Silica pore size

Manufacturer Product Type of silica Pore size (nm) Particle Size Distribution (pm) Excitation Wavelength (nm) Binde... 

Sander et al. [63] investigated the effect of microparticulate silica pore size on the properties of solution-polymerized Cig stationary phases and observed both an increase in bonding density and shape recognition for wider pore (>120 A) silica. A size-exclusion mechanism was proposed, in which the reaction of the silane polymer on the surface is enhanced for wide pores and reduced for narrow pores. Polymeric Ci8 phases prepared on substrates with narrow pores exhibited monomeric-like chromatographic properties. This effect may be the result of an increase in competitive surface linkage with the less sterically hindered monomers that coexist with the bulkier oligomers that have polymerized in the reaction solution (Figure 5.13). 

Instability of the mutant AChE can be a problem with up to 50% of its activity in solution being lost in 10 days. This led to a study in which the enzyme was immobilised in porous silica (pore size 10 nm) or porous carbon (<70nm) beads [36]. The AChE is known to be approximately 6nm in size and therefore it is thought that entrapment within the pores could well inhibit unfolding of the enzyme, so enhancing its stability. 

The silica pore size is up to 30 times higher (catalyst F) than the zeolitic pore size. Catalysts D, E and F both differ in pore size and acidity. The effect of these characteristic data is not clear. An optimum seems to exist for catalyst D. However, it cannot be excluded that different manufacturing procedures may result in different catalytic performances. 

Fig. 30. ATR-IR spectra of CO2 (bending mode) in the bulk (dashed lines) and within a layer of mesoporous silica (pore size 14.5 nm, solid lines) as a function of relative pressure. Conditions 294 K, = (a) 0.829, (b) 0.989, (c) 0.993, and (d) 1.00. Spectra are offset for clarity, and spectra (d) are scaled by a factor of 0.25. The reference spectra (both for the bulk and the silica phase) were recorded in the absence of CO2 94).

Useful separations of oligosaccharides have been achieved using reversed-phase h.p.l.c. Malto-oligosaccharldes were separated up to DP 9 with water as eluent, better resolution being attained at lower temperatures (down to 5°C). Retention was significantly influenced by silica pore size and alkyl chain length, decreasing... 

Poly-L-Lysine Poly-L-lysine (PLL) has been implicated in silica formation because of its abiUty to adopt an a-helix, 3-sheet or random coil conformation. PLL is an excellent silica template due to its ability to create different sihca morphologies by simply changing the reaction conditions to afford a specific secondary structure. Hawkins and coworkers have shown that silica pore sizes could be modified by changing the secondary structure of the polyamine [82]. For example, silica composites that are formed by a-helix PLL under basic conditions (pH 11.2) produced 1.5 run pore sizes, whereas silica formed using PLL P-sheets (heated to -52 °C) resulted in larger pore sizes (-1.5-8nm). In both cases, silica formation was dependent on the PLL concentration and reaction conditions. 

Fig. 3.18 Pore size distributions of a silica geP GSSO, calculated from the desorption branch of the isotherm at 77 K by dilTerent methods. (A) x,...

In using the table for pore size calculations, it is necessary to read off the values of the uptake from the experimental isotherm for the values of p/p° corresponding to the different r values given in the table. Unfortunately, these values of relative pressure do not correspond to division marks on the scale of abscissae, so that care is needed if inaccuracy is to be avoided. This difficulty can be circumvented by basing the standard table on even intervals of relative pressure rather than of r but this then leads to uneven spacings of r . Table 3.6 illustrates the application of the standard table to a specific example—the desorption branch of the silica isotherm already referred to. The resultant distribution curve appears as Curve C in Fig. 3.18. 

Fig. 3.20 Pore size distributions (calculated by the Roberts method) for silica powder compacted at (A) Ibtonin" (B) 64tonin (C) 130 ton in". The distributions in (a) were calculated from the desorption brunch of the isotherms of nitrogen, and in (h) from the adsorption branch.

