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  • DSC
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  • General Chemistry
  • Theoretical, Physical and Computational Chemistry
  • Springer  (202)
  • 1995-1999  (202)
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  • 1
    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.
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  • 2
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    Journal of thermal analysis and calorimetry 55 (1999), S. 9-19 
    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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  • 3
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    Journal of thermal analysis and calorimetry 55 (1999), S. 67-76 
    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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  • 4
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    Journal of thermal analysis and calorimetry 55 (1999), S. 57-65 
    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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  • 5
    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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  • 6
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    Journal of thermal analysis and calorimetry 56 (1999), S. 51-57 
    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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  • 7
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    Journal of thermal analysis and calorimetry 56 (1999), S. 925-929 
    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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  • 8
    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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  • 9
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    Journal of thermal analysis and calorimetry 56 (1999), S. 1285-1304 
    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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  • 10
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    Journal of thermal analysis and calorimetry 57 (1999), S. 61-73 
    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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  • 11
    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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  • 12
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    Journal of thermal analysis and calorimetry 57 (1999), S. 631-642 
    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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  • 13
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    Journal of thermal analysis and calorimetry 58 (1999), S. 29-38 
    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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  • 14
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    Journal of thermal analysis and calorimetry 58 (1999), S. 363-368 
    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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  • 15
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    Journal of thermal analysis and calorimetry 58 (1999), S. 653-662 
    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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  • 16
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    Journal of thermal analysis and calorimetry 58 (1999), S. 725-739 
    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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  • 17
    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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  • 18
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    Journal of thermal analysis and calorimetry 55 (1999), S. 807-816 
    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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  • 19
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    Journal of thermal analysis and calorimetry 55 (1999), S. 789-796 
    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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  • 20
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    Journal of thermal analysis and calorimetry 56 (1999), S. 7-15 
    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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  • 21
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    Journal of thermal analysis and calorimetry 56 (1999), S. 429-435 
    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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  • 22
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    Journal of thermal analysis and calorimetry 56 (1999), S. 547-552 
    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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  • 23
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    Journal of thermal analysis and calorimetry 56 (1999), S. 783-792 
    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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  • 24
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    Journal of thermal analysis and calorimetry 56 (1999), S. 947-951 
    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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  • 25
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    Journal of thermal analysis and calorimetry 56 (1999), S. 1155-1161 
    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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  • 26
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    Journal of thermal analysis and calorimetry 56 (1999), S. 1141-1146 
    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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  • 27
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    Journal of thermal analysis and calorimetry 56 (1999), S. 1353-1357 
    ISSN: 1572-8943
    Keywords: DSC ; terpenoids ; TG ; thermal behaviour
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    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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    Journal of thermal analysis and calorimetry 57 (1999), S. 371-375 
    ISSN: 1572-8943
    Keywords: C14E8 ; detergent ; DSC ; polyethylene glycol tetradecyl ether ; thermal transition
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    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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  • 29
    ISSN: 1572-8943
    Keywords: DSC ; iron(II)-oxime complexes ; kinetic parameters ; Mössbauer spectroscopy
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    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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  • 30
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    Journal of thermal analysis and calorimetry 57 (1999), S. 745-752 
    ISSN: 1572-8943
    Keywords: confinement effects ; DSC ; dynamic light scattering ; finite-size effects ; glass transition ; o-terphenyl
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    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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    Journal of thermal analysis and calorimetry 57 (1999), S. 847-851 
    ISSN: 1572-8943
    Keywords: DSC ; linear low-density polyethylene(LLDPE) ; low density polyethylene (LDPE) ; polymer blend ; thermal properties
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    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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  • 32
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    Journal of thermal analysis and calorimetry 58 (1999), S. 369-373 
    ISSN: 1572-8943
    Keywords: critical temperature ; DSC ; HNNC ; non-isothermal
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    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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  • 33
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    Journal of thermal analysis and calorimetry 55 (1999), S. 155-164 
    ISSN: 1572-8943
    Keywords: DSC ; glass ; relaxation ; structure
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    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%.
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  • 34
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    Journal of thermal analysis and calorimetry 55 (1999), S. 165-172 
    ISSN: 1572-8943
    Keywords: DSC ; nickel(II) squarate ; phase transition ; TG-DTA ; triamine
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    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.
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  • 35
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    Journal of thermal analysis and calorimetry 56 (1999), S. 305-310 
    ISSN: 1572-8943
    Keywords: amorphous palladium alloys ; DSC ; hydrogenation ; mechanical alloying ; phenylacetylene ; structural characterization ; X-ray diffractometry ; X-ray photoelectron spectroscopy
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    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.
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    Journal of thermal analysis and calorimetry 56 (1999), S. 1203-1209 
    ISSN: 1572-8943
    Keywords: conformation of myosin ; DSC ; EPR ; spin labelling
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The internal dynamics and the thermal stability of myosin in rabbit psoas muscle fibres in different intermediate states of the ATP hydrolysis cycle were studied by differential scanning calorimetry (DSC) and electron paramagnetic resonance (EPR) spectroscopy. Three overlapping endotherms were detected in rigor, in strongly binding and weakly binding state of myosin to actin. The transition at 58.4°C can be assigned to the nucleotide-binding domain. The transition at highest temperature represents the unfolding of the actin and the contributions arising from the actin-myosin interaction. The transition of 54°C reflects the interaction between the subunits of myosin. Nucleotide binding induced shifts of the melting temperatures and produced variations in the calorimetric enthalpy changes. The changes of the EPR parameters indicated local rearrangements of the internal structure in myosin heads.
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    Journal of thermal analysis and calorimetry 56 (1999), S. 1323-1327 
    ISSN: 1572-8943
    Keywords: chloramphenicol ; DSC ; quality control ; TG
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The stability and thermal behaviour of chloramphenicol and various of its mixtures were investigated. The thermogravimetric and stability constant results showed that the chloramphenicol base is thermally more stable than the tablet in the studied formulation. The reduction in stability was attributed to the presence of starch in the formulation. The thermal decompositions of the chloramphenicol base and the tablet obey first-order kinetics.
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  • 38
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    Journal of thermal analysis and calorimetry 56 (1999), S. 1311-1316 
    ISSN: 1572-8943
    Keywords: alumina ; aluminum oxide ; compact ; DSC ; particles ; pentaerythritol tetraacetate ; pharmaceuticals ; powder ; thermal resistance ; transient state
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The previously described method involving the use of transient DSC was applied to pharmaceutical powder compacts and to ceramic powder compacts. The samples were prepared by compressing powders of pentaerythritol tetraacetate and two kinds of alumina powder (differing in particle size distribution) up to a pressure of 20 MPa by using a jig. For pentaerythritol tetraacetate, a linear relationship was obtained between the parameter obtained by DSC and the compaction pressure.
