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  • Articles  (121)
  • DSC
  • Springer  (121)
  • American Association for the Advancement of Science
  • American Meteorological Society
  • 1995-1999  (100)
  • 1990-1994  (21)
  • 1999  (52)
  • 1996  (48)
  • 1992  (21)
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  • Articles  (121)
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  • Springer  (121)
  • American Association for the Advancement of Science
  • American Meteorological Society
  • Wiley-Blackwell  (20)
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  • 1995-1999  (100)
  • 1990-1994  (21)
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  • 1
    Electronic Resource
    Electronic Resource
    Study on thermal transitions of toluene diisocyanate-based polyurethane elastomers with poly (tetramethylene oxide) as the soft segment by TSC/RMA, DSC and DMA thermal analyzers (1999)
    Springer
    Journal of polymer research 6 (1999), S. 67-78 
    Details
    ISSN: 1572-8935
    Keywords: TDI-based polyurethane elastomers ; Tg ; Tglobal transition ; DSC ; TSC/RMA ; DMA
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Thermal transitions of TDI-based polyurethane elastomers with PTMO as the soft segment were characterized by the depolarization technique in TSC and by using with the thermal windowing technique on selected specimens in the RMA measurements. Results indicate that the broadened thermal transition in the glass transition region as observed in the DSC thermogram is related to the combined Tg transition and the Tglobal transition in the TSC spectrum. This Tglobal transition is associated with the macromolecular property as detected by tan δ in DMA measurement. The increase in the Tg with a high NCO content may be explained by the structural modification found on the urethanic chain with the additional linkage of the hard segment that affects the cooperative motion of the molecular chain. Data measured from DSC, TSC/RMA and DMA with simulated DEA and wide angle X-ray data are presented for the characterization of the polyurethanes. The RMA measurement leads to a compensation search on Tg transition and provides pertinent thermokinetic data that correlates the NCO content with changes in enthalpy and entropy on the relaxation behaviors in the Tg transition of polyurethane elastomers.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s10965-006-0073-4
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  • 2
    Electronic Resource
    Electronic Resource
    Cubic topology in surfactant and lipid mixtures (1996)
    Springer
    European biophysics journal 24 (1996), S. 293-299 
    Details
    ISSN: 1432-1017
    Keywords: Phase transition ; NMR ; DSC ; X-ray diffraction ; Bonnet Transformation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Physics
    Notes: Abstract Ternary systems of palmitoyl-oleoyl-phosphatidylcholine (POPC) and the non-ionic surfactant C12EO2 (di-ethylene-oxide-mono-dodecyl-ether) in water have been studied with optical microscopy, NMR, DSC and X-rays from ambient temperatures to 45 °C. Below 29 °C the system is in the lamellar liquid crystalline state. Between 30 and 32 °C it transforms into a cubic Ia3d structure which converts into the cubic Pn3m phase at 39 °C. The transitions are fully reversible. An epitaxial relationship between all three phases was found, which is an elegant and convenient way to rearrange molecules from lamellar bilayers to a network of curved surfaces. The la3d (Q230) to Pn3m (Q224) transition occurs without measurable enthalpy change. This, together with the metric relation of 1.60 between the cubic lattice constants is strong evidence for a Bonnet transformation, where the structural changes occur without change in curvature. The potential significance of the cubic phases as intermediate structures for biological processes, e. g. transport across a bilayer or fusion of membranes, are discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00180370
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  • 3
    Electronic Resource
    Electronic Resource
    Dantrolene inhibits halothane-induced membrane reorganization A study using 31P-NMR and differential scanning calorimetry (1992)
    Springer
    European biophysics journal 21 (1992), S. 13-19 
    Details
    ISSN: 1432-1017
    Keywords: Halothane ; Dantrolene ; DPPC ; 31P-NMR ; DSC ; Model membranes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Physics
    Notes: Abstract The action of the relaxing agent dantrolene on dipalmitoylphosphatidylcholine (DPPC) model membranes in the presence and absence of the general anesthetic halothane has been investigated by DSC and 31P-NMR. Dantrolene has a weak effect on both the thermodynamic and NMR parameters of the pure model membrane. When halothane is present in the system, the relaxing agent acts to counterbalance the strong anesthetic-induced membrane pertubation. This is reflected in DSC experiments by a change of the enthalpy variation (ΔH) and of the main gel-to-fluid phase transition temperature (Tc) towards the values of the pure lipid system. The amount of halothane-induced small tumbling vesicles, as detected by 31P-NMR by the superposition of an isotropic line on a lamellar-type powder spectrum, is considerably reduced upon dantrolene addition. This means that the relaxing agent “cures” the membrane de-structuring action promoted by halothane. Membranes first treated with dantrolene are also protected from the halothane perturbation. So, the relaxing agent is both “curative” and “preventative” against halothane. The optimum effect is obtained for 1 dantrolene molecule per ca 34 halothane molecules. The mechanisms of action were discussed in relation to membrane fluidity.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00195439
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  • 4
    Electronic Resource
    Electronic Resource
    The use of differential scanning calorimetry in chemical education (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 455-462 
    Details
    ISSN: 1572-8943
    Keywords: chemical education ; DSC ; polyethylene
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Es wird ein überblick über die Leistungsfähigkeit von DSC in der Chemieausbildung, sowohl in der Hochschul-als auch in der Postgraduate-Phase vermittelt. Es wird ein Weg aufgezeigt, wie die Einführung von DSC in der Chemieausbildung erleichtert werden kann. Die ausführliche Beschreibung eines Hochschulexperimentes, das Schmelzverhalten von ultrahochmolekularem Polyethylenfiber wird gegeben. Es wird gezeigt, da\ derartige Experimente geeignet sind, verschiedene chemische und physikalische Vorgänge leicht demonstrieren zu können.
    Notes: Abstract An overview is given of the potential of DSC in chemical education, both in the under-graduate and in the graduate phase. The way in which the introduction of DSC in chemical education is facilitated, is outlined. A comprehensive description is given of a graduate experiment, the melting behaviour of ultra-high molecular weight polyethylene fiber. It is shown that, using such an experiment, various chemical and physical processes in substances can be easily demonstrated.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01915510
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  • 5
    Electronic Resource
    Electronic Resource
    Hydration studies of modified OPC pastes by differential scanning calorimetry and thermogravimetry (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 495-504 
    Details
    ISSN: 1572-8943
    Keywords: cement hydration ; DSC ; TG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Bei der Untersuchung von Zement und des Einflusses von Additiven auf das Hydratationsverhalten von Zement finden thermoanalytische Methoden eine breite Anwendung. Der effektivste und meistbenutzte Beschleuniger für die Hydratation von Zement ist Calciumchlorid, aber die Ergebnisse hängen stark von der Dosiergeschwindigkeit ab. In vorliegender Studie wird mittels DSC-, TG- und Röntgendiffraktionsmethoden der Einflu\ der Dosierung von Calciumchlorid auf das Hydratationsverhalten von verschieden alten OPC-Zementbreiproben untersucht. Die Ergebnisse wurden in Bezug auf die relativen Mengen Calciumhydroxid und das gebildete Gesamtreaktionsprodukt gewertet. Bei Dosen von mehr als 1% Calciumchlorid konnte als Hydratationsprodukt Chloraluminat festgestellt werden. Sind Monochloraluminat und das Calciumaluminathydrat C4AH13 in geringen Mengen vorhanden, kann man zwischen den beiden mittels Röntgendiffraktion nicht unterscheiden. Thermoanalytische Methoden erwiesen sich als effektives Hilfsmittel bei der Charakterisierung der Produkte der Hydratation in Gegenwart von Chlorid.
    Notes: Abstract Thermal methods are used extensively in investigating cements and effects of additives on their hydration behaviour. Calcium chloride is the most effective and widely used accelerator for cement hydration, but the result is largely dependent on the rate at which it is added. In this study the influence of calcium chloride dosage on the hydration behaviour of OPC pastes aged for different periods has been investigated by means of differential scanning calorimetry (DSC), thermogravimetry (TG) and X-ray diffraction (XRD) methods. The results are discussed in relation to the relative amounts of calcium hydroxide and total reaction product formed. Chloroaluminate was a product of hydration in the samples dosed with greater than 1% calcium chloride. XRD was unable of itself to differentiate between monochloroaluminate and the calcium aluminate hydrate C4AH13 when present in small amounts. Thermal methods proved effective in characterising the products of hydration in the presence of chloride.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01915514
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  • 6
    Electronic Resource
    Electronic Resource
    Thermal decomposition of silver cyano complex and characterization its decomposition products by ETA, DSC, DTA and TG (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 789-796 
    Details
    ISSN: 1572-8943
    Keywords: ETA ; DSC ; DTA ; silver cyano complex ; TG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Mittels DTA und TG wurde [Phenyl2I][Ag(CN)2] untersucht in im festen Zustand bei Erhitzen in einer Argonatmosphäre bis 160°C als thermisch stabil befunden. Beim Erhitzen auf höhere Temperaturen erfolgt eine Zersetzungsvorgang, wobei flüchtige Produkte wie z.B. [Phenyl]I, [Phenyl]NC und (CN)2 entstehen. Bei Erhitzen auf 500°C erhält man metallisches Silber. Die festen Zwischen- und flüchtigen Produkte wurden mittels IR-Spektroskopie untersucht. Anhand der DTA- und ETA-Untersuchungen konnte festgestellt werden, daß bei Erhitzen und Abkühlen unterhalb 100°C reversible Einphasenumwandlungen stattfinden. Bei Erhitzen über 100°C schmilzt die Probe (SchmelzpunktT m=135°C). Die Schmelzenthalpie wurde mittels DSC ermittelt (H=−28 kJ/mol). Mit Hilfe von ETA wurde der Unordnungsgrad des Zersetzungsendproduktes geschätzt. Der Wert der Aktivierungsenergie für die Radondiffusion im Temperaturbereich 720°–500°C beträgt 32,6 kJ/mol.
    Notes: Abstract It was found by DTA and TG that [Phenyl2I][Ag(CN)2] in the solid state is chemically stable on heating in argon up to 160°C. During heating to higher temperatures it decomposes, forming volatile products such as [Phenyl]I, [Phenyl]NC and (CN)2 [1]. After heating the sample to 500°C metallic silver resulted. The volatile and intermediate solid products were analysed by IR-spectroscopy. It was found by means of DTA and ETA that an isophase reversible transition takes place when the sample is heated and cooled, not higher than 100°C. At heating higher than 100°C the sample melts (melting pointT m=135°C). The enthalpy melting was determined by means of DSC (ΔH=−28 kJ·mol−1). By means of ETA the disorder degree of the final decomposition product was estimated. The value of the activation energy of radon diffusion in the temperature range 720°–500°C equals 32.6 kJ·mol−1.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01979410
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  • 7
    Electronic Resource
    Electronic Resource
    Polymerization kinetics of acrylic bone cements by differential scanning calorimetry (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 35-49 
    Details
    ISSN: 1572-8943
    Keywords: bone cement ; DSC ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Bone cements are widely used for the fixation of metallic prostheses in orthopaedics and to form replacements for skull defects in neurosurgery. Acrylic bone cements are based on a mixture of methyl methacrylate (MMA) and a fine powder of polymethyl methacrylate (PMMA). The polymerization of the bone cement occurs in contact with the bone and the prosthesis which act as the boundaries of a bulk polymerization reactor. The kinetic behaviour of the bone cement plays a fundamental role for the final performance of the implant. In this paper, the isothermal and non-isothermal polymerization behaviour of a commercial bone cement is described. A simple phenomenological model, accounting for the autoacceleration ffect, for a diffusion controlled termination mechanism and for the reaction between inhibitor and initiator, is proposed. The reaction kinetics is analysed by DSC. DSC data are used for the determination of the rates of polymerization under isothermal and non-isothermal conditions. The experimental data are processed to calculate the parameters of the proposed phenomenological kinetic model. The analytical and numerical details related to the integration of the model are discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01982684
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  • 8
    Electronic Resource
    Electronic Resource
    Characterizing in situ starch gelatinization (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 181-194 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; gelatinization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Data obtained by dynamic mechanical analysis and DSC analysis of durum wheat dough are presented and discussed. Doughs with water contents ranging from 45 to 55% (w/w) were subjected to sinusoidal shearing by means of a dynamic mechanical spectrometer (Rheometrics, RFS2) equipped with parallel plate geometry, 0.1 strain amplitude and 1 rad/min frequency. The tests were carried on in temperature sweep mode at a heating rate of 2°C min−1. Wheat samples with water contents in the range between 7.5 and 37.5% and doughs with 37.5% moisture content were mixed for different times and subjected to DSC analysis (Perkin-Elmer, DSC-7) at a heating rate of 20°C min−1. Dynamic mechanical analysis revealed that the relationship between the dynamic properties of the dough and the temperature was modified as the water content of the dough increased and was quite different from that for gluten. A similar response was observed in the course of temperature scans made by means of DSC. These experimental findings suggest that the water-starch interaction in the presence of a protein matrix is affected by the availability of water and that the protein system is a competitor with respect to starch.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01982698
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  • 9
    Electronic Resource
    Electronic Resource
    Erfahrungen mit vier Softwarepaketen für Kinetische Auswertungen in der Thermischen Analyse (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 543-557 
    Details
    ISSN: 1572-8943
    Keywords: compensation effect ; DSC ; kinetics ; TG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Four computer programs as well as one demo-version for non-linear evaluation of kinetic data in thermal analysis and calorimetry, were presented. The multi-task program TA-kin meets all mathematical requirements for solving the numerical assignments. It is shown that the so-called compensation effect is due to the mathematical structure of the Arrhenius equation. Several applications of TA-kin to a lot of DSC- and TG-measurements and isoperibolic batch experiments as well as adiabatic semi batch experiments realized by precision calorimetry have been discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01983996
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  • 10
    Electronic Resource
    Electronic Resource
    Co-curing studies of ethynyl terminated oligoimide and (methyl) nadicimide resins (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 685-695 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; polymers ; resins ; TG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The paper describes the co-curing studies of ethynyl and ethenyl end-capped imide resins. The effect of composition and chemical structure of ethenyl end-capped resins (nadicimides) on thermal behavior of ethynyl end-capped resins was evaluated using DSC and thermogravimetric analysis. An increase in char yield was observed on co-curing of few resin formulations. A mechanism has been proposed to account for this observation.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01981804
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  • 11
    Electronic Resource
    Electronic Resource
    DSC and X-ray study of structure and phase transitions of low molecular compounds incorporated into crazes (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 1311-1322 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; low molecolar compounds ; phase transitions ; polymers ; X-ray
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Mittels DSC- uns SAXS-Techniken wurden die Orientierung, Phasenzusammensetzung und Phasenumwandlungen einer Reihe von langkettigen niedermolekularen Verbindungen (LMC) wie z.B. Heneikosan, Zetylalkohol und normalen Fettsäuren untersucht, die in porösen Strukturen (Haarrissen) von in flüssigem Medium ausgerichteten polymeren Matrizen eingebracht wurden. Es konnten verschiedene LMC-Kristallit-TVpen in Haarrissen von polymeren Matrizen beobachtet werden. Es wurde gezeigt, daß der LMC-Phasenzustand in Haarrissen durch eine höhere Stabilität der Hochtemperatur-Polymermodifikationen charakterisiert ist. Die LMC Schmelztemperatur in Haarrissen nimmt im allgemeinen ab, genauso wie die Schmelzenthalpie (Wärme) und die Entropie. Der Grund für die beobachteten Veränderungen der LMC-Eigenschaften liegt in der großen Dispersität (40–100 nm) der LMC-Partikel in den Haarrissen, woraus sich ein sichtbarer Anstieg der Polymer/LMC Grenzflächeneinwirkung auf die grundlegenden thermodynamischen Parameter des untersuchten Systemes ergibt.
