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Page iii
Principles and Practice of Analytical Chemistry
Fifth Edition
F.W. Fifield
Kingston University
and
D. Kealey
University of Surrey
Page iv
© 2000 by
Blackwell Science Ltd
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A catalogue record for this title is available from the British Library
ISBN 0-632-05384-4
Library of Congress
Cataloging-in-Publication Data
Fifield, F.W. (Frederick William)
Principles and practice of analytical
chemistry/F.W. Fifield and D. Kealey.
p. cm.
Includes bibliographical references and
index.
ISBN 0-632-05384-4 (pbk).
1. Chemistry, Analytic. I. Kealey, D.
(David) II. Title.
QD75.2 .F53 2000
543 – dc21 99-059799
For further information on Blackwell Science, visit our website: www.blackwell-science.com
Page v
Contents
Preface
xi
Acknowledgements
xiii
1
Introduction
1
The Scope of Analytical Chemistry. The Function of Analytical
Chemistry. Analytical Problems and Their Solution. The Nature of
Analytical Methods. Trends in Analytical Methods and Procedures.
Glossary of Terms.
2
The Assessment of Analytical Data
13
2.1 Definitions and Basic Concepts
13
2.2 The Nature and Origin of Errors
16
2.3 The Evaluation of Results and Methods
17
The Reliability of Measurements. The Analysis of Data. The
Application of Statistical Tests. Limits of Detection. Quality
Control Charts. Standardization of Analytical Methods.
Chemometrics.
Problems
34
3
pH, Complexation and Solubility Equilibria
37
3.1 Chemical Reactions in Solution
38
Equilibrium Constants. Kinetic Factors in Equilibria.
3.2 Solvents in Analytical Chemistry
41
Ionizing Solvents. Non-ionizing Solvents.
3.3 Acid–base Equilibria
43
Weak Acid and Weak Base Equilibria. Buffers and pH Control. The
pH of Salt Solutions.
3.4 Complexation Equilibria
49
The Formation of Complexes in Solution. The Chelate Effect.
3.5 Solubility Equilibria
52
Solubility Products.
Problems
53
4
Separation Techniques
54
4.1 Solvent Extraction
55
Efficiency of Extraction. Selectivity of Extraction. Extraction
Systems. Extraction of Uncharged Metal Chelates. Methods of
Extraction. Applications of Solvent Extraction.
4.2 Solid Phase Extraction
73
Solid Phase Sorbents. Solid Phase Extraction Formats. Automated
Solid Phase Extraction. Solid Phase Microextraction. Applications
of SPE and SPME.
Page vi
4.3 Chromatography
80
4.3.1 Gas Chromatography. 4.3.2 High Performance Liquid
Chromatography. 4.3.3 Supercritical Fluid Chromatography. 4.3.4
Thin-layer Chromatography. 4.3.5 Ion-exchange Chromatography.
4.3.6 Size Exclusion Chromatography.
4.4 Electrophoresis
170
Factors Affecting Ionic Migration. Effect of Temperature. pH and
Ionic Strength. Electro-osmosis. Supporting Medium. Detection of
Separated Components. Applications of Traditional Zone
Electrophoresis. High-performance Capillary Electrophoresis.
Capillary Electrochromatography. Applications of Capillary
Electrochromatography.
Problems
188
5
Titrimetry and Gravimetry
191
5.1 Titrimetry
191
Definitions. Titrimetric Reactions. Acid-base Titrations.
Applications of Acid–base Titrations. Redox Titrations.
Applications of Redox Titrations. Complexometric Titrations.
Ethylenediaminetetraacetic Acid (EDTA). Applications of EDTA
Titrations. Titrations with Complexing Agents Other Than EDTA.
Precipitation Titrations.
5.2 Gravimetry
216
Precipitation Reactions. Practical Gravimetric Procedures.
Applications of Gravimetry.
Problems
226
6
Electrochemical Techniques
228
6.1 Potentiometry
232
Electrode Systems. Direct Potentiometric Measurements.
