Chemistry Books

Book SynopsisThis broad-based book covers the three major areas of Chemical Engineering. Most of the books in the market involve one of the individual areas, namely, Fluid Mechanics, Heat Transfer or Mass Transfer, rather than all the three. This book presents this material in a single source. This avoids the user having to refer to a number of books to obtain information. Most published books covering all the three areas in a single source emphasize theory rather than practical issues. This book is written with emphasis on practice with brief theoretical concepts in the form of questions and answers, not adopting stereo-typed question-answer approach practiced in certain books in the market, bridging the two areas of theory and practice with respect to the core areas of chemical engineering. Most parts of the book are easily understandable by those who are not experts in the field. Fluid Mechanics chapters include basics on non-Newtonian systems which, for instance find importance in pTrade Review"Overall, the author is commended for providing a lucid, thorough approach to the subject. Recommended. All undergraduate students and professional engineers." (Choice, 1 October 2011) Table of ContentsFOREWORD. PREFACE. ACKNOWLEDGMENTS. ABOUT THE AUTHOR. LIST OF FIGURES. LIST OF TABLES. SECTION I FLUID MECHANICS. 1 Fluid Mechanics Basics. 2 Fluid Flow. 3 Piping, Seals, and Valves. 4 Flow Measurement. 5 Pumps, Ejectors, Blowers, and Compressors. 6 Mixing. 7 Two-Phase Flow Systems. SECTION II HEAT TRANSFER. 8 Dimensionless Numbers, Temperature Measurement, and Conduction Heat Transfer. 9 Convective Heat Transfer Basics. 10 Shell and Tube Heat Exchangers. 11 Heat Transfer Equipment Involving Phase Transfer. 12 Refrigeration, Heat Pumps, Heat Tracing, Coiled and Jacketed Vessels, Steam Traps, and Immersion Heaters. 13 Compact Heat Exchangers, Regenerators, and Recuperators. 14 Radiant Heat Transfer and Fired Heaters. SECTION III MASS TRANSFER. 15 Mass Transfer Basics. 16 Mass Transfer Equipment. 17 Absorption, Distillation, and Extraction. 18 Crystallization, Air–Water Operations, Drying, Adsorption, Membrane Separations, and Other Mass Transfer Processes. INDEX.

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Book SynopsisThis book applies systems biology methods to analyze Traditional Chinese Medicine (TCM), providing a comprehensive resource for modernization of TCM research and drug discovery.Table of ContentsForeword ix Preface xiii Abbreviations xvii 1 Introduction of Systems Biology in Traditional Chinese Medicine (tcm) 1 1.1 Characteristics and Compatibility Principles of Traditional Chinese Medicine (TCM) 1 1.2 Key Scientific Issues in TCM Modernization 9 1.3 Development of Systems Biology 16 1.4 Chemomics Integrated Systems Biology 19 1.5 Research Strategy and Prospective of Systems Biology in Tcm 25 References 34 2 Chemomics of Traditional Chinese Medicine 38 2.1 Characteristics and Research Difficulties in TCM 39 2.2 Background of TCM Chemomics’ Proposal and Development 45 2.3 Chemomics 52 2.4 Chemomics and the Research of Formulas 58 References 63 3 Technological Platform of Tcm Chemomics 66 3.1 Acquisition Methods and Techniques for TCM Chemomics 66 3.2 Characterization Techniques of Chemome-TCM Fingerprinting 73 3.3 Information Processing for the Study of TCM Chemomics 107 3.4 Development of an Intelligent Quality Control System in the Process of Chinese Medicine Production 119 References 127 4 Pharmacokinetic Investigation on Tcm Formulas Based on Global Systems Biology 131 4.1 Pharmacokinetic Characteristics of TCM Formulas 131 4.2 Methodology of Pharmacokinetics of TCM Formulas 133 4.3 Application of PK-PD Model in the Toxicological Research of Liushen Pills (LSP) 138 4.4 Prospect 143 References 144 5 Application of Genomics in the Research of Tcm 146 5.1 Genomics and TCM System Research 146 5.2 Prospect of Genomics in TCM Research 148 5.3 Cases of the Application of Genomics in TCM Research 148 References 168 6 Proteomics Study of Tcm 171 6.1 Proteomics in TCM Research 171 6.2 A Case Study of Proteomics in TCM 174 6.3 The Application of High Content Screening in TCM Research 182 6.4 Limitations and Prospect of TCM Proteomics 186 References 187 7 Application of Metabonomics in Research on Tcm 191 7.1 Current Research Situation of Metabonomics 191 7.2 Integration of Quantitative Metabonomics Platform Technology (qmpt) 191 7.3 Application of Metabonomics in the Field of Medicine 194 7.4 Examples of Metabonomic Research on TCM 198 References 206 8 Application of Chemometrics and Bioinformatics in Tcm Research 210 8.1 Introduction of Chemometrics 210 8.2 Chemometric Techniques and Their Applications in TCM Research 211 8.3 Introduction of Bioinformatics 216 8.4 Bioinformatics Techniques and Their Applications in the Research of TCM 219 8.5 Conclusions 222 References 224 9 Study of Integrated Biomarker System of Diabetic Nephropathy 228 9.1 Introduction of Diabetic Nephropathy 228 9.2 Mogensen Staging and TCM Typing of DN 234 9.3 The Metabonomics Study of DN 244 9.4 Condition of Metabolism after Treatment with TangShen Formula (TSF) 278 9.5 Genomics Study of Diabetic Neuropathy 286 9.6 The Integrated Biomarker System of DN 301 9.7 Conclusions 311 References 312 10 Chemomics Research on the Tcm Formula of The Qingkailing Injection 317 10.1 Chemomics Research of Qingkailing Injection 318 10.2 Pharmacodynamic Evaluation of Qingkailing Injection 330 10.3 Research on the Qingkailing Derived Formula 335 10.4 Conclusions 368 References 369 11 Integrated Global Systems Biology for the Research and Development of Chinese Medicine Shuanglong Formula 371 11.1 Brief Introduction to the Shuanglong Formula 371 11.2 Chemomics Study of the Shuanglong Formula 374 11.3 Pharmacodynamic Evaluation of SLF Effective Ingredients 384 11.4 Systems Biology Study of the Mechanism of Directed Differentiation of Stem Cells Induced by NSLF6 402 11.5 Anti-Myocardial Infarction Effect of NSLF6 426 11.6 Conclusions 429 References 430 12 Demonstrative Research on the Safety Evaluation of Liushen Pills 437 12.1 Introduction 437 12.2 Toxicity Study of Chansu 438 12.3 Chemomics Study of LSP 446 12.4 Assessment of Effectiveness and Safety of LSP 457 12.5 In Vivo Distribution and Metabonomics of LSP and Xionghuang 462 12.6 Metabonomic Research of LSP 467 12.7 Conclusions 477 References 478 Index 481

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Book SynopsisThis book covers important advances in enzymology, explaining the behavior of enzymes and how they can be utilized to develop novel drugs, synthesize known and novel compounds, and understand evolutionary processes.Trade Review"With its discussion of current concepts of the biochemical basis of antibiotic resistance and its impact on modern medicine, this book will appeal to students, researchers, scientists, and clinicians interested in the areas of enzymology and mechanism of bacterial resistance." (Doody's, 26 August 2011) Table of ContentsContributors. Preface. Structure and Mechanism of RND-Type Multidrug Efflux Pumps (Hiroshi Nikaido). Efflux Pumps of Gram-Negative Bacteria: Genetic Responses to Stress and the Modulation of Their Activity by pH, Inhibitors, and Phenothiazines (Leonard Amaral, Seamus Fanning, and Jean-Marie Pagès). Efflux Pumps of the Resistance–Nodulation–Division Family: A Perspective of Their Structure, Function, and Regulation in Gram-Negative Bacteria (Mathew D. Routh, Yaramah Zalucki, Chih-Chia Su, Feng Long, Qijing Zhang, William M. Shafer, and Edward W. Yu). The MFS Efflux Proteins of Gram-Positive and Gram-Negative Bacteria (Massoud Saidijam, Kim E. Bettaney, Dong Leng, Pikyee Ma, Zhiqiang Xu, Jeffrey N. Keen, Nicholas G. Rutherford, Alison Ward, Peter J. F. Henderson, Gerda Szakonyi, Qinghu Ren, Ian T. Paulsen, Ingerid Nes, Jasmin K. Kroeger, and Anne-Brit Kolsto). Efflux Pumps as an Important Mechanism for Quinolone Resistance (Jordi Vila, Anna Fabrega, Ignasi Roca, Alvaro Hernandez, and Jose Luis Martinez). Xenobiotic Efflux in Bacteria and Fungi: A Genomics Update (Ravi D. Barabote, Jose Thekkiniath, Richard E. Strauss, Govindsamy Vediyappan, Joe A. Fralick, and Michael J. San Francisco). A Survey of Oxidative Paracatalytic Reactions Catalyzed by Enzymes That Generate Carbanionic Intermediates: Implications for ROS Production, Cancer Etiology, and Neurodegenerative Diseases (Victoria I. Bunik, John V. Schloss, John T. Pinto, Natalia Dudareva, and Arthur J. L. Cooper). Author Index. Subject Index.

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Book SynopsisVolume 76 in the venerable Organic Reactions series comprises three chapters that cover the ever-increasing emphasis of transition metal catalysis in organic synthesis. These three chapters represent some of the most important transformations that enable the construction of carbon-carbon bonds, heterocycles and carbon-heteratom bonds. This volume features a comprehensive treatment of transition metal (palladium, nickel, copper) catalyzed a-arylation of enolates derived from many common functional groups such as ketones, aldehydes, esters and nitriles (Prim, Marque, Gaucher, Campagne) including enantioselective variants; palladium catalyzed cyclization to form indoles (Cacchi, Fabrizi, Goggiamani) one of the most prevalent and important classes of heterocycles in natural products and pharmaceutical agents; and an overview of a newly developed dihydroxylation reaction of alkenes (Donohoe, Bataille, Innocenti) that uses hydrogen bonding interactions to direct the delivery of an osmTable of Contents1. HYDROGEN-BONDING-MEDIATED DIRECTED OSMIUM DIHYDROXYLATION Timothy J. Donohoe, Carole J. R. Bataille, and Paolo Innocenti1 2. TRANSITION-METAL-CATALYZED α-ARYLATION OF ENOLATES Damien Prim, Sylvain Marque, Anne Gaucher, and Jean-Marc Campagne 49 3. INDOLES VIA PALLADIUM-CATALYZED CYCLIZATION Sandro Cacchi, Giancarlo Fabrizi, and Antonella Goggiamani 281 CUMULATIVE CHAPTER TITLES BY VOLUME535 AUTHOR INDEX, VOLUMES 1–76 551 CHAPTER AND TOPIC INDEX, VOLUMES 1–76 557

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Book SynopsisThis handbook focuses on biopolymers for both environmental and biomedical applications. It shows recent advances in technology in all areas from chemical synthesis or biosynthesis to end use applications. These areas have not been covered in a single book before and they include biopolymers for chemical and biotechnological modifications, material structures, characterization, processing, properties, and applications. After the introduction which summarizes the importance of biopolymer in the market, the book covers almost all the topics related to polysaccharides, biofibers, bioplastics, biocomposites, natural rubber, gums, bacterial and blood compatible polymers, and applications of biopolymers in various fields.Table of ContentsIntroductory Preface. About the Editors. Part I. Polysaccharides. 1. Hyaluronic Acid: A Natural Biopolymer (Juergen Schiller, Nicola Volpi, Eva Hrabárova, and Ladislav Soltes). 2. Polysaccharide Graft Copolymers Synthesis, Properties and Applications (B. S. Kaith, Hemant Mittal, Jaspreet Kaur Bhatia, and Susheel Kalia). 3. Natural Polysaccharides: From Membranes to Active Food Packaging (Keith J. Fahnestock, Marjorie S. Austero, and Caroline L. Schauer). 4. Starch as Source of Polymeric Materials (Antonio A. J. Carvalho). 5. Grafted Polysaccharides: Smart Materials of Future, Synthesis and Applications (Gautam Sen, Ashoke Sharon, and Sagar Pal). 6. Chitosan: The Marine based Biopolymer for Applications (Debasish Sahoo, and P. L. Nayak). Part II. Bioplastics and Biocomposites. 7. Biopolymers Based-on Carboxylic Acids Derived from Renewable Resources (Sushil Kumar, Nikhil Prakash, and Dipaloy Datta). 8. Characteristics and Applications of PLA (Sandra Domenek, Cecile Courgneau, and Violette Ducruet). 9. Biobased Composites & Applications (Smita Mohanty, and Sanjay K. Nayak). Part III. Miscellaneous Biopolymers. 10. Cassia Seed Gums: A Renewable Reservoir for Synthesizing High Performance Materials for Water Remediation (Vandana Singh, and Pramendra Kumar). 11. Bacterial Polymers: Resources, Synthesis and Applications (GVN Rathna, and Sutapa Gosh). 12. Gum Arabica: A Natural Biopolymer (A. Sarkar). 13. Gluten: A Natural Biopolymer (S. Georgiev, and Tereza Dekova). 14. Natural Rubber: Production, Properties, and Applications (Thomas Kurian, and N. M. Mathew). 15. Electronic Structures and Conduction Properties of Biopolymers (Mohsineen Wazir, Vinita Arora, and A. K. Bakhshi). Part IV. Biopolymers for Specific Applications. 16. Applications of Biopolymers in Agriculture with Special Reference to Role of Plant Derived Biopolymers in Crop Protection (S. Niranjan Raj, S. N. Lavanya, J, Sudisha, and H. Shekar Shetty). 17. Modified Cellulose Fibers as a Biosorbent for the Organic Pollutants (Sami Boufi, and Sabrine Alila). 18. Polymers and Biopolymers in Pharmaceutical Technology (István Erös). 19. Biopolymers Employed in Drug Delivery (Betina Giehl Zanetti Ramos). 20. Natural Polymeric Vectors in Gene Therapy (Patit P. Kundu, and Kishor Sarkar).

