Quantitative Chemical Analysis, 10th Edition
- Length: 792 pages
- Edition: 1
- Language: English
- Publisher: W. H. & Company
- Publication Date: 2020
- ISBN-10: 1319324509
- ISBN-13: 9781319324506
- Sales Rank: #3924032 (See Top 100 Books)
The 10th edition of Quantitative Chemical Analysis continues to set the standard for learning analytical chemistry with distinguished writing, the most up-to-date content, and now the acclaimed SaplingPlus program, supporting exceptional problem solving practice. New author Charles Lucy joins Dan Harris, infusing additional subject expertise and classroom experience into the 10th edition.
SaplingPlus combines Sapling’s renowned online homework with an extensive suite of engaging multimedia learning resources and a full eBook of Quantitative Chemical Analysis, 10e.
About this Book Cover Page Periodic Table of the Elements Physical Constants Concentrated Acids and Bases Frontispiece Title Page Copyright Page Brief Contents About the Authors From the Authors Contents About this Book Experiments Spreadsheet Topics Supplementary Spreadsheet Topics Spreadsheets Acknowledgments Chapter 0 The Analytical Process 0-1 The Analytical Chemist’s Job Sampling Sample Preparation Chemical Analysis (At Last!) Calibration Curves Interpreting the Results Simplifying Sample Preparation with Solid-Phase Extraction 0-2 General Steps in a Chemical Analysis Box 0-1 Constructing a Representative Sample End of Chapter Terms to Understand Problems Chapter 1 Chemical Measurements 1-1 SI Units Using Prefixes as Multipliers Converting Between Units 1-2 Chemical Concentrations Molarity and Molality Percent Composition Parts per Million and Parts per Billion 1-3 Preparing Solutions Dilution 1-4 Stoichiometry Calculations for Gravimetric Analysis Limiting Reagent End of Chapter Terms to Understand Summary Exercises Problems Chapter 2 Tools of the Trade 2-1 Safe, Ethical Handling of Chemicals and Waste 2-2 The Lab Notebook 2-3 Analytical Balance How an Electronic Balance Works Weighing Errors Buoyancy 2-4 Burets Mass Titrations and Microscale Titrations 2-5 Volumetric Flasks 2-6 Pipets and Syringes Using a Transfer Pipet Serial Dilution Micropipets Syringes 2-7 Filtration 2-8 Drying 2-9 Calibration of Volumetric Glassware 2-10 Introduction to Microsoft Excel® Getting Started: Buoyancy Correction Arithmetic Operations and Functions Documentation and Readability Absolute and Relative References 2-11 Graphing with Microsoft Excel End of Chapter Terms to Understand Summary Exercises Problems Chapter 3 Experimental Error 3-1 Significant Figures 3-2 Significant Figures in Arithmetic Addition and Subtraction Multiplication and Division Logarithms and Antilogarithms 3-3 Types of Error Systematic Error Box 3-1 Certified Reference Materials Random Error Blunders Box 3-2 Post-mortems of Failed Quant Labs Precision and Accuracy Absolute and Relative Uncertainty 3-4 Propagation of Uncertainty from Random Error Addition and Subtraction Multiplication and Division Mixed Operations The Real Rule for Significant Figures Exponents and Logarithms 3-5 Propagation of Uncertainty from Systematic Error Multiple Deliveries from One Pipet: The Virtue of Calibration Matrix Effects: What Is in the Sample? Uncertainty in Atomic Mass Box 3-3 Atomic Mass of the Elements End of Chapter Terms to Understand Summary Exercises Problems Chapter 4 Statistics 4-1 Gaussian Distribution Mean Value and Standard Deviation Significant Figures in Mean and Standard Deviation Standard Deviation and Probability Standard Deviation of the Mean 4-2 Comparison of