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In this paper, ZrO(OH)2 was prepared with sol-gel method, then a series of metal-ions-doped SO(2)4- /ZrO2 nanosolid superacids were prepared by impregnated ZrO(OH)2 using diluted H2SO4 and Ni2+ , Al3+, Sn4+, Ag+ , Sn2+ etc. salt solutions. The samples were characterized by IR, XRD, TEM and chemical analysis method. The result shows that the IR spectra of samples are the characteristic spectra of the solid superacids. The stretching frequencies of Zr--O and S==O in Ni2+ and Sn4+ doped samples are obviously increased, the v(Zr-o) values of Zr--O increase from 485 cm(-1) for SO(2)4- /ZrO2 to 500 cm(-1) for both Ni2+ and Sn4+ doped samples, the v(as) values of S==O increase from 1 390 cm(-1) for So(2)4- /ZrO2 to 1405 and 1400 cm(-1) for Ni2+ and Sn4+ doped samples respectively, but that in Sn2+ doped sample increases a little. It is indicated that the samples doped by Ni2+ and Sn4+ show higher super acidity than SO(2)4- /ZrO2 . The IR spectra of samples were determined at different calcination temperatures. It was found that the stretching frequencies of Zr--O and S==O in Ni2+ and Al3+ doped samples are obviously increased with the increase in calcination temperature, but that in Ag+ doped sample is not.
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PMID:[Observation of IR spectra from doped SO(2)4- / ZrO2 nanosolid superacid]. 1601 5

Aqueous solutions of the anionic surfactant potassium oleate (K-oleate) were studied using small-angle neutron scattering (SANS), steady-state rheology, and cryogenic transmission electron microscopy (cryo-TEM). The micellar structural changes induced by the addition of potassium chloride (KCl) and sodium polystyrenesulfonate (PSS) of different molecular weights were investigated. Upon addition of KCl, a transition from spherical to wormlike micelles was detected from the SANS data and confirmed by the cryo-TEM pictures. The rheological measurements revealed a strong dependence of the low-shear viscosity on the concentration of salt: a broad maximum in the viscosity curve was observed upon addition of KCl, characteristic of the growth of micelles into long worms, followed by branching. The addition of PSS to salt-free solutions of K-oleate had a significant effect on the scattering patterns, revealing partial growth of the spherical micelles into rodlike micelles. In contrast, in the presence of high salt concentrations, addition of PSS to solutions of wormlike micelles did not bring any noticeable modifications in the scattering. However, in the same salt conditions, a clear effect was observed on the low shear viscosity upon addition of PSS, which was found to depend significantly on molecular weight. This suggests a novel way of impacting the viscosity of solutions of wormlike micelles.
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PMID:Wormlike micelles mediated by polyelectrolyte. 1608 65

Mono-dispersed semiconductor ZnS hollow spheres with the diameter of 300-500 nm and the shell thickness of about 100-150 nm have been synthesized successfully by solvothermal method from ethanol solution in the presence of a special surfactant-quaternary ammonium salt of 2-undecyl-1-dithioureido-ethyl-imidazoline (SUDEI) made in our lab. The mono-dispersed ZnS hollow spheres are characterized by XRD, size distribution investment, UV-vis, TEM, and SEM, respectively. The UV-vis measurement indicates that there is a broad absorption at 210-280 nm, which is likely to be caused by "hollow-effect." A growth mechanism of ZnS hollow spheres has also been put forward and discussed.
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PMID:Solvothermal synthesis of hollow ZnS spheres. 1611 39

Polysaccharide multilayer nanocapsules have been fabricated in aqueous media by the layer-by-layer self-assembly of chitosan (CHI) and sodium alginate (ALG) on monodisperse polystyrene (PS) nanoparticles with a diameter of 180 nm as template, followed by removal of the templates through dissolving in THF. The pH and added salt concentration of the polyelectrolyte deposition solutions were optimized to ensure the alternating deposition. Consequently, the most suitable pH values were found to be 6.0-8.0 for ALG and 3.5 for CHI and were used in the deposition. The concentration of added NaCl used in the adsorption solutions was 0.5 M, which led to an average thickness of about 13 nm for 5 bilayers of CHI/ALG shell-wall. zeta-potential indicated the stepwise and alternating adsorption of CHI and ALG to form multilayer film on the PS nanoparticles. The characteristic bands of PS residue almost disappeared in the IR spectrum of the nanocapsule after dipped in THF, confirming thorough removal of PS templates from the core-shell particles. TEM, SEM and AFM were utilized to observe the nanocapsules of about 225 nm in diameter (by TEM). A hydrophilic drug model, acridine hydrochloride (AH), was chosen to investigate the loading and release properties of the nanocapsules. The positively charged AH spontaneously deposited into the capsule due to the electrostatic interaction with the negatively charged styrene sulfonate residues from the PS template inside the capsule. The rate of AH release became slightly slower when the capsule wall was cross-linked with glutaraldehyde, but the accumulative released amount for the cross-linked capsule was obviously reduced. These nanocapsules made from nature polysaccharides have a potential application in controlled drug release.
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PMID:Multilayer nanocapsules of polysaccharide chitosan and alginate through layer-by-layer assembly directly on PS nanoparticles for release. 1612 96