    Notes: Abstract Orientation, phase composition and phase transitions of a series of long chain low molecular weight compounds (LMC), such as heneicosane, cetyl alcohol, normal fatty acids, introduced into porous structure (crazes) of polymeric matrices oriented in liquid medium have been studied by means of DSC and SAXS techniques. Different types of LMC crystallites orientation in crazes of polymeric matrices have been observed. LMC phase state in crazes is shown to be characterized by higher stability of high-temperature polymer midifications. LMC melting temperature in crazes usually decreases as well as melting enthalpy (heat) and entropy. The origin of LMC properties changes observed is high dispersity (40–100nm) of LMC particles in crazes resulting in a marked growth of polymer/LMC interface influence on principal thermodynamic parameters of the systems studied.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01979190
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  • 12
    Electronic Resource
    Electronic Resource
    Thermal transitions of cassava starch at intermediate water contents (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 1213-1228 
    Details
    ISSN: 1572-8943
    Keywords: cassava starch ; DSC ; starch thermal properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Order-disorder transitions were investigated in native cassava starch at intermediate moisture contents (35 to 60% wt. water), using Differential Scanning Calorimetry (DSC) and dynamic Wide Angle X-ray Diffractometry (WAXS) with a synchrotron radiation source. The gelatinization of granules occurs as a cooperative process, due to constraints induced in crystallites by the amorphous areas. Variations of water content (water volume fraction from 0.28 to 0.86) and heating rate (0.2–10
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01992824
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  • 13
    Electronic Resource
    Electronic Resource
    Isothermal microcalorimetric studies on starch retrogradation (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 1179-1200 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; isothermal microcalorimetry ; retrogradation ; starch
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract In the present study, isothermal microcalorimetry was introduced as a tool to investigate properties of starch retrogradation during the first 24 h. The study was made on purified amylose and amylopectin from corn, as well as on native starches, such as wheat, potato, maize, waxy maize and amylomaize, differing in their amylose content. The results were obtained in the form ofP-t traces (thermal powervs. time), and integration of these traces gave a net exothermic enthalpy of reaction, caused by the crystallization of amylose and amylopectin. TheP-t traces reflected the quantities of amylose and amylopectin in the starch studied. Depending on the amylose content and the botanical source of the starch, the rate of crystallization of amylose was high and predominated over that of amylopectin during the first 5–10 h. The contribution from amylose crystallization to the measured exothermic enthalpy was very substantial during this period. After ∼10 h, amylose crystallized at a lower constant rate. During the first 24 h, amylopectin crystallized at a low steady rate. The exothermic enthalpies obtained by the isothermal microcalorimetric investigations during the first 24 h of retrogradation were generally low in relation to the endothermic melting enthalpies observed by differential scanning calorimetry (DSC) measurements after 24 h of storage. The discrepancies in enthalpy values between the two methods are discussed in relation to phase separation and the endothermic effects owing to the decrease in polymer-water interactions when polymer-rich regions in the starch gel separate. Besides the exothermic enthalpies obtained, theP-t traces also made it possible to study the initial gelation properties of amylose from different botanical sources. The present study further demonstrated that isothermal microcalorimetry can provide a possible way to investigate the antistaling effect of certain polar lipids, such as sodium dodecylsulphate (SDS) and 1-monolauroyl-rac-glycerol (GML), when added to starches of different botanical origin. The net exothermic heat of reaction for starch retrogradation during the first 24 h was decreased when GML or SDS was added to the starch gels. The recordedP-t traces also showed how the effect of the added lipid influenced different periods during the first 24 h of starch retrogradation, and that the effect depended mainly on the amylose content, the botanical source of the starch, and the type of lipid used. When GML or SDS was added to waxy maize, the isothermal microcalorimetric studies clearly indicated some interaction between amylopectin and the polar lipids. These results concerning the action of anti-staling agents are further discussed in relation to the helical inclusion complexes formed between amylose-polar lipid and amylopectin-polar lipid.
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    URL: http://dx.doi.org/10.1007/BF01992822
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  • 14
    Electronic Resource
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    Influence of heating and cooling rates on the glass transition temperature and the fragility parameter of sorbitol and fructose as measured by DSC (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 1419-1436 
    Details
    ISSN: 1572-8943
    Keywords: cooling/heating rate ; DSC ; fragility parameter ; glass transition temperature ; sorbitol-fructose
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The glass transition temperatures of sorbitol and fructose were characterized by four points determined on DSC heating thermograms (onset, mid-point, peak and end-point), plus the limit fictive temperature. The variations of these temperature values, observed as functions of cooling and heating rates, were used to determine the fragility parameter, as defined by Angell [1] to characterize the temperature dependence of the dynamic behavior of glass-forming liquids in the temperature range above the glass transition. The apparent activation energy values, determined for the different temperatures studied, were similar for fructose and sorbitol. These values were compared to data obtained from other techniques, such as mechanical spectroscopy. The variations of the apparent activation values, observed in experiments involving cooling and heating at the same rate, slow cooling followed by rate-heating, or rate-cooling followed by fast heating, were explained by aging effects occurring during the heating step.
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    URL: http://dx.doi.org/10.1007/BF01992837
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  • 15
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    Investigation of the complex thermal behavior of fats (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 1545-1565 
    Details
    ISSN: 1572-8943
    Keywords: cocoa butter ; fat crystallization ; DSC ; fat polymorphism ; fat structure ; fats ; lard ; milk fat ; triacylglycerols ; X-ray diffraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The thermal behavior of three ural fats (displaying very different composition), cocoa butter (CB)2, lard, and a stearin obtained from anhydrous milk-fat (AMF) fractionation, were studied by both DSC and X-ray diffraction as a function of temperature (XRDT). To perform temperature explorations between −30
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01992845
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  • 16
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    Thermal behaviour of solid complexes of phenoxyalkanoic acids and divalent metals (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 5-14 
    Details
    ISSN: 1572-8943
    Keywords: cadmium phenoxyacetate ; complexes ; DSC ; mercury(II) phenoxyacetate ; TG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Solid cadmium and mercury(II) phenoxyacetates were prepared and investigated by DSC and TG techniques. The cadmium salt decomposed in two steps with the loss of 1.5 water molecules at first and the successive formation of CdCO3 as final product. Δdeh H * associated with the loss of one water molecule was compared with the corresponding values obtained for other phenoxyacetates previously studied and the obtained results were discussed. Anhydrous mercury(II) phenoxyacetate gave, on heating, HgCO3 which successively decomposed with the formation of gaseous products and a little amount of solid residue.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01979942
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  • 17
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    Activation energy of Se2Ge0.2Sb0.8 chalcogenide glass by differential scanning calorimetry (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 177-186 
    Details
    ISSN: 1572-8943
    Keywords: activation energy ; chalcogenide glass ; DSC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Results of differential scanning calorimetry (DSC) at different heating rates on Se2Ge0.2Sb0.8 chalcogenide glass are reported and discussed. As the heating rate (α) changed, also the glass transition temperature (T g) and onset temperature of crystallization (T c) changed. As the value of the transition activation energyE t changed, the crystallization fraction (χ), heat flow (Δq and the crystallization peak temperature (T p) also changed. The value of the effective activation energy of crystallizationE c was calculated by means of six different methods. The Se2Ge0.2Sb0.8 chalcogenide glass has two crystallization mechanisms, a one-dimensional and an other surface crystallization growth. The average value ofE t for Se2Ge0.2Sb0.8 is equal to 194.95±3.9 kJ·mol−1 and the average value ofE c is equal to 164±3.3 kJ·mol−1.
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    Thermal study of irradiated polyacetylene films (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 237-243 
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    ISSN: 1572-8943
    Keywords: DSC ; DTG ; polyacetylene films ; TMA
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Polyacetylene films irradiated byγ-rays up to 100 MRad were studied by means of TMA, DTG and DSC methods. It is shown that as the irradiation dose increases the concentration of topological branching knots into the polymer chains and theT g values decrease, the total mass loss and the enthalpy of the thermal isomerization reaction also decrease.
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    URL: http://dx.doi.org/10.1007/BF01979964
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    Nucleation and crystallization of polypropylene filled with BaSO4 (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 619-626 
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    ISSN: 1572-8943
    Keywords: crystallization ; DSC ; filled polypropylene ; nucleation ; structural modification
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The influence of high concentration of BaSO4 as nucleating agent on crystallization of fiber-forming polypropylene was studied by DSC. The work presents experimental and calculated values of melting and crystallization enthalpies of filled polypropylene and the influence on the formation of interface interactions between filler and polymers. These results show minimal interactions of components (BaSO4 and polypropylene) under experimental conditions.
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    URL: http://dx.doi.org/10.1007/BF02135042
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    Thermal analysis of macromolecules (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 643-679 
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    ISSN: 1572-8943
    Keywords: DDTA ; DSC ; macromolecules
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract This review traces the development of thermal analysis over the last 40 years as it was experienced and contributed to by the author. The article touches upon the beginning of calorimetry and thermal analysis of polymers, the development of differential scanning calorimetry (DSC), single run DSC and other special instrumentations, up to the recent addition of modulation to calorimetry. Many new words and phrases have been introduced to the field by the author and his students, leaving a trail of the varied interests one can have over 40 years. It began with “cold crystallization” and most recently the term “oriented, intermediate phase” was coined, creating in-between: “extended chain crystals,” the “irreversible thermodynamics of melting of polymer crystals,” “dynamic differential thermal analysis” (DDTA), “the rule of constant increase ofC p per mobile bead within a molecule at the glass transition temperature,” “superheating of polymer crystals,” “melting kinetics,” “crystallization during polymerization,” the “chain-folding principle, “molecular nucleation,” “rigid amorphous phase,” a “system of classifying molecules,” “macroconformations,” “amorphous defects,” “rules for the entropy of fusion based on molecular shape and flexibility,” “single-molecule single-crystals,” “a system of classifying phases and mesophases,” and “condis phase.”
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    URL: http://dx.doi.org/10.1007/BF01983596
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    Analysis of mesophase formation in side-chain liquid crystalline polycarbosilanes (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 795-808 
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    ISSN: 1572-8943
    Keywords: DSC ; kinetics ; liquid crystalline polymer ; optical transmittance ; polycarbosilane ; side-chain mesogen ; transition parameters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract This paper is concerned with an analysis of the thermodynamics and kinetics of mesophase formation by cooling from the isotropic state of side-chain liquid crystalline polycarbosilanes containing spacers in the range from 3 to 11 CH2-groups. The polymers are characterized by their thermotropic behaviour as far as temperature, enthalpy and entropy of the transitions are concerned. The kinetics was followed by optical and calorimetric methods. Longer spacer length leads to more perfect ordering in the mesophase, higher isotropization temperatures, and lower glass transition temperatures. The Avrami and Ozawa formalism to describe the transition kinetics to the mesophase from the isotropic state cannot be interpreted as the nucleation and growth mechanism known from crystallization.
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    URL: http://dx.doi.org/10.1007/BF01983603
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    A DSC study of the effects of sugars on thermal properties of rice starch gels before and after aging (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 1201-1212 
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    ISSN: 1572-8943
    Keywords: aging ; amylopectin ; DSC ; gels ; glass transition ; recrystallization ; retrogradation ; rice starch ; sugars
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Thermal characterization of gelatinized binary rice starch-water and ternary starch-sugar-water gels before and after aging was carried out using differential scanning calorimetry. The glass transition temperature of the maximally freeze-concentrated solution (T′g) in both fresh and aged gels was observed to decrease progressively with increasing sugar concentration. Aging of the gels generally shiftedT′g to higher temperatures, but had little or no effect on the ice melting peak temperature (T m). The presence of various sugars could either accelerate or retard starch (amylopectin) recrystallization, depending on the type and concentration of sugar, as well as on starch/water ratio. A hypothesis based on the dual antiplasticizing-plasticizing effects of sugars was postulated to explain the observed effects. Of the sugars studied, xylose and fructose appeared to display exceptional retardative and accelerative effects, respectively, on retrogradation.
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    URL: http://dx.doi.org/10.1007/BF01992823
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    Effect of hydrothermal treatment on the gelatinisation properties of potato starch as measured by differential scanning calorimetry (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 1229-1246 
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    ISSN: 1572-8943
    Keywords: DSC ; gelatinisation ; potato starch
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Gelatinisation temperatures as a function of moisture content were determined for potato starch. The native starch was then hydrothermally treated at a temperature 3% (Kelvin degrees) below the gelatinisation peak temperature and at moisture levels varying from 20 to 67% (by weight). Gelatinisation temperatures, temperature ranges and enthalpy values were affected for all treated samples. However, two sample populations could be distinguished: those samples treated under ‘limited’ moisture conditions and other samples treated in the presence of ‘extragranular’ moisture. A two-step hydrothermal treatment further increased the gelatinisation temperature, but the effect of the second step was small in comparison to that of the first.
