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Quantitative Chemical Analysis

Ninth Edition ©2016 Daniel C. Harris

The gold standard in analytical chemistry, Dan Harris’ Quantitative Chemical Analysis provides a sound physical understanding of the principles of analytical chemistry and their applications in the disciplines.
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Look Inside Look Inside Quantitative Chemical Analysis by Daniel C. Harris - Ninth Edition, 2016 from Macmillan Student Store

The gold standard in analytical chemistry, Dan Harris’ Quantitative Chemical Analysis provides a sound physical understanding of the principles of analytical chemistry and their applications in the disciplines.

Features

New to This Edition

New Contributing Author: Chuck Lucy, University of Alberta
Lucy has made significant updates to:
Ch. 23 Introduction to Analytical Separations
Ch. 24 Gas Chromatrography
Ch. 25 High-Performance Liquid Chromatography
Ch. 26 Chromatographic Methods and Capillary Electrophoresis


Chapter 7. Let the Titrations Begin
In the previous edition, titrations coverage was dispersed across several chapters. Based on instructor feedback, that coverage is again brought together in a single dedicated chapter.


Content Update Highlights (see Table of Contents for a more detailed summary of content changes)

  • New discussion of atomic weights and their uncertainty based on 2009 IUPAC report on atomic weights (Ch. 3, Experimental Error)

  • New approach to numerical solution of systematic equilibrium problems with spreadsheets (Ch. 8, Activity and the Systematic Treatment of Equilibrium)

  • New opener: Acid-Base Titration of RNA (Ch. 11, Acid-Base Titrations)

  • New opener: DNA sequencing (Ch. 15, Electrodes and Potentiometry)

  • New opener on doping in sports. (Ch. 24, Gas Chromatography)

  • New opener on DNA profiling and new coverage of a DNA profiling lab on a chip (Ch. 26, Chromatographic Methods and Capillary Electrophoresis)

  • New discussion of nucleation from recent literature was added (Ch. 27, Gravimetric and Combustion Analysis)

  • Extensive new discussion of propagation of uncertainty following recommendations of Joint Committee for Guides in Metrology 2008/2010 (Appendix B)

  • New appendix describes structure of DNA and RNA (Appendix L)


New and Updated Applications

Box 3-2 Certified Reference Materials (new)

Box 3-3 Atomic Masses of the Elements (new)

Box 5-1 Medical Implication of False Positive Results (new)

Box 10-3 Microequilibrium Constants (new)

Box 11-2 What Does a Negative pH Mean? (updated)

Box 11-3 Kjeldahl Nitrogen Analysis Behind the Headlines (updated)

Box 14-1 Ohm’s Law, Conductance, and Molecular Wire (updated)

Box 14-2 Hydrogen-Oxygen Fuel Cell (new) features Apollo 13 fuel cell accident (new)

Box 14-3 Lead-Acid Battery (new)

Box 15-3 How Was Perchlorate Discovered on Mars? (new)

Box 15-4 Ion-Selective Electrode with Electrically Conductive Polymer for a Sandwich Immunoassay (new)

Box 17-1 Metal Reactions at Atomic Steps (new)

Box 17-5 Aptamer Biosensor for Clinical Use (new)

Box 18-4 Designing a Molecule for Fluorescence Detection (new)

Box 19-2 Upconversion (updated)

Box 21-2 Measuring Sodium with a Bunsen Burner Photometer (new)

Box 21-3 Atomic Emission Spectroscopy on Mars (new)

Box 22-3 Isotope Ratio Mass Spectrometry and Dinosaur Body Temperature (updated)

Box 22-5 Making Elephants Fly (Mechanisms of Protein Electrospray)

Box 24-3 Two-Dimensional Gas Chromatography (new)

Box 25-1 One-Million-Plate Colloidal Crystal Columns Operating by Slip Flow (new)

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Table of Contents

0 The Analytical Process

Opened the first chapter with description of home pregnancy test.

Historical section on measurement of atmospheric CO2 by Keeling was removed

1 Chemical Measurements

Discussion of limiting reagent added to Chap 1

2 Tools of the Trade

Reduced discussion of mechanical balance.

