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Praxis der Hochleistungs-Flussigchromatographie

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ISBN-10: 0470682175

ISBN-13: 9780470682173

Edition: 5th 2010

Authors: Veronika R. Meyer

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This textbook aims to present the knowledge which is necessary for everyday HPLC measurements to be made, in a detailed and easy-to-follow manner. It contains a wealth of practical material and covers a wide range of subjects. Topics covered include principles, instrumentation, reverse-phase, ion-exchange, ion-pair, ion, size-exclusion and affinity chromatography, as well as analytical methods, preparative HPLC and enantiomeric separations. Appendices provide information on instrument testing, troubleshooting, column-packing.
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Book details

Edition: 5th
Copyright year: 2010
Publisher: John Wiley & Sons, Limited
Publication date: 4/9/2010
Binding: Paperback
Pages: 426
Size: 6.25" wide x 9.25" long x 1.00" tall
Weight: 1.386
Language: English

Preface to the Fifth Edition
Important and Useful Equations for HPLC
HPLC: A powerful separation method
A first HPLC experiment
Liquid chromatographic separation modes
The HPLC instrument
Safety in the HPLC laboratory
Comparison between high-performance liquid chromatography and gas chromatography
Comparison between high-performance liquid chromatography and capillary electrophoresis
Units for pressure, length and viscosity
Scientific journals
Recommended books
Theoretical Principles
The chromatographic process
Band broadening
The chromatogram and its purport
Graphical representation of peak pairs with different degree of resolution
Factors affecting resolution
Extra-column volumes (dead volumes)
Peak capacity and statistical resolution probability
Effects of temperature in HPLC
The limits of HPLC
How to obtain peak capacity
General requirements
The short-stroke piston pump
Maintenance and repair
Other pump designs
Preparation of Equipment up to Sample Injection
Selection of the mobile phase
Preparation of the mobile phase
Gradient systems
Capillary tubing
Sample injectors
Sample solution and sample volume
Solvent Properties
Table of organic solvents
Solvent selectivity
Shelf life of mobile phases
The mixing cross
UV detectors
Refractive index detectors
Fluorescence detectors
Electrochemical (amperometric) detectors
Light-scattering detectors
Other detectors
Multiple detection
Indirect detection
Coupling with spectroscopy
Columns and Stationary Phases
Columns for HPLC
General properties of stationary phases
Chemically modified silica
Some other stationary phases
Column care and regeneration
HPLC Column Tests
Simple tests for HPLC columns
Determination of particle size
Determination of breakthrough time
The test mixture
Dimensionless parameters for HPLC column characterization
The van Deemter equation from reduced parameters and its use in column diagnosis
van Deemter curves and other coherences
Diffusion coefficients
Adsorption Chromatography: Normal-Phase Chromatography
What is adsorption?
The eluotropic series
Selectivity properties of the mobile phase
Choice and optimization of the mobile phase
Reversed-Phase Chromatography
Mobile phases in reversed-phase chromatography
Solvent selectivity and strength
Stationary phases
Method development in reversed-phase chromatography
Hydrophobic interaction chromatography
Chromatography with Chemically Bonded Phases
Properties of some stationary phases
Hydrophilic interaction chromatography
Ion-Exchange Chromatography
Properties of ion exchangers
Influence of the mobile phase
Special possibilities of ion exchange
Practical hints
Ion-Pair Chromatography
Ion-pair chromatography in practice
Appendix: UV detection using ion-pair reagents
Ion Chromatography
Suppression techniques
Phase systems
Size-Exclusion Chromatography
The calibration chromatogram
Molecular mass determination by means of size-exclusion chromatography
Coupled size-exclusion columns
Phase systems
Affinity Chromatography
Affinity chromatography as a special case of HPLC
Choice of Method
The various possibilities
Method transfer
Solving the Elution Problem
The elution problem
Solvent gradients
Column switching
Comprehensive two-dimensional HPLC
Optimization of an isocratic chromatogram using four solvents
Optimization of the other parameters
Mixed stationary phases
Analytical HPLC
Qualitative analysis
Trace analysis
Quantitative analysis
Peak-height and peak-area determination for quantitative analysis
Integration errors
The detection wavelength
Unexpected peaks: Ghost and system peaks
Quality Assurance
Is it worth the effort?
Verification with a second method
Method validation
Standard operating procedures
Measurement uncertainty
Qualifications, instrument test and system suitability test
The quest for quality
Preparative HPLC
Preparative HPLC in practice
Overloading effects
Fraction collection
Displacement chromatography
Separation of Enantiomers
Chiral mobile phases
Chiral liquid stationary phases
Chiral solid stationary phases
Indirect separation of enantiomers
Special Possibilities
Micro, capillary and chip HPLC
High-speed and super-speed HPLC
Fast separations at 1000 bar: UHPLC
HPLC with supercritical mobile phases
HPLC with superheated water
Applied HPLC Theory
How to Perform the Instrument Test
Test sequence
Pump test
UV detector test
Autosampler test
Column oven test
Equations and calculations
Pressure problems
Leak in the pump system
Deviating retention times
Injection problems
Baseline problems
Peak shape problems
Problems with light-scattering detectors
Other causes
Instrument test
Column Packing
Index of Separations
Subject Index