Principles of Instrumental Analysis 7th edition Skoog

Cover......Page 1
Contents Overview......Page 10
Contents......Page 12
Preface......Page 18
1A Classification of Analytical Methods......Page 24
1B Types of Instrumental Methods......Page 25
1C Instruments for Analysis......Page 26
1D Calibration of Instrumental Methods......Page 32
1E Selecting an Analytical Method......Page 39
Questions and Problems......Page 43
SECTION ONE Measurement Basics......Page 46
2A Direct-Current Circuits and Measurements......Page 47
2B Alternating Current Circuits......Page 53
2C Semiconductors and Semiconductor Devices......Page 62
2D Power Supplies and Regulators......Page 66
2E Readout Devices......Page 68
Questions and Problems......Page 70
3A Properties of Operational Amplifiers......Page 75
3B Operational Amplifier Circuits......Page 77
3C Amplification and Measurement of Transducer Signals......Page 81
3D Application of Operational Amplifiers to Voltage and Current Control......Page 85
3E Application of Operational Amplifiers to Mathematical Operations......Page 86
3F Applications of Operational Amplifiers to Comparison......Page 88
Questions and Problems......Page 89
CHAPTER FOUR Digital Electronics and Computers......Page 94
4B Counting and Arithmetic with Binary Numbers......Page 95
4C Basic Digital Circuits......Page 97
4D Computers and Computerized Instruments......Page 103
4E Components of a Computer......Page 105
4F Computer Software......Page 107
4G Applications of Computers......Page 114
4H Computer Networks......Page 115
Questions and Problems......Page 118
5A The Signal-to-Noise Ratio......Page 121
5B Sources of Noise in Instrumental Analyses......Page 122
5C Signal-to-Noise Enhancement......Page 124
Questions and Problems......Page 133
Instrumental Analysis in Action— The Electronic Analytical Laboratory......Page 136
SECTION TWO Atomic Spectroscopy......Page 142
6A General Properties of Electromagnetic Radiation......Page 143
6B Wave Properties of Electromagnetic Radiation......Page 144
6C Quantum-Mechanical Properties of Radiation......Page 153
6D Quantitative Aspects of Spectrochemical Measurements......Page 164
Questions and Problems......Page 166
7A General Designs of Optical Instruments......Page 171
7B Sources of Radiation......Page 173
7C Wavelength Selectors......Page 183
7E Radiation Transducers......Page 197
7F Signal Processors and Readouts......Page 207
7H Types of Optical Instruments......Page 208
7I Principles of Fourier Transform Optical Measurements......Page 209
Questions and Problems......Page 215
8A Optical Atomic Spectra......Page 219
8B Atomization Methods......Page 226
8C Sample-Introduction Methods......Page 227
Questions and Problems......Page 231
9A Sample Atomization Techniques......Page 233
9B Atomic Absorption Instrumentation......Page 239
9C Interferences in Atomic Absorption Spectroscopy......Page 243
9D Atomic Absorption Analytical Techniques......Page 248
9E Atomic Fluorescence Spectroscopy......Page 249
Questions and Problems......Page 251
CHAPTER TEN Atomic Emission Spectrometry......Page 254
10A Emission Spectroscopy Based on Plasma Sources......Page 255
10B Emission Spectroscopy Based on Arc and Spark Sources......Page 269
10C Other Sources for Optical Emission Spectroscopy......Page 270
Questions and Problems......Page 272
11A Some General Features of Atomic Mass Spectrometry......Page 276
11B Mass Spectrometers......Page 278
11C Inductively Coupled Plasma Mass Spectrometry......Page 286
11D Spark Source Mass Spectrometry......Page 293
11F Other Mass Spectrometric Methods......Page 294
Questions and Problems......Page 295
12A Fundamental Principles......Page 297
12B Instrument Components......Page 303
12C X-ray Fluorescence Methods......Page 310
12D X-ray Absorption Methods......Page 317
Questions and Problems......Page 320
Instrumental Analysis in Action— Monitoring Mercury......Page 324
SECTION THREE Molecular Spectroscopy......Page 326