Standard Deviations with the F Test Box 4-1 Choosing the Null Hypothesis in Epidemiology 4-3 Confidence Intervals Calculating Confidence Intervals The Meaning of a Confidence Interval Confidence Interval as a Measure of Uncertainty Finding Confidence Intervals with Excel 4-4 Comparison of Means with Student’s t Case 1. Comparing a Measured Result with a “Known” Value Case 2. Comparing Replicate Measurements Case 2a: Standard Deviations Are Not Significantly Different Case 2b: Standard Deviations A Significantly Different Case 3. Paired t Test for Comparing Individual Differences One-Tailed and Two-Tailed Significance Tests Is My Blood Glucose Reading Correct? 4-5 t Tests with a Spreadsheet 4-6 Grubbs Test for an Outlier 4-7 The Method of Least Squares Finding the Equation of the Line How Reliable Are Least-Squares Parameters? 4-8 Calibration Curves Constructing a Calibration Curve Box 4-2 Using a Nonlinear Calibration Curve Good Practice Box 4-3 Importance of Graphs to Visualize Data Propagation of Uncertainty with a Calibration Curve Propagation of Uncertainty 4-9 A Spreadsheet for Least Squares Adding Error Bars to a Graph End of Chapter Terms to Understand Summary Exercises Problems Chapter 5 Quality Assurance and Calibration Methods 5-1 Basics of Quality Assurance Use Objectives Specifications Box 5-1 Medical Implication of False Positive Results Assessment Box 5-2 Control Charts 5-2 Method Validation Selectivity Linearity Accuracy Precision Box 5-3 The Horwitz Trumpet: Variation in Interlaboratory Precision Range Limits of Detection and Quantitation Robustness 5-3 Standard Addition Graphical Procedure for Standard Addition to a Single Solution Graphical Procedure for Multiple Solutions with Constant Volume 5-4 Internal Standards Multipoint Calibration Curve for an Internal Standard End of Chapter Terms to Understand Summary Exercises Problems Chapter 6 Chemical Equilibrium 6-1 The Equilibrium Constant Manipulating Equilibrium Constants 6-2 Equilibrium and Thermodynamics Enthalpy Entropy Free Energy Le Châtelier’s Principle 6-3 Solubility Product Box 6-1 Solubility Is Governed by More Than the Solubility Product Common Ion Effect Demonstration 6-1 Common Ion Effect Separation by Precipitation 6-4 Complex Formation Lewis Acids and Bases Effect of Complex Ion Formation on Solubility Box 6-2 Notation for Formation Constants Tabulated Equilibrium Constants Are Usually Not “Constant“ 6-5 Protic Acids and Bases Brønsted-Lowry Acids and Bases Salts Conjugate Acids and Bases The Nature of H+ and OH− Autoprotolysis 6-6 pH Is There Such a Thing as Pure Water? 6-7 Strengths of Acids and Bases Strong Acids and Bases Demonstration 6-2 The HCl Fountain Box 6-3 The Strange Behavior of Hydrofluoric Acid Weak Acids and Bases Common Classes of Weak Acids and Bases Polyprotic Acids and Bases Box 6-4 Carbonic Acid Relation Between Ka and Kb Shorthand for Organic Structures End of Chapter Terms to Understand Summary Exercises Problems Chapter 7 Let the Titrations Begin 7-1 Titrations Box 7-1 Reagent Chemicals and Primary Standards 7-2 Titration Calculations 7-3 Precipitation Titration Curves Before the Equivalence Point At the Equivalence Point After the Equivalence Point Shape of the Titration Curve 7-4 Titration of a Mixture 7-5 Calculating Titration Curves with a Spreadsheet 7-6 End-Point Detection Volhard Titration Fajans Titration Demonstration 7-1 Fajans Titration End of Chapter Terms to Understand Summary Exercises Problems Chapter 8 Activity and the Systematic Treatment of Equilibrium Demonstration 8-1 Effect of Ionic Strength