Mass spectrometry: a textbook
Gespeichert in:
| Beteilige Person: | |
|---|---|
| Format: | Buch |
| Sprache: | Englisch |
| Veröffentlicht: |
Heidelberg [u.a.]
Springer
2011
|
| Ausgabe: | 2. ed. |
| Schlagwörter: | |
| Links: | http://deposit.dnb.de/cgi-bin/dokserv?id=3430798&prov=M&dok_var=1&dok_ext=htm http://bvbr.bib-bvb.de:8991/F?func=service&doc_library=BVB01&local_base=BVB01&doc_number=020326232&sequence=000001&line_number=0001&func_code=DB_RECORDS&service_type=MEDIA |
| Umfang: | XXIV, 753 Seiten Illustrationen, Diagramme 24 cm |
| ISBN: | 9783642107092 |
Internformat
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| 245 | 1 | 0 | |a Mass spectrometry |b a textbook |c Jürgen H. Gross |
| 250 | |a 2. ed. | ||
| 264 | 1 | |a Heidelberg [u.a.] |b Springer |c 2011 | |
| 300 | |a XXIV, 753 Seiten |b Illustrationen, Diagramme |c 24 cm | ||
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Datensatz im Suchindex
| DE-BY-TUM_call_number | 0202 PHY 115f 2004 A 71(2) 0302 CHE 254f 2013 A 2287(2) |
|---|---|
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| DE-BY-TUM_location | 02 03 |
