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Query: UMLS:C0276640 (TEM)
 20,729 document(s) hit in 31,850,051 MEDLINE articles (0.00 seconds)

An alternative method for the calcium phosphate apatite formation onto the surface of flocculated pure silica particles is reported, in an attempt to understand the possible mechanism for the apatite formation. A stable silica sol was flocculated by adding calcium ions in aqueous solution. The wet flocks were resuspended in a basic aqueous solution containing a calcium salt, trying to allow the absorption of calcium ions onto the silica surface through a hydrogen ion exchange. The as-prepared materials were immersed in a modified simulated body fluid at different temperatures (37 and 90 degrees C) and silica concentrations. It was found that these factors have a strong influence on the apatite formation. The apatite formation was confirmed by (31)P MAS-NMR, FT-Raman, XRD, and TEM.
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PMID:Apatite growth on calcium adsorbed surface of wet flocculated silica particles immersed in a modified simulated body fluid. 1063 51

We report here, for the first time, synthesis of anchored Pd complexes in mesoporous supports such as MCM-41 and MCM-48 as true heterogeneous catalysts for hydrocarboxylation of aryl olefins and alcohols to give excellent conversion ( approximately 100%) and regioselectivity ( approximately 99%) for 2-arylpropionic acids. The catalysts were characterized by powder-XRD, 31P CP-MAS NMR, FT-IR, TEM, XPS and ICP-AES. Recycle studies with these anchored Pd mesoporous catalysts were performed to confirm true heterogeneity.
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PMID:Anchored Pd complex in MCM-41 and MCM-48: novel heterogeneous catalysts for hydrocarboxylation of aryl olefins and alcohols. 1217 12

Periodic mesoporous organosilica (PMO) with two-dimensional hexagonal symmetry was synthesised using a bridged silsesquioxane (CH3O)3Si-CH2-CH2-Si(CH3O)3 as precursor and polyoxyethylene non-ionic surfactant (Brij-56) as template. The hybrid material was characterised by X-ray diffraction, N2 adsorption, TEM, and solid-state 29Si MAS NMR spectroscopy.
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PMID:Periodic mesoporous organosilica from micellar oligomer template solution. 1235 6

Sonolysis of diphenylmethane (DPhM) has been studied under the effect of 20 kHz ultrasound (absorbed acoustic power 0.45 W/ml, surface area of sonotrode 1 cm(2), volume of sonicated solution 100 ml) under argon at 60 degrees C. The solid product of the sonolysis was characterized by elemental analysis, FTIR, 13C MAS NMR, TGA/DSC, XRD and TEM techniques. It was found that the sonolysis of DPhM causes formation of the polymer with the composition similar to crosslinked polystyrene. Assumed mechanism of DPhM sonolysis consists of DPhM molecules dissociation inside the cavitating bubble. Secondary radical scavenging and radical recombination processes yields the sonopolymer in the liquid phase. The breakdown of the aromatic ring during DPhM sonolysis confirms that a very high temperature established in the cavitating bubble.
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PMID:Sonochemical polymerization of diphenylmethane. 1245 45

The silica-pillared derivatives from kanemite (NaHSi(2)O(5).3H(2)O) were prepared by intercalation of dialkyldimethylammonium (DADMA) ion and pillaring with tetraethylorthosilicate. The formation of silica pillars between the silicate sheets was demonstrated by X-ray diffraction, (29)Si CP/MAS NMR, and TEM observation. The basal spacing depended on the chain length of DADMA. Nitrogen adsorption study showed that the specific surface area was enlarged over 1000 m(2) g(-1) by the pillaring and that the pore size was in the micropore region. Water and benzene adsorption isotherms revealed that the surface properties of the pillared derivatives show hydrophobic character.
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PMID:Preparation and characterization of silica-pillared derivatives from kanemite. 1270 82

The copper-tellurolate cluster [(Cu(6)(TePh)(6)(PPh(2)Et)(5)] has been loaded into the pores of MCM-41 by solid-state impregnation techniques. It was found that the best loading conditions are 110 degrees C and 10(-)(3) Torr static vacuum. The resulting material was analyzed by powder X-ray diffraction (PXRD), nitrogen adsorption isotherms, thermogravimetric analysis (TGA), (31)P CP MAS NMR spectroscopy, and TEM. It was observed that loading is accompanied by loss of the phosphine shell, with retention of the copper-tellurium core. Condensation of the impregnated material may proceed thermally or photochemically. Thermal condensation results in the formation of Cu(2)Te nanoparticles as demonstrated by PXRD, and TEM data suggests that the process has taken place inside the pores of MCM-41. Photochemical condensation yields larger metal-chalcogen clusters in the pores as suggested by the result of UV-vis diffuse reflectance spectroscopy and TEM measurements.
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PMID:Preparation, characterization, and condensation of copper tellurolate clusters in the pores of periodic mesoporous silica MCM-41. 1470 65

