Differential Scanning Calorimetry enthalpy

Fig. 11. Differential Scanning Calorimetry enthalpy overshoot of samples of different previous physical aging histories plotted as a function of cyclic stress amplitude for a fixed 8000 cycles (43). A aged at 130°C for 24 h aged at 130°C for 12 h aged at 130°C for 6 h. To convert MPa to psi, multiply by 145.

Fig. 12. Differential Scanning Calorimetry enthalpy overshoot as a fimction of cycle number at a given stress amplitude. Note the different scales in the data (43). aged at 130°C for 40 h and fatigued at 20 MPa O quenched from 165°C and fatigued at 31 MPa. To convert...

The crystal stmcture of glycerides may be unambiguously determined by x-ray diffraction of powdered samples. However, the dynamic crystallization may also be readily studied by differential scanning calorimetry (dsc). Crystallization, remelting, and recrystallization to a more stable form may be observed when Hquid fat is solidified at a carefully controlled rate ia the iastmment. Enthalpy values and melting poiats for the various crystal forms are shown ia Table 3 (52). 

Cure kinetics of thermosets are usually deterrnined by dsc (63,64). However, for phenohc resins, the information is limited to the early stages of the cure because of the volatiles associated with the process. For pressurized dsc ceUs, the upper limit on temperature is ca 170°C. Differential scanning calorimetry is also used to measure the kinetics and reaction enthalpies of hquid resins in coatings, adhesives, laminations, and foam. Software packages that interpret dsc scans in terms of the cure kinetics are supphed by instmment manufacturers. 

The differential scanning calorimetry (DSC) thermogram of niclosamide was obtained using a General V4 IC DuPont 2100. The data points represented by the curve shown in Fig. 2 were collected from 200 to 400°C using a heating rate of 5°C/ min. It was found that the compound melted at 231.66°C with an enthalpy of fusion equal to 69.31 J/g. 

Although there are other ways, one of the most convenient and rapid ways to measure AH is by differential scanning calorimetry. When the temperature is reached at which a phase transition occurs, heat is absorbed, so more heat must flow to the sample in order to keep the temperature equal to that of the reference. This produces a peak in the endothermic direction. If the transition is readily reversible, cooling the sample will result in heat being liberated as the sample is transformed into the original phase, and a peak in the exothermic direction will be observed. The area of the peak is proportional to the enthalpy change for transformation of the sample into the new phase. Before the sample is completely transformed into the new phase, the fraction transformed at a specific temperature can be determined by comparing the partial peak area up to that temperature to the total area. That fraction, a, determined as a function of temperature can be used as the variable for kinetic analysis of the transformation. 

Table 2 Melting Temperatures and Enthalpies of Fusion for Compounds Suitable as Reference Materials in Differential Scanning Calorimetry...

When one polymorph can be thermally converted to another, differential scanning calorimetry (DSC) analysis cannot be used to deduce the heat of transition between the two forms, and so solution calorimetry represents an alternative methodology. This situation was encountered when evaluating the polymorphs of losartan [140], Enthalpies of transition were obtained in water (A(A//sol) = 1.723 kcal/mol) and in A A-dimethylformarnide (A(A//S0 ) = 1.757 kcal/mol), with the equivalence in results demonstrating the quality of the results. Although enthalpy does not indicate stability, the authors deduced from solution calorimetry that form I was more stable than form II at ambient temperature. 

Reliable and internationally accepted techniques for screening are differential scanning calorimetry (DSC) and differential thermal analysis (DTA). These techniques can provide exothermic enthalpy of reaction and observed... 

Apart from the qualitative observations made previously about suitable solvents for study, the subject of solvates has two important bearings on the topics of thermochemistry which form the main body of this review. The first is that measured solubilities relate to the appropriate hydrate in equilibrium with the saturated solution, rather than to the anhydrous halide. Obviously, therefore, any estimate of enthalpy of solution from temperature dependence of solubility will refer to the appropriate solvate. The second area of relevance is to halide-solvent bonding strengths. These may be gauged to some extent from differential thermal analysis (DTA), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC) solvates of "aprotic solvents such as pyridine, tetrahydrofuran, and acetonitrile will give clearer pictures here than solvates of "protic solvents such as water or alcohols. 

Differential scanning calorimetry has been used88 to measure the enthalpy change, AH0 for the exothermic decarbonylation reaction... 

Differential scanning calorimetry has been used to measure89,90 the enthalpy of reaction for the displacement of a nitrogen donor ligand, L, from tungsten complexes [W(CO)6 L ] by carbon monoxide under isobaric conditions. The reaction is described by the equation... 

The enthalpies of phase transition, such as fusion (Aa,s/f), vaporization (AvapH), sublimation (Asut,//), and solution (As n//), are usually regarded as thermophysical properties, because they referto processes where no intramolecular bonds are cleaved or formed. As such, a detailed discussion of the experimental methods (or the estimation procedures) to determine them is outside the scope of the present book. Nevertheless, some of the techniques addressed in part II can be used for that purpose. For instance, differential scanning calorimetry is often applied to measure A us// and, less frequently, AmpH and AsubH. Many of the reported Asu, // data have been determined with Calvet microcalorimeters (see chapter 9) and from vapor pressure against temperature data obtained with Knudsen cells [35-38]. Reaction-solution calorimetry is the main source of AsinH values. All these auxiliary values are very important because they are frequently required to calculate gas-phase reaction enthalpies and to derive information on the strengths of chemical bonds (see chapter 5)—one of the main goals of molecular energetics. It is thus appropriate to make a brief review of the subject in this introduction. 

Differential scanning calorimetry (DSC) was designed to obtain the enthalpy or the internal energy of those processes and also to measure temperature-dependent properties of substances, such as the heat capacity. This is done by monitoring the change of the difference between the heat flow rate or power to a sample (S) and to a reference material (R), A

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ISO 11357-3 1999 Plastics - Differential scanning calorimetry (DSC) - Part 3 Determination of temperature and enthalpy of melting and crystallization ISO 11357-7 2002 Plastics - Differential scanning calorimetry (DSC) - Part 7 Determination of crystallization kinetics... 

Differential scanning calorimetry (DSC) and x-ray diffraction (XRD) are the techniques most widely used for the characterization of crystallinity and polymorphism of solid lipid particles. Although DSC is usually more sensitive in detecting crystalline material, XRD is much more reliable in determining the type of polymorph present in the dispersions because it provides structural data. In contrast, DSC can detect the type of polymorph only indirectly via the transition temperatures and enthalpies. Because these parameters may be different from those observed in the bulk material, particularly for small colloidal particles [1,62], assigmnent of polymorphic forms in DSC curves should be supported by x-ray data. 

The melting points, enthalpies, and associated entropies for a series of A -aryl-4//-benzo[ ][l,3]thiazin-2-amines 71 are presented in Table 3 <2004MI6291>. The melting points of the compounds determined by differential scanning calorimetry (DSC) agreed with the results obtained by hot-stage microscope. 

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