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| adam_text | IMAGE 1
TABLE OF CONTENTS
TABLE OF CONTENTS XI
1 INTRODUCTION 1
LEARNING OBJECTIVES 1
1.1 AIMS AND SCOPE 3
1.1.1 FILLING THE BLACK BOX 5
1.2 WHAT IS MASS SPECTROMETRY? 5
1.2.1 MASS SPECTROMETRY 6
1.2.2 MASS SPECTROMETER 7
1.2.3 MASS SCALE 8
1.2.4 MASS SPECTRUM 9
1.3 ION CHROMATOGRAMS 11
1.4 PERFORMANCE OF MASS SPECTROMETERS 13
1.4.1 SENSITIVITY 13
1.4.2 DETECTION LIMIT 14
1.4.3 SIGNAL-TO-NOISE RATIO 14
1.5 TERMINOLOGY - GENERAL ASPECTS 15
1.5.1 BASIC TERMINOLOGY IN DESCRIBING MASS SPECTRA 16
1.6 UNITS, PHYSICAL QUANTITIES, AND PHYSICAL CONSTANTS 17
REFERENCES 17
2 PRINCIPLES OF IONIZATION AND ION DISSOCIATION 21
LEARNING OBJECTIVES 21
2.1 GAS PHASE IONIZATION BY ENERGETIC ELECTRONS 21
.1 FORMATION OF IONS 22
.2 PROCESSES ACCOMPANYING ELECTRON IONIZATION 23
.3 IONS GENERATED BY PENNING IONIZATION 24
.4 IONIZATION ENERGY 25
.5 IONIZATION ENERGY AND CHARGE-LOCALIZATION 25
2.2 VERTICAL TRANSITIONS 27
2.3 IONIZATION EFFICIENCY AND IONIZATION CROSS SECTION 29
BIBLIOGRAFISCHE INFORMATIONEN HTTP://D-NB.INFO/1000389022
DIGITALISIERT DURCH
IMAGE 2
XII TABLE OF CONTENTS
2.4 INTERNAL ENERGY AND THE FURTHER FATE OF IONS 30
2.4.1 DEGREES OF FREEDOM 31
2.4.2 APPEARANCE ENERGY 32
2.4.3 BOND DISSOCIATION ENERGIES AND HEATS OF FORMATION 33 2.4.4
RANDOMIZATION OF ENERGY 35
2.5 QUASI-EQUILIBRIUM THEORY 37
2.5.1 QET S BASIC PREMISES 37
2.5.2 BASIC QET 38
2.5.3 RATE CONSTANTS AND THEIR MEANING 39
2.5.4 &( E ) FUNCTIONS - TYPICAL EXAMPLES 40
2.5.5 REACTING IONS DESCRIBED BY (E) FUNCTIONS 40
2.5.6 DIRECT CLEAVAGES AND REARRANGEMENT FRAGMENTATIONS 40 2.6 TIME
SCALE OF EVENTS 42
2.6.1 STABLE, METASTABLE, AND UNSTABLE IONS 43
2.6.2 TIME SCALE OF ION STORAGE DEVICES 44
2.7 INTERNAL ENERGY - PRACTICAL IMPLICATIONS 45
2.8 REVERSE REACTIONS AND KINETIC ENERGY RELEASE 46
2.8.1 ACTIVATION ENERGY OF THE REVERSE REACTION 46
2.8.2 KINETIC ENERGY RELEASE 48
2.8.3 ENERGY PARTITIONING 49
2.9 ISOTOPE EFFECTS 49
2.9.1 PRIMARY KINETIC ISOTOPE EFFECTS 50
2.9.2 MEASUREMENT OF ISOTOPE EFFECTS 51
2.9.3 SECONDARY KINETIC ISOTOPE EFFECTS 53
2.10 DETERMINATION OF IONIZATION ENERGIES 54
2.10.1 CONVENTIONAL DETERMINATION OF IONIZATION ENERGIES 54 2.10.2
IMPROVED IE ACCURACY FROM DATA POST-PROCESSING 54 2.10.3 IE ACCURACY -
EXPERIMENTAL IMPROVEMENTS 55
2.10.4 PHOTOIONIZATION PROCESSES 55
2.11 DETERMINING THE APPEARANCE ENERGIES 58
2.11.1 KINETIC SHIFT 58
2.11.2 BREAKDOWN GRAPHS 59
2.12 GAS PHASE BASICITY AND PROTON AFFINITY 61
REFERENCES 62
3 ISOTOPIC COMPOSITION AND ACCURATE MASS 67
LEARNING OBJECTIVES 67
3.1 ISOTOPIC CLASSIFICATION OF THE ELEMENTS 67
3.1.1 MONOISOTOPIC ELEMENTS 68
.2 DI-ISOTOPIC ELEMENTS 68
.3 POLYISOTOPIC ELEMENTS 69
.4 REPRESENTATION OF ISOTOPIC ABUNDANCES 69
.5 CALCULATION OF ATOMIC, MOLECULAR, AND IONIC MASS 71
.6 NATURAL VARIATIONS IN RELATIVE ATOMIC MASS 73
3.2 CALCULATION OF ISOTOPIC DISTRIBUTIONS 74
3.2.1 CARBON: AN X+L ELEMENT 74
IMAGE 3
TABLE OF CONTENTS XIII
3.2.2 TERMS RELATED TO ISOTOPIC COMPOSITION 77
3.2.3 BINOMIAL APPROACH 77
3.2.4 HALOGENS 78
3.2.5 COMBINATIONS OF CARBON AND HALOGENS 80
3.2.6 POLYNOMIAL APPROACH 81
3.2.7 OXYGEN, SILICON, AND SULFUR 81
3.2.8 POLYISOTOPIC ELEMENTS 84
3.2.9 PRACTICAL ASPECTS OF ISOTOPIC PATTERNS 84
3.2.10 BOOKKEEPING WITH ISOTOPIC PATTERNS IN MASS SPECTRA 85 3.2.11
INFORMATION FROM COMPLEX ISOTOPIC PATTERNS 86
3.3 ISOTOPIC ENRICHMENT AND ISOTOPIC LABELING 87
3.3.1 ISOTOPIC ENRICHMENT 87
3.3.2 ISOTOPIC LABELING 88
3.4 RESOLUTION AND RESOLVING POWER 88
3.4.1 DEFINITIONS 88
3.4.2 RESOLUTION AND ITS EXPERIMENTAL DETERMINATION 90
3.4.3 RESOLVING POWER AND ITS EFFECT ON RELATIVE PEAK INTENSITY 91 3.5
ACCURATE MASS 92
3.5.1 EXACT MASS AND MOLECULAR FORMULAS 92