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Book SynopsisRapid-Equilibrium Enzyme Kinetics helps readers emphasize the estimation of kinetic parameters with the minimum number of velocity measurements, thereby reducing the amount of laboratory work necessary, and allowing more time for the consideration of complicated mechanisms.

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Book SynopsisThis book covers advances in the methods of catalytic asymmetric synthesis and their applications. Coverage moves from new materials and technologies to homogeneous metal-free catalysts and homogeneous metal catalysts. The applications of several methodologies for the synthesis of biologically active molecules are discussed. Part I addresses recent advances in new materials and technologies such as supported catalysts, supports, self-supported catalysts, chiral ionic liquids, supercritical fluids, flow reactors and microwaves related to asymmetric catalysis. Part II covers advances and milestones in organocatalytic, enzymatic and metal-based mediated asymmetric synthesis, including applications for the synthesis of biologically active molecules. Written by leading international experts, this book consists of 16 chapters with 2000 References and illustrations of 560 schemes and figures.Table of ContentsPREFACE xi FOREWORD xiii CONTRIBUTORS xv I NEW MATERIALS AND TECHNOLOGIES: SUPPORTED CATALYSTS, SUPPORTS, SELFSUPPORTED CATALYSTS, CHIRAL IONIC LIQUID, SUPERCRITICAL FLUIDS, FLOW REACTORS, AND MICROWAVES 1 1 RECYCLABLE STEREOSELECTIVE CATALYSTS 3 Carlos M. Monteiro, Alexandre F. Trindade, Pedro M. P. Gois, and Carlos A. M. Afonso 2 RECYCLABLE ORGANOCATALYSTS IN ASYMMETRIC REACTIONS 83 Michelangelo Gruttadauria, Francesco Giacalone, and Renato Noto 3 SYNTHESIS AND CHARACTERIZATION OF SUPPORTED CHIRAL CATALYSTS 177 Carmela Aprile, Hermenegildo Garcia, and Paolo P. Pescarmona 4 SYNTHESIS OF CHIRAL CATALYSTS SUPPORTED ON ORGANIC POLYMERS 209 Tor Erik Kristensen and Tore Hansen 5 SELF-SUPPORTED CHIRAL CATALYSTS 257 Hongchao Guo and Kuiling Ding 6 CATALYSIS WITH CHIRALLY MODIFIED METAL SURFACES: SCOPE AND MECHANISMS 291 Angelo Vargas, Cecilia Mondelli, and Alfons Baiker 7 CHIRAL IONIC LIQUIDS FOR ASYMMETRIC REACTIONS 323 Annie-Claude Gaumont, Yves Génisson, Frédéric Guillen, Viacheslav Zgonnik, and Jean-Christophe Plaquevent 8 ASYMMETRIC REACTIONS IN FLOW REACTORS 345 Munawwer Rasheed, Simon C. Elmore, and Thomas Wirth 9 ASYMMETRIC CATALYTIC SYNTHESIS IN SUPERCRITICAL FLUIDS 373 Tomoko Matsuda 10 MICROWAVE-ASSISTED TRANSITION METAL-CATALYZED ASYMMETRIC SYNTHESIS 391 Luke R. Odell and Mats Larhed II RECENT ADVANCES IN ORGANOCATALYTIC, ENZYMATIC, AND METAL-BASED MEDIATED ASYMMETRIC SYNTHESIS 413 11 RECENT ADVANCES ON STEREOSELECTIVE ORGANOCATALYTIC REACTIONS. ORGANOCATALYTIC SYNTHESIS OF NATURAL PRODUCTS AND DRUGS 415 Monika Raj and Vinod K. Singh 12 RECENT ADVANCES IN BIOCATALYSIS APPLIED TO ORGANIC SYNTHESIS 491 Gonzalo De Gonzalo, Iván Lavandera, and Vicente Gotor 13 PEPTIDES FOR ASYMMETRIC CATALYSIS 529 Matthias Freund and Svetlana B. Tsogoeva 14 SILICATE-MEDIATED STEREOSELECTIVE REACTIONS CATALYZED BY CHIRAL LEWIS BASES 579 Maurizio Benaglia, Stefania Guizzetti, and Sergio Rossi 15 RECENT ADVANCES IN THE METAL-CATALYZED STEREOSELECTIVE SYNTHESIS OF BIOLOGICALLY ACTIVE MOLECULES 625 Catalina Ferrer, Xavier Verdaguer, and Antoni Riera 16 STEREOSELECTIVE NITROGEN HETEROCYCLE SYNTHESIS MEDIATED BY CHIRAL METAL CATALYSTS 671 Sherry R. Chemler INDEX 689

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Book SynopsisThis series provides the chemical physics field with a forum for critical, authoritative evaluations of advances in every area of the discipline. Volume 145 in the series continues to report recent advances with significant, up-to-date chapters by internationally recognized researchers.Table of ContentsPreface xi Non-Markovian Theory of Vibrational Energy Relaxation and its Applications to Biomolecular Systems 1 By Hiroshi Fujisaki, Yong Zhang, and John E. Straub Protein Functional Motions: Basic Concepts and Computational Methodologies 35 By Sotaro Fuchigami, Hiroshi Fujisaki, Yasuhiro Matsunaga, and Akinori Kidera Non-Brownian Phase Space Dynamics of Molecules, the Nature of Their Vibrational States, and Non-RRKM Kinetics 83 By David M. Leitner, Yasuhiro Matsunaga, Chun-Biu Li, Tamiki Komatsuzaki, Akira Shojiguchi, and Mikito Toda Dynamical Reaction Theory Based on Geometric Structures in Phase Space 123 By Shinnosuke Kawai, Hiroshi Teramoto, Chun-Biu Li, Tamiki Komatsuzaki, and Mikito Toda Ergodic Problems for Real Complex Systems in Chemical Physics 171 By Tamiki Komatsuzaki, Akinori Baba, Shinnosuke Kawai, Mikito Toda, John E. Straub, and R. Stephen Berry Author Index 221 Subject Index 247

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Book SynopsisSets the stage for the development of sustainable, environmentally friendly fuels, chemicals, and materials Taking millions of years to form, fossil fuels are nonrenewable resources; it is estimated that they will be depleted by the end of this century.Trade Review“By providing interesting outlooks on a subject of such high debate and importance in both industry and research, the work of the editors sets itself as foundation for all those interested in development of new and sustainable means of bioresources processing.” (Environmental Engineering and Management Journal, 1 March 2013)Table of ContentsForeword vii Preface xi Contributors xiii About the Editors xvii 1 Introduction of Biomass and Biorefineries 1 Birgit Kamm 2 Recent Advances in Green Chemistry 27 Nicholas Gathergood 3 Biorefinery with Ionic Liquids 75 Haibo Xie, Wujun Liu, Ian Beadham, and Nicholas Gathergood 4 Biorefinery with Water 135 X. Philip Ye, Leming Cheng, Haile Ma, Biljana Bujanovic, Mangesh J. Goundalkar, and Thomas E. Amidon 5 Supercritical CO2 as an Environmentally Benign Medium for Biorefinery 181 Ray Marriott and Emily Sin 6 Dissolution and Application of Cellulose in NaOH/Urea Aqueous Solution 205 Xiaopeng Xiong and Jiangjiang Duan 7 Organosolv Biorefining Platform for Producing Chemicals, Fuels, and Materials from Lignocellulose 241 Xuejun Pan 8 Pyrolysis Oils from Biomass and Their Upgrading 263 Qirong Fu, Haibo Xie, and Dimitris S. Argyropoulos 9 Microwave Technology for Lignocellulosic Biorefinery 281 Takashi Watanabe and Tomohiko Mitani 10 Biorefinery with Microbes 293 Cuimin Hu and Zongbao K. Zhao 11 Heterogeneous Catalysts for Biomass Conversion 313 Aiqin Wang, Changzhi Li, Mingyuan Zheng, and Tao Zhang 12 Catalytic Conversion of Glycerol 349 Jie Xu, Weiqiang Yu, Hong Ma, Feng Wang, Fang Lu, Mukund Ghavre, and Nicholas Gathergood 13 Ultrasonics for Enhanced Fluid Biofuel Production 375 David Grewell and Melissa Montalbo-Lomboy 14 Advanced Membrane Technology for Products Separation in Biorefinery 407 Shenghai Li, Suobo Zhang, and Weihui Bi 15 Assessment of the Ecotoxicological and Environmental Effects of Biorefineries 435 Kerstin Bluhm, Sebastian Heger, Matthew T. Agler, Sibylle Maletz, Andreas Sch€affer, Thomas-Benjamin Seiler, Largus T. Angenent, and Henner Hollert Index 469

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Book SynopsisThis book covers the areas of electrochemical heterogeneity and electrode inhomogeneity and their effects on nonuniform electrode processes, in particular, localized corrosion. It covers the fundamentals, experimental methods, and engineering aspects of electrochemical heterogeneity.Table of ContentsPreface ix 1. Homogeneous Electrode Models and Uniform Corrosion Measurements 1 1.1 Homogeneous electrodes and traditional electrochemical methods 3 1.2 Mixed electrodes and uniform corrosion models 7 1.3 The mixed potential theory and electrochemical corrosion measurement 10 1.4 Electrochemical impedance investigation of electrode-solution interface 19 1.5 Electrochemical noise monitoring of rapid electrode processes 26 1.6 Issues and difficulties in traditional electrochemical methods 31 References 32 2. Probing Electrode Inhomogeneity, Electrochemical Heterogeneity and Localized Corrosion 37 2.1 Probing electrode inhomogeneity 39 2.2 Probing electrochemical heterogeneity and localized corrosion 44 2.3 Overview of various techniques for probing localized corrosion 48 References 61 3. Visualizing Localized Corrosion Using Electrochemically Integrated Multielectrode Arrays 67 3.1 An electrochemically integrated multielectrode array: The wire beam electrode 70 3.2 Visualizing the progression of localized corrosion in an Evans water drop 76 3.3 Visualizing localized corrosion in environments with ion concentration gradients 84 3.4 Visualizing localized corrosion by the WBE in conjunction with scanning probes 91 References 99 4. Measuring Thermodynamic and Kinetic Parameters from Localized Corrosion Processes 101 4.1 Methods of probing localized corrosion thermodynamics and kinetics 103 4.2 Measuring localized corrosion using the overpotential-galvanic current method 109 4.3 Measuring localized corrosion using the galvanic current method 120 4.4 Measuring localized corrosion using the Rn-WBE method 125 References 131 5. Characterizing Inhomogeneity and Localised Corrosion on Coated Electrode Surfaces 135 5.1 Characterising inhomogeneities in organic coatings and inhibitor films 137 5.2 Characterising inhomogeneity in organic coatings using the WBE method 141 5.3 The effects of coating inhomogeneity on electrochemical measurement 145 5.4 Visualisng underfilm corrosion and the effects of cathodic protection 148 5.5 Studying corrosion protection by coatings and cathodic protection 155 References 157 6. Designing Experiments for Studying Localized Corrosion and Its Inhibition in Inhomogeneous Media 161 6.1 Basic issues in localized corrosion and inhibitor test design 162 6.2 Fundamental considerations in selecting corrosion measurement techniques 165 6.3 Designing corrosion tests in highly-resistive and inhomogeneous media 168 6.4 Case studies: Designing crevice corrosion tests by means of the WBE 181 6.5 Case study: Designing experiments for localized corrosion inhibitor discovery 186 References 190 7. Sensing Localized Electrodeposition and Electrodissolution195 7.1 Experimental methods for sensing localized electrodeposition and dissolution 197 7.2 Sensing localized electrodeposition using the WBE 200 7.3 Sensing localized electrodissolution using the WBE 204 7.4 Sensing nonuniform electrochemical deposition of organic coatings 211 References 216 8. Versatile Heterogeneous Electrode Processes 219 8.1 Scanning and modeling various heterogeneous electrode processes 222 8.2 Electrochemical noise generation from electrochemical heterogeneity 225 8.3 Harvesting electrical power from electrochemical using the WBE 231 8.4 Further research issues on electrochemical heterogeneity 237 References 238 Index 243

