Chromatography Books

Book SynopsisGas chromatography is widely used in applications involving food analysis. Typical applications pertain to the quantitative and/or qualitative analysis of food composition, natural products, food additives, and flavour and aroma components. Providing an up-to-date look at the significant advances in the technology, this book includes details on novel sample preparation processes; conventional, high-speed multidimensional gas chromatography systems, including preparative instrumentation; gas chromatography–olfactometry principles; and, finally, chemometrics principles and applications in food analysis. Aimed at providing the food researcher or analyst with detailed analytical information related to advanced gas chromatography technologies, this book is suitable for professionals and postgraduate students learning about the technique in the food industry and research.Table of ContentsHeadspace Sampling: An "Evergreen" Method in Constant Evolution to Characterize Food Flavors through their Volatile Fraction; Sample Preparation for the Gas Chromatography Analysis of Semi-volatiles and Non-volatile Compounds in Food Samples; Conventional Gas Chromatography: Basic Principles and Instrumental Aspects; Conventional Gas Chromatography: Mass Spectrometry Hyphenation and Applications in Food Analysis; High-speed Gas Chromatography: Basic Theory, General Principles, Practical Aspects and Food Analysis; Heart-cutting Two-dimensional Gas Chromatography; Comprehensive Two-dimensional Gas Chromatography; Multidimensional LC-GC; Gas Chromatography-Olfactometry: Principles, Practical Aspects and Applications in Food Analysis; Chemometrics: Basic Principles and Applications

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Book SynopsisHigh-temperature liquid chromatography has attracted much interest in recent years but has not yet recognized its full potential in the chromatographic community. There is a widespread reluctance in industry to use temperature to speed up the separation process, influence the selectivity of a separation or implement novel detection techniques. However, the technology has now matured and could revolutionize chromatography as we see it today. Better equipment, such as heating systems able to generate faster heating rates, is becoming more readily available. Also, columns based on silica gel, which can withstand higher temperatures for an extended period, are now being introduced. Nevertheless, further technological and methodical efforts are needed to establish the method in a regulated environment like the pharmaceutical industry. This is the only text to cover all the practical aspects, as well as the underlying theoretical principles, of setting up an HPLC system for high temperature operation. It is not intended solely for academics but will also benefit the researcher interested in more practical considerations. The author is a recognized expert and has conducted several studies with partners from industry to validate the method. Many real examples from these studies have been included in the book. The aim is to support practitioners in the creation of their own protocols without the need to rely solely on trial and error. The book starts with a brief definition of high temperature liquid chromatography before going on to cover: system set up; the heating system; mobile phase considerations; suitable stationary phases; method development using temperature programming; analyte stability, and special hyphenation techniques using superheated water as a mobile phase. In each chapter, experimental data is used to illustrate the main statements and the advantages over conventional HPLC are evaluated. The book concludes with a critical outlook on further developments and applications underlining the necessary advances needed to make high temperature HPLC more robust.Trade ReviewHigh-temperature liquid chromatography has attracted much interest in recent years but has not yet recognized its full potential in the chromatographic community. There is a widespread reluctance in industry to use temperature to speed up the separation process, influence the selectivity of a separation or implement novel detection techniques. However, the technology has now matured and could revolutionize chromatography as we see it today. Better equipment, such as heating systems able to generate faster heating rates, is becoming more readily available. Also, columns based on silica gel, which can withstand higher temperatures for an extended period, are now being introduced. Nevertheless, further technological and methodical efforts are needed to establish the method in a regulated environment like the pharmaceutical industry. This is the only text to cover all the practical aspects, as well as the underlying theoretical principles, of setting up an HPLC system for high-temperature operation. It is not intended solely for academics but will also benefit the researcher interested in more practical considerations. The