3.5.2 MASS DEFECT 93
3.5.3 MASS ACCURACY 95
3.5.4 ACCURACY AND PRECISION 96
3.5.5 MASS ACCURACY AND THE DETERMINATION OF MOLECULAR FORMULAS 97 3.5.6
EXTREME MASS ACCURACY - SPECIAL CONSIDERATIONS 98
3.6 APPLIED HIGH-RESOLUTION MASS SPECTROMETRY 99
3.6.1 EXTERNAL MASS CALIBRATION 99
3.6.2 INTERNAL MASS CALIBRATION 101
3.6.3 COMPILING MASS REFERENCE LISTS 103
3.6.4 SPECIFICATION OF MASS ACCURACY 104
3.6.5 DELTAMASS 104
3.6.6 KENDRICK MASS SCALE 105
3.6.7 VAN KREVELEN DIAGRAMS 106
3.7 RESOLUTION INTERACTING WITH ISOTOPIC PATTERNS 107
3.7.1 MULTIPLE ISOTOPIC COMPOSITIONS AT VERY HIGH RESOLUTION 107 3.7.2
ISOTOPOLOGS AND ACCURATE MASS 110
3.7.3 LARGE MOLECULES - ISOTOPIC PATTERNS AT SUFFICIENT RESOLUTION 110
3.7.4 LARGE MOLECULES - ISOTOPIC PATTERNS AT LOW RESOLUTION 112 3.8
CHARGE STATE AND INTERACTION WITH ISOTOPIC PATTERNS 112
REFERENCES 114
4 INSTRUMENTATION 117
LEARNING OBJECTIVES 117
4.1 HOW TO CREATE A BEAM OF IONS 119
4.2 TIME-OF-FLIGHT INSTRUMENTS 120
4.2.1 TIME-OF-FLIGHT - BASIC PRINCIPLES 120
4.2.2 TOF INSTRUMENTS - VELOCITY OF IONS AND TIME-OF-FLIGHT 121 4.2.3
LINEAR TIME-OF-FLIGHT ANALYZER 123
IMAGE 4
XIV TABLE OF CONTENTS
4.2.4 REFLECTOR TIME-OF-FLIGHT ANALYZER 126
4.2.5 HIGHER VACUUM IMPROVES RESOLVING POWER 128
4.2.6 DELAY BEFORE EXTRACTION TO IMPROVE RESOLVING POWER 128 4.2.7
ANALOG-TO-DIGITAL CONVERSION 131
4.2.8 ORTHOGONAL ACCELERATION TOF ANALYZERS 132
4.2.9 OPERATION OF THE OATOF ANALYZER 133
4.2.10 DUTY CYCLE 134
4.2.11 TIME-TO-DIGITAL CONVERSION 135
4.3 MAGNETIC SECTOR INSTRUMENTS 135
4.3.1 EVOLUTION OF MAGNETIC SECTOR INSTRUMENTS 135
4.3.2 PRINCIPLE OF THE MAGNETIC SECTOR 136
4.3.3 FOCUSING ACTION OF THE MAGNETIC FIELD 138
4.3.4 DOUBLE-FOCUSING SECTOR INSTRUMENTS 139
4.3.5 GEOMETRIES OF DOUBLE-FOCUSING SECTOR INSTRUMENTS 141 4.3.6
ADJUSTING THE RESOLVING POWER OF A SECTOR INSTRUMENT 143 4.3.7
INNOVATIONS IN SECTOR INSTRUMENTS 144
4.4 LINEAR QUADRUPOLE INSTRUMENTS 146
4.4.1 INTRODUCTION 146
4.4.2 THE LINEAR QUADRUPOLE 147
4.4.3 RESOLVING POWER OF LINEAR QUADRUPOLES 151
4.4.4 RF-ONLY QUADRUPOLES, HEXAPOLES, AND OCTOPOLES 152 4.5 LINEAR
QUADRUPOLE ION TRAPS 155
4.5.1 LINEAR RF-ONLY MULTIPOLE ION TRAPS 155
4.5.2 MASS-ANALYZING LINEAR QUADRUPOLE ION TRAP WITH AXIAL EJECTION .
158 4.5.3 MASS-ANALYZING LINEAR ION TRAP WITH RADIAL EJECTION 160 4.6
THREE-DIMENSIONAL QUADRUPOLE ION TRAP 164
4.6.1 INTRODUCTION 164
4.6.2 THE QUADRUPOLE ION TRAP 164
4.6.3 VISUALIZATION OF ION MOTION IN THE ION TRAP 167
4.6.4 MASS-SELECTIVE STABILITY MODE 168
4.6.5 MASS-SELECTIVE INSTABILITY MODE 168
4.6.6 RESONANT EJECTION 169
4.6.7 AXIAL MODULATION AND AUTOMATIC GAIN CONTROL 170
4.6.8 NONLINEAR RESONANCES 171
4.6.9 DIGITAL WAVEFORM QUADRUPOLE ION TRAP 172
4.6.10 EXTERNAL ION SOURCES FOR THE QUADRUPOLE ION TRAP 173 4.7 FOURIER
TRANSFORM ION CYCLOTRON RESONANCE 174
4.7.1 ION CYCLOTRON RESONANCE 174
4.7.2 ION CYCLOTRON MOTION 174
4.7.3 CYCLOTRON MOTION - EXCITATION AND DETECTION 175
4.7.4 CYCLOTRON FREQUENCY BANDWIDTH AND ENERGY-TIME UNCERTAINTY 177
4.7.5 FOURIER TRANSFORM - BASIC PROPERTIES 179
4.7.6 NYQUIST CRITERION 181
4.7.7 EXCITATION MODES IN FT-ICR-MS 182
4.7.8 AXIAL TRAPPING AND DESIGN OF ICR CELLS 183
4.7.9 MAGNETRON MOTION AND REDUCED CYCLOTRON FREQUENCY 184
IMAGE 5
TABLE OF CONTENTS XV
4.7.10 DETECTION AND ACCURACY IN FT-ICR-MS 186
4.7.11 FT-ICR INSTRUMENTS 187
4.8 ORBITRAP ANALYZER 189
4.8.1 ORBITRAP - PRINCIPLE OF OPERATION 189
4.8.2 ION DETECTION AND RESOLVING POWER OF THE ORBITRAP 191 4.8.3 ION
INJECTION INTO THE ORBITRAP 192
4.8.4 HYBRIDIZATION WITH A LINEAR QUADRUPOLE ION TRAP 193 4.9 HYBRID
INSTRUMENTS 194
4.9.1 EVOLUTION OF HYBRID MASS SPECTROMETERS 196
4.9.2 ION MOBILITY-MASS SPECTROMETRY SYSTEMS 198