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  • 39
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    Journal of thermal analysis and calorimetry 56 (1999), S. 1005-1010 
    ISSN: 1572-8943
    Keywords: DSC ; enthalpic relaxation ; glass transition ; physical ageing
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Enthalpic relaxation has been used to model the development of the glass transition in polymers, using kinetic parameters determined separately. For this purpose the Kohlrausch-Williams-Watt stretched exponential function, relating the extent of relaxation, Φ(t), to time t and an average relaxation time, τa, i.e. $$1 - \Phi \left( t \right) = \exp \left( { - t/ta} \right)^{\beta }$$ where β is inversely related to the breadth of the relaxation spectrum, has been adopted. The relaxation time dependence on temperature was taken to follow the modified Arrhenius relationship, $$\tau _a = A\exp \left[ {\frac{{X\Delta H}}{{RT}} + \frac{{\left( {1 - X} \right)\Delta H}}{{RT'}}} \right]$$ where T is the storage and T′ the fictive temperature, X is the structure factor and ΔH the activation enthalpy. Both have been found to describe the process of enthalpic relaxation in polymer glasses and a direct comparison has been made with the change in specific heat observed with different cooling rates in DSC experiments. The effect of variables, such as activation enthalpies, pre-exponential factors, and the non-linear factors such as X and β on the observed Tgs and the temperature range over which the transition occurred have been determined.
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    Journal of thermal analysis and calorimetry 57 (1999), S. 283-291 
    ISSN: 1572-8943
    Keywords: DSC ; fish ; general proteolytic activity ; pyloric caeca ; ripening ; salted herring product
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The thermoanalytical behaviour of pyloric caeca during salting and ripening was investigated using a Perkin Elmer DSC 7. Not only the thermal stability of the muscle proteins was influenced by salting but also that of pyloric caeca. It was recognised that the salting itself leads to a remarkable increase of the transition temperature compared with raw herring. An influence of the salt:fish ratio could be observed. The higher the salt content the higher the increase of the denaturation temperature. During ripening the transition temperature remained on a high level or showed only a slight decrease during the investigation period. The dependency from the salt content remained evident. The increase of the transition temperature was accompanied by a decrease of the transition enthalpy. The increase of thermal stability is connected with a decrease of the general proteolytic activity in pyloric caeca. Possibly, the enzymes are diffusing from the pyloric caeca into the muscle and cause there an increase of enzymatic activity observable in North Sea herring accompanied by a decrease of activity in pyloric caeca itself. Simultaneous the thermal stability of pyloric caeca is lowered. The reason for the differences in ripening could be seen in some enzyme-inhibiting factors unknown until now.
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    Journal of thermal analysis and calorimetry 57 (1999), S. 409-414 
    ISSN: 1572-8943
    Keywords: DSC ; thermal denaturation ; vegetative bacteria
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Thermal stability of vegetative cells of Listeria monocytogenes, Escherichia coli and Lactobacillus plantarum was studied by counting viable fractions and determining DSC curves of their suspensions. DSC curves in the 5–99°C range showed a series of endothermic transitions between 50 and 60°C, where the heat destruction of cells occurred. Heat denaturation of DNA required a higher temperature than cell killing. Thermal death was strongly influenced by the pH, composition and NaCl content of the suspending buffer. A mathematical model developed by us enabled comparison of DSC peak temperatures and temperatures required for loss of viability.
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  • 42
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    Journal of thermal analysis and calorimetry 57 (1999), S. 517-526 
    ISSN: 1572-8943
    Keywords: DSC ; humic substances ; thermal properties
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Differential Scanning Calorimetry combined with Fourier transform infrared spectroscopy, was applied to the study of a number of fulvic and humic acids extracted from soils, peat, river and seawater. The thermal patterns obtained were related to the nature and origin of samples. The low-temperature endotherms were attributed to dehydration and loss of peripheral polysaccharide chains. The endotherm at 250°C observed for soil FA was ascribed to partial decarboxylation of more labile surface COOH groups, whereas the high-temperature exotherms at about 500°C were related to the degree of polycondensation of the aromatic network of the humic molecules.
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  • 43
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    Journal of thermal analysis and calorimetry 58 (1999), S. 13-18 
    ISSN: 1572-8943
    Keywords: DSC ; enthalpic relaxation ; polyurethane ; TSDC
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Polyurethane acrylate resins cured by two different ways, a thermal way and a photochemical way, are investigated by means of differential scanning calorimetry (DSC) and thermally stimulated depolarization currents (TSDC). Even if both curing methods lead to the same material from a chemical point of view, we show that important differences exist between the thermocured resin and the photocured resin in terms of molecular relaxation behaviour.
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  • 44
    ISSN: 1572-8943
    Keywords: DMTA ; DSC ; mechanical properties ; metallocene catalysts ; polyethylene
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    Topics: Chemistry and Pharmacology
    Notes: Abstract A series of high density polyethylenes (HDPE) were synthesized via homogeneous polymerization with metallocene catalyst in two different reactors (glass and stainless steel). The thermal and mechanical properties of the polyethylenes, synthesized with two types of reactor and different reaction parameters, are discussed.
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  • 45
    ISSN: 1572-8943
    Keywords: adducts ; cobalt complex ; DSC ; kinetics ; nickel complex ; O,O'-dialkyldithiophosphate ; pyridine ; TG-DTG
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Thermal behaviour of tri(O,O'-diisopropyldithiophosphate)cobalt(III), Co(dptp)3 and bis (O,O'-diethyldithiophosphate)nickel(II), Ni(detp)2 and its adducts with pyridine, Ni(detp)2(py)2 or 4-methylpyridine, Ni(detp)(mpy)2 in a dynamic nitrogen atmosphere was investigated by TG-DTG and DSC techniques, which showed a medium endothermic peak for the evolution process of pyridine(or 4-methylpyridine) and a strong exothermic peak for that of O,O'-diethyldithiophosphate. The thermal stability and decomposition patterns for these compounds were compared and interpreted in terms of structural features such as bond character and steric effects. The kinetic parameters and mechanisms of every decomposition stage involved for all these complexes were obtained employing the non-isothermal kinetic analysis method suggested by Malek et al., which showed the kinetics mechanism for pyrolysis of pyridine(or 4-methylpyridine) is an S-B empirical model with lower activation energy, while that of O,O'-dialkyldithiophosphate is a diffusion model. These results are in accord with the fact that two ligands are of different type.
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  • 46
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    Journal of thermal analysis and calorimetry 55 (1999), S. 85-92 
    ISSN: 1572-8943
    Keywords: DSC ; exothermic peak ; human serum albumin ; non-equilibrium state ; pyridine-n-hexane mixtures
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Human serum albumin (HSA) immersed in pyridine-n-hexane mixtures was analyzed using differential scanning calorimetry (DSC). State of the solid HSA in organic solvent mixtures is the non-equilibrium state which is seen as the exothermic peak on the DSC curves. The enthalpy change corresponding to this exothermic peak approaches zero when going from pure pyridine to pure n-hexane. Dependence of the enthalpy change on the pyridine concentration is suggestive that the non-equilibrium state of the immersed HSA results from the HSA-pyridine interactions 'frozen' at the lower temperature. Most likely the temperature-initiated exothermic peak observed on the DSC curves reflects the swelling of HSA by pyridine.
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  • 47
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    Journal of thermal analysis and calorimetry 56 (1999), S. 437-446 
    ISSN: 1572-8943
    Keywords: Al-La-Ni amorphous ribbons ; DSC ; heating rate ; non-isothermal crystallization kinetics
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Crystallization kinetics of Al91La5Ni4 amorphous ribbons produced by a melt-spinning method were studied by DSC analysis and X-ray diffraction. The effect of heating rate (from 4 to 200°C min-1) was investigated in the temperature range from 298 to 700 K. Increases the heating rate from 4 to 200°C min-1 resulted in increases of the temperature difference between the two stages of the transformation process: crystallization of Al and crystallization of the Al compounds from 148.9 to 167.4 K. The apparent activation energies for the first step, related to Al crystallization, and to the second step related to crystallization of Al4La and Al3Ni, were found to be 161±9 and 199±10 kJ mol-1, respectively. The results indicate the possibility of tailoring the heating treatment to produce the required fraction of the amorphous phase.
