Keywords:
Preparative layer chromatography.
;
Electronic books.
Type of Medium:
Online Resource
Pages:
1 online resource (651 pages)
Edition:
3rd ed.
ISBN:
9783527816316
URL:
https://ebookcentral.proquest.com/lib/geomar/detail.action?docID=6109526
DDC:
615.1901
Language:
English
Note:
Cover -- Title Page -- Copyright -- Contents -- Preface -- About the Editors -- List of Abbreviations -- Notation -- Chapter 1 Introduction -- 1.1 Chromatography, Development, and Future Trends -- 1.2 Focus of the Book -- 1.3 Suggestions on How to Read this Book -- References -- Chapter 2 Fundamentals and General Terminology -- 2.1 Principles and Features of Chromatography -- 2.2 Analysis and Description of Chromatograms -- 2.2.1 Voidage and Porosity -- 2.2.2 Retention Times and Capacity Factors -- 2.2.3 Efficiency of Chromatographic Separations -- 2.2.4 Resolution -- 2.2.5 Pressure Drop -- 2.3 Mass Transfer and Fluid Dynamics -- 2.3.1 Principles of Mass Transfer -- 2.3.2 Fluid Distribution in the Column -- 2.3.3 Packing Nonidealities -- 2.3.4 Extra‐Column Effects -- 2.4 Equilibrium Thermodynamics -- 2.4.1 Definition of Isotherms -- 2.4.2 Models of Isotherms -- 2.4.2.1 Single‐Component Isotherms -- 2.4.2.2 Multicomponent Isotherms Based on the Langmuir Model -- 2.4.2.3 Competitive Isotherms Based on the Ideal Adsorbed Solution Theory -- 2.4.2.4 Steric Mass Action Isotherms -- 2.4.3 Relation Between Isotherms and Band Shapes -- 2.5 Column Overloading and Operating Modes -- 2.5.1 Overloading Strategies -- 2.5.2 Beyond Isocratic Batch Elution -- References -- Chapter 3 Stationary Phases -- 3.1 Survey of Packings and Stationary Phases -- 3.2 Inorganic Sorbents -- 3.2.1 Activated Carbons -- 3.2.2 Synthetic Zeolites -- 3.2.3 Porous Oxides: Silica, Activated Alumina, Titania, Zirconia, and Magnesia -- 3.2.4 Silica -- 3.2.4.1 Surface Chemistry -- 3.2.4.2 Mass Loadability -- 3.2.5 Diatomaceous Earth -- 3.2.6 Reversed Phase Silicas -- 3.2.6.1 Silanization of the Silica Surface -- 3.2.6.2 Silanization -- 3.2.6.3 Starting Silanes -- 3.2.6.4 Parent Porous Silica -- 3.2.6.5 Reaction and Reaction Conditions -- 3.2.6.6 Endcapping.
,
3.2.6.7 Chromatographic Characterization of Reversed Phase Silicas -- 3.2.6.8 Chromatographic Performance -- 3.2.6.9 Hydrophobic Properties Retention Factor (Amount of Organic Solvent for Elution), Selectivity -- 3.2.6.10 Shape Selectivity -- 3.2.6.11 Silanol Activity -- 3.2.6.12 Purity -- 3.2.6.13 Improved pH Stability Silica -- 3.2.7 Aluminum Oxide -- 3.2.8 Titanium Dioxide -- 3.2.9 Other Oxides -- 3.2.9.1 Magnesium Oxide -- 3.2.9.2 Zirconium Dioxide -- 3.2.10 Porous Glasses -- 3.3 Cross‐Linked Organic Polymers -- 3.3.1 General Aspects -- 3.3.2 Hydrophobic Polymer Stationary Phases -- 3.3.3 Hydrophilic Polymer Stationary Phases -- 3.3.4 Ion Exchange (IEX) -- 3.3.4.1 Optimization of Ion‐Exchange Resins -- 3.3.5 Mixed Mode -- 3.3.6 Hydroxyapatite -- 3.3.7 Designed Adsorbents -- 3.3.7.1 Protein A Affinity Sorbents -- 3.3.7.2 Other IgG Receptor Proteins: Protein G and Protein L -- 3.3.7.3 Sorbents for Derivatized/Tagged Compounds: Immobilized Metal Affinity Chromatography (IMAC) -- 3.3.7.4 Other Tag‐Based Affinity Sorbents -- 3.3.8 Customized Adsorbents -- 3.3.8.1 Low Molecular Weight Ligands -- 3.3.8.2 Natural Polymers (Proteins, Polynucleotides) -- 3.3.8.3 Artificial Polymers -- 3.4 Advective Chromatographic Materials -- 3.4.1 Adsorptive Membranes and Grafted‐Polymer Membranes -- 3.4.2 Adsorptive Nonwovens -- 3.4.3 Fiber/Particle Composites -- 3.4.4 Area‐Enhanced Fibers -- 3.4.5 Monolith -- 3.4.6 Chromatographic Materials for Larger Molecules -- 3.5 Chiral Stationary Phases -- 3.5.1 Cellulose‐ and Amylose‐Based CSP -- 3.5.2 Antibiotic CSP -- 3.5.3 Cyclofructan‐Based CSP -- 3.5.4 Synthetic Polymers -- 3.5.5 Targeted Selector Design -- 3.5.6 Further Developments -- 3.6 Properties of Packings and Their Relevance to Chromatographic Performance -- 3.6.1 Chemical and Physical Bulk Properties -- 3.6.2 Morphology.
