Analytical Chemistry An Introduction

, by Skoog, Douglas A.; West, Donald M.; Holler, F. James; Crouch, Stanley R.

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ISBN: 9780030202933 | 0030202930
Cover: Hardcover
Copyright: 8/23/1999

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The new edition highlights some of the latest techniques such as supercritical fluid chromatography and capillary electrophoresis. The addition of spreadsheet exercises and problems throughout the text provides students with a more modern approach to analytical chemistry.

Preface

xvii

1 What Is Analytical Chemistry?

(18)

1A The Role of Analytical Chemistry

(2)

1B Classifying Quantitative Analytical Methods

(1)

1C Stepping Through a Typical Quantitative Analysis

(5)

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

(9)

FEATURES

1-1 Deer Kill: A Case Study Illustrating the Use of Analytical Chemistry to Solve a Problem in Toxicology

(7)

Section I The Tools of Analytical Chemistry

(158)

2 The Tools of Analytical Chemistry

(40)

2A Selecting and Handling Reagents and Other Chemicals

(1)

2B Cleaning and Marking Laboratory Ware

(1)

2C Evaporating Liquids

(1)

2D Measuring Mass

(7)

2E The Equipment and Manipulations Associated with Weighing

(4)

2F The Equipment and Manipulations for Filtration and Ignition

(6)

2G Measuring Volume

(9)

2H Calibrating Volumetric Ware

(2)

2I The Laboratory Notebook

(2)

2J Using Spreadsheets in Analytical Chemistry

(5)

2K Safety in the Laboratory

(2)

3 Important Chemical Concepts: Expressing Quantities and Concentrations

(18)

3A Some Important Units of Measurement

(4)

3B Solutions and Their Concentrations

(8)

3C Chemical Stoichiometry

(3)

3D Questions and Problems

FEATURES

3-1 Distinguishing between Mass and Weight

3-2 Atomic Mass Units and the Mole

3-3 Another Approach to Example 3-2

4 The Basic Approach to Chemical Equilibrium

(24)

4A The Chemical Composition of Aqueous Solutions

(4)

4B Chemical Equilibrium

(18)

WEB WORKS

101

(1)

4C Questions and Problems

101

FEATURES

4-1 Amphiprotic Species

4-2 Stepwise and Overall Formation Constants for Complex Ions

4-3 Why [H(2)O} Does Not Appear in Equilibrium-Constant Expressions for Aqueous Solutions

4-4 Relative Strengths of Conjugate Acid/Base Pairs

4-5 The Method of Successive Approximations

5 Errors in Chemical Analyses: How Certain Can We Be?

103

(14)

5A Defining Terms

104

(4)

5B Systematic Errors

108

(8)

WEB WORKS

116

(1)

5C Questions and Problems

116

(1)

6 Random Error: How Certain Can We Be?

117

(32)

6A The Nature of Random Errors

117

(3)

6B Treating Random Errors with Statistics

120

(19)

6C The Standard Deviation of Computed Results

139

(3)

6D Reporting Computed Data

142

(4)

WEB WORKS

146

(1)

6E Questions and Problems

146

FEATURES

6-1 Flipping Coins: A Student Activity to Illustrate a Normal Distribution

121

6-2 How Do You Calculate Those Areas under a Curve?

124

6-3 The Significance of Number of Degrees of Freedom

126

6-4 Equation for Calculating Pooled Standard Deviations

134

7 Statistical Analysis: Evaluating the Data

149

(28)

7A Confidence Limits

149

(4)

7B Statistical Aids to Hypothesis Testing

153

(4)

7C Detecting Gross Errors

157

(3)

7D Analyzing Two-Dimensional Data: The Least Squares Method

160

(13)

WEB WORKS

172

(1)

7E Questions and Problems

173

(4)

Section II Principles and Applications of Chemical Equilibria

177

(210)

8 Gravimetric Methods of Analysis

179

(25)

8A Properties of Precipitates and Precipitating Reagents

180

(11)

8B Drying and Ignition of Precipitates

191

(1)

8C Calculating Results from Gravimetric Data

192

(2)

8D Applications of Gravimetric Methods

194

(7)

