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Journal of Thermal Analysis and Calorimetry
Authors: Daniele Bergamasco, Franco Bulian, Andrea Melchior, Davide Menotti, Paolo Tirelli, and Marilena Tolazzi

their mechanical behavior is similar both to solid materials (elastic properties) and to liquid substances (viscous properties). This complex mechanical behavior can be deeply studied by using DMA [ 19 – 22 ]. The data obtained from DMA [ 17

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segments. Both of these processes can be investigated using differential scanning calorimetry (DSC). The glass transition region can be investigated very well using dynamic mechanical analysis (DMA). However, Saiani et al. [ 2 ] indicate that

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Abstract  

DMA and solid state 13C NMR techniques were used to measure historical parchment samples within the framework of the project (MAP) Micro Analysis of Parchment (EC contract No. SMT4-96-2101) in collaboration with the School of Conservation in Copenhagen. DMA was used in both thermal scan and creep modes. Thermal scans provided information on the transitions associated with the collagen polymer. Microthermal analysis was also used to obtain information on the topography and thermal conductivity of sample areas of 100 μm. Localised heating enabled measurements of softening transitions in the sample. This behaviour is influenced by the chemical composition of parchment. 13C NMR provided information on the carbon atoms associated with the polypeptide chains of the collagen in parchment. The behaviour of samples immersed in water and measured in DMA creep mode was used to measure the shrinkage behaviour of the parchment samples. The different but complementary techniques provided a means for characterising the physicochemical state of parchment samples.

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Abstract  

The physical aging of a system containing tetraglycidyl-4-4′-diaminodiphenylmethane (TGDDM), with a multifunctional novolac glycidyl ether resin hardened by 4,4′-diaminodiphenylsulphone (DDS) has been investigated by differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA). Samples fully cured were aged at temperatures between 200 and 250C, during periods of time from 1 to a maximum of 336 h. Furthermore, the dynamic mechanical relaxation behaviour annealed at temperature of 220C, was studied, aging during 24 and 168 h. The effect of the enthalpy relaxation during DSC heating scan is shown by the presence of an endothermic peak whose position and intensity depends on the aging conditions, both temperature and time. DSC studies suggest that enthalpy relaxation increases gradually with aging time to a limiting value for each temperature where structural equilibrium is reached. DMA results show that the effect of aging is to cause chain stiffening and a decrease in the height of the peak value of the loss factor.

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Abstract  

Mechanical behaviour play an important role in the election of an epoxidic formulation of well determined properties as it has a marked influence on both structural and external factors. Temperature and time strongly act on polymers properties owing to their viscoelastic nature. Knowledge of the dynamic moduli and properties of polymeric materials is indispensable for the design of this materials. At the same time, the influence of the temperature on polymers behaviour may be studied once the activation energy is known. In this paper the different dynamic moduli and activation energy are measured using a Perkin Elmer DMA 7. The relationships between the dynamic mechanical properties and the molecular weight of the polymers make possible the calculation of the molecular weight. Results reasonably agree with literature values.

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(DMA), which normally completes before [ 11 , 13 ]. Then, the simultaneous use of both techniques is recommended to optimise the process. In this article, chestnut shell tannin adhesives were prepared using different hardeners, namely, tris

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Abstract  

Issues encountered with dynamic mechanical analysis of artists’ acrylic emulsion paint films are presented alongside modifications to improve controlled relative humidity (RH) experiments using isothermal and thermal scanning conditions. Free films of titanium white (PW6) artists’ acrylic emulsion paints were cast as free films and their viscoelastic properties measured using the tensile mode of the dynamic mechanical analyser (DMA). Artists’ acrylic emulsion paints are within their glass transition temperature region at room temperature and are highly responsive to changes in ambient temperature and relative humidity, hence controlling relative humidity during analysis is vital to the successful analysis of these paints.

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CTFE content have been characterized by a series of thermal analysis techniques, including Thermogravimetric analysis (TG), Differential scanning calorimetry (DSC), Dynamic mechanical analysis (DMA), and Thermal mechanical analysis (TMA). The work

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Use of DSC and DMA to study crystallization as a possible cause for a glove tear

Neoprene rubber gloves are used as part of a Space Shuttle pressurized astronaut suit

Journal of Thermal Analysis and Calorimetry
Author: Doug Wingard

Abstract  

The Advanced Crew Escape Suit (ACES) is a pressurized suit worn by astronauts during launch and landing phases of Space Shuttle operations. In 2008, a large tear (12.7–25.4 mm long, between the pinky and ring finger) in the ACES left-hand glove made of neoprene latex rubber was found during training for Shuttle flight STS-124. An investigation to help determine the cause(s) of the glove tear was headed by the NASA Johnson Space Center (JSC) in Houston, Texas. Efforts at JSC to reproduce the actual glove tear pattern by cutting/tearing or rupturing were unsuccessful. Chemical and material property data from JSC such as GC-MS, FTIR, DSC, and TGA mostly showed little differences between samples from the torn and control gloves. One possible cause for the glove tear could be a wedding ring/band worn by an astronaut. Even with a smooth edge, such a ring could scratch the material and initiate the tear observed in the left-hand glove. A decision was later made by JSC to not allow the wearing of such a ring during training or actual flight. Another possible cause for the ACES glove tear is crystallinity induced by strain in the neoprene rubber over a long period of time and use. Neoprene is one among several elastomers known to be susceptible to crystallization, and such a process is accelerated with exposure of the material to cold temperatures plus strain. When the temperature is lowered below room temperature, researchers have shown that neoprene crystallization may be maintained at temperatures as high as 7.2–10 °C, with a maximum crystallization rate near −6.7 to −3.9 °C (Kell et al. J Appl Polym Sci 2(4):8–13, 1959 [<cite>1</cite>]). A convenient conditioning temperature for inducing neoprene crystallization is a typical freezer that is held near −17.8 °C. For work at the NASA Marshall Space Flight Center (MSFC), samples were cut from several areas/locations (pinky/ring finger crotch, index finger and palm) on each of two pairs of unstrained ACES gloves for DSC and DMA thermal analysis testing. The samples were conditioned in a freezer for various times up to about 14 days. Some rectangular conditioned samples were unstrained, while most were subjected to strains up to 250% with the aid of two slotted aluminum blocks and two aluminum clamps per sample. Trends were observed to correlate DSC data (heat of fusion) and DMA data (linear CTE and stress for iso-strain testing) with (a) sample location on each glove; and (b) percent strain during conditioning. Control samples cut “as is” from each glove location were also tested by DSC and DMA.

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