Instrumental analysis

Cover......Page 1
Half-title......Page 3
Title......Page 5
Copyright......Page 6
Brief Contents......Page 7
Contents......Page 9
Preface......Page 29
 Chapter 1. The Analyst’s Toolbox......Page 35
  Profile—A Scenario......Page 36
  1.1 Introduction......Page 37
  1.2 Ultraviolet-Visible Spectroscopy......Page 38
  1.3 Infrared Spectroscopy......Page 40
  Compare and Contrast—Ultraviolet-Visible versus Fourier Transform Infrared in Quantitative Analysis......Page 42
  1.4 Nuclear Magnetic Resonance Spectrometry......Page 43
  1.5 Mass Spectrometry......Page 45
  Profile—Putting It All Together......Page 47
  1.6 Chromatography......Page 48
  Profile—Establishing a Forensic Protocol......Page 50
  Further Reading......Page 52
  Exercises......Page 53
 Chapter 2. Quantum Mechanics and Spectroscopy......Page 55
  2.1 Introduction......Page 56
  2.2 The Interaction Between Electromagnetic Radiation and Matter—Absorption and Emission of Light......Page 58
  Profile—Erwin Schrödinger......Page 59
  2.3 Molecular Vibrations Lead to Quantized Energy Levels......Page 63
  Profile—Mass Dampers......Page 66
  2.4 Molecular Rotation Leads to Quantized Energy Levels......Page 69
  2.5 Transitions Between Vibrational and Rotational States: The Role of Thermal Energy and Nonradiative Decay......Page 71
  2.6 Transitions Between Electronic, Vibrational, and Rotational States: Putting It All Together......Page 74
   Fluorescence and Phosphorescence......Page 75
  2.7 Energy Levels of Protons in a Magnetic Field—Nuclear Magnetic Resonance Spectroscopy......Page 76
  Exercises......Page 80
 Chapter 3. An Introduction to Optics......Page 83
  Profile—The Diffraction Grating: A Key Component of Many Optical Instruments......Page 84
   Wavelength, Energy, and Frequency......Page 85
  Profile—The Photoelectric Effect Shows the Particle Nature of Light......Page 86
   Coherence......Page 88
   Polarization......Page 89
   Interference......Page 90
   Diffraction......Page 93
   Scattering......Page 94
   Mirrors and Ref lection......Page 96
   Lenses and Refraction......Page 97
   Collecting and Collimating Light......Page 100
   Focusing a Collimated Laser Beam......Page 101
   Polarizers......Page 103
   Introduction to Prism and Grating Monochromators......Page 104
   The Diffraction Grating......Page 105
  Profile—Optics that Operate by Diffraction: The Fresnel Zone Plate......Page 110
   The Michelson Interferometer......Page 115
   Optical Filters and Power Reduction......Page 116
  3.5 Beyond Linear Optics......Page 118
  Profile—Innovation and Discovery in Optics: Metamaterials Hold Promise for the Perfect Lens, Invisibility Cloaks, and More......Page 119
  Exercises......Page 120
 Chapter 4 An Introduction to Instrumental Electronics......Page 123
  4.1 Introduction......Page 124
   Circuit Symbols......Page 126
   Current, Voltage, and Multimeter Basics......Page 127
   Series Circuit Elements and the Voltage Divider......Page 128
   Parallel Circuit Elements and the Current Divider......Page 130
   The Multimeter......Page 134
   Voltage and Current Loading Error......Page 135
  Profile—Electronics for a Very Simple Light-Sensing Instrument: Voltage Divider Photoresistor Circuit......Page 136
  4.3 Capacitors and Resistor–Capacitor (RC) Circuits......Page 138
  4.4 Alternating Current (AC) Circuits......Page 142
   Ohm’s Law for Alternating Current (AC) Circuits......Page 144
   Low-Pass, High-Pass, Band-Pass, and Band-Stop Filters......Page 145
  4.5 Operational Amplifiers......Page 148
   Inverting and Noninverting Operational Amplifiers......Page 149