on Ion Dissociation 8-1 The Effect of Ionic Strength on Solubility of Salts The Explanation What Do We Mean by “Ionic Strength”? Box 8-1 Salts With Ions Of Charge ≥|2| Do Not Fully Dissociate Box 8-2 Ion Pairing For Single-Cell Analysis 8-2 Activity Coefficients Activity Coefficients of Ions Effect of Ionic Strength, Ion Charge, and Ion Size on the Activity Coefficient How to Interpolate Activity Coefficients of Nonionic Compounds High Ionic Strengths 8-3 pH Revisited 8-4 Systematic Treatment of Equilibrium Charge Balance Mass Balance Box 8-3 Calcium Carbonate Mass Balance in Rivers Systematic Treatment of Equilibrium 8-5 Applying the Systematic Treatment of Equilibrium A Solution of Ammonia Solubility and Hydrolysis of Thallium Azide Solubility of Magnesium Hydroxide with Activity Coefficients We Will Usually Omit Activity Coefficients End of Chapter Terms to Understand Summary Exercises Problems Chapter 9 Monoprotic Acid-Base Equilibria 9-1 Strong Acids and Bases Box 9-1 Concentrated HNO3 Is Only Slightly Dissociated The Dilemma The Cure Water Almost Never Produces 10−7 MH+ and 10−7 M OH− 9-2 Weak Acids and Bases Weak Is Conjugate to Weak Using Appendix G 9-3 Weak-Acid Equilibria A Typical Weak-Acid Problem Fraction of Dissociation Box 9-2 Dyeing Fabrics and the Fraction of Dissociation The Essence of a Weak-Acid Problem 9-4 Weak-Base Equilibria A Typical Weak-Base Problem Conjugate Acids and Bases — Revisited 9-5 Buffers Mixing a Weak Acid and Its Conjugate Base Henderson-Hasselbalch Equation Properties of the Henderson-Hasselbalch Equation A Buffer in Action Box 9-3 Strong Plus Weak Reacts Completely Preparing a Buffer in Real Life! Buffer Capacity How Much Buffer to Use? Buffer pH Depends on Ionic Strength and Temperature When What You Mix Is Not What You Get End of Chapter Terms to Understand Summary Exercises Problems Chapter 10 Polyprotic Acid-Base Equilibria 10-1 Diprotic Acids and Bases The Acidic Form, H2L+ Box 10-1 Carbon Dioxide in the Ocean The Basic Form, L− The Intermediate Form, HL Box 10-2 Successive Approximations Simplified Calculation for the Intermediate Form Summary of Diprotic Acid Calculations 10-2 Diprotic Buffers 10-3 Polyprotic Acids and Bases 10-4 Which Is the Principal Species? Box 10-3 Microequilibrium Constants 10-5 Fractional Composition Equations Monoprotic Systems Diprotic Systems 10-6 Isoelectric and Isoionic pH Proteins Are Polyprotic Acids and Bases Box 10-4 Isoelectric Focusing End of Chapter Terms to Understand Summary Exercises Problems Chapter 11 Acid-Base Titrations 11-1 Titration of Strong Base with Strong Acid Region 1: Before the Equivalence Point Region 2: At the Equivalence Point Region 3: After the Equivalence Point The Titration Curve 11-2 Titration of Weak Acid with Strong Base Region 1: Before Base Is Added Region 2: Before the Equivalence Point Region 3: At the Equivalence Point Region 4: After the Equivalence Point The Titration Curve 11-3 Titration of Weak Base with Strong Acid 11-4 Titrations in Diprotic Systems A Typical Case Point A Point B Point C Point D Point E Blurred End Points 11-5 Finding the End Point with a pH Electrode Box 11-1: Alkalinity and Acidity Using Derivatives to Find the End Point Using a Gran Plot to Find the End Point 11-6 Finding the End Point with Indicators Demonstration 11-1 Indicators and The Acidity of CO2 Box 11-2 What Does a Negative pH Mean? Choosing an Indicator 11-7 Practical Notes 11-8 Kjeldahl Nitrogen Analysis Box 11-3 Kjeldahl Nitrogen Analysis Behind the Headlines 11-9 The Leveling Effect 11-10 Calculating Titration Curves