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Gary D. Christian is the author of Analytical Chemistry, 7th Edition, published by Wiley. Purnendu K. Dasgupta is the author of Analytical Chemistry, 7th Edition, published by Wiley.
Chapter 1 Analytical Objectives, or: What Analytical Chemists Do 1
1.1 What Is Analytical Science?, 2
1.2 Qualitative and Quantitative Analysis:
What Does Each Tell Us?, 3
1.3 Getting Started: The Analytical Process, 6
1.4 Validation of a Method—You Have to Prove It Works!, 15
1.5 Analyze Versus Determine—They Are Different, 16
1.6 Some Useful Websites, 16
Chapter 2 Basic Tools and Operations of Analytical Chemistry 21
2.1 The Laboratory Notebook—Your Critical Record, 22
2.2 Laboratory Materials and Reagents, 24
2.3 The Analytical Balance—The Indispensible Tool, 26
2.4 Volumetric Glassware—Also Indispensible, 31
2.5 Preparation of Standard Base Solutions, 43
2.6 Preparation of Standard Acid Solutions, 44
2.7 Other Apparatus—Handling and Treating Samples, 44
2.8 Igniting Precipitates—Gravimetric Analysis, 51
2.9 Obtaining the Sample—Is It Solid, Liquid, or Gas?, 52
2.10 Operations of Drying and Preparing a Solution of the Analyte, 53
2.11 Laboratory Safety, 60
Chapter 3 Statistics and Data Handling in Analytical Chemistry 65
3.1 Accuracy and Precision: There Is a Difference, 66
3.2 Determinate Errors—They Are Systematic, 67
3.3 Indeterminate Errors—They Are Random, 68
3.4 Significant Figures: How Many Numbers Do You Need?, 69
3.5 Rounding Off, 74
3.6 Ways of Expressing Accuracy, 75
3.7 Standard Deviation—The Most Important Statistic, 76
3.8 Propagation of Errors—Not Just Additive, 79
3.9 Significant Figures and Propagation of Error, 85
3.10 Control Charts, 87
3.11 The Confidence Limit—How Sure Are You?, 88
3.12 Tests of Significance—Is There a Difference?, 90
3.13 Rejection of a Result: The Q Test, 99
3.14 Statistics for Small Data Sets, 102
3.15 Linear Least Squares—How to Plot the Right Straight Line, 104
3.16 Correlation Coefficient and Coefficient of Determination, 108
3.17 Detection Limits—There Is No Such Thing as Zero, 109
3.18 Statistics of Sampling—How Many Samples, How Large?, 111
3.19 Powering a Study: Power Analysis, 114
3.20 Use of Spreadsheets in Analytical Chemistry, 116
3.21 Using Spreadsheets for Plotting Calibration Curves, 121
3.22 Slope, Intercept, and Coefficient of Determination, 122
3.23 LINEST for Additional Statistics, 123
3.24 Statistics Software Packages, 124
Chapter 4 Good Laboratory Practice: Quality Assurance and Method Validation 137
4.1 What Is Good Laboratory Practice?, 139
4.2 Validation of Analytical Methods, 139
4.3 Quality Assurance—Does the Method Still Work?, 146
4.4 Laboratory Accreditation, 150
4.5 Electronic Records and Electronic
Signatures: 21 CFR, Part 11, 150
4.6 Some Official Organizations, 152
Chapter 5 Stoichiometric Calculations: The Workhorse of the Analyst 155
5.1 Review of the Fundamentals, 155
5.2 How Do We Express Concentrations of Solutions?, 158
5.3 Expressions of Analytical Results—So Many Ways, 166
5.4 Volumetric Analysis: How Do We Make Stoichiometric Calculations?, 173
5.5 Volumetric Calculations—Let’s Use Molarity, 176
