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  • Articles  (233)
  • kinetics  (140)
  • DSC  (100)
  • Springer  (233)
  • American Association for the Advancement of Science
  • American Meteorological Society
  • 1995-1999  (233)
  • 1990-1994
  • 1999  (119)
  • 1996  (114)
  • 1
    Electronic Resource
    Electronic Resource
    Kinetics and mechanism of MnO2 dissolution in H2SO4 in the presence of pyrite (1999)
    Springer
    Journal of applied electrochemistry 29 (1999), S. 191-200 
    Details
    ISSN: 1572-8838
    Keywords: cyclic redox reaction ; dissolution ; kinetics ; manganese dioxide ; mechanism ; pyrite
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Electrical Engineering, Measurement and Control Technology
    Notes: Abstract This paper describes a study of the kinetics and mechanism of MnO2 dissolution in H2SO4 in the presence of pyrite through leaching and electrochemical parameters. Manganese(iv) was found to dissolve mainly through reduction by the ferrous ion generated during oxidation of pyrite by the ferric ion. The oxidation which is slower and rate controlling may proceed through two different reactions, one producing S0 and the other SO42−. Manganese dissolution runs at the same rate as that of pyrite oxidation by maintaining ferrous ion concentration at a much lower level than that of ferric. Kinetic equations based on corrosion coupling principles are developed to explain the observed leaching behaviour.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1003490810114
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  • 2
    Electronic Resource
    Electronic Resource
    Frequency response analysis of a closed diffusion cell with two resonators (1996)
    Springer
    Adsorption 2 (1996), S. 265-277 
    Details
    ISSN: 1572-8757
    Keywords: frequency response ; diffusion cell ; kinetics ; diffusion ; heat effects
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Physics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Abstract This paper deals with frequency response (FR) analysis of a closed diffusion cell system with two resonators, that is both the LHS and RHS volumes are modulated. The analysis is made for a homogeneous particle described by a single effective diffusivity as well as a biporous pellet described by macropore and micropore diffusions. It is shown that if the perturbation of the volume of the reservoir #2 is lagged behind that of the reservoir #1 by 3π/2, the pressure response in reservoir #1 is significantly enhanced with larger amplitude as well as phase angle. When the perturbations of the two reservoirs are out of phase, the heat effect is reduced and can become insignificant when the two perturbations are completely out of phase (ψ = π). Under such a condition, the pressure difference between the two reservoirs could be doubled. In the case of biporous pellets, it is shown that the FR behaviours obtained for micropore diffusion control and macropore diffusion control are well distinguished. In the former case, the FR system reduces to a traditional batch adsorber one while in the latter case, the FR behaviour is the same as for a two resonator system with homogeneous particles. This difference can be used for the discrimination of micropore and macropore diffusion processes.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00879541
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  • 3
    Electronic Resource
    Electronic Resource
    Factors affecting bioleaching kinetics of sulfide ores using acidophilic micro-organisms (1999)
    Springer
    BioMetals 12 (1999), S. 1-10 
    Details
    ISSN: 1572-8773
    Keywords: acidophilic ; strain ; oxidation ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Abstract Recovery of metal values from sulfide ores by use of acidophilic microorganisms is gaining importance. A number of commercial/pilot plants are setup to find out the techno-economic feasibility of the overall process. The main drawback in the process is the slow kinetics of dissolution of metal values from the sulfide ores. To make the technology e attractive the kinetics should be improved considerably. There are various factors which determine the overall kinetics such as bacterial activity and concentration, iron and sulfur oxidation, oxygen consumption, reactor design and nature of ore. A brief review has been made dealing with the above parameters
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1009228210654
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  • 4
    Electronic Resource
    Electronic Resource
    The dissociation kinetics of H2S over an alumina supported Co-Mo sulphide catalyst (1996)
    Springer
    Catalysis letters 37 (1996), S. 167-172 
    Details
    ISSN: 1572-879X
    Keywords: dissociation ; kinetics ; Co-Mo sulphide ; H2S
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract In this study, a high surface area 4Co∶6Mo∶100γ-Al2O3 sulphide prepared using precipitation from homogeneous solution (PFHS) has been used for the catalytic splitting of hydrogen sulphide into H2 and elemental sulphur. The activity of this new formulation was significantly better than previously reported recipes. Kinetic data collected over a wide range of H2S partial pressures between 883 and 983 K revealed that, although the decomposition followed a first-order law, a mechanism involving H2S adsorption on co-ordinative unsaturation sites of the Co-Mo sulphide catalyst gave a Langmuir-Hinshelwood rate expression that yielded satisfactory model parameters. In particular, the scission of the surface H-S bond appeared to be the rate determining step.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00807749
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  • 5
    Electronic Resource
    Electronic Resource
    Effect of potassium on the high pressure kinetics of ammonia synthesis over fused iron catalyst (1996)
    Springer
    Catalysis letters 37 (1996), S. 173-179 
    Details
    ISSN: 1572-879X
    Keywords: ammonia synthesis ; iron catalysts ; potassium promotion ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Measurements were performed of reaction rate in the process of ammonia synthesis (T=370–470°C) on doubly promoted (DP) (Al2O3, CaO) and triply promoted (TP) (K2O, Al2O3, CaO) iron catalysts. The latter were obtained by impregnation of the reduced and subsequently passivated DP precursors with alcoholic solution of KOH. The studies were carried out under high total pressure (10 MPa) in a wide range of ammonia partial pressure in the gas phase: from 0.25 to about 7 bar. The results are shown to be authoritative for the so-called kinetic regime. The effect of the presence of K+ cations in the catalyst was the stronger, as the temperature of the reaction was the lower and, in particular, the ammonia pressure in the gas phase the higher. The obtained results are in good accordance with the results of Somorjai's studies on activity of iron single crystal surfaces both clean and covered with (K+O) adlayer.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00807750
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  • 6
    Electronic Resource
    Electronic Resource
    Prediction of paper permanence by accelerated aging II. Comparison of the predictions with natural aging results (1996)
    Springer
    Cellulose 3 (1996), S. 269-279 
    Details
    ISSN: 1572-882X
    Keywords: accelerated tests ; aging tests ; cellulose degradation ; durability ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Abstract Accelerated aging tests are credible and useful to predict paper permanence only if such tests can be shown to correlate with natural aging. In the first part of this study, a kinetic model was developed based on the accelerated aging results. In this report, we have shown that this kinetic model can indeed predict the natural aging results of lignin-free sheets with a statistical confidence. This is the first quantitative comparison of accelerated aging with natural aging.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02228806
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  • 7
    Electronic Resource
    Electronic Resource
    Prediction of paper permanence by accelerated aging I. Kinetic analysis of the aging process (1996)
    Springer
    Cellulose 3 (1996), S. 243-267 
    Details
    ISSN: 1572-882X
    Keywords: aging tests ; cellulose degradation ; durability ; kinetics ; paper properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Abstract The validity of accelerated aging tests to predict and rank papers on their permanence has been under question, preventing the development of performance-based standards for permanent paper. We conducted a general kinetic analysis to investigate the aging process of paper. A general kinetic model is proposed to describe the depolymerization of cellulose. Experimentally it was shown that in the case of aging, cellulose degradation follows classic first-order kinetics as a special case of our general kinetic model. The Arrhenius equation was critically re-examined for the case of a multiple reaction system. It was shown analytically that the Arrhenius equation is still applicable when certain conditions are met. This was convincingly supported by experimental results. We also analysed the dependence of the degradation rate on the moisture content and hydrogen ion concentration. By conducting systematic experiments on these two factors, a general and quantitative relationship was established to explain the contribution of each factor and their interactions. Finally, based on this kinetic analysis, the effects of storage conditions on the life expectancy of paper were estimated.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02228805
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  • 8
    Electronic Resource
    Electronic Resource
    Study on thermal transitions of toluene diisocyanate-based polyurethane elastomers with poly (tetramethylene oxide) as the soft segment by TSC/RMA, DSC and DMA thermal analyzers (1999)
    Springer
    Journal of polymer research 6 (1999), S. 67-78 
    Details
    ISSN: 1572-8935
    Keywords: TDI-based polyurethane elastomers ; Tg ; Tglobal transition ; DSC ; TSC/RMA ; DMA
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Abstract Thermal transitions of TDI-based polyurethane elastomers with PTMO as the soft segment were characterized by the depolarization technique in TSC and by using with the thermal windowing technique on selected specimens in the RMA measurements. Results indicate that the broadened thermal transition in the glass transition region as observed in the DSC thermogram is related to the combined Tg transition and the Tglobal transition in the TSC spectrum. This Tglobal transition is associated with the macromolecular property as detected by tan δ in DMA measurement. The increase in the Tg with a high NCO content may be explained by the structural modification found on the urethanic chain with the additional linkage of the hard segment that affects the cooperative motion of the molecular chain. Data measured from DSC, TSC/RMA and DMA with simulated DEA and wide angle X-ray data are presented for the characterization of the polyurethanes. The RMA measurement leads to a compensation search on Tg transition and provides pertinent thermokinetic data that correlates the NCO content with changes in enthalpy and entropy on the relaxation behaviors in the Tg transition of polyurethane elastomers.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/s10965-006-0073-4
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  • 9
    Electronic Resource
    Electronic Resource
    Degradation of Cellulosic Materials Under the Alkaline Conditions of a Cementitious Repository for Low- and Intermediate-Level Radioactive Waste. II. Degradation Kinetics (1999)
    Springer
    Journal of polymers and the environment 7 (1999), S. 41-51 
    Details
    ISSN: 1572-8900
    Keywords: Cellulose ; alkaline degradation ; peeling off ; degree of polymerization ; kinetics ; (gluco)isosaccharinic acid
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Energy, Environment Protection, Nuclear Power Engineering , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract The degradation of cellulosic materials, differing mainly in the degree of polymerization and the number of reducing end groups, was studied under the alkaline conditions similar to those existing in a cementitious repository for low- and intermediate-level radioactive waste (pH 13.3, T = 25°C). The kinetics of alkaline degradation (peeling-off reaction) were studied and the data analyzed by the model of Haas et al. [13]. The observed kinetic parameters for the propagation reaction and overall stopping reaction were compared with literature data. Although measured under different experimental conditions, literature data and data from this study show a consistent picture. Differences in the extent of degradation observed for the different cellulosic materials could be satisfactorily explained by differences in reducing end group content and, consequently, by differences in the degrees of polymerization. Besides the number of reducing end groups, the degree of amorphousness also plays an important role. The main degradation products formed under the experimental conditions used are α- and β-(gluco)isosaccharinic acid. This is in agreement with many other studies on alkaline degradation of cellulose. The two isomers are formed in roughly equal amounts.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1021894102937
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  • 10
    Electronic Resource
    Electronic Resource
    Sorption Equilibria and Kinetics of Hydrocarbons onto Activated Carbon Samples Having Different Micropore Size Distributions (1999)
    Springer
    Adsorption 5 (1999), S. 25-37 
    Details
    ISSN: 1572-8757
    Keywords: micropore size distribution ; activated carbon ; adsorption ; desorption ; equilibrium ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Physics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Abstract This paper deals with the prediction of adsorption equilibrium and kinetics of hydrocarbons onto activated carbon samples having different micropore size distribution (MPSD). The microporous structure of activated carbon is characterised by the distribution of slit-shaped micropores, which is assumed to be the sole source of surface heterogeneity. The interaction between adsorbate molecule and pore walls is described by the Lennard-Jones potential theory. Different adsorbates have access to different pore size range of activated carbon due to the size exclusion, a phenomenon could have a significant influence on both multicomponent equilibria and kinetics. Activated carbons with three different MPSDs are studied with ethane and propane as the two model adsorbates. The Heterogeneous Macropore Surface Diffusion model (HMSD) is employed to simulate adsorption kinetics. The simulation results show that the MPSD is an important factor affecting both the multicomponent equilibria and kinetics.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1026481704926
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  • 11
    Electronic Resource
    Electronic Resource
    Furfural hydrogenation over carbon‐supported copper (1999)
    Springer
    Catalysis letters 60 (1999), S. 51-57 
    Details
    ISSN: 1572-879X
    Keywords: furfural hydrogenation ; Cu/carbon catalysts ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Furfural hydrogenation over copper dispersed on three forms of carbon – activated carbon, diamond and graphitized fibers – were studied. Only hydrogenation of the C=O bond to form either furfuryl alcohol or 2‐methyl furan occurred at temperatures from 473 to 573 K. Reduction at 573 K gave the most active catalysts, all three catalysts had activation energies of 16 kcal/mol, and turnover frequencies were 0.018–0.032 s-1 based on the number of Cu0 + Cu+ sites, which were counted by N2O adsorption at 363 K and CO adsorption at 300 K, respectively. The Cu/activated carbon catalyst showed no deactivation during 10 h on stream, in contrast to the other two catalysts. A simple Langmuir–Hinshelwood model invoking two types of sites was able to fit all kinetic data quite satisfactorily, thus it was consistent with the presence of both Cu0 and Cu+ sites.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1019090520407
