Quantitative Chemical Analysis / Edition 7

Quantitative Chemical Analysis / Edition 7

by Daniel C. Harris
     
 

This text provides an understanding of the principles of analytic chemistry and shows how these principles are applied in chemistry and related disciplines, especially in the life and environmental sciences. Written to be accessible to nonmajors yet detailed enough for advanced undergraduates, this sixth edition of the text contains new chapters on mass spectrometry… See more details below

Overview

This text provides an understanding of the principles of analytic chemistry and shows how these principles are applied in chemistry and related disciplines, especially in the life and environmental sciences. Written to be accessible to nonmajors yet detailed enough for advanced undergraduates, this sixth edition of the text contains new chapters on mass spectrometry and quality assurance, and moves experiments from the book to a web site. Integrated coverage of spreadsheets is new to this edition, and there is updated material on the F test for comparing variance, pH dependence of solubility, and Gran plots. Harris is affiliated with Michelson Laboratory. Annotation ©2004 Book News, Inc., Portland, OR

Product Details

ISBN-13:
9780716770411
Publisher:
Freeman, W. H. & Company
Publication date:
05/12/2006
Edition description:
Seventh Edition
Pages:
1008
Product dimensions:
9.46(w) x 11.03(h) x 1.42(d)

Table of Contents

0  The Analytical Process
Opener:  The “Most Important” Environmental Data Set of the 20th Century
0-1  Charles David Keeling and the Measurement of Atmospheric CO2
0-2  The Analytical Chemist's Job
0-32  General Steps in a Chemical Analysis
Box 0-1  Constructing a Representative Sample
1  Chemical Measurements
Opener:  Biochemical Measurements with a Nanoelectrode
1-1  SI Units
1-2  Chemical Concentrations
1-3  Preparing Solutions
1-4  Stoichiometry Calculations for Gravimetric Analysis
7-1  Introduction to Titrations
Box 1-1    Reagent Chemicals and Primary Standards
7-2  Titration Calculations
2  Tools of the Trade
Opener:  Quartz Crystal Microbalance in Medical Diagnosis
2-1  Safe, Ethical Handling of Chemicals and Waste
2-2  The Lab Notebook
2-3  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  Introduction to Microsoft Excel®
2-11  Graphing with Microsoft Excel®
Reference Procedure:  Calibrating a 50-mL Buret
3  Experimental Error
Opener:  Experimental Error
3-1  Significant Figures
3-2  Significant  Figures in Arithmetic
3-3  Types of Error
Box 3-1  Case Study in Ethics:  Systematic Error in Ozone Measurement
3-4  Propagation of Uncertainty from Random Error
Box 3-2  Keeling’s Exquisitely Precise Measurement of CO2
3-5  Propagation of Uncertainty from Systematic Error
4  Statistics
Opener:  Is My Red Blood Cell Count High Today?
4-1  Gaussian Distribution
4-2  Confidence Intervals
4-3  Comparison of Means with Student's t
Box 4-1  Choosing the Null Hypothesis in Epidemiology
4-4   F Test
4-5   t Tests with a Spreadsheet
4-6  Grubbs Test for an Outlier
4-7.  The Method of Least Squares
4-8  Calibration Curves
Box 4-2  Using a Nonlinear Calibration Curve
4-9  A Spreadsheet for Least Squares
5  Quality Assurance and Calibration Methods
Opener:  The Need for Quality Assurance
5-1  Basics of Quality Assurance
