Fundamentals of Analytical Chemistry, 10th Edition PDF by Douglas A Skoog, Donald M West, F James Holler and Stanley R Crouch


Fundamentals of Analytical Chemistry, Tenth Edition

By Douglas A. Skoog, Donald M. West, F. James Holler and Stanley R. Crouch

Fundamentals of Analytical Chemistry, Tenth Edition


Chapter 1 The Nature of Analytical Chemistry 1

1A The Role of Analytical Chemistry 2

1B Quantitative Analytical Methods 4

1C A Typical Quantitative Analysis 4

1D An Integral Role for Chemical Analysis: Feedback Control Systems 8

Feature 1-1 Deer Kill: A Case Study Illustrating the Use

of Analytical Chemistry to Solve a Problem in Toxicology 9


Chapter 2 Calculations Used

in Analytical Chemistry 15

2A Some Important Units of Measurement 15

Feature 2-1 Unified Atomic Mass Units and the Mole 18

Feature 2-2 The Factor-Label Approach to Example 2-2 20

2B Solutions and Their Concentrations 20

2C Chemical Stoichiometry 28

Chapter 3 Precision and Accuracy of Chemical Analyses 38

3A Some Important Terms 39

3B Systematic Errors 43

Chapter 4 Random Errors in Chemical Analysis 51

4A The Nature of Random Errors 51

Feature 4-1 Flipping Coins: A Student Activity to Illustrate a Normal Distribution 55

4B Statistical Treatment of Random Errors 56

Feature 4-2 Areas under the Gaussian Curve 59

Feature 4-3 The Significance of the Number of Degrees of Freedom 60

Feature 4-4 Equation for Calculating the Pooled Standard Deviation 64

4C Standard Deviation of Calculated Results 66

4D Reporting Computed Data 71

Chapter 5 Statistical Data Treatment and Evaluation 80

5A Confidence Intervals 81

Feature 5-1 W. S. Gossett (Student) 85

5B Statistical Aids to Hypothesis Testing 86

5C Analysis of Variance 98

5D Detection of Gross Errors 105

Chapter 6 Sampling, Standardization, and Calibration 113

6A Analytical Samples and Methods 114

6B Sampling 116

6C Automated Sample Handling 126

6D Standardization and Calibration 128

Feature 6-1 Lab-on-a-Chip 129

Feature 6-2 A Comparison Method for Aflatoxins 130

Feature 6-3 Multivariate Calibration 141

6E Figures of Merit for Analytical Methods 146


Chapter 7 Aqueous Solutions and Chemical Equilibria 160

7A The Chemical Composition of Aqueous Solutions 160

7B Chemical Equilibrium 165

Feature 7-1 Stepwise and Overall Formation Constants for Complex Ions 169

Feature 7-2 Why [H2O] Does Not Appear in Equilibrium-

Constant Expressions for Aqueous Solutions 170

Feature 7-3 Relative Strengths of Conjugate Acid-Base Pairs 176

Feature 7-4 The Method of Successive Approximations 181

7C Buffer Solutions 183

Feature 7-5 The Henderson-Hasselbalch Equation 185

Feature 7-6 Acid Rain and the Buffer Capacity of Lakes 191

Chapter 8 Effect of Electrolytes on Chemical Equilibria 199

8A The Effect of Electrolytes on Chemical Equilibria 200

8B Activity Coefficients 203

Feature 8-1 Mean Activity Coefficients 206

Chapter 9 Solving Equilibrium Problems for Complex Systems 214

9A Solving Multiple-Equilibrium Problems Using a Systematic Method 215

9B Calculating Solubilities by the Systematic Method 221

Feature 9-1 Algebraic Expressions Needed to Calculate the Solubility of CaC2O4 in Water 226

9C Separation of Ions by Control of the Concentration of the Precipitating Agent 231