author is a recognized expert and has conducted several studies with partners from industry to validate the method. Many real examples from these studies have been included in the book. The aim is to support practitioners in the creation of their own protocols without the need to rely solely on trial and error. The book starts with a brief definition of high-temperature liquid chromatography before going on to cover: system set up; the heating system; mobile phase considerations; suitable stationary phases; method development using temperature programming; analyte stability, and special hyphenation techniques using superheated water as a mobile phase. In each chapter, experimental data is used to illustrate the main statements and the advantages over conventional HPLC are evaluated. The book concludes with a critical outlook on further developments and applications underlining the necessary advances needed to make high-temperature HPLC more robust.Table of ContentsA brief definition of high-temperature liquid chromatography; System set up for high temperature liquid chromatography; The heating system; Mobile phase considerations; Suitable stationary phases; Method development using temperature programming Analyte stability; Special hyphenation techniques using superheated water as a mobile phase; A critical outlook

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Book SynopsisThe concept of a metabolic profile was introduced in 1971, when gas chromatography demonstrated a range of compounds present in human samples. Now termed metabolomics, the field is still emerging, and chromatography remains an essential tool for determining metabolites in a living system. This is the first book to present the chromatographic techniques used in metabolomics in a fundamental way. Sample preparation and quality control are described in detail, and all forms of chromatography applied to metabolomics are included. The editors present guidelines on selecting the most appropriate methodology, making the book an accessible guide to anyone entering the field. Handling data and applications are also described. This is an essential handbook for any laboratory looking to embark on a metabolomics research programme and includes the fundamentals of chromatography alongside the latest developments in the field.Trade ReviewBook’s topic Chromatographic Methods in Metabolomics is the 19th book in the series “RSC Chromatography Monographs”. This monograph focuses on descriptions of important experimental aspects of metabolomics studies that use chromatography methods, including gas chromatography (GC) and liquid chromatography (LC), and other types of separation, including capillary electrophoresis (CE) and microchip technology. Detailed discussions are included of sample collection and preparation, data processing, and examples of applications of the techniques described. The editors state that the aim of the book was to give the reader an overview of chromatographic and electromigration techniques, and to provide practical guidelines for selecting the appropriate technique. Contents The book is 232 pages long and contains nine chapters. Chapter 1 introduces, in brief, the experimental workflow and analytical methods used in metabolomics studies. Chapter 2 describes the methods and techniques used in collecting and preparing a range of sample types, including mammalian biofluids, faecal samples, cells, and tissues. Techniques covered include quenching of materials, homogenisation, extraction, sample fractionation, and derivatisation for GC and LC. Chapter 3 discusses the mass spectrometry (MS) instruments used, including descriptions of the interfaces used to couple MSto GC, LC and CE, and comparisons of the mass analysers used. This chapter also discusses metabolite identification and fluxomics. Chapters 4–6 introduce the separation techniques used in metabolomics. Chapter 4 describes liquid chromatography techniques, including HPLC, UPLC, capillary LC, multi-dimensional LC, turbulent flow LC and supercritical fluid chromatography. Modes of liquid chromatography are also discussed. Chapter 5 introduces the techniques of GC–MS and GC×GC–MS, and includes discussions of sample collection for volatiles analysis and metabolite identification. Chapter 6 introduces capillary electromigration, with specific focus on CE, and includes descriptions of the interfaces used to couple CE to MS. Chapter 7 introduces innovative recent work on microchip fabrication and applications, including use of microchips for sample preparation, LC and CE. Chapter 8 discusses data handling, with emphasis on peak detection, alignment and deconvolution followed by normalisation and quantification. Chapter 9 describes specific applications of the techniques discussed in the previous chapters, with a focus on global profiling or targeted analysis of lipids or polar metabolites. Comparison with the existing literature This monograph adds to the growing number of recent textbooks and review articles