   Current-to-Voltage Amplifier......Page 150
   The Voltage Follower......Page 151
   Operational Amplifier Comparator......Page 152
   Cascading Operational Amplifiers......Page 153
  Profile—Electronics for an Automatic Titrator: Cascaded Operational Amplifiers and the Differentiating Operational Amplifier......Page 156
   Diodes......Page 157
   Integrated Circuits......Page 158
  Profile—Electronics for a Simple Absorption Spectrophotometer: Operational Amplifier as Current-to-Voltage Amplifier......Page 159
  4.7 Analog and Digital Signals......Page 160
  Exercises......Page 162
 Chapter 5. Signals and Noise: An Introduction to Signal Processing......Page 165
  5.1 Introduction to Signals......Page 166
  5.2 Sources and Characteristics of Noise......Page 168
   Thermal Noise......Page 169
   Shot Noise......Page 170
   Flicker Noise......Page 171
  5.3 The Signal-to-Noise Ratio and Ensemble Averaging......Page 173
   Analog Processing......Page 176
   Boxcar Averaging with Hardware......Page 177
   Modulation and the Lock-In Amplifier......Page 179
   Digital Signal Processing......Page 181
   Savitzky-Golay Smoothing......Page 185
   Fourier Filtering......Page 187
  5.5 Sampling Rates, the Nyquist Frequency, and Aliasing......Page 189
  5.6 Analog-to-Digital Conversion......Page 191
  Exercises......Page 192
   Advanced Exercises......Page 193
 Chapter 6. Molecular Ultraviolet and Visible Spectroscopy......Page 195
  Profile—James Clerk Maxwell......Page 196
  6.1 Introduction......Page 197
  6.2 Electronic Excitation and Molecular Structure......Page 199
   Structure and “Color”......Page 201
   Vibronic Transitions......Page 203
  DPK: A Case Study......Page 204
   Transition Metal Coordination Compounds......Page 205
   Selection Rules......Page 207
   Beer’s Law......Page 210
   Deviations from Beer’s Law......Page 212
   Fixed-Wavelength Spectrometers......Page 215
  Profile—HACH DR3900......Page 216
   Scanning Spectrometers......Page 218
  Compare and Contrast—Single- and Dual-Beam Spectrometers......Page 220
   Array Spectrophotometers......Page 221
  6.5 Monochromators: Prisms, Gratings, and the Location of Wavelength Dispersion Components......Page 222
  Profile—Building a Monochromator......Page 223
   Deuterium Arc/Tungsten Halogen Bulb......Page 224
   Xenon Arc Lamps......Page 225
   The Photomultiplier Tube......Page 226
  Profile—The Jaz by Ocean Optics......Page 227
   Photovoltaic Cells......Page 228
   Charge Coupled Devices......Page 229
  Activity—Absorbance and Stray Light......Page 230
  Profile—Walter Hermann Schottky......Page 231
  6.9 Kinetic Ultraviolet-Visible Techniques......Page 232
   Stop Flow Ultraviolet-Visible Studies......Page 233
   Flash Photolysis......Page 235
  6.10 Useful Data......Page 237
  Exercises......Page 238
   Advanced Exercises......Page 239
 Chapter 7. Atomic Absorption Spectroscopy......Page 241
  Profile—The Birth of Atomic Absorption Spectroscopy......Page 242
  7.1 Introduction......Page 243
  7.2 Molecular versus Atomic Absorption......Page 245
   Lifetime Broadening......Page 246
   Magnetic Field Broadening......Page 248
   Pressure Broadening......Page 250
   Doppler Broadening......Page 251
   The Hollow-Cathode Lamp......Page 252
  Profile—Nutritional Contents of Breast Milk......Page 253
   Electrodeless Discharge Lamps......Page 254
  Activity—Soil Analysis......Page 255
   Flame Atomic Absorption Spectroscopy......Page 256
   Electrothermal Atomic Absorption Spectroscopy/ Graphite Furnace Atomic Absorption Spectroscopy......Page 260