5.6 Titer—How to Make Rapid Routine Calculations, 187
5.7 Weight Relationships—You Need These for Gravimetric Calculations, 188
Chapter 6 General Concepts of Chemical Equilibrium 196
6.1 Chemical Reactions: The Rate Concept, 197
6.2 Types of Equilibria, 199
6.3 Gibbs Free Energy and the Equilibrium Constant, 199
6.4 Le Chˆatelier’s Principle, 200
6.5 Temperature Effects on Equilibrium Constants, 200
6.6 Pressure Effects on Equilibria, 201
6.7 Concentration Effects on Equilibria, 201
6.8 Catalysts, 201
6.9 Completeness of Reactions, 202
6.10 Equilibrium Constants for Dissociating or Combining Species—Weak Electrolytes and Precipitates, 202
6.11 Calculations Using Equilibrium Constants—How Much Is in Equilibrium?, 203
6.12 The Common Ion Effect—Shifting the Equilibrium, 211
6.13 Systematic Approach to Equilibrium Calculations—How to Solve Any Equilibrium Problem, 212
6.14 Heterogeneous Equilibria—Solids Don’t Count, 219
6.15 Activity and Activity Coefficients—Concentration Is Not the Whole Story, 220
6.16 The Diverse Ion Effect: The Thermodynamic Equilibrium Constant and Activity Coefficients, 226
Chapter 7 Acid–Base Equilibria 230
7.1 The Early History of Acid–Base Concepts, 231
7.2 Acid–Base Theories—Not All Are Created Equal, 231
7.3 Acid–Base Equilibria in Water, 233
7.4 The pH Scale, 236
7.5 pH at Elevated Temperatures: Blood pH, 240
7.6 Weak Acids and Bases—What Is the pH?, 240
7.7 Salts of Weak Acids and Bases—They Aren’t Neutral, 243
7.8 Buffers—Keeping the pH Constant (or Nearly So), 246
7.9 Polyprotic Acids and Their Salts, 253
7.10 Ladder Diagrams, 256
7.11 Fractions of Dissociating Species at a Given pH: α Values—How Much of Each Species?, 257
7.12 Salts of Polyprotic Acids—Acid, Base, or Both?, 264
7.13 Physiological Buffers—They Keep You Alive, 270
7.14 Buffers for Biological and Clinical Measurements, 271
7.15 Diverse Ion Effect on Acids and Bases: cKa and cKb—Salts Change the pH, 275
7.16 log C – pH Diagrams, 275
7.17 Exact pH Calculators, 278
Chapter 8 Acid–Base Titrations 290
8.1 Strong Acid versus Strong Base—The Easy Titrations, 291
8.2 The Charge Balance Method - An Excel Exercise for the Titration of a Strong Acid and a Strong Base, 295
8.3 Detection of the End Point: Indicators, 298
8.4 Standard Acid and Base Solutions, 300
8.5 Weak Acid versus Strong Base—A Bit Less Straightforward, 300
8.6 Weak Base versus Strong Acid, 305
8.7 Titration of Sodium Carbonate—A Diprotic Base, 306
8.8 Using a Spreadsheet to Perform the Sodium Carbonate—HCl Titration, 308
8.9 Titration of Polyprotic Acids, 310
8.10 Mixtures of Acids or Bases, 313
8.11 Equivalence Points from Derivatives of a Titration Curve, 316
8.12 Titration of Amino Acids—They Are Acids and Bases, 320
8.13 Kjeldahl Analysis: Protein Determination, 321
8.14 Titrations Without Measuring Volumes, 324
Chapter 9 Complexometric Reactions and Titrations 335
9.1 Complexes and Formation Constants—How Stable Are Complexes?, 336
9.2 Chelates: EDTA—The Ultimate Titrating Agent for Metals, 338
9.3 Metal–EDTA Titration Curves, 344
9.4 Detection of the End Point: Indicators—They Are Also Chelating Agents, 348
9.5 Other Uses of Complexes, 350
9.6 Cumulative Formation Constants β and Concentrations of Specific Species in