Potentiometric Titrations. Null-point Potentiometry. Applications of
Potentiometry.
6.2 Polarography, Stripping Voltammetry and Amperometric
247
Techniques
Diffusion Currents. Half-wave Potentials. Characteristics of the
DME. Quantitative Analysis. Modes of Operation Used in
Polarography. The Dissolved Oxygen Electrode and Biochemical
Enzyme Sensors. Amperometric Titrations. Applications of
Polarography and Amperometric Titrations.
6.3 Electrogravimetry and Coulometry
260
Coulometry. Coulometry at Constant Potential. Coulometric
Titrations. Applications of Coulometric Titrations.
6.4 Conductometric Titrations
264
Ionic Conductances.
Problems
267
7
An Introduction to Analytical Spectrometry
270
Electromagenetic Radiation. Atomic and Molecular Energy. The
Absorption and Emission of Electromagnetic Radiation. The
Complexity of Spectra and the Intensity of Spectral Lines.
Analytical Spectrometry. Instrumentation.
Page vii
8
Atomic Spectrometry
284
8.1 Arc/Spark Atomic (Optical) Emission Spectrometry
289
Instrumentation. Sample Preparation. Qualitative and Quantitative
Analysis. Interferences and Errors Associated with the Excitation
Process. Applications of Arc/Spark Emission Spectrometry.
8.2 Glow Discharge Atomic Emission Spectrometry
295
Instrumentation. Applications.
8.3 Plasma Emission Spectrometry
298
Instrumentation. Sample Introduction for Plasma Sources.
Analytical Measurements. Applications of Plasma Emission
Spectrometry.
8.4 Inductively Coupled Plasma–mass Spectrometry (ICP–MS)
305
Principles. Instrumentation. Applications.
8.5 Flame Emission Spectrometry
312
Instrumentation. Flame Characteristics. Flame Processes. Emission
Spectra. Quantitative Measurements and Interferenccs. Applications
of Flame Photometry and Flame Atomic Emission Spectrometry.
8.6 Atomic Absorption Spectrometry
320
Absorption of Characteristic Radiation. Instrumentation. Sample
Vaporization. Quantitative Measurements and Interferences.
Applications of Atomic Absorption Spectrometry.
8.7 Atomic Fluorescence Spectrometry
333
8.8 X-ray Emission Spectrometry
335
X-ray Processes. Instrumentation. Applications of X-ray Emission
Spectrometry.
Problems
352
9
Molecular Spectrometry
354
9.1 Visible and Ultraviolet Spectrometry
363
Polyatomic Organic Molecules. Metal Complexes. Qualitative
Analysis – The Identification of Structural Features. Quantitative
Analysis – Absorptiometry. Choice of Colorimetric and
Spectrophotometric Procedures. Fluorimetry. Applications of
UV/Visible Spectrometry and Fluorimetry.
9.2 Infrared Spectrometry
378
Diatomic Molecules. Polyatomic Molecules. Characteristic
Vibration Frequencies. Factors Affecting Group Frequencies.
Qualitative Anlaysis – The Identification of Structural Features.
Quantitative Analysis. Sampling Procedures. Near Infrared
Spectrometry. Applications of Infrared Spectrometry.
9.3 Nuclear Magnetic Resonance (NMR) Spectrometry
396
Instrumentation. The NMR Process. Chemical Shift. Spin–spin
Coupling. Carbon-13 NMR. Pulsed Fourier transform NMR (FT-
NMR). Qualitative Analysis – The Identification of Structural
Features. Quantitative Analysis. Applications of NMR
Spectrometry.
9.4 Mass Spectrometry
426
Instrumentation. Principle of Mass Spectrometry. Characteristics
and Interpretation of Molecular Mass Spectra. Applications of Mass
Spectrometry.