focussing on the tools used in metabolomics and on the applications of metabolomics in biological sciences. Most other textbooks and review articles provide a detailed overview of either a broader (metabolomics in general) or narrower (e.g. GC–MS) range of metabolomics techniques and applications, with some including detailed procedures for the topics discussed. This monograph is unique in providing the first focused description of a specific range of chromatographic and separation techniques, thus enabling the reader to research each topic and choose appropriate techniques by consulting a single source. Critical assessment This is a general textbook on the metabolomics applications of chromatographic and separation methods, including GC, LC and CE as well as the emerging field of microfluidics and microchip fabrication. The contributing authors are global leaders in their field, with five of nine chapters written by Finnish authors. Each chapter provides a descriptive overview of a topic, and includes information on the important aspects researchers should consider. This approach achieves the editorial objective of enabling the reader to understand the principles and to make decisions regarding the appropriate techniques to use in their research. In several chapters, a greater diversity and number of references describing the research of global leaders in the field would have enabled the reader to research the experimental procedures in more depth. Some topics, namely quality control and metabolite information, are discussed in multiple chapters, and providing more focused and expansive chapters on these subjects would have been beneficial. Summary Chromatographic Methods in Metabolomics is a monograph providing overviews of separation techniques used in metabolomic studies, and of associated sample collection, sample preparation and data processing. Each chapter is written by an expert in the field, and all chapters are written with clarity and focus. The book is a single-source reference work, enabling the reader to understand the important aspects of each topic and providing the information necessary for the reader to investigate the chapter topics in more depth. The work would be an important addition to the bookshelf of under-graduate, post-graduate and post-doctoral scientists starting a research role applying metabolomics. -- Warwick B. Dunn * Analytical and Bioanalytical Chemistry - # Springer-Verlag Berlin Heidelberg 2013 *Tuulia Hyotylainen and Susanne Wiedmer have written and edited an excellent book on a very bold subject area that holds something for everyone. They have managed to get key workers to write chapters, which they have blended in with their own so that the book gives information suitable for a novice but also sufficient detail for an expert. I liked the way the editors have tackled the subjects full on and have written the very difficult chapters themselves and what could be more challenging in this respect than sample preparation. This they address in the first real chapter after the introduction. Of course it is not a full, all-encompassing description, you could write a whole book on this, but they have done an excellent job of condensing the topic to get the basic points across and extending these points in greater detail for the critical issues. An expert will read this and find holes in some of the methods described but they may also find new points that they have not considered. A novice will find the whole chapter very interesting; I did, but if I have a single complaint I would have liked to have seen more on the quality control of samples. An early chapter is on detection in metabolomics and of course the detector is the mass spectrometer. Hyotylainen and Wiedmer have avoided the easy trap of describing each type of mass spectrometer in detail; instead they describe the advantages and disadvantages of the various types and ionisation sources that become important for understanding the later chapters. In the chapter on techniques the authors have done a great job in bringing together the vast array of chromatographic techniques that are now available, assuming you have sufficient funds to buy them. Again another excellent chapter that describes the usefulness of the various techniques in metabolomics as opposed to describing the full technical details of each technique. I think a difficult chapter to have written is the one on gas chromatography in metabolomics. The scope for GCmetabolomics, as the authors point out, may not be as extensive as metabolomics in the liquid phase as it is limited to the analysis of small volatile metabolites but it can still provide excellent data for fingerprinting and profiling. The authors have tackled this well and although they do, as you might expect repeat areas already covered, they go into new details on GCxGC. The description of capillary electromigration and microchip technology work well together. The chapter on microchips contains many nice coloured photographs but