Modern Size-Exclusion Liquid Chromatography

Name: Modern Size-Exclusion Liquid Chromatography | Practice of Gel Permeation and Gel Filtration Chromatography
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Practice of Gel Permeation and Gel Filtration Chromatography

Andre Striegel Wallace W. Yau Joseph J. Kirkland Donald D. Bly(Autor*in)

Wiley (Verlag)

2. Auflage

Erschienen am 10. August 2009

496 Seiten

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978-0-470-44283-8 (ISBN)

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Inhalt

Intro
MODERN SIZE-EXCLUSION LIQUID CHROMATOGRAPHY
CONTENTS
Foreword
Preface
1 Background
1.1 Introduction
1.2 History
1.3 Utility of SEC
1.4 Molar Mass Averages and Molar Mass Distribution
1.5 Structure of The Book
References
2 Retention
2.1 Introduction
2.2 Solute Retention in LC
2.3 Solute Retention in SEC
2.4 SEC Retention Mechanism
2.5 Theoretical Models of SEC Separation
2.5.1 Hard-Sphere Solute Model
2.5.2 Rigid Molecules of Other Shapes
2.5.3 Random-Coil Solute Model
2.6 Other Considerations
2.6.1 Factors Influencing SEC Retention
2.6.2 Failure to Define an Effective Polymer Radius
2.6.3 Hydrodynamic Chromatography Effects in SEC
2.6.4 Slalom Chromatography Effects in SEC
References
3 Band Broadening
3.1 Introduction
3.1.1 Basic Column-Dispersion Processes
3.1.2 Peak Variance
3.2 LC Plate Theory
3.2.1 Basic Plate Theory
3.2.2 The van Deemter Equation
3.2.3 Flow-Diffusion Coupling
3.2.4 Reduced Plate Height
3.3 Mechanism of SEC Band Broadening
3.3.1 Experimental Verification
3.3.2 Rate Theory
3.3.3 Theoretical Inferences
3.4 Influencing Factors
3.4.1 Column Parameters
3.4.2 Kinetic Factors
3.4.3 Experimental Factors
3.5 Experimental Methods
3.5.1 Plate Number
3.5.2 Column-Dispersion Calibration
References
4 Resolution
4.1 Introduction
4.1.1 Chromatographic Resolution
4.1.2 Peak-Capacity Concept
4.2 Resolution Concept in SEC of Polymers
4.3 Molar Mass Accuracy Criterion
4.4 Applications of Column Performance Criteria
4.5 Pore Geometry and Operational Effects
4.5.1 Connecting Columns
4.5.2 Separation Capacity of Single Pores
4.5.3 Effect of Packing Pore-Size Distribution
4.5.4 Effect of Operating Parameters
References
5 Equipment
5.1 Introduction
5.2 Extra-Column Effects: General
5.3 Mobile-Phase Reservoirs, Inlet Filters, and Degassers
5.4 Solvent-Metering Systems (Pumps)
5.4.1 General Pump Specifications
5.4.2 Reciprocating Pumps
5.5 Sample Injectors and Autosamplers
5.6 Miscellaneous Hardware
5.7 Laboratory Safety
References
6 The Column
6.1 Introduction
6.2 Column Packings
6.2.1 Semirigid Organic Gels
6.2.2 Rigid Inorganic Packings
6.3 Column-Packing Methods
6.3.1 Particle Technology
6.3.2 Basis of Column-Packing Techniques
6.4 Column Performance
References
7 Experimental Variables and Techniques
7.1 Introduction
7.2 Solvent Effects
7.2.1 Sample Solubility
7.2.2 Other Solvent Effects
7.2.3 Flow-Rate Effects
7.2.4 Temperature Effects
7.3 Substrate Effects
7.4 Sample Effects
7.4.1 Sample Volume
7.4.2 Sample Weight or Concentration
7.5 Laboratory Techniques
7.6 Solvent Selection and Preparation
7.6.1 Convenience
7.6.2 Sample Type
7.6.3 Effect on Column Packing
7.6.4 Operation
7.6.5 Safety
7.6.6 Solvent Purification and Modification
7.7 Selection and Use of Standard Reference Materials
7.8 Detector Selection
7.9 Column Selection and Handling
7.9.1 Optimum Single Pore-Size Separations
7.9.2 Bimodal Pore-Size Separations: Optimum Linearity and Range
7.9.3 Other Column Selection Guidelines
7.9.4 Column Handling
7.10 Chromatographic Design Considerations
7.11 Making the Separation
7.11.1 Dissolving the Sample and Standards
7.11.2 Sample Solution Filtration
7.11.3 Sample Injection
7.11.4 Baseline Stability
7.11.5 Obtaining and Using a Chromatogram Baseline
7.12 Troubleshooting
7.12.1 Excessively High Pressure
7.12.2 Column Plugging
7.12.3 Air Bubbles and Leaks
7.12.4 Poor Resolution
7.12.5 Low Solute Recovery
7.12.6 Constancy of Separation
7.12.7 Peak Shape
References
8 Calibration
8.1 Introduction
8.2 Calibration with Narrow-MMD Standards
8.2.1 Peak-Position (Calibrant-Relative) Calibration
8.2.2 Universal Calibration
8.2.3 Mark-Houwink Calibration
8.3 Calibration with Broad-MMD Standards
8.3.1 Integral-MMD Method
8.3.2 Linear Calibration Methods
8.4 Accuracy of Calibration Methods
8.5 Actual Molar Mass Across the SEC Elution Curve
8.6 Linear Calibration Ranges
8.7 Recent Developments and Recommendations on Band-Broadening Correction
8.7.1 Algorithm for BBC in Conventional SEC Analysis with Only a Concentration-Sensitive Detector
