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Exploring Chemical Analysis
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Fifth Edition©2012 Daniel C. Harris
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An ideal introduction to analytical chemistry, Exploring Chemical Analysis covers all major analytical topics with effective problem-solving methods. Learn how to understand analytical results and use quantitative manipulations, as the text prepares you for the problems youll encounter in fields from biology and chemistry to geology.
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Learn MoreTable of Contents
Chapter 0 The Analytical Process
Cocaine Use? Ask the River
0-1 The Analytical Chemists Job
0-2 General Steps in a Chemical Analysis
Box 0-1 Constructing a Representative Sample
Cocaine Use? Ask the River
0-1 The Analytical Chemists Job
0-2 General Steps in a Chemical Analysis
Box 0-1 Constructing a Representative Sample
Chapter 1 Chemical Measurements
Biochemical Measurements with a Nanoelectrode
1-1 SI Units and Prefixes
Box 1-1 Exocytosis of Neurotransmitters
1-2 Conversion Between Units
1-3 Chemical Concentrations
1-4 Preparing Solutions
1-5 The Equilibrium Constant
Chapter 2 Tools of the Trade
Catching a Cold with a Quartz Crystal Microbalance
2-1 Safety, Waste Disposal, and Green Chemistry
2-2 Your Lab Notebook
Box 2-1 Dan’s Lab Notebook Entry
2-3 The Analytical Balance
2-4 Burets
2-5 Volumetric Flasks
2-6 Pipets and Syringes
2-7 Filtration
2-8 Drying
2-9 Calibration of Volumetric Glassware
2-10 Methods of Sample Preparation
Reference Procedure: Calibrating a 50-mL buret
Catching a Cold with a Quartz Crystal Microbalance
2-1 Safety, Waste Disposal, and Green Chemistry
2-2 Your Lab Notebook
Box 2-1 Dan’s Lab Notebook Entry
2-3 The Analytical Balance
2-4 Burets
2-5 Volumetric Flasks
2-6 Pipets and Syringes
2-7 Filtration
2-8 Drying
2-9 Calibration of Volumetric Glassware
2-10 Methods of Sample Preparation
Reference Procedure: Calibrating a 50-mL buret
Chapter 3 Math Toolkit
Experimental Error
3-1 Significant Figures
3-2 Significant Figures in Arithmetic
3-3 Types of Error
Box 3-1 What Are Standard Reference Materials?
Box 3-2 Case Study: Systematic Error in Ozone Measurement
3-4 Propagation of Uncertainty
3-5 Introducing Spreadsheets
3-6 Graphing in Excel
Experimental Error
3-1 Significant Figures
3-2 Significant Figures in Arithmetic
3-3 Types of Error
Box 3-1 What Are Standard Reference Materials?
Box 3-2 Case Study: Systematic Error in Ozone Measurement
3-4 Propagation of Uncertainty
3-5 Introducing Spreadsheets
3-6 Graphing in Excel
Chapter 4 Statistics
Is My Red Blood Cell Count High Today?
4-1 The Gaussian Distribution
4-2 Comparison of Standard Deviations with the F Test
Box 4-1 Choosing the Null Hypothesis in Epidemiology
4-3 Students t
4-4 A Spreadsheet for the t test
4-5 Grubbs Test for an Outlier
4-6 Finding the “Best” Straight Line
4-7 Constructing a Calibration Curve
4-8 A Spreadsheet for Least Squares
Is My Red Blood Cell Count High Today?