Stepwise Formed Complexes, 350
Chapter 10 Gravimetric Analysis and Precipitation Equilibria 356
10.1 How to Perform a Successful Gravimetric Analysis, 357
10.2 Gravimetric Calculations—How Much Analyte Is There?, 364
10.3 Examples of Gravimetric Analysis, 368
10.4 Organic Precipitates, 369
10.5 Precipitation Equilibria: The Solubility Product, 370
10.6 Diverse Ion Effect on Solubility: Ksp and Activity Coefficients, 376
Chapter 11 Precipitation Reactions and Titrations 382
11.1 Effect of Acidity on Solubility of Precipitates: Conditional Solubility Product, 383
11.2 Mass Balance Approach for Multiple Equilibria, 384
11.3 Effect of Complexation on Solubility: Conditional Solubility Product, 388
11.4 Precipitation Titrations, 390
Chapter 12 Electrochemical Cells and Electrode Potentials 400
12.1 What Are Redox Reactions?, 401
12.2 Electrochemical Cells—What Electroanalytical Chemists Use, 402
12.3 Nernst Equation—Effects of Concentrations on Potentials, 408
12.4 Formal Potential—Use It for Defined Nonstandard Solution Conditions, 412
12.5 Limitations of Electrode Potentials, 413
Chapter 13 Potentiometric Electrodes and Potentiometry 417
13.1 Metal Electrodes for Measuring the Metal’s Cation, 418
13.2 Metal–Metal Salt Electrodes for Measuring the Salt’s Anion, 419
13.3 Redox Electrodes—Inert Metals, 421
13.4 Voltaic Cells without LiquidJunction—For Maximum Accuracy, 422
13.5 Voltaic Cells with Liquid Junction—The Practical Kind, 423
13.6 Reference Electrodes: The Saturated Calomel Electrode, 426
13.7 Measurement of Potential, 428
13.8 Determination of Concentrations from Potential Measurements, 430
13.9 Residual Liquid-Junction Potential—It Should Be Minimized, 430
13.10 Accuracy of Direct Potentiometric Measurements—Voltage Error versus Activity Error, 431
13.11 Glass pH Electrode—Workhorse of Chemists, 432
13.12 Standard Buffers—Reference for pH Measurements, 437
13.13 Accuracy of pH Measurements, 439
13.14 Using the pH Meter—How Does It Work?, 440
13.15 pH Measurement of Blood—Temperature Is Important, 442
13.16 pH Measurements in Nonaqueous Solvents, 443
13.17 Ion-Selective Electrodes, 443
13.18 Professor’s Favorite Example, 451
Chapter 14 Redox and Potentiometric Titrations 457
14.1 First: Balance the Reduction–Oxidation Reaction, 458
14.2 Calculation of the Equilibrium Constant of a Reaction—Needed to Calculate Equivalence Point Potentials, 458
14.3 Calculating Redox Titration Curves, 461
14.4 Visual Detection of the End Point, 466
14.5 Titrations Involving Iodine: Iodimetry and Iodometry, 468
14.6 Titrations with Other Oxidizing Agents, 473
14.7 Titrations with Other Reducing Agents, 474
14.8 Preparing the Solution—Getting the Analyte in the Right Oxidation State before Titration, 475
14.9 Potentiometric Titrations (Indirect Potentiometry), 477
Chapter 15 Voltammetry and Electrochemical Sensors 487
15.1 Voltammetry, 488
15.2 Amperometric Electrodes—Measurement of Oxygen, 493
15.3 Electrochemical Sensors: Chemically Modified Electrodes, 494
15.4 Ultramicroelectrodes, 496
15.5 Microfabicated Electrochemical Sensors, 496
15.6 Micro and Ultramicroelectrode Arrays, 497
Chapter 16 Spectrochemical Methods 499