it was rather like reading the menu at a Michelin Star restaurant without eating the food. The chapter describes many chips and platforms but, although much has been written about research using microchips in the last twenty years, the number of real commercial chips capable of providing real data is very small. This chapter does not provide the data we are all looking for but maybe like other papers on the subject it is a pointer to the future. If there is a chapter that is too short and does not provide sufficient information it is the one on data handing. As the authors point out, it is not possible to give a complete account of data handling that is required in this area, but I was left wanting to know more about the different techniques that are being used today, their limitations and how, using more and more powerful and new visual displays and virtual reality displays, we are moving forward. The last chapter is on applications. I was pleased that this was a small chapter. It is all too easy to do a literature search and print pages and pages of applications. The authors have not done this, they have carefully selected application areas, described key points and given sufficient references for the reader to find the extensive papers associated with each area. As you may have gathered, I liked this book and recommend it for both your own library, for your research lab and as a good book to recommend to anyone starting out in this very extensive but exciting field. -- Peter Myers, University of Liverpool * Chromatographia, 2014, 77:1405–1406 *"Tuulia Hyotylainen and Susanne Wiedmer have written and edited an excellent book on a very bold subject area that holds something for everyone. They have managed to get key workers to write chapters, which they have blended in with their own so that the book gives information suitable for a novice but also sufficient detail for an expert...I liked this book and recommend it for both your own library, for your research lab and as a good book to recommend to anyone starting out in this very extensive but exciting field." -- Peter Myers, University of Liverpool * Chromatographia *Table of ContentsIntroduction; Sample Preparation; Liquid Chromatographic Methods in Metabolomics; Gas Chromatographic Methods in Metabolomics; Capillary electromigration techniques in metabolomics; Miniaturized Techniques in Metabolomics; Quality Control; Data Handling; Applications

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Book SynopsisGuiding chromatographers working in regulated industries and helping them to validate their chromatography data systems to meet data integrity, business and regulatory needs. This book is a detailed look at the life cycle and documented evidence required to ensure a system is fit for purpose throughout the lifecycle. Initially providing the regulatory, data integrity and system life cycle requirements for computerised system validation, the book then develops into a guide on planning, specifying, managing risk, configuring and testing a chromatography data system before release. This is followed by operational aspects such as training, integration and IT support and finally retirement. All areas are discussed in detail with case studies and practical examples provided as appropriate. The book has been carefully written and is right up to date including recently released FDA data integrity guidance. It provides detailed guidance on good practice and expands on the first edition making it an invaluable addition to a chromatographer’s book shelf.Table of ContentsHow To Use This Book; What is a CDS and its Evolution; Laboratory Informatics and the Role of a CDS; Applicable GXP Regulations and Guidance; Concepts of Computer Validation; Understanding Life Cycles and SW Classification; CDS Data Integrity; CSV Risk Management: System Risk; Working Electronically; Specifying User and System Requirements; Controlling the Validation; System Selection; Auditing the Supplier; Negotiating the Contract and System Purchase; Planning the Installation; CSV Risk Management; Importance of the Traceability Matrix; Writing the Configuration Specification; Writing the Technical Specification; Installing and Integrating System Components; Designing the Test Suite; Writing Test Cases; Executing Test Scripts; User Training and System Documentation; IT Support; System Description; Defining CDS Raw Data and E-Records; Validation Summary Report; Integration in a Regulated Environment; User Account Management; Incident and Problem Management; Change Control and Configuration Management; On-Going IT Support; Conducting a Periodic Review; CDS Records Retention; System Retirement; Data Migration Options; Retrospective Validation

