AIMALYTICAL CHEMISTRY
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1 Fundamentals of AIMALYTICAL CHEMISTRY Seventh Edition Douglas A. Skoog Stanford University Donald M. West San Jose State University F. James Holler University ;of Kentucky W r SAUNDERS COLLEGE PUBLISHING Harcourt Brace College Publishers Fort Worth Philadelphia San Diego New York Orlando Austin San Antonio Toronto Montreal London Sydney Tokyo
2 Contents i Introduction 1 1A Role of Analytical Chemistry in the Sciences 7 1B Classification of Quantitative Methods of Analysis 2 1C Steps in a Typical Quantitative Analysis 3 Errors in Chemical Analyses 11 2A Definition of Terms 12 2B Systematic Errors 16 2C Questions and Problems 20 4 Random Errors in Analyses 21 3A The Nature of Random Errors 21 3B The Statistical Treatment of Random Error 25 3C The Standard Deviation of Computed Results 33 3D Methods for Reporting Computed Data 39 3E Questions and Problems 44 Application of Statistics to Data Treatment and Evaluation 4A Confidence Limits 47 4B Statistical Aids to Hypothesis Testing 51 4C Detection of Gross Errors 57 4D Estimation of Detection Limits 59 4E The Least-Squares Method for Deriving Calibration Plots 4F Quality Assurance and Control Charts 65 4G Questions and Problems 68 Gravimetrie Methods of Analysis 71 5A Gravimetrie Calculations 73 5B Properties of Precipitates and Precipitating Agents 82 5C Drying and Ignition of Precipitates 92 5D Application of Gravimetrie Methods 93 5E Questions and Problems 97
3 xii Contents Titrimetric Methods of Analysis 700 6A Some General Aspects of Volumetrie Titrimetry 100 6B Standard Solutions 702 6C Volumetrie Caiculations 103 6D Gravimetrie Titrimetry E Questions and Problems Aqueous-Solution Chemistry 722 7A The Chemical Composition ofaqueous Solutions 722 7B Chemical Equilibrium 126 7C Questions and Problems 746 Effect of Electrolytes on lonic Equilibria 148 8A Thermodynamic Versus Concentration-Based Equilibrium Consta nts 748 8B Activity Coefficients 757 8C Questions and Problems 758 Application of Equilibrium Caiculations to Complex Systems 159 9A A Systematic Method for Solving Multiple-Equilibrium Problems 760 9B The Calculation of Solubility by the Systematic Method 764 9C Separation of Ions by Control of the Concentration of the Precipitating Agent 783 9D Questions and Problems Theory of Neutralization Titrations A Solutions and Indicators for Acid/Base Titrations B Titration Curves C Titration Curves for Strong Acids and Strong Bases D Buffer Solutions E Titration Curves for Weak Acids F Titration Curves for Weak Bases G The Composition of Buffer Solutions as a Function of ph H Common Types of Acid/Base Indicators Questions and Problems 227.J!.J1L Titration Curves for Complex Acid/Base Systems A Mixtures of Strong and Weak Acids or Strong and Weak Bases 224 IIB Polyfunctional Acids C Polyfunctional Bases D Buffer Solutions Involving Polyprotic Acids 229
4 Contents xiii 11E Caiculation of the ph of Solutions of Amphiprotic Salts F Titration Curves for Polyfunctional Acids G Titration Curves for Polyfunctional Bases H Titration Curves for Amphiprotic Species The Composition of Solutions of a Polyprotic Acid as a Function of ph J Questions and Problems Z 1 '"J Applications of Neutralization Titrations A Reagents for Neutralization Titrations B Typical Applications of Neutralization Titrations C Questions and Problems 262 Precipitation Titrimetry A Titration Curves B End Points for Argentometric Titrations C Applications of Standard Silver Nitrate Solutions D Questions and Problems 275 Complex-Formation Titrations A Complex-Formation Reactions B Titrations with Aminocarboxylic Acids C Titrations with Inorganic Complexing Agents D Questions and Problems 507 -&. mb*f An Introduction to Electrochemistry A Oxidation/Reduction Reactions B Electrochemical Cells C Electrode Potentials D Questions and Problems 327 Applications of Standard Electrode Potentials A The Thermodynamic Potential of Electrochemical Cells B Calculations of Redox Equilibrium Constants C Redox Titration Curves D Oxidation/Reduction Indicators E Potentiometrie End Points F Questions and Problems 358 Applications of Oxidation/Reduction Titrations A Auxiliary Oxidizing and Reducing Reagents B Application of Standard Reductants 362
5 xiv Contents 17C Applications of Standard Oxidants D Some Specialized Oxidants E Questions and Problems Theory of Potentiometry A General Principles B Reference Electrodes C Liquid-Junction Potentials D Indicator Electrodes E Questions and Problems 470 Applications of Potentiometry A Instruments for Measuring Cell Potentials B Direct Potentiometrie Measurements C Potentiometrie Titrations D The Determination of Equilibrium Constants from Electrode Potential Measurements E Questions and Problems 429 Electrogravimetric and Coulometric Methods A The Effect of Current on the Potential of Electrochemical Cells B The Potential Selectivity of Electrolytic Methods C Electrogravimetric Methods ofanalysis D Coulometric Methods of Analysis E Questions and Problems 457 Voltammetry A Excitation Signals in Voltammetry B Linear-Scan Voltammetry C Pulse Polarographic and Voltammetric Methods D Stripping Methods E Voltammetry with Ultramicroelectrodes F Questions and Problems 495 An Introduction to Spectrochemical Methods A General Properties of Electromagnetic Radiation B The Electromagnetic Spectrum C Absorption of Radiation D Emission of Electromagnetic Radiation E Questions and Problems 524