4.10 DETECTORS 202
4.10.1 DISCRETE DYNODE ELECTRON MULTIPLIERS 203
4.10.2 CHANNEL ELECTRON MULTIPLIERS 204
4.10.3 MICROCHANNEL PLATES 205
4.10.4 POST-ACCELERATION AND CONVERSION DYNODE 206
4.10.5 FOCAL PLANE DETECTORS 207
4.11 VACUUM TECHNOLOGY 208
4.11.1 BASIC MASS SPECTROMETER VACUUM SYSTEM 209
4.11.2 HIGH VACUUM PUMPS 209
4.12 PURCHASING AN INSTRUMENT 210
REFERENCES 210
5 PRACTICAL ASPECTS OF ELECTRON IONIZATION 223
LEARNING OBJECTIVES 223
5.1 ELECTRON IONIZATION ION SOURCES 223
5.1.1 LAYOUT OF AN ELECTRON IONIZATION ION SOURCE 223
5.1.2 GENERATION OF PRIMARY ELECTRONS 225
5.1.3 OVERALL EFFICIENCY AND SENSITIVITY OF AN EL ION SOURCE 226 5.1.4
OPTIMIZATION OF ION BEAM GEOMETRY 227
5.2 SAMPLE INTRODUCTION 228
5.2.1 RESERVOIR OR REFERENCE INLET SYSTEM 228
5.2.2 DIRECT INSERTION PROBE 231
5.2.3 SAMPLE VIALS FOR USE WITH DIRECT INSERTION PROBES 232 5.2.4
FRACTIONATION WHEN USING DIRECT INSERTION PROBES 233 5.2.5 DIRECT
EXPOSURE PROBE 235
5.3 PYROLYSIS MASS SPECTROMETRY 237
5.4 GAS CHROMATOGRAPH 237
5.5 LIQUID CHROMATOGRAPH 238
5.6 LOW-ENERGY ELECTRON IONIZATION MASS SPECTRA 239
5.7ANALYTESFOREI 241
5.8 MASS ANALYZERS FOR EL 241
5.9 MASS SPECTRAL DATABASES FOR EL 242
5.9.1 NIST/EPA/NIH MASS SPECTRAL DATABASE 243
5.9.2 WILEY REGISTRY OF MASS SPECTRAL DATA 244
5.9.3 MASS SPECTRAL DATABASES - GENERAL ASPECTS 244
REFERENCES 245
IMAGE 6
XVI TABLE OF CONTENTS
6 FRAGMENTATION OF ORGANIC IONS AND INTERPRETATION OF EL MASS SPECTRA
...249 LEARNING OBJECTIVES 249
6.1 CLEAVAGE OF A SIGMA-BOND 250
6.1.1 WRITING CONVENTIONS FOR MOLECULAR IONS 250
6.1.2 A-BOND CLEAVAGE IN SMALL NONFUNCTIONALIZED MOLECULES 251 6.1.3
EVEN-ELECTRON RULE 252
6.1.4 CT-BOND CLEAVAGE IN SMALL FUNCTIONALIZED MOLECULES 254 6.2
ALPHA-CLEAVAGE 255
6.2.1 A-CLEAVAGE OF ACETONE MOLECULAR ION 255
6.2.2 STEVENSON S RULE 257
6.2.3 A-CLEAVAGE OF NONSYMMETRICAL ALIPHATIC KETONES 259 6.2.4 ACYLIUM
IONS AND CARBENIUM IONS 260
6.2.5 A-CLEAVAGE WHEN HETEROATOMS BELONG TO THE ALIPHATIC CHAIN 262
6.2.6 A-CIEAVAGE OF ALIPHATIC AMINES 262
6.2.7 NITROGEN RULE 265
6.2.8 A-CLEAVAGE OF ALIPHATIC ETHERS AND ALCOHOLS 266
6.2.9 CHARGE RETENTION AT THE HETEROATOM 268
6.2.10 A-CLEAVAGE OF THIOETHERS 269
6.2.11 A-CLEAVAGE OF HALOGENATED HYDROCARBONS 269
6.2.12 DOUBLE A-CLEAVAGE 271
6.2.13 DOUBLE A-CLEAVAGE FOR THE IDENTIFICATION OF REGIOISOMERS 272 6.3
DISTONIC IONS 273
6.3.1 DEFINITION OF DISTONIC IONS 273
6.3.2 FORMATION AND PROPERTIES OF DISTONIC IONS 274
6.3.3 DISTONIC IONS AS INTERMEDIATES 275
6.4 BENZYLIC BOND CLEAVAGE 275
6.4.1 CLEAVAGE OF THE BENZYLIC BOND IN PHENYLALKANES 275
6.4.2 THE FURTHER FATE OF [C 6 H 5 ] + AND [C 7 H 7 J + 277
6.4.3 ISOMERIZATION OF [C 7 H 8 ] + AND [C 8 H 8 ] + IONS 279
6.4.4 RINGS PLUS DOUBLE BONDS 280
6.5 ALLYLIC BOND CLEAVAGE 281
6.5.1 CLEAVAGE OF THE ALLYLIC BOND IN ALIPHATIC ALKENES 281 6.5.2
METHODS FOR THE LOCALIZATION OF THE DOUBLE BOND 283
6.6. CLEAVAGE OF NON-ACTIVATED BONDS 284
6.6.1 SATURATED HYDROCARBONS 284
6.6.2 CARBENIUM IONS 286
6.6.3 VERY LARGE HYDROCARBONS 287
6.6.4 RECOGNITION OF THE MOLECULAR ION PEAK 288
6.7 MCLAFFERTY REARRANGEMENT 290
6.7.1 MCL OF ALDEHYDES AND KETONES 290
6.7.2 FRAGMENTATION OF CARBOXYLIC ACIDS AND THEIR DERIVATIVES 293 6.7.3
MCL OF AROMATIC HYDROCARBONS 296
6.7.4 MCL WITH DOUBLE HYDROGEN TRANSFER 297
6.8 RETRO-DIELS-ALDER REACTION 300
6.8.1 PROPERTIES OF THE RETRO-DIELS-ALDER REACTION 300
IMAGE 7
TABLE OF CONTENTS XVII
6.8.2 INFLUENCE OF POSITIONAL ISOMERISM ON THE RDA REACTION 302 6.8.3
RDA REACTION IN NATURAL PRODUCTS 303
6.8.4 WIDESPREAD OCCURRENCE OF THE RDA REACTION 303
6.9 ELIMINATION OF CARBON MONOXIDE 304
6.9.1 CO LOSS FROM PHENOLS 304
6.9.2 CO AND C 2 H 2 LOSS FROM QUINONES 307