with Spreadsheets Titrating a Weak Acid with a Strong Base Titrating a Weak Acid with a Weak Base End of Chapter Terms to Understand Summary Exercises Problems Chapter 12 EDTA Titrations 12-1 Metal-Chelate Complexes 12-2 EDTA Acid-Base Properties EDTA Complexes Conditional Formation Constant 12-3 EDTA Titration Curves Titration Calculations The Titration Curve 12-4 Do It with a Spreadsheet 12-5 Auxiliary Complexing Agents Metal-Ligand Equilibria EDTA Titration with an Auxiliary Complexing Agent Box 12-1 Metal Ion Hydrolysis Decreases the Effective Formation Constant for EDTA Complexes 12-6 Metal Ion Indicators Demonstration 12-1 Metal Ion Indicator Color Changes 12-7 EDTA Titration Techniques Direct Titration Back Titration Displacement Titration Indirect Titration Masking Box 12-2 Water Hardness End of Chapter Terms to Understand Summary Exercises Problems Chapter 13 Advanced Topics in Equilibrium 13-1 General Approach to Acid-Base Systems Applying the General Procedure Using Excel Solver Ignorance Is Bliss: A Complication of Ion Pairing 13-2 Activity Coefficients Back to Basics Ignorance Is Still Bliss 13-3 Dependence of Solubility on pH Solubility of CaF2 Acid Rain Dissolves Minerals and Creates Environmental Hazards Solubility of Barium Oxalate 13-4 Analyzing Acid-Base Titrations with Difference Plots Using Excel Solver to Optimize More Than One Parameter End of Chapter Terms to Understand Summary Exercises Problems Chapter 14 Fundamentals of Electrochemistry 14-1 Basic Concepts Chemistry and Electricity Electric Charge Electric Current Voltage, Work, and Free Energy Ohm’s Law Box 14-1 Ohm’s Law, Conductance, and Molecular Wire Power 14-2 Galvanic Cells A Cell in Action Electrons Move Toward More Positive Electric Potential Salt Bridge Demonstration 14-1 The Human Salt Bridge Line Notation Box 14-2 Hydrogen-Oxygen Fuel Cell Box 14-3 Lithium-Ion Battery 14-3 Standard Potentials In General, We Will Write All Half-Reactions as Reductions Measuring the Standard Reduction Potential 14-4 Nernst Equation Nernst Equation for a Half-Reaction Nernst Equation for a Complete Reaction Box 14-4 Latimer Diagrams: How to Find E° for a New Half-Reaction Different Descriptions of the Same Reaction Advice for Finding Relevant Half-Reactions The Nernst Equation Is Used in Measuring Standard Reduction Potentials 14-5 Eº and the Equilibrium Constant Box 14-5 Concentrations in the Operating Cell Finding K for Net Reactions That Are Not Redox Reactions 14-6 Biochemists Use Eº’ Relation Between Eº and Eº’ End of Chapter Terms to Understand Summary Exercises Problems Chapter 15 Electrodes and Potentiometry 15-1 Reference Electrodes Silver-Silver Chloride Reference Electrode Calomel Electrode Voltage Conversions Between Different Reference Scales 15-2 Indicator Electrodes Demonstration 15-1 Potentiometry with an Oscillating Reaction 15-3 What Is a Junction Potential? 15-4 How Ion-Selective Electrodes Work 15-5 pH Measurement with a Glass Electrode Calibrating a Glass Electrode Errors in pH Measurement Box 15-1 Systematic Error in Rainwater pH Measurement: Effect of Junction Potential Not All pH Electrodes Are Glass 15-6 Ion-Selective Electrodes Reminder: How Ion-Selective Electrodes Work Selectivity Coefficient Box 15-2 Measuring Selectivity Coefficients for an Ion-Selective Electrode Solid-State Electrodes Liquid-Based Ion-Selective Electrodes Box 15-3 How Was Perchlorate Discovered on Mars? Lowering the Detection Limit for Ion-Selective Electrodes Box 15-4 Ion-Selective Electrode with Electrically Conductive Polymer for a Sandwich