   Flame versus Electrothermal Atomic Absorption Spectroscopy......Page 261
   Hydride Atomic Absorption Spectroscopy......Page 262
   Cold Vapor Atomic Absorption Spectroscopy......Page 263
  7.6 Measuring Atomic Absorption......Page 264
  Profile—Demystifying the Zeeman Effect......Page 265
   Smith-Hieftje Background Correction......Page 267
   Chemical Interferences......Page 268
   Acid Digestion......Page 271
  7.8 Performing an Atomic Absorption Spectroscopy Analysis......Page 272
  Further Reading......Page 274
  Exercises......Page 275
 Chapter 8. Luminescence Spectroscopy......Page 277
  8.1 Introduction......Page 278
  8.2 Theory......Page 279
   Fluorescence Quantum Yield and Time Decay of Fluorescence......Page 283
   Factors that Determine Fluorescence Intensity......Page 285
  Profile—Is Your $100 Bill Real? Find Out with Time-Resolved Fluorescence......Page 286
   Stern-Volmer Quenching......Page 287
   Relating Fluorescence and Molecular Structure......Page 290
  Profile—Fluorescence Quenching Helps with Aerodynamics......Page 291
   Steady-State Luminescence and Time-Resolved Luminescence Measurements......Page 293
   Excitation Source......Page 294
   Wavelength Discrimination and Instrument Resolution......Page 295
   Detectors for Luminescence......Page 297
   Excitation Spectra: An Additional Measurement Mode......Page 298
   Sample Introduction......Page 300
   Source Intensity Corrections......Page 301
   Photobleaching......Page 302
  Profile—Fluorescence Pushes the Limits of Detection: Femtomolar and Single Molecule Detection......Page 303
   Chemiluminescence......Page 304
   Resonance Energy Transfer Spectroscopy......Page 305
   Multiphoton Excitation......Page 307
  Further Reading......Page 308
  Exercises......Page 309
 Chapter 9. Atomic Emission Spectroscopy......Page 311
  9.1 Introduction......Page 312
  9.2 The Atomizer and the Excitation Source......Page 314
  Profile—Columbia......Page 315
   Inductively Coupled Plasma Torch......Page 317
   Direct Current Plasma Source......Page 318
  Profile—The Plasma Torch......Page 319
   Microwave-Induced Plasma Source......Page 320
   Laser-Induced Plasma......Page 321
  Profile—Laser-Induced Breakdown Spectroscopy in Space......Page 322
  9.3 Sample Introduction......Page 323
   Sample Preparation and Interferences......Page 324
   Zeeman Background Correction......Page 325
  9.4 Measuring Atomic Emission......Page 326
  Compare and Contrast—Flame Atomic Absorption Spectroscopy, Graphite Furnace Atomic Absorption Spectroscopy, and Inductively Coupled Plasma–Atomic Emission Spectroscopy......Page 327
  Further Reading......Page 328
   Advanced Exercises......Page 329
 Chapter 10. X-ray–Related Techniques......Page 331
  10.1 Principles of X-ray Fluorescence Spectroscopy......Page 332
  Profile—W. C. Röntgen......Page 333
   X-ray Fluorescence Transitions: Terminology......Page 334
   Photoelectric Absorption......Page 335
   Absorption of X-rays......Page 336
  Compare and Contrast—Optical Absorption versus Photoelectric Absorption......Page 337
   Radioisotopes......Page 339
   X-ray Tubes......Page 340
   Synchrotron Radiation......Page 343
  10.3 X-ray Optics......Page 344
   Reflection Optics......Page 345
  Profile—X-ray Fluorescence Analysis of a Fifteenth-Century Painting......Page 346
   Diffraction Optics......Page 347
   Sequential and Simultaneous......Page 350
  Profile—Lost Painting by Vincent van Gogh......Page 351
   Wavelength-Dispersive X-ray Fluorescence Detectors......Page 353
  10.5 Energy-Dispersive Spectrometers......Page 354
   Energy-Dispersive X-ray Fluorescence Detectors......Page 355
