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Summary Simulation of thermal ageing is an important part of qualification of materials designed for the use in nuclear power plants (NPP). According to standards, the simulation of long-term service thermal ageing is performed isothermally at elevated temperature using Arrhenius methodology. The samples or equipment are aged in thermal chamber, to bring them to the same state as after long-term service time. To proceed a reliable simulation, the testing parameters should be taken very carefully and the accelerator factors should not be too high. The testing temperature and time and the activation energy are the most important parameters. Determination of these factors and the limitations of their use in practice are discussed.

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Abstract  

Thermoanalytical investigations TGA/DTG/DSC of polyamide–imide enamel after thermal ageing have been presented. The lifetimes at 260, 270, 280, 290, 300 °C were determined. The thermograms of the enamels after attaining of their lifetimes much depend on the ageing temperature. The temperatures of 5% loss of mass that much increase after thermal ageing appear the most sensitive indicator of ageing rate. The residue of mass at 800 °C increases after ageing, even to 27%, due to diffusion of copper ions from the conductor into enamel during annealing. The copper contents in aged coatings could be also an indicator of ageing rate.

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Abstract  

The accelerated thermal degradation of low-density polyethylene (LDPE) was studied in air at atmospheric pressure and temperatures of 70, 80, 90 and 100C. The changes in elongation at break, traction resistance and density as a result of accelerated thermooxidative degradation were followed. Thermal analysis curves (TG, DTG and DTA) of non-aged and thermally aged LDPE were recorded, and the thermal analysis results were compared with those relating to the variations in the elongation at break, the traction resistance and the density as a consequence of accelerated thermal aging.

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Abstract  

To reveal the fire injuring of parchment, the changes in the thermal behaviour of some goat parchments, obtained from skins originating from different animals, as a result of thermal aging were determined by thermal analysis methods (DSC; simultaneous TG/DTG, DSC; micro hot table (MHT)). Thermal aging of parchments was revealed to bring about the decrease in shrinkage temperature, absolute value of enthalpy of denaturation in water and some changes in non-isothermal parameters characteristic for dehydration process in static air atmosphere. The results obtained by DSC analysis performed in N2 and O2 flows as well as those obtained by simultaneous TG/DTG, DSC analyses have shown that both softening (melting) process parameters and parameters of thermo-oxidative processes have not been changed by thermal ageing. The results obtained by thermal analysis methods were correlated with those obtained by microscopic investigation of parchment samples immersed in water and scanning electron microscopy (SEM). The application of these microscopic techniques has revealed the morphology changes in the investigated parchments as a result of thermal degradation.

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-cure can be measured and quantified using DSC. However, glass transition, relaxations and thermal ageing [ 2 ] give a low response with DSC, particularly when the polymer is highly crosslinked and mobility restricted by the fibrous filler phase

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-composites were evaluated using a thermal aging test for applications car interior materials. The objective of this study was to investigate and compare the interfacial adhesion of MAPLA-treated bio-composites. We compared the mechanical properties

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Journal of Thermal Analysis and Calorimetry
Authors:
B. Roduit
,
Ch. Borgeat
,
B. Berger
,
P. Folly
,
B. Alonso
, and
J. N. Aebischer

Summary An advanced study on the thermal behaviour of double base (boost and sustain propellant) rocket motor used in a ground to air missile has been carried out by differential scanning calorimetry (DSC). The presence of two propellants as well as the different experimental conditions (open vs. closed crucibles) influence the relative thermal stability of the energetic materials. Several methods have been presented for predictions of the reaction progress of exothermic reactions under adiabatic conditions. However, because decomposition reactions usually have a multi-step nature, the accurate determination of the kinetic characteristics strongly influences the ability to correctly describe the progress of the reaction. For self-heating reactions, incorrect kinetic description of the process is usually the main source of serious errors for the determination of the time to maximum rate under adiabatic conditions (TMRad). It is hazardous to develop safety predictive models that are based on simplified kinetics determined by thermoanalytical methods. Applications of finite element analysis (FEA) and accurate kinetic description allow determination of the effect of scale, geometry, heat transfer, thermal conductivity and ambient temperature on the heat accumulation conditions. Due to limited thermal conductivity, a progressive temperature increase in the sample can easily take place resulting in a thermal explosion. Use of both, kinetics and FEA [1], enables the determination of the reaction progress and temperature profiles in storage containers. The reaction progress and temperature can be determined quantitatively at every point in time and in space. This information is essential for the design of containers of self-reactive chemicals, cooling systems and the measures to be taken in the event of a cooling failure.

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Abstract  

The hyphenated thermal analysis-mass spectrometry technique (TA-MS) was applied for the investigation of the thermal behavior of reference and aged parchment samples. The kinetic parameters of the process were calculated independently from all recorded TA and MS signals. The kinetic analysis showed the distinct dependence of the activation energy on the reaction progress. Such behavior is characteristic for the multistage mechanism of the reaction. The comparison of the kinetic parameters calculated from the different signals i.e. TG, DSC, MS for H2O, NO and CO2, however, indicated that they were differently dependent on the aging of the sample. For the parchment samples, the aging almost does not change the kinetics of the decomposition calculated from the DSC data: the influence of aging seems to be too negligible to be detected by these techniques. On the other hand, the much more sensitive mass spectrometric technique applied to the kinetic analysis allowed monitoring of visible changes in the thermal behavior of the parchment samples due to the aging process. The influence of aging was especially visible when the MS signals of water and nitric oxide were applied for the determination of the kinetic parameters. The applied method of the kinetic analysis allowed also the prediction of the thermal behaviour of reference and aged parchment samples under isothermal and modulated temperature conditions. Presented results have confirmed the usefulness of thermoanalytical methods for investigating behaviour of such complicated systems as leather or parchment.

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Up-scaling of dsc data of high energetic materials

Simulation of cook-off experiments

Journal of Thermal Analysis and Calorimetry
Authors:
B. Roduit
,
Ch. Borgeat
,
B. Berger
,
P. Folly
,
H. Andres
,
U. Schädeli
, and
B. Vogelsanger

Abstract  

Differential scanning calorimetry (DSC) carried out with few heating rates was applied in the studies of the thermal properties of four energetic materials: EI propellant, high explosive PBXW-17, pyrotechnic mixtures with composition B/KNO3 (50:50) and B/KNO3 (30:70). DSC signals, after optimization of the baseline, were used for the calculation of the kinetic parameters (KP) of the decomposition process applying advanced kinetic software designed by AKTS. The determination of the kinetic parameters was based on the differential iso-conversional method of Friedman. The correctness of the estimation of KP was checked by the comparison of the experimental and predicted courses of the decomposition. The slow cook-off experiments of above mentioned energetic materials were carried out with a heating rate of 3.3C h–1. For the simulation of the experimental results, the heat balance based on the finite element analysis (FEA) was applied together with the advanced kinetic description of the reaction. The comparison of the experimental and simulated data indicates that applied procedure resulted in a very good prediction of the temperature of the ignition. Application of commonly used, simplified assumptions concerning the mechanism of the decomposition (such as 1st or n th order mechanisms) led to significantly worse prediction of the cook-off temperatures.

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