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Query: EC:4.1.2.42 (DTA)
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Three kinds of amorphous aluminosilicates were synthesized by coprecipitation of silicic acid with aluminum hydroxide in the presence of different inorganic ions: sulfate, chloride, and nitrate. Although the bulk composition of the aluminosilicates obtained was not affected by anion species, their DTA spectra were significantly different, suggesting that their structures also differ. The local structure of Al and Si in the aluminosilicates was studied in detail by 27Al and 29Si MAS NMR. From the 27Al MAS NMR spectra and comparison between 29Si HD- and CP-MAS NMR spectra, it was concluded that the aluminosilicate obtained in the presence of sulfate ions has only a montmorillonite-like structure, whereas in the cases of chloride and nitrate, the solids are composed of three phases: aluminum hydroxide, silica, and the montmorillonite-like aluminosilicate. The difference in the local structure of Al and Si in the aluminosilicates was explained by the difference in interaction between the anions and aluminum ions. Copyright 1999 Academic Press.
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PMID:Effects of Anions on Local Structure of Al and Si in Aluminosilicates. 1033 80

The strontium ferrite ultrafine particles have been prepared using the microemulsion processing. The mixed hydroxide precursor was obtained via the coprecipitation of Sr(2+) and Fe(3+) in a water-in-oil microemulsion of water/CTAB/n-butanol/isooctane. According to the investigation on the thermochemical properties by TGA/DTA and the phase analysis by XRD, it was shown that the precursor could yield pure strontium ferrite after calcination at 700 degrees C for 5 h while using an appropriate molar ratio of Sr/Fe in microemulsions. From TEM measurement, the diameters of the precursor and calcined particles were 3.8+/-0.7 and 50-100 nm, respectively. The magnetic properties characterized by a SQUID magnetometer showed that the saturation magnetization, remanent magnetization, coercivity, and squareness ratio were 55 emu/g, 28 emu/g, 492 Oe, and 0.51, respectively. The magnetization was also observed to increase with the decrease of temperature at 5-400 K. Compared with those reported earlier, the quite low coercivity implies the potential application of final product in the high-density perpendicular recording media. Copyright 2001 Academic Press.
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PMID:Synthesis of Strontium Ferrite Ultrafine Particles Using Microemulsion Processing. 1125 26

The new hybrid inorganic-organic polymer In(2)(OH)(3)[O(4)C(8)H(4)](1.5) has been hydrothermally obtained. Conditions for the synthesis are reported. The crystal structure of this material has been established by single-crystal X-ray diffraction: it is monoclinic, with space group P2(1)/c (Nomicron. 14), a = 6.772(1) A, b = 10.329(2) A, c = 20.152(3) A, beta = 97.573(3) degrees. The In atoms are octahedrally coordinated by three hydroxide groups and three different molecules of carboxylate ligand. The resulting polymeric 3D structure can be envisaged as having been generated from a honeycomb (6,3) 2D that is cross-linked by the BDC organic anions. Data of IR and TGA-DTA studies, as well as the results of reduction of nitroaromatics and selective oxidation of organic sulfide reactions catalyzed by the new material, are reported.
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PMID:In(2)(OH)(3)(BDC)(1.5) (BDC = 1,4-benzendicarboxylate): an In(III) supramolecular 3D framework with catalytic activity. 1197 9

Arsenic adsorption was carried out on simple materials such as goethite and amorphous iron hydroxide, and more complex matrices such as clay pillared with titanium(IV), iron(III), and aluminum(III). These matrices were synthesized from a bentonite whose montmorillonitic fraction was pillared according to optimized parameters. These sorbents were characterized by various methods: XRD, FTIR, BET, DTA/TGA, surface acidity, and zetametry. Elimination of arsenite and arsenate as a function of pH was studied. Arsenate elimination was favored at acidic pH, whereas optimal arsenite elimination was obtained at 4<pH<9. For pH values above 10, the pillared clays were damaged and elimination decreased. Equilibrium time and adsorption isotherms were also determined for arsenite and arsenate at each matrix auto-equilibrium pH. Amorphous iron hydroxide had the highest adsorption capacities both towards arsenate and arsenite. Adsorption capacities of goethite and iron- and titanium-pillared clays toward arsenate were similar, but those toward arsenite were different. Desorption experiments from the various matrices were carried out. Iron- and titanium-pillared clays showed a desorption capacity above 95% and around 40% respectively, but no desorption rate could be obtained for iron (hydr)oxides as they were damaged during the process.
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PMID:Arsenic adsorption onto pillared clays and iron oxides. 1270 67