  10.6 Direct Comparison: Wavelength-Dispersive and Energy-Dispersive X-ray Fluorescence Spectroscopy......Page 358
  10.8 Total Reflection X-ray Fluorescence......Page 360
   X-ray–Induced Photoelectron Spectroscopy......Page 361
  Compare and Contrast—XRF, XPS, & AS......Page 362
   Auger Electron Spectroscopy......Page 363
  10.10 Single Crystal X-ray Diffractometry......Page 364
   Scatter......Page 366
  Profile—Christiaan Huygens......Page 367
   Bragg’s Law......Page 368
   The Lattice......Page 370
   Obtaining a Crystal Structure......Page 374
   The Diffractometer......Page 376
  Further Reading......Page 377
  Exercises......Page 378
   Advanced Exercises......Page 379
 Chapter 11. Infrared Spectroscopy......Page 381
  Profile—Forensics and Fourier Transform Infrared Spectroscopy......Page 382
  11.1 Chemical Structure and Molecular Vibrations......Page 383
   Wave Numbers and the Infrared Spectral Region......Page 384
   Group Frequencies......Page 385
   Normal Modes......Page 387
   Vibrational Categories......Page 388
  Profile—Olive Oil......Page 389
   The Selection Rule and Molecular Symmetry......Page 390
  Activity—Just for Fun......Page 391
  11.2 Time Domain versus Frequency Domain Spectroscopy: The Fourier Transformation......Page 393
  Activity—Performing a Fourier Transform......Page 395
   The Michelson Interferometer......Page 397
   Resolution......Page 399
  Activity—Exploring Resolution......Page 400
  11.4 Sources......Page 401
   The Globar......Page 403
   Solid-State Sources......Page 404
   Pyroelectric Detectors......Page 405
   Quantum Well Detectors......Page 407
   Quantitative Measurements and Deviations from Beer’s Law......Page 408
  11.7 Developments: Two-Dimensional Infrared Spectroscopy......Page 410
   Optical Materials......Page 411
   Gases......Page 412
   Solution Infrared Spectroscopy......Page 413
   Solids......Page 415
   Attenuated Total Ref lection......Page 416
  Further Reading......Page 418
   Advanced Exercises......Page 419
 Chapter 12. Raman Spectroscopy......Page 421
  Profile—Raman Applications in Art and Medicine......Page 422
  12.1 Introduction......Page 423
   Rayleigh Scattering......Page 424
  12.2 Theory of Raman Scattering......Page 425
   Selection Rules......Page 429
  Vibrations in the Linear Molecule Carbon Dioxide (CO2): A Case Study......Page 432
  Raman Spectroscopy of the Tetrahedral Molecule Carbon Tetrachloride (CCl4): A Case Study......Page 435
   Radiant Source......Page 438
   Filters......Page 441
   Detectors......Page 442
  Compare and Contrast—A Side-by-Side Evaluation of Fourier Transform Infrared and Raman Spectroscopy......Page 444
   Fiber Optic Probes......Page 445
  Profile—Drug Detection Using Handheld Raman Instrument......Page 446
   Raman Imaging......Page 447
   Polarized Raman Spectroscopy......Page 449
   Fourier Transform–Raman Spectroscopy......Page 451
  Profile—Using Raman Spectroscopy to Identify Compounds from a Distance......Page 452
  Further Reading......Page 453
   Advanced Exercises......Page 454
 Chapter 13. Mass Spectrometry......Page 457
  Profile—Puffer MS......Page 458
  13.2 Ion Sources......Page 460
   Electron Ionization......Page 462
  Profile—J. J. Thomson......Page 463
   Chemical Ionization......Page 467
   Electrospray Ionization......Page 470
   Matrix-Assisted Laser Desorption Ionization......Page 472
   Secondary Ion Ionization......Page 473
   Inductively Coupled Plasma Ionization......Page 475
  13.3 Mass Analyzers......Page 478
   Resolution......Page 479
   Sector and Double-Focusing Mass Analyzer......Page 480