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Book SynopsisAndrogen steroids have become virtually synonymous with drug abuse in sports but are in reality overshadowed by a large collection of compounds, which are commercial drugs that share the same structural carbon skeleton. Steroid Chemistry At A Glance provides a concise overview of the main principles and reactions of steroid chemistry.Trade Review"Overall, this timely book is a valuable addition to the stable. It is applicable to both chemistry and pharmacy undergraduate curricula, unlocking part of the wealth of chemistry that is the legacy of the great 20th century steroid chemistry effort." (Chemistry World, 1 October 2011)Table of ContentsPreface. Introduction. 1 Steroids: a Brief History. 1.1 Structure Determination. 1.1.1 Cholesterol and Cholic Acid. 1.1.2 The Sex Steroids. 1.1.3 Corticosteroids. 2 Sources of Steroids. 2.1 Biosynthesis. 2.2 Commercial Steroid Starting Materials. 2.2.1 Diosgenin. 2.2.2 Soybean Sterols. 3 Estranes: Steroids in Which Ring A is Aromatic. 3.1 Biological Activity. 3.2 Sources of Estranes. 3.2.1 From Androstanes. 3.2.2 Estrogens by Total Synthesis. 3.3 Chemical Reactions of Estranes. 3.3.1 Aromatic A-ring Reactions. 3.3.2 Modifications on Ring B. 3.3.3 Modifications on Ring C. 3.3.4 Modifications on Ring D. 3.4. Some Drugs Based on Estranes. 4 Gonanes or 19-nor-Steroids. 4.1 Preparation of Gonane Starting Materials. 4.1.1 Birch Reduction. 4.1.2 Synthesis by Sequential Annulation Reactions. 4.2 Anabolic–Androgenic Gonanes. 4.2.1 Biological Activity. 4.2.2 Synthesis of 19-Norandrogens. 4.3 Progestational Gonanes. 4.3.1 Biological Activity. 4.3.2 Preparation of 19-Norprogestins. 4.4 Some Drugs Based on Gonanes. 4.4.1 Androgenic–Anabolic Agents. 4.4.2 Progestins. 4.4.3 Progestin Antagonists. 5 Androstanes, C19 Steroids and Their Derivatives. 5.1 Biological Activity. 5.2 Sources of Androstanes. 5.2.1 From Pregnenolone. 5.2.2 Fermentations. 5.2.3 Total Synthesis. 5.3 Modified Anabolic–Androgenic Androstanes. 5.3.1 17-Desalkyl Compounds. 5.3.2 17-Alkyl Compounds. 5.3.3 Modifications on Ring B. 5.3.4 Modifications on Ring C. 5.3.5 Modifications on Ring D. 5.4 17-Spirobutyrolactone Aldosterone Antagonists. 5.5 Some Drugs Based on Androstanes. 5.5.1 Androgens. 5.5.2 Spirobutyrolactones. 6 Pregnanes, Part 1: Progestins. 6.1 Biological Activity. 6.2 Sources of Progesterone. 6.2.1 From Phytochemicals. 6.2.2 By Total Synthesis. 6.2.3 From Dehydroepiandrosterone (DHEA) Acetate. 6.3 Modified Pregnanes. 6.3.1 17-Hydroxy and Acyloxy Derivatives. 6.3.2 Modifications on Ring A. 6.3.3 Modifications on Ring B. 6.3.4 General Methods for Modifications on Ring D. 6.3.5 More Progesterone Analogues. 6.4 Some Drugs Based on Progestins. 6.4.1 Medroxyprogesterone Acetate (10-2). 6.4.2 Megestrol Acetate (10-3). 6.4.3 Melengestrol Acetate (26-7). 7 Pregnanes, Part 2: Corticosteroids. 7.1 Biological Activity. 7.2 Sources of Corticoids. 7.2.1. Introduction of Oxygen at C11. 7.2.2 Construction of the Dihydroxyacetone Side Chain. 7.3 Modified Corticoids. 7.3.1 Unsaturation. 7.3.2 Additional Alkyl Groups. 7.3.3 Halogenated Corticoids. 7.3.4 Hydroxylation: 16,17-Diols. 7.3.5 Corticoids with Multiple Modifications. 7.3.6 Miscellaneous Corticoids. 7.4 Some Drugs Based on Corticoids. 8 Miscellaneous Steroids. 8.1 Heterocyclic Steroids. 8.1.1 Introduction. 8.1.2 Steroids with a Heteroatom in Ring A. 8.1.3 Steroids with a Heteroatom in Ring B. 8.1.4 Steroids with a Heteroatom in Ring C. 8.1.5 Steroids with a Heteroatom in Ring D. 8.2 Cardenolides. 8.2.1 Actodigin Aglycone. 8.2.2 Synthesis from a Bile Acid. 8.3 Compounds Related to Cholesterol. Subject Index. Reactions Index.

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Book SynopsisA comprehensive introduction to inorganic chemistry and, specifically, the science of metal-based drugs, Essentials of Inorganic Chemistry describes the basics of inorganic chemistry, including organometallic chemistry and radiochemistry, from a pharmaceutical perspective. Written for students of pharmacy and pharmacology, pharmaceutical sciences, medicinal chemistry and other health-care related subjects, this accessible text introduces chemical principles with relevant pharmaceutical examples rather than as stand-alone concepts, allowing students to see the relevance of this subject for their future professions. It includes exercises and case studies.Trade Review“It would be a useful adjunct to more general chemistry texts for students in first and second years of study in pharmacy, pharmaceutical sciences, and medicinal chemistry, providing a framework to structure the more detailed but less contextualised information on inorganic pharmaceuticals they will doubtless be looking up on the internet.” (Chemistry in Australia, 1 October 2015)Table of ContentsPreface xiii About the Companion Website xv 1 Introduction 1 1.1 Medicinal inorganic chemistry 1 1.1.1 Why use metal-based drugs? 2 1.2 Basic inorganic principles 3 1.2.1 Electronic structures of atoms 3 1.2.2 Bonds 9 1.3 Exercises 17 References 18 Further Reading 18 2 Alkali Metals 19 2.1 Alkali metal ions 19 2.1.1 Extraction of alkali metals: an introduction to redox chemistry 20 2.1.2 Excursus: reduction – oxidation reactions 21 2.1.3 Chemical behaviour of alkali metals 27 2.2 Advantages and disadvantages using lithium-based drugs 29 2.2.1 Isotopes of lithium and their medicinal application 29 2.2.2 Historical developments in lithium-based drugs 29 2.2.3 The biology of lithium and its medicinal application 30 2.2.4 Excursus: diagonal relationship and periodicity 31 2.2.5 What are the pharmacological targets of lithium? 33 2.2.6 Adverse effects and toxicity 34 2.3 Sodium: an essential ion in the human body 34 2.3.1 Osmosis 35 2.3.2 Active transport of sodium ions 37 2.3.3 Drugs, diet and toxicity 38 2.4 Potassium and its clinical application 40 2.4.1 Biological importance of potassium ions in the human body – action potential 40 2.4.2 Excursus: the Nernst equation 40 2.4.3 Potassium salts and their clinical application: hypokalaemia 42 2.4.4 Adverse effects and toxicity: hyperkalaemia 43 2.5 Exercises 45 2.6 Case studies 47 2.6.1 Lithium carbonate (Li2CO3) tablets 47 2.6.2 Sodium chloride eye drops 47 References 48 Further Reading 48 3 Alkaline Earth Metals 49 3.1 Earth alkaline metal ions 49 3.1.1 Major uses and extraction 50 3.1.2 Chemical properties 51 3.2 Beryllium and chronic beryllium disease 52 3.3 Magnesium: competition to lithium? 53 3.3.1 Biological importance 53 3.3.2 Clinical applications and preparations 54 3.4 Calcium: the key to many human functions 55 3.4.1 Biological importance 56 3.4.2 How does dietary calcium intake influence our lives? 57 3.4.3 Calcium deficiency: osteoporosis, hypertension and weight management 57 3.4.4 Renal osteodystrophy 58 3.4.5 Kidney stones 59 3.4.6 Clinical application 59 3.4.7 Side effects 61 3.5 Barium: rat poison or radio-contrast agent? 61 3.6 Exercises 63 3.7 Case studies 65 3.7.1 Magnesium hydroxide suspension 65 3.7.2 Calcium carbonate tablets 65 References 66 Further Reading 66 4 The Boron Group – Group 13 67 4.1 General chemistry of group 13 elements 67 4.1.1 Extraction 68 4.1.2 Chemical properties 69 4.2 Boron 70 4.2.1 Introduction 70 4.2.2 Pharmaceutical applications of boric acid 71 4.2.3 Bortezomib 71 4.3 Aluminium 71 4.3.1 Introduction 71 4.3.2 Biological importance 72 4.3.3 Al3+ and its use in water purification 73 4.3.4 Aluminium-based adjuvants 73 4.3.5 Antacids 74 4.3.6 Aluminium-based therapeutics – alginate raft formulations 75 4.3.7 Phosphate binders 76 4.3.8 Antiperspirant 76 4.3.9 Potential aluminium toxicity 77 4.4 Gallium 77 4.4.1 Introduction 77 4.4.2 Chemistry 77 4.4.3 Pharmacology of gallium-based drugs 78 4.4.4 Gallium nitrate – multivalent use 78 4.4.5 Gallium 8-quinolinolate 79 4.4.6 Gallium maltolate 79 4.4.7 Toxicity and administration 80 4.5 Exercises 81 4.6 Case studies 83 4.6.1 Boric acid – API analysis 83 4.6.2 Aluminium hydroxide tablets 83 References 84 Further Reading 84 5 The Carbon Group 85 5.1 General chemistry of group 14 elements 85 5.1.1 Occurrence, extraction and use of group 14 elements 85 5.1.2 Oxidation states and ionisation energies 87 5.1.3 Typical compounds of group 14 elements 87 5.2 Silicon-based drugs versus carbon-based analogues 89 5.2.1 Introduction of silicon groups 90 5.2.2 Silicon isosters 91 5.2.3 Organosilicon drugs 93 5.3 Organogermanium compounds: balancing act between an anticancer drug and a herbal supplement 94 5.3.1 Germanium sesquioxide 95 5.3.2 Spirogermanium 97 5.4 Exercises 99 5.5 Cases studies 101 5.5.1 Simethicone 101 5.5.2 Germanium supplements 101 References 102 Further Reading 102 6 Group 15 Elements 103 6.1 Chemistry of group 15 elements 103 6.1.1 Occurrence and extraction 103 6.1.2 Physical properties 104 6.1.3 Oxidation states and ionisation energy 105 6.1.4 Chemical properties 106 6.2 Phosphorus 106 6.2.1 Adenosine phosphates: ATP, ADP and AMP 107 6.2.2 Phosphate in DNA 107 6.2.3 Clinical use of phosphate 108 6.2.4 Drug interactions and toxicity 112 6.3 Arsenic 112 6.3.1 Salvarsan: the magic bullet – the start of chemotherapy 113 6.3.2 Arsenic trioxide: a modern anticancer drug? 116 6.4 Exercises 119 6.5 Case studies 121 6.5.1 Phosphate solution for rectal use 121 6.5.2 Forensic test for arsenic 121 References 122 Further Reading 122 7 Transition Metals and d-Block Metal Chemistry 123 7.1 What are d-block metals? 123 7.1.1 Electronic configurations 123 7.1.2 Characteristic properties 124 7.1.3 Coordination numbers and geometries 125 7.1.4 Crystal field theory 129 7.2 Group 10: platinum anticancer agents 132 7.2.1 Cisplatin 134 7.2.2 Platinum anticancer agents 140 7.3 Iron and ruthenium 147 7.3.1 Iron 148 7.3.2 Ruthenium 155 7.4 The coinage metals 159 7.4.1 General chemistry 159 7.4.2 Copper-containing drugs 160 7.4.3 Silver: the future of antimicrobial agents? 163 7.4.4 Gold: the fight against rheumatoid arthritis 165 7.5 Group 12 elements: zinc and its role in biological systems 168 7.5.1 General chemistry 169 7.5.2 The role of zinc in biological systems 170 7.5.3 Zinc: clinical applications and toxicity 173 7.6 Exercises 177 7.7 Case studies 179 7.7.1 Silver nitrate solution 179 7.7.2 Ferrous sulfate tablets 179 7.7.3 Zinc sulfate eye drops 180 References 181 Further Reading 181 8 Organometallic Chemistry 183 8.1 What is organometallic chemistry? 183 8.2 What are metallocenes? 185 8.3 Ferrocene 187 8.3.1 Ferrocene and its derivatives as biosensors 188 8.3.2 Ferrocene derivatives as potential antimalarial agent 189 8.3.3 Ferrocifen – a new promising agent against breast cancer? 191 8.4 Titanocenes 194 8.4.1 History of titanium-based anticancer agents: titanocene dichloride and budotitane 195 8.4.2 Further developments of titanocenes as potential anticancer agents 197 8.5 Vanadocenes 200 8.5.1 Vanadocene dichloride as anticancer agents 202 8.5.2 Further vanadium-based drugs: insulin mimetics 203 8.6 Exercises 207 8.7 Case study – titanium dioxide 209 References 210 Further Reading 210 9 The Clinical Use of Lanthanoids 211 9.1 Biology and toxicology of lanthanoids 211 9.2 The clinical use of lanthanum carbonate 213 9.3 The clinical application of cerium salts 214 9.4 The use of gadolinium salts as MRI contrast agents 215 9.5 Exercises 219 9.6 Case study: lanthanum carbonate tablets 221 References 222 Further Reading 222 10 Radioactive Compounds and Their Clinical Application 223 10.1 What is radioactivity? 223 10.1.1 The atomic structure 223 10.1.2 Radioactive processes 224 10.1.3 Radioactive decay 224 10.1.4 Penetration potential 227 10.1.5 Quantification of radioactivity 227 10.2 Radiopharmacy: dispensing and protection 232 10.3 Therapeutic use of radiopharmaceuticals 233 10.3.1 131Iodine: therapy for hyperthyroidism 233 10.3.2 89Strontium 234 10.3.3 Boron neutron capture therapy (BNCT) 235 10.4 Radiopharmaceuticals for imaging 235 10.4.1 99mTechnetium 237 10.4.2 18Fluoride: PET scan 240 10.4.3 67Gallium: PET 241 10.4.4 201Thallium 242 10.5 Exercises 245 10.6 Case studies 247 10.6.1 A sample containing 99mTc was found to have a radioactivity of 15 mCi at 8 a.m. when the sample was tested. 247 10.6.2 A typical intravenous dose of 99mTc-albumin used for lung imaging contains a radioactivity of 4 mCi 247 10.6.3 Develop a quick-reference radioactive decay chart for 131I 247 References 248 Further Reading 248 11 Chelation Therapy 249 11.1 What is heavy-metal poisoning? 249 11.2 What is chelation? 250 11.3 Chelation therapy 252 11.3.1 Calcium disodium edetate 252 11.3.2 Dimercaprol (BAL) 253 11.3.3 Dimercaptosuccinic acid (DMSA) 254 11.3.4 2,3-Dimercapto-1-propanesulfonic acid (DMPS) 254 11.3.5 Lipoic acid (ALA) 254 11.4 Exercises 257 11.5 Case studies 259 11.5.1 Disodium edetate 259 11.5.2 Dimercaprol 259 References 261 Further Reading 261 Index 263