Added serial dilution and more emphasis on relative uncertainty of volumetric apparatus

3 Experimental Error

New discussion of atomic weights and their uncertainty based on 2009 IUPAC report on atomic weights. See new Box 3-3 for my handling of atomic weights.

Rectangular and triangular distributions could not be treated rigorously in Chapter 3, so they were moved to Appendix B with a NEW discussion of propagation of uncertainty

Appendix B: Extensive new discussion of propagation of uncertainty following recommendations of Joint Committee for Guides in Metrology 2008/2010

4 Statistics

F test was moved ahead of t test so F could be used for t.

Amplified discussion of hypothesis testing.

Increased distinction between standard error (standard deviation of the mean) and standard deviation (for use in Appendix B)

5 Quality Assurance and Calibration Methods

New box on Medical Implication of False Positive Results.

Graph for internal standards introduced. Efficiency in experimental design moved to Appendix C

6 Chemical Equilibrium

Modified discussion of entropy plus other minor revisions

7 Let the Titrations Begin

Chapter was reconstituted and slightly revised from QCA 7e.

New Opener – Titration on Mars.

Experimental detail added for Volhardt titration. New problem 7-36 asks "What is wrong with this procedure?"

8 Activity and the Systematic Treatment of Equilibrium

Fundamental change: new approach to numerical solution of systematic equilibrium problems with spreadsheets was implemented in Section 8-5. One exercise and 8 new problems were added to illustrate the new approach.

New color plate added.

9 Monoprotic Acid-Base Equilibria

Enhanced discussion and problems on practical use of buffer

10 Polyprotic Acid-Base Equilibria

New Opener on CO2 in air.

Enhanced Box on CO2 in ocean.

New Box on microequilibrium constants.

New problem 10-9 gives powerful spreadsheet approach to iterative calculation of pH of intermediate form of diprotic acid

11 Acid-Base Titrations

New opener: Acid-Base Titration of RNA

12 EDTA Titrations

Chelation therapy moved to chapter opener from former Box.

13 Advanced Topics in Equilibrium

Advanced equilibrium implements new spreadsheet approach from Chap 8.

Circular definition in spreadsheet automatically finds ionic strength and activity coefficients without manual iteration.

14 Fundamentals of Electrochemistry

Revised discussion throughout chapter to note that electrons flow from less positive to more positive potential.

Fundamental equations were modified to distinguish n = units of charge and N = moles in the formulas q = nNF and G = nNFE.

Added figure emphasizing that potential changes at phase boundaries.

New Box 14-2 on H2-O2 fuel cell in Apollo 13 spacecraft and new Box 14-3 on lead-acid battery.

15 Electrodes and Potentiometry

There is a new Opener on DNA sequencing, new discussion of ways to reduce the detection limit for ion-selective electrodes and the use of ion-selective electrodes to measure dissolved CO2.

Box 15-3 describes the discovery of perchlorate on Mars

Box 15-4 describes an ion-selective electrode with an electrically conductive polymer for an immunoassay.

16 Redox Titrations

Added environmentally safe alternative for enzymatic pre-reduction of nitrate.

Added dissolved O2 analysis with Winkler titration in Problem 16-28.

17 Electroanalytical Techniques

New Figure 17-7 describes measurement of Ohmic potential with a Luggin capillary. Box 17-1 introduces reactions at atomic steps on a crystal surface. The application of a glucose electrode to measure other analytes is described.

Voltammetry of double strand DNA and stripping analysis of perchlorate with a conductive polymer electrode in Figure 17-26 are new.

Figure 17-32 explains why sigmoidal voltammograms are observed with microelectrodes.

Box 17-5 on aptamers is new.

18 Fundamentals of Spectrophotometry

Section 18-4 now includes an example of preparing standard iron solution and an example of serial dilution.

New problems 18-23, -24, and -25 deal with preparation of standards and serial dilution.

Box 18-2 is updated with a discussion of Hg in fluorescent bulbs and Hg emission from burning coal.

Box 18-4 describes designing a molecule for fluorescence detection.

19 Applications of Spectrophotometry

Figure 19-1 (b) was simplified for clarity.

Figure 19-5 provides data for analysis of a mixture with Excel Solver in Problem 19-8.

