Differential scanning calorimetry (DSC) and temperature-modulated DSC study of three mouthguard materials☆

2007 ◽  
Vol 23 (12) ◽  
pp. 1492-1499 ◽  
Author(s):  
F MENG ◽  
S SCHRICKER ◽  
W BRANTLEY ◽  
D MENDEL ◽  
R RASHID ◽  
...  
2009 ◽  
Vol 81 (10) ◽  
pp. 1931-1952 ◽  
Author(s):  
Bernhard Wunderlich

With standard differential scanning calorimetry (DSC), it is possible to derive calorimetric data for equilibrium or metastable samples. The introduction of temperature-modulated DSC (TMDSC) permits in its quasi-isothermal (non-scanning) mode (TMDC), long-time apparent heat capacity measurements of high precision (±1 %). For flexible molecules, heat capacity measurements from the various calorimetric methods could be combined in the ATHAS Data Bank, which now contains experimental data for over 200 materials. These data were linked to the vibrational and large-amplitude motion of the constituent atoms and molecules, to provide a base for the judgement of the thermal analyses, extending outside the range of equilibrium or metastability with an error of only 2-5 %. The TMDC together with DSC is now able to quantitatively assess the reversibility of thermal processes. A sufficient number of systems have been analyzed in this fashion to develop better understanding of macro-, micro-, and nanophases of flexible macromolecules. The new concepts discussed are: (1) multiple glass transitions due to possible rigid-amorphous fractions (RAFs) and glass transitions within crystals, both observed in semicrystalline macromolecules, and (2) locally reversibly melting on the surface of chain-folded crystals. The locally reversible melting decreases with crystal perfection and also disappears when the chains become rigid.


e-Polymers ◽  
2009 ◽  
Vol 9 (1) ◽  
Author(s):  
Xiong-Yan Zhao

AbstractTwo PA 6/clay nanocomposites, NCN5 and NCN10 with 5 and 10% (wt %) clay, respectively, were prepared by a twin screw extruder. The effects of annealing including solid-state annealing and melt-state annealing on the polymorphic behavior and thermal property of nanocomposites have been comparatively studied as a function of annealing time using Modulated Differential Scanning Calorimetry (MDSC). It was demonstrated that NCN5 and NCN10 exhibit a similar polymorphic behavior when they were annealed in solid-state for different durations. As the annealing temperature was elevated to 245 °C (melt-state annealing), significant differences in thermal behavior and polymorphism between NCN5 and NCN10 could be found. For NCN5, the α structure became the absolutely dominating crystalline phase independent of the annealing durations, for NCN10, however, the formation of γ structure is greatly enhanced and longer annealing time would amplify this phenomenon. Moreover, a low-temperature endothermic peak was observed around 180 °C in both NCN5 and NCN10 samples which was also found to strongly depend on the thermal history.


Pharmaceutics ◽  
2020 ◽  
Vol 12 (9) ◽  
pp. 800
Author(s):  
Agata Drogoń ◽  
Marcin Skotnicki ◽  
Agnieszka Skotnicka ◽  
Marek Pyda

The objective of this study was to characterise amorphous indapamide (IND) subjected to the physical ageing process by differential scanning calorimetry (DSC). The amorphous indapamide was annealed at different temperatures below the glass transition, i.e., 35, 40, 45, 65, 75 and 85 °C for different lengths of time, from 30 min up to a maximum of 32 h. DSC was used to characterise both the crystalline and the freshly prepared glass and to monitor the extent of relaxation at temperatures below the glass transition (Tg). No ageing occurred at 35, 40 and 45 °C at the measured lengths of times. Molecular relaxation time constants (τKWW) for samples aged at 65, 75 and 85 °C were determined by the Kohlrausch-Williams-Watts (KWW) equation. The fragility parameter m (a measure of the stability below the glass transition) was determined from the Tg dependence from the cooling and heating rates, and IND was found to be relatively stable (“moderately fragile”) in the amorphous state. Temperature-modulated DSC was used to separate reversing and nonreversing processes for unaged amorphous IND. The enthalpy relaxation peak was clearly observed as a part of the nonreversing signal. Heat capacities data for unaged and physically aged IND were fitted to Cp baselines of solid and liquid states of IND, were integrated and enthalpy was presented as a function of temperature.