4-1 The Gaussian Distribution
4-2 Comparison of Standard Deviations with the F Test
Box 4-1 Choosing the Null Hypothesis in Epidemiology
4-3 Students t
4-4 A Spreadsheet for the t test
4-5 Grubbs Test for an Outlier
4-6 Finding the “Best” Straight Line
4-7 Constructing a Calibration Curve
4-8 A Spreadsheet for Least Squares
Chapter 5 Quality Assurance and Calibration Methods
The Need for Quality Assurance
5-1 Basics of Quality Assurance
Box 5-1 Control Charts
5-2 Validation of an Analytical Procedure
5-3 Standard Addition
5-4 Internal Standards
The Need for Quality Assurance
5-1 Basics of Quality Assurance
Box 5-1 Control Charts
5-2 Validation of an Analytical Procedure
5-3 Standard Addition
5-4 Internal Standards
Chapter 6 Good Titrations
Titration on Mars
6-1 Principles of Volumetric Analysis
6-2 Titration Calculations
6-3 Chemistry in a Fishtank
Box 6-1 Studying a Marine Ecosystem
6-4 Solubility Product
Box 6-2 The Logic of Approximations
6-5 Titration of a Mixture
6-6 Titrations Involving Silver Ion
Demonstration 6-1 Fajans Titration
Titration on Mars
6-1 Principles of Volumetric Analysis
6-2 Titration Calculations
6-3 Chemistry in a Fishtank
Box 6-1 Studying a Marine Ecosystem
6-4 Solubility Product
Box 6-2 The Logic of Approximations
6-5 Titration of a Mixture
6-6 Titrations Involving Silver Ion
Demonstration 6-1 Fajans Titration
Chapter 7 Gravimetric and Combustion Analysis
The Geologic Time Scale and Gravimetric Analysis
7-1 Examples of Gravimetric Analysis
Box 7-1 Shorthand for Organic Structures
7-2 Precipitation
Demonstration 7-1 Colloids, Dialysis, and Microdialysis
7-3 Examples of Gravimetric Calculations
7-4 Combustion Analysis
The Geologic Time Scale and Gravimetric Analysis
7-1 Examples of Gravimetric Analysis
Box 7-1 Shorthand for Organic Structures
7-2 Precipitation
Demonstration 7-1 Colloids, Dialysis, and Microdialysis
7-3 Examples of Gravimetric Calculations
7-4 Combustion Analysis
Chapter 8 Introducing Acids and Bases
Acid Rain
8-1 What Are Acids and Bases?
8-2 Relation Between [H+], [OH-], and pH
8-3 Strengths of Acids and Bases
Demonstration 8-1 HCl Fountain
8-4 pH of Strong Acids and Bases
8-5 Tools for Dealing with Weak Acids and Bases
8-6 Weak-Acid Equilibrium
Box 8-1 Quadratic Equations
Demonstration 8-2 Acid Rain Chemistry
8-7 Weak-Base Equilibrium
Chapter 9 Buffers
Measuring pH of Natural Waters with Acid-Base Indicators
9-1 What You Mix Is What You Get
9-2 The Henderson-Hasselbalch Equation
9-3 A Buffer in Action
Box 9-1 Strong Plus Weak Reacts Completely
Demonstration 9-1 How Buffers Works
9-4 Preparing Buffers
9-5 Buffer Capacity
9-6 How Acid-Base Indicators Work
Demonstration 9-2 Indicators and Carbonic Acid
Box 9-2 The Secret of Carbonless Copy Paper
Acid Rain
8-1 What Are Acids and Bases?
8-2 Relation Between [H+], [OH-], and pH
8-3 Strengths of Acids and Bases
Demonstration 8-1 HCl Fountain
8-4 pH of Strong Acids and Bases
8-5 Tools for Dealing with Weak Acids and Bases
8-6 Weak-Acid Equilibrium
Box 8-1 Quadratic Equations
Demonstration 8-2 Acid Rain Chemistry
8-7 Weak-Base Equilibrium
Chapter 9 Buffers
Measuring pH of Natural Waters with Acid-Base Indicators
9-1 What You Mix Is What You Get
9-2 The Henderson-Hasselbalch Equation
9-3 A Buffer in Action
Box 9-1 Strong Plus Weak Reacts Completely
Demonstration 9-1 How Buffers Works
9-4 Preparing Buffers
9-5 Buffer Capacity
9-6 How Acid-Base Indicators Work
Demonstration 9-2 Indicators and Carbonic Acid
Box 9-2 The Secret of Carbonless Copy Paper
Chapter 10 Acid-Base Titrations
Kjeldahl Nitrogen Analysis: Chemistry Behind the Headlines
10-1 Titration of Strong Base with Strong Acid
10-2 Titration of Weak Acid with Strong Base
10-3 Titration of Weak Base with Strong Acid
10-4 Finding the End Point
10-5 Practical Notes
10-6 Kjeldahl Nitrogen Analysis
10-7 Putting Your Spreadsheet to Work
Reference Procedure: Preparing standard acid and base
Kjeldahl Nitrogen Analysis: Chemistry Behind the Headlines
10-1 Titration of Strong Base with Strong Acid
10-2 Titration of Weak Acid with Strong Base
10-3 Titration of Weak Base with Strong Acid
10-4 Finding the End Point
10-5 Practical Notes
10-6 Kjeldahl Nitrogen Analysis
10-7 Putting Your Spreadsheet to Work
Reference Procedure: Preparing standard acid and base
Chapter 11 Polyprotic Acids and Bases
Carbon Dioxide in the Air
11-1 Amino Acids Are Polyprotic
11-2 Finding the pH in Diprotic Systems
Box 11-1 Carbon Dioxide in the Ocean
11-3 Which Is the Principal Species?
