Pore size diameter method

Specific surface areas and micropore volumes were obtained from nitrogen adsorption - desorption isotherms at -196°C using Micromeritics ASAP 2010. Prior to the measurements all powdered samples were degassed at 175 °C under vacuum 10 6 Torr for 6 hours. The total surface area was calculated using BET equation. The method of Horvath and Kawazoe was used to determine the pore size diameters of the product. 

Among all the precursors studied, precursor 2a appears to be the most useful precursor of nanocrystalline mesoporous Sn02 for application purposes. In comparison with 2d and 2f, compound 2a provides pure cassiterite tin dioxide materials with very low amounts of carbon from calcination at 400 °C, owing to the rather facile elimination of the p-phenylene spacer. After calcination at 400 and 500 °C, the BET surface area (110 and 70 m g ), the mean pore size diameter (5 and 6.5 nm) and the mean crystallite size (4.5 and 7 nm) are close to those reported for tin dioxide materials prepared by the template method after... 

The major design concept of polymer monoliths for separation media is the realization of the hierarchical porous structure of mesopores (2-50 nm in diameter) and macropores (larger than 50 nm in diameter). The mesopores provide retentive sites and macropores flow-through channels for effective mobile-phase transport and solute transfer between the mobile phase and the stationary phase. Preparation methods of such monolithic polymers with bimodal pore sizes were disclosed in a US patent (Frechet and Svec, 1994). The two modes of pore-size distribution were characterized with the smaller sized pores ranging less than 200 nm and the larger sized pores greater than 600 nm. In the case of silica monoliths, the concept of hierarchy of pore structures is more clearly realized in the preparation by sol-gel processes followed by mesopore formation (Minakuchi et al., 1996). 

Specific surface area (SSA), total pore volume and average pore diameter were measured by N2 adsorption-desorption isotherms at 77K using Micromeritics ASAP 2020. The pore size was calculated on the adsorption branch of the isotherms using Barrett-Joyner-Helenda (BJH) method and the SSA was calculated using the Brunauer-Emmett-Teller (BET) method. 

SBA-15 samples with diameters from 5 to 10 nm have been prepared by tuning the temperature of the first step of the synthesis [5], MCM-41 has been prepared in the presence of hexadecyl trimethyl ammonium by using methylamine as pH-controlling agent [6], The pore size from N2 adsorption at 77 K has been evaluated by the Broekhoff and de Boer method, shown to correctly evaluate the pore size of ordered mesoporous silicas [7]. 

Pores are classified into two types open pores, which connect to the outside of the material, and the closed pores, which are totally within the material. Penetrating pores are kind of open pores these have at least two openings located on two sides of a porous material. Penetrating pores are permeable for fluid, and therefore are important in applications such as filters. Many porous materials have been used in many applications. They are classified by many different criteria such as pore size, pore shape, materials and production methods. Classification by pore size and by pore shape is useful while considering the applications of porous materials. The classification of porous materials by pore size (according to Schaefer30) differentiates between microporous pores (pore diameter < 2 nm), mesoporous pores (2 nm < pore diameter <50 nm) and macroporous pores (pore diameter > 50 nm). 

Thus, either type I or type IV isotherms are obtained in sorption experiments on microporous or mesoporous materials. Of course, a material may contain both types of pores. In this case, a convolution of a type I and type IV isotherm is observed. From the amount of gas that is adsorbed in the micropores of a material, the micropore volume is directly accessible (e.g., from t plot of as plot [1]). The low-pressure part of the isotherm also contains information on the pore size distribution of a given material. Several methods have been proposed for this purpose (e.g., Horvath-Kawazoe method) but most of them give only rough estimates of the real pore sizes. Recently, nonlocal density functional theory (NLDFT) was employed to calculate model isotherms for specific materials with defined pore geometries. From such model isotherms, the calculation of more realistic pore size distributions seems to be feasible provided that appropriate model isotherms are available. The mesopore volume of a mesoporous material is also rather easy accessible. Barrett, Joyner, and Halenda (BJH) developed a method based on the Kelvin equation which allows the calculation of the mesopore size distribution and respective pore volume. Unfortunately, the BJH algorithm underestimates pore diameters, especially at... 

Another method to measure pore size distribution is capillary flow porometry [202,203], in which a sample material is soaked with a low surface tension liquid that fills all its pores. Then, gas pressure is applied on one side of the sample in order to force the liquid out of the pores. At low pressures, the flow rate is close to zero however, as the pressure increases, the flow rate also increases and the amount of liquid inside fhe pores decreases. Thus, the flow rate is determined as a function of pressure and is then used to calculate the desired pore characteristics, such as pore size distribution, largest pore diameter, and mean flow pore diameter. 

Membranes with extremely small pores ( < 2.5 nm diameter) can be made by pyrolysis of polymeric precursors or by modification methods listed above. Molecular sieve carbon or silica membranes with pore diameters of 1 nm have been made by controlled pyrolysis of certain thermoset polymers (e.g. Koresh, Jacob and Soffer 1983) or silicone rubbers (Lee and Khang 1986), respectively. There is, however, very little information in the published literature. Molecular sieve dimensions can also be obtained by modifying the pore system of an already formed membrane structure. It has been claimed that zeolitic membranes can be prepared by reaction of alumina membranes with silica and alkali followed by hydrothermal treatment (Suzuki 1987). Very small pores are also obtained by hydrolysis of organometallic silicium compounds in alumina membranes followed by heat treatment (Uhlhom, Keizer and Burggraaf 1989). Finally, oxides or metals can be precipitated or adsorbed from solutions or by gas phase deposition within the pores of an already formed membrane to modify the chemical nature of the membrane or to decrease the effective pore size. In the last case a high concentration of the precipitated material in the pore system is necessary. The above-mentioned methods have been reported very recently (1987-1989) and the results are not yet substantiated very well. 

For membranes with pore diameters smaller than 3.5 nm, the nitrogen adsorption/desorption method based on the widely used BET theory ean be employed. This measurement technique, however, is good only for pore diameters ranging from 1.5 nm to 100 nm ( = 0.1 micron). Typical data from this method are split into two portions adsorption and desorption. The nitrogen desorption curve is usually used to describe the pore size distribution and corresponds better to the mercury intrusion curve. Given in Figure... 

The diameters of the pores of the surface layer of Loeb-Sourlrajan-type cellulose acetate membranes have been reported by several authors (1-6). The reported values of the diameters cover the range between 10 A and 60 A. For electron microscopic observations, the replication method must be used. In order to obtain the excellently contrasted Images the surface of the sample Is shadowed with heavy metals In vacuum. In many cases the Pt-Pd alloy has been used as a pre-shadowlng metal. But the resolution of the Pt-Pd replica Is at the level of about 50 A, since the size of the evaporated particles Is between 20 X and AO X (7, 8, 9). If the pore sizes are In the range of the above-mentioned level, we cannot observe them. 

Invasiveness of the chemiluminescence (CL) lines was measured by in vitro and in vivo methods. The in vitro monitoring process comprised the movement of cells across a membrane of defined pore size within a specially designed growth chamber or MlCS (membrane invasion culture system). A 10-p diameter Nucleopore membrane was coated with a mixture of laminin (to promote invasion), collagen, and gelatin. Cells were added to the top side of the chamber in media and the extent of cell movement into the bottom of the chamber (invasion) through the membrane determined. 

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