13C CP/MAS NMR and FE/TEM measurements of the aragonite brick of the nacreous layer of Pinctada fucata indicate that it assembles with highly oriented aragonite nanocrystals, which are regulated by biopolymers.
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PMID:Highly oriented aragonite nanocrystal-biopolymer composites in an aragonite brick of the nacreous layer of Pinctada fucata. 1506 12

CpMo(CO)(3)Cl reacts with the hydroxyl (Si-OH or Si-OH-Al) functionalities of mesoporous molecular sieves such as MCM-41, MCM-48 and its aluminium analogues during grafting. XRD, N(2) adsorption-desorption, BET surface area analysis and TEM show the resulting samples as being well ordered and maintaining a uniform pore size. FT-IR spectra, elemental analysis, (13)C and (29)Si CP MAS NMR spectra confirm the successful grafting. In the presence of excess TBHP the materials show high activity in cyclooctene epoxidation and good stability.
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PMID:Heterogenisation of CpMo(CO)3Cl on mesoporous materials and its application as olefin epoxidation catalyst. 1548 19

Two different rehydration procedures in the liquid or gas phase have been applied to reconstruct mixed oxides derived from calcined hydrotalcite-like materials to be used as catalysts for aldol condensation reactions. The as-synthesized hydrotalcite, its decomposition product, as well as the reconstructed solids upon rehydration were characterized by XRD, N(2) adsorption, He pycnometry, FTIR, SEM, TEM, (27)Al MAS-NMR and CO(2)-TPD (TPD=temperature-programmed desorption). Compared to the Mg-Al mixed oxide rehydrated in the gas phase (HT-rg), that rehydrated in the liquid phase (HT-rl) exhibits a superior catalytic performance with respect to the aldol condensation of citral with ketones to yield pseudoionones and in the self-aldolization of acetone. The textural properties of HT-rl and HT-rg differ strongly and determine the catalytic behavior. A memory effect led to a higher degree of reconstruction of the lamellar structure when the mixed oxide was rehydrated in the gas phase rather than in the liquid phase, although liquid-phase rehydration under fast stirring produced a surface area that was 26 times greater. This contrasts to typical statements in the literature claiming a higher degree of reconstruction in the presence of large amounts of water in the medium. CO(2)-TPD shows that the number of OH(-) groups and their nature are very similar in HT-rg and HT-rl, and cannot explain the markedly different catalytic behavior. Accordingly, only a small fraction of the available basic sites in the rehydrated samples is active in liquid-phase aldol condensations. Our results support the model in which only basic sites near the edges of the hydrotalcite platelets are partaking in aldol reactions. Based on this, reconstructed materials with small crystallites (produced by exfoliation during mechanical stirring), that is, possessing a high external surface area, are beneficial in the reactions compared to larger crystals with a high degree of intraplatelet porosity.
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PMID:Aldol condensations over reconstructed Mg-Al hydrotalcites: structure-activity relationships related to the rehydration method. 1558 78

A new approach for the synthesis of double-alkylated L-glutamide-derived stationary phases to use in RP-HPLC is described. TEM observation of lipid distearylglutamide (DSG) showed the formation of fibrous aggregates in methanol or in chloroform through intermolecular hydrogen bonding among the amide moieties while dibutylglutamide (DBG) cannot aggregate in aqueous or organic media due to its lower order of short alkyl chain. DSG and DBG were covalently bonded to silica via amino-propyl linkages. Lipid membrane analogues (e.g., DSG) attached to the silica surface have been found in noncrystalline and solid states and can form supramolecular assemblies with specific properties based on their highly ordered structures in aqueous and organic media. 13C CP/MAS NMR and suspension (in methanol)-state 1H NMR, elemental analysis, and DSC measurements were used to characterize Sil-DSG and were compared with the three other octadecyl phases, i.e., monomeric C18, polymeric C18, and silica grafted poly(octadecyl acrylate) Sil-ODA25. The chromatographic behavior of the new RP material was investigated using detailed retention studies of planar and nonplanar polyaromatic hydrocarbons (PAHs) and nonpolar aromatic positional isomers. Aspects of shape selectivity were also evaluated with Standard Reference Materials 869a, Column Selectivity Test Mixture for Liquid Chromatography. Detailed chromatographic study revealed that Sil-DSG showed extremely enhanced molecular shape selectivity compared with the other phases investigated. The higher molecular shape selectivity obtained by Sil-DSG can be explained by a carbonyl pi (present in lipid-grafted stationary phases)-benzene pi (present in guest PAHs) interaction mechanism, and these interactions are more effective for ordered carbonyl groups.
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PMID:Molecular shape selectivity through multiple carbonyl-pi interactions with noncrystalline solid phase for RP-HPLC. 1622 55


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