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An oxidative reaction of cellulose with sodium metaperiodate was performed. The oxidised groups were decomposed by treatment with UV light into free macroradicals. In the presence of acrylic monomers, in the vapour phase, these reactive sites become the starting points for the graft copolymerisation of the cellulose substrate. In this study we examined the graft yield as a function of the polymerisation time and the oxidation degree of cellulose. The grafted polymer was characterised using several analytical techniques, DSC analysis, GPC analysis, viscosity, FTIR and 13C CP-MAS. Information on the morphology of grafted chains with respect to the bulk cellulose was obtained, measuring the dynamic parameters in a careful 13C CPMAS NMR study. All proposed chemical reactions, if properly conducted, do not affect the crystallinity of cellulose and introduce only a very modest amount of oligomers, therefore they seem suitable for the consolidation and protection of precious cellulose based materials,which are of storical interest.

Multifarious applications of NMR (high-resolution NMR in liquid-state and in semi-solid matrices, low-field NMR relaxometry, and NMR-imaging) in the analysis of food components and entire food samples are described using examples of different food matrices and different problems related to food safety, traceability, geographical and botanical origin, farming methods, food processing, maturation and ageing, etc. Althoug NMR has not yet been recognized as an official methodology for the food control the numerous applications of NMR reported in the literature show the potenziality of this methodology also as an approach complementary to the other recognized conventional methodologies.

Multifarious applications of NMR (high-resolution NMR in liquid-state and in semi-solid matrices, low-field NMR relaxometry, and NMR-imaging) in the analysis of food components and entire food samples are described using examples of different food matrices and different problems related to food safety, traceability, geographical and botanical origin, farming methods, food processing, maturation and ageing, etc. Althoug NMR has not yet been recognized as an official methodology for the food control the numerous applications of NMR reported in the literature show the potenziality of this methodology also as an approach complementary to the other recognized conventional methodologies.

In this study a multi-analytical approach has been performed to characterise the constitutive materials of an ancient painted barkcloth or Tapa. Originating from Wallis Island, Polynesia, this cloth likely served utilitarian or ceremonial purposes and is part of the Felice Junck collection at the Pigorini, Muciv museum of Rome. During a recent conservation project, some micro-samples were taken from the support, brown and black painted areas and were investigated using the complementarity of SEM-EDX, FT-IR, Raman/SERS and solid-state 13C NMR and 1H HR-MAS spectroscopy. The combination of these techniques allowed the chemical characterization of the constitutive materials, from distinguishing the lignin and cellulose content of the support to the use of organic materials including condensed tannins (catechin, anthocyanidins, alkaloids), phlobaphene and vegetal anthraquinone based Morinda genus dyes for the decorations. A primary focus was placed on an understanding of its state of conservation where data of alteration products collected, namely metal carboxylates and oxalates can serve to formulate apt restoration efforts for this specific artefact.

Agar is an interesting and versatile biopolymer capable of forming hydrogels useful in different applications. In particular, in the field of Cultural Heritage agar gels are often used as tools for cleaning the surfaces of artifacts. Agar gels are thermoreversible, peelable materials, exhibiting high retention of water and an intrinsic cleaning capability that can be increased and modulated by loading different cleaning agents. Agar gels are able to solubilize and retain dirt, and allow a confined release of the liquid phase, which is especially important when they are applied on water sensitive substrates. A detailed knowledge of the role of water in agar gels and of water/agar interactions is important to fully understand the properties and performances of agar gels as cleaning materials. Here we report the results of a systematic study aimed at exploring the water state and the types of water (i.e. bound non-freezable, bound freezable and freezable bulk-like) in agar hydrogels prepared from four different types of commercial agar powders. The influence of agar concentration on the water behaviour in the hydrogels was also investigated. The total water content, the identification and quantification of the different types of water was carried out by gravimetric, thermogravimetric and calorimetric analyses, while water mobility and localization in the gel network were investigated by unilateral H-1 NMR. Moreover, H-1 NMR depth profiles of agar gels applied on Noto stone specimens were collected to monitor the gel deformation due to water release and to evaluate the ability of the gel in controlling the water release into a porous material. (C) 2018 Elsevier B.V. All rights reserved.