2016 ◽  
Vol 19 (2) ◽  
pp. 78-87
Author(s):  
Ha Tran Nguyen ◽  
Thu Thi Le Nguyen ◽  
Thang Van Le ◽  
Lam Le

The thiol-isocyanate chemistry was used to create crosslinked polymer networks without the use of solvent and catalyst. The preliminary study of a model thiol-isocyanate reaction was performed to confirm the “efficient linking” feature of the reaction, as indicated by online FTIR method. Temperature-modulated differential scanning calorimetry (TMDSC) was used to characterize the occurrence of the networks thiol-isocyanate reaction between multifunctional reactants, the influence of temperature on the reaction rate and the glass transition temperatures of the partially and fully cured networks. The investigation could pave the way for the design and tailoring of new cross-linked polymer materials for on-demand applications.


2019 ◽  
Author(s):  
Andreas Boelke ◽  
Yulia A. Vlasenko ◽  
Mekhman S. Yusubov ◽  
Boris Nachtsheim ◽  
Pavel Postnikov

<p>The thermal stability of pseudocyclic and cyclic <i>N</i>-heterocycle-stabilized (hydroxy)aryl- and mesityl(aryl)-l<sup>3</sup>-iodanes (NHIs) through thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) is investigated. NHIs bearing <i>N</i>-heterocycles with a high N/C-ratio such as triazoles show among the lowest descomposition temperatures and the highest decomposition energies. A comparison of NHIs with known (pseudo)cyclic benziodoxolones is made and we further correlated their thermal stability with reactivity in a model oxygenation. </p>


Author(s):  
Hariyanti Hariyanti ◽  
Sophi Damayanti ◽  
Sasanti Tarini

Sinkonin praktis tidak larut dalam air, sedikit larut dalam kloroform dan alkohol. Hal ini berdampak pada rendahnya penetrasi transfollicular sinkonin, karena hanya bahan aktif hidrofilik yang mampu melewati hair follicle. Dengan demikian dibutuhkan satu sistem penghantaran yang mampu menurunkan hidrofobisitas sinkonin untuk meningkatkan penetrasi sinkonin ke follicle. Niosom merupakan vesikel ampifilik dengan struktur lapisan rangkap yang terbentuk dari hidrasi kombinasi surfaktan nonionik dan kolesterol yang mampu menurunkan hidrofobisitas sinkonin. Penelitian ini bertujuan untuk menentukan proses pembuatan niosom sinkonin yang optimum. Pembuatan niosom sinkonin diawali dengan menentukan temperatur gelasi (Tg) dari span 60 dengan Differential Scanning Calorimetry (DSC), kemudian dilanjutkan dengan optimasi proses meliputi: optimasi kecepatan rotavapor pembentukan film lapis tipis, temperatur hidrasi, kecepatan rotavapor hidrasi, waktu hidrasi, dan waktu sonikasi. Karakteristik vesikel niosom yang optimal meliputi: ukuran partikel dan indeks polidispersitas dengan menggunakan Particle Size Analized (PSA) serta efisiensi penjeratan sinkonin dengan menggunakan KCKT. Temperatur gelasi (Tg) span 60 45±2 oC, kecepatan rotavapor pembentukan film lapis tipis niosom 210 rpm, temperatur hidrasi 55±2 oC, kecepatan rotavapor hidrasi 210 rpm, waktu hidrasi 20 menit, waktu sonikasi suspensi niosom 1 menit. Ukuran vesikel yang diperoleh adalah 100–200 nm, indeks polidispersitas 0,2–0,4 dan efisiensi penjeratan niosom sinkonin 84,49±0,0025%. Proses pembuatan niosom sinkonin memiliki pengaruh besar terhadap hasil ukuran vesikel dan efisiensi penjeratan niosom sinkonin.


Author(s):  
Sheila Liza B. Dal

Abstract The choice of epoxy mold compound (EMC) for an electronic package is based mostly on how much protection it provides to the active components in the package. But the choice is not a straightforward process. Rather it is mostly trial and error using different assembly parameters to find the most robust material while assembly defects are monitored. One such defect associated to EMC processing is wire sweep, and many studies have shown that it is mainly caused by viscosity changes in the EMC. In this study, samples of EMC in various stages of shelf life and staging times were analyzed for degree of cure using a method called differential scanning calorimetry (DSC). Samples are then processed at assembly for wire sweep measurement. It was found out that degree of cure increases with staging time at different rates for each shelf life. It was also found out that wire sweep did not only increase with degree of cure but it was also found to be predictable with respect to the latter. Using this information, the age and staging limit for each material was identified that would not cause wire sweep issues.


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