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Book SynopsisThe third edition of this popular work is revised to include the latest developments in this fast-changing field. Its interdisciplinary approach elegantly combines the chemistry and engineering to explore the fundamentals and optimization processes involved.Trade Review"I would not hesitate to recommend it to anyone working in this field." Chromatographia "Overall the coverage is a bit uneven - nevertheless the volume does compile some useful material... In conclusion, this is a comprehensive reference text, which should find its way into the libraries of all companies who are serious about process scale preparative chromatography, whether internally or via outsource contracts." Organic Process Research and Development "This special volume is essential for chemists and engineers working in chemical and pharmaceutical industries, as well as for food technologies, due to the interdisciplinary nature of these preparative chromatographic processes." Advances in Food SciencesTable of ContentsPreface xv About the Editors xvii List of Abbreviations xix Notation xxiii 1 Introduction 1Henner Schmidt-Traub and Reinhard Ditz 1.1 Chromatography, Development, and Future Trends 1 1.2 Focus of the Book 4 1.3 Suggestions on How to Read this Book 4 References 6 2 Fundamentals and General Terminology 9Andreas Seidel-Morgenstern 2.1 Principles and Features of Chromatography 9 2.2 Analysis and Description of Chromatograms 13 2.2.1 Voidage and Porosity 13 2.2.2 Retention Times and Capacity Factors 16 2.2.3 Efficiency of Chromatographic Separations 17 2.2.4 Resolution 20 2.2.5 Pressure Drop 23 2.3 Mass Transfer and Fluid Dynamics 25 2.3.1 Principles of Mass Transfer 25 2.3.2 Fluid Distribution in the Column 27 2.3.3 Packing Nonidealities 28 2.3.4 Extra-Column Effects 29 2.4 Equilibrium Thermodynamics 29 2.4.1 Definition of Isotherms 29 2.4.2 Models of Isotherms 31 2.4.2.1 Single-Component Isotherms 31 2.4.2.2 Multicomponent Isotherms Based on the Langmuir Model 33 2.4.2.3 Competitive Isotherms Based on the Ideal Adsorbed Solution Theory 34 2.4.2.4 Steric Mass Action Isotherms 37 2.4.3 Relation Between Isotherms and Band Shapes 38 2.5 Column Overloading and Operating Modes 44 2.5.1 Overloading Strategies 44 2.5.2 Beyond Isocratic Batch Elution 45 References 46 3 Stationary Phases 49Michael Schulte 3.1 Survey of Packings and Stationary Phases 49 3.2 Inorganic Sorbents 50 3.2.1 Activated Carbons 50 3.2.2 Synthetic Zeolites 54 3.2.3 Porous Oxides: Silica, Activated Alumina, Titania, Zirconia, and Magnesia 54 3.2.4 Silica 55 3.2.4.1 Surface Chemistry 57 3.2.4.2 Mass Loadability 59 3.2.5 Diatomaceous Earth 59 3.2.6 Reversed Phase Silicas 60 3.2.6.1 Silanization of the Silica Surface 60 3.2.6.2 Silanization 60 3.2.6.3 Starting Silanes 61 3.2.6.4 Parent Porous Silica 61 3.2.6.5 Reaction and Reaction Conditions 62 3.2.6.6 Endcapping 62 3.2.6.7 Chromatographic Characterization of Reversed Phase Silicas 63 3.2.6.8 Chromatographic Performance 63 3.2.6.9 Hydrophobic Properties Retention Factor (Amount of Organic Solvent for Elution), Selectivity 65 3.2.6.10 Shape Selectivity 65 3.2.6.11 Silanol Activity 67 3.2.6.12 Purity 68 3.2.6.13 Improved pH Stability Silica 68 3.2.7 Aluminum Oxide 69 3.2.8 Titanium Dioxide 70 3.2.9 Other Oxides 71 3.2.9.1 Magnesium Oxide 71 3.2.9.2 Zirconium Dioxide 71 3.2.10 Porous Glasses 72 3.3 Cross-Linked Organic Polymers 73 3.3.1 General Aspects 74 3.3.2 Hydrophobic Polymer Stationary Phases 77 3.3.3 Hydrophilic Polymer Stationary Phases 78 3.3.4 Ion Exchange (IEX) 79 3.3.4.1 Optimization of Ion-Exchange Resins 81 3.3.5 Mixed Mode 88 3.3.6 Hydroxyapatite 88 3.3.7 Designed Adsorbents 91 3.3.7.1 Protein A Affinity Sorbents 91 3.3.7.2 Other IgG Receptor Proteins: Protein G and Protein L 96 3.3.7.3 Sorbents for Derivatized/Tagged Compounds: Immobilized Metal Affinity Chromatography (IMAC) 96 3.3.7.4 Other Tag-Based Affinity Sorbents 101 3.3.8 Customized Adsorbents 102 3.3.8.1 Low Molecular Weight Ligands 105 3.3.8.2 Natural Polymers (Proteins, Polynucleotides) 108 3.3.8.3 Artificial Polymers 111 3.4 Advective Chromatographic Materials 111 3.4.1 Adsorptive Membranes and Grafted-Polymer Membranes 114 3.4.2 Adsorptive Nonwovens 115 3.4.3 Fiber/Particle Composites 117 3.4.4 Area-Enhanced Fibers 117 3.4.5 Monolith 118 3.4.6 Chromatographic Materials for Larger Molecules 121 3.5 Chiral Stationary Phases 121 3.5.1 Cellulose- and Amylose-Based CSP 122 3.5.2 Antibiotic CSP 128 3.5.3 Cyclofructan-Based CSP 128 3.5.4 Synthetic Polymers 128 3.5.5 Targeted Selector Design 130 3.5.6 Further Developments 132 3.6 Properties of Packings and Their Relevance to Chromatographic Performance 132 3.6.1 Chemical and Physical Bulk Properties 132 3.6.2 Morphology 133 3.6.3 Particulate Adsorbents: Particle Size and Size Distribution 133 3.6.4 Pore Texture 134 3.6.5 Pore Structural Parameters 137 3.6.6 Comparative Rating of Columns 137 3.7 Sorbent Maintenance and Regeneration 138 3.7.1 Cleaning in Place (CIP) 138 3.7.2 CIP for IEX 140 3.7.3 CIP of Protein A Sorbents 140 3.7.4 Conditioning of Silica Surfaces 143 3.7.5 Sanitization in Place (SIP) 145 3.7.6 Column and Adsorbent Storage 145 References 146 4 Selection of Chromatographic Systems 159Michael Schulte 4.1 Definition of the Task 164 4.2 Mobile