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Book SynopsisAny successful theory of bonding in chemistry should explain in the easiest way why atoms are bonded in molecules or not, the structure and shape of molecules in space and how molecules interact in long range.Trade Review"In summary, although this book has one foot in the past and the other as well, it serves as a usefulcollection of case studies in standard models of short and long range interactions." (Chemistry World, 18 February 2011) Table of ContentsPreface xi 1 Mathematical Foundations 1 1.1 Matrices and Systems of Linear Equations 1 1.2 Properties of Eigenvalues and Eigenvectors 6 1.3 Variational Approximations 10 1.4 Atomic Units 15 1.5 The Electron Distribution in Molecules 17 1.6 Exchange-overlap Densities and the Chemical Bond 19 Part 1: Short-range Interactions 27 2 The Chemical Bond 29 2.1 An Elementary Molecular Orbital Model 30 2.2 Bond Energies and Pauli Repulsions in Homonuclear Diatomics 34 2.2.1 The Hydrogen Molecular Ion H2+ (N=1) 35 2.2.2 The Hydrogen Molecule H2(N=2) 35 2.2.3 The Helium Molecular Ion He2+ (N=3) 35 2.2.4 The Helium Molecule He2 (N=4) 36 2.3 Multiple Bonds 37 2.3.1 σ2π2 Description of the Double Bond 38 2.3.2 B12B22 Bent (or Banana) Description of the Double Bond 40 2.3.3 Hybridization Effects 42 2.3.4 Triple Bonds 46 2.4 The Three-centre Double Bond in Diborane 47 2.5 The Heteropolar Bond 49 2.6 Stereochemistry of Polyatomic Molecules 55 2.6.1 The Molecular Orbital Model of Directed Valency 55 2.6.2 Analysis of the MO Bond Energy 58 2.7 sp-Hybridization Effects in First-row Hydrides 60 2.7.1 The Methane Molecule 61 2.7.2 The Hydrogen Fluoride Molecule 64 2.7.3 The Water Molecule 75 2.7.4 The Ammonia Molecule 87 2.8 Delocalized Bonds 96 2.8.1 The Ethylene Molecule 98 2.8.2 The Allyl Radical 98 2.8.3 The Butadiene Molecule 100 2.8.4 The Cyclobutadiene Molecule 102 2.8.5 The Benzene Molecule 104 2.9 Appendices 108 2.9.1 The Second Derivative of the Hückel Energy 108 2.9.2 The Set of Three Coulson Orthogonal Hybrids 109 2.9.3 Calculation of Coefficients of Real MOs for Benzene 110 3 An Introduction to Bonding in Solids 119 3.1 The Linear Polyene Chain 120 3.1.1 Butadiene N = 4 122 3.2 The Closed Polyene Chain 123 3.2.1 Benzene N = 6 126 3.3 A Model for the One-dimensional Crystal 131 3.4 Electronic Bands in Crystals 133 3.5 Insulators, Conductors, Semiconductors and Superconductors 138 3.6 Appendix: The Trigonometric Identity 143 Part 2: Long-Range Interactions 145 4 The van der Waals Bond 147 4.1 Introduction 147 4.2 Elements of Rayleigh–Schrödinger (RS) Perturbation Theory 149 4.3 Molecular Interactions 151 4.3.1 Non-expanded Energy Corrections up to Second Order 152 4.3.2 Expanded Energy Corrections up to Second Order 153 4.4 The Two-state Model of Long-range Interactions 157 4.5 The van der Waals Interactions 159 4.5.1 Atom–Atom Dispersion 161 4.5.2 Atom–Linear Molecule Dispersion 162 4.5.3 Atom–Linear Dipolar Molecule10 Induction 163 4.6 The C6 Dispersion Coefficient for the H–H Interaction 165 4.7 The van der Waals Bond 167 4.8 The Keesom Interaction 169 5 The Hydrogen Bond 177 5.1 A Molecular Orbital Model of the Hydrogen Bond 178 5.2 Electrostatic Interactions and the Hydrogen Bond 179 5.2.1 The Hydrogen Fluoride Dimer (HF)2 182 5.2.2 The Water Dimer (H2O)2 185 5.3 The Electrostatic Model of the Hydrogen Bond 186 5.4 The Rg–HF Heterodimers 197 References 201 Author Index 209 Subject Index 213

