Measurement methods scanning electron microscopy

The deactivated catalyst was studied by several methods scanning electron microscopy (SEM)-energy dispersive spectroscopy (EDS), infrared spectroscopy (IR), and by extracting water-insoluble phosphorus. The SEM-EDS studies gave no useful results. IR absorption was measured on samples that were mulled in mineral oil. Comparisons of IR spectra were made with samples of y -alumina and aluminum phosphate. Determination of total P in the deactivated sample, presumed to be present as water-insoluble aluminum phosphate, was made by standard wet chemical analysis dissolution in hot, dilute HCl followed by colorimetric determination of phosphate. ... 

The interface properties can usually be independently measured by a number of spectroscopic and surface analysis techniques such as secondary ion mass spectroscopy (SIMS), X-ray photoelectron spectroscopy (XPS), specular neutron reflection (SNR), forward recoil spectroscopy (FRES), scanning electron microscopy (SEM) and transmission electron microscopy (TEM), infrared (IR) and several other methods. Theoretical and computer simulation methods can also be used to evaluate H t). Thus, we assume for each interface that we have the ability to measure H t) at different times and that the function is well defined in terms of microscopic properties. 

The major gaseous components were analyzed by a gas chromatograph equipped with a TCD and a molecular sieve 13X column. The specific surface areas of carbon produced were measured by the BET method(ASAP 2010, Micromeritics). The morphology and particle size of the formed carbon were investigated by the scanning electron microscopy(S-4200, Hitachi... 

The pH, EC and Fe3+ were used as control parameters. The first two were measured with an Orion probe combined pH/ATC electrode Triode and a conductivity cell DuraProbe ref. 0133030. Fe3+ was determined by molecular absorption (thiocyanate method). Mineralogical composition of the precipitates was determined by X-ray powder diffraction (XRD). Scanning electron microscopy, combined with an energy dispersive system (SEM-EDS), allowed the observation of morphological and compositional aspects of the precipitates. 

In light of the fact that coal ash is measured by removal (combustion) of the organic part of the coal, there are methods for measuring the mineral matter content of coal. Such a method involves demineralization of the coal that depends on the loss of weight of a sample when it is treated with aqueous hydrofluoric acid at 55 to 60°C (130 to 140°F) (Radmacher and Mohrhauer, 1955 Given and Yarzab, 1978 ISO 602). However, pyrite is not dissolved by this treatment and must be determined separately. Other methods include the use of physical techniques such as scanning electron microscopy and x-ray diffraction (Russell and Rimmer, 1979). 

The phase composition from the surface to the interior of the samples was determined by X-ray diffractometry (XRD) through successive grinding of the surface at 100 pm intervals. The microstructural characterization of the sintered specimens was achieved by scanning electron microscopy (SEM) in backscattered mode. The hardness change from the surface to the interior of the sample was measured by the Vickers indentation method at 19.6 N load. 

The sizing methods involve both classical and modem instrumentations, based on a broad spectrum of physical principles. The typical measuring systems may be classified according to their operation mechanisms, which include mechanical (sieving), optical and electronic (microscopy, laser Doppler phase shift, Fraunhofer diffraction, transmission electron miscroscopy [TEM], and scanning electron microscopy [SEM]), dynamic (sedimentation), and physical and chemical (gas adsorption) principles. The methods to be introduced later are briefly summarized in Table 1.2. A more complete list of particle sizing methods is given by Svarovsky (1990). 

Microscopy is often referred to as an absolute method for the determination of size and size distribution of small particles because it allows direct visualization and measurements of individual particles. Three commonly used types are optical microscopy, transmission electron microscopy (TEM), and scanning electron microscopy (SEM). 

Other analytical methods can also be applied for the detection of F in archaeological artefacts, especially when it is possible to take a sample or to perform microdestructive analysis. These are namely the electron microprobe with a wavelength-dispersive detector (WDX), secondary ion mass spectrometry (SIMS), X-ray fluorescence analysis under vacuum (XRF), transmission electron or scanning electron microscopy coupled with an energy-dispersive detector equipped with an ultrathin window (TEM/SEM-EDX). Fluorine can also be measured by means of classical potentiometry using an ion-selective electrode or ion chromatography. 

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