Magnesium oxide/hydroxide was deposited on pitch-based activated carbon fibers which were previously oxidized in air at different temperatures, and the changes in carbon oxidation activity, microporosity, and CH4 adsorptivity of the parent carbons due to Mg deposition were examined. DTA results, chemical analysis, and DRIFT spectra indicate that Mg species are mainly supported on the -COOH groups of the parent carbons, which serve as the catalysts to improve the oxidation activity of carbon. Mg deposition either increases or decreases the specific surface area, pore volume, and average micropore width of the parent carbon depending on the preoxidation temperatures. Mg deposition does not simply enhance CH4 adsorptivity: the complex changes are due to the differences in the supporting states of Mg species and slight modifications in micropore structure.
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PMID:Changes in microporosity and CH4 adsorptivity of preoxidized pitch-based activated carbon fibers by Mg deposition. 1521 43

Self-generation of ionic organic capping from nonionic surfactant polyoxyethylene (20) sorbitan trioleate (Tween-85) has been realized for the controlled synthesis of single crystalline Co(3)O(4) quantum dots (3.0-5.7 nm) in cubic morphology from related layered hydroxide precursors at 80-95 degrees C. With chemical modification of hydrophobic functional groups on the surface of Co(3)O(4) nanocubes; furthermore, various nanocube-containing micellar superstructures can be further assembled through hydrophobic interactions between Tween-85 molecules and the surface coating under "one-pot" conditions. In particular, square arrangements, spherical domains, and line-assemblies of the prepared Co(3)O(4) nanocubes and their inter-transformations have been attained for the first time by manipulating intersurfactant-interactions. Hydrolysis of Tween-85 and the resultant tiered surfactant superstructures have been investigated with FTIR/UV-vis/EA/TGA/DTA/XPS methods, and the capping species has been identified to be alkylated oleic carboxylate anions derived from Tween-85. Pronounced quantum confinement effects have been observed with the prepared Co(3)O(4) nanocubes, and the optical band gap energies determined are 3.95 and 2.13 eV, respectively, for O(2-)--> Co(2+) and O(2-)--> Co(3+) charge-transfer processes.
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PMID:Self-generation of tiered surfactant superstructures for one-pot synthesis of Co3O4 nanocubes and their close- and non-close-packed organizations. 1549 Dec 15

As compared with other candidate carbon sequestration technologies, mineral carbonation offers the unique advantage of permanent disposal via geologically stable and environmentally benign carbonates. The primary challenge is the development of an economically viable process. Enhancing feedstock carbonation reactivity is key. Heat activation dramatically enhances aqueous serpentine carbonation reactivity. Although the present process is too expensive to implement, the materials characteristics and mechanisms that enhance carbonation are of keen interest for further reducing cost. Simultaneous thermogravimetric and differential thermal analysis (TGA/DTA) of the serpentine mineral lizardite was used to isolate a series of heat-activated materials as a function of residual hydroxide content at progressively higher temperatures. Their structure and composition are evaluated via TGA/DTA, X-ray powder diffraction (including phase analysis), and infrared analysis. The meta-serpentine materials that were observed to form ranged from those with longer range ordering, consistent with diffuse stage-2 like interlamellar order, to an amorphous component that preferentially forms at higher temperatures. The aqueous carbonation reaction process was investigated for representative materials via in situ synchrotron X-ray diffraction. Magnesite was observed to form directly at 15 MPa CO2 and at temperatures ranging from 100 to 125 degrees C. Carbonation reactivity is generally correlated with the extent of meta-serpentine formation and structural disorder.
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PMID:Exploration of the role of heat activation in enhancing serpentine carbon sequestration reactions. 1566 55