Two binary oxides, a spinel, ZnAl2O4, and a typical perovskite, LaMnO3, have been prepared via CTAB-1-butanol-n-octane-nitrate salt microemulsion in the reverse and bicontinuous states. The exact point of the reverse and bicontinuous states of the microemulsion used in the synthesis was determined by conductivity experiments. The materials obtained after heating at 800 degrees C were characterized by XRD analysis for their crystal structure, N2 porosimetry for their surface area and porosity, and SEM and TEM photography for their texture. The ZnAl2O4 spinel obtained via the reverse microemulsion appears in SEM in a more fragmented form and with a higher specific surface area (143.7 m(2)g(-1)), compared to the corresponding solid prepared via the bicontinuous microemulsion, which appears more robust with lower surface area (126.7 m(2)g(-1)). Nevertheless both materials reveal in TEM a sponge-like structure. The perovskite materials LaMnO3 prepared via the reverse microemulsion showed in SEM a peculiar doughnut-like texture, each doughnut-like secondary particle having a diameter of 2 microm. The corresponding sample developed via the bicontinuous microemulsion showed in SEM uniform secondary particles of size approximately 0.2 microm. Both perovskite samples LaMnO3 appear well crystallized with relative low surface areas, 23.7 m(2)g(-1) for the reverse sample and 10.9 m(2)g(-1) for the bicontinuous one. The TEM photographs reveal that both of them, of reversed and bicontinuous origin, are made up of primary nanoparticles in the size range 40-100 nm. In SEM those materials showed a different secondary structure.
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PMID:Variation of surface properties and textural features of spinel ZnAl2O4 and perovskite LaMnO3 nanoparticles prepared via CTAB-butanol-octane-nitrate salt microemulsions in the reverse and bicontinuous states. 1625 3

The 37-residue islet amyloid polypeptide (IAPP) is the major protein component of the amyloid deposits found in type-II diabetes. IAPP is stored in a relatively low pH environment in the pancreatic secretory granules prior to its release to the extracellular environment. Human IAPP contains a single histidine at position 18. Aggregation of IAPP is considerably faster at a lower pH (4.0 +/- 0.3) than at high pH (8.8 +/- 0.3), as judged by turbidity and thioflavine-T fluorescence studies. The rate of aggregation at low pH increases drastically in the presence of salt. CD experiments show that the conversion of largely unstructured monomers to beta-sheet-rich structures is faster at high pH. TEM studies show that fibrils are formed at both pH values but are more prevalent at pH 8.8 (+/-0.3). Both the free N terminus of IAPP and His-18 will titrate over the pH range studied. An N-terminal acetylated fragment consisting of residues 8-37 of human IAPP was also studied to isolate contributions from the protonation of His-18. Previous studies have shown that this fragment forms protofibrils that are very similar to those formed by intact IAPP. The effects of varying the protonation state of His-18 in the 8-37 analogue indicate that the rate of aggregation and fibril formation is noticeably faster when His-18 is deprotonated, similar to the wild type. However, the pH-dependent effects are larger for full-length IAPP than for the disulfide-truncated, acetylated analogue. TEM studies indicate differences in the morphology of the deposits formed at high and low pH. These results are discussed in light of recent structural models of IAPP fibrils.
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PMID:The role of His-18 in amyloid formation by human islet amyloid polypeptide. 1633 89