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Book SynopsisNew advances in proteomics, driven largely by developments in massspectrometry, continue to reveal the complexity and diversity ofpathogenic mechanisms among microbes that underpin infectiousdiseases.Trade Review“Summary Mass Spectrometry of Microbial Proteomics provides an authoritative guide to the expanding field of microbial proteomics.” (Anal Bioanal Chem, 2011) Table of ContentsPreface List of contributors Microbial Characterisation; the Transition from Conventional Methods to Proteomics. 1) CHANGING CONCEPTS IN THE CHARACTERISATION OF MICROBES AND THE INFLUENCE OF MASS SPECTROMETRY Haroun Shah et al 1.1 Background and early attempts to use mass spectrometry on microbes. 1.2 Characterisation of microorganisms by MALDI-TOF mass spectrometry; from initial ideas to the development of the first comprehensive database. 1.3 Characterisation of microorganisms from their intracellular/membrane bound protein profiles using affinity capture with particular reference to SELDI-TOF-MS. 1.4 Comparative analysis of proteomes of diverse strains within a species; use of 2-d fluorescence difference gel electrophoresis (dige). 1.5 Searching for low abundant and low molecular weight proteins and peptides using nanoparticles as a selective and concentration probes for MALDI-TOF-MS analysis. 2) MICROBIAL PHYLOGENY AND EVOLUTION BASED ON PROTEIN SEQUENCES (THE CHANGE FROM TARGETED GENES TO PROTEINS) Radhey Gupta 2.1 Abstract 2.2 Microbial phylogeny: overview and key unresolved issues 2.3 New protein-based molecular markers for systematic and evolutionary studies 2.4 Molecular markers elucidating the evolutionary relationships among alpha (a)-proteobacteria 2.5 Molecular markers for the bacteroidetes-chlorobi phyla 2.6 Branching order and interrelationships among bacterial phyla 2.7 Importance of protein markers for discovering unique properties for different groups of bacteria 2.8 Concluding remarks 2.9 Acknowledgements 2.10 References 2: PROTEOMICS TOOLS AND BIOMARKER DISCOVERY. 3) OVERVIEW OF THE PROTEOMIC TOOLS AND IT LINKS TO GENOMICS Raju Misra. 3.1 Protein identification 3.2 Peptide Mass Fingerprint (PMF) 3.3 Peptide Fragment Fingerprint (PFF) 3.4 Peptide sequencing 3.5 False discovery rates (FDR) 3.6 Validating protein identifications 3.7 Reference Database 3.8 Data storage 3.9 Biomarker discovery 3.10 Integrating genomics with proteomics 3.11 Reference List 4) HIGH THROUGHPUT BIOMARKER DISCOVERY IN MICROORGANISMS Ming Fang 4.1 MALDI vs ESI 4.2 Tandem Mass Spectrometry and Hybrid Mass Spectrometers 4.3 Fragmentation in Tandem Mass Spectrometry Proteomic Strategies for Protein Identification 1. Bottom-up Proteomics 2. Top-down Proteomics Multidimensional Protein Identification Mass Spectrometry Based Targeted Protein Quantification and Biomarker Discovery Selected Reaction Monitoring Conclusions 5) MALDI MASS SPECTROMETRY IMAGING, A NEW FRONTIER IN BIOSTRUCTURAL TECHNIQUES: APPLICATIONS IN BIOMEDICINE Simona Francese and Malcolm R. Clench 5.1 Introduction 5.2 Practical Aspects of MALDI-MSI 5.2 Applications 5.3 Microbial molecular investigation by MALDI TOF MS 5.4 Conclusions 5.5 References 3: PROTEIN SAMPLES PREPARATION TECHNIQUES CONVENTIONAL APPROACHES FOR SAMPLE PREPARATION FOR LIQUID CHROMATOGRAPHY AND TWO-DIMENSIONAL GEL ELECTROPHORESIS Vesela Encheva and Robert Parker 6.1 Introduction 6.2 Cell lysis methods 6.3 Sample preparation for 2D GE 6.4 Fractionation strategies 6.5 Sample preparation for Liquid Chromatography coupled to mass 6.6 Conclusion 6.7 Reference list 7) ISOLATION AND PREPARATION OF SPORE PROTEINS AND SUBSEQUENT CHARACTERISATION BY ELECTROPHORESIS AND MASS SPECTROMETRY Nicola Thorne, Saheer Gharbia and Haroun Shah 7.1 Introduction 7.2 Experimental 2.1 Sporulation media 7.3 Conclusion 8) CHARACTERIZATION OF BACTERIAL MEMBRANE PROTEINS USING A NOVEL COMBINATION OF A LIPID BASED PROTEIN IMMOBILIZATION TECHNIQUE WITH MASS SPECTROMETRY Roger Karlsson, Darren Chooneea, Elisabet Carlsohn, Vesela Encheva and Haroun Shah 8.1 Introduction 8.2 The surface proteome 8.3 Proteomics of pathogenic bacteria 8.4 Lipid-based protein immobilization technology 8.5 Salmonella Typhimurium – disease mechanism and outer membrane proteins 8.6 Outer membrane proteins of S. Typhimurium 8.7 Helicobacter pylori – disease mechanism and outer membrane proteins 8.8 Surface proteins of intact Helicobacter pylori 9) Wider Protein Detection from Biological Extracts by the Reduction of Dynamic Concentration Range. Luc Guerrier, Egisto Boschetti and Piergiorgi Roghetti 9.1 Introduction 9.2 Dealing with low-abundance protein discovery 9.3 Conclusions and future prospects 9.4 References 10) 3D-gel electrophoresis - a new development in protein analysis. Robert Ventzki and Josef Stegemann 10.1. Introduction 10.2. Methods 10.3 Results and discussion 10.4 References SECTION 4: CHARACTERISATION OF MICROORGANISMS BY PATTERN MATCHING OF MASS SPECTRAL PROFILES AND BIOMARKER APPROACHES REQUIRING MINIMAL SAMPLE PREPARATION. 11) Microbial Disease Biomarkers using ProteinChip Arrays Shea Hamilton, Michael Levin, J. Simon Kroll, Paul R. Langford 11.1 Introduction 11.2 Biomarker studies involving patients infected with viruses 11.3 Biomarker studies involving patients infected with parasites 11.4 Biomarker studies involving patients infected with bacteria 11.5 Other diseases of possible infectious origin 11.6 Conclusions 11.7 References 12) MALDI-TOF MS and microbial identification: years of experimental development to an established protocol. Wibke Kallow, Marcel Erhard, Haroun N. Shah, Emmanuel Raptakis, Martin Welker. 12.1 Identification of Microorganisms in Clinical Routine 12.2 Mass Spectrometry and Microbiology 12.3 Mass Spectral ‘Fingerprints’ of Whole Cells 12.4 Reproducibility of Mass Spectral Fingerprints 12.5 Species and Strain Discrimination by Mass Spectrometry 12.6 Pattern Matching Approaches for automated Identification 12.7 Mass Spectral Identification of Microorganism – Requirements for Routine Diagnostics 12.8 Automated Mass Spectral Analysis of Microorganisms in Clinical Routine Diagnostics 12.9 Acknowledgements and references 5: Targeted Molecules and Analysis of Specific Microorganisms. 13) Whole Cell MALDI Mass Spectrometry for the Rapid Characterisation of Bacteria; A Survey of Applications to Major Phyletic Lines in Microbial Kingdom. Ben van Baar 13.1 Introduction 13.2Scope 13.3 Reproducibility 13.3.1 Factors concerning the sample 13.4 Factors concerning the MALDI MS process 13.5 Sample application and ionisation 13.5 Data analysis 13.6 Spectrum libraries 13.6Whole cell MALDI MS of particular bacteria genera and species Bacillus spp. Staphylococcus spp. Streptococcus spp. Mycobacterium spp. Other Gram-positive bacteria Escherichia coli Gram-negative food- and waterborne pathogen proteobacteria, other than E. Coli Typical sexually transmitted pathogens: Neisseria spp. and Haemophilus spp. Gram-negative biothreat agent bacteria Other Gram-negative bacteria Pathogenic Cyanobacteria Strategies for the identification of biomarkers in whole cell MALDI MS spectra Protein database consideration On-target treatment and analysis Off-target’ Analysis and correlation with proteomics studies General consideration of biomarker identification strategies Conclusions and outlook 14) The power of Gel-based proteomics to understand physiology in Bacillus subtilis Haike Antelmann and Michael Hecker Introduction Results 1 Proteomics of protein secretion mechanisms in Bacillus subtilis 1.1. Protein export machineries of B. subtilis 1.1 The extracellular proteome of B. subtilis 1.2 The cell wall proteome of B. subtilis 1.3. The membrane attached lipoproteome of B. subtilis 1.3 The proteome analysis of protein secretion mechanisms in B. subtilis 2 Definition of proteomic signatures to study cell physiology 2.1. Proteomic signatures of B. subtilis in response to stress and starvation 2.2. Proteomic signatures of B. subtilis in response to thiol-reactive electrophiles uncovered novel regulatory mechanisms 2.3. The MarR/DUF24-family YodB repressor is directly sensing thiol- reactive electrophiles via the conserved Cys6 residue 3 Proteomics as tool to visualize reversible and irreversible thiol- modifications 3.1. The thiol-redox proteome of B. subtilis in response to diamide and quinones 3.2. Depletion of thiol-containing proteins by quinones due to thiol-(S)- alkylation 4 Proteomics as tool to define regulon structures and targets for non- coding RNAs 5 Acknowledgment 15) Mass Spectrometry in the study of Tularemia Pathogenesis. Jiri Stulik, Juraj Lenco, Jiri Dresler, Jana Klimentova, Lenka Hernychova, Lucie Balonova and Alena Fucikova. 15.1 Introduction to molecular pathogenesis of Francisella tularensis infection 15.2 Francisella tularensis LVS proteome alterations induced by different temperatures and stationary phase of growth 15.3Analysis of membrane protein complexes of Francisella tularensis 15.4 Analysis of Francisella tularensis glycoproteins and phosphoproteins 15.5Identification of Francisella tularensis transcription factors potentially involved in its virulence 15.6 Acknowledgements References 16) Bacterial Post-Genomics for Vaccine development Giulia Bernardini, Daniela Braconi and Annalisa Santucci Summary comparative genomics transcriptomics proteomics and immmunoproteomics other high-throughput technologies meningococcal vaccines and reverse vaccinology helicobacter pylori vaccines conclusions references 6 Statistical Analysis of 2D Gels and Analysis of Mass Spectral Data Machine Learning Techniques for the Analysis of Mass spectrometry Data. Graham Ball and Ali Al-Shahib 17.1 Introduction 17.2 Pre-processing MS data 17.3 Classification of MS data 17.4 Evaluation of Classification Models 18) Mass Spectrometry for microbial Proteomics: Issues in data analysis with electrophoretic or mass spectrometric expression proteomic data. Natasha A. Karp Title page Foreword 18.1 Introduction 18.2 Experimental design 18.3 Data analysis 18.4 Validation 18.5 Conclusions 18.6 Figure legends 18.7 References Section 7: DNA Resequencing by MALDI-TOF-Mass Spectrometry and its Application to Traditional Microbiological Problems. (19) Comparative DNA sequence analysis and typing using Mass Spectrometry Christiane Honisch,Yong Chen and Franz Hillenkamp 19.1 Introduction 19.2 Comparative Sequence Analysis by MALDI-TOF MS 19.3 Applications of nucleic acid analysis by MALDI-TOF MS in clinical microbiology 19.4 Conclusion References (20) Transfer of a Traditional Serotyping System (Kauffmann-White) onto a MALDI-TOF-MS platform for the rapid Typing of Salmonella isolates. Chloe Bishop, Cath Arnold and Saheer Gharbia Typing of salmonella isolates 1.1 Introduction 1.2 Salmonella, the pathogen Biology Pathogenesis Clinical Disease 1.3 Complex genetic structure and the need to subtype this genus Phylogeny Virulence and Gene Transfer Necessity to subtype >1.4 Antigenic Analysis - The Traditional Kauffmann - White Schema and its future Serotyping Flagellar Antigens Flagellar Variation Somatic Antigens 1.5 Sequence-based methods to determine serotypes Flagellin sequences correspond directly to Salmonella serotype. Specific SNPs Subtyping by antigen sequence Variation of the Rfb Genes 1.6 Transferring the Sequences to a MALDI platform for Rapid Analysis Intro Different methods available MALDI-TOF data analysis Salmonella molecular serotyping as a Case Study Gene Selection Results Overview Clustering and Sequence Variation of Amplicons 1.7 Conclusions and Summary Closing Remarks

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Book SynopsisThis 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.Trade Review"This book is very much ‘‘an aid to this end'' and should be number one on every young chromatographer's book list. The publishers too have played their part in producing a book that is pleasing on the eye and a pleasure to read." (Chromatographia, 1 December 2010)Table of ContentsPreface to the Fifth Edition. Important and Useful Equations for HPLC. 1 Introduction. 1.1 HPLC: A powerful separation method. 1.2 A first HPLC experiment. 1.3 Liquid chromatographic separation modes. 1.4 The HPLC instrument. 1.5 Safety in the HPLC laboratory. 1.6 Comparison between high-performance liquid chromatography and gas chromatography. 1.7 Comparison between high-performance liquid chromatography and capillary electrophoresis. 1.8 Units for pressure, length and viscosity. 1.9 Scientific journals. 1.10 Recommended books. 2 Theoretical Principles. 2.1 The chromatographic process. 2.2 Band broadening. 2.3 The chromatogram and its purport. 2.4 Graphical representation of peak pairs with different degree of resolution. 2.5 Factors affecting resolution. 2.6 Extra-column volumes (dead volumes). 2.7 Tailing. 2.8 Peak capacity and statistical resolution probability. 2.9 Effects of temperature in HPLC. 2.10 The limits of HPLC. 2.11 How to obtain peak capacity. 3 Pumps. 3.1 General requirements. 3.2 The short-stroke piston pump. 3.3 Maintenance and repair. 3.4 Other pump designs. 4 Preparation of Equipment up to Sample Injection. 4.1 Selection of the mobile phase. 4.2 Preparation of the mobile phase. 4.3 Gradient systems. 4.4 Capillary tubing. 4.5 Fittings. 4.6 Sample injectors. 4.7 Sample solution and sample volume. 5 Solvent Properties. 5.1 Table of organic solvents. 5.2 Solvent selectivity. 5.3 Miscibility. 5.4 Buffers. 5.5 Shelf life of mobile phases. 5.6 The mixing cross. 6 Detectors. 6.1 General. 6.2 UV detectors. 6.3 Refractive index detectors. 6.4 Fluorescence detectors. 6.5 Electrochemical (amperometric) detectors. 6.6 Light-scattering detectors. 6.7 Other detectors. 6.8 Multiple detection. 6.9 Indirect detection. 6.10 Coupling with spectroscopy. 7 Columns and Stationary Phases. 7.1 Columns for HPLC. 7.2 Precolumns. 7.3 General properties of stationary phases. 7.4 Silica. 7.5 Chemically modified silica. 7.6 Styrene-divinylbenzene. 7.7 Some other stationary phases. 7.8 Column care and regeneration. 8 HPLC Column Tests. 8.1 Simple tests for HPLC columns. 8.2 Determination of particle size. 8.3 Determination of breakthrough time. 8.4 The test mixture. 8.5 Dimensionless parameters for HPLC column characterization. 8.6 The van Deemter equation from reduced parameters and its use in column diagnosis. 8.7 van Deemter curves and other coherences. 8.8 Diffusion coefficients. 9 Adsorption Chromatography: Normal-Phase Chromatography. 9.1 What is adsorption?. 9.2 The eluotropic series. 9.3 Selectivity properties of the mobile phase. 9.4 Choice and optimization of the mobile phase. 9.5 Applications. 10 Reversed-Phase Chromatography. 10.1 Principle. 10.2 Mobile phases in reversed-phase chromatography. 10.3 Solvent selectivity and strength. 10.4 Stationary phases. 10.5 Method development in reversed-phase chromatography. 10.6 Applications. 10.7 Hydrophobic interaction chromatography. 11 Chromatography with Chemically Bonded Phases. 11.1 Introduction. 11.2 Properties of some stationary phases. 11.3 Hydrophilic interaction chromatography. 12 Ion-Exchange Chromatography. 12.1 Introduction. 12.2 Principle. 12.3 Properties of ion exchangers. 12.4 Influence of the mobile phase. 12.5 Special possibilities of ion exchange. 12.6 Practical hints. 12.7 Applications. 13 Ion-Pair Chromatography. 13.1 Introduction. 13.2 Ion-pair chromatography in practice. 13.3 Applications. 13.4 Appendix: UV detection using ion-pair reagents. 14 Ion Chromatography. 14.1 Principle. 14.2 Suppression techniques. 14.3 Phase systems. 14.4 Applications. 15 Size-Exclusion Chromatography. 15.1 Principle. 15.2 The calibration chromatogram. 15.3 Molecular mass determination by means of size-exclusion chromatography. 15.4 Coupled size-exclusion columns. 15.5 Phase systems. 15.6 Applications. 16 Affinity Chromatography. 16.1 Principle. 16.2 Affinity chromatography as a special case of HPLC. 16.3 Applications. 17 Choice of Method. 17.1 The various possibilities. 17.2 Method transfer. 18 Solving the Elution Problem. 18.1 The elution problem. 18.2 Solvent gradients. 18.3 Column switching. 18.4 Comprehensive two-dimensional HPLC. 18.5 Optimization of an isocratic chromatogram using four solvents. 18.6 Optimization of the other parameters. 18.7 Mixed stationary phases. 19 Analytical HPLC. 19.1 Qualitative analysis. 19.2 Trace analysis. 19.3 Quantitative analysis. 19.4 Recovery. 19.5 Peak-height and peak-area determination for quantitative analysis. 19.6 Integration errors. 19.7 The detection wavelength. 19.8 Derivatization. 19.9 Unexpected peaks: Ghost and system peaks. 20 Quality Assurance. 20.1 Is it worth the effort?. 20.2 Verification with a second method. 20.3 Method validation. 20.4 Standard operating procedures. 20.5 Measurement uncertainty. 20.6 Qualifications, instrument test and system suitability test. 20.7 The quest for quality. 21 Preparative HPLC. 21.1 Problem. 21.2 Preparative HPLC in practice. 21.3 Overloading effects. 21.4 Fraction collection. 21.5 Recycling. 21.6 Displacement chromatography. 22 Separation of Enantiomers. 22.1 Introduction. 22.2 Chiral mobile phases. 22.3 Chiral liquid stationary phases. 22.4 Chiral solid stationary phases. 22.5 Indirect separation of enantiomers. 23 Special Possibilities. 23.1 Micro, capillary and chip HPLC. 23.2 High-speed and super-speed HPLC. 23.3 Fast separations at 1000 bar: UHPLC. 23.4 HPLC with supercritical mobile phases. 23.5 HPLC with superheated water. 23.6 Electrochromatography. 24 Appendix 1: Applied HPLC Theory. 25 Appendix 2: How to Perform the Instrument Test. 25.1 Introduction. 25.2 Test sequence. 25.3 Preparations. 25.4 Pump test. 25.5 UV detector test. 25.6 Autosampler test. 25.7 Column oven test. 25.8 Equations and calculations. 25.9 Documentation. 26 Appendix 3: Troubleshooting. 26.1 Pressure problems. 26.2 Leak in the pump system. 26.3 Deviating retention times. 26.4 Injection problems. 26.5 Baseline problems. 26.6 Peak shape problems. 26.7 Problems with light-scattering detectors. 26.8 Other causes. 26.9 Instrument test. 27 Appendix 4: Column Packing. Index of Separations. Subject Index.

