Small-angle X-ray measurements have been used to study structural GDC-0199 (density) changes in polymers in the glassy state upon annealing, and neutron scattering is gaining wider use in the characterization of short-range two-dimensional
order in amorphous materials.18 Frequently used technique to detect the amount of crystalline material is differential scanning calorimetry (DSC).19 In DSC, samples are heated with a constant heating rate and the amount of energy necessary for that is detected. With DSC the temperatures at which thermal events occur can be detected. Thermal events can be a glass to rubber transition, (re)crystallization, melting or degradation. Furthermore, the melting- and (re)crystallization energy can be quantified. The melting energy can be used Selleckchem Androgen Receptor Antagonist to detect the amount of crystalline material.20 High-resolution 13C ss-NMR spectra are obtained using proton decoupling and magic angle spinning (MAS) and sensitivity enhancement is achieved by cross-polarization (CP). 13C ss-NMR has the advantage of being a nondestructive test method that provides information about the structure of the material. Like in any
other one-dimensional NMR method, it is possible to relate straightforwardly the integral of the CPMAS NMR signal to the number of 13C atoms involved, provided relaxation rates, Hartmann–Hahn conditions and cross-polarization rates are properly investigated for each species in the sample.21 In cases where the reference
mafosfamide spectra of the individual constituents are unavailable, quantitative estimation of defects, amorphous contents, or mixed phases by NMR can be done based on the comparison of the integrated intensity of two separate lines in the spectrum. A crystallinity index for microcrystalline cellulose was determined in the following way: CrI1/4a=a/(a+b)Where ‘a’ is the integration of peaks between 86 and 93 ppm and ‘b’ is the integration of peaks between 80 and 86 ppm. However, this type of analysis can sometimes be tricky especially if the two lines under scope are overlapping and cannot be easily deconvoluted. These difficulties can be overcome by resorting to other independent measurements like T1 or T1r relaxation times of 1H or 13C, relying on the expected difference in the mobility of amorphous and crystalline regions. In MTDSC, a sinusoidal wave modulation is superimposed over the conventional linear (or isothermal) heating or cooling temperature program. MTDSC is based on the same theory as conventional DSC, in which the heat flow signal is a combination of the specimen heat capacity Cp, t (heat-rate dependent component) and of any temperature dependent, often irreversible, ‘kinetic’ component.