Chemical Analysis: Modern Instrumentation Methods and Techniques Book

Foreword to the French edition
Foreword to the English edition
Preface to the French edition
Preface to the English edition
Acknowledgements
Introduction
Part 1 Separation Methods
Chapter 1 General aspects of chromatography
1.1 General concepts of analytical chromatography
1.2 Classification of chromatographic techniques
1.3 The chromatogram
1.4 The ideal chromatogram and Gaussian peaks
1.5 Real peaks
1.6 The theoretical plate model
1.7 Column efficiency
1.8 Retention parameters
1.9 Separation factor between two solutes
1.10 Resolution Factor between two peaks
1.11 The van Deemter equation in gas chromatography
1.12 Optimisation of a chromatographic analysis
Problems
Chapter 2 Gas chromatography
2.1 Components of a gas chromatograph
2.2 Carrier gas and flow regulation
2.3 Sample introduction and the injection chamber
2.4 Oven
2.5 Columns
2.6 Stationary phases (liquid type)
2.7 Stationary phases (solid type)
2.8 Common detectors
2.9 Detectors yielding structural information
Appendix - Retention indices and constants related to stationary phases
2.10 Kovats relationship
2.11 Kovats retention indices
2.12 Stationary phase constants
Problems
Chapter 3 High performance liquid chromatography
3.1 Origin of HPLC
3.2 General scheme of an HPLC system
3.3 Pumps and gradient elution
3.4 Injectors
3.5 Columns
3.6 Stationary phases
3.7 Mobile phases
3.8 Chiral chromatography
3.9 Principal detectors
3.10 Applications
Problems
Chapter 4 Ion chromatography
4.1 The principle of ion chromatography
4.2 Mobile phases
4.3 Stationary phases
4.4 The principleof separation
4.5 Conductivity detectors
4.6 Ion suppressors
Appendix - Quantitative analysis by chromatography
4.7 Principle and basic equation
4.8 Recording integrators and data treatment software
4.9 External standard method
4.10 Internal standard method
4.11 Internal normalisation
Problems
Chapter 5 Planar chromatography
5.1 Planar chromatography: principles of application
5.2 Post-chromatography: development of the plate
5.3 Stationary phases
5.4 Retention and separation parameters
5.5 Quantitative TLC
5.6 Aspects of TLC
Problems
Chapter 6 Supercritical fluid chromatography
6.1 Supercritical fluids
6.2 Supercritical phases as mobile phases
6.3 Comparison of SFC with HPLC and GC
6.4 Instrumentation
6.5 SFC in chromatographic techniques
Chapter 7 Size exclusion chromatography
7.1 The principle of SEC
7.2 Stationary phases
7.3 Instrumentation
7.4 Domains of application
Problems
Chapter 8 Capillary electrophoresis
8.1 Zone electrophoresis
8.2 Free solution capillary electrophoresis
8.3 Electrophoretic mobility and electro-osmotic flow
8.4 Instrumentation and techniques
8.5 Indirect detection
8.6 Performance of capillary electrophoresis
Problems
Part 2 Spectroscopic Methods
Chapter 9 Nuclear magnetic resonance spectroscopy
9.1 General description
9.2 Spin/magnetic field interaction for a nucleus
9.3 Nuclei that can be studied by NMR
9.4 Bloch's theory for a nucleus of I = 1/2
9.5 Larmor's frequency
9.6 Chemical shift
9.7 The principle of obtaining an NMR spectrum
9.8 Relaxation processes
9.9 The measurement of chemical shifts
9.10 Shielding and deshielding of the nuclei
9.11 Factors influencing chemical shifts
9.12 Hyperfine structure: spin/spin coupling
9.13 Heteronuclear coupling
9.14 Homonuclear coupling
9.15 Spin decoupling and modes of operation
9.16 Fluorine and phosphorous NMR
Appendix - Quantitative NMR
9.17 Measurement of area - application to simple analysis
9.18 Samples containing compounds that can he identified
9.19 Internal standard method
9.20 Standard additions method
9.21 Analysers using pulsed NMR
Problems
Chapter 10 Infrared spectroscopy
10.1 Spectral representation in the mid infrared (IR)
10.2 Origin of absorption bands in the mid infrared
10.3 Rotational-vibrational bands in the mid infrared
10.4 Simplified model for vibrational interactions
10.5 Real model for vibrational interactions
10.6 Rotational bands of compounds in the gas phase
10.7 Characteristic bands for organic compounds
10.8 Instrumentation
10.9 Optics, sources and detectors used in the mid infrared
10.10 Sample analysis techniques
10.11 Infrared microscopy
10.12 Archiving spectra
10.13 Comparison of spectra
10.14 Calibration of cell thickness
10.15 Raman diffusion
Problems
Chapter 11 Ultraviolet and Visible absorption spectroscopy
11.1 General concepts
11.2 Molecular absorptions
11.3 Origin of absorption in relation to molecular orbitals
11.4 Donor-acceptor association
11.5 Isolated chromophores
11.6 Solvent effects: solvatochromism