Figure 19-7 provides data for curve fitting to find an equilibrium constant with Solver in Figure 19-8.

Exercise 19-C deals with finding and equilibrium constant with Solver.

A new immunoassay for Hg was added to Section 19-5.

Box 19-1 is updated for a dye-sensitized photocell and a solid-state perovskite photocell.

20 Spectrophotometers

Box 20-1 is updated with solar radiation and global temperature data from 2013. Section 20-3 describes an image intensifier in Figure 20-18 and mentions photoacoustic detection described in Box 20-3. Section 20-6 has new Figure 20-35 showing the limits of signal averaging and a new section on Savitzky-Golay polynomial smoothing. Problem 20-38 applies polynomial smoothing.

21 Atomic Spectroscopy

Box 21-2 uses Bunsen burner photometer to illustrate atomic emission.

Laser ablation was separated into a separate section with atomic emission on Mars as an application.

For inductively coupled plasma, dynamic reaction cell replaced collision cell. Added new section on X-ray fluorescence including spectral interpretation.

22 Mass Spectroscopy

Amplified discussion of halogen isotopic peaks. Back cover of book and Chap 22 relate dinosaur body temperature to isotope ratio measurements. Expanded discussion of time-of-flight spectrometer and added examples of orbitrap capability for mass accuracy. Added direct electron ionization and photoionizaiton liquid chromatography‒mass spectrometry interfaces. Updated application of selected reaction monitoring. Added field-portable spectrometry. Enhanced ion mobility section with addition of field asymmetric waveform spectrometry and traveling wave ion mobility state inside a mass spectrometer.

23 Introduction to Analytical Separations

Contributor Chuck Lucy made principal revisions.

New opener on chromatography of components of milk.

New color plate illustrates mechanism of chromatography by partition of solute between immiscible phases.

Updated section on efficiency of separation.

Added illustration on effects of N, α, and k on plate height.

Added band broadening in connective tubing.

Improved illustrations of mechanisms of band broadening with more emphasis on mass transfer.

Distinguished effects of overloading in gas and liquid chromatography.

Added 6 problems with emphasis on conceptual understanding.

24 Gas Chromatrography

Contributor Chuck Lucy made principal revisions.

New opener on doping in sports.

Added 2-dimensional chromatography.

More emphasis on column selectivity and factors affecting retention by columns. New examples in chiral separation and chromatography on a chip.

Added headspace extraction, olfactometric detection, and vacuum ultraviolet detection.

Added 9 new problems including qualitative questions and two literature search problems.

25 High-Performance Liquid Chromatography

Contributor Chuck Lucy made principal revisions.

Enhanced discussion of types of polarity for liquid chromatography, van Deemter terms for fused-core particles, HILIC, sample injection, method development for reversed-phase chromatography, selecting pH for separations, gradient separations.

New table compares HPLC and UHPLC.

New table of solvent properties includes types of polarity.

Box 25-1 introduces slip flow chromatography.

Box 25-3 shows solvent gradient in supercritical fluid chromatography.

Added 7 problems include two requiring literature search

26 Chromatographic Methods and Capillary Electrophoresis

Contributor Chuck Lucy made principal revisions.

DNA profiling opener and DNA profiling lab on a chip Section 26-8 are new. Ion exchange equivalents introduced.

Donnan exclusion reduced to qualitative discussion.

Speciation introduced in ion chromatography.

Mixed mode retention in ion-pair chromatography introduced.

Improved graphic of size exclusion separations.

Electrophoresis has more emphasis on effect of size on ion mobility and effect of pH on mobility of weak acids.

27 Gravimetric and Combustion Analysis

New discussion of nucleation from recent literature was added.

New Figure 27-2 shows onset of crystallization from amorphous particle.

New Figure 27-4 shows effect of electrolyte concentration on particle repulsion.

28 Sample Preparation

Added color plate on solid-phase extraction.

Added dispersive liquid-liquid extraction, solid-supported liquid-liquid extraction, and QuEChERS sample preparation

Notes and References

Glossary

Appendices

Solutions to Exercises

Answers to Problems

Index

Experiments

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.  Sally's work on every edition of the books is essential to their quality and accuracy.

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Daniel Harris | Ninth Edition | ©2016 | ISBN:9781319343538

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