WEB WORKS

201

(1)

8E Questions and Problems

201

FEATURES

8-1 Specific Surface Area of Colloids

187

9 Electrolyte Effects: Activity or Concentration?

204

(17)

9A Effects of Electrolytes on Chemical Equilibria

204

(3)

9B Activity Coefficients

207

(12)

WEB WORKS

219

(1)

9C Questions and Problems

219

FEATURES

9-1 Mean Activity Coefficients

211

10 How Equilibrium Calculations Can Be Applied to Complex Systems

221

(25)

10A Solving Multiple-Equilibrium Problems by a Systematic Method

222

(4)

10B Calculating Solubilities by the Systematic Method

226

(6)

10C Separating Ions by pH Control: Sulfide Separations

232

(12)

WEB WORKS

244

(1)

10D Questions and Problems

244

FEATURES

10-1 Algebraic Expressions Needed to Calculate Solubility of CaC(2)O(4) Water

231

10-2 Immunoassay: Equilibria in the Specific Determination of Drugs

235

11 Titrations: Taking Advantage of Stoichiometric Reactions

246

(19)

11A Some General Aspects of Volumetric Titrimetry

247

(2)

11B Standard Solutions

249

(1)

11C Volumetric Calculations

250

(8)

11D Titration Curves

258

(3)

WEB WORKS

261

(1)

11E Questions and Problems

261

FEATURES

11-1 The Factor-Label Approach to Example 11-6

255

11-2 How Did We Calculate the Volumes of NaOH Shown in the First Column of Table 11-1?

260

12 Principles of Neutralization Titrations: Determining Acids, Bases, and the pH of Buffer Solutions

265

(38)

12A What Solutions and Indicators Are Used?

265

(4)

12B Calculating pH in Titrations of Strong Acids and Strong Bases

269

(7)

12C Buffer Solutions

276

(11)

12D Calculating pH in Weak Acid Titrations

287

(6)

12E Calculating pH in Titrations of Weak Bases

293

(4)

12F How Do Buffer Solutions Change as a Function of pH?

297

(2)

WEB WORKS

299

(1)

12G Questions and Problems

299

FEATURES

12-1 Constructing Titration Curves from the Charge-Balance Equation

274

12-2 How Many Significant Figures Should We Retain in Titration Curve Calculations?

275

12-3 Applying the Systematic Method to Buffer Calculations

277

12-4 The Henderson-Hasselbach Equation

278

12-5 Acid Rain and the Buffer Capacity of Lakes

282

12-6 Determining Dissociation Constants for Weak Acids and Bases

291

12-7 Determining the pK Values for Amino Acids

295

13 Titrating Polyfunctional Acids and Bases

303

(24)

13A Polyfunctional Acids

303

(1)

13B Describing Polyfunctional Bases

303

(2)

13C Finding the pH of Solutions of Amphiprotic Salts

305

(3)

13D Constructing Titration Curves for Polyfunctional Acids

308

(6)

13E Drawing Titration Curves for Polyfunctional Bases

314

(3)

13F The Composition of Polyprotic Acid Solutions as a Function of pH

317

(7)

WEB WORKS

324

(1)

13G Questions and Problems

324

FEATURES

13-1 Combining Equilibrium-Constant Expressions

304

13-2 How Was Equation 13-3 Generated?

306

13-3 The Dissociation of Sulfuric Acid

314

13-4 Titration Curves for Amino Acids

316

13-5 A General Expression for Alpha Values

318

14 Applying Neutralization Titrations

327

(18)

14A Reagents for Neutralization Titrations

327

(6)

14B Typical Applications of Neutralization Titrations

333

(7)

WEB WORKS

340

(1)

14C Questions and Problems

340

FEATURES

14-1 Determining Total Serum Protein

334

14-2 Other Methods for Determining Organic Nitrogen

335

15 Complexation and Precipitation Titrations: Taking Advantage of Complexing and Precipitating Agents

345

(42)

15A Forming Complexes

345

(6)

15B Titrations with Inorganic Complexing Agents

351

(8)

15C Organic Complexing Agents

359

(2)

15D Titrations with Aminocarboxylic Acids

361

(22)

WEB WORKS

382

(1)

15E Questions and Problems

383

FEATURES

15-1 Determination of Hydrogen Cyanide in Acrylonitrile Plant Streams

353

15-2 Species Present in a Solution of EDTA

362

15-3 EDTA as a Preservative

364

15-4 How Can Masking and Demasking Agents Be Used to Enhance the Selectivity of EDTA Titrations?