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  • 48
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    Journal of thermal analysis and calorimetry 56 (1999), S. 1211-1216 
    ISSN: 1572-8943
    Keywords: dispersion-type processed cheese ; DSC ; ELMI
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    Topics: Chemistry and Pharmacology
    Notes: Abstract In contrast with the traditional method of cheese processing, where Ca breaks down from the protein chain and protein is peptized, a new technology has been elaborated, during which cheese is dispersed without phosphate-containing processing salt, when the gel is formed by plant hydrocolloids. Raw material of constant composition was processed with a phosphate-containing salt or in the presence of hydrocolloids. Thermodynamic processes occurring during the processing and in the end-products were examined by an ultra-sensitive micro DSC method. The structures of end-products were also investigated by electronmicroscopy. The temperature ranges of the endothermal processes indicating the transformations of protein and hydrocolloids can be distinguished: 81-90°C for peptization processing and 61-72°C for processing without peptization. The differences are less in the end-products: 75-87°C in traditional processed cheese and 68-74°C in processed cheeses made without peptization. In contrast with the spongy structure of traditional processed cheeses consisting of peptized proteins, processed cheeses made without peptization involve structure-forming elements created by the interaction of linear macromolecules of hydrocolloids and cheese proteins.
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  • 49
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    Journal of thermal analysis and calorimetry 56 (1999), S. 1317-1322 
    ISSN: 1572-8943
    Keywords: cyclodextrins ; drugs ; DSC ; excipients ; prochlorperazine
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Differential scanning calorimetry was used to examine the thermal behaviour of mixtures of the drug prochlorperazine with standard excipients, to assess potential interactions, and of mixtures with cyclodextrins, to investigate inclusion complexation which could increase the photostability of the drug. For most of the excipients (magnesium stearate, stearic acid, Explotab®, Ac-Di-Sol®, Encompress® and Ludipress®, lactose and Starch 1500) disappearance or broadening of the melting endotherm of the drug indicated interactions. Lubritab® was the only 'inert' excipient tested. Mixtures of prochlorperazine and the cyclodextrins gave incomplete inclusion complexation as shown by only partial disappearance of the melting endotherm of the drug.
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    Journal of thermal analysis and calorimetry 57 (1999), S. 599-605 
    ISSN: 1572-8943
    Keywords: DSC ; lead bromide ; melting ; systematic error
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The melting of PbBr2 in sealed crucibles was investigated by means of DSC. Three factors were considered to affect melting point: i) impurities, ii) the bromine pressure over the PbBr2, and iii) photolysis. Both crystals and powders were investigated. The peak of the melting changed after sample grinding. The bromine pressure over the PbBr2 was found to cause a significant error in the determination of the melting point. Lead bromide melts at 370.6±0.2°C. The heat of melting is 42.9±1.8 J g−1.
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  • 51
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    Journal of thermal analysis and calorimetry 58 (1999), S. 243-248 
    ISSN: 1572-8943
    Keywords: actin ; cisplatin ; DSC ; thiol ; transplatin
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The effects of cisplatin and its trans isomer transplatin on the thermal denaturation of G-actin were studied with a Micro DSC-III differential scanning calorimeter. The denaturation enthalpy of G-actin was found to be 12 J g−1, and the denaturation temperature was 328 K. The thermal denaturation curve showed that increasing cisplatin concentration decreased the enthalpy change. However, after the ratio of cisplatin to G-actin attained 8:1 (mol:mol), the denaturation enthalpy no longer decreased. Transplatin decreased the enthalpy change more rapidly. In contrast with cisplatin, the denaturation peak at 328 K disappeared, and a strong exothermic peak appeared at 341 K when the ratio of transplatin to G-actin was 8:1 (mol:mol). The enthalpy change was 75 J g−1, which is far in excess of the range of weak interactions. This strong exothermic phenomenon probably reflects the agglutination of protein. The effects of cisplatin and transplatin on the number of the free thiol groups of G-actin are discussed.
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  • 52
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    Journal of thermal analysis and calorimetry 58 (1999), S. 569-577 
    ISSN: 1572-8943
    Keywords: counterion effect ; DSC ; membrane ; Nafion-H ; Nafion salts ; TG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The thermal behavior of Nafion-117 membranes was investigated by thermogravimetric analysis (TG) and differential scanning calorimetry (DSC). TG measurements revealed that the mechanism of thermal degradation of a Nafion membrane in the acid form is different from that of Nafion in the sodium form. The DSC curves for the first heating, for both acid and salt forms, display two endothermic peaks, near 120 and 230°C. The high-temperature peak was assigned to the crystalline domains melting in Nafion, and the low-temperature peak was attributed to a transition into ionic clusters, since this transition exhibits significant changes depending on the nature of the counterion and the degree of hydration.
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  • 53
    ISSN: 1572-8935
    Keywords: PEEK ; Composites ; DSC ; Crystallinity ; Melting
    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 Films of short carbon fiber reinforced poly(ether ether ketone) (PEEK) composite were formed by compression molding pellets for 10 min at 380 °C under air. A heating stage was used to prepare isothermally treated PEEK composites before DSC scan. The dependence of degree of crystallinity on the heating rate (10–80 °C/min) was investigated for specimens crystallized at different temperatures. The results indicated that 50 °C/min was an optimum heating rate to suppress the reorganization and to avoid the superheating of high crystallinity specimens with the sample weight of 10 mg. The upper peak temperature of double-melting peaks continued to increase with crystallization temperature. This peak temperature was related to the transition from regime II to III. The phenomenon of lower crystallinity and higher melting temperature supports the interpretation that the upper melting peak corresponded to crystals growing during the earlier stage of isothermal crystallization.
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  • 54
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    Journal of thermal analysis and calorimetry 52 (1998), S. 765-772 
    ISSN: 1572-8943
    Keywords: DSC ; isoconversional method ; polyethylene glycol ; T-CR-T diagrams
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The analysis of DSC experimental data from solidification is improved, thanks to a modified isoconversional method. The validity of the proposed method is tested for a polyethylene glycol with a mean molecular weight of 6000. The temperature-cooling rate-transformation diagrams reveal good agreement between the experimental and calculated data.
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  • 55
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    Journal of thermal analysis and calorimetry 53 (1998), S. 35-47 
    ISSN: 1572-8943
    Keywords: DSC ; isothermal crystallization ; thermotropic polyester
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Differential scanning calorimetry was used to study the isothermal kinetics of three-dimensional ordering formation from the mesophase of the thermotropic polyester poly(ethylethylene-4,4-diphenoxyterephthalate). An Avrami exponent of 4 was found and the measured rates of transformation were related with the efficiency of packing. A nucleation and growth process was assumed in the determination of the temperature coefficient, and the interfacial free energies are discussed in terms of the chain flexibility.