Feature 9-2 Immunoassay: Equilibria in the Specific Determination of Drugs 235


Chapter 10 Gravimetric Methods of Analysis 244

10A Precipitation Gravimetry 244

Feature 10-1 Specific Surface Area of Colloids 252

10B Calculation of Results from Gravimetric Data 256

10C Applications of Gravimetric Methods 258

Chapter 11 Titrations in Analytical Chemistry 267

11A Some Terms Used in Volumetric Titrations 268

11B Standard Solutions 270

11C Volumetric Calculations 271

Feature 11-1 Another Approach to Example 11-6(a) 276

Feature 11-2 Rounding the Answer to Example 11-7 277

11D Gravimetric Titrations 279

11E Titration Curves 280

Feature 11-3 Calculating the NaOH Volumes Shown in the

First Column of Table 11-1 282

Chapter 12 Principles of Neutralization Titrations 288

12A Solutions and Indicators for Acid-Base Titrations 288

12B Titration of Strong Acids and Bases 293

Feature 12-1 Using the Charge-Balance Equation to Construct Titration Curves 295

Feature 12-2 Significant Figures in Titration Curve Calculations 297

12C Titration Curves for Weak Acids 298

Feature 12-3 Determining Dissociation Constants of Weak Acids and Bases 301

Feature 12-4 A Master Equation Approach to Weak Acid/ Strong Base Titrations 302

12D Titration Curves for Weak Bases 303

Feature 12-5 Determining the pK Values for Amino Acids 305

12E The Composition of Solutions During Acid-Base Titrations 306

Feature 12-6 Locating Titration End Points from pH Measurements 307

Chapter 13 Complex Acid-Base Systems 314

13A Mixtures of Strong and Weak Acids or Strong and Weak Bases 314

13B Polyfunctional Acids and Bases 317

13C Buffer Solutions Involving Polyprotic Acids 320

13D Calculation of the pH of Solutions of NaHA 321

13E Titration Curves for Polyfunctional Acids 325

Feature 13-1 The Dissociation of Sulfuric Acid 333

13F Titration Curves for Polyfunctional Bases 334

13G Titration Curves for Amphiprotic Species 335

Feature 13-2 Acid-Base Behavior of Amino Acids 335

13H Composition of Polyprotic Acid Solutions as a Function of pH 336

Feature 13-3 A General Expression for Alpha Values 337

Feature 13-4 Logarithmic Concentration Diagrams 339

Chapter 14 Applications of Neutralization Titrations 345

14A Reagents for Neutralization Titrations 345

14B Typical Applications of Neutralization Titrations 351

Feature 14-1 Determining Total Serum Protein 352

Feature 14-2 Other Methods for Determining Organic Nitrogen 352

Feature 14-3 Equivalent Masses of Acids and Bases 358

Chapter 15 Complexation and Precipitation Reactions and Titrations 365

15A The Formation of Complexes 365

Feature 15-1 Calculation of Alpha Values for Metal Complexes 368

15B Titrations with Inorganic Complexing Agents 371

Feature 15-2 Determination of Hydrogen Cyanide in Acrylonitrile Plant Streams 372

15C Organic Complexing Agents 378

15D Aminocarboxylic Acid Titrations 379

Feature 15-3 Species Present in a Solution of EDTA 381

Feature 15-4 EDTA as a Preservative 383

Feature 15-5 EDTA Titration Curves When a Complexing Agent Is Present 393

Feature 15-6 Enhancing the Selectivity of EDTA Titrations

with Masking and Demasking Agents 399

Feature 15-7 Test Kits for Water Hardness 401


Chapter 16 Introduction to Electrochemistry 407

16A Characterizing Oxidation/Reduction Reactions 407

Feature 16-1 Balancing Redox Equations 408

16B Electrochemical Cells 412

Feature 16-2 The Daniell Gravity Cell 414

16C Electrode Potentials 417

Feature 16-3 Why We Cannot Measure Absolute Electrode Potentials 420

Feature 16-4 Sign Conventions in the Older Literature 427

Feature 16-5 Why Are There Two Electrode Potentials for Br2 in Table 16-1? 430

Chapter 17 Applications of Standard Electrode Potentials 437

17A Calculating Potentials of Electrochemical Cells 437

17B Determining Standard Potentials Experimentally 444

Feature 17-1 Biological Redox Systems 446

17C Calculating Redox Equilibrium Constants 446

Feature 17-2 A General Expression for Calculating Equilibrium

Constants from Standard Potentials 450

17D Constructing Redox Titration Curves 452

Feature 17-3 The Inverse Master Equation Approach for Redox Titration Curves 460

Feature 17-4 Reaction Rates and Electrode Potentials 465

17E Oxidation/Reduction Indicators 465

17F Potentiometric End Points 468

Chapter 18 Applications of Oxidation/Reduction Titrations 473

18A Auxiliary Oxidizing and Reducing Reagents 473

18B Applying Standard Reducing Agents 475

18C Applying Standard Oxidizing Agents 479

Feature 18-1 Determination of Chromium Species in Water Samples 481

Feature 18-2 Antioxidants 486

Chapter 19 Potentiometry 500

19A General Principles 501

19B Reference Electrodes 502

19C Liquid Junction Potentials 505

19D Indicator Electrodes 505

Feature 19-1 An Easily Constructed Liquid-Membrane Ion- Selective Electrode 517

Feature 19-2 The Structure and Performance of Ion-Sensitive Field Effect Transistors 519

