Mass Spectrometry of Inorganic and Organometallic Compounds Tools - Techniques - Tips

, by Henderson, William; McIndoe, J. Scott

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ISBN: 9780470850152 | 0470850159
Cover: Hardcover
Copyright: 4/1/2005

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This is the first modern book to treat inorganic and organometallic mass spectrometry simultaneously. It is textbook and handbook in one; as a textbook it introduces the techniques and gives hints on how to apply the various techniques, as a handbook it lists all available ionization techniques for just about any given compound. The book also includes non-mathematical explanations of how modern MS instruments workMass Spectrometry of Inorganic and Organometallic Compounds will inspire the synthetic inorganic and organometallic chemist with the confidence to apply some of the new techniques to their characterization problems.

Preface

List of commonly-used abbreviations

XIX

1 Fundamentals

(22)

1.1 Introduction

(1)

1.2 Inlets

(1)

1.3 Collision-Induced Dissociation

(4)

1.3.1 Bond dissociation energies from CID studies

(1)

1.3.2 Presentation of CID data

(2)

1.4 Detectors

(1)

1.5 Mass Resolution

(5)

1.5.1 Mass accuracy

(2)

1.6 Data Processing

(2)

1.7 Isotopes

(7)

1.7.1 Isotopic abundances of the elements

(2)

1.7.2 Isotope pattern matching

(2)

References

(2)

2 Mass analysers

(24)

2.1 Introduction

(1)

2.2 Sectors

(4)

2.2.1 MS/MS

(1)

2.2.2 Summary

(1)

2.3 Quadrupoles

(3)

2.3.1 MS/MS

(1)

2.3.2 Summary

(1)

2.4 Quadrupole Ion Trap

(5)

2.4.1 MS/MS and MSn

(1)

2.4.2 Summary

(1)

2.5 Time-of-Flight

(5)

2.5.1 Reflectron instruments

(1)

2.5.2 Orthogonal TOF (oa-TOF)

(1)

2.5.3 MS/MS

(2)

2.5.4 Summary

(1)

2.6 Fourier Transform Ion Cyclotron Resonance

(5)

2.6.1 MS/MS

(1)

2.6.2 Summary

(1)

References

(2)

3 Ionisation techniques

(60)

3.1 Introduction

(1)

3.2 Electron Ionisation

(7)

3.2.1 Fragmentation of metal-containing compounds

(1)

3.2.2 Applications

(2)

3.2.3 Summary

(1)

3.3 Chemical Ionisation

(4)

3.3.1 Applications

(1)

3.3.2 Summary

(1)

3.4 Field Ionisation/Field Desorption

(2)

3.4.1 Summary

(1)

3.5 Plasma Desorption

(2)

3.5.1 Applications

(2)

3.5.2 Summary

(1)

3.6 Fast Atom Bombardment/Liquid Secondary Ion Mass Spectrometry

(10)

3.6.1 Matrices

(2)

3.6.2 Ions observed in FAB/LSIMS

(1)

3.6.3 Applications

(5)

3.6.4 Summary

(1)

3.7 Matrix Assisted Laser Desorption Ionisation

(16)

3.7.1 Matrices

(1)

3.7.2 MALDI of air-sensitive samples

(1)

3.7.3 Applications

(10)

3.7.4 Summary

(1)

3.8 Inductively Coupled Plasma Mass Spectrometry

(2)

3.8.1 Applications

(1)

3.8.2 Summary

(1)

3.9 Electrospray Ionisation

(10)

3.9.1 Electrochemistry in the ESI process

(2)

3.9.2 Multiply-charged species

(1)

3.9.3 Nanospray

(1)

3.9.4 ESI MS: Practical considerations

(3)

3.9.5 Applications

(1)

3.9.6 Summary

(1)

References

100

(7)

4 The ESI MS behaviour of simple inorganic compounds

107

(20)

4.1 Introduction

107

(1)

4.2 Simple Metal Salts

107

(12)

4.2.1 Salts of singly-charged ions, M+X-

107

(5)

4.2.2 Salts of multiply-charged ions, e.g. M²+(X-)2, M³+(X-)3 etc.

112

(4)

4.2.3 Negative-ion ESI mass spectra of metal salts

116

(1)

4.2.4 ESI MS behaviour of easily-reduced metal ions: copper(II), iron(III) and mercury(II)

117

(2)

4.3 Polyanions Formed by Main Group Elements

119

(1)

4.4 Oxoanions Formed by Main Group Elements

119

(3)

4.5 Borane Anions

122

(1)

4.6 Fullerenes

122

(1)

4.7 Inorganic Phosphorus Compounds: Phosphoranes and Cyclophosphazenes

123

(1)

4.8 Summary

123

(1)

References

123

(4)

5 The ESI MS behaviour of coordination complexes

127

(48)

5.1 Introduction

127

(1)

5.2 Charged, 'Simple' Coordination Complexes

128

(8)

5.2.1 Cationic coordination complexes

128

(4)

5.2.2 Anionic metal halide complexes

132

(2)

5.2.3 Highly-charged, anionic transition metal complexes - cyanometallate anions

134

(2)

5.3 (Neutral) Metal Halide Coordination Complexes

136

(3)

5.4 Metal Complexes of Polydentate Oxygen Donor Ligands: Polyethers, Crown Ethers, Cryptands and Calixarenes

139

(2)

5.5 Porphyrins and Metalloporphyrins

141

(3)

5.6 Metal Alkoxides - Highly Moisture-Sensitive Coordination Compounds

144

(1)

5.7 &beta'-Diketonate Complexes

145

(3)

5.8 Metal Complexes of Carbohydrates

148

(1)