6.9.3 FRAGMENTATION OF ARYLALKYLETHERS 308
6.9.4 CO LOSS FROM TRANSITION METAL CARBONYL COMPLEXES 310 6.9.5 CO LOSS
FROM CARBONYL COMPOUNDS 311
6.9.6 DIFFERENTIATION BETWEEN LOSS OF CO, N 2 , AND C 2 H 4 311
6.10 THERMAL DEGRADATION VS. ION FRAGMENTATION 312
6.10.1 DECARBONYLATION AND DECARBOXYLATION 312
6.10.2 RETRO-DIELS-ALDER REACTION 312
6.10.3 LOSS OF H 2 O FROM ALKANOLS 312
6.10.4 EL MASS SPECTRA OF ORGANIC SALTS 314
6.11 ALKENE LOSS FROM ONIUM IONS 315
6.11.1 MCL OF ONIUM IONS 316
6.11.2 ONIUM REACTION 319
6.12 ION-NEUTRAL COMPLEXES 322
6.12.1 EVIDENCE FOR THE EXISTENCE OF ION-NEUTRAL COMPLEXES 322 6.12.2
ATTRACTIVE FORCES IN ION-NEUTRAL COMPLEXES 323
6.12.3 CRITERIA FOR ION-NEUTRAL COMPLEXES 324
6.12.4 ION-NEUTRAL COMPLEXES OF RADICAL IONS 325
6.13 ORTHO ELIMINATION (ORTHO EFFECT) 326
6.13.1 ORTHO ELIMINATION FROM MOLECULAR IONS 327
6.13.2 ORTHO ELIMINATION FROM EVEN-ELECTRON IONS 328
6.13.3 ORTHO ELIMINATION IN THE FRAGMENTATION OF NITROARENES 331 6.14
HETEROCYCLIC COMPOUNDS 332
6.14.1 SATURATED HETEROCYCLIC COMPOUNDS 333
6.14.2 AROMATIC HETEROCYCLIC COMPOUNDS 336
6.15 GUIDE TO THE INTERPRETATION OF MASS SPECTRA 340
6.15.1 SUMMARY OF RULES 340
6.15.2 SYSTEMATIC APPROACH TO MASS SPECTRA 341
REFERENCES 342
7 CHEMICAL IONIZATION 351
LEARNING OBJECTIVES 351
7.1 BASICS OF CHEMICAL IONIZATION 351
7.1.1 FORMATION OF IONS IN POSITIVE-ION CHEMICAL IONIZATION 351 7.1.2
CHEMICAL IONIZATION ION SOURCES 352
7.1.3 SENSITIVITY OF CHEMICAL IONIZATION 353
7.1.4 CHEMICAL IONIZATION TECHNIQUES AND TERMS 353
7.2 PROTONATION IN CHEMICAL IONIZATION 354
7.2.1 SOURCE OF PROTONS 354
7.2.2 METHANE REAGENT GAS PLASMA 355
7.2.3 CH 5 + AND RELATED IONS 356
IMAGE 8
XVIII TABLE OF CONTENTS
7.2.4 ENERGETICS OF PROTONATION 356
7.2.5 IMPURITIES OF HIGHER PA THAN THE REAGENT GAS 357
7.2.6 METHANE REAGENT GAS PICI SPECTRA 358
7.2.7 OTHER REAGENT GASES IN PICI 359
7.3 PROTON TRANSFER REACTION MASS SPECTROMETRY 361
7.3.1 REACTANT ION FORMATION IN PTR-MS 362
7.3.2 ANALYTE ION FORMATION IN PTR-MS 362
7.4 CHARGE EXCHANGE CHEMICAL IONIZATION 364
7.4.1 ENERGETICS OF CE 365
7.4.2 REAGENT GASES FOR CE-CI 365
7.4.3 COMPOUND CLASS-SELECTIVE CE-CI 366
7.4.4 REGIO- AND STEREOSELECTIVITY IN CE-CI 368
7.5 NEGATIVE-ION CHEMICAL IONIZATION 368
7.6 ELECTRON CAPTURE 370
7.6.1 ION FORMATION BY ELECTRON CAPTURE 370
7.6.2 ENERGETICS OF EC 370
7.6.3 CREATING THERMAL ELECTRONS 372
7.6.4 APPEARANCE OF EC SPECTRA 373
7.6.5 APPLICATIONS OF EC 373
7.7 DESORPTION CHEMICAL IONIZATION 374
7.8 ANALYTES FOR CI 375
REFERENCES 376
8 FIELD IONIZATION AND FIELD DESORPTION 381
LEARNING OBJECTIVES 381
8.1 FIELD IONIZATION PROCESS 382
8.2 FI AND FD ION SOURCES 383
8.3 FIELD EMITTERS 385
8.3.1 BLANK METAL WIRES AS EMITTERS 385
8.3.2 ACTIVATED EMITTERS 385
8.3.3 EMITTER TEMPERATURE 386
8.3.4 HANDLING OF ACTIVATED EMITTERS 387
8.4 FIELD IONIZATION MASS SPECTROMETRY 388
8.4.1 ORIGIN OF [M+H] + IONS IN FI-MS 389
8.4.2 MULTIPLY-CHARGED IONS IN FI-MS 389
8.4.3 FIELD-INDUCED DISSOCIATION 390
8.4.4 ACCURATE MASS FI SPECTRA 390
8.4.5 COUPLING GAS CHROMATOGRAPHY TO FI-MS 391
8.5 FD SPECTRA 392
8.5.1 ION FORMATION BY FIELD IONIZATION IN FD-MS 393
8.5.2 DESORPTION OF PREFORMED IONS IN FD-MS 394
8.5.3 CLUSTER ION FORMATION IN FD-MS 396
8.5.4 FD-MS OF IONIC ANALYTES 397
8.5.5 BEST ANODE TEMPERATURE AND THERMAL DECOMPOSITION 399 8.5.6 FD-MS
OF POLYMERS 400
8.5.7 TYPES OF IONS IN FD-MS 401
IMAGE 9
TABLE OF CONTENTS XIX
8.6 LIQUID INJECTION FIELD DESORPTION IONIZATION 402
8.7 GENERAL PROPERTIES OF FI-MS AND FD-MS 405
8.7.1 SENSITIVITY OF FI-MS AND FD-MS 405
8.7.2 ANALYTES AND PRACTICAL CONSIDERATIONS FOR FI, FD, AND LIFDI 407
8.7.3 MASS ANALYZERS FOR FI AND FD 407
REFERENCES 408
9 TANDEM MASS SPECTROMETRY 415