16.1 Interaction of Electromagnetic Radiation with Matter, 500
16.2 Electronic Spectra and Molecular Structure, 507
16.3 Infrared Absorption and Molecular Structure, 512
16.4 Near-Infrared Spectrometry for Nondestructive Testing, 514
16.5 Spectral Databases—Identifying Unknowns, 516
16.6 Solvents for Spectrometry, 516
16.7 Quantitative Calculations, 517
16.8 Spectrometric Instrumentation, 527
16.9 Types of Instruments, 542
16.10 Array Spectrometers—Getting the Entire Spectrum at Once, 545
16.11 Fourier Transform Infrared Spectrometers, 546
16.12 Near-IR Instruments, 548
16.13 Spectrometric Error in Measurements, 549
16.14 Deviation from Beer’s Law, 550
16.15 Fluorometry, 553
16.16 Chemiluminescence, 561
16.17 Fiber Optic Sensors, 563
Chapter 17 Atomic Spectrometric Methods 572
17.1 Principles Distribution between Ground and Excited States—Most Atoms Are in the Ground State, 574
17.2 Flame Emission Spectrometry, 577
17.3 Atomic Absorption Spectrometry, 580
17.4 Sample Preparation—Sometimes Minimal, 591
17.5 Internal Standard and Standard Addition Calibration, 592
17.6 Atomic Emission Spectrometry: The Induction Coupled Plasma (ICP), 594
17.7 Atomic Fluorescence Spectrometry, 598
Chapter 18 Sample Preparation: Solvent and Solid-Phase Extraction 604
18.1 Distribution Coefficient, 605
18.2 Distribution Ratio, 605
18.3 Percent Extracted, 606
18.4 Solvent Extraction of Metals, 608
18.5 Accelerated and Microwave-Assisted Extraction, 610
18.6 Solid-Phase Extraction, 611
18.7 Microextraction, 616
18.8 Solid-Phase Nanoextraction (SPNE), 618
Chapter 19 Chromatography: Principles and Theory 621
19.1 Countercurrent Extraction: The
Predecessor to Modern Liquid Chromatography, 623
19.2 Principles of Chromatographic Separations, 629
19.3 Classification of Chromatographic Techniques, 630
19.4 Theory of Column Efficiency in Chromatography, 632
19.5 Chromatography Simulation Software, 642
Chapter 20 Gas Chromatography 645
20.1 Performing GC Separations, 646
20.2 Gas Chromatography Columns, 649
20.3 Gas Chromatography Detectors, 657
20.4 Temperature Selection, 665
20.5 Quantitative Measurements, 666
20.6 Headspace Analysis, 667
20.7 Thermal Desorption, 668
20.8 Purging and Trapping, 668
20.9 Small and Fast, 669
20.10 Separation of Chiral Compounds, 670
20.11 Two-Dimensional GC, 671
Chapter 21 Liquid Chromatography and Electrophoresis 676
21.1 High-Performance Liquid Chromatography, 679
21.2 Stationary Phase in HPLC, 682
21.3 Equipment for HPLC, 694
21.4 Ion Chromatography, 720
21.5 HPLC Method Development, 728
21.6 UHPLC and Fast LC, 730
21.7 Open Tubular Liquid Chromatography (OTLC), 731
21.8 Thin-Layer Chromatography, 731
21.9 Electrophoresis, 737
21.10 Capillary Electrophoresis, 740
21.11 Electrophoresis Related Techniques, 753
Chapter 22 Mass Spectrometry 764
22.1 Principles of Mass Spectrometry, 765
22.2 Inlets and Ionization Sources, 770
22.3 Gas Chromatography – Mass Spectrometry, 771
22.4 Liquid Chromatography – Mass Spectrometry, 776
22.5 Laser Desorption/Ionization, 780
22.6 Secondary Ion Mass Spectrometry, 783
22.7 Inductively-Coupled Plasma – Mass Spectrometry, 783
22.8 Mass Analyzers and Detectors, 784
22.9 Hybrid Instruments and Tandem Mass Spectrometry, 794
