Titration Transmission electron microscopy

Portnaya, I., Cogan, U., Livney, Y.D., Ramon, O., Shimoni, K., Rosenberg, M., Danino, D. (2006). Micellization of bovine p-casein studied by isothermal titration microcalorimetry and cryogenic transmission electron microscopy. Journal of Agricultural and Food Chemistry, 54, 5555-5561. 

Preparation and characterization of the metal deposits. Pt deposit was made by impregnation with PtClg and reduction in H2at 753 K. The Pt particle size distribution was determined by transmission electron microscopy (TEM) (8, 9 ) (Figure 3) and H2, O2 chemisorptions and titrations (43). The Pt particle size distribution was narrow with a surface weighted mean diameter of ca. 2 mn, almost independent of the Pt content between 0.5 and 10 wt (9 ), provided the preparation method, which includes a treatment in O2 before the reduction, was thoroughly followed. 

The various latexes were characterized with respect to particle size and size distribution, surface charge and functional group density, and electrophoretic mobility behavior. As observed by transmission electron microscopy all latexes were found highly monodisperse with a uniformity ratio between 1.001 and 1.010, a property due to the short duration of the nucleation period involved in the various radical-initiated heterogeneous polymerization processes. The surface charge density was determined by a colorimetric titration method reported elsewhere [13]. 

For supported metal catalysts, no simple calculation is possible. A direct measurement of the metal crystallite size or a titration of surface metal atoms is required (see Example 1.3.1). TWo common methods to estimate the size of supported crystallites are transmission electron microscopy and X-ray diffraction line broadening analysis. Transmission electron microscopy is excellent for imaging the crystallites, as illustrated in Figure 5.1.5. However, depending on the contrast difference with the support, very small crystallites may not be detected. X-ray diffraction is usually ineffective for estimating the size of very small particles, smaller than about 2 nm. Perhaps the most common method for measuring the number density of exposed metal atoms is selective chemisorption of a probe molecule like H2, CO, or O2. 

The stability and suitability of the formulations also needs to be determined, for example, whether the viscosity of the formulation is suitable for the administration route and is stable over time. The water content is a parameter that often has a direct influence on the stability of solid formulations and may influence the appearance of freeze-dried products immensely. Karl-Fisher titration, thermogravitometric analysis (TGA), or DSC is normally used to determine the water content. Various microscopic techniques, where both macroscopic and microscopic appearance of formulation can be determined, such as particle appearance by scanning electron microscopy (SEM) or transmission electron microscopy (TEM), are usually only needed for special formulation. There are several other methods, but which one to choose depends entirely on the formulation and the critical parameters (149,150). 

As for all catalysts, well-characterized samples are necessary to be able to relate the catalytic performance to physico-chemical properties. Transmission electron microscopy (TEM) and X-ray absorption spectroscopy (XAFS) were used in this study to characterize the stabilized metal colloid. The necessity of such extensive characterization of particle size has been outlined by Harada et al. [6,7] showing that the formation of aggregates may be overlooked and misinterpreted as large metal particles when using TEM alone. The actual availability of the polymer stabilized surface has been probed by hydrogen/oxygen titration adopted from the description of Bernard et al. [8]. 

Cationic latex particles with surface amino groups were prepared by a multi-step batch emulsion polymerisation. Monodisperse cationic latex particles to be used as the seed were synthesised first. Then the amino-functionalised monomer, aminoethylmethacrylate hydrochloride, was used to synthesise the final functionalised latex particles. Three different azo initiators were used 2,2 -azobisisobutyramidine dihydrochloride, 2,2 -azobisdimethyleneisobutyramidine dihydrochloride, and 2,2 -azobisisobutyronitrile. Hexadecyltrimethylammonium bromide was used as the emulsifier. The latices were characterised by photon correlation spectroscopy to study the mean particle diameters, transmission electron microscopy to deteimine the particle size distributions, and hence the number- and weight-average diameters and the polydispersity index. The conversion was determined gravimetrically, the surface density of the amino groups was detemiined by conductimetric titrations, and the... 

---