Phases for Liquid Chromatography 167 4.2.1 Stability 168 4.2.2 Safety Concerns 172 4.2.3 Operating Conditions 172 4.2.4 Aqueous Buffer Systems 176 4.3 Adsorbent and Phase Systems 178 4.3.1 Choice of Phase System Dependent on Solubility 178 4.3.2 Improving Loadability for Poor Solubilities 180 4.3.3 Dependency of Solubility on Sample Purity 183 4.3.4 Generic Gradients for Fast Separations 184 4.4 Criteria for Choosing Normal Phase Systems 184 4.4.1 Retention in NP Systems 186 4.4.2 Solvent Strength in Liquid–Solid Chromatography 188 4.4.3 Pilot Technique Thin-Layer Chromatography Using the PRISMA Model 190 4.4.3.1 Step (1): Solvent Strength Adjustment 199 4.4.3.2 Step (2): Optimization of Selectivity 199 4.4.3.3 Step (3): Final Optimization of the Solvent Strength 200 4.4.3.4 Step (4): Determination of the Optimum Mobile Phase Composition 200 4.4.4 Strategy for an Industrial Preparative Chromatography Laboratory 202 4.4.4.1 Standard Gradient Elution Method on Silica 203 4.4.4.2 Simplified Procedure 204 4.5 Criteria for Choosing Reversed Phase Systems 206 4.5.1 Retention and Selectivity in RP Systems 208 4.5.2 Gradient Elution for Small Amounts of Product on RP Columns 212 4.5.3 Rigorous Optimization for Isocratic Runs 213 4.5.4 Rigorous Optimization for Gradient Runs 217 4.5.5 Practical Recommendations 222 4.6 Criteria for Choosing CSP Systems 223 4.6.1 Suitability of Preparative CSP 223 4.6.2 Development of Enantioselectivity 224 4.6.3 Optimization of Separation Conditions 226 4.6.3.1 Determination of Racemate Solubility 226 4.6.3.2 Selection of Elution Order 226 4.6.3.3 Optimization of Mobile/Stationary Phase Composition, Including Temperature 226 4.6.3.4 Determination of Optimum Separation Step 227 4.6.4 Practical Recommendations 227 4.7 Downstream Processing of mAbs Using Protein A and IEX 231 4.8 Size-Exclusion Chromatography (SEC) 236 4.9 Overall Chromatographic System Optimization 237 4.9.1 Conflicts During Optimization of Chromatographic Systems 237 4.9.2 Stationary Phase Gradients 241 References 246 5 Process Concepts 251Malte Kaspereit and Henner Schmidt-Traub 5.1 Discontinuous Processes 252 5.1.1 Isocratic Operation 252 5.1.2 Gradient Chromatography 253 5.1.3 Closed-Loop Recycling Chromatography 256 5.1.4 Steady-State Recycling Chromatography (SSRC) 258 5.1.5 Flip-Flop Chromatography 259 5.1.6 Chromatographic Batch Reactors 260 5.2 Continuous Processes 261 5.2.1 Column Switching Chromatography 262 5.2.2 Annular Chromatography 262 5.2.3 Multiport Switching Valve Chromatography (ISEP/CSEP) 263 5.2.4 Isocratic Simulated Moving Bed (SMB) Chromatography 264 5.2.5 SMB Chromatography with Variable Process Conditions 268 5.2.5.1 Varicol 269 5.2.5.2 PowerFeed 270 5.2.5.3 Partial-Feed, Partial-Discard, and Fractionation-Feedback Concepts 271 5.2.5.4 Improved/Intermittent SMB (iSMB) 271 5.2.5.5 Modicon 273 5.2.5.6 FF-SMB 273 5.2.6 Gradient SMB Chromatography 274 5.2.7 Supercritical Fluid Chromatography (SFC) 275 5.2.7.1 Supercritical Batch Chromatography 276 5.2.7.2 Supercritical SMB processes 277 5.2.8 Multicomponent Separations 277 5.2.9 Multicolumn Systems for Bioseparations 278 5.2.9.1 Multicolumn Capture Chromatography (MCC) 279 5.2.9.2 Multicolumn Countercurrent Solvent Gradient Purification (MCSGP) 286 5.2.10 Countercurrent Chromatographic Reactors 288 5.2.10.1 SMB Reactor 288 5.2.10.2 SMB Reactors with Distributed Functionalities 290 5.3 Choice of Process Concepts 292 5.3.1 Scale 292 5.3.2 Range of k’ 292 5.3.3 Number of Fractions 293 5.3.4 Example 1: Lab Scale; Two Fractions 293 5.3.5 Example 2: Lab Scale; Three or More Fractions 294 5.3.6 Example 3: Production Scale; Wide Range of k’ 296 5.3.7 Example 4: Production Scale; Two Main Fractions 297 5.3.8 Example 5: Production Scale; Three Fractions 298 5.3.9 Example 6: Production Scale; Multistage Process 300 References 302 6 Modeling of Chromatographic Processes 311Andreas Seidel-Morgenstern 6.1 Introduction 311 6.2 Models for Single Chromatographic Columns 311 6.2.1 Equilibrium Stage Models 312 6.2.1.1 Discontinuous Model According to Craig 313 6.2.1.2 Continuous Model According to Martin and Synge 315 6.2.2 Derivation of Continuous Mass Balance Equations 316 6.2.2.1 Mass Balance Equations 318 6.2.2.2 Convective Transport 320 6.2.2.3 Axial Dispersion 320 6.2.2.4 Intraparticle Diffusion 321 6.2.2.5 Mass Transfer Between Phases 321 6.2.2.6 Finite Rates of Adsorption and Desorption 322 6.2.2.7 Adsorption Equilibria 323 6.2.3 Equilibrium Model of Chromatography 323 6.2.4 Models with One Band Broadening Effect 329 6.2.4.1 Equilibrium Dispersion Model 329 6.2.4.2 Finite Adsorption Rate Model 331 6.2.5 Continuous Lumped Rate Models 331 6.2.5.1 Transport Dispersion Models 332 6.2.5.2 Lumped Finite Adsorption Rate Model 333 6.2.6 General Rate Models 333 6.2.7 Initial and Boundary Conditions of the Column 335 6.2.8 Dimensionless Model Equations 336 6.2.9 Comparison of Different Model Approaches 338 6.3 Including Effects Outside the Columns 343 6.3.1 Experimental Setup and Simulation Flow Sheet 