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    URL: http://dx.doi.org/10.1007/BF01992825
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    DSC analysis of starch thermal properties related to functionality in low-moisture baked goods (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 1299-1314 
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    ISSN: 1572-8943
    Keywords: baked goods ; cookies ; crackers ; DSC ; pretzels ; starch
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract We describe an application of DSC as an analytical ‘fingerprinting’ method that has been used to characterize the thermal properties of wheat starch in low-moisture, wheat-flour-based baked products, including cookies, crackers, and pretzels. This use of DSC has enabled us to relate starch thermal properties, on the one hand, to starch structure, and on the other hand, to starch functionality, in terms of baking performance and finished-product quality.
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    URL: http://dx.doi.org/10.1007/BF01992829
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    Structure and properties of bread dough and crumb (1996)
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    Journal of thermal analysis and calorimetry 47 (1996), S. 1339-1360 
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    ISSN: 1572-8943
    Keywords: bread crumb ; bread dough ; DSC ; hydrocolloid ; mechanical properties ; pentosans ; protein
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The effects of hydrocolloids (guar and locust bean gums), soluble pentosans, and whey proteins on staling of bread crumb were investigated by means of DSC, rheometry, and image analyis. One current hypothesis, that these ingredients would behave as “water binders” and, at least the former two, as anti-staling agents, was indeed confirmed, although this action might be indirect. All the samples considered showed an exothermic DSC peak preceding the endotherm of the amylopectin fusion. According to a previous work, this signal was attributed to a water-dependent cross-linking process that would involve next-neighbouring polymer chains. To check the effect produced by molecular modifications that were expected to increase the water uptake of these ingredients, doughs containing added succinylated pentosans and whey proteins, and a polycarboxylate polymer, PEMULEN TR-1, were examined. These modifications enhanced starch retrogradation and yielded a firmer crumb. It was tentatively concluded that some direct interaction between these modified molecules and the crumb polymers might have taken place. In line with the food polymer science approach, the use of Time-Temperature-Transformation (TTT) diagrams is also discussed.
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    URL: http://dx.doi.org/10.1007/BF01992832
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    Effects of medium and chemical modification on thermal characteristics of Β-lactoglobulin (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 1513-1525 
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    ISSN: 1572-8943
    Keywords: Β-lactoglobulin ; DSC ; protein modification ; thermal properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The thermal properties of Β-lactoglobulin (Β-LG) were studied by differential scanning calorimetry (DSC) under different medium conditions.pH, neutral salts, protein perturbants, and polyols all affected the DSC characteristics of Β-LG. Acylation with fatty acids also changed the thermal properties, particularly peak width at half-height. The results suggest that the structural stability of Β-LG is controlled by non-covalent forces, particularly electrostatic and hydrophobic interactions. Disulfide bonds did not contribute to the thermal response of Β-LG. Fatty N-acyl-amino acids caused marked increases in thermal stability and decreases in denaturation enthalpy, and additional peaks were observed in the presence of some palmitoyl derivatives.
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    Thermal Analysis Studies on Isopropylnitrate (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 9-19 
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    ISSN: 1572-8943
    Keywords: ARC ; DSC ; HFC ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Isopropylnitrate (IPN) is described as a detonable material used in propellants and explosives. While there is considerable information available on its sensitivity and compatibility with other materials, very little is known about its thermochemical properties. This paper will describe the results obtained from some DSC, heat flux calorimetry (HFC) and accelerating rate calorimetry (ARC) measurements. The ASTM DSC method using a hermetic aluminum pan having a lid with a laser-produced pin hole was used to determine the vapour pressure of IPN1. Results calculated from an Antoine equation are in substantial agreement with those determined from DSC measurements. From the latter measurements, the enthalpy of vaporization was determined to be 35.32±0.62 kJ mol−1. Attempts to determine vapour pressures above about 0.8 MPa resulted in significant decomposition of IPNg. The enthalpy change for decomposition in sealed glass systems was found to be -3.43±0.09 kJ g−1 and -3.85±0.03 kJ g−1, respectively from DSC and HFC measurements on IPN1 samples loaded in air. Slightly larger exotherms were observed for the HFC results in air than those in inert gas, suggesting some oxidation occurs. In contrast, no significant difference in the observed onset temperature of about 150°C was observed for both the HFC and ARC results. From DSC measurements, an Arrhenius activation energy for decomposition of 126±4 kJ mol−1 was found. These measurements were also conducted in sealed glass systems and decomposition appeared to proceed primarily from the liquid phase.
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    Apparent Activation Energies of the Non-isothermal Degradation of Eva Copolymer (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 67-76 
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    ISSN: 1572-8943
    Keywords: activation energy ; DSC ; ethylene-vinyl acetate copolymer ; TG ; TG/IR ; thermal degradation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract When ethylene-vinyl acetate copolymer, EVA, is heated, a two-stage thermal degradation occurs following its melting. The vinyl acetate content of the copolymer was determined to be 43.8% by using TA 2950 and TA 2050 thermogravimetric instruments. TG/FTIR was used to detect the evolved gas. Acetic acid and trans-1-R-4-R'-cyclohexane were the main products evolved from EVA in the first and second stage, respectively. The apparent activation energies were determined for both stages by differential methods.
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    URL: http://dx.doi.org/10.1023/A:1010175904064
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    Crystallization Kinetics of Polypropylene-polyethylene-based Copolymers (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 57-65 
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    ISSN: 1572-8943
    Keywords: artificial ageing ; DSC ; dynamic crystallization ; isoconversional method
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A crystallization kinetics analysis of several polypropylene-polyethylene (PP-PE), PP-rich copolymers was made by means of differential scanning calorimetry. The crystallization was studied via calorimetric measurements at different cooling rates. Several additives were added to the base material. Some test samples were subjected to artificial ageing processes. A modified isoconversional method was used to describe the crystallization process under non-isothermal conditions. The value of the Avrami parameter was determined for primary and secondary crystallization.
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    URL: http://dx.doi.org/10.1023/A:1010123819994
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    Kinetic Analysis of Thermogravimetric Data XXXII. DSC Study of Some [Co(Diox·H)2(amine)2]X and H[Co(Diox·H)2(N3)2] Type Complexes with Alicyclic α-dioximes (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 311-320 
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    ISSN: 1572-8943
    Keywords: dioximine complexes of Co ; DSC ; kinetic compensation effect ; kinetic parameters of thermal decomposition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract 14 mixed Co(III) dioximine chelates of the types [Co(Diox·H)2(amine)2]X (X = Br, I, NO3, ClO4) and H[Co(Diox·H)2(N3)2], respectively (Diox·H2-1,2-cyclohexane dione dioxime (nyoxime), 1,2-cycloheptane dione dioxime (heptoxime) 1,2-cyclooctane dione dioxime (octoxime) were obtained and their thermal decompositions were studied in an argon atmosphere. After the dehydration of the crystallohydrates, both types of complexes exhibit 3 decomposition stages. For the [Co(Diox·H)2(amine)2]X type complexes (X = Br, I) the first endothermal stage is the substitution of an amine molecule for the external sphere anion and this process is followed by two exothermal decomposition stages. With H[Co(Diox·H)2(N3)2] type complexes the first and third processes are relatively slow, but the second process is very fast, corresponding to a vertical portion of the TG curves. From the TG curves kinetic parameters were derived for 11 processes and the validity of a non-linear compensation law was observed.
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    Calorimetric Investigations of Some Phases in the System Sodium Fluoride - Aluminium Fluoride (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 51-57 
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    ISSN: 1572-8943
    Keywords: DSC ; enthalpies ; NaAlF4 ; Na5Al3F14
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Beside the two well-known minerals cryolite, Na3AlF6, and chiolite, Na5Al3F14, the binary system NaF-AlF3 also contains a third compound, NaAlF4, sodium tetrafluoroaluminate. Solid NaAlF4 has been prepared from its vapour under controlled conditions. The stability of NaAlF4 has been investigated by differential scanning calorimetry. It is shown that the disproportionation of the compound: 5NaAlF4(s)=Na5Al3F14(s)+2AlF3(s) takes place at considerable rate between 700 and 900 K. The enthalpy of this reaction is calculated and found to be -66.9 kJ. Enthalpies of the two solid state transitions α-Na3AlF6 → β-Na3AlF6 and α-AlF3 → β-AlF3 have also been measured and new values are reported. The enthalpy of formation of chiolite, Na5Al3F14, at 900 K has been recalculated from enthalpy increment data obtained by drop calorimetry. A value of ΔH900 o = -7513.6±12.0 kJ mol-1 has been obtained. This value is in disagreement with the recommended value given in JANAF Thermochemical Tables given at 900 K ΔHf o = -7559.2 kJ mol-1.
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    The Fe-Ni Distribution Between Pentlandite and Monosulfide Solid Solution Equalized at Low Temperature (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 925-929 
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    ISSN: 1572-8943
    Keywords: DSC ; equilibrium ; Fe-Ni distribution ; monosulfide solid solution ; pentlandite
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Two mixtures of pentlandite and the monosulfide solid solution (mss) have been synthesized. The bulk compositions of the samples are Fe6Ni3S8 and Fe3Ni6S8. Differential scanning calorimetry detected exothermic process in the samples under heating. The process takes place in temperature range between phase transition in the mss (near 400 K) and 690 K and is governed by diffusion. X-ray powder diffraction has showed that equilibrium Fe-Ni distribution between pentlandite and the mss is achieved after short-time heating up to 670 K.
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    Cure Kinetics of Amine Cured Tetrafunctional Epoxy Blends with Poly(Styrene-Co-Acrylonitrile) (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 1033-1040 
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    ISSN: 1572-8943
    Keywords: cure kinetics ; DSC ; epoxy resin ; SAN ; thermoplastic blends
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Cure kinetics using a differential scanning calorimetry (DSC) technique were analyzed for a thermoplastic modified tetraglycidyl-4,4′-diaminodiphenylmethane (TGDDM) epoxy resin cured with diaminodiphenylsulphone (DDS), an aromatic diamine. The neat resin and its blends with the poly(styrene-co-acrylonitrile) (SAN) of various compositions were studied by applying a phenomenological model proposed by Kamal. Kinetic parameters were determined by fitting experimental data. This model gives a good description of cure kinetics up to the onset of vitrification. Diffusion control was incorporated to describe the cure in the latter stages of cure. The results showed that the addition of SAN did not alter the nature of the reaction, but the reaction rates and final conversions decreased when SAN contents increase, due to reduction of mobility of the reacting species.
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    Thermal Analysis, Microcalorimetry and Combined Techniques for the Study of Pharmaceuticals (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 1285-1304 
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    ISSN: 1572-8943
    Keywords: amorphous state ; combined techniques ; drug design ; drug product development ; drug substance ; drug technology ; DSC ; excipients ; failure investigations ; hydrates ; MDSC ; microcalorimetry ; pharmaceuticals ; polymorphism ; polymers ; preformulation ; process optimization ; purity ; quality control ; solvates ; stability ; sub-ambient DSC ; TG ; temperature resolved X-ray diffraction ; water interactions ; thermal microscopy ; water sorption-desorption
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Modern thermal analysis, microcalorimetry and new emerging combined techniques which deliver calorimetric, microscopic and spectroscopic data offer a powerful analytical battery for the study of pharmaceuticals. These techniques are very useful in all steps of development of new drug products as well as methods for quality control in production. The characterization of raw materials enables to understand the relationships between polymorphs, solvates and hydrates and to choose the proper development of new drug products with very small amount of material in a very short time. Information on stability, purity is valuable for new entities as well as for marketed drug substances from different suppliers. Excipients which vary from single organic or inorganic entity to complexes matrixes or polymers need to be characterized and properly controlled. The thermodynamic phase-diagrams are the basis of the studies of drug-excipients interactions. They are very useful for the development of new delivery systems. A great number of new formulations need proper knowledge of the behaviour of the glass transition temperature of the components. Semi-liquid systems, interactions in aqueous media are also successfully studied by these techniques.
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    Thermal Analysis, Microcalorimetry and Combined Techniques for the Study of the Polymorphic Behaviour of a Purine Derivative (1999)
    Springer
    Journal of thermal analysis and calorimetry 57 (1999), S. 61-73 
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    ISSN: 1572-8943
    Keywords: amorphous ; combined techniques for polymorphism ; DSC ; MKS 492 ; polymorphism ; purine ; quantitative determination ofamorphous and polymorphs ; solvent mediated transitions ; temperature resolved X-ray diffraction ; TG ; thermodynamic relation between polymorphs ; xanthine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The polymorphic behaviour of the purine derivative MKS 492 was studied with investigations of suspensions of selected samples in different solvents and of samples obtained by crystallizations. The samples were analyzed by DSC, TG and X-ray diffraction. Six different crystalline modifications called A, B, B’, C, D and E and an amorphous form were identified. Four pure crystalline modifications, A, B, C and D have been manufactured and characterized by DSC, X-ray, IR, solubilities, densities, hygroscopicity and dissolution measurements. The four forms A, C, D and E are monotrop to the form B. The form B is enantiotrop to the form B’, which revealed the highest melting point of all known polymorphs. This form B’ is only stable at high temperature. Temperature resolved X-ray diffraction was very helpful for proper interpretation of the thermal events. The melting peaks of the forms A and C and the endothermic peak corresponding to the enantiotropic transition B into B’ occur in a narrow range of temperature. The form B which is the most stable one at room temperature has been chosen for further development. Quantitative methods to determine the content of the forms A, C and D in samples of form B or to determine the content of form A, B and D in form C have been developed by using X-ray diffraction. Limits of detection are 1 or 2%. For the quantitative determination of the amorphous fraction, X-ray diffraction and microcalorimetry are compared. For high amounts of the amorphous fraction, the X-ray diffraction method is preferred because it is faster. Microcalorimetry is very attractive for levels below 10% amorphous content. The lowest limit of detection is obtained by microcalorimetry, about 1%.
