27Al analysis

This NAA technique is based on the nuclear reactions 23Na(n,7)24Na and 41K(n/y)42K. Half-lives of the activated products are 15.0 hrs and 12.4 hrs, respectively. For Na analysis, the samples were irradiated in a specially designed thermal column to suppress the fast neutron reaction of 27Al(n,a)24Na which interferes with the reaction for Na. For K analysis, the proplnt samples were irradiated at a standard irradiation position of the reactor. For the Na irradiations, the neutron flux in the thermal column was in the order of 1010, whereas for the K assays it was approx 1012 neutrons/cm2-sec... 

The MWCNTs were purified using HF at 20 wt %. The samples were filtrated, washed with deionized water and dried at 100°C overnight. TGA analysis was carried out by heating at 10 °C/min from room temperature to 800°C. Nitrogen physisorption was used to determine BET surface area and BJH pore volume and size. 27Al MAS NMR spectra for the calcined samples were obtained. 

The details of this analysis, which is a generalization of a previous formalism for n = 1 [236], are beyond the scope of this review. Overall, the efficiency of R-INEPT and HMQC experiments has been found to be comparable, at least in applications involving 31P and 27Al. A major advantage of R-INEPT is that it can be combined with MQMAS or STMAS into a simple 2D heteronuclear correlation experiment, MQ/ST-J-HETCOR (Sect. 7.3). 

According to the structure and composition of materials and analysis requirements of the researcher, the following analysis techniques can be selected for the characterization of mesoporous materials XRD, TEM, adsorption-desorption (N2 or other gas), solid MAS NMR (29Si, 27Al, 13C, etc.), scanning electron microscopy (SEM), catalysis test, Fourier Transform infra-red (FT-IR), thermal analysis, UV-visible, and chemical analysis. IR, X-ray photoelectron spectroscopy (XPS), X-ray absorption near-edge structure XANES, extended X-ray absorption fine structure EXAFS and other spectral methods are commonly used to analyse metal elements such as Ti in the mesoporous material frameworks. 

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