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Table of Contents Preface List of commonly-used abbreviations Chapter 1 Fundamentals 1.1 Introduction 1.2 Inlets 1.3 Collision-induced dissociation 1.3.1 Bond dissociation energies from CID studies 1.3.2 Presentation of CID data 1.4 Detectors 1.5 Mass resolution 1.5.1 Mass accuracy 1.6 Data processing 1.7 Isotopes 1.7.1 Isotopic abundances of the elements 1.7.2 Isotope pattern matching References Chapter 2 Mass analysers 2.1 Introduction 2.2 Sectors 2.2.1 MS/MS 2.2.2 Summary 2.3 Quadrupoles 2.3.1 MS/MS 2.3.2 Summary 2.4 Quadrupole Ion Trap 2.4.1 MS/MS and MSn 2.4.2 Summary 2.5 Time-of-flight 2.5.1 Reflectron instruments 2.5.2 Orthogonal TOF (oa-TOF) 2.5.3 MS/MS 2.5.4 Summary 2.6 Fourier Transform Ion Cyclotron Resonance 2.6.1 MS/MS 2.6.2 Summary References Chapter 3 Ionisation techniques 3.1 Introduction 3.2 Electron ionisation 3.2.1 Fragmentation of metal-containing compounds 3.2.2 Applications 3.2.3 Summary 3.3 Chemical Ionisation 3.3.1 Applications 3.3.2 Summary 3.4 Field ionisation / Field desorption 3.4.1 Summary 3.5 Plasma Desorption 3.5.1 Applications 3.5.2 Summary 3.6 Fast Atom Bombardment / Liquid Secondary Ion Mass Spectrometry 3.6.1 Matrices 3.6.2 Ions observed in FAB/LSIMS 3.6.3 Applications 3.6.4 Summary 3.7 Matrix Assisted Laser Desorption Ionisation 3.7.1 Matrices 3.7.2 MALDI of air-sensitive samples 3.7.3 Applications 3.7.4 Summary 3.8 Inductively Coupled Plasma Mass Spectrometry 3.8.1 Applications 3.8.2 Summary 3.9 Electrospray ionisation 3.9.1 Electrochemistry in the ESI process 3.9.2 Multiply-charged species 3.9.3 Nanospray 3.9.4 ESI-MS: Practical considerations 3.9.5 Applications 3.9.6 Summary References Chapter 4 The ESI MS behaviour of simple inorganic compounds 4.1 Introduction 4.2 Simple metal salts 4.2.1 Salts of singly-charged ions, M+X- 4.2.2 Salts of multiply-charged ions, e.g. M2+(X-)2, M3+(X-)3 etc 4.2.3 Negative-ion ESI mass spectra of metal salts 4.2.4 ESI MS behaviour of easily-reduced metal ions: copper(II), iron(III) and mercury(II) 4.3 Polyanions formed by main group elements 4.4 Oxoanions formed by main group elements 4.5 Borane anions 4.6 Fullerenes 4.7 Inorganic phosphorus compounds: phosphoranes and cyclophosphazenes 4.8 Summary References Chapter 5 The ESI MS behaviour of coordination complexes 5.1 Introduction 5.2 Charged, "simple" coordination complexes 5.2.1 Cationic coordination complexes 5.2.2 Anionic metal halide complexes 5.2.3 Highly-charged, anionic transition metal complexes - cyanometallate anions 5.3 (Neutral) metal halide coordination complexes 5.4 Metal complexes of polydentate oxygen donor ligands: polyethers, crown ethers, cryptands and calixarenes 5.5 Porphyrins and metalloporphyrins 5.6 Metal alkoxides - highly moisture-sensitive coordination compounds ?????-Diketonate complexes 5.8 Metal complexes of carbohydrates 5.9 Metal complexes of amino acids, peptides and proteins 5.9.1 Amino acids 5.9.2 Proteins and peptides 5.10 Oxoanions, polyoxoanions and related species 5.10.1 Simple transition metal oxoanions 5.10.2 Reactivity studies involving molybdate and tungstate ions 5.10.3 Polyoxoanions 5.10.4 Miscellaneous oxo complexes 5.11 Metal clusters 5.12 Compounds with anionic sulfur and selenium donor ligands 5.12.1 Metal sulfide, selenide and related complexes 5.12.2 Metal dithiocarbamate and dithiophosphate complexes 5.12.3 Metal thiolate complexes 5.13 Characterisation of metal-based anticancer drugs, their reaction products and metabolites 5.13.1 Characterisation of anticancer-active platinum complexes 5.13.2 Reactions of platinum anticancer drugs with biomolecules and