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Completely revised and updated, Chemical Analysisessential introduction to a wide range of analytical techniques and instruments. Assuming little in the way of prior knowledge, this text carefully guides the reader through the more widely used and important techniques, whilst avoiding excessive technical detail.* Provides a thorough introduction to a wide range of the most important and widely used instrumental techniques* Maintains a careful balance between depth and breadth of coverage* Includes examples, problems and their solutions* Includes coverage of latest developments including supercritical fluid chromatography and capillary electrophoresis
Table of Contents
Foreword to the first English edition xiii
Preface to the first English edition xv
Preface to second edition xvii
Acknowledgments xix
Introduction xxi
PART 1 SEPARATION METHODS 1 (164)
General aspects of chromatography 3 (28)
General concepts of analytical 3 (3)
chromatography
The chromatogram 6 (1)
Gaussian-shaped elution peaks 7 (2)
The plate theory 9 (2)
Nernst partition coefficient (K) 11 (1)
Column efficiency 12 (2)
Retention parameters 14 (3)
Separation (or selectivity) factor 17 (1)
between two solutes
Resolution factor between two peaks 17 (2)
The rate theory of chromatography 19 (3)
Optimization of a chromatographic analysis 22 (2)
Classification of chromatographic 24 (7)
techniques
Problems 27 (4)
Gas chromatography 31 (32)
Components of a GC installation 31 (2)
Carrier gas and flow regulation 33 (1)
Sample introduction and the injection 34 (5)
chamber
Thermostatically controlled oven 39 (1)
Columns 39 (2)
Stationary phases 41 (5)
Principal gas chromatographic detectors 46 (4)
Detectors providing structural data 50 (2)
Fast chromatography 52 (1)
Multi-dimensional chromatography 53 (1)
Retention indexes and stationary phase 54 (9)
constants
Problems 58 (5)
High-performance liquid chromatography 63 (30)
The beginnings of HPLC 63 (1)
General concept of an HPLC system 64 (1)
Pumps and gradient elation 65 (3)
Injectors 68 (1)
Columns 68 (2)
Stationary phases 70 (5)
Chiral chromatography 75 (1)
Mobile phases 76 (2)
Paired-ion chromatography 78 (2)
Hydrophobic interaction chromatography 80 (1)
Principal detectors 80 (7)
Evolution and applications of HPLC 87 (6)
Problems 89 (4)
Ion chromatography 93 (24)
Basics of ion chromatography 93 (3)
Stationary phases 96 (2)
Mobile phases 98 (2)
Conductivity detectors 100 (1)
Ion suppressors 101 (3)
Principle and basic relationship 104 (1)
Areas of the peaks and data treatment 105 (1)
software
External standard method 105 (2)
Internal standard method 107 (3)
Internal normalization method 110 (7)
Problems 112 (5)
Thin layer chromatography 117 (10)
Principle of TLC 117 (3)
Characteristics of TLC 120 (1)
Stationary phases 121 (1)
Separation and retention parameters 122 (1)
Quantitative TLC 123 (4)
Problems 125 (2)
Supercritical fluid chromatography 127 (8)
Supercritical fluids: a reminder 127 (2)
Supercritical fluids as mobile phases 129 (1)
Instrumentation in SFC 130 (1)
Comparison of SFC with HPLC and GC 131 (2)
SFC in chromatographic techniques 133 (2)
Size exclusion chromatography 135 (10)
Principle of SEC 135 (2)
Stationary and mobile phases 137 (1)
Calibration curves 138 (1)
Instrumentation 139 (1)
Applications of SEC 140 (5)
Problems 143 (2)
Capillary electrophoresis and 145 (20)
electrochromatography
From zone electrophoresis to capillary 145 (3)
electrophoresis
Electrophoretic mobility and 148 (4)
electro-osmotic flow
Instrumentation 152 (3)