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  • 12
    Electronic Resource
    Electronic Resource
    Study of the ammonia decomposition over iron catalysts (1999)
    Springer
    Catalysis letters 60 (1999), S. 167-171 
    Details
    ISSN: 1572-879X
    Keywords: ammonia decomposition ; iron catalyst ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The decomposition of ammonia is a reaction associated with the process of the nitriding of metals. The kinetics of the ammonia decomposition on iron catalysts has been studied using a differential reactor with internal mixing. The balance between the inlet and outlet ammonia quantity has been used to determine the degree of conversion. The rate of ammonia decomposition could be described by the following expression: r = k0 exp (Ea/RT)pNH3. The activation energy of the ammonia decomposition process has been found for samples with potassium as E a= 96 kJ/mol, for samples without potassium as E a= 87 kJ/mol.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1019007024041
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  • 13
    Electronic Resource
    Electronic Resource
    Pure and Binary Gas Adsorption Equilibria and Kinetics of Methane and Nitrogen on 4A Zeolite by Isotope Exchange Technique (1999)
    Springer
    Adsorption 5 (1999), S. 145-158 
    Details
    ISSN: 1572-8757
    Keywords: kinetics ; isotope-exchange ; nitrogen ; adsorption ; methane ; zeolite ; equilibria
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Physics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Abstract The Isotope Exchange Technique (IET) was used to simultaneously measure pure and binary gas adsorption equilibria and kinetics (self-diffusivities) of CH4 and N2 on pelletized 4A zeolite. The experiment was carried out isothermally without disturbing the adsorbed phase. CH4 was selectively adsorbed over N2 by the zeolite because of its higher polarizability. The multi-site Langmuir model described the pure gas and binary adsorption equilibria fairly well at three different temperatures. The selectivity of adsorption of CH4 over N2 increased with increasing pressure at constant gas phase composition and temperature. This curious behavior was caused by the differences in the sizes of the adsorbates. The diffusion of CH4 and N2 into the zeolite was an activated process and the Fickian diffusion model described the uptake of both pure gases and their mixtures. The self-diffusivity of N2 was an order of magnitude larger than that for CH4. The pure gas self-diffusivities for both components were constants over a large range of surface coverages (0 〈 θ 〈 0.5). The self-diffusivities of CH4 and N2 from their binary mixtures were not affected by the presence of each other, compared to their pure gas self-diffusivities at identical surface coverages.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1008917308002
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  • 14
    Electronic Resource
    Electronic Resource
    Non-uniform surface kinetics with two types of sites: the case of ethanol oxidation on molybdenum oxide (1996)
    Springer
    Catalysis letters 39 (1996), S. 67-71 
    Details
    ISSN: 1572-879X
    Keywords: non-uniform surface ; kinetics ; ethanol ; oxidation ; molybdenum oxide
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Temkin's theory of rates of catalytic reactions on non-uniform surfaces is extended to the MoO3-catalyzed oxidation of ethanol to acetaldehyde. Two types of sites are assumed to be present, an oxygen atom site that can be modeled with uniform properties and a metal atom site characterized by non-uniform properties both for ethanol chemisorption to an ethoxide intermediate and the conversion of this intermediate to acetaldehyde. The rate-limiting step is the cleavage of a C-H bond in the absorbed ethoxide intermediate. Non-uniform surface kinetics leads to a kinetic rate expression of the form $$v = kP_{C_2 H_5 OH}^{1 - m} P_{O_2 }^{(1 - m)/4} P_{H_2 O}^{ - (1 - m)/2} $$ . Such a rate expression, withm=0.14, is shown to provide a good fit to kinetic data for the selective oxidation of ethanol on a silica supported molybdenum oxide catalyst.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00813732
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  • 15
    Electronic Resource
    Electronic Resource
    Platinum particle size effect on the oxidative dehydrogenation of aqueous ethanol (1996)
    Springer
    Catalysis letters 36 (1996), S. 31-36 
    Details
    ISSN: 1572-879X
    Keywords: ethanol ; kinetics ; oxidation ; oxydehydrogenation ; platinum ; structure sensitivity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The effect of the platinum particle size was investigated for the catalytic oxidative dehydrogenation of aqueous ethanol to ethanal at a temperature of 303 K, an ethanol concentration of 260 mol m−3, a partial oxygen pressure 60 kPa, a pH of 9, and an ethanal and ethanoate concentration of 20 mol m−3. A particle size effect on the turnover frequency was observed but only for particle sizes smaller than 2 nm. Hence, the reaction shows a limited structure sensitivity.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00807202
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  • 16
    Electronic Resource
    Electronic Resource
    The detailed kinetics of the desorption of hydrogen from polycrystalline copper catalysts (1999)
    Springer
    Catalysis letters 59 (1999), S. 143-149 
    Details
    ISSN: 1572-879X
    Keywords: hydrogen ; desorption ; copper ; activation energy ; kinetics ; order of desorption
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The kinetics of desorption of hydrogen from the copper component of an alumina-supported polycrystalline copper catalyst has been studied in detail by temperature-programmed desorption (TPD). Line-shape analysis of the hydrogen TPD spectra shows: (i) that the desorption is second order, (ii) that the desorption activation energy is in the range 64–68 kJ mol−1 in the coverage range 7–44% of a monolayer, and (iii) that the desorption pre-exponential term has a value ∼10−5 cm2 s−1 atom−1 consistent with the desorption being second order, involving mobile adsorbates and a mobile desorption transition state.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1019080823616
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  • 17
    Electronic Resource
    Electronic Resource
    Improving the performance of the two-rate parameter by use of the integrating ratemeter and temporal optimization (1996)
    Springer
    Microchimica acta 124 (1996), S. 13-25 
    Details
    ISSN: 1436-5073
    Keywords: kinetics ; rates ; integrating ratemeter ; optimization ; first-order
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The integrating ratemeter is used in concert with the two-rate parameter to form the integrating ratemeter two-rate parameter. Propagation of error theory is applied to the integrating ratemeter two-rate parameter to yield expressions for the precision of rates calculated from the integrating ratemeter two-rate parameter in terms of the precision of the rates measured with the integrating ratemeter. Simulations and experimental results show that in cases where the standard deviation of the rate is relatively constant, the optimum time to make a rate measurement using the integrating ratemeter is also the optimum time to measure either of the rates in the two-rate parameter. If either of the two rates comprising the two-rate parameter is measured at the optimum time, then the precision and accuracy of concentrations measured with this technique are optimized.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01244952
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  • 18
    Electronic Resource
    Electronic Resource
    Growth of Ordered Domains in a Computer Model Alloy with Lattice Misfit (1999)
    Springer
    Journal of statistical physics 95 (1999), S. 23-43 
    Details
    ISSN: 1572-9613
    Keywords: model alloy ; Monte Carlo ; elastic interactions ; phase separation ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Physics
    Notes: Abstract We study via Monte Carlo simulations the influence of elastic interactions on the ordering and decomposition of a two-dimensional model binary alloy with antiferromagnetic nearest and ferromagnetic next nearest neighbor type interactions following a quench into the coexistence region. The elastic interaction leads to the development of a platelet morphology for the segregated ordered and disordered regions. A length scale characterizing the coarsening process follows a law of the type R=a+bt 1/3 with the growth b decreasing with the amount of ordered phase; this appears to be due to the presence of anti-phase boundaries between neighboring domains ordered on different sublattices which are difficult to eliminate. The application of uniaxial external stress results in “rafting” of the domains. Many of the simulation results are in agreement with experimentally observed effects in nickel-base superalloys.
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    URL: http://dx.doi.org/10.1023/A:1004569209618
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  • 19
    Electronic Resource
    Electronic Resource
    Effect of concentration and environmental form of tetradecenyl succinic acid on its mineralization in soil (1996)
    Springer
    Biodegradation 7 (1996), S. 377-382 
    Details
    ISSN: 1572-9729
    Keywords: bioavailability ; builders ; detergents ; kinetics ; mineralization ; sewage sludge ; soil
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Energy, Environment Protection, Nuclear Power Engineering , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract Tetradecenyl succinic acid (TSA) is the major component of a detergent builder (C12-C14 alkenyl succinic acid), which is inherently biodegradable. 14C-TSA was dosed as a component of sewage sludge into a soil with a history of sludge amendment at final added concentrations of 1.5 and 30 mg (kg soil)-1. In addition, it was dosed to the soil in an aqueous solution to a final added concentration of 30 mg (kg soil)-1. Dose and form were found to have a pronouced effect on the mineralization kinetics. When dosed in a realistic form and concentration (i.e. 1.5 mg (kg soil)-1 as a component of sludge), TSA was mineralized at its highest rate and to its greatest extent, and the mineralization half-life was 2.4 days. When dosed at 30 mg (kg soil)-1 as a component of sludge, mineralization began immediately, and the half-life was 23 days. In contrast, when dosed at this concentration in aqueous solution, the onset of mineralization was preceded by a 13 day lag period and the mineralization half-life was 69 days. Primary biodegradation and mineralization rates of TSA were very similar. Approximately, half the radioactivity was evolved as 14CO2, while the remaining radioactivity became non-extractable, having presumably been incorporated into biomass or natural soil organic matter (humics). This study demonstrated that TSA is effectively removed from sludge-amended soils as a result of biodegradation. Furthermore, it showed the effect that dose form and concentration have on the biodegradation kinetics and the importance of dosing a chemical not only at a relevant concentration but also in the environmental form in which it enters the soil environment.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00056421
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  • 20
    Electronic Resource
    Electronic Resource
    Biodegradability of diesel oil (1996)
    Springer
    Biodegradation 7 (1996), S. 73-81 
    Details
    ISSN: 1572-9729
    Keywords: diesel oil ; biodegradation ; CSTR ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Energy, Environment Protection, Nuclear Power Engineering , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Abstract In batch culture diesel oil was degraded rapidly, with a maximum growth rate (for a consortium of microorganisms) of 0.55 h-1. The corresponding yield Y SX was 0.1 Cmol/Cmol. In a continuous stirred tank reactor the maximum dilution rate was about 0.25 h-1, with a yield of 0.3 Cmol/Cmol. With a residence time of 1 day 82% of the influent oil was degraded. In the batch reactor, of the mixture of linear and branched alkanes the linear alkanes were degraded fastest and with the highest yield. Only after most of the linear alkanes had disappeared were the branched alkanes consumed. In a CSTR a large part of the branched alkanes was not degraded.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00056560
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  • 21
    Electronic Resource
    Electronic Resource
    Invariant kinetic approach to the description of a rock fracture process and induced seismic events (1996)
    Springer
    Pure and applied geophysics 147 (1996), S. 367-375 
    Details
    ISSN: 1420-9136
    Keywords: Induced seismicity ; kinetics ; rock fracture ; rockburst ; earthquake
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences , Physics
    Notes: Abstract Powerful seismic events, such as earthquakes and rockbursts, are caused by the accumulation of energy in rocks and loss of rock mass stability. Usually methods of their forecasting are based on the registration of anomalous behavior of geophysical fields. However an efficiency of this approach is low. The present paper proposes a kinetic approach to the description of rock fracture process, which can be used for the forecasting of seismic events and an investigation of structure and energy distributions in rock. 3-D and 1-D kinetic equations describing a process of cluster formation in rock were obtained. The equations are invariant to deformation conditions and to the scale level of events. They showed a good agreement with the results of field observations and laboratory experiments. It was also shown that these equations well describe the processes of earthquake, rockburst and rock sample failure preparation. Catalogues of rockbursts in mines were analyzed with the use of the kinetic equations to find out evidence of induced seismic events. The proposed approach makes it possible to reveal trends in rock behavior and thus predict the rock failure at different scale levels.
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    URL: http://dx.doi.org/10.1007/BF00877489
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    Cubic topology in surfactant and lipid mixtures (1996)
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    European biophysics journal 24 (1996), S. 293-299 
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    ISSN: 1432-1017
    Keywords: Phase transition ; NMR ; DSC ; X-ray diffraction ; Bonnet Transformation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Physics
    Notes: Abstract Ternary systems of palmitoyl-oleoyl-phosphatidylcholine (POPC) and the non-ionic surfactant C12EO2 (di-ethylene-oxide-mono-dodecyl-ether) in water have been studied with optical microscopy, NMR, DSC and X-rays from ambient temperatures to 45 °C. Below 29 °C the system is in the lamellar liquid crystalline state. Between 30 and 32 °C it transforms into a cubic Ia3d structure which converts into the cubic Pn3m phase at 39 °C. The transitions are fully reversible. An epitaxial relationship between all three phases was found, which is an elegant and convenient way to rearrange molecules from lamellar bilayers to a network of curved surfaces. The la3d (Q230) to Pn3m (Q224) transition occurs without measurable enthalpy change. This, together with the metric relation of 1.60 between the cubic lattice constants is strong evidence for a Bonnet transformation, where the structural changes occur without change in curvature. The potential significance of the cubic phases as intermediate structures for biological processes, e. g. transport across a bilayer or fusion of membranes, are discussed.