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    Comparison of Experimental Methods and Theoretical Calculations on Crystal Energies of ‘Isoenergetic’ Polymorphs of Cimetidine (1999)
    Springer
    Journal of thermal analysis and calorimetry 57 (1999), S. 7-22 
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    ISSN: 1572-8943
    Keywords: crystal modifications ; DSC ; Gibbs free energy function ; molecular modelling ; solution calorimetry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The thermodynamic energy relationship between two crystal modifications of cimetidine was investigated and compared with differences in their processing properties with respect to transformation from one modification to the other. The crystal energies of the two modifications A and D were found to be almost identical and therefore the polymorphs are regarded as virtually isoenergetic crystals. This statement is based on DSC measurements of the melting points and of the enthalpies of fusion for the two crystal forms, which enable the calculation of the Gibbs free energy functions. Furthermore, the statement is supported by measurements of the enthalpies of solution in two different solvents. Both DSC and solution experiments reveal a slightly higher stability of the D modification with respect to the A form. In addition, tribomechanical treatment also indicates modification D to be the more stable one, as well as the higher density of the D form. No transformation during DSC at low heating rate was found which could be used in a stability consideration. As the explicit crystal structures of the two modifications are resolved, it was possible to calculate crystal energies theoretically as well. The theoretical results showed a remarkable difference in the crystal energies at zero degree Kelvin. Furthermore, they were just contradicting experimental findings by stating A being more stable than D. Possible reasons for this discrepancy and the feasibility of today's calculation methods with respect to prediction of stability properties are discussed.
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    Polymorphism of Acrylic and Methacrylic Acid Esters Containing Long Fluorocarbon Chains and Their Polymerizability (1999)
    Springer
    Journal of thermal analysis and calorimetry 57 (1999), S. 631-642 
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    ISSN: 1572-8943
    Keywords: DSC ; fluorocarbon chain ; polymerizability ; polymorphic behaviors ; X-ray diffraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The molecular aggregation of acrylic and methacrylic acid esters containing long-fluorocarbon chains: 2-(perfluoroalkyl)ethyl acrylate (FFnEA) and 2-(perfluoroalkyl)ethyl methacrylate (FFnEMA) (F(CF2)nCH2CH2OCOC(X)=CH2, where X=H, CH3 and n=6, 8, 10) was investigated by differential scanning calorimetry (DSC) and temperature controlled X-ray powder diffraction measurement. These compounds exhibited some characteristic polymorphic behaviors depending on the length of fluorocarbon chain and the α-position methyl group. The solid-state polymerization by γ-ray irradiation was studied for these compounds in the various crystal forms. In the solid-state polymerization, highest polymerizability was observed in the crystal form that exists in the highest temperature region for each compound.
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    URL: http://dx.doi.org/10.1023/A:1010113420330
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    Study of Ethyl Cellulose—Benzoic Acid Interactions in Matrices for Controlled Drug Release by DSC (1999)
    Springer
    Journal of thermal analysis and calorimetry 58 (1999), S. 29-38 
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    ISSN: 1572-8943
    Keywords: benzoicacid ; controlled release ; DSC ; ethyl cellulose ; FTIR
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The physical state of benzoic acid (BA) and its interaction with ethyl cellulose (EC) were examined in ethyl cellulose—benzoic acid matrices by Differential Scanning Calorimetry (DSC). The glass transition temperature (Tg) of EC of various matrices having BA in solid solution form (upto 27.7%) was reduced. The BA in matrices containing more than 38.9% drug exhibited distinct melting endotherms due to crystalline form. The peak temperatures of these endotherms were lowered and they broadened as the concentration was lowered. The solubility of BA increased at its melting point as compared to ambient temperature. The melting enthalpy of BA, when plotted as a function of its concentration yielded a straight line with intercept of 330 mg g−1 of matrix. This is the solubility of BA in EC at its melting temperature. Fourier Transform Infra Red Spectroscopy (FTIR) investigations confirmed that hydrogen bonding occurred between EC and BA through hydroxyl groups.
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    Combination of DSC and X-ray Diffraction in the Study of the Phase Behaviour of Lipids: Mini-review (1999)
    Springer
    Journal of thermal analysis and calorimetry 58 (1999), S. 363-368 
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    ISSN: 1572-8943
    Keywords: DSC ; lipid ; phase behaviour ; synchrotron radiation ; X-ray diffraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The phase behaviour and phase stability of lipids are of importance in an understanding of the biological functions of cell membranes. Among a variety of physical techniques employed to study the phase behaviour and structural properties of polar lipids, differential scanning calorimetry and X-ray diffraction have proved to be successful and are the most frequently used methods. Applications involving a combination of the two techniques, particularly when synchrotron radiation is used as the light source of X-ray diffraction, are reviewed in this article.
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    Measurements of Heat of Zeolite Dehydration by Scanning Heating (1999)
    Springer
    Journal of thermal analysis and calorimetry 58 (1999), S. 653-662 
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    ISSN: 1572-8943
    Keywords: dehydration ; DSC ; TG ; water ; zeolites
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A procedure for measurement of the heat of zeolite dehydration by scanning heating has been designed. Simultaneous data on heat flow (DSC) and mass loss (TG) are required for evaluation. The heating rate depends on the experimental conditions (point-spread function, sample mass, crucible design, and calorimetric reproducibility). Dehydration measurements have three advantages as compared with the sorption procedure: i) one can investigate samples with irreversible dehydration; ii) no approximation model is needed for calculation of the partial molar heat of dehydration; and iii) the procedure is not labor-consuming. The procedure was tested on the natural zeolites heulandite, chabazite and mordenite. The results are close to those measured by the sorption procedure. The partial molar heat of dehydration was found to depend on the water content. It increases from 50 to 87 J mol−1 K−1 for heulandite, from 53 to 81 J mol−1 K−1 for chabazite, and from 51 to 71 J mol−1 K−1 for mordenite. The approximation of the heat of sorption by linear regression was found to be wrong. Detection of a ‘phase transitioN’ after this approximation has no meaning.
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    Transformation-Governed Heating Techniques in Thermal Analysis II. (1999)
    Springer
    Journal of thermal analysis and calorimetry 58 (1999), S. 725-739 
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    ISSN: 1572-8943
    Keywords: DDC ; DSC ; DTA ; transformation-governed TA
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The described instrumental method makes it possible that the quasi-static heating technique, well applicable to thermogravimetric measurements, (see Part I of this paper) can be used in the case of DTA and DSC examinations, too. Based on the new type of curves the characteristic transformation temperatures, the whole course of the transformation in dependence of sample temperature, the extent of the enthalpy change caused by the transformation or by its partial processes can accurately be determined. The essentially greater accuracy of the measurements — in comparison to the conventional ones — is due to the quasi-static heating technique which ensures that the transformations should take place under quasi-equilibrium conditions.
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    Thermische Analyse binärer Systeme Organischer Verbindungen, die induzierte smektische Phasen bilden (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 1607-1626 
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    ISSN: 1572-8943
    Keywords: binary systems of cholesteryl ; DSC ; esters ; induced smectic phases ; thermomicroscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Acht binäre Systeme einer homologen Reihe von Cholesterylestern (Cholesterylpropionat bis Cholesteryldecanoat) mit trans-4-Propylcyclohexyl-4-(trans-4-pentylcyclohexyl) benzoat (Licristal 1223, Merck, Darmstadt) wurden thermomikroskopisch und DSC-analytisch untersucht. In sechs Fällen wurden induzierte smektische A-Phasen mit Umwandlungspunktmaxima festgestellt. Die cholesterischen bzw. nematischen Phasen bilden kontinuierliche Reihen von cholesterischen Mischkristallen, während die festkristallinen Phasen bei allen Systemen einfache Eutektika aufweisen.
    Notes: Abstract Eight binary systems of a homologous series of cholesteryl esters (from cholesteryl propionate to cholesteryl decanoate) with trans-4-propylcyclohexyl-4-(trans-4-pentyl-cyclohexyl) benzoate (Licristal 1223, Merck, Darmstadt) were examined by thermomicroscopy and DSC analysis. In six cases induced smectic A phases with transition point maxima were observed. The cholesteric resp. nematic phases form continuous series of cholesteric mixed crystals, while the solid phases show simple eutectics.
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    Effects of Added Urea and Alkylureas on Gel to Liquid-Crystal Transitions in Doab Vesicles (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 29-35 
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    ISSN: 1572-8943
    Keywords: alkylureas ; DOAB vesicles ; DSC ; gel-liquid transitions ; urea
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The gel to liquid-crystal transition for vesicles in aqueous solution formed by dimethyldi-n-octadecylammonium bromide (DOAB) occurs at 44.7°C. Moreover, the shapes of the scans recorded by a sensitive DSC microcalorimeter are very similar when the vesicular solutions are prepared starting with solid DOAB and comparable amounts of either solid urea or solid alkylureas. Therefore, the DOAB vesicles in aqueous solution accommodate this class of solutes without marked changes in the melting temperature and the enthalpy of the transition. The contrast with effects of added surfactants and simple organic solutes such as THF and ethanol is particularly significant.
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    Thermal and Spectroscopic Study of Dehydration of Lithium Formate Monohydrate Single-crystals (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 807-816 
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    ISSN: 1572-8943
    Keywords: DSC ; hydrogen-bond ; IR ; lithium formate monohydrate ; Raman spectroscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Differential scanning calorimetry (DSC) and thermogravimetric analysis (TG) of lithium formate monohydrate (LiHCOO·H2O) were performed in the temperature range 300–700 K. The DSC/TG measurements show that the dehydration process to anhydrous lithium formate (LiHCOO) is complex and occurs in two stages. The data are correlated to the structure and to the arrangement of the molecules in the crystal, including the hydrogen-bonding. Infrared transmittance and Raman spectra of this crystal are reported and commented on.
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    Thermal Decomposition of Strontium and Barium Malonates (1999)
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    Journal of thermal analysis and calorimetry 55 (1999), S. 789-796 
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    ISSN: 1572-8943
    Keywords: alkaline earth malonates ; DSC ; DTA ; kinetic parameters ; TG ; thermal decomposition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The thermal decomposition of strontium and barium malonates has been studied isothermally and non-isothermally employing simultaneous TG-DTG-DTA, DSC, XRD and IR spectroscopic techniques. DSC of these malonates has been recorded both in oxygen and nitrogen atmospheres. The decomposition is a single step process and the end product formed is carbonate. The energy of activation and frequency factor values for the decomposition of strontium malonate are 547 kJ mol−1 and 1041 s−1 respectively. The activation energy and frequency factor values for isothermal dehydration of barium malonate sester-hydrate are 57–111 kJ mol−1 and 107–1012 s−1 respectively and the corresponding values for decomposition from DSC are 499.5 kJ mol−1 and 1044 s−1 respectively. The higher thermal stability of strontium malonate as compared to that of barium salt is ascribed to its being anhydrous so that decomposition proceeds without restructuring. Their thermal stabilities have also been compared with that of respective oxalate salts.
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    From Precursors to Thin Films - Thermoanalytical Techniques in the Thin Film Technology (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 7-15 
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    ISSN: 1572-8943
    Keywords: ALE ; CVD ; DSC ; DTA ; EGA ; EL display ; solar cell ; sol-gel ; spray pyrolysis ; super-conductor ; TG ; thin films
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Processing thin films for advanced applications, for instance in electronics and optoelectronics, involves several steps starting from precursor synthesis and ending up with the devices. Especially when optimizing the first steps of this chain of processes, thermoanalytical techniques play an important role. The review will focus on the main chemical deposition methods (CVD, ALE, spray pyrolysis, sol-gel) giving selected examples of problem-solving by thermal analysis. The techniques discussed are TG, DTA/DSC, EGA and their combinations. High-temperature X-ray diffraction (HTXRD) is also a powerful tool for in situ studies of thin films. The examples are taken from solar cell, superconductor and flat panel electroluminescent display technologies.
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    α-β Phase Re-Transformation Kinetics in Nickel Sulphide (1999)
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    Journal of thermal analysis and calorimetry 56 (1999), S. 429-435 
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    ISSN: 1572-8943
    Keywords: DSC ; nickel sulphide ; TG ; toughened glass ; X-ray diffraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Nickel sulphide (NiS) was characterised using X-ray diffraction, thermal gravimetric analysis (TG) and differential scanning calorimetry (DSC). The 'as received' Millerite, stoichiometric NiS, observed to be slightly nickel deficient, was found to readily decompose in a nitrogen atmosphere at elevated temperatures (450°C max.) to the sulphur deficient Godlevskite, Ni7S6. DSC and X-ray measurements demonstrated that the high temperature form of the Godlevskite was readily stabilised at room temperature. The kinetics of the α-β re-transformation in Godlevskite were then investigated using DSC and were observed to be first order.
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    Thermochemistry of the Decomposition of Some Cobalt Compounds (1999)
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    Journal of thermal analysis and calorimetry 56 (1999), S. 547-552 
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    ISSN: 1572-8943
    Keywords: cobalt oxysalts ; DSC ; enthalpy of decomposition ; enthalpy of dehydration ; thermal decomposition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Differential scanning calorimetry (DSC) was used to determine the molar enthalpies of dehydration and decomposition of CoC2O4·2H2O, Co(HCOO)2·2H2O and [Co(NH3)6]2(C2O4)3·4H2O. The first stage of dissociation of each compound is a single-step dehydration both in air and argon atmospheres. The next stages are decomposition processes influenced by experimental parameters. The enthalpies of dehydration and decomposition vary from compound to compound in each atmosphere. The obtained data have been related to the macromechanisms proposed for the thermal decomposition and the parallel-consecutive decomposition-oxidation processes.
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    URL: http://dx.doi.org/10.1023/A:1010156728374
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    Isothermal and Non-Isothermal Kinetics When Mechanistic Information Available (1999)
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    Journal of thermal analysis and calorimetry 56 (1999), S. 783-792 
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    ISSN: 1572-8943
    Keywords: complex process ; DSC ; isoconversional methods ; kinetics ; model-free kinetics ; peak maximum evolution methods ; simulations
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract In the case of a complex mechanism of two parallel independent reactions, peak maximum evolution methods and model-fitting methods give only a mean value of the kinetic parameters, while isoconversional methods are useful to describe the complexity of the mechanism. Isothermal and non-isothermal isoconversional methods can be used to elucidate the kinetics of the process. Nevertheless, isothermal isoconversional methods can be limited by restrictions on the temperature regions experimentally available because of duration times or detection limits.
