Optical microscopy crystalline material analysis

Polymer material/product characterisation crystallinity, amorphous content, phase analysis WAXS, WAXD, SAXS, SALLS, density, DSC, IR, Raman, s-NMR, AFM, optical microscopy, SEM, TEM... 

The use of solid state NMR for the investigation of polymorphism is easily understood based on the following model. If a compound exists in two, true polymorphic forms, labeled as A and B, each crystalline form is conformationally different. This means for instance, that a carbon nucleus in form A may be situated in a slightly different molecular geometry compared with the same carbon nucleus in form B. Although the connectivity of the carbon nucleus is the same in each form, the local environment may be different. Since the local environment may be different, this leads to a different chemical shift interaction for each carbon, and ultimately, a different isotropic chemical shift for the same carbon atom in the two different polymorphic forms. If one is able to obtain pure material for the two forms, analysis and spectral assignment of the solid state NMR spectra of the two forms can lead to the origin of the conformational differences in the two polymorphs. Solid state NMR is thus an important tool in conjunction with thermal analysis, optical microscopy, infrared (IR) spectroscopy, and powder... 

The role chitin as a material of highly ordered crystalline structure has been reported in the study [96]. X-ray diffraction analysis was carried out in order to find the changes of the crystalline structure upon the substitution reaction with NCO terminated prepolymer. The X-ray diffraction studies showed that crystallinity mainly depends on the concentration of chitin in the polyurethane backbone, crystallinity increased as the concentration of chitin into the final PU increased (Fig. 3.22). The crystallinity of some polymers was clearly observed by optical microscopic studies [114]. The results of X-ray diffraction experiments correlate with optical microscopy findings. A crystalline polymer is distinguished from an amorphous polymer by the presence of sharp X-ray Unes superimposed on an amorphous halo. Under an optical microscope, the presence of polycrystalline aggregates appear as spherulites [114]. The spheruhtes are made of small crystallites and grow Irom a nucleus at their centre. They consist of narrow chain folded lamellae growing radially. Since the fibrous crystals are radial, the chains folded with the lamellae are circumferentially oriented. From the evaluation of the X-ray and optical microscopic studies, it has been observed that the involvement of chitin in the PU formulation and have improved crystallinity of the final polyurethane. 

Although the above approaches may all be amenable to detection of crystallization in finished products, they can also be used to characterize the HME (i.e., prior to downstream processing). Further, many other techniques are often applied exclusively to the HME intermediate. For instance, optical microscopy offers excellent detectability of crystalline material in transparent extrudates. Dielectric analysis (DBA Alie et al. 2004 Bhugra et al. 2007, 2008) and thermally stimulated current IR spectroscopy (Shah et al. 2006 Rumondor and Taylor 2010), atomic force microscopy (ATM Lauer et al. 2013 Marsac et al. 2012 Price and Young 2004), and calorimetric methods have also been used to detect crystallization from an amorphous matrix (Baird and Taylor 2012 Pikal and Dellerman 1989 Avella et al. 1991). 

X-ray, electron scattering and thermal analysis remain the main tools in analyzing liquid crystalline order in condensed polymeric materials. The effectiveness of optical microscopy and of the compatibility rules formulated by Sackmann and Demus a decade ago and widely used in identification of mesophases formed by low molecular compounds (41, 42) is questionable in the case of... 

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