  Profile—Eugen Goldstein......Page 482
   Quadrupole Mass Analyzer......Page 484
   Time-of-Flight Mass Analyzer......Page 485
   Fourier Transform Ion Cyclotron Resonance......Page 488
   Quadrupole Ion Trap Mass Analyzer......Page 490
  13.4 Detectors......Page 491
   Tandem Techniques......Page 493
   Accelerator Mass Spectrometry......Page 494
  Profile—The Isotope 10Be as a Geological Clock......Page 495
  Profile—Human Scent Fingerprinting......Page 496
  Exercises......Page 497
   Advanced Exercises......Page 498
 Chapter 14. An Introduction to Nuclear Magnetic Resonance Spectroscopy......Page 501
  14.1 Introduction......Page 502
  Profile—Spectral Analysis: A Quick Review......Page 504
   Nuclear Quantum Numbers......Page 505
   A Nucleus in a Magnetic Field......Page 506
  14.3 The Nuclear Magnetic Resonance Signal......Page 509
  Compare and Contrast—Population Distribution for Common Spectroscopic Methods......Page 513
  14.4 The Radiofrequency Pulse: Inducing Nuclear Magnetic Resonance......Page 514
   Fourier Transform–Nuclear Magnetic Resonance: Time Domain versus Frequency Domain Spectroscopy and the Fourier Transformation......Page 516
   Free Induction Decay: The Fourier Transform– Nuclear Magnetic Resonance “Beat Pattern”......Page 517
  14.5 Chemical Shift and Resolution......Page 518
   The Chemical Shift (ppm)......Page 519
   Resolution......Page 521
  14.6 The Instrument......Page 522
   Loading......Page 523
  14.7 Signal Processing......Page 524
   Increasing the Signal-to-Noise Ratio......Page 525
  Profile—Angela Gronenborn......Page 526
  14.8 Magnetic Resonance Imaging......Page 527
  Profile—Magnetic Resonance Imaging and Brain Concussion......Page 528
  Profile—Magnetic Resonance Imaging Has a Fascinating Backstory......Page 529
  Further Reading......Page 532
  Exercises......Page 533
 Chapter 15. Liquid Chromatography......Page 535
  15.1 Introduction......Page 536
   Distribution Equilibrium......Page 537
   Principles of Chromatography......Page 540
  Activity—Chromatography at Home......Page 542
   The Retention Factor......Page 543
   Resolution and Theoretical Plates......Page 545
   Band Broadening......Page 550
   Thermodynamic and Kinetic Factors......Page 553
   Isocratic versus Gradient Elution......Page 555
   Quantitative versus Qualitative Analysis......Page 556
  Profile—Analysis of Wine: Qualitative and Quantitative......Page 559
  Profile—Liquid Chromatography–Mass Spectroscopy in Athletic Doping......Page 560
   Reversed Phase Chromatography......Page 563
   Hydrophilic Interaction Chromatography......Page 565
   Chiral Chromatography......Page 566
   Size Exclusion Chromatography......Page 567
   Overview......Page 569
   High-Performance Liquid Chromatography Components......Page 570
   Mobile Phase......Page 571
   Columns......Page 572
   Injectors......Page 573
   Pumps......Page 574
   Detectors......Page 575
  Profile—Major Players in the Analytical Industry......Page 577
  Further Reading......Page 578
  Exercises......Page 579
 Chapter 16. Gas Chromatography......Page 583
  16.1 Introduction......Page 584
  Profile—Gas Chromatography on Mars......Page 587
  16.2 Basic Gas Chromatography Instrument Design......Page 589
   Peanut Butter: A Case Study......Page 590
   The Column......Page 593
  Profile—The NIST 14 Gas Chromatography Library with Search Software......Page 594
  Profile—Erika Cremer......Page 596
   Carrier Gases......Page 601
  16.6 Detectors......Page 603
   Ionizing Detectors......Page 604
   Optical Detectors......Page 605
   Atomic Emission Detectors......Page 606