,
3.6.3 Particulate Adsorbents: Particle Size and Size Distribution -- 3.6.4 Pore Texture -- 3.6.5 Pore Structural Parameters -- 3.6.6 Comparative Rating of Columns -- 3.7 Sorbent Maintenance and Regeneration -- 3.7.1 Cleaning in Place (CIP) -- 3.7.2 CIP for IEX -- 3.7.3 CIP of Protein A Sorbents -- 3.7.4 Conditioning of Silica Surfaces -- 3.7.5 Sanitization in Place (SIP) -- 3.7.6 Column and Adsorbent Storage -- References -- Chapter 4 Selection of Chromatographic Systems -- 4.1 Definition of the Task -- 4.2 Mobile Phases for Liquid Chromatography -- 4.2.1 Stability -- 4.2.2 Safety Concerns -- 4.2.3 Operating Conditions -- 4.2.4 Aqueous Buffer Systems -- 4.3 Adsorbent and Phase Systems -- 4.3.1 Choice of Phase System Dependent on Solubility -- 4.3.2 Improving Loadability for Poor Solubilities -- 4.3.3 Dependency of Solubility on Sample Purity -- 4.3.4 Generic Gradients for Fast Separations -- 4.4 Criteria for Choosing Normal Phase Systems -- 4.4.1 Retention in NP Systems -- 4.4.2 Solvent Strength in Liquid-Solid Chromatography -- 4.4.3 Pilot Technique Thin‐Layer Chromatography Using the PRISMA Model -- 4.4.3.1 Step (1): Solvent Strength Adjustment -- 4.4.3.2 Step (2): Optimization of Selectivity -- 4.4.3.3 Step (3): Final Optimization of the Solvent Strength -- 4.4.3.4 Step (4): Determination of the Optimum Mobile Phase Composition -- 4.4.4 Strategy for an Industrial Preparative Chromatography Laboratory -- 4.4.4.1 Standard Gradient Elution Method on Silica -- 4.4.4.2 Simplified Procedure -- 4.5 Criteria for Choosing Reversed Phase Systems -- 4.5.1 Retention and Selectivity in RP Systems -- 4.5.2 Gradient Elution for Small Amounts of Product on RP Columns -- 4.5.3 Rigorous Optimization for Isocratic Runs -- 4.5.4 Rigorous Optimization for Gradient Runs -- 4.5.5 Practical Recommendations -- 4.6 Criteria for Choosing CSP Systems.