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    Pharmacokinetics of diphemanil methylsulphate in neonates and in premature infants (1996)
    Springer
    European journal of clinical pharmacology 50 (1996), S. 429-430 
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    ISSN: 1432-1041
    Keywords: Key words Diphemanil methylsulphate ; Neonate; antimuscarinic agent ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Medicine
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    URL: http://dx.doi.org/10.1007/s002280050136
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    Assessment of inhibition kinetics of the growth of strain P5 on pentachlorophenol under steady-state conditions in a nutristat (1996)
    Springer
    Archives of microbiology 165 (1996), S. 194-200 
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    ISSN: 1432-072X
    Keywords: Key words Auxostat ; Batch culture ; Chemostat ; Continuous culture ; Fermentation control ; Inhibition ; kinetics ; Nutristat ; On-line measurement ; Pentachlorophenol ; Pollutant ; Sphingomonas ; Steady-state conditions ; Toxicity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology
    Notes: Abstract A bacterium degrading pentachlorophenol (PCP) as the only source of carbon and energy was grown in a “nutristat”, i.e., a continuous culture with on-line measurement and control of the substrate concentration. We improved the PCP nutristat by incorporation of a personal computer with a proportional integral derivative (PID) algorithm for controlling the medium feed pump. The controlled value deviated from the average (set-point) value by 1% maximally. In the PCP nutristat (30°C), the steady-state dilution rate, and hence, specific growth rate, showed a maximum value of 0.142 ± 0.004 h–1 at set-point PCP concentrations between 37 and 168 μM. At PCP concentrations above 168 μM, the steady-state growth rate decreased because of inhibition. The growth yield coefficient was not seriously affected by the PCP concentration, suggesting that uncoupling was not the inhibitory mechanism. It was concluded that the PCP nutristat is very useful for establishing steady-state conditions that maintain growth-inhibitory PCP concentrations and high cell concentrations, conditions for which the chemostat is not suitable.
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    Polymerization kinetics of acrylic bone cements by differential scanning calorimetry (1996)
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    Journal of thermal analysis and calorimetry 47 (1996), S. 35-49 
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    ISSN: 1572-8943
    Keywords: bone cement ; DSC ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Bone cements are widely used for the fixation of metallic prostheses in orthopaedics and to form replacements for skull defects in neurosurgery. Acrylic bone cements are based on a mixture of methyl methacrylate (MMA) and a fine powder of polymethyl methacrylate (PMMA). The polymerization of the bone cement occurs in contact with the bone and the prosthesis which act as the boundaries of a bulk polymerization reactor. The kinetic behaviour of the bone cement plays a fundamental role for the final performance of the implant. In this paper, the isothermal and non-isothermal polymerization behaviour of a commercial bone cement is described. A simple phenomenological model, accounting for the autoacceleration ffect, for a diffusion controlled termination mechanism and for the reaction between inhibitor and initiator, is proposed. The reaction kinetics is analysed by DSC. DSC data are used for the determination of the rates of polymerization under isothermal and non-isothermal conditions. The experimental data are processed to calculate the parameters of the proposed phenomenological kinetic model. The analytical and numerical details related to the integration of the model are discussed.
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    Characterizing in situ starch gelatinization (1996)
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    Journal of thermal analysis and calorimetry 47 (1996), S. 181-194 
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    ISSN: 1572-8943
    Keywords: DSC ; gelatinization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Data obtained by dynamic mechanical analysis and DSC analysis of durum wheat dough are presented and discussed. Doughs with water contents ranging from 45 to 55% (w/w) were subjected to sinusoidal shearing by means of a dynamic mechanical spectrometer (Rheometrics, RFS2) equipped with parallel plate geometry, 0.1 strain amplitude and 1 rad/min frequency. The tests were carried on in temperature sweep mode at a heating rate of 2°C min−1. Wheat samples with water contents in the range between 7.5 and 37.5% and doughs with 37.5% moisture content were mixed for different times and subjected to DSC analysis (Perkin-Elmer, DSC-7) at a heating rate of 20°C min−1. Dynamic mechanical analysis revealed that the relationship between the dynamic properties of the dough and the temperature was modified as the water content of the dough increased and was quite different from that for gluten. A similar response was observed in the course of temperature scans made by means of DSC. These experimental findings suggest that the water-starch interaction in the presence of a protein matrix is affected by the availability of water and that the protein system is a competitor with respect to starch.
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    Erfahrungen mit vier Softwarepaketen für Kinetische Auswertungen in der Thermischen Analyse (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 543-557 
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    ISSN: 1572-8943
    Keywords: compensation effect ; DSC ; kinetics ; TG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Four computer programs as well as one demo-version for non-linear evaluation of kinetic data in thermal analysis and calorimetry, were presented. The multi-task program TA-kin meets all mathematical requirements for solving the numerical assignments. It is shown that the so-called compensation effect is due to the mathematical structure of the Arrhenius equation. Several applications of TA-kin to a lot of DSC- and TG-measurements and isoperibolic batch experiments as well as adiabatic semi batch experiments realized by precision calorimetry have been discussed.
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    Kinetics of the decomposition of calcium carbonate in the presence of Bi2O3 (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 569-575 
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    ISSN: 1572-8943
    Keywords: Bi2O3 ; CaCO3 decomposition ; kinetics
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    Topics: Chemistry and Pharmacology
    Notes: Abstract Former studies concerning the formation of the compounds in the pseudobinary systems of Bi2O3-MO type (M =Ca, Sr, Ca+Sr) have shown that the reaction which occurs with the highest rate is that between Bi2O3 and CaO. In the present work CaCO3 was used as CaO source. We carried out an investigation of the thermal decomposition of CaCO3 in the presence of Bi2O3 in comparison with the decomposition of pure CaCO3. The presence of Bi2O3 exerts a complex influence on the CaCO3 decomposition acting on the nucleation as well as on the diffusion of CO2. The decomposition of the samples with low Bi2O3 content follows the mechanism of a contracting sphere. A change from surface nucleation to bulk nucleation is recorded for higher amounts of Bi2O3.
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    Co-curing studies of ethynyl terminated oligoimide and (methyl) nadicimide resins (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 685-695 
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    ISSN: 1572-8943
    Keywords: DSC ; polymers ; resins ; TG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The paper describes the co-curing studies of ethynyl and ethenyl end-capped imide resins. The effect of composition and chemical structure of ethenyl end-capped resins (nadicimides) on thermal behavior of ethynyl end-capped resins was evaluated using DSC and thermogravimetric analysis. An increase in char yield was observed on co-curing of few resin formulations. A mechanism has been proposed to account for this observation.
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    Thermal transitions of cassava starch at intermediate water contents (1996)
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    Journal of thermal analysis and calorimetry 47 (1996), S. 1213-1228 
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    ISSN: 1572-8943
    Keywords: cassava starch ; DSC ; starch thermal properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Order-disorder transitions were investigated in native cassava starch at intermediate moisture contents (35 to 60% wt. water), using Differential Scanning Calorimetry (DSC) and dynamic Wide Angle X-ray Diffractometry (WAXS) with a synchrotron radiation source. The gelatinization of granules occurs as a cooperative process, due to constraints induced in crystallites by the amorphous areas. Variations of water content (water volume fraction from 0.28 to 0.86) and heating rate (0.2–10
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    Isothermal microcalorimetric studies on starch retrogradation (1996)
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    Journal of thermal analysis and calorimetry 47 (1996), S. 1179-1200 
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    ISSN: 1572-8943
    Keywords: DSC ; isothermal microcalorimetry ; retrogradation ; starch
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract In the present study, isothermal microcalorimetry was introduced as a tool to investigate properties of starch retrogradation during the first 24 h. The study was made on purified amylose and amylopectin from corn, as well as on native starches, such as wheat, potato, maize, waxy maize and amylomaize, differing in their amylose content. The results were obtained in the form ofP-t traces (thermal powervs. time), and integration of these traces gave a net exothermic enthalpy of reaction, caused by the crystallization of amylose and amylopectin. TheP-t traces reflected the quantities of amylose and amylopectin in the starch studied. Depending on the amylose content and the botanical source of the starch, the rate of crystallization of amylose was high and predominated over that of amylopectin during the first 5–10 h. The contribution from amylose crystallization to the measured exothermic enthalpy was very substantial during this period. After ∼10 h, amylose crystallized at a lower constant rate. During the first 24 h, amylopectin crystallized at a low steady rate. The exothermic enthalpies obtained by the isothermal microcalorimetric investigations during the first 24 h of retrogradation were generally low in relation to the endothermic melting enthalpies observed by differential scanning calorimetry (DSC) measurements after 24 h of storage. The discrepancies in enthalpy values between the two methods are discussed in relation to phase separation and the endothermic effects owing to the decrease in polymer-water interactions when polymer-rich regions in the starch gel separate. Besides the exothermic enthalpies obtained, theP-t traces also made it possible to study the initial gelation properties of amylose from different botanical sources. The present study further demonstrated that isothermal microcalorimetry can provide a possible way to investigate the antistaling effect of certain polar lipids, such as sodium dodecylsulphate (SDS) and 1-monolauroyl-rac-glycerol (GML), when added to starches of different botanical origin. The net exothermic heat of reaction for starch retrogradation during the first 24 h was decreased when GML or SDS was added to the starch gels. The recordedP-t traces also showed how the effect of the added lipid influenced different periods during the first 24 h of starch retrogradation, and that the effect depended mainly on the amylose content, the botanical source of the starch, and the type of lipid used. When GML or SDS was added to waxy maize, the isothermal microcalorimetric studies clearly indicated some interaction between amylopectin and the polar lipids. These results concerning the action of anti-staling agents are further discussed in relation to the helical inclusion complexes formed between amylose-polar lipid and amylopectin-polar lipid.
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    Influence of heating and cooling rates on the glass transition temperature and the fragility parameter of sorbitol and fructose as measured by DSC (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 1419-1436 
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    ISSN: 1572-8943
    Keywords: cooling/heating rate ; DSC ; fragility parameter ; glass transition temperature ; sorbitol-fructose
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The glass transition temperatures of sorbitol and fructose were characterized by four points determined on DSC heating thermograms (onset, mid-point, peak and end-point), plus the limit fictive temperature. The variations of these temperature values, observed as functions of cooling and heating rates, were used to determine the fragility parameter, as defined by Angell [1] to characterize the temperature dependence of the dynamic behavior of glass-forming liquids in the temperature range above the glass transition. The apparent activation energy values, determined for the different temperatures studied, were similar for fructose and sorbitol. These values were compared to data obtained from other techniques, such as mechanical spectroscopy. The variations of the apparent activation values, observed in experiments involving cooling and heating at the same rate, slow cooling followed by rate-heating, or rate-cooling followed by fast heating, were explained by aging effects occurring during the heating step.
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    Non-enzymatic browning-induced water plasticization (1996)
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    Journal of thermal analysis and calorimetry 47 (1996), S. 1437-1450 
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    ISSN: 1572-8943
    Keywords: browning ; crystallization ; glass transition ; kinetics ; milk powder ; water
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract An exotherm, observed in differential scanning calorimetry (DSC) scans of amorphous food materials above their glass transition temperature,T g, may occur due to sugar crystallization, nonenzymatic browning, or both. In the present study, this exothermal phenomenon in initially anhydrous skim milk and lactose-hydrolyzed skim milk was considered to occur due to browning during isothermal holding at various temperatures above the initialT g. The nonenzymatic, Maillard browning reaction produces water that in amorphous foods, may plasticize the material and reduceT g. The assumption was that quantification of formation of water from theT g depression, which should not be observed as a result of crystallization under anhydrous conditions, can be used to determine kinetics of the nonenzymatic browning reaction. The formation of water was found to be substantial, and the amount formed could be quantified from theT g measured after isothermal treatment at various temperatures using DSC. The rate of water formation followed zero-order kinetics, and its temperature dependence well aboveT g was Arrhenius-type. Although water plasticization of the material occurred during the reaction, and there was a dynamic change in the temperature differenceT−T g, the browning reaction was probably diffusioncontrolled in anhydrous skim milk in the vicinity of theT g of lactose. This could be observed from a significant increase in activation energy. The kinetics and temperature dependence of the Maillard reaction in skim milk and lactose-hydrolyzed skim milk were of similar type well above the initialT g. The difference in temperature dependence in theT g region of lactose, but above that of lactose-hydrolyzed skim milk, became significant, as the rate in skim milk, but not in lactose-hydrolyzed skim milk, became diffusion-controlled. The results showed that rates of diffusion-controlled reactions may follow the Williams-Landel-Ferry (WLF) equation, as kinetic restrictions become apparent within amorphous materials in reactions exhibiting high rates at the same temperature under non-diffusion-controlled conditions.