Electrophoretic techniques 155 (2)
Performance of CE 157 (2)
Capillary electrochromatography 159 (6)
Problems 161 (4)
PART 2 SPECTROSCOPIC METHODS 165 (202)
Ultraviolet and visible absorption 167 (40)
spectroscopy
The UV/Vis spectral region and the origin 167 (2)
of the absorptions
The UV/Vis spectrum 169 (2)
Electronic transitions of organic 171 (2)
compounds
Chromophore groups 173 (1)
Solvent effects: solvatochromism 174 (2)
Fieser-Woodward rules 176 (2)
Instrumentation in the UV/Visible 178 (3)
UV/Vis spectrophotometers 181 (5)
Quantitative analysis: laws of molecular 186 (4)
absorption
Methods in quantitative analysis 190 (2)
Analysis of a single analyte and purity 192 (1)
control
Multicomponent analysis (MCA) 193 (3)
Methods of baseline correction 196 (2)
Relative error distribution due to 198 (2)
instruments
Derivative spectrometry 200 (2)
Visual colorimetry by transmission or 202 (5)
reflection
Problems 203 (4)
Infrared spectroscopy 207 (34)
The origin of light absorption in the 207 (1)
infrared
Absorptions in the infrared 208 (1)
Rotational-vibrational bands in the mid-IR 208 (2)
Simplified model for vibrational 210 (2)
interactions
Real compounds 212 (1)
Characteristic bands for organic compounds 212 (4)
Infrared spectrometers and analysers 216 (5)
Sources and detectors used in the mid-IR 221 (4)
Sample analysis techniques 225 (5)
Chemical imaging spectroscopy in the 230 (2)
infrared
Archiving spectra 232 (1)
Comparison of spectra 233 (1)
Quantitative analysis 234 (7)
Problems 238 (3)
Fluorimetry and chemiluminescence 241 (22)
Fluorescence and phosphorescence 241 (2)
The origin of fluorescence 243 (2)
Relationship between fluorescence and 245 (2)
concentration
Rayleigh scattering and Raman bands 247 (2)
Instrumentation 249 (4)
Applications 253 (2)
Time-resolved fluorimetry 255 (1)
Chemiluminescence 256 (7)
Problems 259 (4)
X-ray fluorescence spectrometry 263 (22)
Basic principles 263 (1)
The X-ray fluorescence spectrum 264 (2)
Excitation modes of elements in X-ray 266 (5)
fluorescence
Detection of X-rays 271 (2)
Different types of instruments 273 (4)
Sample preparation 277 (1)
X-ray absorption - X-ray densimetry 278 (1)
Quantitative analysis by X-ray 279 (1)
fluorescence
Applications of X-ray fluorescence 279 (6)
Problems 281 (4)
Atomic absorption and flame emission 285 (24)
spectroscopy
The effect of temperature upon an element 285 (3)
Applications to modern instruments 288 (1)
Atomic absorption versus flame emission 288 (2)
Measurements by AAS or by FES 290 (1)
Basic instrumentation for AAS 291 (6)
Flame photometers 297 (1)
Correction of interfering absorptions 298 (4)
Physical and chemical interferences 302 (2)
Sensitivity and detection limits in AAS 304 (5)
Problems 305 (4)
Atomic emission spectroscopy 309 (18)
Optical emission spectroscopy (OES) 309 (1)
Principle of atomic emission analysis 310 (1)
Dissociation of the sample into atoms or 311 (4)
ions
Dispersive systems and spectral lines 315 (2)
Simultaneous and sequential instruments 317 (4)
Performances 321 (2)
Applications of OES 323 (4)
Problems 324 (3)
Nuclear magnetic resonance spectroscopy 327 (40)
General introduction 327 (1)
Spin/magnetic field interaction for a 328 (3)
nucleus
Nuclei that can be studied by NMR 331 (1)
Bloch theory for a nucleus of spin number 331 (2)
I = 1/2
Larmor frequency 333 (2)
Pulsed NMR 335 (4)
The processes of nuclear relaxation 339 (1)
Chemical shift 340 (1)
Measuring the chemical shift 341 (1)
Shielding and deshielding of the nuclei 342 (1)
Factors influencing chemical shifts 342 (2)
Hyperfine structure - spin-spin coupling 344 (1)
