Front Matter
Preface
Preface to first edition
Introduction and overview
Introduction
Coverage
Chromatographic separation simply explained
Classification of chromatography
Mobile phase
Reversed-phase and normal-phase chromatography
Development mode
Technique
Planar and column chromatography
Column types
Separation mechanism
Adsorption chromatography
Partition chromatography
Bonded phase chromatography
Hydrophilic interaction liquid chromatography (HILIC)
Ion-exchange chromatography
Ion-interaction chromatography
Size-exclusion chromatography
Affinity chromatography
Micellar or Pseudophase liquid chromatography
Complexation chromatography
Ion-exclusion chromatography
Chiral chromatography
Other systems of classification
Chromatography: Publications and equipment sales
Applications of chromatography
Qualitative applications
Quantitative applications
Chromatographic metabolomics
Preparative applications
Comparison of chromatographic techniques
Analyte characteristics
Characteristics of the sample matrix
Purpose of the analysis
Historical aspects
Historical developments in the theory of chromatography
Concluding remarks
Obtaining assistance
References
Theoretical considerations
Introduction
Theory of chromatography
Why bother with theory?
Model or theory, which is it?
Taxonomy of models
Equilibrium models
Kinetic models
Macroscopic kinetic models
Microscopic kinetic models
Retention, dispersion, and distortion
Measures of peak asymmetry
Distribution isotherms
Retention: Thermodynamics and molecular interactions
Retention
Prediction of retention
Stationary phase selection
Method development
Measures of chromatographic retention
Planar techniques
Column techniques
Retention factor, k
Retention time
Compressible mobile phases
Retention volume
Net and specific retention volume
Dispersion
Plate theory
Plate height
Rate theory
Factors contributing to dispersion or zone broadening: Van Deemter equation
The A term: Eddy diffusion
The B term: Molecular or longitudinal diffusion
The C term: Resistance to mass transfer
Van Deemter plot
Is it resolution or separation?
Measures of separation and resolution
Separation factor
Resolution
Peak capacity and Trennzahl
Summary
Optimizing resolution
Column length
Retention factor
General elution problem
Column efficiency
Column selectivity
Summary
Extra-column dispersion
Worked example
Summary: Retention and dispersion
Column testing
References
Planar chromatography
Introduction
Paper chromatography
Mobile phases for paper chromatography
Thin layer chromatography
Why thin layer chromatography?
Comparison of conventional TLC and HPTLC
Comparison of TLC with other techniques
Theoretical considerations
Sample application in TLC
Plate development in TLC
Development chambers
Development techniques
Linear development
Vertical and horizontal development (one-dimensional single development)
One-dimensional multiple and continuous development
Two-dimensional development
Rotational development
Circular and anti-circular development
Forced flow development
Innovation in TLC
Forced flow conditions
Ultrathin layer chromatography
Hyphenated techniques
Thin layer plates
Stationary phases
Polar inorganic adsorbents
Silica gel
Alumina
Others
Activity
Pre-loading
Standardization of activity
Activity order of different adsorbents
Layer pre-treatment
Non-polar inorganic adsorbents
Modified adsorbents
Non-polar bonded phases
Polar bonded phases
Other phases
Mobile phases
Mobile phase optimization
Normal-phase systems
Reversed-phase systems
Detection: Qualitative analysis
Direct examination
Spray reagents
Spectrometry
Mass spectrometry
Analyte sampling and ionization
Miscellaneous
Quantitative analysis
In situ visual evaluation
Elution techniques
Densitometry
Slit scanning densitometers
Transmittance mode
Reflectance mode
Combined transmittance-reflectance mode
Decrease of phosphorescence
Fluorescence mode
Instrumentation
Diode-array densitometers
Image analysers
Separations
References
Gas chromatography
Introduction
Samples analysed by GC
Organization of this chapter
Mobile phases and delivery systems
Safety considerations
Carrier gas delivery systems
Carrier gas purification
Choosing a mobile phase
Carrier gas flow
Regulation of carrier gas flow and pressure control
Measurement of carrier gas flow
Practical considerations
Sample introduction in GC
Septa
Microsyringes
Manual syringe handling techniques
Packed columns
Open tubular columns
Auto injection
Sample inlet systems
Packed column
Open tubular column
Split injection
Splitless injection
Cool on-column injection
Programmed temperature vaporizer
Summary
Large volume injection
Pyrolysis gas chromatography
Headspace gas chromatography
Column packings and hardware
Columns
Packed columns
Open tubular columns
Column diameter
Column length
Stationary phase film thickness
Column diameter and film thickness
Column packings
Gas solid chromatography
Stationary phases
Inorganic oxides
Carbon adsorbents
Molecular sieves
Porous polymers
Gas liquid chromatography
Solid supports
Stationary phases
Representative stationary phases
Selection of a stationary phase
Classification of stationary phases
Summary
Column installation
Measuring system performance
Column bleed
Solvent and unretained solute test