Feature 19-3 Point-of-Care Testing: Blood Gases and Blood

Electrolytes with Portable Instrumentation 523

19E Instruments for Measuring Cell Potential 525

Feature 19-4 The Loading Error in Potential Measurements 525

Feature 19-5 Operational Amplifier Voltage Measurements 527

19F Direct Potentiometry 528

19G Potentiometric Titrations 534

19H Potentiometric Determination of Equilibrium Constants 538

Chapter 20 Bulk Electrolysis: Electrogravimetry and Coulometry 544

20A The Effect of Current on Cell Potential 545

Feature 20-1 Overvoltage and the Lead-Acid Battery 551

20B The Selectivity of Electrolytic Methods 552

20C Electrogravimetric Methods 553

20D Coulometric Methods 559

Feature 20-2 Coulometric Titration of Chloride in Biological Fluids 568

Chapter 21 Voltammetry 575

21A Excitation Signals in Voltammetry 576

21B Voltammetric Instrumentation 577

Feature 21-1 Voltammetric Instruments Based on Operational Amplifiers 578

21C Hydrodynamic Voltammetry 583

21D Polarography 598

21E Cyclic Voltammetry 601

21F Pulse Voltammetry 604

21G Applications of Voltammetry 607

21H Stripping Methods 608

21I Voltammetry with Microelectrodes 610


Chapter 22 Introduction to Spectrochemical Methods 617

22A Properties of Electromagnetic Radiation 618

22B Interaction of Radiation and Matter 621

Feature 22-1 Spectroscopy and the Discovery of Elements 623

22C Absorption of Radiation 624

Feature 22-2 Deriving Beer’s Law 627

Feature 22-3 Why Is a Red Solution Red? 631

22D Emission of Electromagnetic Radiation 639

Chapter 23 Instruments for Optical Spectrometry 649

23A Instrument Components 649

Feature 23-1 Laser Sources: The Light Fantastic 653

Feature 23-2 Origin of Equation 23-1 659

Feature 23-3 Producing Ruled and Holographic Gratings 661

Feature 23-4 Basis of Equation 23-2 664

Feature 23-5 Signals, Noise, and the Signal-to-Noise Ratio 666

Feature 23-6 Measuring Photocurrents with Operational Amplifiers 674

23B Ultraviolet/Visible Photometers and Spectrophotometers 676

23C Infrared Spectrophotometers 679

Feature 23-7 How Does a Fourier Transform Infrared Spectrometer Work? 681

Chapter 24 Molecular Absorption Spectrometry 689

24A Ultraviolet and Visible Molecular Absorption Spectroscopy 689

24B Automated Photometric and Spectrophotometric Methods 711

24C Infrared Absorption Spectroscopy 714

Feature 24-1 Producing Spectra with an FTIR Spectrometer 718

Chapter 25 Molecular Fluorescence Spectroscopy 728

25A Theory of Molecular Fluorescence 728

25B Effect of Concentration on Fluorescence Intensity 732

25C Fluorescence Instrumentation 733

25D Applications of Fluorescence Methods 734

Feature 25-1 Use of Fluorescence Probes in Neurobiology: Probing the Enlightened 735

25E Molecular Phosphorescence Spectroscopy 737

25F Chemiluminescence Methods 738

Chapter 26 Atomic Spectroscopy 742

26A Origins of Atomic Spectra 743

26B Production of Atoms and Ions 746

26C Atomic Emission Spectrometry 756

26D Atomic Absorption Spectrometry 760

Feature 26-1 Determining Mercury by Cold-Vapor Atomic Absorption Spectroscopy 767

