Authors:J. Farkas, É. Andrássy, Z. Formanek, and L. Mészáros
Farkas, J., Mohácsi-Farkas, Cs.: Application of differentialscanningcalorimetry in food research and food quality assurance. J Thermal Analysis 47 , 1787-1803 (1996)
Application of differentialscanningcalorimetry in
Authors:D. Hourston, M. Song, H. Pollock, and A. Hammiche
Modulated-temperature differential scanning calorimetry was used to measure the glass transition temperature,Tg, the heat capacity relaxation in the glassy state and the increment of heat capacity, δCp, in the glass transition region for several polymers. The differential of heat capacity with respect to temperature was used
to analyseTg and δCp simply and accurately. These measurements are not affected by complex thermal histories.
Differentialscanningcalorimetry (DSC) is extensively used in chemistry and physics to analyze, e.g. phase transitions of different compounds [ 1 , 2 ]. Recently this technique has been used with increasing
Authors:A. Samuni, D. Crommelin, N. Zuidam, and Y. Barenholz
This study was aimed to investigate the physicochemical changes induced in 200 nm extruded oligolamellar DPPC:DPPG (10:1)
liposomes by freezing, followed by γ-irradiation, in the absence and presence of 5 mM stable cyclic nitroxide radicals, 2,2,6,6-tetramethylpiperidine-1-oxyl
(Tempo) and 4-hydroxy-2,2,6,6-tetramethylpiperidine-1-oxyl (Tempol). The characterization is based on the use of differential
scanning calorimetry (DSC) and was aimed to differentiate the contribution of freezing and γ-irradiation in the presence and
absence of nitroxides. Liposomal preparations of DPPC/DPPG which have sub-, pre- and main-phase transitions in the temperature
range (0�C<Tm<50�C) were used.
Our results show that: (1) freezing modified and induced fusion to MLV as well as fission to SUV, (2) freezing did not fully
prevent the radiation-induced changes in the thermotropic characteristics of the liposomes, and (3) Tempo and Tempol did not
prevent the changes in thermotropic behavior caused as a result of freezing of the liposomal dispersion. These results demonstrate
that DSC is a powerful and sensitive tool in both physical and chemical studies of lipid assemblies.
Authors:E. Marti, E. Kaisersberger, and E. Füglein
Multicycle Differential Scanning Calorimetry (MCDSC) is a procedure where repeated temperature cycles are executed and the
measured data are superimposed for a selected number of cycles. Temperature cycles with a single sample are executed under
selected experimental conditions in one of these procedures, namely, the MCDSCs. The second one, MCDSCm is a procedure in which every identical temperature cycle starts with a new sample of the same substance of a similar mass.
The procedure MCDSCs using the same sample for a number of cycles is only applicable for substances and materials which are chemically and physically
stable under the selected experimental conditions. The application of MCDSC enhances two extremely important qualities of
a DSC measurement, namely, the sensitivity and the statistical base, both qualities with respect to the final data elucidated.
Another possibility by MCDSC also related to the enhanced sensitivity can lead the discovery of a phenomenon which hitherto
has not been observed. The most important result of any MCDSC application is the determination of the mean DSC curve within
the temperature interval of interest by superimposing the single curves point by point and by the division of the calorimetric
values obtained with the number of scans evaluated. The signal-to-noise-ratio (SNR) for the mean curve can be compared with
the value determined for one or even for all the single curves measured yielding the improvement factor achieved with a MCDSC
measurement. This experimentally determined improvement of the SNR can be compared with the value given on a statistical consideration
by Gauss as the square root of the number of cycles evaluated. The main aims of this article are to prove the practical application
of the procedure and the efficiency in case of rather small sample masses. Substances were selected with known enthalpy transitions
and, in addition, polystyrene was taken for a determination of the data for the glass transition by MCDSC. Rather small sample
masses in the order of micrograms as well as the experimental conditions have been selected for the measurements with 4,4′-azoxyanisole
and n-hexatriacontane with the expectation to get a value of SNR for the single curves of about unity or even below. Two aims should
be achieved with these experiments. First, the multicycle procedures and the data evaluation developed should be capable of
establishing, after performing of a certain number of cycles, a mean curve showing an improvement over the SNR with respect
to the single curves. Second, we should be able to get a rough estimation of the lower limit of the SNR for a single curve,
below the instrumental noise level of the DSC used, necessary to achieve with a MCDSC experiment a mean curve with a clearly
Authors:M. Ruiz, I. Reyes, A. Parera, and V. Gallardo
Differential scanning calorimetry was used to study the stability of omeprazole in two forms: granules and powder. The drug
was subjected to light, elevated temperature (40 and 60�C) and different pH values. The greatest alterations in stability
were caused by pH, followed by light.
Modulated temperature differential scanning calorimetry (MTDSC) is used to study simultaneously the evolution of heat flow
and heat capacity for the isothermal and non-isothermal cure of an epoxy-anhydride thermosetting system. Modelling of the
(heat flow related) chemical kinetics and the (heat capacity related) mobility factor contributes to a quantitative construction
of Temperature-Time-Transformation (TTT) and Continuous-Heating-Transformation (CHT) diagrams for the thermosetting system.
Authors:G. Van Assche, A. Van Hemelrijck, and B. Van Mele
The influence of temperature modulation and signal treatment (deconvolution procedure) of modulated temperature differential
scanning calorimetry is discussed with respect to the investigation of cure kinetics of thermosetting systems. The use of
a ‘dynamic’ heat capacity calibration is not important for this purpose due to normalization of the heat capacity signal in
all cure experiments. The heat flow phase during isothermal and non-isothermal cure is always small, giving rise to negligible
corrections on the heat capacity and reversing heat flow signals in-phase with the modulated heating rate. The evolution of
the heat flow phase contains information on relaxation phenomena in the course of the chemical reactions.
Authors:K. Cieśla, E. Svensson, and A.-C. Eliasson
Differential scanning calorimetry was applied in studies of the effect of gamma irradiation on the potato starch and wheat
flour. Essential differences were noticed between endothermal effects observed in concentrated suspensions of the initial
and irradiated potato starch and wheat flour heated at a rate of 2.5C min-1, while only small differences were noticed between gelatinization thermal effects recorded for ca. 20% suspensions of the
initial and irradiated potato starch samples heated at a rate 10C min-1. Moreover, in the case of wheat flour, a decrease of decomposition temperature of the amylose-lipid complex was concluded.
Differential scanning calorimetry (DSC) was used to measure the decomposition rates of four commercially used initiators,
2,2′-azobis(isobutyronitrile) 2,2′-azobis(2,4-dimethylvaleronitrile), dilauroyl peroxide and bis(4-t-butylcyclohexyl)peroxydicarbonate,
in dynamic mode, while the courses of methyl methacrylate polymerization with the listed initiators at 65, 75 and 85°C were
measured isothermally. From the DSC curves, the polymerization enthalpies, the overall reaction rate constants and the activation
energies for the initial steady-state polymerization were calculated. It was found that the polymerization enthalpy and the
kinetic parameters depended on the type of the initiator. An initiator with a shorter decomposition half-lifetime shifted
the onset of the gel effect to a higher conversion, intensified it and decreased the average molar mass of the polymer.