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

by Henderson, William; McIndoe, J. Scott

• ISBN13: 9780470850169
• ISBN10: 0470850167
• Edition: 1st
• Format: Paperback
• Copyright: 2005-04-01
• Publisher: Wiley-Interscience

Summary

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 work Mass 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.

Author Biography

William Henderson is the author of Mass Spectrometry of Inorganic and Organometallic Compounds: Tools - Techniques - Tips, published by Wiley.

J. Scott McIndoe is the author of Mass Spectrometry of Inorganic and Organometallic Compounds: Tools - Techniques - Tips, published by Wiley.

Table of Contents

Preface	XV
List of commonly-used abbreviations	XIX
1 Fundamentals	1	(22)
1.1 Introduction	1	(1)
1.2 Inlets	1	(1)
1.3 Collision-Induced Dissociation	2	(4)
1.3.1 Bond dissociation energies from CID studies	4	(1)
1.3.2 Presentation of CID data	4	(2)
1.4 Detectors	6	(1)
1.5 Mass Resolution	7	(5)
1.5.1 Mass accuracy	10	(2)
1.6 Data Processing	12	(2)
1.7 Isotopes	14	(7)
1.7.1 Isotopic abundances of the elements	17	(2)
1.7.2 Isotope pattern matching	19	(2)
References	21	(2)
2 Mass analysers	23	(24)
2.1 Introduction	23	(1)
2.2 Sectors	23	(4)
2.2.1 MS/MS	26	(1)
2.2.2 Summary	26	(1)
2.3 Quadrupoles	27	(3)
2.3.1 MS/MS	29	(1)
2.3.2 Summary	30	(1)
2.4 Quadrupole Ion Trap	30	(5)
2.4.1 MS/MS and MSn	33	(1)
2.4.2 Summary	34	(1)
2.5 Time-of-Flight	35	(5)
2.5.1 Reflectron instruments	37	(1)
2.5.2 Orthogonal TOF (oa-TOF)	38	(1)
2.5.3 MS/MS	38	(2)
2.5.4 Summary	40	(1)
2.6 Fourier Transform Ion Cyclotron Resonance	40	(5)
2.6.1 MS/MS	43	(1)
2.6.2 Summary	44	(1)
References	45	(2)
3 Ionisation techniques	47	(60)
3.1 Introduction	47	(1)
3.2 Electron Ionisation	47	(7)
3.2.1 Fragmentation of metal-containing compounds	50	(1)
3.2.2 Applications	51	(2)
3.2.3 Summary	53	(1)
3.3 Chemical Ionisation	54	(4)
3.3.1 Applications	56	(1)
3.3.2 Summary	57	(1)
3.4 Field Ionisation/Field Desorption	58	(2)
3.4.1 Summary	59	(1)
3.5 Plasma Desorption	60	(2)
3.5.1 Applications	60	(2)
3.5.2 Summary	62	(1)
3.6 Fast Atom Bombardment/Liquid Secondary Ion Mass Spectrometry	62	(10)
3.6.1 Matrices	63	(2)
3.6.2 Ions observed in FAB/LSIMS	65	(1)
3.6.3 Applications	66	(5)
3.6.4 Summary	71	(1)
3.7 Matrix Assisted Laser Desorption Ionisation	72	(16)
3.7.1 Matrices	75	(1)
3.7.2 MALDI of air-sensitive samples	76	(1)
3.7.3 Applications	77	(10)
3.7.4 Summary	87	(1)
3.8 Inductively Coupled Plasma Mass Spectrometry	88	(2)
3.8.1 Applications	89	(1)
3.8.2 Summary	90	(1)
3.9 Electrospray Ionisation	90	(10)
3.9.1 Electrochemistry in the ESI process	92	(2)
3.9.2 Multiply-charged species	94	(1)
3.9.3 Nanospray	95	(1)
3.9.4 ESI MS: Practical considerations	96	(3)
3.9.5 Applications	99	(1)
3.9.6 Summary	99	(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 β-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