LEARNING OBJECTIVES 415
9.1 CONCEPTS OF TANDEM MASS SPECTROMETRY 415
9.1.1 TANDEM-IN-SPACE AND TANDEM-IN-TIME 416
9.1.2 PICTOGRAMS FOR MS/MS EXPERIMENTS 418
9.2 METASTABLE ION DISSOCIATION 420
9.3 COLLISION-INDUCED DISSOCIATION 420
9.3.1 EFFECTING COLLISIONS IN A MASS SPECTROMETER 420
9.3.2 ENERGY TRANSFER DURING COLLISIONS 421
9.3.4 SINGLE AND MULTIPLE COLLISIONS IN CID 424
9.3.5 TIME SCALE OF ION ACTIVATING PROCESSES 426
9.4 SURFACE-INDUCED DISSOCIATION 426
9.5 TANDEM MS ON TOF INSTRUMENTS 427
9.5.1 UTILIZING A RETOF FOR TANDEM MS 427
9.5.2 CURVED-FIELD REFLECTRON 429
9.5.3 TANDEM MS ON TRUE TANDEM TOF INSTRUMENTS 429
9.6 TANDEM MS WITH MAGNETIC SECTOR INSTRUMENTS 431
9.6.1 DISSOCIATIONS IN THE FFR PRECEDING THE MAGNETIC SECTOR 431 9.6.2
MASS-ANALYZED ION KINETIC ENERGY SPECTRA 432
9.6.3 DETERMINATION OF KINETIC ENERGY RELEASE 432
9.6.4 B/E = CONST. LINKED SCAN 434
9.6.5 ADDITIONAL LINKED SCAN FUNCTIONS 434
9.6.6 MULTI-SECTOR INSTRUMENTS 436
9.7 TANDEM MS WITH LINEAR QUADRUPOLE ANALYZERS 437
9.7.1 TRIPLE QUADRUPOLE MASS SPECTROMETERS 437
9.7.2 SCAN MODES FOR TANDEM MS WITH TRIPLE QUADRUPOLE INSTRUMENTS..438
9.7.3 PENTA QUADRUPOLE INSTRUMENTS 438
9.8 TANDEM MS WITH THE QUADRUPOLE ION TRAP 439
9.9 TANDEM MS WITH LINEAR QUADRUPOLE ION TRAPS 443
9.9.1 TANDEM MS ON QQLIT INSTRUMENTS 444
9.9.2 TANDEM MS ON LITS WITH RADIAL EJECTION 444
9.10 TANDEM MS WITH ORBITRAP INSTRUMENTS 445
9.10.1 HIGHER-ENERGY C-TRAP DISSOCIATION 446
9.10.2 EXTENDED LIT-ORBITRAP HYBRID INSTRUMENTS 446
9.11 TANDEM MS WITH FT-ICR INSTRUMENTS - PART I 448
9.11.1 SUSTAINED OFF-RESONANCE IRRADIATION-CID IN ICR CELLS 448 9.12
INFRARED MULTIPHOTON DISSOCIATION 451
9.12.1 IRMPD IN QITS AND LITS 452
9.13 ELECTRON CAPTURE DISSOCIATION 452
IMAGE 10
XX TABLE OF CONTENTS
9.13.1 PRINCIPLES OF ELECTRON CAPTURE DISSOCIATION 452
9.13.2 PEPTIDE ION CLEAVAGES UPON ECD 454
9.14 TANDEM MS WITH FT-ICR INSTRUMENTS - PART II 455
9.14.1 IRMPD FOR TANDEM FT-ICR-MS 455
9.14.2 INFRARED PHOTODISSOCIATION SPECTROSCOPY 456
9.14.3 BLACKBODY INFRARED RADIATIVE DISSOCIATION 457
9.14.4 ECD FOR TANDEM FT-ICR-MS 458
9.15 ELECTRON TRANSFER DISSOCIATION 459
9.16 ELECTRON DETACHMENT DISSOCIATION 461
9.17 SUMMARY OF ION ACTIVATION TECHNIQUES 462
9.18 SPECIAL APPLICATIONS OF TANDEM MS 463
9.18.1 ION-MOLECULE REACTIONS IN CATALYTIC STUDIES 464
9.18.2 GAS PHASE HYDROGEN-DEUTERIUM EXCHANGE 464
9.18.3 DETERMINATION OF GAS PHASE BASICITIES AND PROTON AFFINITIES 466
9.18.4 NEUTRALIZATION-REIONIZATION MASS SPECTROMETRY 467 REFERENCES 468
10 FAST ATOM BOMBARDMENT 479
LEARNING OBJECTIVES 479
10.1 ION SOURCES FOR FAB AND LSIMS 480
10.1.1 FAB ION SOURCES 480
10.1.2 LSIMS ION SOURCES 482
10.1.3 FAB PROBES 482
10.2 ION FORMATION IN FAB AND LSIMS 483
10.2.1 ION FORMATION FROM INORGANIC SAMPLES 483
10.2.2 ION FORMATION FROM ORGANIC SAMPLES 484
10.3 LIQUID MATRICES FOR FAB AND LSIMS 486
10.3.1 THE ROLE OF THE LIQUID MATRIX 486
10.3.2 FAB MATRIX SPECTRA - GENERAL CHARACTERISTICS 487
10.3.3 UNWANTED REACTIONS IN FAB-MS 487
10.4 APPLICATIONS OF FAB-MS 488
10.4.1 FAB-MS OF ANALYTES OF LOW TO MEDIUM POLARITY 488 10.4.2 FAB-MS OF
IONIC ANALYTES 490
10.4.3 HIGH-MASS ANALYTES IN FAB-MS 491
10.4.4 ACCURATE MASS MEASUREMENTS IN FAB MODE 492
10.4.5 CONTINUOUS-FLOW FAB 494
10.4.6 LOW-TEMPERATURE FAB 495
10.4.7 FAB-MS AND PEPTIDE SEQUENCING 496
10.5 FAB AND LSIMS - GENERAL CHARACTERISTICS 496
10.5.1 SENSITIVITY OF FAB-MS 496
10.5.2 TYPES OF IONS IN FAB-MS 497
10.5.3 ANALYTES FOR FAB-MS 497
10.5.4 MASS ANALYZERS FOR FAB-MS 497
10.6 MASSIVE CLUSTER IMPACT 498
10.7 252 CALIFORNIUM PLASMA DESORPTION 498
REFERENCES 499
IMAGE 11
TABLE OF CONTENTS XXI
11 MATRIX-ASSISTED LASER DESORPTION/IONIZATION 507
