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The glass transition temperatures,T g, and thermal effects of polymerization,ΔH, have been determined for five epoxy adhesives of unknown composition. From the trendsΔH vs./t cure it has been possible to attain a phenomenological kinetic order of the polymerization rate at 100° through an iterative calculation procedure. For most of the investigated adhesives there are reasons (double peak of polymerization and doubleT g signal) to assume that they are graft copolymers.

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Abstract

Prehistoric metal findings from Liguria are numerous, however, even though there were many metalliferous mines, the metal-working sites have not yet been ascertained.

This work discusses results on some metal objects from different archaeological sites in Liguria.

The objects examined were: 1) two melting drops 2) an axe, and 3) a knife. The physico-chemical investigation techniques employed were:

  1. -X-ray diffraction,
  2. -radiography,
  3. -microdrawing method, followed by optical and electron scanning microscopy observations,
  4. -differential thermal and thermogravimetric analyses to characterize the clay core found inside a socketed knife.

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Journal of Thermal Analysis and Calorimetry
Authors: F. Giordano, A. Rossi, R. Bettini, A. Savioli, A. Gazzaniga, and Cs. Novák

Abstract  

The thermal behavior of binary mixtures of paracetamol and a polymeric excipient (microcrystalline cellulose, hydroxypropylmethylcellulose and cross-linked poly(vinylpyrrolidone)) was investigated. The physical mixtures, ranging from 50 to 90% by mass of drug, were submitted to a heating-cooling-heating program in the 35–180C temperature range. Solid-state analysis was performed by means of differential scanning calorimetry (DSC), hot stage microscopy (HSM), micro-Fourier transformed infrared spectroscopy (MFTIR), and scanning electron microscopy (SEM). The polymeric excipients were found to address in a reproducible manner the recrystallization of molten paracetamol within the binary mixture into Form II or Form III. The degree of crystallinity of paracetamol in the binary mixtures, evaluated from fusion enthalpies during the first and second heating scans, was influenced by the composition of the mixture, the nature of the excipient and the thermal history. In particular, DSC on mixtures with cross-linked poly(vinylpyrrolidone) and hydroxypropylmethylcellulose with drug contents below 65 and75%, respectively, evidenced the presence only of amorphous paracetamol after the cooling phase. Microcrystalline cellulose was very effective in directing the recrystallization of molten paracetamol as Form II.

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Abstract  

The thermal behaviour of binary mixtures between β-cyclodextrin (β-CD) and either carbamazepine polymorphic Form I (CBZ I), Form III (CBZ III) or dihydrate was investigated in order to assess possible interactions of CBZ solid phases with β-CD. Physical mixtures and kneaded binaries of β-CD and different CBZ crystal forms were studied by differential scanning calorimetry, thermogravimetric analysis and hot stage microscopy. The pattern of transition of CBZ Form III into Form I is strongly influenced by β-CD. The liquid-solid transition is practically absent when anhydrous CBZ/β-CD mixes are tested, as a consequence of an interaction between β-CD and liquid CBZ that hinders CBZ recrystallisation as Form I occurring after CBZ Form III melting. Water loss on heating of CBZ dihydrate in the presence of β-CD leads in all cases to the formation of CBZ Form I.

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Abstract  

Three different analytical techniques: INAA, X-ray fluorescence and atomic absorption spectrometry were used at the JRC Ispra to test the total homogeneity of four candidate botanic reference materials supplied by NBS. Without adopting complex statistical formalities a “degree of inhomogeneity” was estimated in each sample for the elements considered in the test. The operating procedures and the results obtained are presented and discussed.

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Journal of Thermal Analysis and Calorimetry
Authors: L. El Watik, P. Antonetti, Y. Claire, H. Zineddine, J. Kaloustian, C. Rossi, and A. Perichaud

Abstract  

The authors studied the ignifugation and the kinetic of thermal degradation of the Styrene-Butadiene copolymer with an intumescent system Ammonium polyphosphate-Pentaerythrinol-Melamine. For that, they used the thermogravimetric and oxygen index techniques. The best formulation of intumescent system which can give the optimum results is proposed.

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Community Ecology
Authors: M. Marignani, C. Ricotta, F. Rossi, A. Pavesi, and G.C. Avena

Subtaxon-to-taxon ratios such as the species-to-genus ratio have been frequently used in ecology and biogeography despite their well-known sample size dependence. For instance, any subtaxon-to-taxon ratio is an increasing function of the area sampled. Hence, its validity as an ecological indicator is problematic at best. This drawback can be avoided by constructing taxon-subtaxon curves. Owing to their scale-free nature, taxon-subtaxon curves standardize the information in subtaxon-to-taxon ratios allowing for meaningful comparison of datasets.

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Journal of Thermal Analysis and Calorimetry
Authors: R. Bettini, G. Bertolini, E. Frigo, A. Rossi, I. Casini, I. Pasquali, and F. Giordano

Abstract  

The aim of this work was to study the solubility in supercritical CO2 of the hydrated phase of three model drugs, namely theophylline, carbamazepine, and diclofenac sodium, in comparison with the respective anhydrous form. Possible solid-state modifications, stemming from the interaction with supercritical CO2, were investigated by differential scanning calorimetry, thermogravimetric analysis, hot stage microscopy, Fourier Transform infrared spectroscopy and Karl-Fischer titrimetry. It was found that all three pharmaceutical hydrates exhibited higher solubility in supercritical CO2 than the relevant anhydrous phases. In the case of theophylline monohydrate, the instability of the crystal phase at the experimental temperature adopted has been evidenced. Diclofenac sodium tetrahydrate represents a peculiar case of chemical interaction with the acid supercritical fluid, mediated by crystal water.

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Abstract  

Aim of this work was to investigate the solid-state characteristics of micronized acetylsalicylic acid (ASA), produced by rapid expansion of a supercritical carbon dioxide solution (RESS) and to assess whether a correlation could be found between process parameters and solid-state characteristics. Drug solubility in supercritical CO2 was first assessed under various pressure and temperature conditions. DSC, FT-IR, PXRD, SEM, laser light scattering and HPLC were used to characterise the solid phases produced by the RESS. The obtained particles were crystalline, with spectroscopical and diffractometrical pattern overlapping those of the starting available product. However, a strong reduction of particle size was obtained, linearly correlated to pressure imposed during the RESS process, while temperature did not seem to have a major effect. Similar influence of pressure was observed on the final melting temperature of the micronized ASA. The application of a mathematical model allowed to conclude that the melting temperature depression of RESS-prepared ASA powders can be attributed to the decrease of particle dimension rather than to the formation of different solid phases or impurities.

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Journal of Thermal Analysis and Calorimetry
Authors: L. El Watik, Y. Claire, H. Zineddine, C. Rossi, J. Kaloustian, M. Sergent, and A. Périchaud

Abstract  

The study of the thermal degradation of the fireproof polystyrene—butadiene copolymer by an intumescent system: ammonium polyphosphate (APP)—pentaerythritol (PER)—talc (TAL), was done through an experimental process. Thermogravimetry under air sweeping was used. We observed for the degradation rate of the mixture with fireproofing agents, in the field of 20 to 50% mass loss, a better linear increasing when this mixture contains more TAL and the ratio APP/PER is smaller.

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