343 6.3.2 Modeling Extra-Column Equipment 345 6.3.2.1 Injection System 345 6.3.2.2 Piping 345 6.3.2.3 Detector 345 6.4 Calculation Methods and Software 346 6.4.1 Analytical Solutions 346 6.4.2 Numerical Solution Methods 346 6.4.2.1 Discretization 346 6.4.2.2 General Solution Procedure and Software 349 References 350 7 Determination of Model Parameters 355Andreas Seidel-Morgenstern, Andreas Jupke, and Henner Schmidt-Traub 7.1 Parameter Classes for Chromatographic Separations 355 7.1.1 Design Parameters 355 7.1.2 Operating Parameters 356 7.1.3 Model Parameters 356 7.2 Concept to Determine Model Parameters 357 7.3 Detectors and Parameter Estimation 359 7.3.1 Calibration of Detectors 359 7.3.2 Parameter Estimation 360 7.3.3 Evaluation of Chromatograms 362 7.4 Determination of Packing Parameters 363 7.4.1 Void Fraction and Porosity of the Packing 363 7.4.2 Axial Dispersion 363 7.4.3 Pressure Drop 364 7.5 Adsorption Isotherms 365 7.5.1 Determination of Adsorption Isotherms 365 7.5.2 Estimation of Henry Coefficients 365 7.5.3 Static Isotherm Determination Methods 370 7.5.3.1 Batch Method 370 7.5.3.2 Adsorption–Desorption Method 370 7.5.3.3 Circulation Method 371 7.5.4 Dynamic Methods 371 7.5.5 Frontal Analysis 371 7.5.6 Analysis of Dispersed Fronts 378 7.5.7 Peak Maximum Method 380 7.5.8 Minor Disturbance/Perturbation Method 380 7.5.9 Curve Fitting of the Chromatogram 383 7.5.10 Data Analysis and Accuracy 384 7.6 Mass Transfer Kinetics 386 7.6.1 Correlations 386 7.6.2 Application of Method of Moments 388 7.7 Plant Parameters 389 7.8 Experimental Validation of Column Models and Model Parameters 391 7.8.1 Batch Chromatography 391 7.8.2 Simulated Moving Bed Chromatography 394 7.8.2.1 Model Formulation and Parameters 394 7.8.2.2 Experimental Validation 400 References 404 8 Process Design and Optimization 409Andreas Jupke, Andreas Biselli, Malte Kaspereit,Martin Leipnitz, and Henner Schmidt-Traub 8.1 Basic Principles and Definitions 409 8.1.1 Performance, Costs, and Objective Functions 409 8.1.1.1 Performance Criteria 410 8.1.1.2 Economic Criteria 411 8.1.1.3 Objective Functions 412 8.1.2 Degrees of Freedom 413 8.1.2.1 Categories of Parameters 413 8.1.2.2 Dimensionless Operating and Design Parameters 414 8.1.3 Scaling by Dimensionless Parameters 418 8.1.3.1 Influence of Different HETP Coefficients for Every Component 419 8.1.3.2 Influence of Feed Concentration 420 8.1.3.3 Examples for a Single-Column Batch Chromatography 421 8.1.3.4 Examples for SMB Processes 424 8.2 Batch Chromatography 426 8.2.1 Fractionation Mode (Cut Strategy) 426 8.2.2 Design and Optimization of Batch Chromatographic Columns 427 8.2.2.1 Process Performance Depending on Number of Stages and Loading Factor 427 8.2.2.2 Design and Optimization Strategy 432 8.2.2.3 Other Strategies 436 8.3 Recycling Chromatography 437 8.3.1 Design of Steady-State Recycling Chromatography 437 8.3.2 Scale-Up of Closed-Loop Recycling Chromatography 440 8.4 Conventional Isocratic SMB Chromatography 445 8.4.1 Considerations to Optimal Concentration Profiles in SMB Process 445 8.4.2 Process Design Based on TMB Models (Shortcut Methods) 446 8.4.2.1 Triangle Theory for an Ideal Model with Linear Isotherms 447 8.4.2.2 Triangle Theory for an Ideal Model with Nonlinear Isotherms 449 8.4.2.3 Shortcut to Apply the Triangle Theory on a System with Unknown Isotherms Assuming Langmuir Character 452 8.4.3 Process Design and Optimization Based on Rigorous SMB Models 455 8.4.3.1 Estimation of Operating Parameter 456 8.4.3.2 Optimization of Operating Parameters for Linear Isotherms Based on Process Understanding 457 8.4.3.3 Optimization of Operating Parameters for Nonlinear Isotherms Based on Process Understanding 458 8.4.3.4 Optimization of Design Parameters 460 8.5 Isocratic SMB Chromatography Under Variable Operating Conditions 465 8.5.1 Performance Comparison of Varicol and Conventional SMB 466 8.5.2 Performance Comparison of Varicol, PowerFeed, and Modicon with Conventional SMB 470 8.5.3 Performance Trends Applying SMB Concepts Under Variable Operating Conditions 475 8.6 Gradient SMB Chromatography 476 8.6.1 Step Gradient 476 8.6.2 Multicolumn Solvent Gradient Purification Process 482 8.7 Multicolumn Systems for Bioseparations 487 8.7.1 Design of Twin-Column Capture SMB 488 8.7.2 Modeling of Multicolumn Capture processes 490 References 493 9 Process Control 503Sebastian Engell and Achim Kienle 9.1 Standard Process Control 504 9.2 Advanced Process Control 504 9.2.1 Online Optimization of Batch Chromatography 505 9.2.2 Advanced Control of SMB Chromatography 507 9.2.2.1 Purity Control for SMB Processes 508 9.2.2.2 Direct Optimizing Control of SMB Processes 510 9.2.3 Advanced Parameter and State Estimation for SMB Processes 515 9.2.4 Adaptive Cycle-to-Cycle Control 517 9.2.5 Control of Coupled Simulated Moving Bed Processes for the Production of Pure Enantiomers 519 References 521 10 Chromatography Equipment: Engineering and Operation 525Henner Schmidt-Traub and Arthur Susanto 10.1 Challenges for Conceptual Process Design 