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 Dr. Brian M. Tissue Committee Chair Dr. Gary Long Committee Member Dr. Mark Anderson 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

If you have questions or technical problems, please Contact DLA.