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dc.contributor.authorRound, Catherine I.
dc.contributor.authorWilliams, Craig D.
dc.contributor.authorLatham, Kay
dc.contributor.authorDuke, Catherine V. A.
dc.date.accessioned2008-06-25T14:15:54Z
dc.date.available2008-06-25T14:15:54Z
dc.date.issued2001
dc.identifier.citationJournal of Thermal Analysis and Calorimetry, 63(2): 329-338
dc.identifier.issn14182874
dc.identifier.issn15728943
dc.identifier.doi10.1023/A:1010133822423
dc.identifier.urihttp://hdl.handle.net/2436/30478
dc.description.abstractThe synthesis of pure silica ZSM-5 has been modified to produce highly crystalline material in the protonated form, necessary for catalytic activity, directly from a low water fluoride gel. Tetrahedrally co-ordinated divalent species of nickel and copper have been synthesised as salts of large organic cations and increasing mole fractions incorporated into the zeolite gels. The products have been analysed and characterised using simultaneous thermogravimetric and derivative thermogravimetric analysis (TG-DTG). The thermal decomposition under nitrogen of the metal associated cations, tetraethylammonium (TEA+), occluded within the zeolite channels is indicative and characteristic of the incorporation of heteroatoms into the zeolite framework. Anomalous losses in the systems can be explained by Jahn–Teller distortions. The mass losses increased with increased metal loading and were consistent with those reported in full water system, analysis also confirmed that the material was hydrophobic and thermally stable. Analysis by X-ray diffraction (XRD), scanning electron microscope (SEM), X-ray fluorescence (XRF), Fourier transform infrared spectroscopy (FTIR) and Atomic Absorption Spectroscopy (AAS) has confirmed the reliability of TG-DTG as a diagnostic tool. The maximum levels of substitution achieved were (mass%) Ni 3.93 and Cu 4.38.
dc.language.isoen
dc.publisherSpringerLink
dc.relation.urlhttps://link.springer.com/article/10.1023%2FA%3A1010133822423
dc.subjectSpectroscopy, Fourier Transform Infrared
dc.subjectX Ray Diffraction
dc.subjectScanning Electron Microscope
dc.subjectMicroscopy, Electron
dc.subjectSpectroscopy, Atomic Absorption
dc.subjectX Ray Fluorescence
dc.subjectGeochemistry
dc.subjectZeolites
dc.subjectZSM-5
dc.subjectNickel
dc.subjectCopper
dc.subjectThermogravimetric analysis
dc.subjectIsomorphous substitution
dc.subjectGels, aqueous fluoride
dc.subjectFluoride
dc.titleThermogravimetric Evidence of Nickel or Copper Isomorphously Substituted into a Zeolite.
dc.typeJournal article
dc.identifier.journalJournal of Thermal Analysis and Calorimetry
html.description.abstractThe synthesis of pure silica ZSM-5 has been modified to produce highly crystalline material in the protonated form, necessary for catalytic activity, directly from a low water fluoride gel. Tetrahedrally co-ordinated divalent species of nickel and copper have been synthesised as salts of large organic cations and increasing mole fractions incorporated into the zeolite gels. The products have been analysed and characterised using simultaneous thermogravimetric and derivative thermogravimetric analysis (TG-DTG). The thermal decomposition under nitrogen of the metal associated cations, tetraethylammonium (TEA+), occluded within the zeolite channels is indicative and characteristic of the incorporation of heteroatoms into the zeolite framework. Anomalous losses in the systems can be explained by Jahn–Teller distortions. The mass losses increased with increased metal loading and were consistent with those reported in full water system, analysis also confirmed that the material was hydrophobic and thermally stable. Analysis by X-ray diffraction (XRD), scanning electron microscope (SEM), X-ray fluorescence (XRF), Fourier transform infrared spectroscopy (FTIR) and Atomic Absorption Spectroscopy (AAS) has confirmed the reliability of TG-DTG as a diagnostic tool. The maximum levels of substitution achieved were (mass%) Ni 3.93 and Cu 4.38.


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