Dispersion Elemental Analysis

Fig. 7.6. SEM micrograph of photopolymerized polypyrrole film on fiberglass. Electron dispersive elemental analysis confirms that bright spots are silver. Scale bar is 200 fim.

The electron-optical performance of the EPMA system is indistinguishable from that of a conventional scanning electron microscope (SEM) thus, EPMA combines all of the imaging capabilities of a SEM with quantitative elemental analysis using both energy- and wavelength-dispersive X-ray spectrometry. ... 

A dispersive element for spectral analysis of PL. This may be as simple as a filter, but it is usually a scanning grating monochromator. For excitation spectroscopy or in the presence of much scattered light, a double or triple monochromator (as used in Raman scattering) may be required. 

Table 8 shows results obtained from the application of various bulk and surface analysis methods to lithium metal at rest or after cyclization experiments, as well as at inert and carbon electrodes after cathodic polarization. The analytical methods include elemental analysis, X-ray photoelectron spectroscopy (XPS or ESCA), energy-dispersive analysis of X-rays (X-ray mi-... 

TEM observation and elemental analysis of the catalysts were performed by means of a transmission electron microscope (JEOL, JEM-201 OF) with energy dispersion spectrometer (EDS). The surface property of catalysts was analyzed by an X-ray photoelectron spectrometer (JEOL, JPS-90SX) using an A1 Ka radiation (1486.6 eV, 120 W). Carbon Is peak at binding energy of 284.6 eV due to adventitious carbon was used as an internal reference. Temperature programmed oxidation (TPO) with 5 vol.% 02/He was also performed on the catalyst after reaction, and the consumption of O2 was detected by thermal conductivity detector. The temperature was ramped at 10 K min to 1273 K. 

The number of surface atoms can be determined by chemisorption of probe molecules (H2, O2...), knowing the stoichiometry of the adsorbed species. As an example, in the case of Pt, the stoichiometry of irreversibly adsorbed hydrogen (H/Pts) and oxygen (0/Pts) at room temperature are both close to 1/1 [108-111]. Knowing the total number of atoms (elemental analysis) and the number of irreversibly adsorbed H and O, the dispersion of the particles (D = Pts/Pt) is then easily obtained. Note that the dispersion of these particles decreases when their size increases (Fig. 5). 

Conductive sample coatings are not needed because the gas molecules in the chamber replenish electrons on the sample surface to prevent charging. Direct observation of either wet or dry specimens is possible based on the continuously variable specimen environment. The instrument accommodates a micromanipulator, heatable stage, and gaseous environment. Energy dispersive x-ray (EDX) units can also be added to the sample chamber for elemental analysis. Samples can be analyzed in their natural state, at elevated relative humidities, elevated temperatures, and in various gas environments (including 100% relative humidity). 

Elemental analysis can also be performed on SEM samples using x-ray spectrometer attachments [55], The techniques are known as energy dispersive x-ray (EDX) analysis and wavelength dispersive x-ray (WDX) analysis and require installation of a detector in the sample chamber. 

The primary dispersion halo and wallrock alteration around the Elura deposit was established from integrated petrographic, mineralogical and geochemical (major-, minor- and trace-element) analysis of diamond drill core samples. Seventy eight samples of variably altered and unaltered host rocks, as well as 67 near-surface weathered equivalents, were analysed for major elements using fusion disc. X-ray fluorescence analysis (XRF). Trace elements were determined by pressed powder XRF analysis. Carbonate carbon... 

The composition of the surface-bound species must be considered they contribute to the stability of the dispersions of metal nanoparticles. In the case of electrostatically stabilized dispersions, the techniques to measure the interfacial electronic phenomena, including electrophoresis, electroosmosis, etc., are useful (54). In order to understand the composition (as well as structures) of the chemical species bound in the surface of metal particles, spectroscopic measurements used for common organic substances are used as well as the elemental analysis. 

Other modifications to the reaction conditions of the Brust-Schiffrin method, such as a reduction temperature of — 78 °C and the use of a hyperexcess of hexanethiol, results in an Au38(thiolate)24, based on observations, LDI-TOF mass spectrometry, TGA analysis and elemental analysis [69]. The influence of preparation temperature on the size and monodispersity of dodecylthiol monolayer protected gold clusters has also been reported. Both and SAXS measurements show that higher temperatures increase polydispersity. This modification of poly-dispersity may be related to the existence of a dynamic exchange of thiols at the particle surface with thiols in the solvent [70]. 

However, solvent extraction has proven to be more effective. When a sample of 1 g MTS-W was dispersed in 50 mL of ethanol and refluxed for 12 hours. Elemental analysis showed that ca. 50% of the organic templates could be removed without any apparent effect on the stability of the mesostrucutre. We have also found that the mesostructured compounds are stable in concentrated HC1 solution. For example, when MTS-W was stirred in a 12M HC1 solution at room temperature for 12 hours, ca. 30% of the organic templates could be removed without collapsing the mesostructure or decomposing the inorganic walls. 

The SEM is also used to do X-ray/elemental analysis. This technique is qualitative. X-ray analysis and mapping of the particular elements present is useful for the identification of inorganic fillers and their dispersion in compounds as well as inorganic impurities in gels or on surfaces and curatives, e.g., aluminum, silicon, or sulfur in rubber compounds and Cl and Br in halobutyl blends. (Figure 9)... 

Current methods used to image MCM-41 include (1) analytical transmission electron microscopy (TEM) to determine structure, size, morphology, and local chemical composition (2) energy-dispersive X-ray spectroscopy (EDXS) in a scanning electron microscope (SEM) to determine chemical composition 5 and (3) electron energy loss spectroscopy (EELS) for elemental analysis.6... 

---