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    Investigation of the complex thermal behavior of fats (1996)
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    Journal of thermal analysis and calorimetry 47 (1996), S. 1545-1565 
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    ISSN: 1572-8943
    Keywords: cocoa butter ; fat crystallization ; DSC ; fat polymorphism ; fat structure ; fats ; lard ; milk fat ; triacylglycerols ; X-ray diffraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The thermal behavior of three ural fats (displaying very different composition), cocoa butter (CB)2, lard, and a stearin obtained from anhydrous milk-fat (AMF) fractionation, were studied by both DSC and X-ray diffraction as a function of temperature (XRDT). To perform temperature explorations between −30
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    Thermal behaviour of solid complexes of phenoxyalkanoic acids and divalent metals (1996)
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    Journal of thermal analysis and calorimetry 46 (1996), S. 5-14 
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    ISSN: 1572-8943
    Keywords: cadmium phenoxyacetate ; complexes ; DSC ; mercury(II) phenoxyacetate ; TG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Solid cadmium and mercury(II) phenoxyacetates were prepared and investigated by DSC and TG techniques. The cadmium salt decomposed in two steps with the loss of 1.5 water molecules at first and the successive formation of CdCO3 as final product. Δdeh H * associated with the loss of one water molecule was compared with the corresponding values obtained for other phenoxyacetates previously studied and the obtained results were discussed. Anhydrous mercury(II) phenoxyacetate gave, on heating, HgCO3 which successively decomposed with the formation of gaseous products and a little amount of solid residue.
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    Activation energy of Se2Ge0.2Sb0.8 chalcogenide glass by differential scanning calorimetry (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 177-186 
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    ISSN: 1572-8943
    Keywords: activation energy ; chalcogenide glass ; DSC
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Results of differential scanning calorimetry (DSC) at different heating rates on Se2Ge0.2Sb0.8 chalcogenide glass are reported and discussed. As the heating rate (α) changed, also the glass transition temperature (T g) and onset temperature of crystallization (T c) changed. As the value of the transition activation energyE t changed, the crystallization fraction (χ), heat flow (Δq and the crystallization peak temperature (T p) also changed. The value of the effective activation energy of crystallizationE c was calculated by means of six different methods. The Se2Ge0.2Sb0.8 chalcogenide glass has two crystallization mechanisms, a one-dimensional and an other surface crystallization growth. The average value ofE t for Se2Ge0.2Sb0.8 is equal to 194.95±3.9 kJ·mol−1 and the average value ofE c is equal to 164±3.3 kJ·mol−1.
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    Thermal study of irradiated polyacetylene films (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 237-243 
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    ISSN: 1572-8943
    Keywords: DSC ; DTG ; polyacetylene films ; TMA
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Polyacetylene films irradiated byγ-rays up to 100 MRad were studied by means of TMA, DTG and DSC methods. It is shown that as the irradiation dose increases the concentration of topological branching knots into the polymer chains and theT g values decrease, the total mass loss and the enthalpy of the thermal isomerization reaction also decrease.
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    Nucleation and crystallization of polypropylene filled with BaSO4 (1996)
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    Journal of thermal analysis and calorimetry 46 (1996), S. 619-626 
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    ISSN: 1572-8943
    Keywords: crystallization ; DSC ; filled polypropylene ; nucleation ; structural modification
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The influence of high concentration of BaSO4 as nucleating agent on crystallization of fiber-forming polypropylene was studied by DSC. The work presents experimental and calculated values of melting and crystallization enthalpies of filled polypropylene and the influence on the formation of interface interactions between filler and polymers. These results show minimal interactions of components (BaSO4 and polypropylene) under experimental conditions.
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    Thermal analysis of macromolecules (1996)
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    Journal of thermal analysis and calorimetry 46 (1996), S. 643-679 
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    ISSN: 1572-8943
    Keywords: DDTA ; DSC ; macromolecules
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract This review traces the development of thermal analysis over the last 40 years as it was experienced and contributed to by the author. The article touches upon the beginning of calorimetry and thermal analysis of polymers, the development of differential scanning calorimetry (DSC), single run DSC and other special instrumentations, up to the recent addition of modulation to calorimetry. Many new words and phrases have been introduced to the field by the author and his students, leaving a trail of the varied interests one can have over 40 years. It began with “cold crystallization” and most recently the term “oriented, intermediate phase” was coined, creating in-between: “extended chain crystals,” the “irreversible thermodynamics of melting of polymer crystals,” “dynamic differential thermal analysis” (DDTA), “the rule of constant increase ofC p per mobile bead within a molecule at the glass transition temperature,” “superheating of polymer crystals,” “melting kinetics,” “crystallization during polymerization,” the “chain-folding principle, “molecular nucleation,” “rigid amorphous phase,” a “system of classifying molecules,” “macroconformations,” “amorphous defects,” “rules for the entropy of fusion based on molecular shape and flexibility,” “single-molecule single-crystals,” “a system of classifying phases and mesophases,” and “condis phase.”
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    Analysis of mesophase formation in side-chain liquid crystalline polycarbosilanes (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 795-808 
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    ISSN: 1572-8943
    Keywords: DSC ; kinetics ; liquid crystalline polymer ; optical transmittance ; polycarbosilane ; side-chain mesogen ; transition parameters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract This paper is concerned with an analysis of the thermodynamics and kinetics of mesophase formation by cooling from the isotropic state of side-chain liquid crystalline polycarbosilanes containing spacers in the range from 3 to 11 CH2-groups. The polymers are characterized by their thermotropic behaviour as far as temperature, enthalpy and entropy of the transitions are concerned. The kinetics was followed by optical and calorimetric methods. Longer spacer length leads to more perfect ordering in the mesophase, higher isotropization temperatures, and lower glass transition temperatures. The Avrami and Ozawa formalism to describe the transition kinetics to the mesophase from the isotropic state cannot be interpreted as the nucleation and growth mechanism known from crystallization.
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    Kinetic compensation effect in the thermal degradation of polymers (1996)
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    Journal of thermal analysis and calorimetry 47 (1996), S. 1081-1091 
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    ISSN: 1572-8943
    Keywords: kinetics ; thermal degradation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The kinetic study of thermal degradation takes into account the validity of the Arrhenius equation. From TG data, the activation energy,E a and pre-exponential factor,A, are evaluated. These results are interpreted by using the ‘kinetic compensation effect’ as basis. A linear correlation between In(A) andE a is obtained in all cases studied. However, in a plot of the logarithm of the rate constant as a function of reciprocal temperature for the same series of reactions, the thermal oxidative degradations of Nylon-6 and PVC display a point of concurrence and one isokinetic temperature, whereas those of HIPS and PC do not. Therefore, in the thermal oxidative degradations of Nylon-6 and PVC a ‘true’ compensation effect occurs, which could be related to the bulk properties of metal oxides, such as different valence states, whereas for other polymers it displays only an ‘apparent’ compensation effect. This means that degradation is largely independent of the bulk properties of oxides, but may be related to the distribution of different kinds of active links in the polymer surface having different activation energies.
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    A DSC study of the effects of sugars on thermal properties of rice starch gels before and after aging (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 1201-1212 
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    ISSN: 1572-8943
    Keywords: aging ; amylopectin ; DSC ; gels ; glass transition ; recrystallization ; retrogradation ; rice starch ; sugars
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Thermal characterization of gelatinized binary rice starch-water and ternary starch-sugar-water gels before and after aging was carried out using differential scanning calorimetry. The glass transition temperature of the maximally freeze-concentrated solution (T′g) in both fresh and aged gels was observed to decrease progressively with increasing sugar concentration. Aging of the gels generally shiftedT′g to higher temperatures, but had little or no effect on the ice melting peak temperature (T m). The presence of various sugars could either accelerate or retard starch (amylopectin) recrystallization, depending on the type and concentration of sugar, as well as on starch/water ratio. A hypothesis based on the dual antiplasticizing-plasticizing effects of sugars was postulated to explain the observed effects. Of the sugars studied, xylose and fructose appeared to display exceptional retardative and accelerative effects, respectively, on retrogradation.
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    Effect of hydrothermal treatment on the gelatinisation properties of potato starch as measured by differential scanning calorimetry (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 1229-1246 
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    ISSN: 1572-8943
    Keywords: DSC ; gelatinisation ; potato starch
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Gelatinisation temperatures as a function of moisture content were determined for potato starch. The native starch was then hydrothermally treated at a temperature 3% (Kelvin degrees) below the gelatinisation peak temperature and at moisture levels varying from 20 to 67% (by weight). Gelatinisation temperatures, temperature ranges and enthalpy values were affected for all treated samples. However, two sample populations could be distinguished: those samples treated under ‘limited’ moisture conditions and other samples treated in the presence of ‘extragranular’ moisture. A two-step hydrothermal treatment further increased the gelatinisation temperature, but the effect of the second step was small in comparison to that of the first.
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    DSC analysis of starch thermal properties related to functionality in low-moisture baked goods (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 1299-1314 
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    ISSN: 1572-8943
    Keywords: baked goods ; cookies ; crackers ; DSC ; pretzels ; starch
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract We describe an application of DSC as an analytical ‘fingerprinting’ method that has been used to characterize the thermal properties of wheat starch in low-moisture, wheat-flour-based baked products, including cookies, crackers, and pretzels. This use of DSC has enabled us to relate starch thermal properties, on the one hand, to starch structure, and on the other hand, to starch functionality, in terms of baking performance and finished-product quality.
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    URL: http://dx.doi.org/10.1007/BF01992829
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    Structure and properties of bread dough and crumb (1996)
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    Journal of thermal analysis and calorimetry 47 (1996), S. 1339-1360 
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    ISSN: 1572-8943
    Keywords: bread crumb ; bread dough ; DSC ; hydrocolloid ; mechanical properties ; pentosans ; protein
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The effects of hydrocolloids (guar and locust bean gums), soluble pentosans, and whey proteins on staling of bread crumb were investigated by means of DSC, rheometry, and image analyis. One current hypothesis, that these ingredients would behave as “water binders” and, at least the former two, as anti-staling agents, was indeed confirmed, although this action might be indirect. All the samples considered showed an exothermic DSC peak preceding the endotherm of the amylopectin fusion. According to a previous work, this signal was attributed to a water-dependent cross-linking process that would involve next-neighbouring polymer chains. To check the effect produced by molecular modifications that were expected to increase the water uptake of these ingredients, doughs containing added succinylated pentosans and whey proteins, and a polycarboxylate polymer, PEMULEN TR-1, were examined. These modifications enhanced starch retrogradation and yielded a firmer crumb. It was tentatively concluded that some direct interaction between these modified molecules and the crumb polymers might have taken place. In line with the food polymer science approach, the use of Time-Temperature-Transformation (TTT) diagrams is also discussed.
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    URL: http://dx.doi.org/10.1007/BF01992832
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    Effects of medium and chemical modification on thermal characteristics of Β-lactoglobulin (1996)
    Springer
    Journal of thermal analysis and calorimetry 47 (1996), S. 1513-1525 
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    ISSN: 1572-8943
    Keywords: Β-lactoglobulin ; DSC ; protein modification ; thermal properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The thermal properties of Β-lactoglobulin (Β-LG) were studied by differential scanning calorimetry (DSC) under different medium conditions.pH, neutral salts, protein perturbants, and polyols all affected the DSC characteristics of Β-LG. Acylation with fatty acids also changed the thermal properties, particularly peak width at half-height. The results suggest that the structural stability of Β-LG is controlled by non-covalent forces, particularly electrostatic and hydrophobic interactions. Disulfide bonds did not contribute to the thermal response of Β-LG. Fatty N-acyl-amino acids caused marked increases in thermal stability and decreases in denaturation enthalpy, and additional peaks were observed in the presence of some palmitoyl derivatives.
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    Thermal Analysis Studies on Isopropylnitrate (1999)
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    Journal of thermal analysis and calorimetry 55 (1999), S. 9-19 
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    ISSN: 1572-8943
    Keywords: ARC ; DSC ; HFC ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Isopropylnitrate (IPN) is described as a detonable material used in propellants and explosives. While there is considerable information available on its sensitivity and compatibility with other materials, very little is known about its thermochemical properties. This paper will describe the results obtained from some DSC, heat flux calorimetry (HFC) and accelerating rate calorimetry (ARC) measurements. The ASTM DSC method using a hermetic aluminum pan having a lid with a laser-produced pin hole was used to determine the vapour pressure of IPN1. Results calculated from an Antoine equation are in substantial agreement with those determined from DSC measurements. From the latter measurements, the enthalpy of vaporization was determined to be 35.32±0.62 kJ mol−1. Attempts to determine vapour pressures above about 0.8 MPa resulted in significant decomposition of IPNg. The enthalpy change for decomposition in sealed glass systems was found to be -3.43±0.09 kJ g−1 and -3.85±0.03 kJ g−1, respectively from DSC and HFC measurements on IPN1 samples loaded in air. Slightly larger exotherms were observed for the HFC results in air than those in inert gas, suggesting some oxidation occurs. In contrast, no significant difference in the observed onset temperature of about 150°C was observed for both the HFC and ARC results. From DSC measurements, an Arrhenius activation energy for decomposition of 126±4 kJ mol−1 was found. These measurements were also conducted in sealed glass systems and decomposition appeared to proceed primarily from the liquid phase.