11.7 Chromophores in conjugated systems
11.8 Woodward-Fieser rules
11.9 UV/Visible spectrophotometers
11.10 Quantitative analysis in the UV/Visible
11.11 Beer--Lambert's law
11.12 Visual colorimetry
11.13 Absorbance measurements
11.14 Confirmation analysis (purity control)
11.15 Distribution of relative errors due to instruments
11.16 Baseline correction
11.17 Multicomponent analysis (MCA)
11.18 Derivative spectrometry
Problems
Chapter 12 Fluorimetry
12.1 Fluorescence and phosphorescence
12.2 Origin of fluorescence
12.3 Fluorescence intensity
12.4 Rayleigh and Raman bands
12.5 Instrumentation
12.6 Applications
12.7 Chemiluminescence
Problems
Chapter 13 X-ray fluorescence spectrometry
13.1 General principle
13.2 X-ray fluorescence spectrum
13.3 Excitation modes of elements in X-ray fluorescence
13.4 X-ray absorption
13.5 Sample preparation
13.6 Different types of instruments
13.7 Quantitative analysis by X-ray fluorescence
13.8 X-ray fluorescence applications
Problems
Chapter 14 Atomic absorption and flame emission spectroscopy
14.1 Principles common to the two methods
14.2 Interpretation of the phenomena involved
14.3 Atomic absorption vs flame emission
14.4 Measurements by absorption or flame emission
14.5 Basic instrumentation for atomic absorption
14.6 Flame photometers
14.7 Correction of interfering absorptions
14.8 Physical and chemical interferences
14.9 Sensitivity and detection limits in AAS
Problems
Chapter 15 Atomic emission spectroscopy
15.1 Optical emission spectrophotometry (OES) 273
15.2 Excitation by inductively coupled plasma (ICP)
15.3 Ionisation by arc, spark or electronic impact
15.4 The principles of atomic emission analysis
15.5 Spectral lines
15.6 Simultaneous and sequential instruments
15.7 Performance
15.8 GC coupled to atomic emission relatively
15.9 Applications of atomic emission spectrometry
Problems
Part 3 Other Methods 287
Chapter 16 Mass spectrometry
16.1 Principles
16.2 The Bainbridge spectrometer
16.3 Magnetic analysers (EB type)
16.4 Time of flight (TOF) analysers
16.5 Ion cyclotron resonance
16.6 Quadrupole analysers
16.7 Ion traps
16.8 Performance of mass spectrometers
16.9 Sample introduction
16.10 Major ionisation techniques (under vacuum)
16.11 Atmospheric pressure ionisation (API)
16.12 Ion detection
16.13 Tandem mass spectrometry
Appendix - Applications in mass spectrometry
16.14 Determination of empirical formulae
16.15 Determination of isotope ratios for an element
16.16 Identification using spectral libraries
16.17 Fragmentation of organic ions
Problems
Chapter 17 Labelling methods
17.1 Principle of labelling methods
17.2 Isotopic dilution with a radioactive label
17.3 Measurement of radioisotope activity
17.4 Choice of a sub-stoichiometric method
17.5 Labelling with stable isotopes
17.6 Immunoenzymatic (IEA) methods of measurement
17.7 Other immunoenzymatic techniques
17.8 Advantages and limitations of the ELISA test in chemistry
17.9 Radio-immunoassay (RIA)
17.10 immunofluorescence assay (IFA)
17.11 Neutron activation analysis (NAA)
17.12 Thermal neutrons
17.13 Induced activity -- irradiation time
17.14 Detection by γ-counting -- measurement principle
17.15 Applications
Problems
Chapter 18 Potentiometric methods
18.1 General principles
18.2 A particular ion selective electrode: the pH electrode
18.3 Ion selective electrodes
18.4 Calculations and different methods
18.5 Applications
Problems
Chapter 19 Coulometric and voltammetric methods
19.1 General principles
19.2 Dropping-mercury electrode
19.3 Continuous current polarography
19.4 Diffusion current
19.5 Pulse polarography
19.6 Amperometric detection in HPLC and CE
19.7 Special sensors
19.8 Stripping voltammetry
19.9 Coulometric measurements
19.10 Karl Fischer coulometric determination of water
19.11 Determination by the Karl Fischer method
Problems
Chapter 20 Some sample preparation methods
20.1 Evolution of methods
20.2 Solid-phase extraction using columns or discs
20.3 Gas-solid extraction using columns or discs
20.4 Headspace sample analysis
20.5 Supercritical fluid extraction (SFE)
20.6 Mineralisation by microwave digestion
Chapter 21 Basic statistical parameters
21.1 Mean value and accuracy
21.2 Precision and standard deviation of a group of results
21.3 Indeterminate or random errors
21.4 Confidence interval
21.5 Parametric tests -- comparison of results
21.6 Rejection criteria -- Q test (Dixon test)
21.7 Linear regression
21.8 Robust methods
21.9 Method optimisation using factorial analysis
Problems
Solutions
Appendix -- List of acronyms
Bibliography
Table of physico-chemical constants
Index