LEARNING OBJECTIVES 507
11.1 ION SOURCES FOR LDI AND MALDI 508
11.2 ION FORMATION 509
11.2.1 ION YIELD AND LASER FLUENCE 510
11.2.2 EFFECT OF LASER IRRADIATION ON THE SURFACE 511
11.2.3 TEMPORAL EVOLUTION OF A LASER DESORPTION PLUME 512 11.2.4
PROCESSES OF ION FORMATION IN MALDI 513
11.2.5 LUCKY SURVIVOR MODEL OF ION FORMATION 514
11.3 MALDI MATRICES 516
11.3.1 ROLE OF THE SOLID MATRIX 516
11.3.2 MATRICES IN UV-MALDI 516
11.3.3 CHARACTERISTICS OF MALDI MATRIX SPECTRA 519
11.4 SAMPLE PREPARATION 519
11.4.1 MALDI TARGET 519
11.4.2 STANDARD SAMPLE PREPARATION 520
11.4.3 CATIONIZATION 522
11.4.4 CATION REMOVAL 524
11.4.5 SOLVENT-FREE SAMPLE PREPARATION 526
11.4.6 ADDITIONAL METHODS OF SAMPLE SUPPLY 527
11.5 APPLICATIONS OF LDI 527
11.6 APPLICATIONS OF MALDI 529
11.6.1 PROTEIN ANALYSIS BY MALDI-MS 529
11.6.2 PEPTIDE SEQUENCING AND PROTEOMICS 531
11.6.3 CARBOHYDRATE ANALYSIS BY MALDI-MS 536
11.6.4 OLIGONUCLEOTIDE ANALYSIS BY MALDI-MS 538
11.6.5 MALDI-MS OF SYNTHETIC POLYMERS 539
11.7 SPECIAL SURFACES TO MIMIC THE MATRIX 541
11.7.1 DESORPTION/IONIZATION ON SILICON 541
11.7.2 NANO-ASSISTED LASER DESORPTION/IONIZATION 542
11.7.3 FURTHER VARIATIONS OF THE MALDI THEME 543
11.8 MALDI IMAGING 544
11.9 ATMOSPHERIC PRESSURE MALDI 546
11.10 GENERAL CHARACTERISTICS OF MALDI 547
11.10.1 SAMPLE CONSUMPTION AND DETECTION LIMIT 547
11.10.2 ANALYTES FOR MALDI 547
11.10.3 TYPES OF IONS IN LDI AND MALDI-MS 548
11.10.4 MASS ANALYZERS FOR MALDI-MS 548
REFERENCES 549
12 ELECTROSPRAY IONIZATION 561
LEARNING OBJECTIVES 561
12.1 DEVELOPMENT OF ESI AND RELATED METHODS 562
12.1.1 ATMOSPHERIC PRESSURE IONIZATION 563
12.1.2 THERMOSPRAY 564
12.1.3 ELECTROHYDRODYNAMIC IONIZATION 565
IMAGE 12
XXII TABLE OF CONTENTS
12.1.4 ELECTROSPRAY IONIZATION 565
12.2 ION SOURCES FOR ESI 566
12.2.1 BASIC DESIGN CONSIDERATIONS 566
12.2.2 ADAPTATION TO DIFFERENT FLOW RATES 568
12.2.3 IMPROVED ELECTROSPRAY CONFIGURATIONS 569
12.2.4 ADVANCED ELECTROSPRAY INTERFACE DESIGNS 571
12.2.5 NOZZLE-SKIMMER DISSOCIATION 573
12.3 NANOELECTROSPRAY 574
12.3.1 PRACTICAL CONSIDERATIONS FORNANOESI 575
12.3.2 SPRAY MODES OF NANOESI 576
12.3.3 NANOELECTROSPRAY FROM A CHIP 577
12.4 ION FORMATION IN ESI 578
12.4.1 FORMATION OF THE ELECTROSPRAY PLUME 578
12.4.2 DISINTEGRATION OF CHARGED DROPLETS 581
12.4.3 FORMATION OF IONS FROM CHARGED DROPLETS 582
12.5 MULTIPLY CHARGED IONS AND CHARGE DECONVOLUTION 585
12.5.1 DEALING WITH MULTIPLY CHARGED IONS 585
12.5.2 MATHEMATICAL CHARGE DECONVOLUTION 587
12.5.3 COMPUTERIZED CHARGE DECONVOLUTION 588
12.5.4 HARDWARE CHARGE DECONVOLUTION 590
12.5.5 CONTROLLED CHARGE REDUCTION IN ESI 592
12.6 APPLICATIONS OF ESI-MS 593
12.6.1 ESI-MS OF SMALL MOLECULES 593
12.6.2 ESI OF METAL COMPLEXES 594
12.6.3 ESI OF SURFACTANTS 596
12.6.4 OLIGONUCLEOTIDES, DNA, AND RNA 596
12.6.5 ESI-MS OF OLIGOSACCHARIDES 599
12.6.6 HIGH-MASS PROTEINS AND PROTEIN COMPLEXES 600
12.7 SUMMARY OF ESI CHARACTERISTICS 601
12.7.1 SAMPLE CONSUMPTION 603
12.7.2 TYPES OF IONS IN ESI 603
12.7.3 MASS ANALYZERS FOR ESI 603
12.8 ATMOSPHERIC PRESSURE CHEMICAL IONIZATION 604
12.8.1 ION SOURCES FOR APCI 604
12.8.2 ION FORMATION IN APCI 605
12.8.3 APCI SPECTRA 605
12.9 ATMOSPHERIC PRESSURE PHOTOIONIZATION 608
12.9.1 ION FORMATION IN APPI 608
12.9.2 APPI SPECTRA 610
REFERENCES 612
13 AMBIENT MASS SPECTROMETRY 621
LEARNING OBJECTIVES 621
13.1 DESORPTION ELECTROSPRAY IONIZATION 622
13.1.1 EXPERIMENTAL SETUP FOR DESI 622
13.1.2 MECHANISMS OF ION FORMATION IN DESI 626
IMAGE 13
TABLE OF CONTENTS XXIII
13.1.3 ANALYTICAL FEATURES OF DESI 627
13.2 DESORPTION ATMOSPHERIC PRESSURE CHEMICAL IONIZATION 631 13.3
DESORPTION ATMOSPHERIC PRESSURE PHOTOIONIZATION 632 13.4 OTHER METHODS
RELATED TO DESI 634