As pointed out earlier (Section 3.5), certain shapes of hysteresis loops are associated with specific pore structures. Thus, type HI loops are often obtained with agglomerates or compacts of spheroidal particles of fairly uniform size and array. Some corpuscular systems (e.g. certain silica gels) tend to give H2 loops, but in these cases the distribution of pore size and shape is not well defined. Types H3 and H4 have been obtained with adsorbents having slit-shaped pores or plate-like particles (in the case of H3). The Type I isotherm character associated with H4 is, of course, indicative of microporosity. 

Two classes of micron-sized stationary phases have been encountered in this section silica particles and cross-linked polymer resin beads. Both materials are porous, with pore sizes ranging from approximately 50 to 4000 A for silica particles and from 50 to 1,000,000 A for divinylbenzene cross-linked polystyrene resins. In size-exclusion chromatography, also called molecular-exclusion or gel-permeation chromatography, separation is based on the solute s ability to enter into the pores of the column packing. Smaller solutes spend proportionally more time within the pores and, consequently, take longer to elute from the column. 

We showed that these mesoporous silica materials, with variable pore sizes and susceptible surface areas for functionalization, can be utilized as good separation devices and immobilization for biomolecules, where the ones are sequestered and released depending on their size and charge, within the channels. Mesoporous silica with large-pore-size stmctures, are best suited for this purpose, since more molecules can be immobilized and the large porosity of the materials provide better access for the substrates to the immobilized molecules. The mechanism of bimolecular adsorption in the mesopore channels was suggested to be ionic interaction. On the first stage on the way of creation of chemical sensors on the basis of functionalized mesoporous silica materials for selective determination of herbicide in an environment was conducted research of sorption activity number of such materials in relation to 2,4-D. 

Low temperature sol-gel technology is promising approach for preparation of modified with organic molecules silica (SG) thin films. Such films are perspective as sensitive elements of optical sensors. Incorporation of polyelectrolytes into SG sol gives the possibility to obtain composite films with ion-exchange properties. The addition of non-ionic surfactants as template agents into SG sol results formation of ordered mechanically stable materials with tunable pore size. 

Separation of C oand C70 can be achieved by HPLC on a dinitroanilinopropyl (DNAP) silica (5pm pore size, 3(X)A pore diameter) column with a gradient from H-hexane to 50% CH2CI2 using a diode array detector at wavelengths 330nm (for C q) and 384nm (for C70). [J Am Chem Soc 113, 2940, 1991.]... 

New templated polymer support materials have been developed for use as re versed-phase packing materials. Pore size and particle size have not usually been precisely controlled by conventional suspension polymerization. A templated polymerization is used to obtain controllable pore size and particle-size distribution. In this technique, hydrophilic monomers and divinylbenzene are formulated and filled into pores in templated silica material, at room temperature. After polymerization, the templated silica material is removed by base hydrolysis. The surface of the polymer may be modified in various ways to obtain the desired functionality. The particles are useful in chromatography, adsorption, and ion exchange and as polymeric supports of catalysts (39,40). 

The third line of development was to increase the selectivity in order to achieve the highest possible resolution to address difficult separations. This may be achieved by a very narrow pore size distribution of the media, e.g., such as achieved by porous silica microspheres (PSM) or by modifying the porous phase by a composite material, e.g., as for Superdex. In practice, this material shows a maximum selectivity over the separation range (e.g., see Fig. 2.2). 

Zorbax PSM particles are made from small (80-2000 A), extremely uniform colloidal silica sol beads. In a patented polymerization process, these beads are agglutinated to form spherical particles. The size of the Zorbax PSM particles is controlled by the polymerization process, and the pore size is determined by the size of the silica sol beads. After polymerization, the silica is heated to remove the organic polymer and sinter the particles. The result is a spherical, porous, mechanically stable, pure silica particle that provides excellent chromatographic performance (Pig. 3.1). 

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