A portable unilateral nuclear magnetic resonance (NMR) instrument was used to detect in field conditions the water status of leaves of herbaceous crops (Zea mays, Phaseolus vulgaris), mesophyllous trees (Populus nigra), and natural Mediterranean vegetation characterized by water-spending shrubs (Cistus incanus) and water-saving sclerophyllous trees (Quercus ilex). A good relationship was observed between NMR signal, leaf relative water content, and leaf transpiration in herbaceous leaves undergoing fast dehydration or slowly developing a drought stress. A relationship was also observed between NMR signal and water potential of Populus leaves during the development of a water stress and when leaves recovered from the stress. In the natural vegetation, the relationship between NMR signal and water status was found in Cistus, the species characterized by high transpiration rates, when measured during a drought stress period and after a rainfall. In the case of the sclerophyllous Quercus, the NMR signal, the relative water content, and the transpiration rate did not change at different leaf water status, possibly because a large amount of water is compartmentalized in cellular structures and macromolecules. The good association between NMR signal and relative water content was lost in leaves exposed for 24 h to dehydration or to an osmotic stress caused by polyethylene glycol feeding. At this time, the transverse relaxation time became longer than in leaves maintained under optimal water conditions, and two indicators of membrane damage, the ion leakage and the emission of products of membrane lipoxygenation [(Z)-3-hexenal, (Z)-3-hexenol, and (E)-2-hexenol], increased. These results taken all together give information on the physiological state of a leaf under a developing stress and show the usefulness of the NMR instrumentation for screening vegetation health and fitness in natural and cultivated conditions. It is concluded that the portable unilateral NMR instrument may be usefully employed in field conditions to monitor nondestructively the water status of plants and to assist agricultural practices, such as irrigation scheduling, to minimize stomatal closure and the consequent limitation to plant production.

A series of copolyesters (PE) of low molecular weight containing propyloxy-substituted aromatic ring and/or ethylenic sequences between aromatic units were prepared by melt polycondensation between corresponding diacids and diacetates, and used as precursor of poly(ester-co-polyhydrazide) (PEH) new copolymers. The PEs showed to have thermotropic properties, with transition temperatures which depend on the chemical composition and with a good interval of stability of the mesophase. The corresponding PEHs were obtained by high-temperature polycondensation of carboxyl-terminated PEs with terephthalic dihydrazide. The PEHs showed as well a stable mesophase in the melt, and improved thermal stability respect to polyesters. All the polymers were characterized by elemental analysis, inherent viscosity, infrared and 13 C solid state NMR spectroscopy, thermal and thermogravimetric analysis and optical microscopy. Fibers of PEHs were obtained by melt-spinning and characterized by WAXS analysis.

A new series of alkoxy-substituted poly(p-phenylene 1,3,4-oxadiazole)s modified by the insertion of small percentages of various comonomers were synthesized through the precursor polyhydrazides. The comonomers used contained trans double bonds or meta-alkoxy-substituted aromatic rings to improve the solubility of the final polymers. The synthesized copolymers were chemically characterized by 1H NMR and Fourier transform infrared spectroscopy. In some cases, the copolymers really showed improved solubility in organic solvents. The 15N solid-state NMR technique was applied to examine the degree of conversion from the precursor polyhydrazides to the final polymers, which determined the effective conjugated length in the target polyoxadiazoles. Thermal stability and structural characteristics of all the polymers as well as a preliminary investigation on the optical properties of polyoxadiazoles are also reported. The copolymers retained high absorbance in the UV region and high transmission in the whole telecommunication range. © 2003 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 41: 3916–3928, 2003