26E Atomic Fluorescence Spectrometry 770

Chapter 27 Mass Spectrometry 774

27A Principles of Mass Spectrometry 774

27B Mass Spectrometers 776

27C Atomic Mass Spectrometry 780

27D Molecular Mass Spectrometry 783


Chapter 28 Kinetic Methods of Analysis 792

28A Rates of Chemical Reactions 793

Feature 28-1 Enzymes 800

28B Determining Reaction Rates 806

Feature 28-2 Fast Reactions and Stopped-Flow Mixing 806

28C Applications of Kinetic Methods 813

Feature 28-3 The Enzymatic Determination of Urea 815

Chapter 29 Introduction to Analytical Separations 821

29A Separation by Precipitation 822

29B Separation of Species by Distillation 826

29C Separation by Extraction 826

Feature 29-1 Derivation of Equation 29-3 828

29D Separating Ions by Ion Exchange 831

Feature 29-2 Home Water Softeners 833

29E Chromatographic Separations 835

Feature 29-3 What Is the Source of the Terms Plate and Plate Height? 843

Feature 29-4 Derivation of Equation 29-24 845

Chapter 30 Gas Chromatography 860

30A Instruments for Gas-Liquid Chromatography 861

30B Gas Chromatographic Columns and Stationary Phases 870

30C Applications of Gas-Liquid Chromatography 874

Feature 30-1 Use of GC/MS to Identify a Drug Metabolite in Blood 876

30D Gas-Solid Chromatography 882

Chapter 31 High-Performance Liquid Chromatography 886

31A Instrumentation 887

Feature 31-1 LC/MS and LC/MS/MS 894

31B Partition Chromatography 895

31C Adsorption Chromatography 898

31D Ion Chromatography 899

31E Size-Exclusion Chromatography 901

Feature 31-2 Buckyballs: The Chromatographic Separation of Fullerenes 903

31F Affinity Chromatography 905

31G Chiral Chromatography 905

31H Comparison of High-Performance Liquid Chromatography

and Gas Chromatography 906

Chapter 32 Miscellaneous Separation Methods 910

32A Supercritical Fluid Separations 910

32B Planar Chromatography 915

32C Capillary Electrophoresis 917

Feature 32-1 Capillary Array Electrophoresis in DNA Sequencing 924

32D Capillary Electrochromatography 924

32E Field-Flow Fractionation 927



The following chapters are available as Adobe

Acrobat® PDF files on the companion site for the book.

Chapter 33 The Analysis of Real Samples 935

33A Real Samples 935

33B Choice of Analytical Method 937

33C Accuracy in the Analysis of Complex Materials 942

Chapter 34 Preparing Samples for Analysis 945

34A Preparing Laboratory Samples 945

34B Moisture in Samples 947

34C Determining Water in Samples 950

Chapter 35 Decomposing and Dissolving the Sample 951

35A Sources of Error in Decomposition and Dissolution 952

35B Decomposing Samples with Inorganic Acids in Open Vessels 952

35C Microwave Decompositions 954

35D Combustion Methods for Decomposing Organic Samples 957

35E Decomposing Inorganic Materials with Fluxes 959

Chapter 36 Chemicals, Apparatus, and Unit

Operations of Analytical Chemistry 961

36A Selecting and Handling Reagents

and Other Chemicals 962

36B Cleaning and Marking

of Laboratory Ware 963

36C Evaporating Liquids 964

36D Measuring Mass 964

36E Equipment and Manipulations

Associated with Weighing 971

36F Filtration and Ignition of Solids 974

36G Measuring Volume 980

36H Calibrating Volumetric Glassware 989

36I The Laboratory Notebook 991

36J Safety in the Laboratory 992

Chapter 37 Selected Methods of Analysis 994

37A An Introductory Experiment 995

37B Gravimetric Methods of Analysis 1004

37C Neutralization Titrations 1008

37D Precipitation Titrations 1017

37E Complex-Formation Titrations with EDTA 1020

37F Titrations with Potassium Permanganate 1023

37G Titrations with Iodine 1029

37H Titrations with Sodium Thiosulfate 1031

37I Titrations with Potassium Bromate 1034

37J Potentiometric Methods 1036

37K Electrogravimetric Methods 1040

37L Coulometric Titrations 1042

37M Voltammetry 1044

37N Methods Based on the Absorption of Radiation 1046

37O Molecular Fluorescence 1050

37P Atomic Spectroscopy 1051

37Q Application of Ion-Exchange Resins 1054

37R Gas-Liquid Chromatography 1056

Glossary G-1

APPENDIX 1 The Literature of Analytical Chemistry A-1

APPENDIX 2 Solubility Product Constants at 25°C A-6

APPENDIX 3 Acid Dissociation Constants at 25°C A-8

APPENDIX 4 Formation Constants at 25°C A-10

APPENDIX 5 Standard and Formal Electrode Potentials A-12

APPENDIX 6 Use of Exponential Numbers and Logarithms A-15

APPENDIX 7 Volumetric Calculations Using Normality and Equivalent Weight A-19

APPENDIX 8 Compounds Recommended for the

Preparation of Standard Solutions of Some Common Elements A-26

APPENDIX 9 Derivation of Error Propagation Equations A-28

Answers to Selected Questions and Problems A-33

Index I-1

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