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  • 56
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    Journal of thermal analysis and calorimetry 53 (1998), S. 71-85 
    ISSN: 1572-8943
    Keywords: DSC ; enantiomer ; IR ; powder X-ray diffractometry ; racemate ; TG ; thermomicroscopy
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The physicochemical characterization of the solid-state enantiomers and racemate of efaroxan hydrochloride (C13H17N2O+Cl-, M=252.5 g mol-1) was performed by thermoanalytical methods (differential scanning calorimetry, thermogravimetry and thermomicroscopy) and spectral methods (infrared spectrometry and X-ray diffractometry). The efaroxan enantiomers and racemate were shown to be unstable near the melting point. At the beginning of the decomposition, a loss of hydrogen chloride was observed. However when sealed pans were used, the compounds decomposed at higher temperature, allowing a precise evaluation of the melting enthalpies by means of differential scanning calorimetry. The nature of the racemate and its thermal stability were assessed by evaluating its free formation enthalpy. An enantiotropic solid-solid transformation (II→I) was noted for the racemate; the reverse process (I→II) follows zero-order kinetics.
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  • 57
    ISSN: 1572-8943
    Keywords: copper(II)-oxime complexes ; DSC ; kinetic parameters
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Several new complexes of the types [Cu(DioxH)2] and [CuX2·DioxH2] (DioxH2: aliphatic or alicyclic α-dioxime) were obtained and characterized by means of near and far Fourier transformation IR spectroscopy. The thermal decompositions of seven complexes of these types were studied by using DSC measurement data. For several decomposition stages, apparent kinetic parameters were derived by means of the nomogram method.
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  • 58
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    Journal of thermal analysis and calorimetry 54 (1998), S. 467-476 
    ISSN: 1572-8943
    Keywords: DSC ; TMDSC ; thermal conductivity ; thermal diffusivity
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    Topics: Chemistry and Pharmacology
    Notes: Abstract One of the benefits of temperature-modulated DSC (TMDSC) is its ability to measure thermal conductivity and thermal diffusivity without DSC cell modifications or additional accessories. Thermal conductivity of solid materials from 0.1 to about 1 W m-1 K-1 measured. Applications of this approach have been discussed in the literature but no description is yet available concerning the derivation of the working equations. This presentation provides a detailed derivation of the working equations used to obtain thermal conductivity and thermal diffusivity from TMDSC data.
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  • 59
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    Journal of thermal analysis and calorimetry 54 (1998), S. 721-729 
    ISSN: 1572-8943
    Keywords: branching ; chain extension ; cross-linking ; diepoxides or bis-epoxides ; DSC ; PET ; poly(ethylene terephthalate)
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    Topics: Chemistry and Pharmacology
    Notes: Abstract A series of chain-extended PET samples were obtained by the use of different amounts of a diepoxide as chain extender, which was prepared for this purpose. These samples exhibited different intrinsic viscosities and degrees of branching or cross-linking. The effects of this differentiation on the thermal properties were studied by differential scanning calorimetry. The thermal parameters studied were the glass transition temperature (Tg), the cold-crystallization temperature (Tcc), the melting temperature (Tm), the enthalpy (ΔHm) and the degree of crystallinity. The data revealed that, the higher the quantity of chain extender or the chain extension time, the higher Tgand Tcc, but the lower Tmand ΔHm, i.e. the more amorphous the chain-extended samples, as also shown by density measurements.
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  • 60
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    Journal of thermal analysis and calorimetry 52 (1998), S. 109-113 
    ISSN: 1572-8943
    Keywords: amorphous solid water ; aqueous systems ; DSC ; glass transition ; supercooling
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    Topics: Chemistry and Pharmacology
    Notes: Abstract After a brief introduction of the terms supercooling, amorphous solid state, glass transition and devitrification, the known ways of production of amorphous solid water are discussed. DSC experiments with quench cooled aqueous solutions show the phenomenon of glass transition and devitrification.
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    Journal of thermal analysis and calorimetry 52 (1998), S. 157-164 
    ISSN: 1572-8943
    Keywords: dicarboxylic acid ; DSC ; glass transition temperature ; mechanical parameters ; plasticizer
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    Topics: Chemistry and Pharmacology
    Notes: Abstract A study was made of the applicability of dicarboxylic acid diesters for the plasticization of starch acetate. The ratio of the carboxyl and methylene groups was found to be the most important criterion for the use of this group of substances. This ratio should have values between 0.45 and 0.66. From the available dicarboxylic acid diesters, the diethyl esters and dibutyl esters were investigated.
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  • 62
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    Journal of thermal analysis and calorimetry 52 (1998), S. 125-130 
    ISSN: 1572-8943
    Keywords: DSC ; impression materials ; photopolymerization
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The photopolymerization of a commercial sheet material as used in the dental laboratory was investigated by using the photocalorimeter DSC7/DPA7 (Perkin-Elmer). Using normal reaction conditions (light wavelength ≤400 nm, light intensity ≥1 mW cm−2 and sample thickness ≤2.5 mm), the curing was completed within few min. The reaction rate was nearly independent on the light wavelength in the range between λ=300 and 380 nm, but decreased distinctively at longer wavelengths. After desmearing the DSC curves, the dependence of the reaction rate on light intensity and sample thickness could be described in very good approximation by an equation derived by Tryson [1]. Comparable with pure acrylates or methacrylates, a pronounced dark reaction was found after interruption of the illumination.
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  • 63
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    Journal of thermal analysis and calorimetry 52 (1998), S. 177-185 
    ISSN: 1572-8943
    Keywords: azobenzene ; DSC ; kinetics
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Contrary to the situation in the field of temperature, heat and heat flow rate calibration, so far no generally accepted and easily practicable chemical reaction exists with regard to a kinetic evaluation. A possible reaction would be the well-known first-order cis-trans isomerization of subcooled liquid azobenzene. Surprisingly, the evaluation of measurements performed with a power compensated calorimeter yields activation parameters, which are dependent on the heating rate. The desmearing of the curves does not produce any improvements. However, constant activation parameters are obtained, if a small self-heating of the sample during the exothermic reaction is taken into account.
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  • 64
    ISSN: 1572-8943
    Keywords: DSC ; manganese oxides ; reduction
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The aim of this work was to study the thermal transitions of several manganese oxides (MnO, MnOOH, Mn2O3, Mn3O4 and MnO2) under reducing conditions. Differential scanning calorimetry (DSC) was used to analyse the transitions of some oxides into others. A comparison of the behavior of the synthetic samples with that of a natural manganese dioxide demonstrated that DSC is a quick tool for the distinction of natural manganese dioxide from synthetic γ-MnO2 from other manganese oxides.
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  • 65
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    Journal of thermal analysis and calorimetry 52 (1998), S. 1013-1022 
    ISSN: 1572-8943
    Keywords: activation energies ; DMA ; DSC ; elastic moduli ; epoxy resin
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The influence of the resin/diamine ratio on the properties of the system diglycidyl ether of bisphenol A (BADGE n=0/m-xylylenediamine) (m-XDA) was studied. Variation of this ratio resulted in significant effects on the cure kinetics and final dynamic mechanical properties of the product material. The study was made in terms of storage modulus (E′), vss modulus (E″) and molecular mass between cross-links (Mc) at different ratios. Two geometries (cylindrical and rectangular) were considered. The influence of temperature was studied through the activation energy (Ea〉), which depends on the epoxy/amine ratio and the geometry of the samples. Glass transition temperatures (Tg〉) and glass transition temperatures for thermosets with null degree of conversion (Tgo〉) were determined by DSC. Tg〉 decreases when amounts of curing agent greatly in excess of the stoichiometric composition were used.