detection of metabolites 5.13.3 Other non-platinum anticancer agents 5.14 In situ formation of coordination complexes as an ionisation technique 5.15 Summary References Chapter 6 The ESI MS behaviour of main group organometallic compounds 6.1 Introduction 6.2 Organometallic derivatives of group 14 elements 6.2.1 Organosilicon compounds 6.2.2 Organogermanium compounds 6.2.3 Organotin compounds 6.2.4 Organolead compounds 6.3 Organometallic derivatives of group 15 elements 6.3.1 Organophosphorus compounds 6.3.1.1 Analysis of phosphine ligands by in situ formation of coordination complexes, oxide or alkylated derivatives 6.3.1.2 Electrospray-friendly phosphine ligands 6.3.1.3 Miscellaneous organophosphorus compounds 6.3.2 Organoarsenic compounds 6.3.2.1 Tertiary arsines 6.3.2.2 Organo-arsenic acids 6.3.2.3 Miscellaneous organoarsenic compounds 6.3.3 Organoantimony and -bismuth compounds 6.4 Organometallic derivatives of group 16 elements; organo-sulfur, -selenium and -tellurium compounds 6.5 Organomercury compounds 6.6 Other organometallic derivatives 6.7 Summary References Chapter 7 The ESI MS behaviour of transition metal and lanthanide organometallic compounds 7.1 Introduction 7.2 Metal carbonyl complexes 7.2.1 Ionic mononuclear metal carbonyl compounds 7.2.2 Ionic metal carbonyl clusters 7.2.3 Neutral metal carbonyl compounds 7.2.3.1 Alkoxide derivatisation 7.2.3.2 Azide derivatisation 7.2.3.3 Metal ion adduction 7.2.3.4 Hydride addition 7.2.4 Oxidation and reduction processes involving metal carbonyls 7.2.5 Characterisation of reaction mixtures involving metal carbonyl clusters 7.2.6 Fragmentation of transition metal carbonyl clusters; electrospray as a source of bare metal clusters 7.2.7 The use of "Electrospray-friendly" ligands in organometallic chemistry 7.3 Metal isocyanide complexes 7.4 Metal cyclopentadienyl and related complexes 7.4.1 Ferrocene-based compounds 7.4.2 Use of ferrocene derivatives as electroactive derivatisation agents for electrospray ionisation 7.4.3 Other metallocene systems 7.4.4 Monocyclopentadienyl complexes 7.5 Metal ?3-allyl complexes 7.6 Metal arene complexes 7.7 Formation of ?-hydrocarbon complexes and their use as an ionisation aid 7.8 Metal-acetylene/acetylide complexes, and complexes of metal-acetylides 7.9 Transition metal ?-alkyl and aryl complexes 7.10 Mass spectrometry of lanthanide organometallic complexes 7.11 Summary References Chapter 8 A selection of special topics 8.1 Introduction 8.2 The characterisation of dendrimers using ESI and MALDI-TOF MS techniques 8.3 Investigating the formation of supramolecular coordination assemblies using ESI MS 8.4 Using ESI MS as a tool for directing chemical synthesis: A case study involving the platinum metalloligands [Pt2(?-E)2(PPh3)4] (E = S, Se) 8.4.1 Background 8.4.2 Analysis of the metalloligands [Pt2(?-E)2(PPh3)4] (E = S, Se) themselves; formation of protonated species. 8.4.3 Reactivity of [Pt2(?-E)2(PPh3)4] towards metal-halide complexes, probed by ESI MS 8.5 Applications of ESI MS in the detection of reactive intermediates and catalyst screening 8.5.1 Detection of intermediates in reactions of organic compounds 8.5.2 Detection and chemistry of reaction intermediates in the gas phase 8.5.3 Screening of new catalysts using mass spectrometry References Appendix 1 Naturally occurring isotopes Appendix 2 Periodic table of the elements Appendix 3 Alphabetical list of elements Appendix 4 Mass Spectrometry Glossary of Terms Appendix 5 Useful sources of information on mass spectrometry
Library of Congress Subject Headings for this publication:
Mass spectrometry.
Chemistry, Inorganic.
Organometallic compounds.