381

15-5 Test Kits for Water Hardness

382

Section III Electrochemical Methods

387

(158)

16 Elements of Electrochemistry

389

(30)

16A Characterizing Oxidation/Reduction Reactions

389

(5)

16B Electrochemical Cells

394

(3)

16C Electrode Potentials

397

(19)

WEB WORKS

415

(1)

16D Questions and Problems

416

FEATURES

16-1 Balancing Redox Equations

391

16-2 The Daniell Gravity Cell

396

16-3 Why We Cannot Measure Absolute Electrode Potentials

401

16-4 Sign Conventions in the Older Literature

411

16-5 Why Are There Two Electrode Potentials for Br(2) in Table 16-1?

413

17 Using Electrode Potentials

419

(25)

17A Calculating Potentials of Electrochemical Cells

419

(4)

17B Calculating Redox Equilibrium Constants

423

(5)

17C Constructing Redox Titration Curves

428

(11)

17D Oxidation/Reduction Indicators

439

(2)

17E Potentiometric End Points

441

(1)

WEB WORKS

441

(1)

17F Questions and Problems

442

FEATURES

17-1 Biological Redox Systems

424

18 Applying Oxidation/Reduction Titrations

444

(27)

18A Auxiliary Oxidizing and Reducing Reagents

444

(2)

18B Applying Standard Reducing Agents

446

(4)

18C Applying Standard Oxidizing Agents

450

(17)

WEB WORKS

466

(1)

18D Questions and Problems

467

FEATURES

18-1 Determination of Chromium Species in Water Samples

453

18-2 Antioxidants

458

19 Potentiometry: Measuring Concentrations of Ions and Molecules

471

(37)

19A General Principles

471

(1)

19B What Reference Electrodes Are Used?

472

(2)

19C Dealing with Liquid-Junction Potentials

474

(1)

19D Indicator Electrodes

475

(18)

19E Instruments for Measuring Cell Potential

493

(1)

19F Direct Potentiometry

493

(6)

19G Following Titrations by Potentiometry

499

(6)

WEB WORKS

505

(1)

19H Questions and Problems

505

FEATURES

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

487

19-2 Point-of-Care Testing: Blood Gases and Blood Electrolytes with Portable Instrumentation

490

20 A Brief Look at Some Other Electroanalytical Methods

508

(37)

20A How Does Current Affect the Potential of Electrochemical Cells?

509

(6)

20B Are Electrolytic Methods Selective?

515

(1)

20C Electrogravimetric Methods: Weighing the Deposit

516

(6)

20D Coulometric Methods of Analysis

522

(9)

20E Voltammetry

531

(8)

20F Some Additional Electroanalytical Methods

539

(1)

WEB WORKS

540

(1)

20G Questions and Problems

540

FEATURES

20-1 Overvoltage and the Lead-Acid Battery

515

Section IV Spectrochemical Analysis

545

(92)

21 Spectroscopic Methods of Analysis: Making Measurements with Light

547

(25)

21A Light: A Particle, a Wave, or Both?

548

(2)

21B How Radiation and Matter Interact

550

(5)

21C Absorbing Light

555

(13)

WEB WORKS

568

(1)

21D Questions and Problems

568

FEATURES

21-1 Spectroscopy and the Discovery of Elements

554

21-2 Why Is a Red Solution Red?