11-4 Titrations in Polyprotic Systems
Box 11-2 What is Isoelectric Focusing?
Carbon Dioxide in the Air
11-1 Amino Acids Are Polyprotic
11-2 Finding the pH in Diprotic Systems
Box 11-1 Carbon Dioxide in the Ocean
11-3 Which Is the Principal Species?
11-4 Titrations in Polyprotic Systems
Box 11-2 What is Isoelectric Focusing?
Chapter 12 A Deeper Look at Chemical Equilibrium
Chemical Equilibrium in the Environment
12-1 The Effect of Ionic Strength on Solubility of Salts
Demonstration 12-1 Effect of Ionic Strength on Ion Dissociation
12-2 Activity Coefficients
12-3 Charge and Mass Balances
12-4 Systematic Treatment of Equilibrium
Box 12-1 Aluminum Mobilization From Minerals by Acid Rain
12-5 Fractional Composition Equations
Chemical Equilibrium in the Environment
12-1 The Effect of Ionic Strength on Solubility of Salts
Demonstration 12-1 Effect of Ionic Strength on Ion Dissociation
12-2 Activity Coefficients
12-3 Charge and Mass Balances
12-4 Systematic Treatment of Equilibrium
Box 12-1 Aluminum Mobilization From Minerals by Acid Rain
12-5 Fractional Composition Equations
Chapter 13 EDTA Titrations
Chelation Therapy and Thalassemia
13-1 Metal-Chelate Complexes
13-2 EDTA
Box 13-2 Notation for Formation Constants
13-3 Metal Ion Indicators
Demonstration 13-1 Metal Ion Indicator Color Changes
13-4 EDTA Titration Techniques
Box 13-3 What Is Hard Water?
13-5 The pH-Dependent Metal-EDTA Equilibrium
13-6 EDTA Titration Curves
Chelation Therapy and Thalassemia
13-1 Metal-Chelate Complexes
13-2 EDTA
Box 13-2 Notation for Formation Constants
13-3 Metal Ion Indicators
Demonstration 13-1 Metal Ion Indicator Color Changes
13-4 EDTA Titration Techniques
Box 13-3 What Is Hard Water?
13-5 The pH-Dependent Metal-EDTA Equilibrium
13-6 EDTA Titration Curves
Chapter 14 Electrode Potentials
Lithium-Ion Battery
14-1 Redox Chemistry and Electricity
Demonstration 14-1 Electrochemical Writing
14-2 Galvanic Cells
Demonstration 14-2 The Human Salt Bridge
14-3 Standard Potentials
Box 14-1 Why Biochemist Use E°
Lithium-Ion Battery
14-1 Redox Chemistry and Electricity
Demonstration 14-1 Electrochemical Writing
14-2 Galvanic Cells
Demonstration 14-2 The Human Salt Bridge
14-3 Standard Potentials
Box 14-1 Why Biochemist Use E°
14-4 The Nernst Equation
14-5 E° and the Equilibrium Constant
14-6 Reference Electrodes
14-5 E° and the Equilibrium Constant
14-6 Reference Electrodes
Chapter 15 Electrode Measurements
How Perchlorate Was Discovered on Mars
15-1 The Silver Indicator Electrode
Demonstration 15-1 Potentiometry with an Oscillating Reaction
15-2 What Is a Junction Potential?