Box 5-1  Control Charts
5-2   Method Validation
Box 5-2   The Horwitz Trumpet:  Variation in Interlaboratory Precision
5-3  Standard Addition
5-4  Internal Standards
5-5  Efficiency in Experimental Design
6  Chemical Equilibrium
Opener:  Chemical Equilibrium in the Environment
6-1  The Equilibrium Constant
6-2  Equilibrium and Thermodynamics
6-3  Solubility Product
Box 6-1  Solubility is Governed by More than the Solubility Product
Demonstration 6-1   Common Ion Effect
6-4  Complex Formation
Box 6-2  Notation for Formation Constants
6-5  Protic Acids and Bases
6-6  pH
6-7  Strengths of Acids and Bases
Demonstration 6-2   The HCl Fountain
Box 6-3  The Strange Behavior of Hydrofluoric Acid
Box 6-4  Carbonic Acid
7   Activity and the Systematic Treatment of Equilibrium
Opener:  Hydrated Ions
7-1  The Effect of Ionic Strength on Solubility of Salts
Demonstration 7-1   Effect of Ionic Strength on Ion Dissociation
Box 7-1   Salts with Ions of Charge =|2| Do Not Fully Dissociate
7-2  Activity Coefficients
7-3  pH Revisited
7-4  Systematic Treatment of Equilibrium
Box 7-2   Calcium Carbonate Mass Balance in Rivers
7-5  Applying the Systematic Treatment of Equilibrium
8  Monoprotic Acid-Base Equilibria
Opener:  Measuring pH Inside Cellular Compartments
8-1  Strong Acids and Bases
Box 8-1   Concentrated HNO3 is Only Slightly Dissociated
8-2  Weak Acids and Bases
8-3  Weak-Acid Equilibria
Demonstration 8-1   Conductivity of Weak Electrolytes
Box 8-2   Dyeing Fabrics and the Fraction of Dissociation
8-4  Weak-Base Equilibria
8-5  Buffers
Box 8-3   Strong Plus Weak Reacts Completely
Demonstration 8-2   How Buffers Work
9  Polyprotic Acid-Base Equilibria
Opener:  Proteins are Polyprotic Acids and Bases
9-1  Diprotic Acids and Bases
Box 9-1  Carbon Dioxide in the Air and Ocean (new)
Box 9-2  Successive Approximations
9-2  Diprotic Buffers
9-3  Polyprotic Acids and Bases
9-4  Which Is the Principal Species?
9-5  Fractional Composition Equations
9-6  Isoelectric and Isoionic pH
Box 9-3  Isoelectric Focusing
10  Acid-Base Titrations
Opener:  Acid-Base Titration of a Protein
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  Titrations in Diprotic Systems
10-5  Finding the End Point with a pH Electrode
Box 10-1     Alkalinity and Acidity
10-6  Finding the End Point with Indicators
Demonstration 10-1     Indicators and the Acidity of CO2
Box 10-2  What Does a Negative pH Mean?
10-7  Practical Notes
10-8  Kjeldahl Nitrogen Analysis
Box 10-3  Kjeldahl Nitrogen Analysis Behind the Headline
10-9  Leveling Effect
10-10  Calculating Titration Curves with Spreadsheets
Reference Procedure:  Preparing Standard Acid and Base
11  EDTA Titrations
Opener:  Ion Channels in Cell Membranes
11-1  Metal-Chelate Complexes
Box 11-1   Chelation Therapy and Thalassemia
11-2  EDTA
11-3  EDTA Titration Curves
11-4  Do It with a Spreadsheet
11-5  Auxiliary Complexing Agents
Box 11-2   Metal Ion Hydrolysis Decreases the Effective Formation Constant for
 EDTA Complexes
11-6  Metal Ion Indicators
Demonstration 13-1   Metal Ion Indicator Color Changes
11-7  EDTA Titration Techniques
Box 11-3   Water Hardness
12   Advanced Topics in Equilibrium
Opener:  Acid Rain
12-1  General Approach to Acid-Base Systems
12-2  Activity Coefficients
12-3  Dependence of Solubility on pH