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    Feasibility Study of Crude Oil Fields by Thermal Analysis Techniques (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 947-951 
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    ISSN: 1572-8943
    Keywords: combustion ; crude oil ; DSC ; TG/DTG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract This paper investigates the minimum oil content necessary for self-sustained combustion, which is introduced as a criterion for the selection of suitable reservoirs for in-situ combustion processes. Differential scanning calorimetry was used to determine the heat values of oil-limestone mixtures. The minimum temperature required for the total consumption of the fuel was obtained by thermogravimetry (TG/DTG). The minimum amount of oil necessary to sustain combustion was calculated from these two parameters and compared with the oil content of the reservoir. Reservoirs with an oil content greater than or equal to this minimum value were considered feasible. It was seen that the fields examined are generally not suitable for in-situ combustion processes.
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    URL: http://dx.doi.org/10.1023/A:1010155617412
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    Isothermal Crystallisation of PCL Studied by Temperature Modulated Dynamic Mechanical and TMDSC Analysis (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 1155-1161 
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    ISSN: 1572-8943
    Keywords: crystallisation ; DMA ; DSC ; PCL ; polymer ; temperature modulation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Temperature modulated dynamic mechanical analysis (TMDMA) was performed in the same way as temperature modulated DSC (TMDSC) measurements. As in TMDSC TMDMA allows the investigation of reversible and non-reversible phenomena during crystallisation of polymers. The advantage of TMDMA compared to TMDSC is the high sensitivity for small and slow changes in crystallinity, e.g. during re-crystallisation. The combination of TMDMA and TMDSC yields new information about local processes at the surface of polymer crystallites. It is shown that during and after isothermal crystallisation the surface of the individual crystallites is in equilibrium with the surrounding melt.
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    The Influence of Annealing and Heavy Ion Irradiation of Multiple Melting and Crystallization in PBT Films (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 1141-1146 
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    ISSN: 1572-8943
    Keywords: crystallization ; DSC ; heavy ion irradiation ; melting ; PBT films ; poly(butyleneterephthalate) films
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The influence of heavy ion-irradiation (Ar 5.5 MeV amu-1, 5·1011 ion cm-2) on the melting and crystallization of two PBT films subjected to different modes of thermal treatment was investigated. Differences were observed between the processes occurring in both initial films, due to differences in crystalline phase content. The course of melting and crystallization in heavy ion-irradiated films during first heating, cooling and second heating differs from that in the initial films. The density data and DSC results indicate a decreased crystalline phase content in the PBT films after irradiation.
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    Thermal Behaviour of Some Terpenoids (1999)
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    Journal of thermal analysis and calorimetry 56 (1999), S. 1353-1357 
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    ISSN: 1572-8943
    Keywords: DSC ; terpenoids ; TG ; thermal behaviour
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The terpenoids acetyl sitosterol, lupeol, acetyl diosgenin and stigmasterol were studied. Comparison of the thermogravimetric curves and the activation energies of the terpenoids suggested the following sequence of thermal stability: acetyl sitosterol 〈 acetyl diosgenin 〈 lupeol 〈 stigmasterol. The DSC curves allowed determination of the melting points and the degrees of purity. Comparison of the TG and DSC curves revealed the presence of phase transitions without mass loss that were attributed to rearrangements in the terpenoid molecules.
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    Lipid-similar Thermal Transition of Polyethylene Glycol Alkyl Ether Detergents (1999)
    Springer
    Journal of thermal analysis and calorimetry 57 (1999), S. 371-375 
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    ISSN: 1572-8943
    Keywords: C14E8 ; detergent ; DSC ; polyethylene glycol tetradecyl ether ; thermal transition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A narrow, reversible endothermic main transition is found in the aqueous micellar phase of octaethylene glycol tetradecyl ether (C14E8) by DSC, characterized by a transition temperature of 41°C and a ΔH value of 0.5 kcal mol−1, which is not observed by light scattering. This transition is assigned to a cooperative conformational rearrangement of the assembled amphiphilic detergent molecules and not to a micelle aggregation process. It is suggested that the detergent’s polar head group is primarily involved in this rearrangement.
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    On the Oximine Complexes of Transition Metals: Part 110: Spectroscopic and DSC study on some [Fe(Diox·H)2L2] and [Fe(Diox)3(BOR)2] type chelates and clathrochelates (1999)
    Springer
    Journal of thermal analysis and calorimetry 57 (1999), S. 433-445 
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    ISSN: 1572-8943
    Keywords: DSC ; iron(II)-oxime complexes ; kinetic parameters ; Mössbauer spectroscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A number of 15 [Fe(Diox#x00B7;H)2L2] type chelates and [Fe(Diox)3(BOR)2] clathrochelates (Diox#x00B7;H2 — dimethylglyoxime, glyoxime, propoxime, nyoxime, furyl-dioxime; L-pyridine, alkyl-pyridine derivatives, diethyl-phenyl-phosphine, diethyl-p-tolyl-phosphine) were obtained and characterized by means of far and middle FTIR and Mössbauer spectroscopic methods. Some structural problems were discussed on the basis of the optical data. The DSC measurements show the higher thermal stability of the clathrochelates without O—H⋯O intramolecular hydrogen bonds (with asymmetric octahedral structure), as compared to the [Fe(Diox#x00B7;H)2L2] trans, symmetric chelates containing O—H⋯O bonds. The kinetic parameters of the thermal decomposition of the complexes have been derived using the nomogram method.
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    Decoupled Molecular Dynamics of Glass-forming Liquids Confined in Nano-meter Pores (1999)
    Springer
    Journal of thermal analysis and calorimetry 57 (1999), S. 745-752 
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    ISSN: 1572-8943
    Keywords: confinement effects ; DSC ; dynamic light scattering ; finite-size effects ; glass transition ; o-terphenyl
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Calorimetry is the method first used by Jackson and McKenna to study the effect of finite-size on the molecular dynamics of glass-formers confined in nano-meter scale pores. It was found that the glass transition is shifted to lower temperature as pore size decreases. Since then, other spectroscopic techniques have corroborated this finding and given more information on the molecular dynamics. These results are used to compare with the predictions of several theories of glass transition, and in particular the coupling model of the author.
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    Identification of Polyethylene by Differential Scanning Calorimetry: Application to forensic science (1999)
    Springer
    Journal of thermal analysis and calorimetry 57 (1999), S. 847-851 
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    ISSN: 1572-8943
    Keywords: DSC ; linear low-density polyethylene(LLDPE) ; low density polyethylene (LDPE) ; polymer blend ; thermal properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A forensic sample consisting of melt-recrystallized polymers that was recovered from the scene of a fire in a factory was identified by differential scanning calorimetry. The factory commonly used two kinds of film sheets, A and B, made by different manufacturers. It was necessary to decide whether the forensic sample related to material A or B. The forensic sample and reference samples of materials A and B were subjected to infrared spectroscopy and pyrolysis gas chromatograph mass spectrometry measurements, which revealed their polyethylene nature. The thermal behaviour of the samples was examined by differential scanning calorimetry (DSC) and they were found to be blends of two kinds of polyethylenes, low-density polyethylene and linear low-density polyethylene. The samples could be identified and distinguished from each other via the DSC measurements.
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    Estimation of the Critical Temperature of Thermal Explosion for the Highly Nitrated Nitrocellulose Using Non-isothermal DSC (1999)
    Springer
    Journal of thermal analysis and calorimetry 58 (1999), S. 369-373 
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    ISSN: 1572-8943
    Keywords: critical temperature ; DSC ; HNNC ; non-isothermal
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Two methods for estimating the critical temperature (Tb) of thermal explosion for the highly nitrated nitrocellulose (HNNC) are derived from the Semenov's thermal explosion theory and two non-isothermal kinetic equations, dα/dt=Af(α)e−E/RT and dα/dt=Af(α)[1+E/(RT)(1–To/T)]e−E/RT, using reasonable hypotheses. We can easily obtain the values of the thermal decomposition activation energy (E), the onset temperature (Te) and the initial temperature (To) at which DSC curve deviates from the baseline of the non-isothermal DSC curve of HNNC, and then calculate the critical temperature (Tb) of thermal explosion by the two derived formulae. The results obtained with the two methods for HNNC are in agreement to each other.
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    Single run heat capacity measurements (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 2257-2272 
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    ISSN: 1572-8943
    Keywords: heat capacity ; data analysis ; differential scanning calorimeter ; DSC ; single run
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Es werden die Grundzüge für die Datenanalyse von Wärmekapazitätsmessungen durch Doppelproben- DSC mit Einfachdurchgängen beschrieben: 1. Korrektion des Wärmeflusses durch Subtraktion des Beitrages des Probenbehälters, einschließlich der Korrektion nicht angeglichener Behältermassen. 2. Korrektion des Wärme flusses und der Temperatur mit einer nichtlinearen Temperaturkalibrierung, Korrektion von Temperaturverzögerung und Aufheizgeschwindigkeit. 3. Berechnung der Zellen-konstanten für beide Zellenpositionen und Ermittlung des Asymmetriefaktors zwischen den Zellenpositionen A und B. 4. Kalibrierung der Wärmekapazität und Berechnung mit Anstiegs- und Asymmetriekorrektion. 5. Berechnung der Wärmekapazität für Mehrfachdurchgänge. 6. Kurvenanpassung für die Wärmekapazität.
    Notes: Abstract An outline for the data analysis of single-run heat capacity measurments by dual sample DSC is presented with the following features: 1. Heat flow correction by subtracting the contribution due to the sample pan, including correction for mismatched pan masses. 2. Heat flow and temperature correction with a nonlinear temperature calibration, temperature lag correction, and heating rate correction. 3. Calculation of the cell constants for both cell positions and evaluation of the asymmetry factor between cell positions A and B. 4. Heat capacity calibration and calculation with slope and asymmetry correction. 5. Calculation of heat capacity for multiple runs. 6. Data curve fitting for heat capacity.
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    Thermal and calorimetric studies of M(IO3)2·6H2O and M(IO3)2·6D2O forM 2+=Ca2+ and Sr2+ (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 2491-2499 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; DTA ; M(IO3)2· 6H2O ; M(IO3)2·6D2O
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Mittels DTA- und DSC-Methoden wurden Me(IO3)2·6H2O und Me(IO3)2·6D2O (mitMe 2+=Ca2+ und Sr2+) thermisch und kalorimetrisch untersucht. Es wird ein Überblick über das thermische Verhalten ordentlicher und deuterierter Hydrate gegeben, in dem auch die Unterschiede zwischen beiden diskutiert werden. Die Enthalpien der untersuchten Phasenumwandlungen wurden bestimmt. Aus den Daten für Hdeh wurde Hf von Ca(IO3)2·6H2O, Ca(IO3)2H2O(D2O) und Sr(IO3)2·6H2O(D2O) berechnet und Bemerkungen zum beobachteten Isotopeneffektes gemacht.
    Notes: Abstract Thermal and calorimetric studies were carried out on M(IO3)2·6H2O and M(IO3)2·6D2O forM 2+=Ca2+ and Sr2+, using DTA and DSC methods. The thermal behaviour of the ordinary and deuterated hydrates is outlined and the differences observed between them are discussed. The enthalpies of the phase transitions were determined. The ΔH f o for Ca(IO3)2·6H2O, Ca(IO3)2·6H2O(D2O) and Sr(IO3)2·6H2O(D2O) were calculated from the ΔH deh data and comments are made on the isotope effect observed.
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    URL: http://dx.doi.org/10.1007/BF01974627
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    (RS)-, (R)- and (S)-3-benzyl-3-ethyl 2-oxetanone polymerization with chiral and achiral initiators (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 303-311 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; polyester ; polymerization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Die Polymerisation von 3-benzyl-3-ethyl 2-oxetanon führt zu drei Polymer Typen: PolyRS (überschuss des Enantiomers,EE=0), PolyR oder PolyS (REE 〉 SEE) und Polyracemate. Alle Polymere sind kristallin und die thermischen Eigenschaften (T g, SchmelzeT M und δH M) hängen wesentlich vonEE des Polymers ab. Die Fortpflanzung der Polymerisation ist nicht stereospeeifisch. Die Verwendung von Aufheitzen Abkühl Zyklen führt zu einer reinen kristallinen Form, die bei der höchsten Temperatur schmilzt. Das Polyracemat verhält sich wie ein reines Polymer, das bei niedrigeren Temperatur schmilzt; es racemisiert im Laufe einer verlängerten Erhitzung im Schemlzfluss.
    Notes: Abstract The polymerization of 3-benzyl-3-ethyl 2-oxetanones leads to three types of polymers: polyRS (enantiomer excess,ee=0), polyR or polyS (Ree 〉See) and polyracemate. All these polymers are crystalline and the thermal properties (T g, meltingT M and δH M) depend mainly on theee of the polymer. The propagation of the polymerization is not stereospecific. The use of heating-cooling cycles leads to a pure crystalline form melting at the highest temperature. The polyracemate has the behaviour of a pure polymer which melts at a lower temperature, a prolonged heating in the melt induces a strong racemization.
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    The limit of detection in differential scanning calorimetry (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 277-287 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; limit of detection ; polymorphic transitions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Anhand von sehr kleinen Signalen von spontanen polymorphen übergängen bei CsCl, K2Cr2O7 und Na2SO4 wird ein Verfahren zur Bestimmung der Nachweisgrenze von DSC-Geräten beschrieben. Es wird gezeigt, wie derartige Signale gut aufgelöst in DSC-Diagrammen von Pulverproben erhalten werden können. Um sie vom Rauschen der Basislinie zu unterscheiden, sollten sie eine Höhe von mindestens dem Doppelten der Basislinienbreite aufweisen. Für das angewendete Gerät beträgt die entsprechende geringste Wärmemenge, d.h. die Nachweisgrenze 0.1 mJ.
    Notes: Abstract A procedure is described to determine the limit of detection of DSC instruments by using tiny signals from spontaneous polymorphic transitions of CsCl, K2Cr2O7 and Na2SO4. It is shown how such signals can be found well-resolved in DSC diagrams of powder samples. To distinguish them from the baseline noise they should exhibit a height at least twice that of the baseline width. For the instrument employed the corresponding smallest amount of heat, i.e., the limit of detection, was found to be 0.1 mJ.