15-3 How Ion-Selective Electrodes Work
15-4 pH Measurement with a Glass Electrode
Box 15-1 Systematic Error in Rainwater pH Measurement
15-5 Ion-Selective Electrodes
Box 15-2 Ammonium Ion-Selective Microelectrode
Box 15-3 Protein Immunosensing by Ion-Selective Electrodes with Electrically Conductive Polymers
How Perchlorate Was Discovered on Mars
15-1 The Silver Indicator Electrode
Demonstration 15-1 Potentiometry with an Oscillating Reaction
15-2 What Is a Junction Potential?
15-3 How Ion-Selective Electrodes Work
15-4 pH Measurement with a Glass Electrode
Box 15-1 Systematic Error in Rainwater pH Measurement
15-5 Ion-Selective Electrodes
Box 15-2 Ammonium Ion-Selective Microelectrode
Box 15-3 Protein Immunosensing by Ion-Selective Electrodes with Electrically Conductive Polymers
Chapter 16 Redox Titrations
High-Temperature Superconductors
Box 16-1 Environmental Carbon Analysis and Oxygen Demand
16-1 Theory of Redox Titrations
Demonstration 16-1 Potentiometric Titration of Fe2+ with MnO-4
16-2 Redox Indicators
16-3 Titrations Involving Iodine
Box 16-2 Disinfecting Drinking Water with Iodine
High-Temperature Superconductors
Box 16-1 Environmental Carbon Analysis and Oxygen Demand
16-1 Theory of Redox Titrations
Demonstration 16-1 Potentiometric Titration of Fe2+ with MnO-4
16-2 Redox Indicators
16-3 Titrations Involving Iodine
Box 16-2 Disinfecting Drinking Water with Iodine
Chapter 17 Instrumental Methods in Electrochemistry
A Biosensor for Personal Glucose Monitoring
17-1 Electrogravimetric and Coulometric Analysis
17-2 Amperometry
17-3 Voltammetry
17-4 Polarography
A Biosensor for Personal Glucose Monitoring
17-1 Electrogravimetric and Coulometric Analysis
17-2 Amperometry
17-3 Voltammetry
17-4 Polarography
Chapter 18 Let There Be Light
The Ozone Hole
18-1 Properties of Light
18-2 Absorption of Light
Box 18-1 Discovering Beers Law
Demonstration 18-1 Absorption Spectra
18-3 Practical Matters
18-4 Using Beers Law
Box 18-2 Designing a Colorimetric Reagent to Detect Phosphate
The Ozone Hole
18-1 Properties of Light
18-2 Absorption of Light
Box 18-1 Discovering Beers Law
Demonstration 18-1 Absorption Spectra
18-3 Practical Matters
18-4 Using Beers Law
Box 18-2 Designing a Colorimetric Reagent to Detect Phosphate
Chapter 19 Spectrophotometry: Instruments and Applications
Flu Virus Identification with an RNA Array and Fluorescent Markers
19-1 The Spectrophotometer
19-2 Analysis of a Mixture
19-3 Spectrophotometric Titrations
19-4 What Happens When a Molecules Absorbs Light?
Demonstration 19-1 In Which Your Class Really Shines
19-5 Luminescence in Analytical Chemistry
Box 19-1 How Does a Home Pregnancy Test Work?
Flu Virus Identification with an RNA Array and Fluorescent Markers
19-1 The Spectrophotometer
19-2 Analysis of a Mixture
19-3 Spectrophotometric Titrations
19-4 What Happens When a Molecules Absorbs Light?
Demonstration 19-1 In Which Your Class Really Shines
19-5 Luminescence in Analytical Chemistry
Box 19-1 How Does a Home Pregnancy Test Work?
Chapter 20 Atomic Spectroscopy
Historical Record of Mercury in the Snow Pack
20-1 What is Atomic Spectroscopy?