12-4  Analyzing Acid-Base Titrations with Difference Plots
13  Fundamentals of Electrochemistry
Opener:  Lithium-Ion Battery
13-1  Basic Concepts
Box 13-1   Ohm’s Law, Conductance, and Molecular Wire
13-2  Galvanic Cells
Demonstration 13-1   The Human Salt Bridge
13-3  Standard Potentials
13-4  Nernst Equation
Box 13-2   E° and the Cell Voltage Do Not Depend on How You Write the Cell Reaction
Box 13-3   Latimer Diagrams:  How to Find E° for a New Half-Reaction
13-5  E° and the Equilibrium Constant
Box 13-4   Concentrations in the Operating Cell
13-6  Cells as Chemical Probes
13-7  Biochemists Use E°'
14  Electrodes and Potentiometry
Opener:  Chem Lab on Mars
14-1  Reference Electrodes
14-2  Indicator Electrodes
Demonstration 14-1  Potentiometry with an Oscillating Reaction
14-3  What Is a Junction Potential?
14-4  How Ion-Selective Electrodes Work
14-5  pH Measurement with a Glass Electrode
Box 14-1  Systematic Error in Rainwater pH Measurement  The Effect of Junction Potential
14-6  Ion-Selective Electrodes
Box 14-2  Measuring Selectivity Coefficients for an Ion-Selective Electrode (new)
Box 14-3  How Was Perchlorate Discovered on Mars? (new)
14-7  Using Ion-Selective Electrodes
14-8  Solid-State Chemical Sensors
15  Redox Titrations
Opener:  Chemical Analysis of High-Temperature Superconductors
15-1  The Shape of a Redox Titration Curve
Box 15-1   Many Redox Reactions are Atom-Transfer Reactions
Demonstration 15-1   Potentiometric Titration of Fe2+ with MnO4-
15-2  Finding the End Point
15-3  Adjustment of Analyte Oxidation State
15-4  Oxidation with Potassium Permanganate
15-5  Oxidation with Ce4+
15-6  Oxidation with Potassium Dichromate
Box 15-2   Environmental Carbon Analysis and Oxygen Demand
15-7  Methods Involving Iodine
Box 15-3  Iodometric Analysis of High-Temperature Superconductors
16  Electroanalytical Techniques
Opener:  How Sweet It Is!
Demonstration 16-1   Electrochemical Writing
16-1  Fundamentals of Electrolysis
16-2  Electrogravimetric Analysis
16-3  Coulometry
16-4  Amperometry
Box 16-1   Clark Oxygen Electrode
Box 16-2   What Is an “Electronic Nose”?
16-5  Voltammetry
Box 16-3   The Electric Double Layer
16-6  Karl Fischer Titration of H2O
17  Fundamentals of Spectrophotometry
Opener:  The Ozone Hole
17-1  Properties of Light
17-2  Absorption of Light
Box 17-1   Why Is There a Logarithmic Relation Between Transmittance and Concentration?
Demonstration 17-1   Absorption Spectra
17-3  Measuring Absorbance
17-4  Beer's Law in Chemical Analysis
17-5  Spectrophotometric Titrations
17-6  What Happens When a Molecule Absorbs Light?
Box 17-2   Fluorescence All Around Us
17-7  Luminescence
Box 17-3   Rayleigh and Raman Scattering
18  Applications of Spectrophotometry
Opener:  Fluorescence Resonance Energy Transfer Biosensor
18-1  Analysis of a Mixture
18-2  Measuring an Equilibrium Constant:  The Scatchard Plot
18-3  The Method of Continuous Variation
18-4  Flow Injection Analysis and Sequential Injection
18-5  Immunoassays and Aptamers
18-6  Sensors Based on Luminescence Quenching
Box 18-1   Converting Light into Electricity
Box 18-2   Upconversion
19   Spectrophotometers
Opener:  Cavity Ring-Down Spectroscopy:  Do You Have an Ulcer?
19-1  Lamps and Lasers:  Sources of Light
Box 19-1   Blackbody Radiation and the Greenhouse Effect
19-2  Monochromators