Immunoassay Compound Electrodes Another Way to Measure Dissolved CO2 15-7 Using Ion-Selective Electrodes Standard Addition with Ion-Selective Electrodes Metal Ion Buffers 15-8 Solid-State Chemical Sensors Semiconductors and Diodes Chemical-Sensing Field Effect Transistor An “Electronic Nose” End of Chapter Terms to Understand Summary Exercises Problems Chapter 16 Redox Titrations 16-1 The Shape of a Redox Titration Curve Box 16-1 Many Redox Reactions Are Atom-Transfer Reactions Region 1: Before the Equivalence Point Region 2: At the Equivalence Point Region 3: After the Equivalence Point Shapes of Redox Titration Curves Demonstration 16-1 Potentiometric Titration of Fe2 with MnO4 16-2 Finding the End Point Redox Indicators Gran Plot The Starch-Iodine Complex 16-3 Adjustment of Analyte Oxidation State Preoxidation Prereduction 16-4 Oxidation with Potassium Permanganate Preparation and Standardization 16-5 Oxidation with Ce4+ Preparation and Standardization 16-6 Oxidation with Potassium Dichromate Box 16-2 Environmental Carbon Analysis and Oxygen Demand 16-7 Methods Involving Iodine Use of Starch Indicator Preparation and Standardization of I−3 Solutions Use of Sodium Thiosulfate Analytical Applications of Iodine Box 16-3 Iodometric Analysis of High-Temperature Superconductors End of Chapter Terms to Understand Summary Exercises Problems Chapter 17 Electroanalytical Techniques Demonstration 17-1 Electrochemical Writing 17-1 Fundamentals of Electrolysis Current Measures the Rate of Reaction Voltage Changes When Current Flows Controlled-Potential Electrolysis with a Three-Electrode Cell Box 17-1 Metal Reactions at Atomic Steps 17-2 Electrogravimetric Analysis Underpotential Deposition 17-3 Coulometry Types of Coulometry 17-4 Amperometry Box 17-2 Clark Oxygen Electrode Blood Glucose Monitor Box 17-3 Using a Glucose Meter and Aptamer to Measure Melamine in Milk “Electrical Wiring” of Enzymes and Mediators for Blood Glucose Monitor 17-5 Voltammetry Rotating Disk Electrode Cyclic Voltammetry at a Stationary, Planar Electrode Polarography Faradaic and Charging Currents Box 17-4 The Electric Double Layer Square Wave Voltammetry Box 17-5 Aptamer Biosensor for Clinical Use Uses Square Wave Voltammetry Stripping Analysis Microelectrodes 17-6 Karl Fischer Titration of H2O End of Chapter Terms to Understand Summary Exercises Problems Chapter 18 Fundamentals of Spectrophotometry 18-1 Properties of Light 18-2 Absorption of Light Box 18-1 Why Is There a Logarithmic Relation Between Transmittance and Concentration? Demonstration 18-1 Absorption Spectra 18-3 Measuring Absorbance 18-4 Beer’s Law in Chemical Analysis Formation of an Absorbing Product: Serum Iron Determination When Beer’s Law Fails 18-5 Spectrophotometric Titrations 18-6 What Happens When a Molecule Absorbs Light? Electronic States of Formaldehyde Vibrational and Rotational States of Formaldehyde Combined Electronic, Vibrational, and Rotational Transitions What Happens to Absorbed Energy? Box 18-2 Fluorescence All Around Us 18-7 Luminescence Relation Between Absorption and Emission Spectra Excitation and Emission Spectra Box 18-3 Rayleigh and Raman Scattering Luminescence Intensity Example: Fluorimetric Assay of Selenium in Brazil Nuts End of Chapter Terms to Understand Summary Exercises Problems Chapter 19 Applications of Spectrophotometry 19-1 Analysis of a Mixture Solving for Two Unknowns Using Two Wavelengths Solving Simultaneous Linear Equations with Excel Using More Wavelengths Than Unknowns (Recommended) Inverse Multivariate Calibration Box 19-1 Multivariate Calibration