,
4.6.1 Suitability of Preparative CSP -- 4.6.2 Development of Enantioselectivity -- 4.6.3 Optimization of Separation Conditions -- 4.6.3.1 Determination of Racemate Solubility -- 4.6.3.2 Selection of Elution Order -- 4.6.3.3 Optimization of Mobile/Stationary Phase Composition, Including Temperature -- 4.6.3.4 Determination of Optimum Separation Step -- 4.6.4 Practical Recommendations -- 4.7 Downstream Processing of mAbs Using Protein A and IEX -- 4.8 Size‐Exclusion Chromatography (SEC) -- 4.9 Overall Chromatographic System Optimization -- 4.9.1 Conflicts During Optimization of Chromatographic Systems -- 4.9.2 Stationary Phase Gradients -- References -- Chapter 5 Process Concepts -- 5.1 Discontinuous Processes -- 5.1.1 Isocratic Operation -- 5.1.2 Gradient Chromatography -- 5.1.3 Closed‐Loop Recycling Chromatography -- 5.1.4 Steady‐State Recycling Chromatography (SSRC) -- 5.1.5 Flip‐Flop Chromatography -- 5.1.6 Chromatographic Batch Reactors -- 5.2 Continuous Processes -- 5.2.1 Column Switching Chromatography -- 5.2.2 Annular Chromatography -- 5.2.3 Multiport Switching Valve Chromatography (ISEP/CSEP) -- 5.2.4 Isocratic Simulated Moving Bed (SMB) Chromatography -- 5.2.5 SMB Chromatography with Variable Process Conditions -- 5.2.5.1 Varicol -- 5.2.5.2 PowerFeed -- 5.2.5.3 Partial‐Feed, Partial‐Discard, and Fractionation‐Feedback Concepts -- 5.2.5.4 Improved/Intermittent SMB (iSMB) -- 5.2.5.5 Modicon -- 5.2.5.6 FF‐SMB -- 5.2.6 Gradient SMB Chromatography -- 5.2.7 Supercritical Fluid Chromatography (SFC) -- 5.2.7.1 Supercritical Batch Chromatography -- 5.2.7.2 Supercritical SMB processes -- 5.2.8 Multicomponent Separations -- 5.2.9 Multicolumn Systems for Bioseparations -- 5.2.9.1 Multicolumn Capture Chromatography (MCC) -- 5.2.9.2 Multicolumn Countercurrent Solvent Gradient Purification (MCSGP) -- 5.2.10 Countercurrent Chromatographic Reactors.
,
5.2.10.1 SMB Reactor -- 5.2.10.2 SMB Reactors with Distributed Functionalities -- 5.3 Choice of Process Concepts -- 5.3.1 Scale -- 5.3.2 Range of k′ -- 5.3.3 Number of Fractions -- 5.3.4 Example 1: Lab Scale -- Two Fractions -- 5.3.5 Example 2: Lab Scale -- Three or More Fractions -- 5.3.6 Example 3: Production Scale -- Wide Range of k′ -- 5.3.7 Example 4: Production Scale -- Two Main Fractions -- 5.3.8 Example 5: Production Scale -- Three Fractions -- 5.3.9 Example 6: Production Scale -- Multistage Process -- References -- Chapter 6 Modeling of Chromatographic Processes -- 6.1 Introduction -- 6.2 Models for Single Chromatographic Columns -- 6.2.1 Equilibrium Stage Models -- 6.2.1.1 Discontinuous Model According to Craig -- 6.2.1.2 Continuous Model According to Martin and Synge -- 6.2.2 Derivation of Continuous Mass Balance Equations -- 6.2.2.1 Mass Balance Equations -- 6.2.2.2 Convective Transport -- 6.2.2.3 Axial Dispersion -- 6.2.2.4 Intraparticle Diffusion -- 6.2.2.5 Mass Transfer Between Phases -- 6.2.2.6 Finite Rates of Adsorption and Desorption -- 6.2.2.7 Adsorption Equilibria -- 6.2.3 Equilibrium Model of Chromatography -- 6.2.4 Models with One Band Broadening Effect -- 6.2.4.1 Equilibrium Dispersion Model -- 6.2.4.2 Finite Adsorption Rate Model -- 6.2.5 Continuous Lumped Rate Models -- 6.2.5.1 Transport Dispersion Models -- 6.2.5.2 Lumped Finite Adsorption Rate Model -- 6.2.6 General Rate Models -- 6.2.7 Initial and Boundary Conditions of the Column -- 6.2.8 Dimensionless Model Equations -- 6.2.9 Comparison of Different Model Approaches -- 6.3 Including Effects Outside the Columns -- 6.3.1 Experimental Setup and Simulation Flow Sheet -- 6.3.2 Modeling Extra‐Column Equipment -- 6.3.2.1 Injection System -- 6.3.2.2 Piping -- 6.3.2.3 Detector -- 6.4 Calculation Methods and Software -- 6.4.1 Analytical Solutions.
,
6.4.2 Numerical Solution Methods.
Permalink