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LUND UNIVERSITY LIBRARIES

Chemical and X-ray Absorption Spectroscopy Characterization of a New Platinum Catalyst

Talukder, Md. Mahbubul Islam LU (2014) FYSM60 20122
Department of Physics
Synchrotron Radiation Research
MAX IV Laboratory
Abstract
Abstract

The present thesis is concerned with the investigation of a metalorganic catalyst, a Pt complex used for C-C or C-N single bond formation in a cross coupling reaction. The investigated catalysts are used in a homogeneous reaction. In this study I have used chemical methods for the synthesis of the catalytic materials, a number of different techniques for the characterization of the catalyst structure and purity, and synchrotron based X–ray Absorption Spectroscopy (XAS) for further structural characterization of the compounds.
The chemical methods used for complex chracterization were proton NHR spectroscopy, carbon-13 NMR spectroscopy, elemental analysis, X-ray crystallography, mass spectroscopy and fourier transform infrared... (More)
Abstract

The present thesis is concerned with the investigation of a metalorganic catalyst, a Pt complex used for C-C or C-N single bond formation in a cross coupling reaction. The investigated catalysts are used in a homogeneous reaction. In this study I have used chemical methods for the synthesis of the catalytic materials, a number of different techniques for the characterization of the catalyst structure and purity, and synchrotron based X–ray Absorption Spectroscopy (XAS) for further structural characterization of the compounds.
The chemical methods used for complex chracterization were proton NHR spectroscopy, carbon-13 NMR spectroscopy, elemental analysis, X-ray crystallography, mass spectroscopy and fourier transform infrared spectroscopy, and these were applied to three batches of the studied complex, a NHC-Pt complex. All spectroscopic data analysis are compared with either literature values or calculated, theoretical values.
X-ray absorption spectroscopy (XAS) measures the energy-dependent X-ray absorption cross section. The XAS spectral region is divided into three regimes,. the pre-edge, XANES, and EXAFS regions. The three batches of the Pt complexes differ in intensity of the white line in the XANES region, which possibly is related to a Cl ligand and the oxidation state of the complex. The Pt absorption energy is different for the pure and recrystallized complex. Moreover, from the EXAFS region a smaller bond distance was found for the pure and recrystallized NHC-Pt complex compared to the non-recrystallized complex. (Less)
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author
Talukder, Md. Mahbubul Islam LU
supervisor
organization
course
FYSM60 20122
year
type
H2 - Master's Degree (Two Years)
subject
keywords
Key word: N-heterocyclic carbene, cross coupling reaction, NHC-PtCl2-3-chloropyridine, X-ray crystallography.
language
English
id
4360065
date added to LUP
2014-03-21 11:43:51
date last changed
2014-10-22 10:13:36
@misc{4360065,
  abstract     = {{Abstract

The present thesis is concerned with the investigation of a metalorganic catalyst, a Pt complex used for C-C or C-N single bond formation in a cross coupling reaction. The investigated catalysts are used in a homogeneous reaction. In this study I have used chemical methods for the synthesis of the catalytic materials, a number of different techniques for the characterization of the catalyst structure and purity, and synchrotron based X–ray Absorption Spectroscopy (XAS) for further structural characterization of the compounds. 
The chemical methods used for complex chracterization were proton NHR spectroscopy, carbon-13 NMR spectroscopy, elemental analysis, X-ray crystallography, mass spectroscopy and fourier transform infrared spectroscopy, and these were applied to three batches of the studied complex, a NHC-Pt complex. All spectroscopic data analysis are compared with either literature values or calculated, theoretical values. 
X-ray absorption spectroscopy (XAS) measures the energy-dependent X-ray absorption cross section. The XAS spectral region is divided into three regimes,. the pre-edge, XANES, and EXAFS regions. The three batches of the Pt complexes differ in intensity of the white line in the XANES region, which possibly is related to a Cl ligand and the oxidation state of the complex. The Pt absorption energy is different for the pure and recrystallized complex. Moreover, from the EXAFS region a smaller bond distance was found for the pure and recrystallized NHC-Pt complex compared to the non-recrystallized complex.}},
  author       = {{Talukder, Md. Mahbubul Islam}},
  language     = {{eng}},
  note         = {{Student Paper}},
  title        = {{Chemical and X-ray Absorption Spectroscopy Characterization of a New Platinum Catalyst}},
  year         = {{2014}},
}