Chapter 23 Kinetic Methods of Analysis 800
23.1 Kinetics—The Basics, 801
23.2 Catalysis, 803
23.3 Enzyme Catalysis, 804
Chapter 24 Automation in Measurements 817
24.1 Principles of Automation, 818
24.2 Automated Instruments: Process Control, 818
24.3 Automatic Instruments, 821
24.4 Flow Injection Analysis, 822
24.5 Sequential Injection Analysis, 825
24.6 Laboratory Information Management Systems, 826
Chapter 25 Clinical Chemistry 828
25.1 Composition of Blood, 829
25.2 Collection and Preservation of Samples, 829
25.3 Clinical Analysis—Common Determinations, 831
25.4 Immunoassay, 834
Chapter 26 Environmental Sampling and Analysis 841
26.1 Getting a Meaningful Sample, 841
26.2 Air Sample Collection and Analysis, 842
26.3 Water Sample Collection and Analysis, 849
26.4 Soil and Sediment Sampling, 851
26.5 Sample Preparation for Trace Organics, 852
26.6 Contaminated Land Sites—What Needs to Be Analyzed?, 853
26.7 EPA Methods and Performance-Based Analyses, 853
APPENDIX A LITERATURE OF ANALYTICAL CHEMISTRY 859
APPENDIX B REVIEW OF MATHEMATICAL OPERATIONS: EXPONENTS, LOGARITHMS, AND THE QUADRATIC
FORMULA 863
APPENDIX C TABLES OF CONSTANTS 867
Table C.1 Dissociation Constants for Acids, 867
Table C.2a Dissociation Constants for Basic Species, 868
Table C.2b Acid Dissociation Constants for Basic Species, 869
Table C.3 Solubility Product Constants, 869
Table C.4 Formation Constants for Some EDTA Metal Chelates, 871
Table C.5 Some Standard and Formal Reduction Electrode Potentials, 872
APPENDIX D SAFETY IN THE LABORATORY 874
APPENDIX E PERIODIC TABLES ON THE WEB 875
APPENDIX F ANSWERS TO PROBLEMS 876
(Website)
APPENDIX G CENTURY OF THE GENE—GENOMICS AND PROTEOMICS: DNA SEQUENCING AND PROTEIN PROFILING G1
G.1 Of What Are We Made?, G2
G.2 What Is DNA?, G3
G.3 Human Genome Project, G4
G.4 How Are Genes Sequenced?, G5
G.5 Replicating DNA: The Polymerase Chain Reaction, G6
G.6 Plasmids and Bacterial Artificial Chromosomes (BACs), G7
G.7 DNA Sequencing, G8
G.8 Whole Genome Shotgun Sequencing, G11
G.9 Single-Nucleotide Polymorphisms, G12
G.10 DNA Chips, G12
G.11 Draft Genome, G13
G.12 Genomes and Proteomics: The Rest of the Story, G14
EXPERIMENTS E1
USE OF APPARATUS
Experiment 1 Use of the Analytical Balance, E1
Experiment 2 Use of the Pipet and Buret and Statistical Analysis, E3
Experiment 3 Analysis of Volumetric
Measurements Using
Spectrophotometric Microplate
Readers and Spreadsheet
Calculations, E4
GRAVIMETRY
Experiment 4 Gravimetric Determination of Chloride, E7
Experiment 5 Gravimetric Determination of SO3in a Soluble Sulfate, E9
Experiment 6 Gravimetric Determination of Nickel in a Nichrome Alloy, E11
ACID-BASE TITRATIONS
Experiment 7 Determination of Replaceable Hydrogen in Acid by Titration with Sodium Hydroxide, E13
Experiment 8 Determination of Total Alkalinity of Soda Ash, E15
Experiment 9 Determination of Aspirin Using Back Titration, E17
Experiment 10 Determination of Hydrogen Carbonate in Blood Using Back-Titration, E18
COMPLEXOMETRIC TITRATION
Experiment 11 Determination of Water Hardness with EDTA, E20
PRECIPITATION TITRATIONS Experiment 12 Determination of Silver in an Alloy: Volhard’s Method, E21