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    Thermomechanical analysis (TMA) correlated to differential scanning calorimetry (DSC) for ageing study of some metallic glasses (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 409-420 
    Details
    ISSN: 1572-8943
    Keywords: metallic glasses ; DSC ; TMA
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Zur Charakterisierung des Alterns einiger metallischer Gläser wird in einer Vergleichsstudie der DSC-Methode und der thermomechanischen Analyse (TMA) die Spezifität letzterer hervorgehoben. Es wurden metallische Gläser untersucht, die entweder mittels chemischer Verfahren oder durch Schmelzverdüsen hergestellt wurden. Mittels DSC und TMA wurde festgestellt, da\ die Entspannung der metallischen Gläser stark von der Behandlungsweise abhängt, d.h. ob es sich um eine thermische oder mechanische Vorgeschichte handelt. Im Gegensatz dazu konnten bei der Kristallisation keine gro\en Unterschiede zwischen DSC und TMA gefunden werden. Anhand experimenteller Daten wurde versucht, das Verhalten derartiger Materialien unter den Betriebsbedingungen zu modellieren.
    Notes: Abstract To characterize the ageing of some metallic glasses, a correlated study of the differential scanning calorimetry method (DSC) and of the thermomechanical analysis (TMA) emphasizes the specificity of the latter. We analyzed metallic glasses which have been produced either by chemical methods or by melt spinning techniques. Using TMA and DSC, we have established that the relaxation of metallic glasses is strongly dependent on treatment applied: either thermal or mechanical history. Conversely, we do not observe large differences between DSC and TMA analysis for the crystallisation. From experimental data, we try to modelize the behaviour of this type of materials under operating conditions.
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    Interpolymer complexes of a new type (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 347-352 
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    ISSN: 1572-8943
    Keywords: DSC ; optical densities ; thermal stability ; three-component interpolymer complexes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A new type of three-component interpolymer complexes (3IPCM) formed by two similarly charged polyelectrolytes and an oppositely charged low molar mass compound was studied by DSC, NMR and X-ray methods. The low molar mass monobasic compounds in these complexes act as mediators. This type of complexes differs from earlier-obtained 3IPCM, which contained a dibasic low molar mass mediator. The present 3IPCM were obtained from two polymers (polyacrylic acid and sodium polyphosphate) and bases such as 4-vinylpyridine and 2-methyl-5-vinylpyridine.
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    Kinetics of curing reaction of a diglycidyl ether of bisphenol A/1,3-bisaminomethyl-cyclohexane (DGEBA/1,3-BAC) epoxy resin system (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 387-395 
    Details
    ISSN: 1572-8943
    Keywords: cure kinetics ; DSC ; epoxy resins ; gelation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract By employing differential scanning calorimetry (DSC) we have studied the kinetic of the cure reaction for a system containing a diglycidyl ether of bisphenol A (DGEBA) and 1,3-bisaminomethylcyclohexane (1,3-BAC) as a curing agent, using an isothermal approach over the temperature range of 60–110°C. We have determined the reached conversions at several cure temperatures and the reaction rates. The results showed that this cure reaction is autocatalytic. The experimental data were compared with the autocatalytic model proposed by Kamal, which includes two rate constants and two reaction orders. This model gives a good description of cure kinetics up to vitrification point. The activation energies for these rate constants were 44-57 kJ mol−1. From the gel time measurements the value obtained for the overall activation energy was 49.5 kJ mol−1.
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    Lifetime prediction of ABS polymers based on thermoanalytical data (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 465-470 
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    ISSN: 1572-8943
    Keywords: ABS polymer ; DSC ; lifetime estimation ; thermooxidation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The service life of ABS polymer, stabilized by 2-(3,5-di-tert-butyl-4-hydroxyanilino)-4,6-bis(octylthio)-1,3,5-triazine and containing 50% of a modifying rubber component, was estimated from oxidative induction times measured by DSC in isothermal mode in the temperature interval 140–170°C. The lifetime of ABS powder at the actual temperature of drying was predicted by linear extrapolation according to Arrhenius. However, the extrapolated value was much longer than the real lifetime determined from the long-term oven aging tests at 70 and 90°C, simulating the industrial drying process. The effect of changes in the apparent activation energy of oxidation due to antioxidant consumption during polymer aging is discussed.
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    URL: http://dx.doi.org/10.1007/BF02135023
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    Thermochemical investigation of guest-host interactions in Werner clathrates of type [Ni(4-Etpy)4(NCS)2]·nG (G=naphthalene derivatives) (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 539-548 
    Details
    ISSN: 1572-8943
    Keywords: complexes ; DSC ; guest-host interactions ; X-ray
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The stoichiometry of thermal decomposition and the thermochemistry were studied for [NiL4(NCS)2] (I) as a host complex, and for its clathrates of type [NiL4(NCS)2]·2G, where L=4-ethylpyridine and guest molecule G=1-methylnaphthalene in clathrate (II), 1-chloronaphthalene in (III) or 1-bromonaphthalene in (IV). For I, the loss of volatile components proceeds in three steps (−2L, −L, −L); the first steps for II–IV also involve the release of G (−2G, −2L). DSC and X-ray powder measurements indicated a phase transition in the host lattice, and allowed differentiation of the escape of G and L molecules. The enthalpy changes give the following sequence of thermodynamic stability for the studied chlathrates: I〉II〉III.
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    Thermal analysis of poly(2-methylpentamethylene terephthalamide) (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 753-771 
    Details
    ISSN: 1572-8943
    Keywords: crystal-crystal transitions ; crystal forms ; DMA ; DSC ; Nylon M5T ; X-ray
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Poly(2-methylpentamethylene terephthalamide) (Nylon M5T) is a new high temperature aromatic polyamide developed by Hoechst Celanese. In this paper thermal properties of Nylon M5T chips, as well as as-spun and drawn fibers were studied by DSC, DMA, hot stage microscopy and WAXS.T g of the fully amorphous Nylon M5T is 143°C when measured by DSC;T g increases with crystallinity to 151°C. The temperature dependence of the solid and melt specific heat capacities has also been determined. The heat capacity increase at the glass transition of the amorphous polymer is 103.9 J °C−1 mol−1.T g by DMA for the as-spun fiber is 155°C, for a drawn fiber is 180°C. Three secondary transitions were observed by DMA in addition to the glass transition. These correspond to a local mode relaxation of the methylene groups at −120°C, onset of rotation of the amide-groups at −65°C and the onset of the rotation of the phenylenegroups (at 63°C). The crystallinity of Nylon M5T strongly depends on the rate of cooling from the melt. The isothermal crystallization data are melt temperature dependent: two-dimensional crystallization takes place when the samples are crystallized from higher melt temperatures, and this phase changes into a spherulitic structure during cooling to room temperature. Spherulitic crystallization occurs when lower melt temperatures are used. This polymer has three crystal forms as indicated by DSC, DMA and WAXS data. The crystal to crystal transitions are clearly visible when amorphous samples are heated in the DSC, or the DMA curves of as-spun fibers are recorded. It is experimentally shown that a considerable melting of the lower temperature crystal forms takes place during the crystal to crystal transitions. The equilibrium melting point as measured by the Hoffman-Weeks method, has been determined to be 339°C.
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    On the determination of the melting point of semicrystalline polymer by DSC (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 871-878 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; melting point ; polyethylene ; Raman-active longitudinal acoustical mode ; semi-crystalline polymers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract This is a study for criteria to judge the melting point of semi-crystalline polymers from the DSC endotherm for polymer melting. Beyond standard indium DSC melting results an evaluation has been made on a series of polyethylenes for which crystal sizes were measured and predicted from Raman LAM analysis. The results confirm the conclusion of Prof. Wunderlich that the DSC content of melting is the proper basis of reporting melting points.
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    Modulated temperature DSC measurements relating to the cold crystallization process of poly(ethylene terephtalate) (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 893-903 
    Details
    ISSN: 1572-8943
    Keywords: cold crystallization ; DSC ; heat capacity ; modulated temperature DSC ; poly(ethylene terephtalate)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The modulated temperature differential scanning calorimetric method (MT-DSC) yields three temperature dependent signals, an underlying heat capacity curve from the underlying heat flow rate (corresponding to the conventional DSC signal), and a complex heat capacity curve with a real part (storage heat capacity) and an imaginary part (loss heat capacity). These curves have been measured in the cold crystallization region for poly(ethylene terephtalate) with a modified Perkin-Elmer DSC-7. The underlying curve shows the well known large exothermic crystallization peak. The storage heat capacity shows a step change which reproduces the change in heat capacity during crystallization. This curve may be used as baseline, to separate the crystallization heat flow rate from the underlying heat flow rate curve. The loss heat capacity curve exhibits a small exothermic peak at the temperature of the step change of the storage curve. It could be caused by changes of the molecular mobility during crystallization.
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    Thermogravimetric analysis for boiling points and vapour pressure (1996)
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    Journal of thermal analysis and calorimetry 46 (1996), S. 1251-1258 
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    ISSN: 1572-8943
    Keywords: boiling points ; DSC ; TGA ; vapour pressure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A TGA instrument has been adapted for rapid measurement of boiling points and vapour pressure at temperatures from ambient up to 400°C and pressures from ambient down to 20 mm Hg. Samples were contained in sealed holders having a laser-drilled aperture. Several organic liquids in the 100 to 300 gMW range showed good agreement with reference vapour pressure data. Sample mass, heating rate, and use of inert diluents were important variables affecting accuracy of vapour pressure measurements.
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    New reference materials for the calibration (temperature and energy) of differential thermal analysers and scanning calorimeters (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 855-863 
    Details
    ISSN: 1572-8943
    Keywords: calibration materials ; DSC ; DTA
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Als neue Referenzsubstanzen für Temperatur- und Energiekalibrierung von DTA- und DSC-Geräten wurden im Temperaturbereich 300–600 K einige organische Verbindungen, wie z.B. Phenanthren, Benzanilid, Anissäure, Triphenylen, 2-Chloranthrachinon, Hexachlorbenzol, Karbazol, 4-Jodbenzoesäure, Perylen und Anthrachinon untersucht.
    Notes: Abstract Several organic compounds like phenanthrene, benzanilide, anisic acid, triphenylene, 2-chloroanthraquinone, hexachlorobenzene, carbazole, 4-iodobenzoic acid, perylene, anthraquinone, as new reference materials for temperature and energy calibration of DTA and DSC apparatuses were studied in the range 300—600 K.
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    Reinforcement characterization of metal matrix composites by DSC technique (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 989-996 
    Details
    ISSN: 1572-8943
    Keywords: aerospace industry ; DSC ; metal matrix composites (MMC)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Metallmatrixverbundwerkstoffe (MMC) sind für die Raumfahrtindustrie von großem Interesse, insbesondere zum Bau thermisch-struktureller Komponenten ist es wichtig, Methoden zur Verfügung zu haben, die leicht und einfach zur Charakterisierung der mechanischen Festigkeit der Materialien benutzt werden können. Es wurde gezeigt, daß DSC es ermöglicht, die Kohäsionsenergie im Fiber/Matrix-Grenzflächengebiet eines mit SiC-Whiskern verstärkten Aluminiumverbundstoffes quantitativ zu bestimmen. Diese Kohäsionsenergie ist abgängig vom Verstärkungsgrad bezogen auf die Matrixfestigkeit und berücksichtigt sowohl die chemischen als auch mechanischen Eigenschaften der Kohäsion im Fiber/Matrix-Grenzflächengebiet. In jedem Falle bedarf diese Methode einer systematischen Kalibrierung anhand von Test der mechanischen Eigenschaften.
    Notes: Abstract The metal matrix composites (MMC) being of very high interest for the aerospace industry, particularly to build up thermal-structural components, it is important to have available methods which are easy and simple to conduct for characterization of the mechanical strength of the material. This study shows that the differential scanning calorimetry (DSC) may enable us to quantify the energy of cohesion in the fiber/matrix interface area of an aluminium composite reinforced by SiC whiskers. The energy of cohesion is dependent on the state of reinforcement compared to the matrix strength and take into account both chemical and mechanical characteristics of the cohesion in the fiber/matrix interface area. However, this method would require a systematic calibration based on tests of mechanical characteristics.
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    DSC investigation of oxygen subsystem in Ba-Y-Cu-O superconductors (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 1123-1137 
    Details
    ISSN: 1572-8943
    Keywords: Ba-Y-Cu-O superconductor ; DSC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Für eine Reihe von Verbindungen der allgemeinen Formel Ba2YCu3Oy und einem Sauerstoffgehalt vony=6.0....6.9 wurden mittels verschiedener Wärmebehandlungen bei 800–1200 K, gefolgt durch Abschrecken oder beim chemischen Sauerstoffentzug durch Einbringen der Probe in Diwasserstoff bei 470–490 K DSC-Untersuchungen durchgeführt. Wird die Probe in Stickstoff erhitzt, so behält sie ihren Sauerstoffgehalt bei und zeigt bei 450–850 K einen exothermen Effekt. Es wurde gezeigt, daß die Funktion ΔH(y) bei etwa y=6.5 ein Maximum erreicht. Kinetische Messungen zeigen, daß für diesen Effekt die diffusive Beweglichkeit der Sauerstoffatome im Gitter verantwortlich ist.
    Notes: Abstract DSC investigations have been performed for a series of compounds Ba2YCu3Oy with the oxygen content varying in the rangey=6.0...6.9 by means of various heat treatments at 800–1200 K followed by quenching, or through the chemical extraction of oxygen by placing the sample in dihydrogen at 470–490 K. The sample preserving a constant oxygen content during heating in nitrogen exhibited exothermal effects between 450 and 850 K. It has been shown that the ΔH vs. y function reaches maximum aty ≈ 6.5. Kinetic measurements have shown that the diffusive mobility of oxygen atoms in the lattice is responsible for these effects, viz. the Arrhenius and cooperative processes of reorganization in the non-equilibrium oxygen subsystem of the bulk.