Column efficiency
System activity
Ratio testing
Column care and use
Detectors
Make-up gas
Thermal conductivity detector
Flame ionization detector
Electron capture detector
Thermionic ionization detector
Flame photometric detector
Other detectors
Dual detection
Column temperature and temperature programming
Temperature programming
Derivatization
Silylation
Acylation
Alkylation
Oxime formation
Innovation
Multi-column gas chromatography
High-speed gas chromatography
High temperature gas chromatography
Micro gas chromatography
Separations
Gas solid chromatography
Mechanism of gas solid chromatography
Applications
Gas liquid chromatography
Mechanism of gas liquid chromatography
Applications
References
High performance liquid chromatography: Instrumentation and techniques
Introduction
From HPLC to UHPLC and beyond
Solvent delivery systems
General requirements
Materials of construction
Mobile phase reservoirs
Reciprocating HPLC pumps
Multisolvent pumps
Other types of HPLC pump
Sample introduction in HPLC
Manual injection
Autosamplers
Autosampler vials and microplates
Column packings and hardware
Columns
Column packings
Packed columns
Monolithic and other columns
Column packing and preparation methods
Column configuration and hardware
Column dimensions
Measuring column performance
Column care and use
Detectors
Introduction
UV-visible absorbance detectors
Fluorescence detectors
Electrochemical detectors
Refractive index detectors
Conductivity detectors
Aerosol-based detectors
Other detectors
Detector requirements for UHPLC
Post-column derivatization
Gradient elution
Introduction
Gradient elution theory and optimization
Dwell volume and gradient elution
Gradient applications and considerations
Multidimensional liquid chromatography
References
High performance liquid chromatography: Separations
Introduction
Chromatographic separations
Organization of this chapter
Separation of neutral compounds
Normal-phase chromatography
Introduction
Mechanism of normal-phase chromatography
Stationary phases for normal-phase chromatography
Mobile phases for normal-phase chromatography
Solvent strength
Solvent selectivity
Effect of water
Applications of normal-phase chromatography
Reversed-phase liquid chromatography
Introduction
Mechanism of reversed-phase chromatography
Stationary phases for reversed-phase liquid chromatography
Bonded phase silica columns
Silica and silica functionalization
Ligands used for bonded phase silica columns
Characteristics of bonded phase silica columns
Hybrid reversed-phase columns
Choosing a reversed-phase column
Mobile phases for reversed-phase liquid chromatography
Solvent classification
Solvent strength
Solvent selectivity
Other factors
Applications of reversed-phase liquid chromatography
Hydrophilic interaction liquid chromatography
Introduction
Mechanism of hydrophilic interaction liquid chromatography
Stationary phases for hydrophilic interaction liquid chromatography
Mobile phases for hydrophilic interaction liquid chromatography
Applications of hydrophilic interaction liquid chromatography
Size exclusion chromatography
Introduction
Mechanism of size exclusion chromatography
Stationary phases for size exclusion chromatography
Mobile phases for size exclusion chromatography
Applications of size exclusion chromatography
Techniques for ionic and ionizable species
Ion-suppression chromatography
Ion-interaction chromatography
Introduction
Stationary and mobile phases for ion-interaction chromatography
Mechanism of ion-interaction chromatography
Factors affecting retention in ion-interaction chromatography
Applications of ion-interaction chromatography
Ion-exchange chromatography
Introduction
Mechanism of ion-exchange chromatography
Stationary and mobile phases for ion-exchange chromatography
Factors affecting retention in ion-exchange chromatography
Applications of ion-exchange chromatography
Ion chromatography
Introduction
Stationary and mobile phases for ion chromatography
Mechanism of ion chromatography
Applications of ion chromatography
Ion-exclusion chromatography
Introduction
Mechanism of ion-exclusion chromatography
Stationary and mobile phases for ion-exclusion chromatography
Factors affecting retention in ion-exclusion chromatography
Applications of ion-exclusion chromatography
Specialty separation modes
Hydrophobic interaction chromatography
Affinity chromatography
Complexation chromatography
Chiral chromatography
Choosing a chromatographic method
References
Supercritical fluid chromatography
Introduction
History
Instrumentation
Factors affecting retention
Mobile phases and delivery systems
Safety considerations
Hardware
Back pressure regulators
Mobile phases
Alternatives to carbon dioxide
Modifiers
Mobile phase flow
Temperature/Pressure effects
Sample introduction in SFC
Column packings and hardware
Open tubular columns
Packed column SFC
Detectors
Programming techniques
Separations
References
Coupled systems
Introduction
Multidimensional chromatography
LC-GC and LCxGC
Hyphenated techniques
Mass spectrometry
Infrared spectrometry
Nuclear magnetic resonance spectrometry
GC-based
Gas chromatography-mass spectrometry
Ionization methods
Mass analyser
Scanning mode
Data
Gas chromatography-Fourier transform infrared spectrometry
GC-MS or GC-FTIR?