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    Apparent Activation Energies of the Non-isothermal Degradation of Eva Copolymer (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 67-76 
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    ISSN: 1572-8943
    Keywords: activation energy ; DSC ; ethylene-vinyl acetate copolymer ; TG ; TG/IR ; thermal degradation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract When ethylene-vinyl acetate copolymer, EVA, is heated, a two-stage thermal degradation occurs following its melting. The vinyl acetate content of the copolymer was determined to be 43.8% by using TA 2950 and TA 2050 thermogravimetric instruments. TG/FTIR was used to detect the evolved gas. Acetic acid and trans-1-R-4-R'-cyclohexane were the main products evolved from EVA in the first and second stage, respectively. The apparent activation energies were determined for both stages by differential methods.
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    Crystallization Kinetics of Polypropylene-polyethylene-based Copolymers (1999)
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    Journal of thermal analysis and calorimetry 55 (1999), S. 57-65 
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    ISSN: 1572-8943
    Keywords: artificial ageing ; DSC ; dynamic crystallization ; isoconversional method
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A crystallization kinetics analysis of several polypropylene-polyethylene (PP-PE), PP-rich copolymers was made by means of differential scanning calorimetry. The crystallization was studied via calorimetric measurements at different cooling rates. Several additives were added to the base material. Some test samples were subjected to artificial ageing processes. A modified isoconversional method was used to describe the crystallization process under non-isothermal conditions. The value of the Avrami parameter was determined for primary and secondary crystallization.
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    Kinetics of Thermal Decomposition of Mixed Ligand Trinuclear Compound of Cadmium(II) (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 233-241 
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    ISSN: 1572-8943
    Keywords: cadmium(II) atom ; kinetics ; non-isothermal decomposition ; Schiff-base compound
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystal C81H78N12O6Cd3 was synthesized and its structure was determined by single crystal X-ray diffraction method. The complex crystallizes in the monoclinic system space group P21/n with cell parameters, a=15.959(4) Å, b=26.222(3) Å, c=25.907(6) Å, β=101.60(2)°. The non-isothermal kinetics of the crystal was studied by use of non-isothermal TG and DTG curves. The kinetic parameters were analyzed by means of integral and differential methods, and mechanism functions of the thermal decomposition reaction for its second step were proposed. The kinetic equation of thermal decomposition is expressed as: dα/dt=Aexp(-E/RT)1.5(1-α)4/3[1/(1-α)1/3-1]−1. The average values of E(kJ mol−1) and lnA/s−1 are 339.25, 43.95, respectively.
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    Re-examination of the Kinetics of the Thermal Dehydroxylation of Goethite (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 301-309 
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    ISSN: 1572-8943
    Keywords: dehydroxylation ; goethite ; kinetics
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The kinetics of thermal dehydroxylation of aluminuous goethites [1] synthesised from a ferrous salt has been re-examined using the general reaction order kinetic law. The utilised data processing was based on the procedures employed by dissolution kinetics. Recalculation of the activation energies EA of the dehydroxylation yielded the values 130, 132, 128, and 123 kJ mol−1 for pure goethite, goethite with 10, 20, and 30 mol% Al substitution, respectively. The values of EA are in a good agreement with those given for goethite in literature. The EA values are linearly related with the chemically bound excess H2O/OH− in the crystal lattice that is apparently influenced by Al substitution.
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    Kinetic Analysis of Thermogravimetric Data XXXII. DSC Study of Some [Co(Diox·H)2(amine)2]X and H[Co(Diox·H)2(N3)2] Type Complexes with Alicyclic α-dioximes (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 311-320 
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    ISSN: 1572-8943
    Keywords: dioximine complexes of Co ; DSC ; kinetic compensation effect ; kinetic parameters of thermal decomposition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract 14 mixed Co(III) dioximine chelates of the types [Co(Diox·H)2(amine)2]X (X = Br, I, NO3, ClO4) and H[Co(Diox·H)2(N3)2], respectively (Diox·H2-1,2-cyclohexane dione dioxime (nyoxime), 1,2-cycloheptane dione dioxime (heptoxime) 1,2-cyclooctane dione dioxime (octoxime) were obtained and their thermal decompositions were studied in an argon atmosphere. After the dehydration of the crystallohydrates, both types of complexes exhibit 3 decomposition stages. For the [Co(Diox·H)2(amine)2]X type complexes (X = Br, I) the first endothermal stage is the substitution of an amine molecule for the external sphere anion and this process is followed by two exothermal decomposition stages. With H[Co(Diox·H)2(N3)2] type complexes the first and third processes are relatively slow, but the second process is very fast, corresponding to a vertical portion of the TG curves. From the TG curves kinetic parameters were derived for 11 processes and the validity of a non-linear compensation law was observed.
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    Thermogravimetric Analysis of Cobalt(II)-dothiepin Complexes (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 841-849 
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    ISSN: 1572-8943
    Keywords: cobalt(II)-dothiepin ; kinetics ; TG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The complexes of cobalt(II) with dothiepin (DOT) hydrochloride have been studied for kinetics of thermal degradation by thermogravimetric analysis (TG) and derivative thermogravimetric studies (DTG) in a static nitrogen atmosphere at a heating rate of 10° C min−1. A general mechanism of thermal decomposition is advanced involving dehydration and decomposition process for both organic and inorganic ligands. The thermal degradation reactions were found to proceed in three steps having an activation energy in the range 6.75–170 kJ mol−1. Thermal decomposition kinetics parameters were computed on the basis of thermal decomposition data.
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    Calorimetric Investigations of Some Phases in the System Sodium Fluoride - Aluminium Fluoride (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 51-57 
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    ISSN: 1572-8943
    Keywords: DSC ; enthalpies ; NaAlF4 ; Na5Al3F14
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Beside the two well-known minerals cryolite, Na3AlF6, and chiolite, Na5Al3F14, the binary system NaF-AlF3 also contains a third compound, NaAlF4, sodium tetrafluoroaluminate. Solid NaAlF4 has been prepared from its vapour under controlled conditions. The stability of NaAlF4 has been investigated by differential scanning calorimetry. It is shown that the disproportionation of the compound: 5NaAlF4(s)=Na5Al3F14(s)+2AlF3(s) takes place at considerable rate between 700 and 900 K. The enthalpy of this reaction is calculated and found to be -66.9 kJ. Enthalpies of the two solid state transitions α-Na3AlF6 → β-Na3AlF6 and α-AlF3 → β-AlF3 have also been measured and new values are reported. The enthalpy of formation of chiolite, Na5Al3F14, at 900 K has been recalculated from enthalpy increment data obtained by drop calorimetry. A value of ΔH900 o = -7513.6±12.0 kJ mol-1 has been obtained. This value is in disagreement with the recommended value given in JANAF Thermochemical Tables given at 900 K ΔHf o = -7559.2 kJ mol-1.
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    Gegeneration of Deactivated β-Zeolite by Coke Oxidation (1999)
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    Journal of thermal analysis and calorimetry 56 (1999), S. 297-303 
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    ISSN: 1572-8943
    Keywords: β-zeolite ; coke ; cumene ; kinetics ; regeneration ; TG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract An accurate description of coke burn off is obtained from a catalyst based on β-zeolite and used for benzene alkylation with propylene giving cumene by using the thermogravimetric technique. A simple empirical kinetic model was successfully applied to interpolate the data of thermogravimetric analysis performed on samples after partial burn off. Different temperatures, partial pressures of oxygen and gas flow rates were the variables studied in order to calculate the apparent rates and the activation energy for the coke oxidation reaction and to outline the best conditions for the industrial regeneration procedure of our proprietary catalyst PBE-1 for cumene synthesis. Combining the unusually long lifetime per reaction cycle with the optimized regeneration procedure leads to an outstanding overall catalyst life.
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    The Fe-Ni Distribution Between Pentlandite and Monosulfide Solid Solution Equalized at Low Temperature (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 925-929 
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    ISSN: 1572-8943
    Keywords: DSC ; equilibrium ; Fe-Ni distribution ; monosulfide solid solution ; pentlandite
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Two mixtures of pentlandite and the monosulfide solid solution (mss) have been synthesized. The bulk compositions of the samples are Fe6Ni3S8 and Fe3Ni6S8. Differential scanning calorimetry detected exothermic process in the samples under heating. The process takes place in temperature range between phase transition in the mss (near 400 K) and 690 K and is governed by diffusion. X-ray powder diffraction has showed that equilibrium Fe-Ni distribution between pentlandite and the mss is achieved after short-time heating up to 670 K.
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    Non-Isothermal Pyrolysis and Kinetics of Oil Shales (1999)
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    Journal of thermal analysis and calorimetry 56 (1999), S. 953-958 
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    ISSN: 1572-8943
    Keywords: differential scanning calorimeter ; kinetics ; oil shale ; pyrolysis ; thermogravimetry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract In this research, non-isothermal pyrolysis behavior and kinetics of three oil shales were studied by thermal analysis methods. All the thermal effects were endothermic and no exothermic region was observed in DSC curves. When oil shales are heated in nitrogen atmosphere in TG/DTG, two different mechanisms causing loss of mass were observed. The region between ambient temperature and 500 K was distillation. The second mechanism was visbreaking and cracking and it was observed between the region 500 and 800 K. Kinetic parameters of all the samples are determined by Coats and Redfern method and the results are discussed with regard to their accuracy and the ease of interpretation.
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    Cure Kinetics of Amine Cured Tetrafunctional Epoxy Blends with Poly(Styrene-Co-Acrylonitrile) (1999)
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    Journal of thermal analysis and calorimetry 56 (1999), S. 1033-1040 
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    ISSN: 1572-8943
    Keywords: cure kinetics ; DSC ; epoxy resin ; SAN ; thermoplastic blends
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Cure kinetics using a differential scanning calorimetry (DSC) technique were analyzed for a thermoplastic modified tetraglycidyl-4,4′-diaminodiphenylmethane (TGDDM) epoxy resin cured with diaminodiphenylsulphone (DDS), an aromatic diamine. The neat resin and its blends with the poly(styrene-co-acrylonitrile) (SAN) of various compositions were studied by applying a phenomenological model proposed by Kamal. Kinetic parameters were determined by fitting experimental data. This model gives a good description of cure kinetics up to the onset of vitrification. Diffusion control was incorporated to describe the cure in the latter stages of cure. The results showed that the addition of SAN did not alter the nature of the reaction, but the reaction rates and final conversions decreased when SAN contents increase, due to reduction of mobility of the reacting species.
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    Thermal Analysis, Microcalorimetry and Combined Techniques for the Study of Pharmaceuticals (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 1285-1304 
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    ISSN: 1572-8943
    Keywords: amorphous state ; combined techniques ; drug design ; drug product development ; drug substance ; drug technology ; DSC ; excipients ; failure investigations ; hydrates ; MDSC ; microcalorimetry ; pharmaceuticals ; polymorphism ; polymers ; preformulation ; process optimization ; purity ; quality control ; solvates ; stability ; sub-ambient DSC ; TG ; temperature resolved X-ray diffraction ; water interactions ; thermal microscopy ; water sorption-desorption
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Modern thermal analysis, microcalorimetry and new emerging combined techniques which deliver calorimetric, microscopic and spectroscopic data offer a powerful analytical battery for the study of pharmaceuticals. These techniques are very useful in all steps of development of new drug products as well as methods for quality control in production. The characterization of raw materials enables to understand the relationships between polymorphs, solvates and hydrates and to choose the proper development of new drug products with very small amount of material in a very short time. Information on stability, purity is valuable for new entities as well as for marketed drug substances from different suppliers. Excipients which vary from single organic or inorganic entity to complexes matrixes or polymers need to be characterized and properly controlled. The thermodynamic phase-diagrams are the basis of the studies of drug-excipients interactions. They are very useful for the development of new delivery systems. A great number of new formulations need proper knowledge of the behaviour of the glass transition temperature of the components. Semi-liquid systems, interactions in aqueous media are also successfully studied by these techniques.