525 10.1.1 Main Cost Factors for a Chromatographic System 527 10.1.2 Conceptual Process Design 528 10.1.2.1 A Case Study: Large-Scale Biotechnology Project 529 10.2 Engineering Challenges 533 10.2.1 Challenges Regarding Sanitary Design 535 10.2.2 Challenges During Acceptance Tests and Qualifications 539 10.3 Commercial Chromatography Columns 540 10.3.1 General Design 541 10.3.1.1 Manually Moved Piston 542 10.3.1.2 Electrically or Hydraulically Moved Piston 542 10.3.2 High- and Low-Pressure Columns 543 10.3.2.1 Chemical Compatibility 544 10.3.2.2 Frit Design 546 10.3.2.3 Special Aspects of Bioseparation 549 10.4 Commercial Chromatographic Systems 551 10.4.1 General Design Aspects: High-Pressure and Low-Pressure Systems 551 10.4.2 Material 553 10.4.3 Batch Low-Pressure Liquid Chromatographic (LPLC) Systems 553 10.4.3.1 Inlets 553 10.4.3.2 Valves to Control Flow Direction 555 10.4.3.3 Pumps 556 10.4.3.4 Pump- and Valve-Based and Gradient Formation 556 10.4.4 Batch High-Pressure Liquid Chromatography 558 10.4.4.1 General Layout 558 10.4.4.2 Inlets and Outlets 559 10.4.4.3 Pumps 559 10.4.4.4 Valves and Pipes 562 10.4.5 Continuous Systems: Simulated Moving Bed 563 10.4.5.1 General Layout 563 10.4.5.2 A Key Choice: The Recycling Strategy 565 10.4.5.3 Pumps, Inlets, and Outlets 566 10.4.5.4 Valves and Piping 566 10.4.6 Auxiliary Systems 567 10.4.6.1 Slurry Preparation Tank 567 10.4.6.2 Slurry Pumps and Packing Stations 568 10.4.6.3 Cranes and Transport Units 568 10.4.6.4 Filter Integrity Test 568 10.4.7 Detectors 569 10.5 Packing Methods 571 10.5.1 Column and Packing Methodology Selection 571 10.5.2 Slurry Preparation 572 10.5.3 Column Preparation 574 10.5.4 Flow Packing 575 10.5.5 Dynamic Axial Compression (DAC) Packing 577 10.5.6 Stall Packing 577 10.5.7 Combined Method (Stall+DAC) 578 10.5.8 Vacuum Packing 580 10.5.9 Vibration Packing 581 10.5.10 Column Equilibration 582 10.5.11 Column Testing and Storage 583 10.5.11.1 Test Systems 583 10.5.11.2 Hydrodynamic Properties and Column Efficiency 584 10.5.11.3 Column and Adsorbent Storage 585 10.6 Process Troubleshooting 585 10.6.1 Technical Failures 586 10.6.2 Loss of Performance 587 10.6.2.1 Pressure Increase 587 10.6.2.2 Loss of Column Efficiency 590 10.6.2.3 Variation of Elution Profile 591 10.6.2.4 Loss of Purity/Yield 592 10.6.3 Column Stability 592 10.7 Disposable Technology for Bioseparations 593 10.7.1 Prepacked Columns 596 10.7.2 Membrane Chromatography 597 References 599 Appendix A Data of Test Systems 601 A.1 EMD53986 601 A.2 Tröger’s Base 602 A.3 Glucose and Fructose 604 A.4 β-Phenethyl Acetate 606 References 607 Index 609

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Book SynopsisChromatography has been developed as a powerful and rapid technique for the separation of compounds with highly similar molecular characteristics, even from complicated matrices. Due to their excellent separation characteristics and Versatility, chromatographic methods have found growing acceptance and application in environmental protection for residue analysis in air, ground and surface waters, sewage, sludge, soil matrices, etc The book will be of interest to analytical chemists in legalisation and research and to analytical control specialists, as well as to researchers and students.Table of Contents1. Separation Strategies for Environmental Pollutants: Theory and Practice 2. Hydrocarbons and Hydrocarbon-Based Pollutants 3. Aromatic and Polyaromatic Pollutants 4. Pesticides

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Book SynopsisThe porphyrins, chlorophylls, bilins and related tetrapyrroles are vital for all living organisms. Natural and synthetic tetrapyrroles are used extensively in foods, cosmetics, biotechnology, pharmaceuticals, diagnostics and medicine. Methods for their separation and characterization therefore, have a very wide area of applications. Yet, there is a dearth of books dedicated to HPLC and HPLC/MS of tetrapyrroles. Lim addresses this problem admirably by providing practical HPLC and HPLC/MS protocols coupled with in-depth chromatographic and mass spectrometric reference data. These are invaluable in the analysis, identification and characterization of porphyrins, chlorophylls, bilins and other related compounds found in biological and clinical materials. HPLC method development and optimization for coupling to mass spectrometry are also described in rich detail. Sample preparation, and suggestions for avoiding procedural artifacts during extraction of clinical and biological samples are discussed. Clinical biochemists involved in biochemical diagnosis of human porphyrias will find this monograph assuredly helpful, as would analysts, biochemists and chemists involved in the separation, isolation and characterization of natural and synthetic tetrapyrroles. Undoubtedly, Lim has contributed a master-piece containing sufficient background material for beginners and up-to-date references for all researchers in the field.

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