Ten new lanthanum(III) and praseodymium(III) complexes of the general formula Na[La(L)2H2O] (Ln=La(III) or Pr(III); LH2=thiosemicarbazones) derived from the condensation of isatin with 4-phenyl thiosemicarbazide, 4-(4-chlorophenyl) thiosemicarbazide, 4-(2-nitrophenyl) thiosemicarbazide, 4-(2-bromophenyl) thiosemicarbazide and 4-(2-methylphenyl) thiosemicarbazide, have been synthesized in methanol in presence of sodium hydroxide. The XRD spectra of the complexes were monitored to verify complex formation. The complexes have also been characterized by elemental analysis, molar conductance, electronic absorption and fluorescence, infrared, far infrared, 1H and 13C NMR spectral studies. Thermal studies of these complexes have been carried out in the temperature range 25-800 degrees C using TG, DTG and DTA techniques. All these complexes decompose gradually with the formation of Ln2O3 as the end product. The Judd-ofelt intensity parameter, oscillator strength, transition probability, stimulated emission cross section for different transitions of Pr3+ for 4-phenyl thiosemicarbazones have been calculated.
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PMID:Lanthanum(III) and praseodymium(III) complexes with isatin thiosemicarbazones. 1604 75

Hydrotalcite-like compounds (HTlcs) containing Mg(2+), Al(3+), and Ce(3+) in the hydroxide layer and with carbonate as charge-balancing anion have been prepared by a co-precipitation (at constant pH) method. The Al/Ce ratio in the final product depends on the concentration in the initial solution. The crystallinity of the layered materials decreases with the increase in cerium content, probably, due to the distortions introduced by the large difference in the ionic radii of the cations. All the synthesized materials were characterized by XRD, FT-IR spectroscopy and TG/DTA. The textural properties were determined from low-temperature nitrogen adsorption-desorption measurements.
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PMID:Preparation and characterization of Mg-Al hydrotalcite-like compounds containing cerium. 1678 Aug 59

Calcium hydroxyapatite (CaHAP) and barium hydroxyapatite (BaHAP) have been prepared by a wet method from aqueous solutions with cation/P molar ratio of 1.67. The prepared particles were characterized using XRD, IR, TG-DTA and BET-N(2) adsorption measurements. The potential of the synthesized hydroxyapatites to remove Zn(II) from aqueous solutions was investigated in batch reactor under different experimental conditions. Both hydroxyapatites remove Zn(II) from aqueous solutions with an efficiency higher than 98% at initial pH around 6-8. The data reveal that the initial uptake was rapid and equilibrium was established in 20 and 60 min for CaHAP and BaHAP. The sorption process follows the pseudo-first-order kinetic with a rate constant (k(ads)) equals to 1.06x10(-2) and 1.91x10(-2) min(-1) for CaHAP and BaHAP, respectively. Zn(II) removal was quantitatively evaluated using Langmuir isotherm model and the monolayer sorption capacity (Q(max)) shows the values 102.04 and 36.62 mg g(-1) for CaHAP and BaHAP clarifying the high affinity of these novel sorbents for Zn(II) ions. Kinetically, the prepared apatites are feasible sorbents retain Zn(II) ions through a favorable and spontaneous sorption process. The possibility of metal recovery and regeneration of hydroxyapatites were investigated using several eluting agents include hydrochloric acids, double distilled water, calcium chloride, barium hydroxide, and copper chloride. Different desorption levels were obtained with the different adsorbents and the maximum recovery yield was achieved with copper chloride.
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PMID:Sorption behavior of Zn(II) ions on synthesized hydroxyapatites. 1732 33


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