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    Thermal Analysis, Microcalorimetry and Combined Techniques for the Study of the Polymorphic Behaviour of a Purine Derivative (1999)
    Springer
    Journal of thermal analysis and calorimetry 57 (1999), S. 61-73 
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    ISSN: 1572-8943
    Keywords: amorphous ; combined techniques for polymorphism ; DSC ; MKS 492 ; polymorphism ; purine ; quantitative determination ofamorphous and polymorphs ; solvent mediated transitions ; temperature resolved X-ray diffraction ; TG ; thermodynamic relation between polymorphs ; xanthine
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The polymorphic behaviour of the purine derivative MKS 492 was studied with investigations of suspensions of selected samples in different solvents and of samples obtained by crystallizations. The samples were analyzed by DSC, TG and X-ray diffraction. Six different crystalline modifications called A, B, B’, C, D and E and an amorphous form were identified. Four pure crystalline modifications, A, B, C and D have been manufactured and characterized by DSC, X-ray, IR, solubilities, densities, hygroscopicity and dissolution measurements. The four forms A, C, D and E are monotrop to the form B. The form B is enantiotrop to the form B’, which revealed the highest melting point of all known polymorphs. This form B’ is only stable at high temperature. Temperature resolved X-ray diffraction was very helpful for proper interpretation of the thermal events. The melting peaks of the forms A and C and the endothermic peak corresponding to the enantiotropic transition B into B’ occur in a narrow range of temperature. The form B which is the most stable one at room temperature has been chosen for further development. Quantitative methods to determine the content of the forms A, C and D in samples of form B or to determine the content of form A, B and D in form C have been developed by using X-ray diffraction. Limits of detection are 1 or 2%. For the quantitative determination of the amorphous fraction, X-ray diffraction and microcalorimetry are compared. For high amounts of the amorphous fraction, the X-ray diffraction method is preferred because it is faster. Microcalorimetry is very attractive for levels below 10% amorphous content. The lowest limit of detection is obtained by microcalorimetry, about 1%.
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    Pre-Eutectic Densification of Calcium Carbonate Doped with Lithium Carbonate (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 1461-1473 
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    ISSN: 1572-8943
    Keywords: CaCO3 ; densification ; kinetics ; Li2CO3
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Pressureless sintering of CaCO3 was carried out, with Li2CO3 (from 0.5 to 8 wt%) as an additive, under different pressures of CO2. Densification occurs between 600 and 700°C. Sintering above the eutectic temperature (T〉662°C) leads to the decomposition of calcium carbonate and the materials become expanded. At 620° under 1 kPa of CO2, a relative density of 96% is reached. Li2CO3 enhances the densification process and grain growth of calcium carbonate. CO2 pressure slows down densification and grain growth kinetics. These results are explained by the influence of carbonate and calcium ion vacancies on the sintering mechanisms.
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    Comparison of Experimental Methods and Theoretical Calculations on Crystal Energies of ‘Isoenergetic’ Polymorphs of Cimetidine (1999)
    Springer
    Journal of thermal analysis and calorimetry 57 (1999), S. 7-22 
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    ISSN: 1572-8943
    Keywords: crystal modifications ; DSC ; Gibbs free energy function ; molecular modelling ; solution calorimetry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The thermodynamic energy relationship between two crystal modifications of cimetidine was investigated and compared with differences in their processing properties with respect to transformation from one modification to the other. The crystal energies of the two modifications A and D were found to be almost identical and therefore the polymorphs are regarded as virtually isoenergetic crystals. This statement is based on DSC measurements of the melting points and of the enthalpies of fusion for the two crystal forms, which enable the calculation of the Gibbs free energy functions. Furthermore, the statement is supported by measurements of the enthalpies of solution in two different solvents. Both DSC and solution experiments reveal a slightly higher stability of the D modification with respect to the A form. In addition, tribomechanical treatment also indicates modification D to be the more stable one, as well as the higher density of the D form. No transformation during DSC at low heating rate was found which could be used in a stability consideration. As the explicit crystal structures of the two modifications are resolved, it was possible to calculate crystal energies theoretically as well. The theoretical results showed a remarkable difference in the crystal energies at zero degree Kelvin. Furthermore, they were just contradicting experimental findings by stating A being more stable than D. Possible reasons for this discrepancy and the feasibility of today's calculation methods with respect to prediction of stability properties are discussed.
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    Polymorphism of Acrylic and Methacrylic Acid Esters Containing Long Fluorocarbon Chains and Their Polymerizability (1999)
    Springer
    Journal of thermal analysis and calorimetry 57 (1999), S. 631-642 
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    ISSN: 1572-8943
    Keywords: DSC ; fluorocarbon chain ; polymerizability ; polymorphic behaviors ; X-ray diffraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The molecular aggregation of acrylic and methacrylic acid esters containing long-fluorocarbon chains: 2-(perfluoroalkyl)ethyl acrylate (FFnEA) and 2-(perfluoroalkyl)ethyl methacrylate (FFnEMA) (F(CF2)nCH2CH2OCOC(X)=CH2, where X=H, CH3 and n=6, 8, 10) was investigated by differential scanning calorimetry (DSC) and temperature controlled X-ray powder diffraction measurement. These compounds exhibited some characteristic polymorphic behaviors depending on the length of fluorocarbon chain and the α-position methyl group. The solid-state polymerization by γ-ray irradiation was studied for these compounds in the various crystal forms. In the solid-state polymerization, highest polymerizability was observed in the crystal form that exists in the highest temperature region for each compound.
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    Study of Ethyl Cellulose—Benzoic Acid Interactions in Matrices for Controlled Drug Release by DSC (1999)
    Springer
    Journal of thermal analysis and calorimetry 58 (1999), S. 29-38 
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    ISSN: 1572-8943
    Keywords: benzoicacid ; controlled release ; DSC ; ethyl cellulose ; FTIR
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The physical state of benzoic acid (BA) and its interaction with ethyl cellulose (EC) were examined in ethyl cellulose—benzoic acid matrices by Differential Scanning Calorimetry (DSC). The glass transition temperature (Tg) of EC of various matrices having BA in solid solution form (upto 27.7%) was reduced. The BA in matrices containing more than 38.9% drug exhibited distinct melting endotherms due to crystalline form. The peak temperatures of these endotherms were lowered and they broadened as the concentration was lowered. The solubility of BA increased at its melting point as compared to ambient temperature. The melting enthalpy of BA, when plotted as a function of its concentration yielded a straight line with intercept of 330 mg g−1 of matrix. This is the solubility of BA in EC at its melting temperature. Fourier Transform Infra Red Spectroscopy (FTIR) investigations confirmed that hydrogen bonding occurred between EC and BA through hydroxyl groups.
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    Thermal Behaviour and Decomposition Kinetics for Two Palladium(II) Complexes with 1-aminopyrene and its Derivative (1999)
    Springer
    Journal of thermal analysis and calorimetry 58 (1999), S. 383-391 
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    ISSN: 1572-8943
    Keywords: 1-aminopyrene (apyr) ; N-(2-pyridylmethylene)-1-pyrenylamine (pmpa) ; kinetics ; palladium(II)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The thermal decomposition studies for two palladium(II) complexes Pd(apyr)2Cl2 and Pd(pmpa)Cl2 (apyr=1−aminopyrene and pmpa=N−(2−pyridylmethylene)−1−pyrenylamine) were carried out in pure nitrogen using TG-DTG techniques. The non-isothermal kinetic parameters for the two complexes were evaluated employing the method suggested by Málek, Šesták, Koga et al. Based on the above results, thermal behaviour of the complexes were carefully discussed, which showed that not only the parameters value, but also the decomposition pattern and mechanism for complex 1 are different from complex 2.
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    Studies on the Kinetics of the First Order Autocatalytic Decomposition Reaction of Highly Nitrated Nitrocellulose (1999)
    Springer
    Journal of thermal analysis and calorimetry 58 (1999), S. 403-411 
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    ISSN: 1572-8943
    Keywords: first order autocatalytic reaction ; HNNC ; kinetics ; TG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The kinetics of the first order autocatalytic decomposition reaction of highly nitrated nitrocellulose (HNNC, 14.14%N) was studied by using thermogravimetry (TG). The results show that the TG curve for the initial 50% of mass-loss of HNNC can be described by the first order autocatalytic equation $$\frac{{{\text{d}}y}} {{dt}} = - 10^{16.4} \exp \left( { - \frac{{210380}} {{RT}}} \right)y - 10^{16.7} \exp \left( { - \frac{{171205}} {{RT}}} \right)y(1 - y)$$ and that for the latter 50% mass-loss of HNNC described by the reaction equations $$\frac{{dy}} {{dy}} = - 10^{16.3} \exp \left( { - \frac{{169483}} {{RT}}} \right)y\quad (n = 1)$$ and $$\frac{{dy}} {{dt}} = - 10^{16.8} \exp \left( { - \frac{{165597}} {{RT}}} \right)y^{2.61} \quad (n \ne 1)$$
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    Combination of DSC and X-ray Diffraction in the Study of the Phase Behaviour of Lipids: Mini-review (1999)
    Springer
    Journal of thermal analysis and calorimetry 58 (1999), S. 363-368 
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    ISSN: 1572-8943
    Keywords: DSC ; lipid ; phase behaviour ; synchrotron radiation ; X-ray diffraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The phase behaviour and phase stability of lipids are of importance in an understanding of the biological functions of cell membranes. Among a variety of physical techniques employed to study the phase behaviour and structural properties of polar lipids, differential scanning calorimetry and X-ray diffraction have proved to be successful and are the most frequently used methods. Applications involving a combination of the two techniques, particularly when synchrotron radiation is used as the light source of X-ray diffraction, are reviewed in this article.
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    Measurements of Heat of Zeolite Dehydration by Scanning Heating (1999)
    Springer
    Journal of thermal analysis and calorimetry 58 (1999), S. 653-662 
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    ISSN: 1572-8943
    Keywords: dehydration ; DSC ; TG ; water ; zeolites
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A procedure for measurement of the heat of zeolite dehydration by scanning heating has been designed. Simultaneous data on heat flow (DSC) and mass loss (TG) are required for evaluation. The heating rate depends on the experimental conditions (point-spread function, sample mass, crucible design, and calorimetric reproducibility). Dehydration measurements have three advantages as compared with the sorption procedure: i) one can investigate samples with irreversible dehydration; ii) no approximation model is needed for calculation of the partial molar heat of dehydration; and iii) the procedure is not labor-consuming. The procedure was tested on the natural zeolites heulandite, chabazite and mordenite. The results are close to those measured by the sorption procedure. The partial molar heat of dehydration was found to depend on the water content. It increases from 50 to 87 J mol−1 K−1 for heulandite, from 53 to 81 J mol−1 K−1 for chabazite, and from 51 to 71 J mol−1 K−1 for mordenite. The approximation of the heat of sorption by linear regression was found to be wrong. Detection of a ‘phase transitioN’ after this approximation has no meaning.
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    Transformation-Governed Heating Techniques in Thermal Analysis II. (1999)
    Springer
    Journal of thermal analysis and calorimetry 58 (1999), S. 725-739 
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    ISSN: 1572-8943
    Keywords: DDC ; DSC ; DTA ; transformation-governed TA
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The described instrumental method makes it possible that the quasi-static heating technique, well applicable to thermogravimetric measurements, (see Part I of this paper) can be used in the case of DTA and DSC examinations, too. Based on the new type of curves the characteristic transformation temperatures, the whole course of the transformation in dependence of sample temperature, the extent of the enthalpy change caused by the transformation or by its partial processes can accurately be determined. The essentially greater accuracy of the measurements — in comparison to the conventional ones — is due to the quasi-static heating technique which ensures that the transformations should take place under quasi-equilibrium conditions.
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    Spectroscopic and Thermal Studies on 2,4,6-trinitro Toluene (TNT) (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 173-185 
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    ISSN: 1572-8943
    Keywords: IRS ; kinetics ; mechanism ; nitro aromatic ; TA
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The kinetics and mechanism of the initial stage of thermal decomposition of 2,4,6-trinitro toluene (TNT), a widely used high explosive, have been studied, together with its morphology and evolved gaseous products using thermogravimetry (TG), differential thermal analysis (DTA), infrared spectroscopy (IR) and hot-stage microscopy. The kinetics of the thermolysis has been followed by IR after suppressing volatilisation by matrixing and by isothermal TG without suppressing volatilisation to simulate actual user conditions. The best linearity was obtained for Avrami-Erofeev equation for n=1 in isothermal IR and also in isothermal TG. The activation energy was found to be 135 kJ mol−1, with logA (in s−1) 12.5 by IR. The effect of additives on the initial thermolysis of TNT has also been studied. Evolved gas analysis by IR showed that CO2, NO2, NO and H2O are more dominant than N2O, HCN and CO. The decomposition involves the initial rupture of the C-NO2 bond, weakened by hydrogen bonding with the labile hydrogen atom of the adjacent CH3 group, followed by the abstraction of the hydrogen atom of the methyl group by NO2, generated in the initial step.
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    Effects of Added Urea and Alkylureas on Gel to Liquid-Crystal Transitions in Doab Vesicles (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 29-35 
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    ISSN: 1572-8943
    Keywords: alkylureas ; DOAB vesicles ; DSC ; gel-liquid transitions ; urea
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The gel to liquid-crystal transition for vesicles in aqueous solution formed by dimethyldi-n-octadecylammonium bromide (DOAB) occurs at 44.7°C. Moreover, the shapes of the scans recorded by a sensitive DSC microcalorimeter are very similar when the vesicular solutions are prepared starting with solid DOAB and comparable amounts of either solid urea or solid alkylureas. Therefore, the DOAB vesicles in aqueous solution accommodate this class of solutes without marked changes in the melting temperature and the enthalpy of the transition. The contrast with effects of added surfactants and simple organic solutes such as THF and ethanol is particularly significant.