13A Measurement of Transmittance and Absorbance......Page 327
13B Beer’s Law......Page 328
13C The Effects of Instrumental Noise on Spectrophotometric Analyses......Page 333
13D Instrumentation......Page 338
Questions and Problems......Page 350
14B Absorbing Species......Page 354
14C Qualitative Applications of Ultraviolet Visible Absorption Spectroscopy......Page 358
14D Quantitative Analysis by Absorption Measurements......Page 360
14E Photometric and Spectrophotometric Titrations......Page 365
14F Spectrophotometric Kinetic Methods......Page 367
14G Spectrophotometric Studies of Complex Ions......Page 370
Questions and Problems......Page 376
CHAPTER FIFTEEN Molecular Luminescence Spectrometry......Page 384
15A Theory of Fluorescence and Phosphorescence......Page 385
15B Fluorescence and Phosphorescene Instrumentation......Page 395
15C Applications of Photoluminescence Methods......Page 401
15D Chemiluminescence......Page 405
Questions and Problems......Page 407
CHAPTER SIXTEEN An Introduction to Infrared Spectrometry......Page 412
16A Theory of IR Absorption Spectrometry......Page 413
16B IR Instrumentation......Page 419
16C IR Sources and Transducers......Page 429
Questions and Problems......Page 432
17A Mid-IR Absorption Spectrometry......Page 435
17B Mid-IR Reflection Spectrometry......Page 448
17C Photoacoustic IR Spectroscopy......Page 451
17D Near-IR Spectroscopy......Page 452
17F IR Emission Spectroscopy......Page 454
17G IR Microscopy and Imaging......Page 455
Questions and Problems......Page 456
18A Theory of Raman Spectroscopy......Page 460
18B Instrumentation......Page 465
18C Applications of Raman Spectroscopy......Page 470
18D Other Types of Raman Spectroscopy......Page 472
Questions and Problems......Page 474
CHAPTER NINETEEN Nuclear Magnetic Resonance Spectroscopy......Page 476
19A Theory of NMR......Page 477
19B Environmental Effects on NMR Spectra......Page 488
19C NMR Spectrometers......Page 497
19D Applications of Proton NMR......Page 501
19E Carbon-13 NMR......Page 504
19F Application of NMR to Other Nuclei......Page 508
19G Multiple Pulse and Multidimensional NMR......Page 509
19H Magnetic Resonance Imaging......Page 511
Questions and Problems......Page 516
CHAPTER TWENTY Molecular Mass Spectrometry......Page 524
20B Ion Sources......Page 525
20C Mass Spectrometers......Page 537
20D Applications of Molecular Mass Spectrometry......Page 550
20E Quantitative Applications of Mass Spectrometry......Page 555
Questions and Problems......Page 556
21A Introduction to the Study of Surfaces......Page 560
21B Spectroscopic Surface Methods......Page 561
21C Electron Spectroscopy......Page 562
21D Ion Spectroscopic Techniques......Page 572
21E Surface Photon Spectroscopic Methods......Page 573
21F Electron-Stimulated Microanalysis Methods......Page 575
21G Scanning Probe Microscopes......Page 581
Questions and Problems......Page 589
Instrumental Analysis in Action—Assessing the Authenticity of the Vinland Map: Surface Analysis in the Service of History, Art, and Forensics......Page 591
SECTION FOUR Electroanalytical Chemistry......Page 594
22A Electrochemical Cells......Page 595
22B Potentials in Electroanalytical Cells......Page 600
22C Electrode Potentials......Page 602
22D Calculation of Cell Potentials from Electrode Potentials......Page 610
22E Currents in Electrochemical Cells......Page 612
22F Types of Electroanalytical Methods......Page 616
Questions and Problems......Page 617
23A General Principles......Page 624
23B Reference Electrodes......Page 625
23C Metallic Indicator Electrodes......Page 627
23D Membrane Indicator Electrodes......Page 629
23E Ion-Selective Field-Effect Transistors......Page 639
23F Molecular-Selective Electrode Systems......Page 640
23G Instruments for Measuring Cell Potentials......Page 646
23H Direct Potentiometric Measurements......Page 648
23I Potentiometric Titrations......Page 653