6 Contents xv Instruments for Optical Spectrometry A Instrument Components B Optical Instrument Designs C Questions and Problems 555 Molecular Absorption Spectroscopy A Ultraviolet and Visible Molecular Absorption Spectroscopy B Automated Photometrie and Spectrophotometric Methods C Infrared Absorption Spectroscopy D Questions and Problems 598 Molecular Fluorescence Spectroscopy A Theory of Molecular Fluorescence B Effect of Concentration on Fluorescence Intensity C Fluorescence Instruments D Applications of Fluorescence Methods E Questions and Problems 609 Atomic Spectroscopy Based on Ultraviolet and Visible Radiation A Sources of Atomic Spectra B Atomic Spectroscopy Based upon Flame Atomization C Atomic Spectroscopy with Electrothermal Atomizers D Atomic Emission Methods Based on Plasma Sources E Questions and Problems 635 Kinetic Methods of Analysis 'A Rates of Chemical Reactions: Rate Laws B The Determination of Reaction Rates C Applications of Kinetic Methods D Questions and Problems 658 An Introduction to Chromatographie Methods A A General Description of Chromatography B Migration Rates of Solutes C Band Broadening and Column Efficiency D Column Resolution E Applications of Chromatography F Questions and Problems 684 Gas-Liquid Chromatography A Instruments for Gas-Liquid Chromatography B Gas-Chromatographie Columns and the Stationary Phase 693
7 xvi Contents 29C Applications of Gas-Liquid Chromatography D Gas-Solid Chromatography E Questions and Problems High-Performance Liquid Chromatography A Instruments B High-Performance Partition Chromatography C High-Performance Adsorption Chromatography D High-Performance Ion-Exchange Chromatography E High-Performance Size-Exclusion Chromatography F Comparison of High-Performance Liquid Chromatography with Gas- Liquid Chromatography G Supercritical-Fluid Chromatography H Planar Chromatography Questions and Problems 724 The Analysis of Real Samples 725 %&*^r.jl 32 31A Choice of Method for the Analysis of Real Samples B The Accuracy Obtainable in the Analysis of Complex Materials 732 Preparing Samples for Analysis A Sampling B Moisture in Samples C The Determination of Water in Samples D Questions and Problems 748 Decomposing and Dissolving the Sample 749 sw^ m*j 33A Sources of Errors in Decompositipn and Dissolution B Decomposing Samples by Inorganic Acids in Open Vessels C Microwave Decompositions D Combustion Methods for Decomposing Organic Samples E Decomposition of Inorganic Materials by Fluxes F Questions and Problems 759 "**% A \/t =s&..j Eliminating Interferences A The Nature of the Separation Process B Separation by Precipitation C Separation by Extraction D Application of Extraction Procedures E Ion-Exchange Separations F The Separation of Inorganic Species by Distillation G Questions and Problems 776
8 Contents xvii 1^ 1 I 36 The Chemicals, Apparatus, and Unit Operations of Analytical Chemistry A The Selection and Handling of Reagents and Other Chemicals B The Cleaning and Marking of Laboratory Ware C The Evaporation of Liquids D The Measurement of Mass E The Equipment and Manipulations Associated with Weighing F Weight Titrations G The Equipment and Manipulations for Filtration and Ignition H The Measurement of Volume The Calibration of Volumetrie Ware J The Laboratory Notebook K Safety in the Laboratory 870 Selected Methods of Analysis A Gravimetrie Methods of Analysis B Neutralization Titrations C Precipitation Titrations D Complex-Formation Titrations with EDTA E Titrations with Potassium Permanganate F Titration with lodine G Titrations with Sodium Thiosulfate H Titrations with Potassium Bromate Potentiometrie Methods J Electrogravimetric Methods K Coulometric Titrations L Voltammetry M Methods Based on the Absorption of Radiation N Molecular Fluorescence Atomic Spectroscopy P Applications of Ion-Exchange Resins Q Gas-Liquid Chromatography 868 Glossary G-7 A P P E N D I X j Selected References to the Literature of Analytical Chemistry A- A P P E N D I X 2 Solubility Product Constants A-6 3 A P P E N D I X o Dissociation Constants for Acids A-8
9 xviii Contents A P P E N D I X A Stepwise Formation Constants A-10 A P P E N D I X c Some Standard and Formal Electrode Potentials A-12 A P P E N D I X /r Designations Carried by Ashless Filter Papers A-16 A P P E N D I X -i Designations and Porosities for Filtering Crucibles A-17 A P P E N D I X Q Use of Exponential Numbers and Logarithms A-18 A P P E N D I X Q Volumetrie Caiculations Using Normality and Equivalent Weight A-23 A P P E N D I X Q Compounds Recommended for the Preparation of Standard Solutions of Common Elements A-32 A P P E N D I X i Propagation of Measurement Uncertainties A-34 Answers to Selected Questions and Problems A-40 Index 1-1
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