In this article, we report the synthesis of methylene-bridged periodic mesoporous organosilicas (PMOs) of the SBA-15 type. The materials were characterized by SAXS, BET, NMR, FESEM, and TEM. It was found that the synthesis of methylene-bridged SBA-15 PMOs requires more rigorous conditions than that of SBA-15 PMOs bearing organic bridges other than methylene. A mild acidic environment, which slows down the hydrolysis and condensation rates of the precursor, with the assistance of a salt, which enhances precursor-template interaction, should be used to synthesize high-quality large-pore methylene-bridged PMOs. We attributed this to the fast hydrolysis and condensation rates and the rigid backbone of precursor 1,2-bis(triethoxysilyl)methylene. By examining and comparing the synthesis of three large-pore PMOs with different bridges, we concluded that the inductive, bridging, and conformation effects of the organic bridging group play an important role in the synthesis of large-pore PMO materials.
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PMID:Synthesis of large-pore methylene-bridged periodic mesoporous organosilicas and its implications. 1647 68

The structural and dynamic properties of low ionic strength micellar solutions of the cationic surfactant perfluorooctylbutane trimethylammonium bromide have been investigated by cryo-TEM, small-angle neutron scattering, small-angle X-ray scattering, T-jump and rheological experiments. The surfactant molecules self-assemble into narrow ribbons with average dimensions on the order of 4 nm x 3 nm, either under salt-free conditions or in the presence of up to 30 mM KBr or NaF. Cryo-TEM also reveals in the salt-free systems the presence of networks of multiconnected micelles. Rheological experiments showed that these surfactant systems exhibit a strong shear-thickening effect even in the presence of up to 30 mM KBr. The T-jump response of the micellar solutions was found to be multiexponential. This observation rules out the presence of only linear micelles with an exponential length distribution and suggests more complex topologies of the micellar aggregates. The relaxation time associated with the predominant process in the T-jump relaxation is strongly correlated to the critical shear rate beyond which shear thickening occurs, thus indicating that this critical shear rate is controlled by the micellar kinetics.
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PMID:Structural and dynamical properties of ribbonlike self-assemblies of a fluorinated cationic surfactant. 1651 52

The surface activity and the rheological properties of aqueous solutions of the amphiphilic block copolymer poly(n-butyl acrylate)-block-poly(acrylic acid) (PnBA-b-PAA) were studied as a function of the degree of neutralization, alpha, of the poly(acrylic acid) block. Although the block copolymer spontaneously forms spherical micelles having a stretched PAA corona and a collapsed PnBA core in water for alpha > 0.1, the solutions do not exhibit any surface activity at this degree of neutralization. Cryo-TEM micrographs show that the radii of the hydrophobic core of the largest micelles are as long as the length of the hydrophobic chain. The micelles, however, have a broad size distribution, and on average, as shown by SANS, the micelles are only about half as long. At concentrations as low as 1 wt %, the solutions exhibit highly viscoelastic behavior and have a yield stress value depending on alpha. The globular micelles are highly ordered in the bulk phase, and the viscoelastic properties are a result of the dense packing of the micelles. The addition of salt or cationic surfactants dramatically decreases the viscosity of the solution. The observed properties seem to be due to electrostatic interactions between the PAA chains of the micelles.
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PMID:Rheology and phase behavior of poly(n-butyl acrylate)-block-poly(acrylic acid) in aqueous solution. 1664 94

We isolated hydroxyproline-rich extensin precursors from suspension-cultured tomato, cucumber, and sycamore-maple by salt-elution of intact cells and cell wall preparations. Cation exchange chromatography and HPLC gel filtration resolved these precursors into monomeric and oligomeric fractions, confirmed by amino acid analysis, immunological cross-reactivity, and TEM visualization. After rotary shadowing monomers appeared as flexuous rods with a contour length of 70 to 100 nanometers and a ;persistence length' (maximum linear displacement) of 44 to 51 nanometers. Oligomers were larger branched assemblies with occasional pores. Native extensin monomers gave uniform gel filtration retention times (Rts), but the Rts of HF-deglycosylated monomers varied depending on concentration, implying ionic interaction between the highly basic deglycosylated monomers and a weakly cationic gel matrix. Succinylation of the deglycosylated monomers reversed the net charge, and restored the retention time to that of glycosylated monomers, confirming the ionic interaction. Succinylation enhanced visualization of the deglycosylated monomers, which previously were barely discernible flexuous rods. The persistence length:contour length ratios of succinylated deglycosylated monomers (tomato sdP2) and glycosylated monomers (sP2) were the same, implying a similar molecular flexibility for both glycosylated and deglycosylated monomers at room temperature. These molecular properties are consistent with suggestions that extensin monomers reptate into the wall as a transmural protein ;weft' which becomes progressively cross-linked forming a network penetrated by the cellulose ;warp.'
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PMID:Characterization of native and modified extensin monomers and oligomers by electron microscopy and gel filtration. 1666 99


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