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  • XRD  (4)
  • crystallization  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 13 (1992), S. 207-218 
    ISSN: 1573-1111
    Keywords: Gallosilicate (MFI) synthesis ; crystallization kinetics ; 29Si71Ga MASNMR ; XRD ; IR
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Crystalline gallosilicates with a pentasil (MFI) framework containing Ga3+ in lattice positions were synthesised. The kinetic features of the hydrothermal system containing triethyl-n-butylammonium cations (TEBA)+ as template in the gel system have been investigated. The gallosilicate products were characterized by XRD, framework-IR, TG/DTA,29Si and71Ga MASNMR and sorption measurements using standard techniques. $$Na_2 O:(TEBA)_2 O:Ga_2 O_3 :SiO_2 :H_2 O$$ The values of the apparent activation energies for nucleation (E n) and crystallization (E c) were evaluated by applying the Arrhenius equation. Evidence from29Si and71Ga MASNMR as well as the estimated unit-cell volumes computed from XRD powder patterns indicate that a significant amount of Ga3+ is substituted in the pentasil (MFI) framework.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 20 (1994), S. 197-210 
    ISSN: 1573-1111
    Keywords: Synthesis ; isomorphous substitution ; XRD ; ion exchange ; catalytic activity ; β-zeolite B and Ga isomorphs
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The crystalline isomorphs ofβ-zeolite containing boron or gallium in the framework positions have been synthesized and the products characterized by comparing them with Al-β zeolite. Evidence for the presence of B or Ga in the zeolite lattice framework has been confirmed by spectroscopic (XRD, IR and29Si,27Al and11B MASNMR), DTA/TG, ion exchange, sorption and catalytic activity results. Chemical analysis and NMR confirm the absence of any significant amount of Al in the zeolite (SiO2/Al2O3=2000). The XRD pattern of the as-synthesized B-β and Ga-β compounds matched well with that of Al-β zeolite. Lattice B and Ga leads to a change in the X-rayd values. Framework and bridging hydroxyl stretching IR bands ofβ-zeolite are shifted due to incorporation of gallium and boron into the zeolitic framework. MASNMR spectra of11B and29Si also suggest the presence of tetrahedrally coordinated B(III) or Ga(III) ions in theβ-zeolite framework. B and Gaβ-zeolites exhibit significant ion exchange capacity and catalytic activity in them-xylene isomerization reaction. The shifts in the IR bands towards higher frequency in B-β and lower frequency in Ga-β, the observed ion exchange capacities and catalytic properties, indicate the presence of B3+ or Ga3+ ions in the framework ofβ-zeolite.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 29 (1997), S. 1-13 
    ISSN: 1573-1111
    Keywords: Zeolite ; thermal behaviour ; adsorption ; isosteric heats ; XRD ; IR ; TG ; DTA
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Crystals collected from the Ellora valley(Aurangabad, MS, India) of the Deccan traps of India have beencharacterized as a stilbite (St) by X-ray diffraction, IRspectroscopy and chemical analyses. The thermal behaviour was studiedusing TG and DTA techniques. The sample was exchanged at refluxtemperature with NH4Cl and NH4St was prepared. This was furthertransformed to the H-form of stilbite (HSt) by heating at 573 K for 12 h.The samples so prepared were used for adsorption studies. The comparativestudy of sorption of these samples shows an increase in the sorptioncapacity of HSt. The isosteric heat was also computed for these samples.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 9 (1990), S. 91-99 
    ISSN: 1573-1111
    Keywords: Zeolite ; ZSM-5 ; synthesis ; crystallization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Pentasil zeolites of ZSM-5 type are synthesised hydrothermally using triethyl-n-proplyammonium bromide (TEPA-Br) and triethyl-n-butylammonium bromide (TEBA-Br). The crystallization kinetics, followed by XRD, SEM and thermal analysis, clearly demonstrate the influence of size and molecular weight of the templating quaternary ammonium cation (QAC) species on the rates of nucleation and crystallization. The values of the apparent activation energies for nucleation and crystal growth indicate that both nucleation and crystal growth are faster when TEPA-Br rather than TEBA-Br is used as a template. The quantitative identification of intergrown phases characterizes both the phases to be ZSM-5 zeolite. Thermoanalytical curves for both these zeolites in as-synthesised forms exhibit two-step oxidative decomposition of the occluded organic species. This suggests that the quaternary ammonium cation may be located at two energetically different sites within the zeolite channels. The equilibrium sorption capacity, however, is found to increase in the order of size and molecular weight of the templating species in both the zeolites. The nature of acid site distribution, obtained from the temperature programmed desorption of ammonia is found to be independent of the templating species used during the synthesis.
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    Journal of inclusion phenomena and macrocyclic chemistry 13 (1992), S. 171-179 
    ISSN: 1573-1111
    Keywords: Zeolite synthesis ; small port mordenite ; ZSM-5 ; IR ; XRD ; sorption properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Zeolites ZSM-5 and mordenite were synthesized without the aid of a template, in the gel composition ofXSiO2 : Al2O3 :YNa2O: 1500 H2O, whereX = 20–40 andY = 3.5–10.0 at 463 K. After 48 h of crystallisation the aluminosilicate gel system yielded either ZSM-5 or mordenite and their mixtures as zeolitic phases in addition to α- quartz depending on the variation in oxide mole composition. Transformation of crystalline ZSM-5 to mordenite was accompanied by a lower yield of solid product as a result of an increase in SiO2/Al2O3 and Na2O/SiO2 ratios in the aluminosilicate gel. At constant Na2O/SiO2 ratio, the decrease in SiO2/Al2O3 in the gel mixture was operative in lowering the product SiO2/Al2O3 ratio. Similarly, at constant SiO2/Al2O3 the increase in Na2O/SiO2 in the gel decreased the product SiO2/Al2O3 ratio. The mordenite obtained was found to be of the small port variety. Crystalline phases obtained were further characterised by XRD, IR, SEM and sorption studies.
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