Title page for ETD etd-10397-131328


Type of Document Master's Thesis
Author Watson, R. Craig Jr.
Author's Email Address cwatson@vt.edu
URN etd-10397-131328
Title Laser-Ionization Time-of-Flight Mass Spectrometry of High Molecular Mass Inorganic Complexes
Degree Master of Science
Department Chemistry
Advisory Committee
Advisor Name Title
Tissue, Brian M. Committee Chair
Anderson, Mark R. Committee Member
Long, Gary L. Committee Member
Keywords
  • Laser ionization
  • Mass spectrometry
  • Matrix-assisted-laser desorption/ionization
  • MALDI
  • Organometallic complexes
  • Reflectron
  • Time-of-flight
Date of Defense 1997-10-17
Availability unrestricted
Abstract
Laser-Ionization Time-of-Flight Mass Spectrometry (LI-TOF-MS) is a sophisticated tool for the molecular-weight determination and structural characterization of a variety of molecules. Advances in instrumentation and ionization methods have recently expanded its role in the analysis of high-mass analytes. Large multimetallic complexes, which are efficient solar-energy converters, rely heavily on their chemical structure for optimum operation. Molecular mass determinations of these multimetallic complexes have been problematic due to their lability and high molecular weights.

This thesis describes the characterization of a LI-TOF-MS instrument and confirmation of theoretical time-of-flight mass-separation principles. Several test cases demonstrate the instrument's proper operation and calibration for a wide mass range of analytes. Mass spectral results of three organometallic compounds: i. [Ir(dpp)2Cl2](PF6), ii. {[(bpy)2Ru(dpp)]2IrCl2}(PF6)5, and iii. {[(bpy)2Ru(dpp)]2RuCl2}(PF6)5 under a variety of laser ionization and sample preparation conditions are compared. A complete structural characterization of the monometallic complex, [Ir(dpp)2Cl2](PF6), is presented. The two trimetallic analytes fragmented easily, but significant components of the molecules are successfully identified. After optimizing the ionization and analytical procedure, LI-TOF-MS proved useful in the analysis of high molecular mass metal complexes.

Files
  Filename       Size       Approximate Download Time (Hours:Minutes:Seconds) 
 
 28.8 Modem   56K Modem   ISDN (64 Kb)   ISDN (128 Kb)   Higher-speed Access 
  ch1introduction.pdf 144.56 Kb 00:00:40 00:00:20 00:00:18 00:00:09 < 00:00:01
  ch2instrumentdesign.pdf 64.44 Kb 00:00:17 00:00:09 00:00:08 00:00:04 < 00:00:01
  ch3instrumcharact.PDF 185.01 Kb 00:00:51 00:00:26 00:00:23 00:00:11 < 00:00:01
  ch4dopedmetaloxides.pdf 74.95 Kb 00:00:20 00:00:10 00:00:09 00:00:04 < 00:00:01
  ch5fullerenes.pdf 170.66 Kb 00:00:47 00:00:24 00:00:21 00:00:10 < 00:00:01
  ch6inorganicsmaldi.pdf 393.85 Kb 00:01:49 00:00:56 00:00:49 00:00:24 00:00:02
  ch7conclusions.pdf 12.64 Kb 00:00:03 00:00:01 00:00:01 < 00:00:01 < 00:00:01
  etd-titleabstractacknowl.pdf 15.32 Kb 00:00:04 00:00:02 00:00:01 < 00:00:01 < 00:00:01
  TABLE_OF_CONTENTS.pdf 15.07 Kb 00:00:04 00:00:02 00:00:01 < 00:00:01 < 00:00:01
  TABLE_OF_FIGURES.pdf 20.34 Kb 00:00:05 00:00:02 00:00:02 00:00:01 < 00:00:01
  VITA.pdf 3.77 Kb 00:00:01 < 00:00:01 < 00:00:01 < 00:00:01 < 00:00:01

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