Mercury porosimetry method characteristics

In order to describe the geometrical and structural properties of several anode electrodes of the molten carbonate fuel cell (MCFC), a fractal analysis has been applied. Four kinds of the anode electrodes, such as Ni, Ni-Cr (lOwt.%), Ni-NiaAl (7wt.%), Ni-Cr (5wt.%)-NijAl(5wt.%) were prepared [1,2] and their fractal dimensions were evaluated by nitrogen adsorption (fractal FHH equation) and mercury porosimetry. These methods of fractal analysis and the resulting values are discussed and compared with other characteristic methods and the performances as anode of MCFC. 

The texture properties of the ultrathin porous glass membranes prepared in our laboratory were initially characterized by the equilibrium based methods nitrogen gas adsorption and mercury porosimetry. The nitrogen sorption isotherms of two membranes are shown in Fig. 1. The fully reversible isotherm of the membrane in Fig. 1 (A) can be classified as a type I isotherm according to the lUPAC nomenclature which is characteristic for microporous materials. The membrane in Fig. 1 (B) shows a typical type IV isotherm shape with hysteresis of type FIl (lUPAC classification). This indicates the presence of fairly uniform mesopores. The texture characteristics of selected porous glass membranes are summarized in Tab. 1. The variable texture demanded the application of various characterization techniques and methods of evaluation. 

The aim of this study is to eompare pore structure characteristics of two industrial catalysts determined by standard methods of textural analysis (physical adsorption of nitrogen and mercury porosimetry) and selected methods for obtaining parameters relevant to transport processes (multicomponent diffusion and permeation of gases). 

In the present work the meso- and macro-structural characteristics of the mesoporous adsorbent MCM-41 have been estimated with the help of various techniques. The structure is found to comprise four different length scales that of the mesopores, the crystaUites, the grains and of the particles. It was found that the surface area estimated by the use of small angle scattering techniques is higher, while that estimated by mercury porosimetry is much lower, than that obtained from gas adsorption methods. Based on the macropore characterization by mercury porosimetry, and the considerable macropore area determined, it is seen that the actual mesopore area of MCM-41 may be significantly lower than the BET area. TEM studies indicated that MCM-41 does not have an ideal mesopore structure however, it may still be treated as a model mesoporous material for gas adsorption studies because of the large radius of curvature of the channels. 

The testing of battery separators and control of their pore characteristics are important requirements for proper functioning of batteries. Mercury porosimetry historically has been used to characterize the separators in terms of percentage porosity, mean pore size, and pore size distribution." In this method, the size and volume of pores in a material are measured by determining the quantity of mercury. 

Two standard methods (mercury porosimetry and helium pycnometry) together with liquid expulsion permporometry (that takes into account only flow-through pores) were used for determination of textural properties. Pore structure characteristics relevant to transport processes were evaluated fiom multicomponent gas counter-current difhision and gas permeation. For data analysis the Mean Transport-Pore Model (MTPM) based on Maxwell-Stefan diffusion equation and a simplified form of the Weber permeation equation was used. 

The porous materials are known to be of importance in many different industrial processes e.g., catalysis, oil recovery, soil pollution, chromatography and separation. In all these systems, the pore structure is known to determine the physico-chemical characteristics. The pore shape and form is not easily determined. Microsporous material is not easily analyzed using electron microscope or diffraction methods, when the mean pore-radius is 2 -50 fjm. One generally uses mercury porosimetry for larger pores, which is based on a capillary phenomena. Other methods have also been used, which are based upon the effect of the curvature of a liquid on its solid - liquid phase transition equilibria, i.e. freezing point depression, vapor pressure or heat of evaporation. 

Thermoporometry probes the freezing characteristics of a pore liquid the data can be used to determine a pore size distribution and the shape of the pores. The method is expected to be sensitive to pores in the range between about 2 and 30 nm. In contrast to classical porosimetry (involving mercury or gas adsorption), the technique can be applied to gels rather than requiring dry samples. 

The determination of the buckling constant h by calibration from mercury intrusion porosimetry, or from nitrogen adsorption-desorption, can lead in some cases to different results. It is likely that, beyond the imprecision due to the method, the differences in pore sizes observed arise from a fundamental difference in the pore size concept. lUPAC proposed to define pore size as the distance between two opposite pore walls (Rouquerol, 1994). In the case of materials from the sol-gel process, this definition is not applicable, because pores are not included between walls, but are only delimited by interconnected filaments. In practice, it is considered that the sizes obtained from analysis methods of the texture of porous materials are characteristic pore sizes. Because the different analysis methods are based on different physical phenomena, it is not astonishing that they lead to slightly different characteristic pore sizes. Discrepancies resulting from using different characterization methods appear in several publications, often when the same material is analyzed by nitrogen adsorption-desorption and mercmy intrusion porosimetry (Smith, 1990, Brown, 1974, Milburn, 1988, Minihan, 1994). Me Enaney et al. noted that the distribution profiles obtained by different characterization techniques are often similar, but that differences, sometimes important, between the absolute values of characteristic pore sizes are almost unavoidable (Me Enaney et al., 1995). 

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