Experiment 13 Determination of Chloride in a Soluble Chloride: Fajans’ Method, E23
POTENTIOMETRIC MEASUREMENTS
Experiment 14 Determination of the pH of Hair Shampoos, E24
Experiment 15 Potentiometric Determination of Fluoride in Drinking Water Using a Fluoride Ion-Selective Electrode, E26
REDUCTION-OXIDATION TITRATIONS
Experiment 16 Analysis of an Iron Alloy or Ore by Titration with Potassium Dichromate, E27
Experiment 17 Analysis of Commercial Hypochlorite or Peroxide Solution by Iodometric Titration, E30
Experiment 18 Iodometric Determination of Copper, E33
Experiment 19 Determination of Antimony by Titration with Iodine, E34
Experiment 20 Microscale Quantitative Analysis of Hard-Water Samples Using an Indirect Potassium Permanganate Redox Titration, E36
POTENTIOMETRIC TITRATIONS
Experiment 21 pH Titration of Unknown Soda Ash, E39
Experiment 22 Potentiometric Titration of a Mixture of Chloride and Iodide, E40
SPECTROCHEMICAL MEASUREMENTS
Experiment 23 Spectrophotometric Determination of Iron, E41
Experiment 24 Spectrophotometric Determination of Iron in Vitamin Tablets Using a 96 Well Plate Reader, E43
Experiment 25 Determination of Nitrate Nitrogen in Water, E46
Experiment 26 Spectrophotometric Determination of Lead on Leaves Using Solvent Extraction, E47
Experiment 27 Spectrophotometric Determination of Inorganic Phosphorus in Serum, E49
Experiment 28 Spectrophotometric Determination of Manganese and Chromium in Mixture, E50
Experiment 29 Spectrophotometric Determination of Manganese in Steel Using a 96 Well Plate Reader, E52
Experiment 30 Ultraviolet Spectrophotometric Determination of Aspirin, Phenacetin, and Caffeine in APC Tablets Using Solvent Extraction, E55
Experiment 31 Infrared Determination of a Mixture of Xylene Isomers, E56
Experiment 32 Fluorometric Determination of Riboflavin (Vitamin B2), E57
ATOMIC SPECTROMETRY MEASUREMENTS
Experiment 33 Determination of Calcium by Atomic Absorption Spectrophotometry, E58
Experiment 34 Flame Emission Spectrometric Determination of Sodium, E60
SOLID-PHASE EXTRACTION AND CHROMATOGRAPHY
Experiment 35 Solid Phase Extraction with Preconcentration, Elution, and Spectrophotometric Analysis, E61
Experiment 36 Thin-Layer Chromatography Separation of Amino Acids, E68
Experiment 37 Gas Chromatographic Analysis of a Tertiary Mixture, E69
Experiment 38 Qualitative and Quantitative Analysis of Fruit Juices for Vitamin C Using High-Performance Liquid Chromatography, E71
Experiment 39 Analysis of Analgesics Using High-Performance Liquid Chromatography, E72
MASS SPECTROMETRY
Experiment 40 Capillary Gas Chromatography-Mass Spectrometry, E73
KINETIC ANALYSIS
Experiment 41 Enzymatic Determination of Glucose in Blood, E74
FLOW INJECTION ANALYSIS
Experiment 42 Characterization of Physical Parameters of a Flow Injection Analysis System, E76
Experiment 43 Single-Line FIA: Spectrophotometric Determination of Chloride, E79
Experiment 44 Three-Line FIA: Spectrophotometric Determination of Phosphate, E80
TEAM EXPERIMENTS
Experiment 45 Method Validation and Quality Control Study, E82
Experiment 46 Proficiency Testing: Determination of z Values of Class Experiments, E84
Index 877
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