Other hyphenated techniques involving GC
LC based
Liquid chromatography-mass spectrometry
Ionization methods
Mass analyser
Enhancing specificity
UHPLC
Liquid chromatography-nuclear magnetic resonance spectrometry
Liquid chromatography-fourier transform infrared spectrometry
SFC-based
References
Analyses
Introduction
Detectors for chromatography
Specifications
Sensitivity
Linear response
Dynamic range
Minimum detectable quantity
Time constant and response time
Selectivity of response
Other factors
Noise
Classification
Data handling
Peak area versus peak height measurement
Manual approaches
Computerized approaches
Data acquisition
Data processing
Peak shape
Peak finding
Integration
Mathematical peak deconvolution
Chromatography data management system report
Chromatographic efficiency
Qualitative analysis
Retention parameters
Relative retention
Retention indices
Gas chromatography
High-performance liquid and supercritical fluid chromatography
Retention and molecular structure
Chemical methods
Peak trapping and off-line spectrometric methods
Selective detectors
Coupled techniques
Quantitative analysis
Calibration procedures
Normalization
External calibration
Internal standard
Standard addition
Worked examples
Case 1. The gas chromatographic determination of xylenes in a commercial mixture
Case 2. The characterization of a vegetable oil by gas chromatographic determination of fatty acid content.
Case 3. Determination of nicotinic acid in instant coffee
Case 4. Determination of bromate in bread dough
Case 5. The determination of polychlorinated biphenyls in environmental samples
Case 6. The determination of ethanol in a blood sample
Case 7. The determination of cocaine
Case 8. The determination of caffeine and theobromine in chocolate products
What can be done if no analyte is detected?
Metabolomics and chromatography
Measurement of analytical signal
Separation
Gas chromatography
Liquid chromatography
Supercritical fluid chromatography
Two-dimensional chromatography
Detection
Data handling
Peak detection
Peak alignment
Normalization
Compound annotation
Chemometrics
Applications
References
Sample handling in chromatography
Introduction
Why bother with sample handling?
Sample collection procedures
Sustainable green chemistry
Sample preparation
Solvent extraction
Efficiency in liquid-liquid extraction
Selection of extracting solvent
Extraction modes
Batch extraction
Continuous extraction
Countercurrent extraction
Extraction of solid samples
Supercritical fluid extraction
Instrumentation
Selecting a supercritical fluid and extraction conditions
Microwave- and sonication-assisted solvent extraction
Accelerated solvent extraction
Membrane-assisted techniques
Filtration
Microfiltration
Ultrafiltration (and nanofiltration)
Reverse osmosis
Dialysis
Volatilization processes
Sublimation
Freeze drying
Distillation
Fractional distillation
Steam distillation
Assisted co-distillation
Chromatography
Columns
Separation mechanisms
Adsorption
Column packings
Mobile phase
Ion Exchange
Size Exclusion
Solid-phase extraction
Modes of operation
Applications
Microextraction techniques
Pre-concentration techniques
References
Preparative chromatography
Introduction
History
Theoretical considerations
Thin layer chromatography
Plates for PTLC
Sample application
Mobile phases
Layer development
Visualization
Applications
Gas chromatography
Instrumentation
Applications
Supercritical fluid chromatography
Instrumentation
Applications
High-performance liquid chromatography
Instrumentation
Separations
Applications
References
Index
A
B
C
D
E
F
G
H
I
K
L
M
N
O
P
Q
R
S
T
U
V
W
Z