9.5 Spectrometric Identification of Organic Compounds
440
[...]... metals are there in a tin of tuna fish? What is the purity and chemical structure of a newly prepared compound? These and a host of other questions concerning the composition and structure of matter fall within the realms of analytical chemistry The answers may be given by simple chemical tests or by the use of costly and complex instrumentation The techniques and methods employed and the problems encountered... choice of method and the interpretation of analytical data thereby minimizing the expenditure of time, effort and money The purpose of this book is to provide a basic understanding of the principles, instrumentation and applications of chemical analysis as it is currently practised The amount of space devoted to each technique is based upon its application in industry as determined in a national survey of. .. Netherlands Figure 8.25 from Brown and Dymott, The use of platform atomisation and matrix modification as methods of interference control in graphite furnace analysis, by permission of Philips Scientific and Analytical Equipment Figures 11.21 and 11.24 from Frearson and Haskins, Chromatography and Analysis, Issue 7, (1989) by permission of RGC Publications Figures 4.18, 4.32, 9.2(a), 11.11, 11.20, 12.1 and. .. 4.43 and 4.45 from Smith, Gas and Liquid Chromatography in Analytical Chemistry (1988); figures 4.42 and 13.2 from Berridge, Techniques for the Automated Optimisation of Hplc Separations (1985) reproduced by permission of John Wiley and Sons Limited; 11.1, 11.5, 11.6, 11.12, 11.13, 11.14, 11.18 and 11.19 from Wendlandt, Thermal Analysis, 3rd edn., (1986); reprinted by permission of John Wiley and Sons... permission of Rose Ward Publishing, Guildford, U.K Figure 4.23 from McNair and Bonelli, Basic Gas Chromatography; with permission from Varian Associates, Inc Figures 4.38(c) and (d), 4.40, 9.52(a) and (b) from de Hoffmann, Charette and Stroobant, Mass Spectrometry, Principles and Application (1996) by permission of John Wiley & Sons Figure 4.39 from Huang, Wachs, Conboy and Henion, Analytical Chemistry, ... International, U.K Figures 8.14 and 8.15 from Date and Gray, Applications of Inductively Coupled Plasma Mass Spectrometry (1989); figures 2.7 and 2.8 from Kealey, Experiments in Modern Analytical Chemistry (1986); by permission of Blackie, U.K Figure 8.24 from Manahan, Quantitative Chemical Analysis (1986) by permission of Brookes Cole, U.K Figures 8.27 and 8.28(a) and (b) from Allmand and Jagger, Electron Beam... right across the traditional divisions of inorganic, organic and physical chemistry as well as embracing aspects of such areas as bio -chemistry, physics, engineering and economics Analytical chemistry is therefore a subject which is broad in its scope whilst requiring a specialist and disciplined approach An enquiring and critical mind, a keen sense of observation and the ability to pay scrupulous attention... 501 12 Overall Analytical Procedures and Their Automation 12.1 Sampling and Sample Pretreatment 503 503 Representative Samples and Sample Storage Sample Concentration and Clean-up: Solid Phase Extraction 12.2 Examples of Analytical Problems and Procedures 506 1: Evaluation of Methods for the Determination of Fluoride in Water Samples 2: Analysis of a Competitive Product 3: The Assessment of the Heavy... generation and diagnostic testing of the system Microcomputers with sophisticated data handling and graphics software packages have likewise made a considerable impact on the collection, storage, processing, enhancement and interpretation of analytical data Laboratory Information and Management Systems (LIMS), for the automatic logging of large numbers of samples, Chemometrics, which involve computerized and. .. identification and determination of the element in a specific chemical form presents the analyst with some of the more difficult problems Glossary of Terms The following list of definitions, though by no means exhaustive, will help both in the study and practice of analytical chemistry Accuracy The closeness of an experimental measurement or result to the true or accepted value (p 13) Analyte Constituent of the . Scope of Analytical Chemistry. The Function of Analytical
Chemistry. Analytical Problems and Their Solution. The Nature of
Analytical Methods. Trends in Analytical. 0-632-05384-4
Library of Congress
Cataloging-in-Publication Data
Fifield, F.W. (Frederick William)
Principles and practice of analytical
chemistry/ F.W. Fifield and D.
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