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    Journal of thermal analysis and calorimetry 52 (1998), S. 831-836 
    ISSN: 1572-8943
    Keywords: DSC ; fullerenes ; solubility ; solvated crystals
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Differential scanning calorimetry (DSC) was used to study the binary systems of C60-o-xylene and C70-o-xylene and the ternary system C60-C70-o-xylene. Fullerene C60 formed solvated crystals C60·2C8H10 with incongruent melting point 320 K and with enthalpy of decomposition 31±3 kJ (mol of C60)-1. Two solvated crystals of C70 with incongruent melting points 283 and 369 K, and with decomposition enthalpies 18.5±2.2 and 23.0±1.5 kJ (mol of C70)-1, were formed from o-xylene solutions. Three ternary compositions with C60/C70 mole ratios of 3:1, 1:1 and 1:3 were scanned by DSC.
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    Journal of thermal analysis and calorimetry 52 (1998), S. 853-862 
    ISSN: 1572-8943
    Keywords: crystallization ; DSC ; melt spinning ; T-HR-T diagrams ; T-T-T diagrams
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The low-temperature parts of the temperature-heating rate-transformation (T-HR-T) and temperature-time transformation (T-T-T) diagrams were obtained for crystallization processes. A knowledge of the kinetic model governing crystallization is not needed because both transformation curves can be obtained from non-isothermal calorimetric experiments. The calorimetric study was performed by means of differential scanning calorimetry. The method was applied to analyse crystallization processes of Fe-Ni-based amorphous alloys prepared by melt spinning. The compositions studied were Fe40Ni40P14Si6, Fe40Ni40P10Si10 and Fe40Ni40P6Si14. A good concordance was observed between the experimental T-HR-T curves obtained by calculation and the experimental data, which verifies the reliability of the method. In the T-T-T diagrams, the agreement was good in process B1, while in processes A1 and C1 there are small differences that could be related to different crystallization products obtained in isothermal/non-isothermal experiments.
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    Journal of thermal analysis and calorimetry 54 (1998), S. 139-149 
    ISSN: 1572-8943
    Keywords: crystallization ; DSC ; melting curves ; peak-fitting ; polymorphism ; terfenadine
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Several samples of terfenadine prepared by crystallization from different solvents under different experimental conditions were studied. The DSC curves obtained at a heating rate of 1°C min−1 afforded the temperature of melting and the mole fractions of the components of each sample. Certain of the samples were composed of two solid phases mixed in molar ratios varying between nearly one and a single structural form. Three polymorphic forms were identified.
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  • 69
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    Journal of thermal analysis and calorimetry 54 (1998), S. 211-217 
    ISSN: 1572-8943
    Keywords: DSC ; fatty acids esters ; kinetics ; oxidation
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Oxidation of saturated fatty acids ethyl esters: laurate, myristate, palmitate and stearate was investigated by means of DSC techniques under isothermal and non-isothermal conditions. The activation energies of isothermal oxidation were similar to each other (112–123 kJ mol−1) and no influence of carbon length on the rate of oxidative decomposition was observed. Results obtained from non-isothermal experiments were similar only for the first stage of oxidation.
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    Journal of thermal analysis and calorimetry 54 (1998), S. 161-170 
    ISSN: 1572-8943
    Keywords: DSC ; glass transition ; side-chain liquid crystal polymer (SCLC)
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Bis [(ω-(4′-cyanobiphenyl)-4-yl)oxy-n-alkyl]norborn-5-ene-2,3-dicarboxylate was polymerised via ring opening metathesis polymerisation (ROMP). Two disubstituted polynorbornene derivatives both of cis configuration with different length of the side-chain were studied. Differential scanning calorimetry (DSC) was used to study the effect of thermal history on the assignment of the glass transition event associated with the biaxial orientation of a smectic phase. Glass transition temperatures, the change of isobaric specific heats at Tg and the enthalpies of isotropisation were calculated. The DSC traces only show the classic step-wise change in Tg in some cases, giving the evidence that the amorphous domains are constrained and highly restricted in movement due to the morphology developed as a result of the biaxial stretching. Based on the literature data of mono- and disubstituted polynorbornene derivatives and our calorimetric experiments, the shape of Tg dependence on number of (CH2) units is interpreted. The origin of this shape is discussed.
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    Journal of thermal analysis and calorimetry 52 (1998), S. 837-844 
    ISSN: 1572-8943
    Keywords: DSC ; high hydrostatic pressure ; plasma proteins ; spray-drying
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    Topics: Chemistry and Pharmacology
    Notes: Abstract One use of blood generated in abattoirs is to obtain dehydrated plasma which can be used as a functional ingredient in the preparation of foods. High hydrostatic pressure is a new technique for improvement of the sanitary quality of food products or their ingredients. The changes caused in the proteins by treatment can affect their functional properties, and differential scanning calorimetry DSC was therefore applied to detect possible conformational changes in the plasma proteins. The DSC results in the present study show that spray-drying does not appreciably affect the protein structure, but high-pressure treatment seems to have a denaturing effect.
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    Journal of thermal analysis and calorimetry 52 (1998), S. 903-914 
    ISSN: 1572-8943
    Keywords: Bi2Sr2CaCu2Oy〉 ; DSC ; electrophoretically deposited superconducting coatings ; high-temperature superconductors ; magnetic measurements ; Raman spectroscopy ; X-ray diffraction ; YBa2Cu3O7-x
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The optimum calcination and sintering conditions for the preparation of the desired phases with the proper stoichiometry of the bulk high-temperature superconductors YBa2Cu3O7-x (YBCO) and Bi2Sr2CaCu2Oy〉 (BSCCO) were investigated by differential scanning calorimetry. DSC analysis on the corresponding superconducting coatings, electrophoretically deposited, indicated that the sintering and annealing procedure was suitable for the production of stable, strong and adherent coatings. X-ray diffraction analysis, Raman spectroscopy and magnetic measurements confirmed the improved properties of the superconducting powders and coatings obtained.
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    Journal of thermal analysis and calorimetry 52 (1998), S. 871-879 
    ISSN: 1572-8943
    Keywords: burnability ; cement raw meal ; DSC
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    Topics: Chemistry and Pharmacology
    Notes: Abstract DSC was used in order to evaluate the reactivity of cement raw meal. Two groups of samples were studied: five industrial raw meals for ordinary Portland cement production, with similar compositions, but differences in granulometry; and five industrial raw meals for white Portland cement production, with similar granulometric features, but different compositions. The burnability indices of the samples were correlated with certain data obtained from the DSC curves. It is concluded that the DSC curve data, and especially the temperature and enthalpy effect of belite formation, are strongly correlated with the burnability of the cement raw meal. The temperature of belite formation is affected by chemical and mineralogical factors, while the enthalpy effect is additionally affected by the fineness of the raw meal.
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  • 74
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    Journal of thermal analysis and calorimetry 52 (1998), S. 145-155 
    ISSN: 1572-8943
    Keywords: acrylates ; DMA ; DSC ; epoxides ; radiation curing ; structure-property relationship ; TG ; thermal analysis
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Thermo-oxidative and thermo-mechanical stabilities of radiation-cured acrylates and epoxides were examined by TG, DMA and DSC. The polymeric trifunctional acrylates PETIA, TMPTA and THEIC displayed the highest temperatures of onset of degradation. The high crosslinking density of the films resulted in an almost temperature-independent complex E-modulus, as measured by DMA. With increasing degree of ethoxylation or propoxylation of the monomers, decreases in thermal stability and strength were found. For difunctional polymeric acrylates and epoxides, the glass transition temperature was measured. The average degree of curing of UV-cured epoxy films can be determined from the temperature of the maximum in the loss modulus (E″max.