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Book SynopsisThis 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.Table of ContentsPreface to the Fifth Edition xiii Important and Useful Equations for HPLC 1 vii 1 Introduction 5 1.1 HPLC: A powerful separation method 5 1.2 A first HPLC experiment 5 1.3 Liquid chromatographic separation modes 8 1.4 The HPLC instrument 9 1.5 Safety in the HPLC laboratory 10 1.6 Comparison between high-performance liquid chromatography and gas chromatography 11 1.7 Comparison between high-performance liquid chromatography and capillary electrophoresis 12 1.8 Units for pressure, length and viscosity 13 1.9 Scientific journals 14 1.10 Recommended books 15 2 Theoretical Principles 17 2.1 The chromatographic process 17 2.2 Band broadening 19 2.3 The chromatogram and its purport 23 2.4 Graphical representation of peak pairs with different degree of resolution 30 2.5 Factors affecting resolution 35 2.6 Extra-column volumes (dead volumes) 40 2.7 Tailing 41 2.8 Peak capacity and statistical resolution probability 46 2.9 Effects of temperature in HPLC 49 2.10 The limits of HPLC 51 2.11 How to obtain peak capacity 55 3 Pumps 59 3.1 General requirements 59 3.2 The short-stroke piston pump 59 3.3 Maintenance and repair 62 3.4 Other pump designs 63 4 Preparation of Equipment up to Sample Injection 65 4.1 Selection of the mobile phase 65 4.2 Preparation of the mobile phase 67 4.3 Gradient systems 68 4.4 Capillary tubing 70 4.5 Fittings 72 4.6 Sample injectors 74 4.7 Sample solution and sample volume 78 5 Solvent Properties 81 5.1 Table of organic solvents 81 5.2 Solvent selectivity 83 5.3 Miscibility 83 5.4 Buffers 84 5.5 Shelf life of mobile phases. 87 5.6 The mixing cross 88 6 Detectors 91 6.1 General 91 6.2 UV detectors 96 6.3 Refractive index detectors 99 6.4 Fluorescence detectors 101 6.5 Electrochemical (amperometric) detectors 103 6.6 Light-scattering detectors 104 6.7 Other detectors 106 6.8 Multiple detection 107 6.9 Indirect detection 108 6.10 Coupling with spectroscopy 109 7 Columns and Stationary Phases 117 7.1 Columns for HPLC 117 7.2 Precolumns 119 7.3 General properties of stationary phases 120 7.4 Silica 125 7.5 Chemically modified silica 126 7.6 Styrene-divinylbenzene 129 7.7 Some other stationary phases 133 7.8 Column care and regeneration 136 8 HPLC Column Tests 141 8.1 Simple tests for HPLC columns 141 8.2 Determination of particle size 143 8.3 Determination of breakthrough time 144 8.4 The test mixture 146 8.5 Dimensionless parameters for HPLC column characterization 148 8.6 The van Deemter equation from reduced parameters and its use in column diagnosis 152 8.7 van Deemter curves and other coherences 153 8.8 Diffusion coefficients 155 9 Adsorption Chromatography: Normal-Phase Chromatography 159 9.1 What is adsorption? 159 9.2 The eluotropic series 162 9.3 Selectivity properties of the mobile phase 165 9.4 Choice and optimization of the mobile phase 166 9.5 Applications 168 10 Reversed-Phase Chromatography 173 10.1 Principle 173 10.2 Mobile phases in reversed-phase chromatography 174 10.3 Solvent selectivity and strength 177 10.4 Stationary phases 181 10.5 Method development in reversed-phase chromatography 185 10.6 Applications 188 10.7 Hydrophobic interaction chromatography 191 11 Chromatography with Chemically Bonded Phases 195 11.1 Introduction 195 11.2 Properties of some stationary phases 195 11.3 Hydrophilic interaction chromatography 200 12 Ion-Exchange Chromatography 203 12.1 Introduction 203 12.2 Principle 203 12.3 Properties of ion exchangers 204 12.4 Influence of the mobile phase 207 12.5 Special possibilities of ion exchange 208 12.6 Practical hints 210 12.7 Applications 213 13 Ion-Pair Chromatography 217 13.1 Introduction 217 13.2 Ion-pair chromatography in practice 218 13.3 Applications 220 13.4 Appendix: UV detection using ion-pair reagents 221 14 Ion Chromatography 225 14.1 Principle 225 14.2 Suppression techniques 226 14.3 Phase systems 226 14.4 Applications 230 15 Size-Exclusion Chromatography 231 15.1 Principle 231 15.2 The calibration chromatogram 234 15.3 Molecular mass determination by means of size-exclusion chromatography 238 15.4 Coupled size-exclusion columns 241 15.5 Phase systems 243 15.6 Applications 244 16 Affinity Chromatography. 249 16.1 Principle 249 16.2 Affinity chromatography as a special case of HPLC 251 16.3 Applications 252 17 Choice of Method 255 17.1 The various possibilities 255 17.2 Method transfer 260 18 Solving the Elution Problem 263 18.1 The elution problem 263 18.2 Solvent gradients 264 18.3 Column switching 270 18.4 Comprehensive two-dimensional HPLC 272 18.5 Optimization of an isocratic chromatogram using four solvents 273 18.6 Optimization of the other parameters 276 18.7 Mixed stationary phases 284 19 Analytical HPLC 285 19.1 Qualitative analysis 285 19.2 Trace analysis 287 19.3 Quantitative analysis 291 19.4 Recovery 296 19.5 Peak-height and peak-area determination for quantitative analysis 299 19.6 Integration errors 303 19.7 The detection wavelength 304 19.8 Derivatization 306 19.9 Unexpected peaks: Ghost and system peaks 308 20 Quality Assurance 311 20.1 Is it worth the effort? 311 20.2 Verification with a second method 312 20.3 Method validation 312 20.4 Standard operating procedures 314 20.5 Measurement uncertainty 315 20.6 Qualifications, instrument test and system suitability test 317 20.7 The quest for quality 318 21 Preparative HPLC 321 21.1 Problem 321 21.2 Preparative HPLC in practice 322 21.3 Overloading effects 325 21.4 Fraction collection 328 21.5 Recycling 330 21.6 Displacement chromatography 331 22 Separation of Enantiomers 333 22.1 Introduction 333 22.2 Chiral mobile phases 335 22.3 Chiral liquid stationary phases 336 22.4 Chiral solid stationary phases 337 22.5 Indirect separation of enantiomers 345 23 Special Possibilities 349 23.1 Micro, capillary and chip HPLC 349 23.2 High-speed and super-speed HPLC 352 23.3 Fast separations at 1000 bar: UHPLC 353 23.4 HPLC with supercritical mobile phases 355 23.5 HPLC with superheated water 359 23.6 Electrochromatography 361 24 Appendix 1: Applied HPLC Theory 363 25 Appendix 2: How to Perform the Instrument Test 373 25.1 Introduction 373 25.2 Test sequence 373 25.3 Preparations 374 25.4 Pump test. 377 25.5 UV detector test 379 25.6 Autosampler test 383 25.7 Column oven test 383 25.8 Equations and calculations. 384 25.9 Documentation 385 26 Appendix 3: Troubleshooting 387 26.1 Pressure problems 387 26.2 Leak in the pump system 389 26.3 Deviating retention times 389 26.4 Injection problems 390 26.5 Baseline problems 390 26.6 Peak shape problems 392 26.7 Problems with light-scattering detectors 393 26.8 Other causes 394 26.9 Instrument test 395 27 Appendix 4: Column Packing 397 Index of Separations 401 Subject Index 403

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Book SynopsisThis text offers an open-learning approach to Raman spectroscopy providing detail on instrumentation, applications and discussions questions throughout the book. It provides a valuable guide to assist with teaching Raman spectroscopy which is gaining attention in (analytical) chemistry, and as a consequence, teaching programs have followed. Today, education in Raman spectroscopy is often limited to theoretical aspects (e.g. selection rules), but practical aspects are usually disregarded. With these course notes, the author hopes to fill this gap and include information about Raman instrumentation and how it is interpreted. Provides auser-friendly text that tackles the theoretical background, and offers everyday tips for common practice Raman instrumentation and practical aspects, which are sometimes overlooked, are covered Appropriate for students, and includes summaries, text boxes, illustrating the ideas with examples from research literatTrade Review“The book is written in the style of an introductory university lecture, each chapter beginning with a list of learning objectives, which can be later used as a quick reference guide to the chapter contents.” (Chemistry World, 1 June 2014) Table of ContentsPreface xi Acknowledgements xiii Acronyms, Abbreviations and Symbols xv About the Author xvii Introduction to Raman spectroscopy xix 1 Theoretical Aspects 1 1.1 Classical Approach 1 1.2 Selection Rule 7 1.3 Energy Levels and Group Frequencies 13 1.4 Raman Intensity 19 1.5 Raman Bandwidth 35 1.6 The General Appearance of a Raman Spectrum 37 1.7 Summary 38 Intermezzo 1.1 The Harmonic Oscillator and the Position of the Vibrational Energy Levels 6 Intermezzo 1.2 The Anharmonic Oscillator and the Position of Vibrational Energy Levels 11 Intermezzo 1.3 Raman Intensity Annotations 30 2 Interferences and Side-effects 39 2.1 Absorption 40 2.2 Fluorescence 40 2.3 Thermal Effects, Photodecomposition and Laser Ablation 43 2.4 Ambient Light and Background Radiation 44 2.5 Summary 44 3 Enhancement of the Raman Signal 47 3.1 Resonance Raman (RR) Spectroscopy 48 3.2 Surface-Enhanced Raman Spectroscopy (SERS) 48 3.3 Summary 59 Intermezzo 3.1 The Analysis of Organic Dyes by SERS 58 4 Raman Instrumentation 61 4.1 Lasers 62 4.2 Detectors 74 4.3 Filters 81 4.4 Dispersion Systems 83 4.5 Components for Transportation of Light 88 4.6 Sample Chambers and Measurement Probes 91 4.7 Noise in Raman Spectroscopy 95 4.8 Summary 99 5 Raman Spectroscopy in Daily Lab-life 101 5.1 Calibration of a Raman Spectrometer 102 5.2 Raman Spectral Post-processing 108 5.3 Interpretation of Raman Spectra of Organic Molecules 116 5.4 Interpretation of Raman Spectra of Inorganic Molecules 131 5.5 Quantitative Aspects of Raman Spectroscopy 134 5.6 Fingerprinting and Spectral Searching Algorithms 137 5.7 Raman Mapping and Imaging 141 5.8 Combination with Other Techniques 145 5.9 Summary 147 Intermezzo 5.1 Micro-Raman Spectroscopy in Microbiology 107 Intermezzo 5.2 Raman Spectroscopy in a Forensics Laboratory 117 Intermezzo 5.3 Pigment Analysis with Raman Spectroscopy 132 Intermezzo 5.4 Detection of Counterfeit Medicines with Raman Spectroscopy 136 Intermezzo 5.5 Exobiology: Raman Spectroscopy Helps the Search for Life on Mars 139 Intermezzo 5.6 Direct Analysis of Precious Art Objects 144 Responses to Questions 149 Bibliography 153 Glossary of Terms 155 SI Units and Physical Constants 157 Periodic Table 163 Index 165