565

22 Instruments for Measuring Absorption: Is It a Photometer, a Spectrophotometer, or a Spectrometer?

572

(22)

22A Instrument Components

572

(14)

22B UV/Visible Photometers and Spectrophotometers

586

(4)

22C Infrared Spectrophotometers

590

(2)

WEB WORKS

592

(1)

22D Questions and Problems

592

FEATURES

22-1 Gratings Rule 57

23 Applying Molecular and Atomic Spectroscopic Methods: Shedding More Light on the Subject

594

(43)

23A Applying Ultraviolet/Visible Molecular Absorption Methods

595

(16)

23B Absorbing Infrared Radiation: Good Vibrations

611

(4)

23C Assessing Errors in Spectrophotometry

615

(1)

23D Molecular Luminescence Spectroscopy

616

(9)

23E Molecular Scattering Methods

625

(1)

23F Atomic Spectroscopy

626

(6)

WEB WORKS

631

(1)

23G Questions and Problems

632

FEATURES

23-1 Infrared Photometers for Routine Determination of Atmospheric Pollutants

614

23-2 How Is Fluorescence Related to Concentration?

620

23-3 Use of Fluorescence Probes in Neurobiology: Probing the Enlightened Mind

622

23-4 Mercury and Its Determination by Cold-Vapor Atomic Absorption Spectroscopy

628

Section V Separation Methods

637

(82)

24 An Introduction to Analytical Separations

638

(29)

24A Masking

638

(1)

24B Precipitation and Filtration

639

(1)

24C Separating Species by Distillation

639

(1)

24D Separating Solutes by Extraction

640

(4)

24E Separating Ions by Ion Exchange

644

(2)

24F Chromatographic Separations

646

(17)

WEB WORKS

663

(1)

24G Questions and Problems

663

FEATURES

24-1 Derivation of Equation 24-2

641

24-2 What Is the Source of the Terms Plate and Plate Height?

658

25 Gas-Liquid and High-Performance Fluid Chromatography

667

(33)

25A Gas-Liquid Chromatography

667

(16)

25B High-Performance Liquid Chromatography

683

(12)

25C High-Performance Liquid Chromatography versus Gas-Liquid Chromatography

695

(3)

WEB WORKS

698

(1)

25D Questions and Problems

698

FEATURES

25-1 Use of Gas Chromatography/Mass Spectrometry to Identify a Drug Metabolite in Blood

679

25-2 Buckyballs: The Chromatographic Separation of Fullerenes

696

26 Supercritical-Fluid Chromatography, Capillary Electrophoresis, and Capillary Electrochromatography

700

(19)

26A Supercritical-Fluid Chromatography

700

(5)

26B Capillary Electrophoresis

705

(10)

26C Capillary Electrochromatography

715

(3)

WEB WORKS

717

(1)

26D Questions and Problems

718

(1)

Section VI Selected Methods of Analysis

719

27 Selected Methods of Analysis

721

27A An Introductory Experiment

723

(5)

27B Gravimetric Methods of Analysis

728

(4)

27C Neutralization Titrations

732

(8)

27D Precipitation Titrations

740

(1)

27E Complex-Formation Titrations with EDTA

741

(2)

27F Titrations with Potassium Permanganate

743

(6)

27G Titrations with Iodine

749

(3)

27H Titrations with Sodium Thiosulfate

752

(3)

27I Titrations with Potassium Bromate

755

(2)

27J Potentiometric Methods

757

(5)

27K Electrogravimetric Methods

762

(2)

27L Methods Based on the Absorption of Radiation

764

(4)

27M Atomic Spectroscopy

768

(2)

27N Separating Cations by Ion Exchange

770

(2)

27O Gas-Liquid Chromatography

772

WEB WORKS

773

Appendix 1 Solubility Product Constants at 25^(Degree)C

A-1

(2)

Appendix 2 Acid Dissociation Constants at 25^(Degree)C

A-3

(2)

Appendix 3 Formation Constants of Complex Compounds at 25^(Degree)C

A-5

(2)

Appendix 4 Standard and Formal Electrode Potentials

A-7

(3)

Appendix 5 Use of Exponential Numbers and Logarithms

A-10

(5)

Appendix 6 Volumetric Calculations Using Normality and Equivalent Weight

A-15

(8)

Appendix 7 Acronyms and Abbreviations of Significance in Analytical Chemistry

A-23

(2)

Answers to Selected Questions and Problems

A-25

Glossary

G-1

Index

I-1

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Analytical Chemistry An Introduction

Summary

Table of Contents

Supplemental Materials