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  • 75
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    Keywords: DSC ; infrared spectrometry ; oxidation ; polyethylenes ; thermal analysis
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The oxidation of pure and recycled polyethylene samples was studied by thermal analysis (DTA-TG-DSC): presence of two exothermic peaks and mass loss. The thermo-oxidation products, containing C-O and C=O links, were identified by IR spectrometry and GC-MS spectrometry. The oxidation is easier from low to high density polyethylene.
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    Journal of thermal analysis and calorimetry 53 (1998), S. 659-669 
    ISSN: 1572-8943
    Keywords: DSC ; heat capacity ; high temperature
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Scanning calorimetric methods permit determination of heat capacities at high temperatures up to 1600°C. For disk systems with power compensation application limits are in order of 700°C, and for cylindrical systems with electrical calibration up to 1000°C. For the high temperature range above 1000°C DSC plates and a cylindrical calorimetric systems based on the CALVET principle ('MULTI HTC’) are known. For cylindrical calorimetric systems the precision of the Cp data is between 2 and 5% even at high temperatures without any requirements on the kind and shape of samples. These results are better than data provided by DSC plate systems.
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    Journal of thermal analysis and calorimetry 52 (1998), S. 697-703 
    ISSN: 1572-8943
    Keywords: DSC ; novolac resin ; thermogravimetry ; X-ray diffraction
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The thermal stability of p-cresol novolac resin was studied by means of DSC, X-ray diffraction, thermogravimetry and SEC investigations. After 30 thermal cycles in which the same sample was heated, cooled and heated again, without attainment of the temperature of degradation at any time in the experiment, important structural modifications are observed. At the end of the experiments, the resin, which is initially highly crystalline, exhibits all the characteristics of a semi-crystalline material.
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    Journal of thermal analysis and calorimetry 53 (1998), S. 123-131 
    ISSN: 1572-8943
    Keywords: chiral molecule isomorphisme ; DSC ; phase diagram
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    Topics: Chemistry and Pharmacology
    Notes: Abstract We have shown that efaxoran hydrochloride and efaxoran hydrobromide form solid solution over the entire range of compositions. The small values of enthalpy of mixing indicate that the system is close to ideality. Consequently, Oonk's method was used for its modelling, assuming that the liquid phase is ideal and the departure of the solid phase from ideality was expressed by the excess free enthalpy gE. The results obtained agreed with experience.
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    Journal of thermal analysis and calorimetry 53 (1998), S. 317-322 
    ISSN: 1572-8943
    Keywords: α-phenylcinnamic acid ; DSC ; polymorphic transitions ; stereoisomers
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Polymorphic transitions of α-phenylcinnamic acid stereoisomers crystallized from various solvents (CHCl3, ethanol, diethyl ether), precipitated with different acids (acetic acid or HCl) or sublimed have been studied by differential scanning calorimetry (DSC). Measurements were also supplemented by powder X-ray diffractometry (XRD). Polymorphic transitions were not found for any of the E isomer samples irrespective of the method of treatment. However, in heating-cooling cycles reversible transitions could be detected for the Z isomer. On heating an exothermic peak was registered on samples sublimed, crystallized from ethanol or diethyl ether before melting, while samples precipitated by HCl or crystallized from chloroform exhibited more complex transitions. Here, endothermic effects were also observed. Enthalpy values for transformations (either for melting or polymorphic and other transitions) are also given.
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    Journal of thermal analysis and calorimetry 53 (1998), S. 333-335 
    ISSN: 1572-8943
    Keywords: compatibility ; DSC ; liquid crystal
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The phase transition curves of a multi-component TN liquid crystal mixture (TN 88-1) and a multi-component cholesteric liquid crystal mixture (Ch 88-2) were plotted by using a differential scanning calorimeter. The phase transition temperature and phase transition heat were obtained from the DSC curves. The results show that the components of TN 88-1 are compatible and they can form a stable mixture with CB 15 chiral liquid crystal. The components of Ch 88-2 are not compatible and Poly (MMA-BMA) can greatly improve their compatibility.
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    Journal of thermal analysis and calorimetry 54 (1998), S. 203-210 
    ISSN: 1572-8943
    Keywords: antioxidants ; DSC ; thermoxidation
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Thermoxidation of linolenic acid inhibited by addition of 2,6-di-t-butyl-4-methylphenol and 2,4,6-trimethylphenol at various concentrations was investigated. The measurements were carried out under non-isothermal conditions in an atmosphere of oxygen. DSC curves permitted the determination of onset point and maximum points of the peaks. The influence of inhibitor concentration on temperature of the start of oxidation was noticed. However, no significant changes in temperatures of the maximum heat flow was observed. Measurements and calculations described in this report prove that the assessment of the antioxidant activity of chain-breaking inhibitors can be performed only from the onset temperatures. Calculations of the activation energy of inhibited linolenic acid thermoxidation were performed in order to elucidate the antioxidant activity of the phenolic compounds.
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    Journal of thermal analysis and calorimetry 53 (1998), S. 697-709 
    ISSN: 1572-8943
    Keywords: DSC ; efaroxan hydrochloride ; phase diagram ; racemic compound
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The phase diagram of R(+)-S(-) efaroxan hydrochloride (Tfus.(R)=245.1±0.3°C. ΔHfus.(R)=119.6±3.0 J g-1) shows a racemic compound. The melting temperature and melting enthalpy of the compound are: Tfus.(RS)=247.8±0.2°C and ΔHfus. (RS)=124.6±2.4 J g-1. A solid ↔ solid transformation takes place at Ttrs.=180±1°C, ΔHtrs.=15.0±0.4 J g-1. This transition is observed between 3 and 97% R(+). The stability of the racemic compound already established in a previous study was confirmed by the value of Petterson's coefficient (i=1.19). The two eutectic positions at 20 and 80% R(+) that define the range over which the racemic compound is found, exclude the use of resolution methods by preferential crystallization.
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    Journal of thermal analysis and calorimetry 53 (1998), S. 685-695 
    ISSN: 1572-8943
    Keywords: DSC ; isothermal microcalorimetry ; specific heat capacity ; tissue equivalent liquid
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The specific heat capacities (cp) for the brain and muscle equivalent liquids were determined with isothermal heat conduction microcalorimetry (IMC) and differential scanning calorimetry (DSC). IMC was found to afford an accurate technique to measure cp for solid and liquid samples, when an appropriate reference is employed. The accuracy of obtained cp values was estimated to be better than 0.7% with the equivalent liquids. Intercomparison with a conventional isoperibolic calorimeter showed an excellent agreement within the estimated uncertainty of the isoperibolic calorimeter (±3%). Additionally, suitability of different kinds of IMC sample vessels was tested, and the standard electrical calibration procedure of IMC was evaluated through the determination of cp with and without a reference material.