on the Farm 19-2 Measuring an Equilibrium Constant Isosbestic Points Measuring an Equilibrium Constant 19-3 Spectrophotometric Reactions Colorimetric Kits Discrete Analyzers Microplates Scattering by Particles 19-4 Flow Injection Analysis and Sequential Injection Sequential Injection 19-5 Luminescence in Analytical Chemistry Fluorescence Derivatization Box 19-2 Designing a Molecule for Fluorescence Detection Fluorescence in Molecular Biology Bioluminescence and Chemiluminescence 19-6 Sensors Based on Luminescence Quenching Luminescence Quenching A Luminescent Intracellular O2 Sensor Förster Resonance Energy Transfer Box 19-3 Upconversion Photobleaching 19-7 Immunoassays Box 19-4 How Does a Home Pregnancy Test Work? Immunoassays in Environmental Analysis Time-Resolved Fluorescence Immunoassays End of Chapter Terms to Understand Summary Exercises Problems Chapter 20 Spectrophotometers 20-1 Lamps and Lasers: Sources of Light Blackbody Continuum Sources Box 20-1 The Greenhouse Effect Arc Sources Line Sources Lasers Light-Emitting Diodes 20-2 Monochromators Gratings Resolving Power, Dispersion, and Efficiency of a Grating Choosing the Monochromator Bandwidth Polychromatic Light Stray Light Validation Filters 20-3 Detectors Photomultiplier Tube Box 20-2 The Most Important Photoreceptor Photodiode Photodiode Array Charge Coupled Device Infrared Detectors Box 20-3 Nondispersive Photoacoustic Infrared Measurement of CO2 on Mauna Loa Calibrating Detector Response for Luminescence Measurements 20-4 Optical Sensors Refraction Optical Fibers Optodes Fiber-Optic Spectrophotometer Attenuated Total Reflectance Surface Plasmon Resonance 20-5 Fourier Transform Infrared Spectroscopy Fourier Analysis Interferometry Fourier Transform Spectroscopy Advantages of Fourier Transform Spectroscopy Quantitative Infrared Spectroscopy 20-6 Dealing with Noise Signal Averaging Types of Noise Minimizing Noise with a Double Beam Spectrophotometer Digital Smoothing of Noisy Data End of Chapter Terms to Understand Summary Exercises Problems Chapter 21 Atomic Spectroscopy 21-1 An Overview Box 21-1 Mercury Analysis by Cold Vapor Atomic Fluorescence 21-2 Atomization: Flames, Furnaces, and Plasmas Flames Box 21-2 Measuring Sodium with a Bunsen Burner Photometer Chemical Vapor Generation Furnaces Matrix Modifiers for Furnaces Inductively Coupled Plasma 21-3 How Temperature Affects Atomic Spectroscopy The Boltzmann Distribution Effect of Temperature on Excited-State Population The Effect of Temperature on Absorption and Emission 21-4 Instrumentation Atomic Linewidths Hollow-Cathode Lamp Multielement Detection with Atomic Emission Background Correction Detection Limits 21-5 Interference Types of Interference Virtues of the Inductively Coupled Plasma 21-6 Inductively Coupled Plasma–Mass Spectrometry Atomic Isobaric Interference Collision and Dynamic Reaction Cell for Polyatomic Interference 21-7 Atomic Spectroscopy of Solid Samples Laser Ablation Laser-Induced Breakdown Spectroscopy Box 21-3 Atomic Emission Spectroscopy on Mars Quantitative Analysis 21-8 X-Ray Fluorescence 21-9 Choosing the Right Atomic Spectrometer End of Chapter Terms to Understand Summary Exercises Problems Chapter 22 Mass Spectrometry 22-1 What Is Mass Spectrometry? Box 22-1 Molecular Mass and Nominal Mass A Time-of-Flight Mass Spectrometer Electron Ionization Chemical Ionization Resolving Power 22-2 Oh, Mass Spectrum, Speak to Me! Molecular Ion and Isotope Patterns Box 22-2 Establishing Elemental Composition from Isotope Peak Intensities Box 22-3 Isotope Ratio Mass Spectrometry and Dinosaur