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Book SynopsisAs an area of high topical interest, Biopolymers New materials for Sustainable Films and Coatings covers the development and utilization of polymers derived from bioresources, with a particular focus on film and coating applications. With growing concern for the environment and the rising price of crude oil, there is increasing demand for non-petroleum-based polymers from renewable resources. Leading research groups worldwide in industry and academe are working on such technology with the objective of applying the latest advances in the field. Written by well-respected experts, this text systematically covers the extraction and production of selected biopolymers as well as their properties and application as films or coatings in a variety of uses. The areas addressed include food packaging, edible coatings, paper coatings and agricultural films. Intended for researchers and students, this book will also be of interest to industry, especially in terms of the prTrade Review"All in all it gives a very good insight in the use of films and coatings from bio-based polymers for technicians as well as for other interested experts." (Encyclopedia of Industrial Biotechnology, 5 September 2011) Table of ContentsPreface. About the Editor. List of Contributors. PART I. 1 Introductory Overview (David Plackett). 1.1 Introduction. 1.2 Worldwide Markets for Films and Coatings. 1.3 Sustainability. 1.4 Bio-Derived Polymers. 1.5 Other Topics. References. 2 Production, Chemistry and Degradation of Starch-Based Polymers (Analía Vázquez, María Laura Foresti and Viviana Cyras). 2.1 Introduction. 2.2 Gelatinization. 2.3 Effect of Gelatinization Process and Plasticizer on Starch Properties. 2.4 Retrogradation. 2.5 Production of Starch–Polymer Blends. 2.6 Biodegradation of Starch-Based Polymers. 2.7 Concluding Remarks. 2.8 Acknowledgement. References. 3 Production, Chemistry and Properties of Polylactides (Anders Södergård and Saara Inkinen). 3.1 Introduction. 3.2 Production of Polylactides. 3.3 Polylactide Chemistry. 3.4 Properties of Polylactides. 3.5 Concluding Remarks. References. 4 Production, Chemistry and Properties of Polyhydroxyalkanoates (Eric Pollet and Luc Avérous). 4.1 Introduction. 4.2 Polyhydroxyalkanoate Synthesis. 4.3 Properties of Polyhydroxyalkanoates. 4.4 Polyhydroxyalkanoate Degradation. 4.5 PHA-Based Multiphase Materials. 4.6 Production and Commercial Products. References. 5 Chitosan for Film and Coating Applications (Patricia Fernandez-Saiz and José M. Lagaron). 5.1 Introduction. 5.2 Physical and Chemical Characterization of Chitosan. 5.3 Properties and Applications of Chitosan. 5.4 Processing of Chitosan. 5.5 Concluding Remarks. References. 6 Production, Chemistry and Properties of Proteins (Mikael Gällstedt, Mikael S. Hedenqvist and Hasan Ture). 6.1 Introduction. 6.2 Plant-Based Proteins. 6.3 Animal-Based Proteins. 6.4 Solution Casting of Proteins – an Overview. 6.5 Dry Forming of Protein Films. 6.6 Concluding Remarks. References. 7 Synthesis, Chemistry and Properties of Hemicelluloses (Ann-Christine Albertsson, Ulrica Edlund and Indra K. Varma). 7.1 Introduction. 7.2 Structure. 7.3 Sources. 7.4 Extraction Methodology. 7.5 Modifications. 7.6 Applications. 7.7 Concluding Remarks. References. 8 Production, Chemistry and Properties of Cellulose-Based Materials (Mohamed Naceur Belgacem and Alessandro Gandini). 8.1 Introduction. 8.2 Pristine Cellulose as a Source of New Materials. 8.3 Novel Cellulose Solvents. 8.4 Cellulose-Based Composites and Superficial Fiber Modification. 8.5 Cellulose Coupled with Nanoparticles. 8.6 Electronic Applications. 8.7 Biomedical Applications. 8.8 Cellulose Derivatives. 8.9 Concluding Remarks. References. 9 Furan Monomers and their Polymers: Synthesis, Properties and Applications (Alessandro Gandini). 9.1 Introduction. 9.2 Precursors and Monomers. 9.3 Polymers. 9.4 Biodegradability of Furan Polymers. 9.5 Concluding Remarks. References. PART II. 10 Food Packaging Applications of Biopolymer-Based Films (N. Gontard, H. Angellier-Coussy, P. Chalier, E. Gastaldi, V. Guillard, C. Guillaume and S. Peyron). 10.1 Introduction. 10.2 Food Packaging Material Specifications. 10.3 Examples of Biopolymer Applications for Food Packaging Materials. 10.4 Research Directions and Perspectives. 10.5 Concluding Remarks. References. 11 Biopolymers for Edible Films and Coatings in Food Applications (Idoya Ferández-Pan and Juan Ignacio Maté Caballero). 11.1 Introduction. 11.2 Materials for Edible Films and Coatings. 11.3 Edible Films and Coatings for Food Applications. 11.4 Concluding Remarks. References. 12 Biopolymer Coatings for Paper and Paperboard (Christian Aulin and Tom Lindström). 12.1 Introduction. 12.2 Biopolymer Films and Coatings. 12.3 Bio-Nanocomposite Films and Coatings. 12.4 Concluding Remarks. 12.5 Acknowledgement. References. 13 Agronomic Potential of Biopolymer Films (Lluís Martín-Closas and Ana M. Pelacho). 13.1 Introduction. 13.2 The Potential Role of Biodegradable Materials in Agricultural Films. 13.3 Presently Available Biopolymers and Biocomposites. 13.4 Past and Current International Projects on Biodegradable Agricultural Films. 13.5 Present Applications of Biopolymer Films in Agriculture. 13.6 Potential Uses: Current Limitations and Future Applications. 13.7 Concluding Remarks. 13.8 Acknowledgements. References. 14 Functionalized Biopolymer Films and Coatings for Advanced Applications (David Plackett and Vimal Katiyar). 14.1 Introduction. 14.2 Optoelectronics. 14.3 Sensors. 14.4 Miscellaneous Applications. 14.5 Concluding Remarks. References. 15 Summary and Future Perspectives (David Plackett). 15.1 Introduction. 15.2 Bioplastics. 15.3 Bio-Thermoset Resins. 15.4 Nanocomposites Based on Inorganic Nanofillers. 15.5 Nanocomposites Based on Cellulose Nanofillers. 15.6 Concluding Remarks. References. Index.

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Book SynopsisMethods of Molecular Quantum Mechanics This advanced text introduces to the advanced undergraduate and graduate student the mathematical foundations of the methods needed to carry out practical applications in electronic molecular quantum mechanics, a necessary preliminary step before using commercial programmes to carry out quantum chemistry calculations. Major features of the book include: Consistent use of the system of atomic units, essential for simplifying all mathematical formulae Introductory use of density matrix techniques for interpreting properties of many-body systems An introduction to valence bond methods with an explanation of the origin of the chemical bond A unified presentation of basic elements of atomic and molecular interactions The book is intended for advanced undergraduate and first-year graduate students in chemical physics, theoretical and quantum chemistry. In addition, it is relevant to students fTable of ContentsPreface. 1. Principles. 1.1 The Orbital Model. 1.2 Mathematical Methods. 1.3 Basic Postulates. 1.4 Physical Interpretation of the Basic Principles. 2. Matrices. 2.1 Definitions and Elementary Properties. 2.2 Properties of Determinants. 2.3 Special Matrices. 2.4 The Matrix Eigenvalue Problem. 3. Atomic Orbitals. 3.1 Atomic Orbitals as a Basis for Molecular Calculations. 3.2 Hydrogen-like Atomic Orbitals. 3.3 Slater-type Orbitals. 3.4 Gaussian-type Orbitals. 4. The Variation Method. 4.1 Variation Principles. 4.2 Nonlinear Parameters. 4.3 Linear Parameters and the Ritz Method. 4.4 Applications of the Ritz Method. 5. Spin. 5.1 The Zeeman Effect. 5.2 The Pauli Equations for One-electron Spin. 5.3 The Dirac Formula for N-electron Spin. 6. Antisymmetry of Many-electron Wavefunctions. 6.1 Antisymmetry Requirement and the Pauli Principle. 6.2 Slater Determinants. 6.3 Distributions Functions. 6.4 Average Values of Operators. 7. Self-consistent-field Calculations and Model Hamiltonians. 7.1 Elements of Hartree-Fock Theory for Closed Shells. 7.2 Roothaan Formulation of the LCAO-MO-SCF Equations. 7.3 Molecular Self-consistent-field Calculations. 7.4 Hückel Theory. 7.5 A Model for the One-dimensional Crystal. 8. Post-Hartree-Fock Methods. 8.1 Configuration Interaction. 8.2 Multiconfiguration Self-consistent-field. 8.3 Møller-Plesset Theory. 8.4 The MP2-R12 Method. 8.5 The CC-R12 Method. 8.6 Density Functional Theory. 9. Valence Bond Theory and the Chemical Bond. 9.1 The Born-Oppenheimer Approximation. 9.2 The Hydrogen Molecule H2. 9.3 The Origin of the Chemical Bond. 9.4 Valence Bond Theory and the Chemical Bond. 9.5 Hybridization and Molecular Structure. 9.6 Pauling’s Formula for Conjugated and Aromatic Hydrocarbons. 10. Elements of Rayleigh-Schroedinger Perturbation Theory. 10.1 Rayleigh-Schroedinger Perturbation Equations. 10.2 First-order Theory. 10.3 Second-order Theory. 10.4 Approximate E2 Calculations: The Hylleraas Functional. 10.5 Linear Pseudostates and Molecular Properties. 10.6 Quantum Theory of Magnetic Susceptibilities. 11. Atomic and Molecular Interactions. 11.1 The H-H Nonexpanded Interactions up to Second Order. 11.2 The H-H Expanded Interactions up to Second Order. 11.3 Molecular Interactions. 11.4 Van der Waals and Hydrogen Bonds. 11.5 The Keesom Interaction. 12. Symmetry. 12.1 Molecular Symmetry. 12.2 Group Theoretical Methods. 12.3 Illustrative Examples. References. Author Index. Subject Index.

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Book SynopsisThe book offers an open learning/distance learning text covering analytical techniques used in forensic science. After an introduction, chapters describe specific techniques including background theory, instrumentation, and sampling techniques, along with examples of their forensic samples.Trade Review“I would recommend this work to chemistry students with an interest in the chemical analysis of forensic evidence.” (Chemistry & Industry, 1 July 2013)Table of ContentsSeries Preface xiii Preface xv About the Author xvii Acronyms, Abbreviations and Symbols xix 1 The Chemistry of Forensic Evidence 1 1.1 Introduction 1 1.2 Evidence Types 2 1.3 Introduction to Data Analysis 23 1.4 Summary 24 References 24 2 Preliminary Tests 27 2.1 Introduction 27 2.2 Chemical Tests 27 2.3 Density 32 2.4 Light Examination 35 2.5 Summary 39 References 39 3 Microscopic Techniques 41 3.1 Introduction 41 3.2 Optical Microscopy 42 3.3 Transmission Electron Microscopy 51 3.4 Scanning Electron Microscopy 54 3.5 Atomic Force Microscopy 59 3.6 X-Ray Diffraction 60 3.7 Summary 66 References 66 4 Molecular Spectroscopy 69 4.1 Introduction 70 4.2 Infrared Spectroscopy 70 4.3 Raman Spectroscopy 89 4.4 Ultraviolet–visible Spectroscopy 95 4.5 Fluorescence Spectroscopy 101 4.6 Nuclear Magnetic Resonance Spectroscopy 104 4.7 Summary 109 References 109 5 Elemental Analysis 113 5.1 Introduction 113 5.2 Atomic Spectrometry 114 5.3 Inductively Coupled Plasma–Mass Spectrometry 117 5.4 X-Ray Fluorescence Spectroscopy 119 5.5 Particle-Induced X-Ray Emission Spectroscopy 123 5.6 Neutron Activation Analysis 125 5.7 Summary 125 References 126 6 Mass Spectrometry 129 6.1 Introduction 129 6.2 Molecular Mass Spectrometry 129 6.3 Isotope Ratio Mass Spectrometry 134 6.4 Ion Mobility Spectrometry 137 6.5 Summary 140 References 140 7 Separation Techniques 143 7.1 Introduction 144 7.2 Paper Chromatography 144 7.3 Thin Layer Chromatography 145 7.4 Gas Chromatography 149 7.5 Liquid Chromatography 155 7.6 Ion Chromatography 159 7.7 Capillary Electrophoresis 161 7.8 Summary 163 References 164 8 Thermal Analysis 167 8.1 Introduction 167 8.2 Pyrolysis Techniques 168 8.3 Differential Scanning Calorimetry and Differential Thermal Analysis 171 8.4 Thermogravimetric Analysis 174 8.5 Summary 178 References 178 Bibliography 195 Glossary of Terms 197 SI Units and Physical Constants 203 Periodic Table 207 Index 209