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    DSC study of melting and glass transition in gelatins (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 1189-1201 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; gelatins ; glass transition temperature
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Mittels DSC wurde im Bereich −50° bis +130°C die Temperaturabhängigkeit der Wärmekapazität für verschiedene Arten von Gelantine mit einem Wassergehalt von 2 bis 95% untersucht. Es wurde gezeigt, daß in allen untersuchten Fällen metastabile kollagenähnliche Strukturen in Gelen oder kristallinen Gelantinen gebildet werden, deren thermodynamische Parameter von den Bildungsbedingungen abhängen. Es wurden die charakteristischen Eigenschaften der Glasumwandlungen in amorphen Gelantinen und kristallinen Gelantinen mit unterschiedlichen Schmelzwärmen und einem unterschiedlichen Gehalt an geordneter Phase bestimmt. Spezielle Aufmerksamkeit wurde den strukturellen Eigenschaften von freiem und gebundenem Wasser gewidmet. Es wurde gezeigt, daß die Ab-hängigkeit der GlasumwandlungstemperaturT g vom Gehalt an gebundenem Wasser generell für viele denaturierte Biopolymere anwendbar ist. Im Unterschied zu gebundenem Wasser fungiert freies Wasser in Gelatinen nicht als ein Weichmacher, bildet aber eine starre Matrix, die die Glasumwandlung verhindert.
    Notes: Abstract In the range from −50° to +130°C, the temperature dependence of the heat capacity for different kinds of gelatins with water contents of from 2 to 95% was studied by the DSC method. It was shown that, in all studied cases, metastable collagen-like structures are formed in gels or crystalline gelatins, with thermodynamic parameters depending on the formation conditions. The characteristic properties of the glass transitions in amorphous gelatins and crystalline gelatins with different melting heats and different contents of the ordered phase were established. Special attention is paid to the structural properties of free and bound water. The dependence of the glass transition temperatureT g on the bound water content was shown to be of general applicability for many denatured biopolymers. Free water in gelatins, in distinction to the bound water, does not act as a plasticizer, but forms a rigid matrix inhibiting the glass transition.
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    Differential scanning calorimetry of irradiated polymers (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 1215-1231 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; irradiated polymers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung DSC wurde zur Untersuchung des Einflusses von Bestrahlung mit schnellen Elektronen auf die molekulare Mobilität und den Schmelzvorgang von semikristallinen Polymeren und Kopolymeren von Ethylen und von Fluorkopolymer angewendet. Die Temperaturabhängigkeit der Wärmekapazität im Bereich 100 bis 500 K zeigte die besonderen Wesenszüge des Bestrahlungseffektes auf vier Relaxationsumwandlungen in Verbindung mit dem Auftreten von Segmentbewegungen in verschiedenen Molekülteilen der gestörten Regionen des Polymers. Man fand, daß die Bestrahlungsbeständigkeit der Kristallite eindeutig von der Vorgeschichte des untersuchten Objektes abhängt. Die Ergebnisse wurden ausgehend von der bestimmenden Rolle von Molekülbeweglichkeit und freiem Volumen für das Überwiegen der Strahlungsvernetzung der Moleküle gedeutet. Es wurden Zusammenhänge zwischen den Wesenszügen der thermischen Umwandlungen und den mechanischen Eigenschaften der bestrahlten Polymere festgestellt.
    Notes: Abstract DSC was used to study the influence of fast electron irradiation on the molecular mobility and melting of semicrystalline polymers and copolymers of ethylene and of fluorocopolymer. The heat capacity-temperature dependences obtained in the range from 100 K to 500 K revealed the specific features of the irradiation effect on four relaxational transitions associated with the appearance of segmental motion in different molecular elements of the disordered regions in the polymer. The pronounced dependence of the radiation stability of crystallites on the thermal prehistory of the object under study was found. The results were interpreted on the basis of the decisive role of the molecular mobility and free volume for the predominance of the radiation cross-linking of the molecules. Correlations were established between the characteristics of the thermal transitions and the mechanical properties of the irradiated polymers.
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    Thermodynamic transition properties of highly ordered smectic phases (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 957-973 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; Gibbs energy ; liquid crystalline polyethers
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A series of polyethers have been synthesized from 1-(4-hydroxy-4′-biphenyl)-2-(4-hydroxyphenyl)propane and α, Ω-dibromoalkanes having different numbers of methylene units [TPPs]. Both odd- and even-numbered TPPs [TPP(n=odd)s and TPP(n=even)s) exhibit multiple transitions during cooling and heating and they show little supercooling dependence, indicating close-to-equilibrium nature of these transitions. Combining the structural characterization obtainedvia wide angle X-ray diffraction powder and fiber patterns at different temperatures and the morphological observations from microscopy techniques, not only the nematic liquid crystalline phase but also highly ordered smecticF, smectic crystalG andH phases have been identified. The phase diagrams for both TPP(n=odd)s and TPP(n=even)s have been constructed [1–3]. Thermodynamic properties (enthalpy and entropy changes) during these transitions are studied based on differential scanning calorimetry experiments. The contributions of the mesogenic groups and methylene units to each ordering process can be separated and they indicate the characteristics of these processes thereby providing estimations of the transition types.
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    Study of thermal decomposition of ammonium cerium sulphate (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 1345-1355 
    Details
    ISSN: 1572-8943
    Keywords: ammonium cerium sulphate ; DSC ; kinetic parameters ; TG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Mittels DSC und TG wurde die thermische Zersetzung von Ammoniumzersulfat untersucht. Die Ergebnisse zeigen in Sauerstoff einen fünfstufigen Zersetzungsprozeß im Temperaturbereich 364–1116 K. Ausgehend von den thermoanalytischen Angaben, der Elementaranalyse und den Messungen der magnetischen Suszeptibilität wurde eine Sequenz für die Zersetzung erstellt. Das Endprodukt wurde mittels Röntgendiffraktion als CeO2 identifiziert. Ammoniumzersulfat und die Produkte des ersten und des letzten Überganges enthalten Zerionen mit der Oxydationsstufe +4, während in den drei Zwischenschritten Zerionen mit der Oxydationsstufe +3 vorkommen. Anhand der nichtisothermen DSC-Untersuchungen wurden die kinetischen Parameter berechnet. Die isothermen Angaben zeigen, daß der Dehydratationsprozeß einem Ginstling-Brounstein Mechanismus folgt, während die folgenden drei Schritte durch das Mampelsche unimolekulare Gesetz der Randomkeimbildung bestimmt werden.
    Notes: Abstract Thermal decomposition of ammonium cerium sulphate has been studied by differential scanning calorimetry and thermogravimetry. The results show that the material decomposes in five steps in the temperature region 364–1116 K in oxygen. Based on the thermal data, elemental analysis and magnetic susceptibility measurements, sequence of decomposition has been established. The final product has been identified as CeO2 by X-ray diffractometry. Ammonium cerium sulphate and the products of the first and the final transitions contain cerium ion in 4+ oxidation state, while the three intermediate phases have cerium ion in 3+ oxidation state. From the non-isothermal DSC studies, kinetic parameters have been computed. The isothermal data show that the dehydration process follows Ginstling-Brounshtein mechanism, while the next three steps are governed by Mampel's unimolecular law of random nucleation.
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    Analyse du comportement thermique d'une serie de derives camphoriques (1992)
    Springer
    Journal of thermal analysis and calorimetry 38 (1992), S. 1545-1562 
    Details
    ISSN: 1572-8943
    Keywords: camphor derivatives ; DSC ; IR ; X-ray
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Mittels DSC wurde eine Reihe von Kampferderivaten untersucht. Dabei konnte verschiedenes Verhalten mit dem Auftreten von glasartigen, amorphen, kristallinen und polymorphen Verbindungen und tautomeren Gemischen beobachtet werden. Die erhaltenen Resultate wurden durch IR-Spektroskopie und Röntgendiffraktion bestätigt.
    Notes: Abstract Thermal analysis of a series of camphor derivatives has been studied by differential scanning calorimetry. Different behaviors with the appearance of glassy, amorphous, crystalline, polymorphous compounds and tautomeric mixture were detected. These results have been confirmed by infrared spectroscopy and by X-ray diffraction.
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    Thermal investigation of PEG 4000 — oxazepam binary system (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 1743-1753 
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    ISSN: 1572-8943
    Keywords: DSC ; HSM ; oxazepam ; PEG 4000 ; solid dispersion
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A thermal study using DSC and Hot Stage Microscopy (HSM) was carried out to investigate the interaction in solid state of the binary system PEG 4000 — oxazepam, and to establish their phase diagram. The eutectic composition, which melting occurs at lower temperature as compared with the pure components, has been determined. The results obtained by DSC and HSM have indicated that PEG 4000 — oxazepam mixtures displays no obvious incompatibilities, and that the system shows a typical eutectic behaviour. However because of the closeness of the melting of PEG 4000 to the eutectic temperature, it was difficult to determine precisely the eutectic composition and temperature on the basis of DSC measurements alone. The use of heats of fusion corresponding to physical mixtures allowed an estimation of the eutectic composition at 6% w/w oxazepam. Additional information of temperature (57.6
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    étude thermodynamique de certains médicaments (1996)
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    Journal of thermal analysis and calorimetry 47 (1996), S. 1755-1758 
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    ISSN: 1572-8943
    Keywords: combustion calorimetry ; DSC ; sulphamide type compounds
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Two compounds of sulphamide type:p-amino-benzene sulphonamide (I) and 3,4-dimethylisoxazol 5-sulphanylamide (II) were studied by combustion calorimetry and by differential scanning calorimetry (DSC). The enthalpies in solid state at 298,15 K of combustion, δc H m o (I)=-2788,5±1,6 kJ mol−1, δc H m o (II)=-5036±3,8 kJ mol−1 and of formation, δf H m o (I)=-458,3±1,6 kJ mol−1, δfH m o (II)=-180,1±3,8 kJ mol−1 were determined. The thermal effects concerning the melting and phase transition of this compounds were also measured.
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    URL: http://dx.doi.org/10.1007/BF01980921
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    Application of differential scanning calorimetry in food research and food quality assurance (1996)
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    Journal of thermal analysis and calorimetry 47 (1996), S. 1787-1803 
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    ISSN: 1572-8943
    Keywords: DSC ; food components ; food microbiology ; food quality
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Differential scanning calorimetry (DSC) is the most widely used thermal analytical technique in food research and it has a great utility in quality assurance of food. Proteins are the most studied food components by thermal analysis including studies on conformation changes of food proteins as affected by various environmental factors, thermal denaturation of tissue proteins, food enzymes and enzyme preparations for the food industry, as well as effects of various additives on their thermal properties. Freezing-induced denaturation of food proteins and the effect of cryoprotectants are also monitored by DSC. Polymer characterization based on DSC of polysaccharides, gelatinization behaviour of starches and interaction of starch with other food components can be determined, and phase transitions during baking processes can be studied by DSC. Studies on crystallization and melting behaviour of fats observed by DSC indicate changes in lipid composition or help characterizing products. Thermal oxidative decomposition of edible oils examined by DSC can be used for predicting oil stability. Using DSC in the freezing range has a great potential for measuring and modelling frozen food thermal properties, and to estimate the state of water in foods and food ingredients. Research in food microbiology utilizes DSC in better understanding thermoadaptive mechanisms or heat killing of food-borne microorganisms. Isothermic microcalorimetric techniques provide informative data regarding microbial growth and microbial metabolism.
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    URL: http://dx.doi.org/10.1007/BF01980925
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    Thermal characterization of polyethylene glycols applied in the pharmaceutical technology using differential scanning calorimetry and hot stage microscopy (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 291-304 
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    ISSN: 1572-8943
    Keywords: DSC ; pharmaceutical technology ; polymer
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract In the present study, the effect of the molecular weight and thermal treatments on commercial polyethylene glycols (PEG) samples used in the pharmaceutical processing technology, has been analyzed using DSC and HSM. The molecular weight of these polymers range from 1500 to 200000. Thermal investigations on the melting behavior of original PEG samples (as received from the manufacturer) showed only one single melting DSC endotherm effect before 373 K. This fact was associated to the presence of only one type of polymeric chain. Using standard conditions, PEG samples were solidified from the melt at 373 K, either by flash cooling (using liquid nitrogen and an ice bath) and by slow cooling, soaked and by slow cooling at room temperature. They were further studied by DSC. It was found that after cooling, PEG with molecular weight 1500 and 15000 showed DSC thermograms with a single endothermic peak. However, thermograms for PEG 4000 and 6000 produced a splitted melting endotherm. This fact was attributed to the presence of two types of chains, that are the folded and extended chains. Ageing time influences also the shape of the DSC endothermal effects. It was concluded that the endotherms obtained after heating these PEG indicate that the thermal history determine the structure (extended or folded chain type forms) and the degree of crystallinity, as evidenced by changes in heat of fusion values, melting points and structures after crystallization. The relationships between melting enthalpies and melting points, as deduced from DSC diagrams, with molecular weight of the polymers are also presented.
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    Thermal properties of a molecule in a constrained state (1996)
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    Journal of thermal analysis and calorimetry 46 (1996), S. 1081-1092 
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    ISSN: 1572-8943
    Keywords: chemical ionization MS ; constrained dye ; DSC ; dye-amylose inclusion complex ; Tandem MS ; TGA ; Thermal Desorption MS
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The thermal properties of a dye molecule (guest) inside the cavity of a host amylose helix were studied by TGA, DSC, and Thermal Desorption MS. The results show that the degradation temperature of dye shifts to a higher temperature by approximately 20°C.
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    URL: http://dx.doi.org/10.1007/BF01983622
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    Analysis of a symmetric neopolyol ester (1996)
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    Journal of thermal analysis and calorimetry 46 (1996), S. 1093-1111 
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    ISSN: 1572-8943
    Keywords: conformational disorder ; crystal ; DSC ; glass ; glass transition ; heat capacity ; melting transition ; tetra[methyleneoxycarbonyl (2,4,4-trimethyl) pentyl] methane
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Quantitative thermal analysis was carried out for tetra[methyleneoxycarbonyl(2,4,4-trimethyl)pentyl]methane. The ester has a glass transition temperature of 219 K and a melting temperature of 304 K. The heat of fusion is 51.3 kJ mol−1, and the increase in heat capacity at the glass transition is 250 J K−1 mol−1. The measured and calculated heat capacities of the solid and liquid states from 130 to 420 K are reported and a discussion of the glass and melting transitions is presented. The computation of the heat capacity made use of the Advanced Thermal Analysis System, ATHAS, using an approximate group-vibration spectrum and a Tarasov treatment of the skeletal vibrations. The experimental and calculated heat capacities of the solid ester were compared over the whole temperature range to detect changes in order and the presence of large-amplitude motion. An addition scheme for heat capacities of this and related esters was developed and used for the extrapolation of the heat capacity of the liquid state for this ester. The liquid heat capacity for the title ester is well represented by 691.1+1.668T [J K−1 mol−1]. A deficit in the entropy and enthalpy of fusion was observed relative to values estimated from empirical addition schemes, but no gradual disordering was noted outside the transition region. The final interpretation of this deficit of conformational entropy needs structure and mobility analysis by solid state13C NMR and X-ray diffraction. These analyses are reported in part II of this investigation.
