Molecular composites mobility measurement

Thermal Properties. Thermal properties include heat-deflection temperature (HDT), specific heat, continuous use temperature, thermal conductivity, coefficient of thermal expansion, and flammability ratings. Heat-deflection temperature is a measure of the minimum temperature that results in a specified deformation of a plastic beam under loads of 1.82 or 0.46 N/mm (264 or 67 psi, respectively). Eor an unreinforced plastic, this is typically ca 20°C below the glass-transition temperature, T, at which the molecular mobility is altered. Sometimes confused with HDT is the UL Thermal Index, which Underwriters Laboratories estabflshed as a safe continuous operation temperature for apparatus made of plastics (37). Typically, UL temperature indexes are significantly lower than HDTs. Specific heat and thermal conductivity relate to insulating properties. The coefficient of thermal expansion is an important component of mold shrinkage and must be considered when designing composite stmctures. 

Experimental variables such as temperature, flow rate, sample concentration and mobile phase composition can cause changes in the elution volume of a polymer [439,457,460-464]. Chromatographic measurements made with modem equipment are limited more by the errors in the absolute methods used to characterize the molecular weight of the calibration standards than any errors Inherent in the measurements themselves, since the determination of molecular weights by SEC is not an absolute method and is dependent on calibration [462]. The Influence of temperature on retention in SEC is not very great, since no strong sorptive interactions are involved in the retention mechanism. Temperature differences between the column and solvent delivery... 

With regard to quantitative measurements of APG surfactants in, e.g. environmental samples, the authors stressed that it was of crucial importance to promote the formation of the desired molecular (or adduct) ion in order to obtain reproducible mass spectra. If tuning of the ESI interface parameters did not suffice to yield abundant ions of the selected species, acquisitions of the mass spectrometric detector after negative ionisation in conjunction with appropriate selection of the mobile phase composition were used as an alternative despite the lower sensitivity in this mode [1,2],... 

The thermodynamic dead volume includes those static fractions of the mobile phase that have the same composition as the moving phase, and thus do not contribute to solute retention by differential interaction in a similar manner to those with the stationary phase. It is seen that, in contrast to the kinetic dead volume, which by definition can contain no static mobile phase, and as a consequence is independent of the solute chromatographed, the thermodynamic dead volume will vary from solute to solute depending on the size of the solute molecule (i.e. is dependent on both ( i )and (n). Moreover, the amount of the stationary phase accessible to the solute will also vary with the size of the molecule (i.e. is dependent on (%)). It follows, that for a given stationary phase, it is not possible to compare the retentive properties of one solute with those of another in thermodynamic terms, unless ( ), (n) and (fc) are known accurately for each solute. This is particularly important if the two solutes differ significantly in molecular volume. The experimental determination of ( ), (n) and( ) would be extremely difficult, if not impossible In practice, as it would be necessary to carry out a separate series of exclusion measurements for each solute which, at best, would be lengthy and tedious. 

The effect of solvent composition on the retention of a series of solutes, commonly used to measure column dead volumes, was also investigated by these authors. They employed mixtures of methanol and water as the mobile phase and measured the retention volume of the same salts together with a silica gel dispersion (containing particles 0.002 micron in diameter). They also measured the retention volume of the components of the mobile phase methanol, and water. The silica dispersion was chosen to simulate a solute of very large molecular size. The results they obtained are shown in figure (2). 

In composite systems, 2H NMR is particularly suited to investigate interfacial properties. Indeed, isolated nuclei are observed, which potentially allows spatially selective information to be obtained. It has been used to investigate polymer chain mobility at the polymer-filler interface, mainly in filled silicon (in particular PDMS) networks. The chain mobility differs considerably at the polymer-filler interface, and this may be interpreted in terms of an adsorbed polymer layer at the filler surface. T1 relaxation measurements allowed to determine the fraction of chain units involved in the adsorption layer, or equivalently, the thickness of the layer [75, 76, 77]. The molecular mobility and the thickness of the adsorption layer are very sensitive to the type of filler surface [78]. 

The solid-state NMR technique can be used to deduce quantitative measurements of phase composition, as has been reported for the anhydrate and dihydrate phases of carbamazepine. The applications of solid-state C-NMR spectra for the study of polymorphs and solvates can go beyond evaluations of resonance band positions, making use of additional spectral characteristics. For instance, studies of Tip relaxation times of furosemide polymorphs were used to show the presence of more molecular mobility and disorder in Form II, while the structure of Form I was judged to be more rigid and uniformly ordered. " ... 

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