, 2017
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Journal of Polymer Science Part A: Polymer Chemistry, 2017
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Zeitschrift für Physikalische Chemie, 2016
Ce:YAG-poly(methyl methacrylate) (PMMA) composites were prepared by using a melt compounding meth... more Ce:YAG-poly(methyl methacrylate) (PMMA) composites were prepared by using a melt compounding method, adding several amounts of Ce:YAG in the range 0.1–5 wt. %. The optical properties of the obtained composites and of the composites combined with a blue LED were measured to investigate the effect of the amount of Ce:YAG on the resulting emitted light in view of possible application in white LED manufacture. An increase in Ce:YAG amount caused an increase in the emission and a shift of 15 nm, influencing the white LED performance. The structure and morphology of the composites were studied. The results show that the interaction between the two components, observed by using solid state NMR experiments, are the responsible for the observed shift.
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Microchemical Journal, 2016
Abstract Solid-state NMR spectroscopy was applied to characterize the wooden part of a roman Rost... more Abstract Solid-state NMR spectroscopy was applied to characterize the wooden part of a roman Rostrum recovered in the Tyrrhenian Sea in the Acqualadroni area (Messina, Italy). The Acqualadroni Rostrum has been, in the recent past, investigated to establish its provenance and conservation. In this paper, solid-state NMR was used to obtain information on the conservation state of the wood as a preliminary step for the conservation process. A wooden sample of this artifact, collected by coring, was divided in four parts in order to correlate the conservation state to the depth. Results were compared with those obtained for a modern wood of the same species. A structural study was performed by acquiring 13C cross-polarization magic angle spinning spectra to evaluate the cellulose crystallinity degree and the lignin condensation degree. In addition, the holocellulose–lignin ratio and the cellulose–lignin residual interactions were determined through variable contact time experiments and relaxation times determination respectively. Being the solid-state NMR a non-destructive technique, all measurements were performed with no modification of the samples such as solvent extraction or other chemical treatment, making the samples available for further analytical investigation.
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Polymeric composites of lanthanide-doped materials were recently considered as potential candidat... more Polymeric composites of lanthanide-doped materials were recently considered as potential candidates for the development of light emitting diodes, lasers and luminescent concentrators for solar cells. In particular, nanoparticles of yttrium aluminum garnet (YAG) doped with cerium ions embedded in polymetylmetacrylate (PMMA) have been valuable for white LED devices [1,2]. Different structures and micromechanical properties have been observed when the methacrylic acid (MAA) is present in the composite. With the aim to understand the effect of MAA on the composite structure, a series of Eu:YAG composites prepared by in situ polymerization starting from mixtures of MAA and methylmetacrylate (MMA) were investigated. The structure were investigated by using Small Angle X-ray Scattering, X-ray Diffraction, and 13C Cross-Polarization Magic Angle Spinning NMR. The last technique gave information also about the interactions between the components. Results will be presented and discussed
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The roman rostrum found in the sea of Acqualadrone (ME) was characterized in our previous papers.... more The roman rostrum found in the sea of Acqualadrone (ME) was characterized in our previous papers. In the present work solid state NMR spectroscopy was applied on a wooden sample of the same artefact collected by coring and divided in four parts in order to correlate the conservation state to the depth. Results were compared with those obtained for a modern wood of the same species. A structural study was performed by the acquisition of 13C Cross Polarization Magic Angle Spinning (13C CP MAS NMR) spectra. These spectra were acquired to assign the chemical shifts of the species that are present in the wooden matrix. In addition the spectra analysis allowed us to determine the cellulose crystallinity degree and the lignin condensation degree. The holocellulose-lignin ratio and the cellulose-lignin residual interactions were evaluated through variable contact time (VCT) experiments and through the relaxation times determination respectively. Furthermore these latter experiments allowed us to evaluate the dynamic modifications occurring in the lignin and in the cellulose during the degradation process. Solid state NMR results showed a decrease of carbohydrates with a complete cleavage of hemicelluloses. The crystallinity degree decreases in depth while the lignin condensation was not modified. Dynamic relaxation times studies demonstrated cellulose and lignin are still interacting to each other in the deepest samples of the wood
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Journal of Hazardous Materials, 2015
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Lecture Notes in Chemistry, 2012
ABSTRACT An overview of applications of Small Angle X-ray Scattering (SAXS) techniques to topics ... more ABSTRACT An overview of applications of Small Angle X-ray Scattering (SAXS) techniques to topics of interest in the field of Cultural Heritage is presented. The basic concepts of the technique, a description of sources and laboratory instrumentation and some models and methods for data analysis are discussed. Applications of SAXS to various kinds of materials are reported to obtain information on the structure useful to shed light in some subjects such as preparation, physical treatment, traceability and degradation of materials.
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Polymer Degradation and Stability, 2012
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aidic.it
... Fig. 4. left) 13 C í 1 Hý CP-MAS NMR spectra of pure PMMA and of Ce:YAG-PMMA composite; right... more ... Fig. 4. left) 13 C í 1 Hý CP-MAS NMR spectra of pure PMMA and of Ce:YAG-PMMA composite; right) HR-TEM micrograph of Ce:YAG-PMMA composite. ... Soc. 149, J85. [3] Kasuya, R., Isobe, T., Kuma, H., Katano, J., 2005, J. Phys. Chem. B, 109, 22126-22130. ...
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Materials, 2013
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Papers by Alberto Spinella