19-3  Detectors
Box 19-2   The Most Important Photoreceptor
Box 19-3   Nondisperesive Infrared Measurement of CO2 on Mauna Loa
19-4  Optical Sensors
19-5  Fourier Transform Infrared Spectroscopy
19-6  Dealing with Noise
20  Atomic Spectroscopy
Opener:  An Anthropology Puzzle
20-1  An Overview
Box 20-1   Mercury Analysis by Cold Vapor Atomic Fluorescence
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
Box 20-2   GEOTRACES
21  Mass Spectrometry
Opener:  Droplet Electrospray
21-1  What Is Mass Spectrometry?
Box 21-1   Molecular Mass and Nominal Mass
Box 21-2   How Ions of Different Masses Are Separated by a Magnetic Field
21-2  Oh, Mass Spectrum, Speak to Me!
Box 21-3   Isotope Ratio Mass Spectrometry
21-3  Types of Mass Spectrometers
21-4  Chromatography–Mass Spectrometry
Box 21-4   Matrix-Assisted Laser Desorption/Ionization
21-5  Open-Air Sampling for Mass Spectrometry
22  Introduction to Analytical Separations
Opener:  Measuring Silicones Leaking from Breast Implants
22-1  Solvent Extraction
Demonstration 22-1   Extraction with Dithizone
Box 22-1   Crown Ethers and Phase Transfer Agents
22-2  What Is Chromatography?
22-3  A Plumber's View of Chromatography
22-4  Efficiency of Separation
22-5  Why Bands Spread
Box 22-2   Microscopic Description of Chromatography
23   Gas Chromatography
Opener:  What Did They Eat in the Year 1000?
23-1  The Separation Process in Gas Chromatography
Box 23-1   Chiral Phases for Separating Optical Isomers
Box 23-2   Chromatography Column on a Chip (new)
23-2  Sample Injection
23-3  Detectors
23-4  Sample Preparation
23-5  Method Development in Gas Chromatography
24  High-Performance Liquid Chromatography
Opener:  Paleothermometry:  How to Measure Historical Ocean Temperatures
24-1   The Chromatographic Process
Box 24-1   Monolithic Silica Columns
Box 24-2   Structure of the Solvent–Bonded Phase Interface
Box 24-3   “Green” Technology:  Supercritical Fluid Chromatography
24-2   Injection and Detection in HPLC
24-3   Method Development for Reversed-Phase Separations
24-4   Gradient Separations
24-5   Do it with a Computer!
Box 24-4   Choosing Gradient Conditions and Scaling Gradients
25  Chromatographic Methods and Capillary Electrophoresis
Opener:  Capillary Electrochromatography
25-1   Ion-Exchange Chromatography
25-2   Ion Chromatography
Box 25-1  Surfactants and Micelles
25-3   Molecular Exclusion Chromatography
25-4   Affinity Chromatography
Box 25-2  Molecular Imprinting
25-5   Hydrophobic Interaction Chromatography (new)
25-6   Principles of Capillary Electrophoresis
25-7   Conducting Capillary Electrophoresis
25-8   Lab-on-a-Chip:  Probing Brain Chemistry
26  Gravimetric Analysis, Precipitation Titrations, and Combustion Analysis
Opener:  The Geologic Time Scale and Gravimetric Analysis
26-1   Examples of Gravimetric Analysis
26-2   Precipitation
Demonstration 26-1   Colloids and Dialysis
26-3   Examples of Gravimetric Calculations
26-4   Combustion Analysis
26-5  Precipitation Titration Curves
26-6  Titration of a Mixture
26-7  Calculating Titration Curves with a Spreadsheet
26-8  End-Point Detection
Demonstration 26-2  Fajans Titration
27  Sample Preparation
Opener:  Cocaine Use?  Ask the River
27-1   Statistics of Sampling
27-2   Dissolving Samples for Analysis
27-3 Sample Preparation Techniques
 