8.7.2 Algorithm for BBC in Dual-Detector SEC Using an Online Static Light-Scattering Detector
8.7.3 Algorithm for BBC in Universal Calibration Using an Online Viscosity Detector
8.7.4 Algorithm for BBC in Triple-Detector SEC Using Online Static Light Scattering, Viscosity, and Concentration Detectors
References
9 Physical Detectors
9.1 Introduction
9.2 Concentration-Sensitive Detectors
9.2.1 Differential Refractometers
9.2.2 UV/Visible Detectors
9.2.3 Evaporative-Type Detectors
9.3 Static Light-Scattering Detection
9.3.1 Multiangle Light Scattering
9.3.2 Low-Angle Light Scattering
9.3.3 Off-Line, Batch-Mode MALS
9.3.4 Depolarized MALS
9.4 Quasielastic Light-Scattering Detection
9.4.1 QELS Instrumentation
9.5 Viscometric Detection
9.5.1 Single-Capillary Viscometers
9.5.2 Differential Viscometers
9.5.3 Intrinsic Viscosity and the Viscometric Radius
9.5.4 Viscometry Instrumentation
9.6 SEC(3)
References
10 Chemical Detectors
10.1 Introduction
10.2 Mass Spectrometry
10.2.1 Electrospray Ionization Mass Spectrometry
10.2.2 Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry
10.2.3 Inductively Coupled Plasma Mass Spectrometry
10.3 Fourier Transform Infrared Spectroscopy
10.3.1 FTIR as a Pseudophysical Detector: Short-Chain Branching Distribution of Polyolefins
10.3.2 FTIR as a Chemical Detector
10.3.3 Comparison of Online and Continuous Off-Line SEC/FTIR
10.4 Nuclear Magnetic Resonance Spectroscopy
10.5 Other Chemical Detectors
10.5.1 Ultraviolet Detection
10.5.2 Fluorescence
10.5.3 Conductivity
10.5.4 Dynamic Surface Tension Detection
10.5.5 Microscale Molecular Mass Sensor
10.6 Coupling of Chemical Detectors
References
11 Polymer Architecture and Dilute Solution Thermodynamics
11.1 Introduction
11.2 Long-Chain Branching
11.2.1 Quantitating the Long-Chain Branching Distribution by SEC/MALS
11.2.2 Qualitative and Semiquantitative Descriptions of the Long-Chain Branching Distribution by SEC/VISC
11.2.3 Average Molar Mass Between Long-Chain Branches
11.3 Determining the Short-Chain Branching Distribution
11.4 Polymer Architecture: Conformation and Topology
11.4.1 Determining the Fractal Dimension
11.4.2 Dimensionless Radii Ratios
11.4.3 Dimensionless Functions
11.4.4 Caveats Regarding Dimensionless Parameters
11.5 Star Polymers
11.6 Determining the Persistence Length
11.7 Determining the Characteristic Ratio
11.8 Local Polydispersity
References
12 Aqueous SEC
12.1 Introduction
12.2 Aqueous SEC Columns
12.3 Non-Size-Exclusion Effects and Mobile-Phase Additives
12.4 Select Applications of Aqueous SEC
12.4.1 Polysaccharides
12.4.2 Proteins and Peptides
12.4.3 Synthetic Polymers
12.4.4 Polyelectrolytes
12.4.5 Inorganic Compounds
References
13 Oligomeric SEC
13.1 Introduction
13.2 What is an Oligomer?
13.3 Preliminary Considerations
13.3.1 Advantages over Polymeric SEC
13.3.2 Difficulties as Compared to Polymeric SEC
13.4 Oligomeric SEC Columns
13.5 Select Applications of Oligomeric SEC
13.5.1 Characterization of Tackifiers, Resins, and Resin Prepolymers
13.5.2 Characterization of Antioxidant Lubricant Additives
13.5.3 Characterization and Quantitation of Plasticizers
13.5.4 Polymer Exemption Data
13.5.5 SEC of Oligosaccharides
13.5.6 Determining the Solution Conformational Entropy of Oligomers
13.5.7 Determining Molar Masses of Oligomers by SEC/MALS
13.6 Optimizing Resolution in Oligomeric SEC
References
14 SEC in 2D-LC Separations
14.1 Introduction
14.2 Principles of 2D Polymer Separations
14.2.1 Separation Angle and Percent Synentropy
14.3 Designing an Experimental 2D-LC Protocol
14.4 Eluent Transfer in 2D-LC
14.5 Stop-Flow SEC × LC
14.6 Select Applications of 2D-LC
14.6.1 HPLC
14.6.2 Liquid Chromatography at the Critical Condition
14.6.3 Other Methods
14.7 SEC in 3D Separations
References
15 Special Techniques
15.1 Introduction
15.2 Preparative SEC
15.2.1 Experimentation
15.2.2 Applications
15.3 Recycle SEC
15.3.1 Theory
15.3.2 Equipment
15.3.3 Uses of the Recycle Method
15.4 High-Speed SEC
15.5 Inverse SEC
15.6 Vacancy and Differential SEC
15.7 Size-Exclusion Electrochromatography
References
16 High-Temperature SEC and Rheological Connections
16.1 Introduction
16.2 High-Temperature SEC
16.2.1 HT-SEC Instrumentation
16.3 Complementarity of SEC and Rheology
16.3.1 Obtaining the MMD from Rheological Measurements
16.3.2 Obtaining Rheological Properties from SEC Measurements
16.3.3 Behavior of Dilute Oligomer Solutions
References
Symbols
Abbreviations
Index

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