Questions and Problems......Page 654
24A Current-Voltage Relationships during an Electrolysis......Page 659
24B An Introduction to Coulometric Methods of Analysis......Page 663
24C Controlled-Potential Coulometry......Page 664
24D Coulometric Titrations......Page 667
Questions and Problems......Page 672
CHAPTER TWENTY-FIVE Voltammetry......Page 676
25A Excitation Signals in Voltammetry......Page 677
25B Voltammetric Instrumentation......Page 678
25C Hydrodynamic Voltammetry......Page 683
25D Cyclic Voltammetry......Page 695
25E Pulse Voltammetry......Page 699
25F High-Frequency and High-Speed Voltammetry......Page 701
25G Applications of Voltammetry......Page 703
25H Stripping Methods......Page 704
25I Voltammetry with Microelectrodes......Page 707
Questions and Problems......Page 709
Instrumental Analysis in Action— Measuring the Parts to Understand the Whole: The Microphysiometer......Page 713
SECTION FIVE Separation Methods......Page 718
26A General Description of Chromatography......Page 719
26B Migration Rates of Solutes......Page 722
26C Band Broadening and Column Efficiency......Page 725
26D Optimization of Column Performance......Page 731
26F Applications of Chromatography......Page 736
Questions and Problems......Page 739
27A Principles of GLC......Page 743
27B Instruments for GLC......Page 744
27C Gas Chromatographic Columns and Stationary Phases......Page 754
27D Applications of GC......Page 759
27E Advances in GC......Page 760
27F Gas-Solid Chromatography......Page 763
Questions and Problems......Page 764
CHAPTER TWENTY-EIGHT High-Performance Liquid Chromatography......Page 769
28B Column Efficiency in LC......Page 770
28C Instrumentation......Page 772
28D Partition Chromatography......Page 780
28F Ion Chromatography......Page 789
28G Size-Exclusion Chromatography......Page 794
28H Affinity Chromatography......Page 797
28I Thin-Layer Chromatography......Page 798
Questions and Problems......Page 801
29A Properties of Supercritical Fluids......Page 805
29B Supercritical Fluid Chromatography......Page 806
29C Supercritical Fluid Extraction......Page 812
Questions and Problems......Page 814
30A An Overview of Electrophoresis......Page 816
30B Capillary Electrophoresis......Page 817
30C Applications of CE......Page 823
30E Field-Flow Fractionation......Page 831
Questions and Problems......Page 836
Instrumental Analysis in Action— The Bisphenol A Controversy......Page 838
SECTION SIX Miscellaneous Methods......Page 842
31A Thermogravimetric Analysis......Page 843
31B Differential Thermal Analysis......Page 847
31C Differential Scanning Calorimetry......Page 848
31D Microthermal Analysis......Page 852
Questions and Problems......Page 854
32A Radioactive Nuclides......Page 857
32B Instrumentation......Page 863
32C Neutron Activation Methods......Page 865
32D Isotope Dilution Methods......Page 870
Questions and Problems......Page 871
33A Overview......Page 875
33B Flow Injection Analysis......Page 877
33C Microfluidics......Page 885
33D Discrete Automatic Systems......Page 887
Questions and Problems......Page 892
34A Introduction to Particle Size Analysis......Page 894
34B Low-Angle Laser Light Scattering......Page 895
34C Dynamic Light Scattering......Page 899
34D Photosedimentation......Page 901
Questions and Problems......Page 905
Instrumental Analysis in Action— The John F. Kennedy Assassinaton......Page 906
a1A Precision and Accuracy......Page 910
a1B Statistical Treatment of Random Errors......Page 913
a1C Hypothesis Testing......Page 924
a1D Method of Least Squares......Page 926
Questions and Problems......Page 929
a2A Properties of Activity Coefficients......Page 933
a2C The Debye-Hückel Equation......Page 934
APPENDIX THREE Some Standard and Formal Electrode Potentials......Page 936
APPENDIX FOUR Compounds Recommended for the Preparation of Standard Solutions of Some Common Elements......Page 940
Answers to Selected Problems......Page 942
Index......Page 950