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    Analysis of a symmetric neopolyol ester (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 1113-1132 
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    ISSN: 1572-8943
    Keywords: chiral molecule ; conformational disorder and motion ; crystal ; DSC ; heat capacity ; γ-gauche effect ; glass ; glass transition ; melting transition ; molecular mechanics computations ; tetra[methyleneoxycarbonyl (2,4,4-trimethyl) pentyl] methane ; solid state13C NMR ; X-ray diffraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The symmetric neopolyol ester tetra[methyleneoxycarbonyl(2,4,4-trirnethyl)pentyl]methane (MOCPM) has been studied by variable-temperature solid-state13C NMR and X-ray powder diffraction and compared to molecular mechanics calculations of the molecular structure. Between melting and glass transition temperatures the material is semicrystalline, consisting of two conformationally and motionally distinguishable phases. The more mobile phase is liquid-like and is, thus attributed to an amorphous phase (≈16%). The branches of the molecules in the crystal exhibit two conformationally distinguishable behaviors. In one, the branches are well ordered (≈56%), in the other, the branches are conformationally disordered (≈28%). Different branches of the same molecule may show different conformational order. This unique character of the rigid phase is the reason for the deficit of the entropy of fusion observed earlier by DSC. In the melt, solid state NMR can identify two bonds that are rotationally immobile, even though the molecules as a whole have liquid-like mobility. This partial rigidity of the branches accounts quantitatively for the observed increase in heat capacity at the glass transition. The reason for this unique behavior of MOCPM, a small molecule, is the existence of one chiral centers in each of the four arms of the molecule. A statistical model assuming that at least two of the chiral centers must fit into the order of the crystal can explain the crystallization behavior and would require 12.5% amorphous phase, 28.1% conformational disorder, and 59.4% crystallinity, close to the observed maximum perfection.
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    Thermoporosimetry (1996)
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    Journal of thermal analysis and calorimetry 46 (1996), S. 1177-1189 
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    ISSN: 1572-8943
    Keywords: DSC ; mercury porosimetry ; pore size distribution ; porous glass ; thermoporosimetry ; water
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The pore size distributions (PSDs) of microporous glass, which were controlled by acid leaching subsequent to phase separation of CaO-Al2O3-B2O3-SiO2 glass, were determined via both mercury porosimetry and thermoporosimetry (thermal porosimetry). As a result, the pore radii, the cumulative pore volumes, and the surface areas determined via thermoporosimetry were in good agreement with those determined via mercury porosimetry. It was revealed that thermoporosimetry could be applied to pore structure analysis for porous materials having pore sizes at least up to 58 nm in radius.
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    URL: http://dx.doi.org/10.1007/BF01983628
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    Investigation of dehydroxylation of gibbsite into boehmite by DSC analysis (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 1339-1347 
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    ISSN: 1572-8943
    Keywords: boehmite ; DSC ; gibbsite
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The dehydroxylation of gibbsite into boehmite was investigated by means of DSC analysis under non-isothermal conditions in the temperature range 453–673 K at heating rates from 2.5 to 20.0 K min−1. Mathematical analysis of the experimental DSC curves revealed the mechanism and kinetics of the gibbsite dehydroxylation process. The kinetic curvesα=f(t) andα=f(T) are sigmoidal in shape; their inflection points and the νm point of the curvesν=f(T) andν=f(T) are interrelated and are defined by the concept of a stationary point. The activation energy for the first stage of gibbsite dehydroxylation in the temperature range 453–673 K is 132.92±8.33–142.26±8.33 kJ mol−1.
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    Thermal analysis of the polymerization process on the surface of inorganic fillers (1996)
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    Journal of thermal analysis and calorimetry 46 (1996), S. 1541-1550 
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    ISSN: 1572-8943
    Keywords: DSC ; FTIR ; grafting ; IDSC ; kinetic parameters ; polymerization ; TG ; thermodynamic parameters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The thermal polymerization of pentabromobenzyl (mono)acrylate (PBB-MA) on the surface of the inorganic fillers Mg(OH)2 and CaCO3 was studied. FTIR spectroscopy and extraction of the polymer in bromobenzene show that polypentabromobenzyl acrylate (PBB-PA) was mostly grafted on the surface of Mg(OH)2. Thermal analysis (TG, DSC, isothermal DSC (IDSC)) demonstrated an increase in polymerization starting temperature, and differences in polymerization enthalpy and apparent activation energy when an inorganic filler is added. These differences depend on the chemical composition of the filler used.
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    Thermoplastic polymers quality control (1996)
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    Journal of thermal analysis and calorimetry 47 (1996), S. 117-121 
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    ISSN: 1572-8943
    Keywords: baseline ; DSC ; heat of fusion ; polyethylene
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A technique is proposed for improving the accuracy of the heat of fusion of semicrystalline polymers by DSC. The results of three commercially available instruments are compared.
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    URL: http://dx.doi.org/10.1007/BF01982691
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    Characterization of thermomechanical properties in starch and cereal products (1996)
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    Journal of thermal analysis and calorimetry 47 (1996), S. 195-213 
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    ISSN: 1572-8943
    Keywords: DMA ; DSC ; rheological impacts ; thermomechanical properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Thermomechanical properties of bread components can be used to characterize various events that have direct rheological impacts. The objective is to observe changes that occur during staling and toughening of a bread or similar products. In this article, characterization of bread polymers, starch and gluten, were examined by differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA).
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    Measurement of heterogeneously catalyzed gas reactions by DSC (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 445-452 
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    ISSN: 1572-8943
    Keywords: catalysts ; catalyst activity ; catalyst deactivation ; DSC ; gas reactions ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Gas reactions, catalyzed by solid catalysts, can be measured by DSC. In the experimental set-up an open sample pan with catalyst (powder or pellet) is placed on the sample side of the DSC sensor. The reactive gas mixture flows through the cell and reacts on the catalyst surface. The heat effect, caused by this reaction, results into a DSC signal. The calibration procedure is described for quantitative evaluation of the DSC measurements. For illustration four different reaction systems are discussed.
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    Internal flexibility of cardiac myosins (1996)
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    Journal of thermal analysis and calorimetry 47 (1996), S. 503-514 
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    ISSN: 1572-8943
    Keywords: cardiac myosin ; DSC ; flexibility of myosin heads ; spin-labelling
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Conventional and saturation transfer electron paramagnetic resonance spectroscopy (EPR and ST EPR) and differential scanning calorimetry (DSC) were used to study the motional dynamics and segmental flexibility of cardiac myosins. Cardiac myosins isolated from bovine and human heart muscle were spin-labelled with isothiocyanate- or maleimide-based probe molecules at the reactive sulfhydryl sites (Cys-697 and Cys-707) of the motor domain. The maleimide probe molecules attached to human cardiac myosin rotated with an effective rotational correlation time of 33 ns which was at least eight times shorter than the rotational correlation time of the same label on skeletal myosin (260 ns). In the presence of MgADP and MgADP plus orthovanadate, flexibility changes in the multisubunit structure of myosins were detected, but this did not lead to changes of the overall rotational property of the myosin heads. Significant difference in the internal flexibility was detected on myosin samples isolated from ischemic tissue, the rotational correlation time decreased to 25 ns. DSC measurements supported the view that addition of nucleotides produced additional loosening in the multisubunit structure of cardiac myosin. It is postulated that there is an intersite communication between the nucleotide binding domain and the 20 kDa subunit where the reactive thiol sites are located.
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    Thermal analysis of hydrated calcium aluminates (1996)
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    Journal of thermal analysis and calorimetry 47 (1996), S. 765-774 
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    ISSN: 1572-8943
    Keywords: calcium aluminates ; cement ; DSC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Differential scanning calorimeter (DSC) has been used to study the dehydration characteristics of hydrated calcium aluminates such as CA, CA2 and C12A7 where C and A stand for CaO and Al2O3 respectively. Dehydration of CAH10 and C2AH8 (whereH=H2O) occur ∼ at 160–180°C and 200–280°C respectively. These two phases are unstable and ultimately get transformed to AH3 and C3AH6. Dehydration of AH3 and C3AH6 occur between 290 and 350°C and overlap at lower scanning rate. The activation energy for dehydration of the stable AH3 and C2AH6 phases has been found to be 107.16 and 35.58 kJ mol−1 respectively. The compressive strength of the hydrated calcium aluminates has been determined. The result shows that in the case of CA, almost 90% of ultimate strength has been attained in 1 day whereas in CA2, ultimate strength has been attained in 14 days and in C12A7 in 1 day. DSC results have been correlated with the rate of strength developments.
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    Caracterisation par analyse calorimetrique differentielle des complexes entre LiAlH4 et les ethers-couronnes 12-C-4, 15-C-5, dicyclohexano-18-C-6 (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 833-846 
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    ISSN: 1572-8943
    Keywords: crown-ethers (CE) ; 12-C-4 ; 15-C-5 ; DC 18-C-6anti ; DC 18-C-6syn ; DSC ; LiAlH4-CE complexes ; glass-transition ; solvates
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The thermal behaviour of complexes [Li+-EC](AlH4)− withEC=12-C-4, 15-C-5, DC 18-C-6 (cis-anti-cis andcis-syn-cis isomers) was investigated by Differential Scanning Calorimetry (DSC). These complexes were prepared as solids from benzene solutions. Pure EC and several solvated species [Li+-EC](AlH4)−·nC6H6 (EC=15-C-5, DC 18-C-6syn) were also studied. DSC has revealed various phenomena. Solid-solid transitions were observed before melting for [Li+-EC](AlH4)− withEC=12-C-4 and 15-C-5. They are probably explained by small molecular modifications strongly dependent on the thermal history of the sample. A glass-transition was found for the pure crown-ether DC 18-C-6anti, the complex [Li+-EC](A1H4)− withEC=DC-18-C-6anti and the two solvates mentioned above.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01981818
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  • 96
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    The glass transition (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 887-896 
    Details
    ISSN: 1572-8943
    Keywords: compensation temperature ; DSC ; fictive temperature ; poly(ethylene terephthalate) ; thermally stimulated depolarization current
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract This work deals with a comparison of data obtained from differential scanning calorimetry (DSC) and thermally stimulated depolarization current (TSDC) investigations. Measurements were performed on various poly(ethylene terephthalate) films: a wholly amorphous, a thermally crystallized and drawn samples. For each specimen, the TSDC complex spectra, resolved into elementary ones, led to the determination of the classical compensation temperature (T c ). The glass transition temperature (T g) and the fictive equilibrium temperature (T f) were determined by means of DSC. It appears thatT c is different fromT g and very close toT f.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01981823
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  • 97
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    Isothermal melt crystallization kinetics of poly(L-lactic acid) (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 931-939 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; isothermal melt crystallization ; kinetic parameters ; Mathematica® ; new kinetic model ; poly(L-lactic acid)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A DSC study was carried out of the isothermal melt crystallization kinetics of poly(L-lactic acid), PLLA, at 110, 115, 120, 125 and 130
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01979440
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  • 98
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    Enthalpic Relaxation of 25Na2O·xTiO2·(75-x)SiO2 Glasses (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 155-164 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; glass ; relaxation ; structure
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The enthalpic relaxation of the title glasses, studied by differential scanning calorimetry, is well described by a mathematical model based on the stretched exponential relaxation function with the relaxation time proportional to the actual viscosity. The dependence of viscosity on temperature and the fictive temperature was expressed by Mazurin's approximation. The relaxation parameters obtained correlated significantly with the glass composition, indicating the changes in the structural of the TiO2 role near a TiO2 content of 3–4 mol%.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1010148525445
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  • 99
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    Thermal Studies of Nickel(II) Squarate Complexes of Triamines in the Solid State (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 165-172 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; nickel(II) squarate ; phase transition ; TG-DTA ; triamine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract [NiL2]C4O4·nH2O [where n=2 when L=diethylenetriamine(dien) and N-(3-aminopropyl)-1,3-propanediamine (dpt); n=3 when L=N-(2-aminoethyl)-1,3-propanediamine (aepn); n=0 when L=N2-methyldiethylenetriamine (medien)] and Ni(tmdien)C4O4·2H2O (where tmdien=1,4,7 trimethyl-diethylenetriamine) have been synthesised and investigated thermally in the solid state. Ni(dpt)C4O4·H2O has also been synthesised pyrolytically in the solid state from the corresponding bis complex. All the complexes possess octahedral geometry. The squarate anion takes part in coordination only in monotriamine species. [Ni(medien)2]C4O4 upon heating undergoes phase transition (270–285°C; ΔH=4.9 kJ mol−1) accompanied by colour change pink to grey. Thermal stability decreases with increase in chain length of the triamines.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1010100609516
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  • 100
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    Effects of Pretreatments on the Structure of Palladium-Containing Amorphous Alloys Followed by DSC (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 305-310 
    Details
    ISSN: 1572-8943
    Keywords: amorphous palladium alloys ; DSC ; hydrogenation ; mechanical alloying ; phenylacetylene ; structural characterization ; X-ray diffractometry ; X-ray photoelectron spectroscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Amorphous PdZr, PdCuZr and PdCuSi alloy ribbons and powders are characterized by DSC, XRD and XPS in the as-received state and after treatments with oxygen, hydrogen or dilute hydrogen fluoride solution. Zr-containing alloys are shown to undergo substantial structural changes resulting in palladium enrichment on their surface, whereas no apparent changes in the bulk structure are found for PdCuSi. Catalytic activity and selectivity of the pretreated samples were tested in the hydrogenation of phenylacetylene.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1010134230886
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