   Thermal Conductivity Detectors......Page 607
   Tandem Instrument Detection......Page 608
   Quantitative and Qualitative Considerations......Page 610
   Multidimensional Gas Chromatography Techniques......Page 611
   Miniaturization, Portability, Speed, and Throughput......Page 612
  Profile—Breath and Air Quality......Page 613
   Evaluation of the Gas Chromatography Separation......Page 615
   The General Elution Problem: Review of Resolution and Band Broadening......Page 619
  Exercises......Page 622
   Advanced Exercises......Page 623
 Chapter 17. Electrophoresis......Page 625
  Profile—The Father of Electrophoresis......Page 626
  17.2 Fundamental Principles......Page 627
  17.3 The Basic Apparatus......Page 633
  17.4 Paper Electrophoresis......Page 635
  Activity—Demystifying Electrophoresis: Build Your Own Electrophoresis Apparatus......Page 636
   Polyacrylamide Gel Electrophoresis......Page 637
   Sodium Dodecyl Sulfate Polyacrylamide Gel Electrophoresis......Page 640
  17.6 Ending the Analysis: The Time Factor......Page 641
   Visualization......Page 642
   Quantitative Electrophoresis......Page 644
   Discontinuous Electrophoresis......Page 646
   Isoelectric Focusing......Page 648
   Two-Dimensional Electrophoresis......Page 649
   The Instrument......Page 650
  Profile—Capillary Electrophoresis and the Human Genome Project......Page 651
   Separation Efficiency......Page 652
   Electro-osmotic Flow......Page 653
  Profile—Micellar Electrokinetic Capillary Chromatography......Page 656
   Sample Loading and Throughput......Page 657
   Dynamic Coating......Page 658
   Detection......Page 659
   Recent Developments in Capillary Electrophoresis......Page 661
  Compare and Contrast—A Look Back at Five Different Separation Techniques......Page 662
  Further Reading......Page 663
  Exercises......Page 664
 Chapter 18 Potentiometry and Probes......Page 667
  18.1 Basic Principles: Probes and Biosensors......Page 668
  18.2 Potentiometric Probes......Page 674
  Profile—The Standard Hydrogen Electrode......Page 675
   The pH Probe......Page 677
  Profile—Nanoscale pH Probe for In Vivo Use......Page 681
   The Nitrate Probe......Page 682
   The Oxygen Probe......Page 683
  18.3 Nonpotentiometric Probes......Page 684
   The Dissolved Oxygen Probe......Page 685
   The Chloride Probe......Page 686
   The Total Salinity Probe......Page 688
   The Glucose Probe: A Biosensor......Page 690
  Profile—Percentage of Adults Treated for Diabetes Nearly Doubled in a Decade......Page 692
   The Alcohol Fuel Cell Probe......Page 693
  Profile—“Smart” Toilets: Intelligent Toilets that Monitor Your Health......Page 694
  Exercises......Page 695
 Chapter 19 Analytical Voltammetry......Page 697
  19.1 Basic Principles......Page 698
  Profile—Parsing Method Names......Page 700
  19.2 The Three-Electrode Cell......Page 701
   The Experiment......Page 703
   Charging Current......Page 705
   Mass Transport......Page 706
  Profile—VX Probe......Page 707
   Controlling Mass Transport......Page 708
   The Cottrell Equation......Page 709
  Profile—The International Space Station......Page 710
   Background......Page 712
   The Experiment......Page 713
   Reversibility......Page 715
   Quantitative Analysis with Cyclic Voltammetry: The Randles-Sevcik Equation......Page 717
   Qualitative Analysis with Cyclic Voltammetry......Page 720
   Solvents, Electrolytes, and the Electrochemical Window......Page 725
  19.5 Square Wave Voltammetry......Page 726
   Ultramicroelectrodes and Nanoelectrodes......Page 730
   Compare and Contrast— Instrumental Costs......Page 733
  Profile—Cyclic Voltammetry in a Single Cell......Page 734
