Electron microscopy fracturing

Figure 5.141. A glass fiber reinforced LCP composite is shown to have interesting morphology. A polished thin section is shown in polarized light (A) to exhibit a fine domain texture with some orientation of the polymer on the glass surfaces (see color insert). Scanning electron microscopy fracture views (B-D) show the tenacious adhesion of the LCP to the fibers. Fibrillar structures are oriented parallel to the fiber surface, and submicrometer sized domains are observed (D).

Analysis of results using mathematical/theoretical and numerical models, electronic microscopy, fracture mechanics and non-destructive testing. 

B. Donnio, D. N. Bruce, H. Delacroix, T. Gulik-Krzywicki. Freeze-fracture electron microscopy of thermotropic cubic and columnar mesophases. Liq... 

Scanning electron microscopy (thickness topography porosity barrier layers fracture sections) Energy dispersive X-ray analysis (EDX)... 

Cationic quaternary ammonium compounds such as distearyldimethylammonium-chloride (DSDMAC) used as a softener and as an antistatic, form hydrated particles in a dispersed phase having a similar structure to that of the multilayered liposomes or vesicles of phospholipids 77,79). This liposome-like structure could be made visible by electron microscopy using the freeze-fracture replica technique as shown by Okumura et al. 79). The concentric circles observed should be bimolecular lamellar layers with the sandwiched parts being the entrapped water. In addition, the longest spacings of the small angle X-ray diffraction pattern can be attributed to the inter-lamellar distances. These liposome structures are formed by the hydrated detergent not only in the gel state but also at relatively low concentrations. 

To ensure quality control material suppliers and developers routinely measure such complex properties as molecular weight and its distribution, crystallinity and crystalline lattice geometry, and detailed fracture characteristics (Chapter 6). They use complex, specialized tests such as gel permeation chromatography (2, 3), wide- and narrow-angle X-ray diffraction, scanning electron microscopy, and high-temperature pressurized solvent reaction tests to develop new polymers and plastics applications. 

In the matrix of PLA/ polycaprilactone (PCL)/OMMT nano-composites, the silicate layers of the organoclay were intercalated and randomly distributed (Zhenyang et at, 2007). The PLA/PCL blend significantly improved the tensile and other mechanical properties by addition of OMMT. Thermal stability of PLA/PCL blends was also explicitly improved when the OMMT content is less than 5%wt. Preparation of PLA/thermoplastic starch/MMT nano-composites have been investigated and the products have been characterized using X-Ray diffraction, transmission electron microscopy and tensile measurements. The results show improvement in the tensile and modulus, and reduction in fracture toughness (Arroyo et ah, 2010). 

FIGURE 12.11 Scanning electron microscopy (SEM) photomicrographs of the tensile fracture surface of the ethylene-propylene-diene monomer (EPDM) rubber-melamine fiber composites. A, before ageing and B, after ageing at 150°C for 48 h. Test specimen is cut in tbe direction parallel to the milling direction. (From Rajeev, R.S., Bhowmick, A.K., De, S.K., Kao, G.J.P., and Bandyopadhyay, S., Polym. Compos., 23, 574, 2002. With permission.)... 

With the freeze-fracture technique, the fracture plane passes through liposomes which are randomly positioned in the frozen sample. Some liposomes will be cut far from their midplane sections, others through their midplane section. Therefore, the analysis of freeze-fracture pictures requires corrections for nonequatorial fracture. Besides, corrections have to be made for the size-dependent probability of a vesicle being in the fracture plane (Jousma et al., 1987 Guiot et al., 1980). Recently, results with a new technique based on electron microscopy was discussed this technique allows analysis not only of liposome size, but also of the number of bilayers (Lauten-schlager et al., 1988). 

The dimer chains of Ca -ATPase can also be observed by freeze-fracture electron microscopy [119,165,166,172-174], forming regular arrays of oblique parallel ridges on the concave P fracture faces of the membrane, with complementary grooves or furrows on the convex E fracture faces. Resolution of the surface projections of individual Ca -ATPase molecules within the crystalline arrays has also been achieved on freeze-dried rotary shadowed preparations of vanadate treated rabbit sarcoplasmic reticulum [163,166,173,175]. The unit cell dimensions derived from these preparations are a = 6.5 nm b = 10.7 nm and 7 = 85.5° [175], in reasonable agreement with earlier estimates on negatively stained preparations [88]. 

Analysis of the lanthanide-induced crystalline arrays by negative staining (Fig. 5) or freeze-fracture electron microscopy reveals obliquely oriented rows of particles, corresponding to individual Ca -ATPase molecules [119]. The unit cell dimensions for the gadolinium-induced Ca -ATPase crystals are a = 6. l A, b = 54.4 A and y = 111°. Similar cell constants were obtained for the crystals induced by lanthanum, praseodymium and calcium. The unit cell dimensions of the Ei crystals are consistent with a single Ca -ATPase monomer per unit cell. The space group of the Eptype crystals is PI [119], while that of the E2 crystals is P2 [88,90]. 

Two distinct patterns of repeats were observed by electron microscopy of sectioned, negatively stained, frozen-hyd rated, or freeze-fractured specimens of Ca -ATPase crystals that represent different projections of the same structure... 

Sternberg, B., Sorgi, F.L., and Huang, L., New structures in complex formation between DNA and cationic liposomes visualized by freeze-fracture electron microscopy, FEBS Letters, 1994, 356, 361-366. 

Freeze fracture electron microscopy has revealed the distribution of the preceding three components as... 

Incorporated amount of PS II and freeze-fracture electron microscopy images of PS II reconstituted vesicles. 

Figure 5.9 Transmission electron microscopy (TEM) photographs of 3 wt % fluorinated glu-cophospholipid (13) dispersion at room temperature (a) cryo TEM (b) freeze-fracture TEM. Reprinted from Ref. 50 with permission of Academic Press.

Epi-illumination Subcellular imaging structures Freeze fracture Preparation of cellular ultrastructures in frozen-hydrated and living state for electron microscopy macromolecular organization of bilayer membranes... 

Subsequent to possible solubilization of membrane-bound proteins, solubilization must be verified. The criteria listed in Table 2 are relevant in assessing whether solubilization has been accomplished. To ascertain whether the solubilized protein has retained biological activity, membrane reconstitution (28) is attempted subsequent to detergent removal (24). Reconstitution is often visualized by electron microscopy employing either negative staining or freeze fracture. 

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