Quantitative Chemical Analysis / Edition 8

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Overview

Chemical analysis is required for characterization and quality control in the manufacture of semiconductors, metals, plastics, paints, fabrics, fertilizers and nearly everything else that we use.
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Editorial Reviews

Booknews
New edition of a text that provides a sound physical understanding of the principles of analytical chemistry and shows how these principles are applied in chemistry and related disciplines, especially environmental and life sciences. Twenty-nine chapters discuss topics including laboratory operations, statistics, volumetric and gravimetric analysis, chemical and electrochemical equilibrium, acid- base chemistry, complex formation, electrochemical measurements, spectrophotometry, atomic spectroscopy, chromatography, and sample preparation. Includes a CD-ROM with supplementary discussions of topics not in the text, spreadsheet files, and practice problems. Annotation c. by Book News, Inc., Portland, Or.
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Product Details

  • ISBN-13: 9781429218153
  • Publisher: Freeman, W. H. & Company
  • Publication date: 4/30/2010
  • Edition description: Eighth Edition
  • Edition number: 8
  • Pages: 750
  • Sales rank: 77,135
  • Product dimensions: 9.20 (w) x 11.00 (h) x 1.60 (d)

Meet the Author

Biographical Statement for Nomination of Daniel C. Harris for J. Calvin Giddings Award for Excellence in Analytical Chemical Education

I was born in 1948 in Brooklyn, New York.  As a teenager, I enjoyed a science program on Saturdays at Columbia University, where I took note of especially good teaching by astronomy professor Lloyd Motz.  In my freshman year at Massachusetts Institute of Technology, excellent teaching of organic chemistry by Daniel S. Kemp diverted me from biochemistry to chemistry.  A spectroscopy class from George F. Whitesides led me to Whitesides and his student Chuck Casey (later President of the American Chemical Society) for senior thesis research.  I developed a strong consciousness for high quality teaching.  Two other classes with noteworthy teaching quality were quantum mechanics from John S. Waugh and group theory from F. A. Cotton.

After graduating from MIT shortly before my 20th birthday, I headed to Caltech where I joined the research group of Harry B. Gray—an exceptional lecturer.  After a year as a teaching assistant in organic chemistry, George S. Hammond and Harry Gray recognized a spark for teaching and offered me the opportunity to team teach an advanced freshman course.  My graduate student partner, Michael D. Bertolucci, and I were given carte blanche to develop an interesting course for freshman that would not overlap other courses in the curriculum.  We chose an overview of general chemistry for one term, followed by two terms of introduction to group theory and spectroscopy.  We conducted a critique of each other’s lecture immediately after every class.  I placed highest value in interest, content, clarity, and physical understanding, which became main goals in my textbook writing.  At the age of 21, I found myself driven to write lecture notes which, upon the recommendation of Harry Gray, evolved into the book Symmetry and Spectroscopy.  I team-taught the freshman course with other graduate students and had the academic rank of Instructor during my last year of graduate studies.  For part of that year, I was a postdoc in the fledgling field of 13C-NMR spectroscopy with John D. Roberts.

After two years as a postdoc at the Albert Einstein College of Medicine in New York City with Philip Aisen—an exemplary mentor—I started my first faculty position at the University of California at Davis in 1975.  I was assigned to teach analytical chemistry for sophomores and accelerated freshmen.  This assignment was interesting because I had never taken a course in analytical chemistry.  I arrived at MIT after analytical chemistry became an elective and flew through MIT too quickly to partake in the analytical course.  I had practical analytical experience from undergraduate, graduate, and postdoctoral research.  My source of instruction in chemical equilibrium was the graduate course “Aquatic Chemistry” taught by J. J. Morgan at Caltech.  At Davis, I sat in on an analytical courses taught by a senior member of the department to “learn the ropes” before being thrust before my first students in analytical chemistry.

My burning desire at Davis was to be the best teacher I could be.  I was known for being available at all hours for student questions, for circulating through laboratories every day, and for memorizing the names and faces of every student.  It became apparent to students that sitting in the back row of a 300-seat lecture hall did not offer immunity from being called upon by name to answer a question during lecture.  I brought a demonstration into almost every lecture and each term ended with a series of explosions.  The last class each term attracted far more students than were enrolled in the course.  The majority of my students at Davis were life science majors whose interests resonated with my research interest in metalloproteins.

I surveyed every analytical textbook I could find and taught from several.  I found the more thorough books to be dull and the more interesting books to be less thorough.  After two years, I decided to write text to accompany my lectures.  My goal was to be interesting and thorough in the selected topics.  Publisher’s representatives saw my notes in the bookstore and soon there were five offers for publication.  I visited each publisher and unashamedly adopted the best suggestions from each editor.  In 1978, I signed with W. H. Freeman as the publisher I thought would produce the nicest book.  After two more years of writing, a year of revision, and a year of production, the first edition of Quantitative Chemical Analysis was born in 1982.