13.4.1 DESORPTION SONIC SPRAY IONIZATION 635
13.4.2 EXTRACTIVE ELECTROSPRAY IONIZATION 635
13.4.3 ELECTROSPRAY-ASSISTED LASER DESORPTION/IONIZATION (ELDI) 637
13.4.4 LASER ABLATION ELECTROSPRAY IONIZATION 638
13.4.5 ATMOSPHERIC PRESSURE SOLIDS ANALYSIS PROBE 640
13.5 DIRECT ANALYSIS IN REAL TIME 640
13.5.1 EXPERIMENTAL SETUP FOR DART 640
13.5.2 ION FORMATION IN DART 642
13.5.3 ANALYTICAL APPLICATIONS OF DART 642
13.6 OVERVIEW OF AMBIENT MASS SPECTROMETRY 644
REFERENCES 645
14 HYPHENATED METHODS 651
LEARNING OBJECTIVES 651
14.1 CONCEPT OF CHROMATOGRAPHY-MASS SPECTROMETRY 652
14.1.1 ION CHROMATOGRAMS 653
14.1.2 REPETITIVE ACQUISITION OF MASS SPECTRA DURING ELUTION 654 14.1.3
SELECTED ION MONITORING 656
14.1.4 SELECTED REACTION MONITORING 658
14.2 QUANTITATION 659
14.2.1 QUANTITATION BY EXTERNAL STANDARDIZATION 659
14.2.2 QUANTITATION BY INTERNAL STANDARDIZATION 660
14.2.3 QUANTITATION BY ISOTOPE DILUTION 661
14.2.4 RETENTION TIMES OF ISOTOPOLOGS 663
14.3 GAS CHROMATOGRAPHY-MASS SPECTROMETRY 663
14.3.1 GC-MS INTERFACES 663
14.3.2 VOLATILITY AND DERIVATIZATION 664
14.3.3 COLUMN BLEED 665
14.3.4 FAST GC-MS 667
14.3.5 MULTIPLEXING FOR INCREASED THROUGHPUT 667
14.4 LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY 668
14.4.1 MULTIPLEXED LC-ESI-MS 671
14.5 ION MOBILITY SPECTROMETRY-MASS SPECTROMETRY 673
14.6 TANDEM MS AS A COMPLEMENT TO LC-MS 675
14.7 ULTRAHIGH-RESOLUTION MASS SPECTROMETRY 678
REFERENCES 680
15 INORGANIC MASS SPECTROMETRY 685
LEARNING OBJECTIVES 685
15.1 THERMAL IONIZATION MASS SPECTROMETRY 689
15.2 SPARK SOURCE MASS SPECTROMETRY 691
15.3 GLOW DISCHARGE MASS SPECTROMETRY 694
IMAGE 14
XXIV TABLE OF CONTENTS
15.4 INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY 697
15.4.1 LASER ABLATION ICP-MS 700
15.5 SECONDARY ION MASS SPECTROMETRY 701
15.5.1 ATOMIC SIMS 702
15.5.2 INSTRUMENTATION FOR ATOMIC SIMS 702
15.5.3 MOLECULAR SIMS 704
15.5.4 POLYATOMIC PRIMARY ION BEAMS 705
15.6 ACCELERATOR MASS SPECTROMETRY 707
15.7 CONCLUSION 710
REFERENCES 711
APPENDIX 717
A.I UNITS, PHYSICAL QUANTITIES, AND PHYSICAL CONSTANTS 717
A.2 ISOTOPIC COMPOSITION OF THE ELEMENTS 718
A.3 CARBON ISOTOPIC PATTERNS 725
A.4 CHLORINE AND BROMINE ISOTOPIC PATTERNS 726
A.5 SILICON AND SULFUR ISOTOPIC PATTERNS 727
A.6 ISOTOPOLOGS AND ACCURATE MASS 727
A.7 CHARACTERISTIC IONS 728
A.8 COMMON IMPURITIES 729
A.9 AMINO ACIDS 730
A.10 METHOD SELECTION GUIDE 731
A.I 1 HOW TO RECOGNIZE CATIONIZATION 732
A.12 SYSTEMATIC APPROACH TO MASS SPECTRA 733
A.13 RULES FOR THE INTERPRETATION OF MASS SPECTRA 733
A.14 NOBEL PRIZES FOR MASS SPECTROMETRY 734
SUBJECT INDEX 735
|
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| discipline | Chemie / Pharmazie Physik |
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| spellingShingle | Gross, Jürgen H. 1963- Mass spectrometry a textbook Massenspektrometrie (DE-588)4037882-2 gnd |
| subject_GND | (DE-588)4037882-2 (DE-588)4123623-3 |
| title | Mass spectrometry a textbook |
| title_auth | Mass spectrometry a textbook |
| title_exact_search | Mass spectrometry a textbook |
| title_full | Mass spectrometry a textbook Jürgen H. Gross |
| title_fullStr | Mass spectrometry a textbook Jürgen H. Gross |
| title_full_unstemmed | Mass spectrometry a textbook Jürgen H. Gross |
| title_short | Mass spectrometry |
| title_sort | mass spectrometry a textbook |
| title_sub | a textbook |
| topic | Massenspektrometrie (DE-588)4037882-2 gnd |
| topic_facet | Massenspektrometrie Lehrbuch |
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0202 PHY 115f 2004 A 71(2)
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| Exemplar 2 | Ausleihbar Am Standort |
Teilbibliothek Chemie
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