Notes and References
Glossary
Appendices
A.  Logarithms and Exponents
B.  Graphs of Straight Lines
C.  Propagation of Uncertainty
 New material added
D.  Oxidation Numbers and Balancing Redox Equations
E.  Normality
F. Solubility Products
G.  Acid Dissociation Constants
H.  Standard Reduction Potentials
I.  Formation Constants
J.  Logarithm of the Formation Constant for the Reaction M(aq) + L(aq)   ML(aq)
K.  Analytical Standards
Solutions to Exercises
Answers to Problems
Index

Experiments
Experiments are found at the web site www.whfreeman.com/qca/
0. Green Chemistry
1. Calibration of Volumetric Glassware
2 Gravimetric Determination of Calcium as CaC2O4.H2O
3. Gravimetric Determination of Iron as Fe2O3
4. Penny Statistics
5. Statistical Evaluation of Acid-Base Indicators
6. Preparing Standard Acid and Base
7. Using a pH Electrode for an Acid-Base Titration
8. Analysis of a Mixture of Carbonate and Bicarbonate
9. Analysis of an Acid-Base Titration Curve: The Gran Plot
10. Fitting a Titration Curve with Excel Solver®
11. Kjeldahl Nitrogen Analysis
12. EDTA Titration of Ca2+ and Mg2+ in Natural Waters
13. Synthesis and Analysis of Ammonium Decavanadate
14. Iodimetric Titration of Vitamin C
15. Preparation and Iodometric Analysis of High-Temperature Superconductor
16. Potentiometric Halide Titration with Ag+
17. Electrogravimetric Analysis of Copper
18. Polarographic Measurement of an Equilibrium Constant
19. Coulometric Titration of Cyclohexene with Bromine
20. Spectrophotometric Determination of Iron in Vitamin Tablets
21. Microscale Spectrophotometric Measurement of Iron in Foods by Standard Addition
22. Spectrophotometric Measurement of an Equilibrium Constant
23. Spectrophotometric Analysis of a Mixture:  Caffeine and Benzoic Acid in a Soft Drink
24. Mn2+ Standardization by EDTA Titration
25. Measuring Manganese in Steel by Spectrophotometry with Standard Addition
26. Measuring Manganese in Steel by Atomic Absorption Using a Calibration Curve
27. Properties of an Ion-Exchange Resin
28. Analysis of Sulfur in Coal by Ion Chromatography
29. Measuring Carbon Monoxide in Automobile Exhaust by Gas Chromatography
30. Amino Acid Analysis by Capillary Electrophoresis
31. DNA Composition by High-Performance Liquid Chromatography
32. Analysis of Analgesic Tablets by High Performance Liquid Chromatography
33. Anion Content of Drinking Water by Capillary Electrophoresis
34. Green Chemistry:  Liquid Carbon Dioxide Extraction of Lemon Peel Oil
Spreadsheet Topics (Not yet Updated for 8e)
2-10 Introduction to Microsoft Excel
2-11 Graphing with Microsoft Excel
Problem 3-8 Controlling the appearance of a graph
4-1 Average, standard deviation, normal distribution
4-5 t-Test
4-7 Equation of a straight line
4-9 Spreadsheet for least squares
Problem 4-25 Adding error bars to a graph
5-2 Square of the correlation coefficient (R2)
Problem 5-14 Using TRENDLINE
6-8 Solving equations with Excel GOAL SEEK
7-6 Precipitation titration curves
7-8 Multiple linear regression and experimental design
8-5 Using GOAL SEEK in equilibrium problems
Problem 8-27 Circular reference
9-5 Excel GOAL SEEK and naming cells
11-9 Acid-base titration curves
12-4 EDTA titrations
Problem 12-18 Auxiliary complexing agents in EDTA titrations
Problem 12-20 Complex formation
13-1 Using Excel SOLVER
13-2 Activity coefficients with the Davies equation
13-4 Fitting nonlinear curves by least squares
13-4 Using Excel SOLVER for more than one unknown
19-1 Solving simultaneous equations with Excel SOLVER
19-1 Solving simultaneous equations by matrix inversion
Problem 24-29 Binomial distribution function for isotope patterns

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