Box 20-1 Atomic Emission Spectroscopy on Mars
20-2 Atomization: Flames, Furnaces, and Plasmas
20-3 How Temperature Affects Atomic Spectroscopy
20-4 Instrumentation
20-5 Interference
20-6 Inductively Coupled Plasma–Mass Spectrometry
Chapter 21 Principles of Chromatography and Mass Spectrometry
Bisphenol A
21-1 What is Chromatography?
21-2 How We Describe a Chromatogram
21-3 Why Do Bands Spread?
Box 21-1 Polarity
21-4 Mass Spectrometry
Box 21-2 Volatile Flavor Components of Candy
Box 21-3 Bisphenol A in Canned Foods
21-5 Information in a Mass Spectrum
Historical Record of Mercury in the Snow Pack
20-1 What is Atomic Spectroscopy?
Box 20-1 Atomic Emission Spectroscopy on Mars
20-2 Atomization: Flames, Furnaces, and Plasmas
20-3 How Temperature Affects Atomic Spectroscopy
20-4 Instrumentation
20-5 Interference
20-6 Inductively Coupled Plasma–Mass Spectrometry
Chapter 21 Principles of Chromatography and Mass Spectrometry
Bisphenol A
21-1 What is Chromatography?
21-2 How We Describe a Chromatogram
21-3 Why Do Bands Spread?
Box 21-1 Polarity
21-4 Mass Spectrometry
Box 21-2 Volatile Flavor Components of Candy
Box 21-3 Bisphenol A in Canned Foods
21-5 Information in a Mass Spectrum
Chapter 22 Gas and Liquid Chromatography
Protein Electrospray
22-1 Gas Chromatography
22-2 Classical Liquid Chromatography
22-3 High-Performance Liquid Chromatography
22-4 Sample Preparation for Chromatography
Protein Electrospray
22-1 Gas Chromatography
22-2 Classical Liquid Chromatography
22-3 High-Performance Liquid Chromatography
22-4 Sample Preparation for Chromatography
Chapter 23 Chromatographic Methods and Capillary Electrophoresis
Chromated Copper Arsenate Wood Preservative
23-1 Ion-Exchange Chromatography
Box 23-1 Applications of Ion Exchange
23-2 Ion Chromatography
23-3 Molecular Exclusion Chromatography
23-4 Affinity Chromatography
23-5 What is Capillary Electrophoresis?
23-6 How Capillary Electrophoresis Works
23-7 Types of Capillary Electrophoresis
Box 23-2 What is a Micelle?
Chromated Copper Arsenate Wood Preservative
23-1 Ion-Exchange Chromatography
Box 23-1 Applications of Ion Exchange
23-2 Ion Chromatography
23-3 Molecular Exclusion Chromatography
23-4 Affinity Chromatography
23-5 What is Capillary Electrophoresis?
23-6 How Capillary Electrophoresis Works
23-7 Types of Capillary Electrophoresis
Box 23-2 What is a Micelle?
23-8 Lab on a Chip: DNA Profiling
Glossary
Appendix A: Solubility Products
Appendix B: Acid Dissociation Constants
Appendix C: Standard Reduction Potentials
Appendix D: Oxidation Numbers and Balancing Redox Equations
Solutions to "Ask Yourself" Questions
Answers to Problems
Index
Daniel C. Harris
Dan Harris was born in Brooklyn, NY in 1948. He earned degrees in Chemistry from MIT in 1968 and Caltech 1973 and was a postdoc at Albert Einstein College of Medicine in New York. After teaching at the University of California at Davis from 1975-1980 and at Franklin and Marshall College from 1980-1983, he moved to the Naval Air Systems Command at China Lake, California, where he is now a Senior Scientist and Esteemed Fellow. While teaching analytical chemistry at Davis, he wrote his lectures in bound form for his students. This volume caught the attention of publishers representatives wandering through the college bookstore. The first edition of Quantitative Chemical Analysis was published in 1982. The first edition of Exploring Chemical Analysis came out in 1996. Both have undergone regular revision. Dan is also co-author of Symmetry and Spectroscopy published in 1978 by Oxford University Press and now available from Dover Press. His book Materials for Infrared Windows and Domes was published by SPIE press in 1999. Dan and his wife Sally were married in 1970. They have two children and four grandchildren. Sallys work on every edition of the books is essential to their quality and accuracy.
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