Ortho-positronium migration in mesopores of MCM-41, MSF and SBA-3

Three materials: MCM-41, MSF and SBA-3 with a very similar pore diameter but different lengths of cylindrical pores were investigated using the nitrogen sorption method and positron annihilation lifetime spectroscopy. The size of primary pores and interparticle spaces obtained by both methods is similar. However, volume ratios between the discussed kinds of pores found by the above-mentioned methods differ significantly. Such discrepancy is the result of both ortho-positronium migration and the inaccessibility of the pores for nitrogen. Comparing the results of nitrogen sorption and positron annihilation lifetime spectroscopy allows us to estimate that connectivity between the primary pores and the interparticle spaces is the highest in MCM-41 and lowest in SBA-3

Gas filling of SBA - 15 silica micropores probed by positron annihilation lifetime spectroscopy (PALS)

Positron annihilation lifetime measurements were conducted in situ while two gasses (nitrogen and oxygen, respectively) were introduced into the SBA-15 porous silica sample. Slow changes in lifetime spectra were observed during a long lasting gas interaction with the sample. Introduced gases slowly filled the free volumes, starting from the smallest ones, especially small micropores. In the presence of a gas, the rate of change of ortho-positronium (o-Ps) and unbound positron intensity was larger than the rate of change of lifetime. This suggests the existence of an additional process, which reduces the number of ortho-positronium atoms due to the interaction with the gas. Moreover, the process of filling pores with gas was slower than the process of emptying them while the gas was pumped out

Porosity of Silica Monoliths with Tailored Mesopores of Ink-Bottle Shape Determined by Nitrogen Adsorption and Positron Annihilation Lifetime Spectroscopy

The comparison of pore size distributions obtained with the use of two porosimetric methods: low temperature nitrogen sorption (LN2) and positron annihilation lifetime spectroscopy (PALS), was performed for porous silica monoliths. Four investigated samples were prepared under various synthesis conditions. Nitrogen sorption showed the presence of bottle-shaped pores in all investigated samples. In addition, it seems that the presence of methanol during synthesis influences porosity to a greater extent than organic additives. Quite good agreement between the LN2 and PALS results was observed only for the silica monolith synthesized with β-cyclodextrins as pore directing agent. The biggest discrepancy in the results obtained from these two techniques was observed for the silica gel synthesized with no additives. The origin of such discrepancies, taking into account the shape of pore size distribution and deficiencies of data analysis techniques, is discussed

Porosity of Silica Monoliths with Tailored Mesopores of Ink-Bottle Shape Determined by Nitrogen Adsorption and Positron Annihilation Lifetime Spectroscopy

The comparison of pore size distributions obtained with the use of two porosimetric methods: low temperature nitrogen sorption (LN2) and positron annihilation lifetime spectroscopy (PALS), was performed for porous silica monoliths. Four investigated samples were prepared under various synthesis conditions. Nitrogen sorption showed the presence of bottle-shaped pores in all investigated samples. In addition, it seems that the presence of methanol during synthesis influences porosity to a greater extent than organic additives. Quite good agreement between the LN2 and PALS results was observed only for the silica monolith synthesized with β-cyclodextrins as pore directing agent. The biggest discrepancy in the results obtained from these two techniques was observed for the silica gel synthesized with no additives. The origin of such discrepancies, taking into account the shape of pore size distribution and deficiencies of data analysis techniques, is discussed

Thermal stability of chemically bonded phases on silica gel by photoacoustic FT-IR spectroscopy

The temperature resistance of chemically bonded phases on commercial silica gel, LiChrosorb RP 2, RP 8, RP 18 and unmodified Si 60 were tested at different temperatures by photoacoustic FT-IR spectroscopy. The surface characteristics and possible degradation of hydrocarbon phase at higher temperatures were investigated by means of FT-IR/PAS technique. For a series of investigated samples heated up to 423 K, the FT-IR/PAS spectra are similar to those for initial silica samples. The most characteristic band for alkyl modified silica gel, i.e., RP 2, RP 8, and RP 18 was observed between 3200 cm-1 to 2800 cm-1 corresponding to various hydrocarbon species. The bands at 3745 cm-1, 3650 cm-1, and 3430 cm-1 observed in the photoacoustic FT-IR spectra may be ascribed to isolated silanol groups (Si-OH), geminal groups (Si-(OH)$_2$) and hydrogen-bonded Si-OH groups, respectively. For all samples the intensity of the broad band in the region 3800 cm-1 to 3200 cm-1 decreases with the increasing temperature. The additional peak at 3745 cm-1 for chemically bonded long hydrocarbon chain, i.e., C18 and C8 after thermal treatment at 573 K is observed

Organic deposits on MCM-41 surface after thermal treatment of as-synthesized samples

FT-IR spectroscopy with photoacoustic detector has been applied to investigate organic template transformations during thermal treatment of silica and silica-alumina MCM-41 molecular sieve. The role of surfactant degradation and type of organic deposits on silica surface remaining after surfactant elimination depends on the presence of alumina in MCM-41 pore network