  19.7 Useful Data......Page 735
  Exercises......Page 737
 Chapter 20. Material and Surface Analysis Techniques......Page 739
  Profile—Characterizing Metal Nanoparticles for Water Purification: Electron Microscopy in Action......Page 740
  20.2 Microscopy......Page 741
  Profile—Microscopy and the Nobel Prize in Physics......Page 742
   Atomic Force Microscopy......Page 743
   Scanning Tunneling Microscopy......Page 745
  Profile—Controlling the Shape of Silver Nanoparticles with pH: Atomic Force Microscopy in Action......Page 746
   Transmission Electron Microscopy and Scanning Electron Microscopy......Page 748
  Compare and Contrast—Resolutions for Different Microscopy Techniques......Page 754
  Profile—Thermogravimetric Analysis......Page 755
   Thermogravimetric Analysis......Page 757
   Differential Scanning Calorimetry......Page 758
  Compare and Contrast—Differential Thermal Analysis, Thermogravimetric Analysis, and Differential Scanning Calorimetry......Page 760
  Profile—A Crime Scene Analysis......Page 761
  20.4 Mechanical Stress Analysis......Page 763
   Dynamic Mechanical Analysis......Page 764
  Exercises......Page 766
 Chapter 21. Understanding the Nuclear Magnetic Resonance Experiment......Page 769
  Profile—Adriaan “Ad” Bax......Page 770
   Relaxation of the Excited State......Page 774
   Longitudinal Relaxation (Spin-Lattice): T1......Page 777
   Measuring T1: Inversion Recovery......Page 778
   Transverse Relaxation (Spin-Spin): T2......Page 781
   Measuring T2: Spin-Echo......Page 782
  21.4 The Influence of Nuclear Neighbors......Page 784
   J-Coupling......Page 785
   Dipolar Coupling and the Nuclear Overhauser Effect......Page 789
  Profile—Albert W. Overhauser......Page 790
  Profile—Jean Jeener......Page 792
  21.5 Introduction to Two-Dimensional Nuclear Magnetic Resonance......Page 793
   Correlation Spectroscopy and Total Correlation Spectroscopy......Page 794
   Nuclear Overhauser Effect Spectroscopy......Page 797
  Profile—G. Marius Clore......Page 800
   Variable Temperature Nuclear Magnetic Resonance......Page 801
   Solid-State Nuclear Magnetic Resonance......Page 802
   Other Spin-Active Nuclei......Page 805
  21.7 Useful Data......Page 809
  Further Reading......Page 810
  Exercises......Page 811
 Chapter 22. Statistical Data Analysis......Page 813
   Gross Error......Page 814
  22.3 Precision versus Accuracy......Page 815
   Population versus Sample......Page 816
   Standard Deviation and Variance......Page 817
  Activity—Using Microsoft Excel to Generate a Mean and Standard Deviation......Page 818
   Standard Error and Error Bars......Page 819
   Normal Distributions......Page 820
  Activity—Random Number Generation and Plotting a Histogram in Microsoft Excel......Page 822
   Confidence Limits......Page 824
  Activity—Using Microsoft Excel to Calculate Confidence Limits......Page 826
   Propagation of Error......Page 827
   Identifying Outliers: Q-Test......Page 829
   Identifying Outliers: Grubbs’ Test......Page 831
   Analyzing Variance: F-Tests......Page 832
  22.5 Linear Regression Analysis......Page 835
  Activity—Letting Microsoft Excel Perform ANOVA......Page 836
  Activity—Letting Microsoft Excel Perform LINEST to Give Linear Regression Data......Page 839
  22.6 Limit of Detection, Limit of Quantitation, and Linear Dynamic Range......Page 841
  Activity—Using Microsoft Excel to Add a Trend Line to a Data Set......Page 842
  Exercises......Page 845
   Advanced Exercises......Page 846
Appendix: Table of Abbreviations and Acronyms......Page 847
Credits......Page 855
Index......Page 861