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    Thermal Decompositions of (RE)Ba2Cu3O6 (RE=Y, Nd, Er) (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 691-698 
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    ISSN: 1572-8943
    Keywords: activation energy ; kinetics ; solid-state reactions ; superconductors ; thermogravimetry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Thermogravimetric in situ measurements of oxygen loss from (RE)Ba2Cu3O6 samples (RE=Y, Nd, Er) heated isothermally in a relatively high dynamic vacuum were made with a Cahn RG electrobalance. Single-phase orthorhombic samples of composition (RE)Ba2Cu3O7-x (highest oxygen content) were synthesized from stoichiometric (1:2:3) mixtures of high-purity (RE)2O3, BaCO3 and CuO. The original 1:2:3 mixture was prepared by the two-stage procedure described earlier. The crystal structure of the sample in the original orthorhombic phase was controlled by the X-ray powder method (CuKα radiation) using a Stadi P Stoe diffractometer with a position-sensitive detector. The decomposition curves are described by the sum of exponential terms corresponding to rapid and slow first-order processes in which differently sized grains of the powder samples are involved. The activation energies are estimated from appropriate Arrhenius plots.
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    Thermal and Spectroscopic Study of Dehydration of Lithium Formate Monohydrate Single-crystals (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 807-816 
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    ISSN: 1572-8943
    Keywords: DSC ; hydrogen-bond ; IR ; lithium formate monohydrate ; Raman spectroscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Differential scanning calorimetry (DSC) and thermogravimetric analysis (TG) of lithium formate monohydrate (LiHCOO·H2O) were performed in the temperature range 300–700 K. The DSC/TG measurements show that the dehydration process to anhydrous lithium formate (LiHCOO) is complex and occurs in two stages. The data are correlated to the structure and to the arrangement of the molecules in the crystal, including the hydrogen-bonding. Infrared transmittance and Raman spectra of this crystal are reported and commented on.
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    Thermal Decomposition of Strontium and Barium Malonates (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 789-796 
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    ISSN: 1572-8943
    Keywords: alkaline earth malonates ; DSC ; DTA ; kinetic parameters ; TG ; thermal decomposition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The thermal decomposition of strontium and barium malonates has been studied isothermally and non-isothermally employing simultaneous TG-DTG-DTA, DSC, XRD and IR spectroscopic techniques. DSC of these malonates has been recorded both in oxygen and nitrogen atmospheres. The decomposition is a single step process and the end product formed is carbonate. The energy of activation and frequency factor values for the decomposition of strontium malonate are 547 kJ mol−1 and 1041 s−1 respectively. The activation energy and frequency factor values for isothermal dehydration of barium malonate sester-hydrate are 57–111 kJ mol−1 and 107–1012 s−1 respectively and the corresponding values for decomposition from DSC are 499.5 kJ mol−1 and 1044 s−1 respectively. The higher thermal stability of strontium malonate as compared to that of barium salt is ascribed to its being anhydrous so that decomposition proceeds without restructuring. Their thermal stabilities have also been compared with that of respective oxalate salts.
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    Thermal Decompositions of the Molybdotellurates of Nickel(II) and Cobalt(II) (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 779-788 
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    ISSN: 1572-8943
    Keywords: cobalt ; dynamic and isothermal methods ; kinetics ; molybdotellurates ; nickel
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Molybdotellurates [M(H2O)6]3·[TeMo6O24], with M=Ni(II) and Co(II), were synthesized and characterized by single-crystal X-ray diffraction for compound 1 and X-ray powder diffraction for compound 2, EDAX, IR, electronic spectra in the solid phase and in solution, and magnetic properties. Thermogravimetry and differential scanning calorimetry of both compounds revealed a loss of 11 water molecules through an endothermal process with ΔH=800 kJ mol−1 for the nickel compound and ΔH=833 kJ mol−1 for the cobalt compound. The residual compounds were characterized by chemical analysis, IR and XPS spectroscopy
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    Physicochemical Studies and Thermal Decomposition Kinetics of Co(II), Ni(II), Cu(II) and Zn(II) Complexes of Citronellal Anthranilic Acid (1999)
    Springer
    Journal of thermal analysis and calorimetry 55 (1999), S. 817-831 
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    ISSN: 1572-8943
    Keywords: kinetics ; Schiff-bases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Cobalt(II), nickel(II), copper(II) and zinc(II) complexes of two new Schiff-bases, citronellal anthranilic acid and citronellal-5-bromoanthranilic acid have been synthesized. On the basis of spectral, magnetic and thermal data, octahedral structure was assigned to all complexes [ML2(H2O)2]. Thermal decomposition of these complexes was studied by TG. Kinetic parameters, viz activation energy, E, pre-exponential factor, A, and order of reaction, n, were calculated from the TG curves using mechanistic and non-mechanistic integral equations.
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    From Precursors to Thin Films - Thermoanalytical Techniques in the Thin Film Technology (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 7-15 
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    ISSN: 1572-8943
    Keywords: ALE ; CVD ; DSC ; DTA ; EGA ; EL display ; solar cell ; sol-gel ; spray pyrolysis ; super-conductor ; TG ; thin films
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Processing thin films for advanced applications, for instance in electronics and optoelectronics, involves several steps starting from precursor synthesis and ending up with the devices. Especially when optimizing the first steps of this chain of processes, thermoanalytical techniques play an important role. The review will focus on the main chemical deposition methods (CVD, ALE, spray pyrolysis, sol-gel) giving selected examples of problem-solving by thermal analysis. The techniques discussed are TG, DTA/DSC, EGA and their combinations. High-temperature X-ray diffraction (HTXRD) is also a powerful tool for in situ studies of thin films. The examples are taken from solar cell, superconductor and flat panel electroluminescent display technologies.
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    α-β Phase Re-Transformation Kinetics in Nickel Sulphide (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 429-435 
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    ISSN: 1572-8943
    Keywords: DSC ; nickel sulphide ; TG ; toughened glass ; X-ray diffraction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Nickel sulphide (NiS) was characterised using X-ray diffraction, thermal gravimetric analysis (TG) and differential scanning calorimetry (DSC). The 'as received' Millerite, stoichiometric NiS, observed to be slightly nickel deficient, was found to readily decompose in a nitrogen atmosphere at elevated temperatures (450°C max.) to the sulphur deficient Godlevskite, Ni7S6. DSC and X-ray measurements demonstrated that the high temperature form of the Godlevskite was readily stabilised at room temperature. The kinetics of the α-β re-transformation in Godlevskite were then investigated using DSC and were observed to be first order.
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    RCTA Techniques Used in Studies of Solid State Reactions in Inorganic Compounds (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 17-26 
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    ISSN: 1572-8943
    Keywords: kinetics ; reaction controlled thermal analysis ; stepwise isothermal analysis ; thermogravimetry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The Reaction Controlled Thermal Analysis techniques, RCTA, are very useful both in thermogravimetric and dilatometric studies. In the present paper this big family of techniques is divided into three main classes: Quasi-Isothermal techniques (QIA); Controlled Reaction Rate Thermal Analysis (CRTA) and Reaction (Event) Controlled Heating Rate Adaption. After a short presentation of these techniques and the general advantages of RCTA, two examples of kinetic studies on thermal decomposition of Ba- and Ce oxalates by using Stepwise Isothermal Analysis, SIA, introduced by the author is presented and discussed.
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    Thermochemistry of the Decomposition of Some Cobalt Compounds (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 547-552 
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    ISSN: 1572-8943
    Keywords: cobalt oxysalts ; DSC ; enthalpy of decomposition ; enthalpy of dehydration ; thermal decomposition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Differential scanning calorimetry (DSC) was used to determine the molar enthalpies of dehydration and decomposition of CoC2O4·2H2O, Co(HCOO)2·2H2O and [Co(NH3)6]2(C2O4)3·4H2O. The first stage of dissociation of each compound is a single-step dehydration both in air and argon atmospheres. The next stages are decomposition processes influenced by experimental parameters. The enthalpies of dehydration and decomposition vary from compound to compound in each atmosphere. The obtained data have been related to the macromechanisms proposed for the thermal decomposition and the parallel-consecutive decomposition-oxidation processes.
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    Isothermal and Non-Isothermal Kinetics When Mechanistic Information Available (1999)
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    Journal of thermal analysis and calorimetry 56 (1999), S. 783-792 
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    ISSN: 1572-8943
    Keywords: complex process ; DSC ; isoconversional methods ; kinetics ; model-free kinetics ; peak maximum evolution methods ; simulations
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract In the case of a complex mechanism of two parallel independent reactions, peak maximum evolution methods and model-fitting methods give only a mean value of the kinetic parameters, while isoconversional methods are useful to describe the complexity of the mechanism. Isothermal and non-isothermal isoconversional methods can be used to elucidate the kinetics of the process. Nevertheless, isothermal isoconversional methods can be limited by restrictions on the temperature regions experimentally available because of duration times or detection limits.
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    Feasibility Study of Crude Oil Fields by Thermal Analysis Techniques (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 947-951 
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    ISSN: 1572-8943
    Keywords: combustion ; crude oil ; DSC ; TG/DTG
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract This paper investigates the minimum oil content necessary for self-sustained combustion, which is introduced as a criterion for the selection of suitable reservoirs for in-situ combustion processes. Differential scanning calorimetry was used to determine the heat values of oil-limestone mixtures. The minimum temperature required for the total consumption of the fuel was obtained by thermogravimetry (TG/DTG). The minimum amount of oil necessary to sustain combustion was calculated from these two parameters and compared with the oil content of the reservoir. Reservoirs with an oil content greater than or equal to this minimum value were considered feasible. It was seen that the fields examined are generally not suitable for in-situ combustion processes.
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    Kinetic Study of Thermal Decomposition of the DMIT Complex of Cobalt (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 805-810 
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    ISSN: 1572-8943
    Keywords: cobalt ; dmit ligand ; kinetics ; non-linear method ; Zsakó method
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract In this work, a cobalt complex with dmit (1,3-dithiol-2-thione-4,5-dithiolate) as ligand was prepared and its thermal stability was studied by thermogravimetric analysis and kinetics by means of the Zsakó method and a non-linear method. For both methods, numerical binomial and polynomial filters were used, where points in the central interval were utilized.
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    Isothermal Crystallisation of PCL Studied by Temperature Modulated Dynamic Mechanical and TMDSC Analysis (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 1155-1161 
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    ISSN: 1572-8943
    Keywords: crystallisation ; DMA ; DSC ; PCL ; polymer ; temperature modulation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Temperature modulated dynamic mechanical analysis (TMDMA) was performed in the same way as temperature modulated DSC (TMDSC) measurements. As in TMDSC TMDMA allows the investigation of reversible and non-reversible phenomena during crystallisation of polymers. The advantage of TMDMA compared to TMDSC is the high sensitivity for small and slow changes in crystallinity, e.g. during re-crystallisation. The combination of TMDMA and TMDSC yields new information about local processes at the surface of polymer crystallites. It is shown that during and after isothermal crystallisation the surface of the individual crystallites is in equilibrium with the surrounding melt.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1010161113295
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    DSC Analysis of the Induction Period in the Vulcanisation of Rubber Compounds (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 1107-1113 
    Details
    ISSN: 1572-8943
    Keywords: differential scanning calorimetry ; induction period ; kinetics ; vulcanisation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Vulcanisation of rubber compounds was studied by DSC under isothermal and non-isothermal conditions. The parameters of an Arrhenius-like equation describing the temperature dependence of induction period have been obtained both from isothermal and non-isothermal measurements. A new method for obtaining the kinetic parameters from non-isothermal measurements, based on the dependence of onset temperature of vulcanisation peak on heating rate, is presented. Also, a procedure for the evaluation of temperature difference between the furnace and sample is proposed. It has been shown that the treatment of non-isothermal DSC measurements gives the kinetic parameters free of systematic errors. The new method can also be used for studying other reactions exhibiting the induction period.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1010148810569
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    The Influence of Annealing and Heavy Ion Irradiation of Multiple Melting and Crystallization in PBT Films (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 1141-1146 
    Details
    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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    URL: http://dx.doi.org/10.1023/A:1010157012386
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    Thermal Behaviour of Some Terpenoids (1999)
    Springer
    Journal of thermal analysis and calorimetry 56 (1999), S. 1353-1357 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; terpenoids ; TG ; thermal behaviour
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The terpenoids acetyl sitosterol, lupeol, acetyl diosgenin and stigmasterol were studied. Comparison of the thermogravimetric curves and the activation energies of the terpenoids suggested the following sequence of thermal stability: acetyl sitosterol 〈 acetyl diosgenin 〈 lupeol 〈 stigmasterol. The DSC curves allowed determination of the melting points and the degrees of purity. Comparison of the TG and DSC curves revealed the presence of phase transitions without mass loss that were attributed to rearrangements in the terpenoid molecules.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1010110624198
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    Lipid-similar Thermal Transition of Polyethylene Glycol Alkyl Ether Detergents (1999)
    Springer
    Journal of thermal analysis and calorimetry 57 (1999), S. 371-375 
    Details
    ISSN: 1572-8943
    Keywords: C14E8 ; detergent ; DSC ; polyethylene glycol tetradecyl ether ; thermal transition
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A narrow, reversible endothermic main transition is found in the aqueous micellar phase of octaethylene glycol tetradecyl ether (C14E8) by DSC, characterized by a transition temperature of 41°C and a ΔH value of 0.5 kcal mol−1, which is not observed by light scattering. This transition is assigned to a cooperative conformational rearrangement of the assembled amphiphilic detergent molecules and not to a micelle aggregation process. It is suggested that the detergent’s polar head group is primarily involved in this rearrangement.
