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Analytical Chemistry

by ; ;
Edition:
7th
ISBN13:

9780470887578

ISBN10:
0470887575
Format:
Hardcover
Pub. Date:
10/7/2013
Publisher(s):
John Wiley & Sons Inc
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Summary

The 7th Edition of Gary Christian's Analytical Chemistry focuses on more in-depth coverage and information about Quantitative Analysis (aka Analytical Chemistry) and related fields. The content builds upon previous editions with more enhanced content that deals with principles and techniques of quantitative analysis with more examples of analytical techniques drawn from areas such as clinical chemistry, life sciences, air and water pollution, and industrial analyses.

Table of Contents

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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