Heteronuclear coupling 345 (2)
Homonuclear coupling 347 (5)
Spin decoupling and particular pulse 352 (2)
sequences
HPLC-NMR coupling 354 (1)
Fluorine and phosphorus NMR 355 (1)
Quantitative NMR 356 (4)
Analysers using pulsed NMR 360 (7)
Problems 364 (3)
PART 3 OTHER METHODS 367 (152)
Mass spectrometry 369 (50)
Basic principles 369 (3)
The magnetic-sector design 372 (2)
`EB' or `BE' geometry mass analysers 374 (5)
Time of flight analysers (TOF) 379 (2)
Quadrupole analysers 381 (4)
Quadrupole ion trap analysers 385 (2)
Ion cyclotron resonance analysers (ICRMS) 387 (2)
Mass spectrometer performances 389 (2)
Sample introduction 391 (1)
Major vacuum ionization techniques 392 (5)
Atmospheric pressure ionization (API) 397 (4)
Tandem mass spectrometry (MS/MS) 401 (1)
Ion detection 402 (2)
Identification by means of a spectral 404 (1)
library
Analysis of the elementary composition of 405 (2)
ions
Determination of molecular masses from 407 (1)
multicharged ions
Determination of isotope ratios for an 408 (2)
element
Fragmentation of organic ions 410 (9)
Problems 415 (4)
Labelling methods 419 (22)
The principle of labelling methodologies 419 (1)
Direct isotope dilution analysis with a 420 (1)
radioactive label
Substoichiometric isotope dilution 421 (1)
analysis
Radio immuno-assays (RIA) 422 (1)
Measuring radioisotope activity 423 (2)
Antigens and antibodies 425 (1)
Enzymatic-immunoassay (EIA) 426 (3)
Other immunoenzymatic techniques 429 (1)
Advantages and Limitations of the Elisa 430 (1)
test in chemistry
Immunofluorescence analysis (IFA) 431 (1)
Stable isotope labelling 431 (1)
Neutron activation analysis (NAA) 432 (9)
Problems 437 (4)
Elemental analysis 441 (12)
Particular analyses 441 (1)
Elemental organic microanalysis 442 (3)
Total nitrogen analysers (TN) 445 (2)
Total sulfur analysers 447 (1)
Total carbon analysers (TC, TIC and TOC) 447 (3)
Mercury analysers 450 (3)
Problems 451 (2)
Potentiometric methods 453 (12)
General principles 453 (2)
A particular ISE: the pH electrode 455 (2)
Other ion selective electrodes 457 (3)
Slope and calculations 460 (3)
Applications 463 (2)
Problems 463 (2)
Voltammetric and coulometric methods 465 (22)
General principles 465 (2)
The dropping-mercury electrode 467 (1)
Direct current polarography (DCP) 467 (1)
Diffusion current 468 (2)
Pulsed polarography 470 (2)
Amperometric detection in HPLC and HPCE 472 (1)
Amperometric sensors 472 (6)
Stripping voltammetry (SV) 478 (2)
Potentiostatic coulometry and 480 (1)
amperometric coulometry
Coulometric titration of water by the 481 (6)
Karl Fischer reaction
Problems 484 (3)
Sample preparation 487 (14)
The need for sample pretreatment 487 (1)
Solid phase extraction (SPE) 488 (2)
Immunoaffinity extraction 490 (1)
Microextraction procedures 491 (2)
Gas extraction on a cartridge or a disc 493 (1)
Headspace 494 (2)
Supercritical phase extraction (SPE) 496 (2)
Microwave reactors 498 (1)
On-line analysers 498 (3)
Basic statistical parameters 501 (18)
Mean value, accuracy of a collection of 501 (3)
measurements
Variance and standard deviation 504 (1)
Random or indeterminate errors 504 (2)
Confidence interval of the mean 506 (2)
Comparison of results - parametric tests 508 (2)
Rejection criteria Q-test (or Dixon test) 510 (1)
Calibration curve and regression analysis 511 (2)
Robust methods or non-parametric tests 513 (2)
Optimization through the 515 (4)
one-factor-at-a-time (OFAT)
experimentation
Problems 516 (3)
Solutions 519 (42)
Appendix - List of acronyms 561 (4)
Bibliography 565 (2)
Table of some useful constants 567 (2)
Index 569