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    URL: http://dx.doi.org/10.1023/A:1010158312153
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    On the Oximine Complexes of Transition Metals: Part 110: Spectroscopic and DSC study on some [Fe(Diox·H)2L2] and [Fe(Diox)3(BOR)2] type chelates and clathrochelates (1999)
    Springer
    Journal of thermal analysis and calorimetry 57 (1999), S. 433-445 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; iron(II)-oxime complexes ; kinetic parameters ; Mössbauer spectroscopy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A number of 15 [Fe(Diox#x00B7;H)2L2] type chelates and [Fe(Diox)3(BOR)2] clathrochelates (Diox#x00B7;H2 — dimethylglyoxime, glyoxime, propoxime, nyoxime, furyl-dioxime; L-pyridine, alkyl-pyridine derivatives, diethyl-phenyl-phosphine, diethyl-p-tolyl-phosphine) were obtained and characterized by means of far and middle FTIR and Mössbauer spectroscopic methods. Some structural problems were discussed on the basis of the optical data. The DSC measurements show the higher thermal stability of the clathrochelates without O—H⋯O intramolecular hydrogen bonds (with asymmetric octahedral structure), as compared to the [Fe(Diox#x00B7;H)2L2] trans, symmetric chelates containing O—H⋯O bonds. The kinetic parameters of the thermal decomposition of the complexes have been derived using the nomogram method.
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    URL: http://dx.doi.org/10.1023/A:1010155706218
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    Decoupled Molecular Dynamics of Glass-forming Liquids Confined in Nano-meter Pores (1999)
    Springer
    Journal of thermal analysis and calorimetry 57 (1999), S. 745-752 
    Details
    ISSN: 1572-8943
    Keywords: confinement effects ; DSC ; dynamic light scattering ; finite-size effects ; glass transition ; o-terphenyl
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Calorimetry is the method first used by Jackson and McKenna to study the effect of finite-size on the molecular dynamics of glass-formers confined in nano-meter scale pores. It was found that the glass transition is shifted to lower temperature as pore size decreases. Since then, other spectroscopic techniques have corroborated this finding and given more information on the molecular dynamics. These results are used to compare with the predictions of several theories of glass transition, and in particular the coupling model of the author.
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    URL: http://dx.doi.org/10.1023/A:1010169519847
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    Identification of Polyethylene by Differential Scanning Calorimetry: Application to forensic science (1999)
    Springer
    Journal of thermal analysis and calorimetry 57 (1999), S. 847-851 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; linear low-density polyethylene(LLDPE) ; low density polyethylene (LDPE) ; polymer blend ; thermal properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A forensic sample consisting of melt-recrystallized polymers that was recovered from the scene of a fire in a factory was identified by differential scanning calorimetry. The factory commonly used two kinds of film sheets, A and B, made by different manufacturers. It was necessary to decide whether the forensic sample related to material A or B. The forensic sample and reference samples of materials A and B were subjected to infrared spectroscopy and pyrolysis gas chromatograph mass spectrometry measurements, which revealed their polyethylene nature. The thermal behaviour of the samples was examined by differential scanning calorimetry (DSC) and they were found to be blends of two kinds of polyethylenes, low-density polyethylene and linear low-density polyethylene. The samples could be identified and distinguished from each other via the DSC measurements.
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    URL: http://dx.doi.org/10.1023/A:1010106612095
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    Estimation of the Critical Temperature of Thermal Explosion for the Highly Nitrated Nitrocellulose Using Non-isothermal DSC (1999)
    Springer
    Journal of thermal analysis and calorimetry 58 (1999), S. 369-373 
    Details
    ISSN: 1572-8943
    Keywords: critical temperature ; DSC ; HNNC ; non-isothermal
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Two methods for estimating the critical temperature (Tb) of thermal explosion for the highly nitrated nitrocellulose (HNNC) are derived from the Semenov's thermal explosion theory and two non-isothermal kinetic equations, dα/dt=Af(α)e−E/RT and dα/dt=Af(α)[1+E/(RT)(1–To/T)]e−E/RT, using reasonable hypotheses. We can easily obtain the values of the thermal decomposition activation energy (E), the onset temperature (Te) and the initial temperature (To) at which DSC curve deviates from the baseline of the non-isothermal DSC curve of HNNC, and then calculate the critical temperature (Tb) of thermal explosion by the two derived formulae. The results obtained with the two methods for HNNC are in agreement to each other.
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    URL: http://dx.doi.org/10.1023/A:1010155221958
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    Convexity requirement in the geometric-probabilistic approach to heterogeneous chemical kinetics (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 49-54 
    Details
    ISSN: 1572-8943
    Keywords: kinetics ; solid-phase reactions
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The convexity of localization forms, strictly required by conventional geometric-probabilistic formalism, is not in agreement with many experimental observations concerning solid-phase chemical reactions. In a discussion of the essence of this requirement, it is shown that it may be weakened for non-convex localization forms consistent with the symmetry of a solid reagent and described within the geometric-probabilistic approach in terms of planigons and Wigner-Seitz cells.
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    URL: http://dx.doi.org/10.1007/BF01979946
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    Spectroscopic and thermal studies on the decomposition of l,3,5-triamino-2,4,6-trinitrobenzene (TATB) (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 225-236 
    Details
    ISSN: 1572-8943
    Keywords: IR ; kinetics ; TG-DTG-DTA ; l,3,5-triamino-2,4,6-trinitrobenzene
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The kinetics of the thermal decomposition of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) in condensed state has been investigated by high temperature infrared spectroscopy (IR) and thermogravimetry (TG) in conjunction with pyrolysis gas analysis, differential thermal analysis (DTA) and hot stage microscopy. The decomposition proceeds in two main stages under isothermal conditions and the initial stage involving about 24% loss in weight obeys Avrami-Erofe'ev equation (n= 1), and is governed by an activation energy (E) of 150.58 kJ·mol−1 and log(A in s−1) 12.06. The second stage corresponding to 24 to 90% loss in weight gave best fit for Avrami-Erofe'ev equation,n=2, withE=239.56 kJ·mol−1 and log(A in s−1) 19.88 by isothermal TG. The effect of additives, on the initial thermolysis of TATB has also been studied. Evolved gas analysis by IR showed that NH3, CO2, NO2, HCN and H2O are produced in the initial stage of decomposition. The decomposition in KBr matrix in the temperature range 272 to 311.5°C shows relative preferential loss in the -NH2 to -NO2 band intensity which indicates that the rupture of C-NH2 bond, weakened also by the interaction of the NH2 with the neighbouring NO2 group, appears to be the primary step in the thermolysis of TATB.
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    URL: http://dx.doi.org/10.1007/BF01979963
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    Kinetics and mechanism of processes in the system FeSO4·7H2O-MnO2 (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 285-290 
    Details
    ISSN: 1572-8943
    Keywords: kinetics ; system FeSO4·7H2O-MnO2
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Processes which occur during the thermal treatment of system FeSO4·7H2O-MnO2 are of the interest for obtaining MnSO4, which can be easily soluted in water and separated from impurities in manganese slime in zinc metallurgy. Results of the experimental investigations of such processes are given in this paper. Kinetic parameters for the previously defined mechanism were determined using Borchardt and Daniels method.
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    URL: http://dx.doi.org/10.1007/BF01979968
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    Interpolymer complexes of a new type (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 347-352 
    Details
    ISSN: 1572-8943
    Keywords: DSC ; optical densities ; thermal stability ; three-component interpolymer complexes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A new type of three-component interpolymer complexes (3IPCM) formed by two similarly charged polyelectrolytes and an oppositely charged low molar mass compound was studied by DSC, NMR and X-ray methods. The low molar mass monobasic compounds in these complexes act as mediators. This type of complexes differs from earlier-obtained 3IPCM, which contained a dibasic low molar mass mediator. The present 3IPCM were obtained from two polymers (polyacrylic acid and sodium polyphosphate) and bases such as 4-vinylpyridine and 2-methyl-5-vinylpyridine.
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    URL: http://dx.doi.org/10.1007/BF02135012
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    Non-isothermal crystallization kinetics of hot drawn polyester films (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 377-385 
    Details
    ISSN: 1572-8943
    Keywords: crystallization ; drawing ; kinetics ; Kissinger ; Ozawa ; poly(ethylene terephthalate)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The non-isothermal crystallization kinetics of hot drawn poly(ethylene terephthalate) films were studied using the Kissinger and Ozawa equations. The influence of the initial drawing on the crystallization kinetics was investigated. The values of the apparent activation energy and of the Avrami exponent indicates that the nucleation and growth of crystallites depend greatly on the stress submitted to the samples.
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    URL: http://dx.doi.org/10.1007/BF02135016
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    Kinetics of curing reaction of a diglycidyl ether of bisphenol A/1,3-bisaminomethyl-cyclohexane (DGEBA/1,3-BAC) epoxy resin system (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 387-395 
    Details
    ISSN: 1572-8943
    Keywords: cure kinetics ; DSC ; epoxy resins ; gelation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract By employing differential scanning calorimetry (DSC) we have studied the kinetic of the cure reaction for a system containing a diglycidyl ether of bisphenol A (DGEBA) and 1,3-bisaminomethylcyclohexane (1,3-BAC) as a curing agent, using an isothermal approach over the temperature range of 60–110°C. We have determined the reached conversions at several cure temperatures and the reaction rates. The results showed that this cure reaction is autocatalytic. The experimental data were compared with the autocatalytic model proposed by Kamal, which includes two rate constants and two reaction orders. This model gives a good description of cure kinetics up to vitrification point. The activation energies for these rate constants were 44-57 kJ mol−1. From the gel time measurements the value obtained for the overall activation energy was 49.5 kJ mol−1.
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    URL: http://dx.doi.org/10.1007/BF02135017
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    Lifetime prediction of ABS polymers based on thermoanalytical data (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 465-470 
    Details
    ISSN: 1572-8943
    Keywords: ABS polymer ; DSC ; lifetime estimation ; thermooxidation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The service life of ABS polymer, stabilized by 2-(3,5-di-tert-butyl-4-hydroxyanilino)-4,6-bis(octylthio)-1,3,5-triazine and containing 50% of a modifying rubber component, was estimated from oxidative induction times measured by DSC in isothermal mode in the temperature interval 140–170°C. The lifetime of ABS powder at the actual temperature of drying was predicted by linear extrapolation according to Arrhenius. However, the extrapolated value was much longer than the real lifetime determined from the long-term oven aging tests at 70 and 90°C, simulating the industrial drying process. The effect of changes in the apparent activation energy of oxidation due to antioxidant consumption during polymer aging is discussed.
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    URL: http://dx.doi.org/10.1007/BF02135023
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    Thermochemical investigation of guest-host interactions in Werner clathrates of type [Ni(4-Etpy)4(NCS)2]·nG (G=naphthalene derivatives) (1996)
    Springer
    Journal of thermal analysis and calorimetry 46 (1996), S. 539-548 
    Details
    ISSN: 1572-8943
    Keywords: complexes ; DSC ; guest-host interactions ; X-ray
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The stoichiometry of thermal decomposition and the thermochemistry were studied for [NiL4(NCS)2] (I) as a host complex, and for its clathrates of type [NiL4(NCS)2]·2G, where L=4-ethylpyridine and guest molecule G=1-methylnaphthalene in clathrate (II), 1-chloronaphthalene in (III) or 1-bromonaphthalene in (IV). For I, the loss of volatile components proceeds in three steps (−2L, −L, −L); the first steps for II–IV also involve the release of G (−2G, −2L). DSC and X-ray powder measurements indicated a phase transition in the host lattice, and allowed differentiation of the escape of G and L molecules. The enthalpy changes give the following sequence of thermodynamic stability for the studied chlathrates: I〉II〉III.
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    URL: http://dx.doi.org/10.1007/BF02135033
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