5.9 Metal Complexes of Amino Acids, Peptides and Proteins

149

(2)

5.9.1 Amino acids

149

(1)

5.9.2 Proteins and peptides

150

(1)

5.10 Oxoanions, Polyoxoanions and Related Species

151

(6)

5.10.1 Simple transition metal oxoanions

151

(3)

5.10.2 Reactivity studies involving molybdate and tungstate ions

154

(1)

5.10.3 Polyoxoanions

155

(2)

5.10.4 Miscellaneous oxo complexes

157

(1)

5.11 Metal Clusters

157

(1)

5.12 Compounds with Anionic Sulfur and Selenium Donor Ligands

158

(5)

5.12.1 Metal sulfide, selenide and related complexes

158

(1)

5.12.2 Metal dithiocarbamate and dithiophosphate complexes

159

(1)

5.12.3 Metal thiolate complexes

160

(3)

5.13 Characterisation of Metal-Based Anticancer Drugs, their Reaction Products and Metabolites

163

(3)

5.13.1 Characterisation of anticancer-active platinum complexes

163

(2)

5.13.2 Reactions of platinum anticancer drugs with biomolecules and detection of metabolites

165

(1)

5.13.3 Other non-platinum anticancer agents

166

(1)

5.14 In situ Formation of Coordination Complexes as an Ionisation Technique

166

(1)

5.15 Summary

167

(1)

References

168

(7)

6 The ESI MS behaviour of main group organometallic compounds

175

(20)

6.1 Introduction

175

(1)

6.2 Organometallic Derivatives of Group 14 Elements

175

(5)

6.2.1 Organosilicon compounds

175

(1)

6.2.2 Organogermanium compounds

176

(1)

6.2.3 Organotin compounds

176

(2)

6.2.4 Organolead compounds

178

(2)

6.3 Organometallic Derivatives of Group 15 Elements

180

(8)

6.3.1 Organophosphorus compounds

180

(5)

6.3.2 Organoarsenic compounds

185

(2)

6.3.3 Organoantimony and -bismuth compounds

187

(1)

6.4 Organometallic Derivatives of Group 16 Elements; Organosulfur, -Selenium and -Tellurium Compounds

188

(1)

6.5 Organomercury Compounds

188

(2)

6.6 Other Organometallic Derivatives

190

(1)

6.7 Summary

190

(1)

References

190

(5)

7 The ESI MS behaviour of transition metal and lanthanide organometallic compounds

195

(26)

7.1 Introduction

195

(1)

7.2 Metal Carbonyl Complexes

195

(9)

7.2.1 Ionic mononuclear metal carbonyl compounds

196

(1)

7.2.2 Ionic metal carbonyl clusters

196

(2)

7.2.3 Neutral metal carbonyl compounds

198

(3)

7.2.4 Oxidation and reduction processes involving metal carbonyls

201

(1)

7.2.5 Characterisation of reaction mixtures involving metal carbonyl clusters

201

(2)

7.2.6 Fragmentation of transition metal carbonyl clusters; electrospray as a source of bare metal clusters

203

(1)

7.2.7 The use of 'Electrospray-friendly' ligands in organometallic chemistry

204

(1)

7.3 Metal Isocyanide Complexes

204

(1)

7.4 Metal Cyclopentadicnyl and Related Complexes

205

(6)

7.4.1 Fenocene-based compounds

205

(4)

7.4.2 Use of ferrocene derivatives as elcctroactive derivatisation agents for electrospray ionisation

209

(1)

7.4.3 Other metallocene systems

210

(1)

7.4.4 Monocyclopentadienyl complexes

210

(1)

7.5 Metal η³-allyl Complexes

211

(1)

7.6 Metal Arene Complexes

212

(1)

7.7 Formation of π-Hydrocarbon Complexes and their Use as an Ionisation Aid

212

(1)

7.8 Metal-Acetylene/acetylide Complexes and Complexes of Metal-Acetylides

213

(1)

7.9 Transition Metal σ-Alkyl and Aryl Complexes

214

(1)

7.10 Mass Spectrometry of Lanthanide Organometallic Complexes

215

(1)

7.11 Summary

215

(1)

References

215

(6)

8 A selection of special topics

221

(14)

8.1 Introduction

221

(1)

8.2 Characterisation of Dendrimers Using ES1 and MALDI-TOF MS Techniques

221

(1)

8.3 Investigating the Formation of Supramolecular Coordination Assemblies Using ESI MS

222

(2)

8.4 Using ESI MS as a Tool for Directing Chemical Synthesis: A Case Study Involving the Platinum Metalloligands [Pt2(μ-Epsilon)2(PPh3)4]

224

(4)

8.4.1 Background

224

(1)

8.4.2 Analysis of the metalloligands; formation of protonated species

225

(1)

8.4.3 Reactivity of [Pt2(μ-Epsilon)2(PPh3)4] towards metal-halide complexes

226

(2)

8.5 Applications of ESI MS in the Detection of Reactive Intermediates and Catalyst Screening

228

(4)

8.5.1 Detection of intermediates in reactions of organic compounds

228

(2)

8.5.2 Detection and chemistry of reaction intermediates in the gas phase

230

(1)

8.5.3 Screening of new catalysts using mass spectrometry

231

(1)

References

232

(3)

Appendix 1 Naturally occurring isotopes

235

(12)

Appendix 2 Periodic table of the elements

247

(2)

Appendix 3 Alphabetical list of elements

249

(2)

Appendix 4 Glossary of terms

251

(14)

Appendix 5 Useful sources of information

265

(2)

Index

267

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Mass Spectrometry of Inorganic and Organometallic Compounds Tools - Techniques - Tips

Summary

Author Biography

Table of Contents

Supplemental Materials