Body Temperature High-Resolution Mass Spectrometry Rings + Double Bonds Identifying the Molecular Ion Peak Interpreting Fragmentation Patterns 22-3 Types of Mass Spectrometers Transmission Quadrupole Mass Spectrometer Detectors for Mass Spectrometry Time-of-Flight Mass Spectrometer with Electrostatic Mirror Linear Quadrupole Ion-Trap Mass Spectrometer Orbitrap Mass Spectrometer 22-4 Chromatography–Mass Spectrometry Interfaces Electrospray Ionization Atmospheric Pressure Chemical Ionization 22-5 Chromatography–Mass Spectrometry Techniques Selected Ion Monitoring Extracted Ion Chromatogram Tandem Mass Spectrometry Selected Reaction Monitoring Enhancement of Signal-to-Background Ratio by Selected Reaction Monitoring 22-6 Protein Mass Spectrometry Electrospray of Proteins Box 22-4 Making Elephants Fly (Mechanisms of Protein Electrospray) Electron-Transfer Dissociation for Protein Sequencing Tandem Mass Tags for Quantitative Analysis 22-7 Open-Air Sampling for Mass Spectrometry Direct Analysis in Real Time (DART) Low-Temperature Plasma Desorption Electrospray Ionization (DESI) Miniature Mass Spectrometer and Paper Spray Sample Introduction Chemical Reactions Accelerated in Microdroplets Matrix-Assisted Ionization 22-8 Ion Mobility Spectrometry Ion Mobility–Mass Spectrometry End of Chapter Terms to Understand Summary Exercises Problems Chapter 23 Introduction to Analytical Separations 23-1 Solvent Extraction pH Effects Extraction with a Metal Chelator Demonstration 23-1 Extraction with Dithizone Box 23-1 Greener Extractions Ion-Pair Extraction 23-2 What is Chromatography? Types of Chromatography 23-3 A Plumber’s View of Chromatography The Chromatogram Relation Between Retention Time and the Distribution Constant Scaling Up 23-4 Efficiency of Separation Resolution Diffusion Plate Height: A Measure of Column Efficiency Factors Affecting Resolution 23-5 Why Bands Spread Broadening Outside the Column Plate Height Equation Longitudinal Diffusion Finite Time for Mass Transfer Between Phases Multiple Flow Paths Advantages of Open Tubular Columns A Touch of Reality: Asymmetric Peaks Box 23-2 Microscopic Description of Chromatography End of Chapter Terms to Understand Summary Exercises Problems Chapter 24 Gas Chromatography 24-1 The Separation Process in Gas Chromatography Open Tubular Columns Box 24-1 Chiral Phases for Separating Optical Isomers Packed Columns Retention Temperature and Pressure Programming Carrier Gas Guard Columns and Retention Gaps 24-2 Sample Injection Split Injection Splitless Injection On-Column Injection 24-3 Detectors Classifications of Detectors Thermal Conductivity Detector Flame Ionization Detector Electron Capture Detector Box 24-2 Chromatography Column on a Chip Gas Chromatography–Mass Spectrometry Other Detectors 24-4 Sample Preparation 24-5 Method Development in Gas Chromatography Goal of the Analysis Sample Preparation Choosing the Detector Selecting the Column Box 24-3 Two-Dimensional Gas Chromatography Choosing the Injection Method End of Chapter Terms to Understand Summary Exercises Problems Chapter 25 High-Performance Liquid Chromatography 25-1 The Chromatographic Process Small Particles Give High Efficiency but Require High Pressure The Column The Stationary Phase Box 25-1 One-Million-Plate Colloidal Crystal Columns Operating by Slip Flow The Elution Process Demonstration 25-1 Normal- and Reversed-Phase Chromatography Isocratic and Gradient Elution Box 25-2 “Green” Technology: Supercritical Fluid Chromatography Hydrophilic Interaction Chromatography (HILIC) Selecting the Separation Mode