By this time, I had not been offered tenure at Davis or at Franklin and Marshall College.  I loved teaching, but decided to try a different career.  In 1983, I moved to the U.S. Navy’s Michelson Laboratory at China Lake, California, where my present title is Senior Scientist.  In the course of 25 years with the Navy, I was elected an Esteemed Fellow and received a Top Navy Scientist award.  My research concerns transparent ceramic sensor windows.  I have been teaching a professional course in this subject several times each year since 1990 and wrote the monograph Materials for Infrared Windows and Domes, which is the standard reference in its field.

Meanwhile, Quantitative Chemical Analysis sold well enough for the publisher to invite me to prepare a 2nd edition.  I found myself with two full-time jobs—one for the Navy and a second as a textbook writer.  My wife Sally has been editorial assistant and proofreader on every book.  She produced all of the illustrations for Symmetry and Spectroscopy with a one-year-old watching over her shoulder.  Thirty years after signing our contract with Freeman, we are working on the 8th edition.  The book has had 12 foreign translations.

Our chief competitor, Doug Skoog (with coauthors West, Holler, and Crouch) had “big” and “little” books to serve two market levels.  Freeman asked me to write a small book to complement Quantitative Chemical Analysis, but I hesitated to go into competition with myself.  By 1995, we no longer had children in the house and the time was ripe for a “small” book.  My priorities for Exploring Chemical Analysis were to be (1) short, (2) interesting, and (3) elementary—in that order.  This book has now gone through 4 editions and 3 foreign translations.

A survey published in 2002 found that my two books were used in over half of the analytical chemistry courses in the United States.  [P. A. Mabrouk, Anal. Chem. 2002, 74, 269A.]  In 2008, Quantitative Chemical Analysis received the McGuffey Longevity Award from the Textbook and Academic Authors Association.

In my writing, I try to catch the reader’s attention and to convey excitement by illustrating each topic with interesting real-world examples.  I try to get to the heart of a topic with the minimum number of words.  It is good pedagogy to explain everything and not to assume prior knowledge on the part of the reader.  Heavy use of illustrations makes ideas more understandable and memorable.  Chapters are broken into short sections which are more digestable than long sections.  Recalling my own student days, I include answers to all problems at the back of the book.  Some teachers would rather have a set of problems without answers, but I have never heard a student complain about immediate feedback after working a problem.  An informal writing style and a little humor provide a relaxed tone.

Quantitative Chemical Analysis evolved over 30-years.  Spectrophotometry grew from one to three chapters as it moved from the middle of the book to the front and then to the middle again.  Chromatography expanded from two to four chapters as its importance grew.  Electrophoresis and mass spectrometry were added.  Quality assurance, sampling, and sample preparation were added and quality assurance increased in importance.  Computer programming projects were introduced in the second edition.  Spreadsheets appeared in the fourth edition and increased in each subsequent edition.  A spreadsheet-oriented chapter on advanced chemical equilibrium appeared in the seventh edition.  Uniform, high-interest opening vignettes appeared in the fourth edition.  Chapter 0 on the “analytical process” describing an actual student analysis of caffeine in chocolate appeared in the fifth edition.  Gravimetric analysis was demoted to the back of the book.  Electroanalytical chemistry decreased from five to four chapters.  Instructions for experiments moved to the web in the sixth edition to make room for growth in other subjects.

Exploring Chemical Analysis began with brevity as the first goal.  User feedback directed me to add several topics that had been rejected for the first edition.  These topics included activity coefficients, systematic treatment of equilibrium, EDTA and redox titration curve calculations, and an expanded discussion of spectrophotometry.  Placement of spectrophotometry early in the book did not fit well with many curricula, so the subject was moved back in the second edition.  The third edition increased emphasis on quality assurance, integrated mass spectrometry with chromatography, and introduced inductively coupled plasma-mass spectrometry.  Spreadsheets gradually increased in every edition.  A short “ask yourself” question with an answer at the end of every worked example appeared in the fourth edition.

The most common comment I receive from teachers can be paraphrased as “I love your book and I wish it weren’t so long.  And please add more on (fill in favorite topic).”  Kolthoff, Sandell, Mehan, and Bruckenstein wrote in the preface of what was perhaps the most venerable analytical textbook of the 20th century, “as much as anyone, we regret the length of this revised edition ” (1170 pages) and “it is a very hard undertaking to seek to please everybody.”

A good textbook has the attributes of a good teacher.  The best description I have seen for a good teacher is a person with a “deep understanding of the subject, unbounded enthusiasm, humor, and the ability to communicate excitement, clarity and precision of thought and word, and the ability to put oneself in the mind of a student new to the subject.”  [C. Thyagaraja, Caltech News, 2000, 34[2], 11.]  To these I would add the ability to convey the significance and applications of the subject.  I strive toward these ends in my writing.

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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

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  • Posted February 4, 2011

    Great textbook but fail shipment... :(

    This book is outstanding in terms of contents and I would have given 5++ stars if I actually received a so called 'brand new' book which I paid the full price for. But instead, my shipment arrived damaged. Corner of the box was literally open/damaged and book had high signs of usage by someone. Things such as finger prints, rubbed marks, edge/tear wear etc. B&N gotta be kidding me. They can't do this to customer who buy these expensive books. This was my first purchase at B&N and it will be the LAST. Hopefully this review will at least warn/help others deciding whether to get these kind of college textbooks from B&N or from another site.

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