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    Journal of thermal analysis and calorimetry 54 (1998), S. 825-835 
    ISSN: 1572-8943
    Keywords: Al alloy ; DSC ; hardness measurement ; peak-aging ; precipitation
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    Topics: Chemistry and Pharmacology
    Notes: Abstract The precipitation of a supersaturated 6061 Al alloy reinforced with 10% SiCpwas monitored by using a DSC technique. DSC thermal curves were used to predict peak-aging temperatures and durations. The activation energies for precipitation of the β″ phase were found to increase with elevation of the solution temperature from 510 to 600°C, and hence the peak-aging temperature and duration also increased. Microstructural examination revealed an increase in grain size when a high solution temperature was applied. To compare predicted peak-aging temperatures and durations, hardness measurements were carried out after artificial aging. The studies revealed that peak-aging hardening was obtained when the aging temperatures and durations corresponded to about 95% to 97% precipitation of β″ phase from conversion plots.
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    Journal of thermal analysis and calorimetry 54 (1998), S. 891-899 
    ISSN: 1572-8943
    Keywords: DSC ; DTG ; levynite ; TG ; thermal analysis ; QTMD
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract DSC, TG and quadrupole mass spectrometer data concerning methylquinuclidinium iodide (MeQ1), dried precursor gel, and crystalline levyne-type zeolite are discussed together with the thermal degradation of MeQ1 mixed with single inorganic components of the gel. It is shown that MeQ+ions play a role in the organization of the gel structure.
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  • 86
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    Journal of thermal analysis and calorimetry 54 (1998), S. 477-499 
    ISSN: 1572-8943
    Keywords: base-line heat capacity ; crystallization ; curing ; deconvolution ; DSC ; excess heat capacity ; glass-transition ; linear response theory ; melting ; polymers ; regime ; TMDSC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Temperature-modulated differential scanning calorimetry (TMDSC) has recently been introduced as a promising calorimetric technique. However, the added value of TMDSC in practice is still not very obvious, in particular with respect to crystallization and melting. An important reason is that the evaluation is less transparent than in case of other dynamic techniques since in TMDSC the response is also based on temperature. Moreover, the temperature program applied is very critical. In this paper an overview is given of the different aspects of TMDSC using a general theoretical description based on the full heat capacity formulation. It is demonstrated that processes studied with the aid of TMDSC can simply be classified into three distinct regimes, depending on the time scale and the susceptibility of the process to the temperature modulation.
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  • 87
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    Journal of thermal analysis and calorimetry 54 (1998), S. 605-622 
    ISSN: 1572-8943
    Keywords: DSC ; MDSC ; polyamide 12 ; poly(p-phenylene sulfide) ; poly(vinylidene fluoride) ; reorganization ; TMDSC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Although reorganization in metastable polymeric crystals has been recognized for over 30 years, the effect of molecular weight on the reorganization process has not been widely investigated. In this work three polymeric systems were studied: poly(vinylidene fluoride), polyamide 12, and poly(p-phenylene sulfide). For the polymers investigated, the lowest molecular weight sample was found to reorganize the most and, conversely, the highest molecular weight sample was found to reorganize the least. Comparisons of each system show that independent of molecular weight the reorganization rates among the three systems could be differentiated with the polyamide showing the greatest reorganization and the poly(phenylene sulfide) the least. Both conventional differential scanning calorimetry (DSC) and temperature-modulated DSC (TMDSC) were used in this study to investigate the reorganization process.
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  • 88
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    Journal of thermal analysis and calorimetry 54 (1998), S. 741-752 
    ISSN: 1572-8943
    Keywords: butyl rubber ; confinement ; DSC ; thermoporosimetry ; water crystallization ; water droplet
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract It is shown that for porous systems filled with a solvent, if the temperature domains of crystallization and melting of the solvent are well separated, DSC technique, combined with suitably chosen thermal cycles, provides crystallization and melting curves which are independent of a) the mass of the material, b) the thermal contact between DSC pan and material and c) the thermal conductivity of the material. This method called DSC fractionation is applied to butyl rubber containing small water nodules. Thermoporosimetry is then applied to get the size distribution of mesoscopic solvent droplets.
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  • 89
    ISSN: 1572-882X
    Keywords: cellulose alkyl esters ; poly(∈-caprolactone) ; blends ; miscibility ; DSC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Abstract Cellulose alkyl esters, CELL- OCOCnH2n+1(n = 1 ∼ 6), were synthesized by a homogeneous reaction of cotton cellulose with different acyl chlorides in N,N-dimethylacetamide--lithium chloride solution. The miscibility of the esterified celluloses with poly(∈-caprolactone) (PCL) was investigated, mainly through thermal analysis by differential scanning calorimetry (DSC). A polymer pair, cellulose butyrate (CB)/PCL, showed the highest miscibility of all the binary blends examined here; this is usual when relatively high-substituted esters (DS ≥ 2.0) are used as the respective component. The butyl ester derivatives with DS ≤ 1.5 showed poor miscibility with PCL
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  • 90
    ISSN: 1432-1017
    Keywords: Key words Phosphatidylcholine ; Phosphatidylglycerol ; DSC ; Phase diagrams ; Miscibility ; Nonideality parameter
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Physics
    Notes: Abstract The miscibility of phosphatidylcholine (PC) and phosphatidylglycerol (PG) with different chain lengths (n = 14, 16) was examined by differential scanning calorimetry (DSC) at pH 2 and pH 7. The determination of the coexistence curves of the phase diagrams was performed using a new procedure, namely the direct simulation of the heat capacity curves as described recently (Johann et al. 1996, Garidel et al. 1997). From the simulations of the heat capacity curves first estimates for the nonideality parameters for nonideal mixing as a function of composition were obtained and phase diagrams were constructed using temperatures for the onset and offset of melting which were corrected for the broadening effect caused by a decrease in cooperativity of the transition. In most cases, the composition dependence of the nonideality parameters indicated nonsymmetric mixing behavior. The phase diagrams were further refined by simulations of the coexisting curves using a four-parameter model to account for nonideal and nonsymmetric mixing in the gel as well as in the liquid-crystalline phase. The mixing behavior of the systems was analyzed as a function of pH and chain length difference to elucidate the effect of these two parameters on the shape of the phase diagrams. At pH 7 the phase boundaries are much closer together and a narrower coexistence range is obtained compared to the corresponding phase diagrams at pH 2. For DPPC/DMPG at pH 2, the shape of the phase diagram and the strongly positive nonideality parameter ρ 1 for the liquid-crystalline phase indicates an upper azeotropic point. This indicates an unusual behavior of the system, namely more pronounced clustering of like molecules in the liquid-crystalline phase compared to the gel phase.
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  • 91
    ISSN: 1572-8943
    Keywords: DSC ; polyethylenes ; X-ray
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract In thermal analysis polyethylenes can be characterized by their melting temperature. With the polyethylene mixtures studied, we obtained the best results during solidification. Crystallization temperature decreased in the order: high density PE, low density PE linear, radical low density PE. Calorimetric measurement of crystallization enthalpies allowed the determination of the composition of each of the polyethylenes, in regenerated and recycled mixtures in relation with the frame of the plastic waste valorisation process. The rate of crystallization obtained from X-ray diffraction spectra of these polymers is function of their volumic mass. A good agreement has been observed between these two techniques.