Solvents Maintaining Symmetric Bandshape 25-2 Injection and Detection in HPLC Pumps and Injection Valves Spectrophotometric Detectors Evaporative Light-Scattering Detector Charged Aerosol Detector Electrochemical Detector Refractive Index Detector Comments on Mass Spectrometric Detection in Liquid Chromatography 25-3 Method Development for Isocratic Reversed-Phase Separations Criteria for an Adequate Separation Optimization of Isocratic Separation How pH Affects Retention Optimization of Isocratic Separations of Acids and Bases 25-4 Gradient Separations Begin Method Development with a Scouting Gradient Developing a Gradient Separation Box 25-3 Choosing Gradient Conditions and Scaling Gradients Dwell Volume and Dwell Time 25-5 Do It with a Computer End of Chapter Terms to Understand Summary Exercises Problems Chapter 26 Chromatographic Methods and Capillary Electrophoresis 26-1 Ion-Exchange Chromatography Ion Exchangers Ion-Exchange Selectivity and Equivalents Donnan Exclusion Conducting Ion-Exchange Chromatography Applications of Ion Exchange 26-2 Ion Chromatography Suppressed-Ion Anion and Cation Chromatography Ion Chromatography Without Suppression Detectors Ion-Pair Chromatography Box 26-1 Surfactants and Micelles 26-3 Size Exclusion Chromatography The Elution Equation Stationary Phase Molecular Mass Determination 26-4 Affinity Chromatography Box 26-2 Molecular Imprinting 26-5 Hydrophobic Interaction Chromatography 26-6 Principles of Capillary Electrophoresis Electrophoresis Electroosmosis Mobility Plate Number and Resolution 26-7 Conducting Capillary Electrophoresis Controlling the Environment Inside the Capillary Sample Injection and Composition Conductivity Effects: Stacking and Skewed Peaks Detectors Micellar Electrokinetic Chromatography Capillary Sieving Electrophoresis Method Development 26-8 Lab-on-a-Chip End of Chapter Terms to Understand Summary Exercises Problems Chapter 27 Gravimetric and Combustion Analysis 27-1 An Example of Gravimetric Analysis 27-2 Precipitaion Demonstration 27-1 Colloids, Dialysis, and Microdialysis Crystal Growth Homogeneous Precipitation Precipitation in the Presence of Electrolyte Box 27-1 van der Waals Attraction Digestion Purity Product Composition 27-3 Examples of Gravimetric Calculations 27-4 Combustion Analysis Gravimetric Combustion Analysis Combustion Analysis Today End of Chapter Terms to Understand Summary Exercises Problems Chapter 28 Sample Preparation 28-1 Statistics of Sampling Origin of Sampling Variance Choosing a Sample Size Choosing the Number of Replicate Analyses 28-2 Dissolving Samples for Analysis Grinding Dissolving Inorganic Materials with Acids Dissolving Inorganic Materials by Fusion Decomposition of Organic Substances 28-3 Sample Preparation Techniques Liquid Extraction Techniques Solid-Phase Extraction QuEChERS Derivatization End of Chapter Terms to Understand Summary Exercises Problems Notes and References Glossary Appendix A Logarithms and Exponents and Graphs of Straight Lines Appendix B Propagation of Uncertainty Appendix C Additional Data Handling Techniques Appendix D Oxidation Numbers and Balancing Redox Equations Appendix E Normality Appendix F Solubility Products Appendix G Acid Dissociation Constants Appendix H Standard Reduction Potentials Appendix I Formation Constants Appendix J Logarithm of the Formation Constant for the Ion-Pairing Reaction M(aq) + L(aq) ⇌ ML(aq) Appendix K Analytical Standards Appendix L DNA and RNA Solutions to Exercises Answers to Problems Color Plate Index Back Cover
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