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  • 92
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    Journal of thermal analysis and calorimetry 49 (1997), S. 79-85 
    ISSN: 1572-8943
    Keywords: cross-linking degree ; DSC ; enthalpy relaxation ; epoxy resins ; physical aging ; reactive diluent
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Structural relaxation in different epoxy-anhydride and epoxy-diamine resins has been investigated by differential scanning calorimetry using annealing and cooling rate experiments. The annealing experiments lead to the determination of enthalpy loss,δH, at an equivalent annealing temperatureT a=T g-20, and for periods of annealing time, ta, between 1 h and 4 months. The variation ofδH with logta, defines a relaxation rate per decade,rrpd, which is very sensitive to changes of the epoxy network. The cooling rate experiments allow the determination of the apparent activation energy,δh *. The effect of the degree of crosslinking, the addition of a reactive diluent, which acts as flexibilizer, and the length of cross-link onrrpd and δh* was studied.
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  • 93
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    Journal of thermal analysis and calorimetry 49 (1997), S. 149-154 
    ISSN: 1572-8943
    Keywords: DSC ; heterogeneity in polymer network ; poly(methacrylic acid)-net-poly(oxytetramethylene) ; thermogravimetry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract TG and DSC were carried out on PMAA-net-POTM in order to elucidate the relation between the heterogeneity and the thermal changes; moreover, TG and DSC were carried out on PPOTMDM and PMAA to compare the results. The onset temperature in the last stage in the TG curve of PMAA-net-POTM increases as the concentrations of DMF and POTMDM in the polymerization decrease. This is explained in terms of plasticizers effects. A single peak due to fusion of POTM chains appears in the DSC curves of most copolymers. However, it is not seen in the DSC curves of copolymers with high heterogeneity. This is explained in terms of the freezing of POTM chains by frozen heterogeneous moieties.
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  • 94
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    Journal of thermal analysis and calorimetry 49 (1997), S. 177-182 
    ISSN: 1572-8943
    Keywords: bismaleimide resin ; CTBN ; curing behaviour ; DSC ; TG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Bismaleimide resin (Compimide 353) was modified with the liquid elastomer carboxyl-terminated acrylonitrile butadiene (CTBN). The prereaction synthesis and curing of the CTBN-bismaleimide resin is discussed. The structure of the modified resin was identified by IR and NMR spectroscopy. The basic curing mechanism is also discussed. DSC and TG were used to study the curing behaviour and kinetic parameters, viz. the order of reaction, energy of activation and preexponential factor. Adhesive properties such as lap shear strength and peel strength at room temperature and elevated temperature were evaluated and are discussed.
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  • 95
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    Journal of thermal analysis and calorimetry 49 (1997), S. 343-349 
    ISSN: 1572-8943
    Keywords: double melting peak ; DSC ; fiber ; polyethylene
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The multiple melting peaks observed on differential scanning calorimetry (DSC) of ultrahigh molar-mass polyethylene fibers (UHMMPE) are analyzed as a function of sample mass. Using modern DSC capable of recognizing single fibers of microgram size, it is shown that the multiple peaks are in part or completely due to sample packing. Loosely packed fibers fill the entire volume of the pan with rather large thermal resistance to heat flow. On melting, the fibers contract and flow to collect ultimately at the bottom of the pan. This process seems to be able to cause an artifact of multistage melting dependent on the properties of the fibers. A method is proposed to greatly reduce, or even eliminate, errors of this type. The crucial elements of the analysis of melting behavior and melting temperature are decreasing the sample size and packing the individual fibers in a proper geometry, or to introduce inert media to enhance heat transport.
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  • 96
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    Journal of thermal analysis and calorimetry 49 (1997), S. 399-405 
    ISSN: 1572-8943
    Keywords: DSC ; polyimide fiber ; TMA ; TG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A commercially available polyimide fiber was investigated as a possible precursor for the formation of carbon fibers. The thermal response of the fiber was thoroughly investigated using DSC, TMA and TG. These responses were dependent on the atmosphere and tension during scanning. The fiber was stabilized at high temperatures both in inert and oxidative environments and the effect of these stabilization treatments on the structure and properties of the fiber was carefully followed. During heating, the fiber showed shrinkage tendency at small tensions, but at higher tensions the fibers could be stretched. Among the two environments investigated, air was more effective than nitrogen in getting a more stable fiber.
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  • 97
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    Journal of thermal analysis and calorimetry 49 (1997), S. 407-415 
    ISSN: 1572-8943
    Keywords: compatibility ; covulcanization ; derivative heat flow (δW/δT) ; DSC ; microheterogeneous
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Derivative heat flow curves give much more information about the phase heterogeneity of binary blends composed of NR, SBR and BR elastomers thanT g. In blend compositions, the areas under the derivative heat flow curves appear to be an additive function of the concentration of elastomers in the case of incompatible blends (NR/BR, NR/SBR). They are less than additive for either a partially compatible blend (uncured SBR/BR) or a compatible blend (covulcanized SBR/BR). In the case of 60/40 SBR/BR blends, a DSC (T 0.5) reveals a singleT g, in conformity with the earlier investigators, whereas the derivative heat flow curve shows two peaks (T p) indicating incomplete homogenization of the phases. This is a new observation not mentioned in the published literature. Thus, derivative heat flow traces are likely to provide a unique tool to determine compatibility of elastomers. The study also reveals the importance of sample contact with the DSC pan in quantitative determinations.
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  • 98
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    Journal of thermal analysis and calorimetry 49 (1997), S. 449-454 
    ISSN: 1572-8943
    Keywords: DSC ; network ; polyethylene ; turbidimetry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Semicrystalline polymers are made of a crystalline phase and of an amorphous phase. Recently, NMR, Raman and FTIR experiments have identified a third phase comprised of defects such as tie-molecules, in the organization of chains. Our investigation of physical gels has led us to believe that by following the heat flow in a very slow temperature ramp (0.05 K min−1), phasechanges, unnoticed in the usual fast ramp, could be detected. These are associated to a physical network strained in the temperature ramp. In order to obtain more information on the network phase, the polymer has been crosslinked The characteristics obtained by slow calorimetry and turbidimetry of the original and modified materials are compared.
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  • 99
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    Journal of thermal analysis and calorimetry 49 (1997), S. 483-490 
    ISSN: 1572-8943
    Keywords: carboxyterminated polybutadiene ; DSC ; DMA ; SEM ; toughened epoxy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A new type of toughened epoxy polymer based on epoxy cresol novolac resin (ECN) and carboxy terminated polybutadiene (CTPB) liquid functional rubber has been studied. ECN has been synthesized in the laboratory and CTPB used was also of indigenised origin. Rubber modified epoxies were characterized with the help of differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA) and scanning electron microscopy (SEM) techniques.
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  • 100
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    Journal of thermal analysis and calorimetry 49 (1997), S. 477-481 
    ISSN: 1572-8943
    Keywords: DSC ; EVA blends ; phenolic resin ; TG-DTG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The properties of polymeric blends originate from the synergistic association of their components. In this investigation, phenolic resins obtained by the reaction of cashew-nut shell liquid (CNSL) and aldehyde are used in several applications. Mixtures of CNSL with industrial reject ethylene-co-vinyl acetate (EVA reject) were prepared with an EVA reject content up to 70%. The thermal compatibility and stability were evaluated by means of thermogravimetry (TG), derivative thermogravimetry (DTG) and differential scanning calorimetry (DSC). For blends containing a high percentage of EVA reject, the TG curves clearly show two decomposition stages, one at 350
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