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Book Synopsis

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Book SynopsisIn recent years natural fibers have become increasingly popular for use in industrial applications as reinforcement for plastics. This essential resource brings detailed information on natural fibers from agriculture to the final product.Trade Review“The book offers comprehensive information on natural fibres including many aspects of the value-added chain from plant cultivation to the final technical application . . . It is therefore suitable to serve as a basis for teaching or as a reference book also for undergraduate and graduate students in several fields of studies, e.g. material sciences, engineering, agricultural sciences and resource management.” (Journal of Cleaner Production, 1 May 2015)Table of Contents Series Preface xi Preface xiii Foreword xv List of Contributors xvii List of Illustrators xxiii Part I Background 1 Historic Usage and Preservation of Cultural Heritage 3 Fenella G. France 2 What Are Natural Fibres? 11 2.1 Chemistry of Plant Fibres 13 Danny E. Akin 2.2 Natural Fibres – Function in Nature 23 Michaela Eder and Ingo Burgert 2.3 Types of Fibre 41 Jörg Müssig and Tanja Slootmaker 3 Economic Aspects 49 3.1 Grades and Standards 51 Axel Drieling and Jörg Müssig 3.2 Technical Applications of Natural Fibres: An Overview 63 Nina Graupner and Jörg Müssig 3.3 Natural Fibres in Technical Applications: Market and Trends 73 Stephan Piotrowski and Michael Carus Copyrighted Material Part II Vegetable Fibres 4 Flax – Structure, Chemistry, Retting and Processing 89 Danny E. Akin 5 Hemp – Cultivation, Extraction and Processing 109 Stefano Amaducci and Hans-Jörg Gusovius 6 Jute – A Versatile Natural Fibre. Cultivation, Extraction and Processing 135 Md. Siddiqur Rahman 7 Abacá – Cultivation, Extraction and Processing 163 Friedhelm Göltenboth and Werner Mühlbauer 8 Sisal – Cultivation, Processing and Products 181 Rajesh D. Anandjiwala and Maya John 9 Coir – Coconut Cultivation, Extraction and Processing of Coir 197 Chitrangani Jayasekara and Nalinie Amarasinghe 10 Cotton Production and Processing 219 Muhammed Rafiq Chaudhry Part III Animal Fibres 11 Mulberry Silk, Spider Dragline and Recombinant Silks 237 Anja Glišović and Fritz Vollrath 12 Wool – Structure, Mechanical Properties and Technical Products based on Animal Fibres 255 Crisan Popescu and Franz-Josef Wortmann Part IV Testing and Quality Management 13 Testing Methods for Measuring Physical and Mechanical Fibre Properties (Plant and Animal Fibres) 269 Jörg Müssig, Holger Fischer, Nina Graupner and Axel Drieling 14 SEM Catalogue for Animal and Plant Fibres 311 Tanja Slootmaker and Jörg Müssig 15 Combined (In Situ) Methods 337 Ingo Burgert and Michaela Eder 16 DNA-Analytical Identification of Species and Genetic Modifications in Natural Fibres 345 Lothar Kruse 17 Cotton/Worldwide Harmonisation 353 Axel Drieling and Jean-Paul Gourlot 18 Flax – ASTM Standardisation and Harmonisation 371 Danny E. Akin Part V Applications: Current and Potential 19 Composites 383 19.1 Historical, Contemporary and Future Applications 385 Tuomas Hänninen and Mark Hughes 19.2 Design, Material Properties and Databases 397 Erwin Baur and Frank Otremba 19.3 Natural Fibre Composite Processing: A Technical Overview 407 Tim Huber, Nina Graupner and Jörg Müssig 19.4 Natural Fibre-Reinforced Polymers in Automotive Interior Applications 423 Eugen Prömper 19.5 Composites Based on Natural Resources 437 Martien van den Oever and Harriëtte Bos 19.6 Cellulose Nanocomposites 459 Sanchita Bandyopadhyay-Ghosh, Subrata Bandhu Ghosh and Mohini Sain 20 Insulation Materials Based on Natural Fibres 481 Franz Neubauer 21 Natural Fibres in Geotextiles for Soil Protection and Erosion Control 509 Gero Leson, Michael V. Harding, and Klaus Dippon Index 523

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Book SynopsisThis text gives a critical presentation of the most common thermodynamic models and highlights the practical advantages, giving recommendations for different applications. It includes worked examples of how the models can be extended to new systems, and provides review tables with the parameters of advanced association models.Table of ContentsPreface. About the Authors. Acknowledgments. List of Abbreviations. List of Symbols. PART A INTRODUCTION. 1 Thermodynamics for Process and Product Design. Appendix. References. 2 Intermolecular Forces and Thermodynamic Models. 2.1 General. 2.2 Coulombic and van der Waals forces. 2.3 Quasi-chemical forces with emphasis on hydrogen bonding. 2.4 Some applications of intermolecular forces in model development. 2.5 Concluding remarks. References. PART B THE CLASSICAL MODELS. 3 Cubic equations of state: the classical mixing rules. 3.1 General. 3.2 On the parameter estimation. 3.3 Analysis of the advantages and shortcomings of cubic EoS. 3.4 Some recent developments with cubic EoS. 3.5 Concluding remarks. Appendix. References. 4 Activity coefficient models Part 1: random-mixing based models 4.1 Introduction to the random-mixing models. 4.2 Experimental activity coefficients. 4.3 The Margules equation. 4.4 From the van der Waals and van Laar equation to the regular solution theory. 4.5 Applications of the Regular Solution Theory. 4.6 SLE with emphasis on wax formation. 4.7 Asphaltene precipitation. 4.8 Concluding remarks about the random-mixing-based models. Appendix. References. 5 Activity coefficient models Part 2: local composition models, from Wilson and NRTL to UNIQUAC and UNIFAC. 5.1 General. 5.2 Overview of the local composition models. 5.3 The theoretical limitations. 5.4 Range of applicability of the LC models. 5.5 On the theoretical significance of the interaction parameters. 5.6 LC models: some unifying concepts. 5.7 The group contribution principle and UNIFAC. 5.8 Local-composition-free–volume models for polymers. 5.9 Conclusions: is UNIQUAC the best local composition model available today? Appendix. References. 6 The EoS/ GE mixing rules for cubic equations of state. 6.1 General. 6.2 The infinite pressure limit (the Huron-Vidal mixing rule). 6.3 The zero-reference pressure limit (The Michelsen approach). 6.4 Successes and limitations of zero reference pressure models. 6.5 The Wong–Sandler (WS) mixing rule. 6.6 EoS/ GE approaches suitable for asymmetric mixtures. 6.7 Applications of the LCVM, MHV2, PSRK and WS mixing rules. 6.8 Cubic EoS for polymers. 6.9 Conclusions: achievements and limitations of the EoS/ GE models. 6.10 Recommended models – so far. Appendix. References. PART C ADVANCED MODELS AND THEIR APPLICATIONS. 7 Association theories and models: the role of spectroscopy. 7.1 Introduction. 7.2 Three different association theories. 7.3 The chemical and perturbation theories. 7.4 Spectroscopy and association theories. 7.5 Concluding remarks. Appendix. References. 8 The Statistical Associating Fluid Theory (SAFT). 8.1 The SAFT EoS: a brief look at the history and major developments. 8.2 The SAFT equations. 8.3 Parameterization of SAFT. 8.4 Applications of SAFT to non-polar molecules. 8.5 GC SAFT approaches. 8.6 Concluding remarks. Appendix. References. 9 The Cubic-Plus-Association equation of state. 9.1 Introduction. 9.2 The CPA EoS. 9.3 Parameter estimation: pure compounds. 9.4 The First applications. 9.5 Conclusions. Appendix. References. 10 Applications of CPA to the oil and gas industry. 10.1 General. 10.2 Glycol–water–hydrocarbon phase equilibria. 10.3 Gas hydrates. 10.4 Gas phase water content calculations. 10.5 Mixtures with acid gases (CO2 and H2S). 10.6 Reservoir fluids. 10.7 Conclusions. References. 11 Applications of CPA to chemical industries. 11.1 Introduction. 11.2 Aqueous mixtures with heavy alcohols. 11.3 Amines and ketones. 11.4 Mixtures with organic acids. 11.5 Mixtures with ethers and esters. 11.6 Multifunctional chemicals: glycolethers and alkanolamines. 11.7 Complex aqueous mixtures. 11.8 Concluding remarks. Appendix. References. 12 Extension of CPA and SAFT to new systems: worked examples and guidelines. 12.1 Introduction. 12.2 The case of sulfolane: CPA application. 12.3 Application of sPC–SAFT to sulfolane-related systems. 12.4 Applicability of association theories and cubic EoS with advanced mixing rules (EoS/GEmodels) to polar chemicals. 12.5 Phenols. 12.6 Conclusions. References. 13 Applications of SAFT to polar and associating mixtures. 13.1 Introduction. 13.2 Water-hydrocarbons. 13.3 Alcohols, amines and alkanolamines. 13.4 Glycols. 13.5 Organic Acids. 13.6 Polar non-associating compounds. 13.7 Flow assurance (asphaltenes and gas hydrate inhibitors). 13.8 Concluding Remarks. References. 14 Applications of SAFT to polymers. 14.1 Overview. 14.2 Estimation of parameters for polymers for SAFT-type EoS. 14.3 Low-pressure phase equilibria (VLE and LLE) using simplified PC–SAFT. 14.4 High-pressure phase equilibria. 14.5 Co-polymers. 14.6 Concluding remarks. Appendix. References. PART D THERMODYNAMICS AND OTHER DISCIPLINES. 15 Models for electrolyte systems. 15.1 Introduction: importance of electrolyte systems and modeling challenges. 15.2 Theories of ionic (long-range) interactions. 15.3 Electrolyte models: activity coefficients. 15.4 Electrolyte models: Equation of State. 15.5 Comparison of electrolyte EoS: capabilities and limitations. 15.6 Thermodynamic models for CO2–water–alkanolamines. 15.7 Concluding remarks. References. 16 Quantum chemistry in engineering thermodynamics. 16.1 Introduction. 16.2 The COSMO—RS method. 16.3 Estimation of association model parameters using QC. 16.4 Estimation of size parameters of SFT-type models from QC. 16.5 Conclusions. References. 17 Environmental thermodynamics. 17.1 Introduction. 17.2 Distribution of chemicals in environmental ecosystems. 17.3 Environmentally friendly solvents: supercritical fluids. 17.4 Conclusions. References. 18 Thermodynamics and colloid and surface chemistry. 18.1 General. 18.2 Intermolecular vs. interparticle forces. 18.3 Interparticle forces in colloids and interfaces. 18.4 Acid–base concepts in adhesion studies. 18.5 Surface and interfacial tensions from thermodynamic models. 18.6 Hydrophilicity. 18.7 Micellization and surfactant solutions. 18.8 Adsorption. 18.9 Conclusions. References. 19 Thermodynamics for biotechnology. 19.1 Introduction. 19.2 Models for Pharmaceuticals. 19.3 Models for amino acids and polypeptides. 19.4 Adsorption of proteins and chromatography. 19.5 Semi-productive models for protein systems. 19.6 Concluding Remarks. Appendix. References. 20 Epilogue: thermodynamic challenges in the twenty-first century. 20.1 In brief. 20.2 Petroleum and chemical industries. 20.3 Chemicals including polymers and complex product design. 20.4 Biotechnology including pharmaceuticals. 20.5 How future needs will be addressed. References. Index.

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Book Synopsis Entirely devoted to the failure analysis of coatings and paints an excellent reference to a select market. Latest edition contains new material on surface preparation, transfer of salt to steel from contaminated abrasive, effect of peak density on coating performance, on galvanizing, silane-modified coatings, polyurea coatings, polyaspartics, and powder coatings and on dry spray. Balances scientific background and practical advice, giving both the theory and applications in a slim, easily readable form. Includes case studies of laboratory tests. Written by an author with over 25 years of experience in the paint and coatings industry. Table of ContentsPreface to the Revised Edition. Preface to the First Edition. Acknowledgements. 1 General Principles of Coating Formulation. 1.1 Introduction. 1.2 Binders. 1.3 Pigments. 1.4 Solvents. 1.5 Additives. 1.6 Formulation Concepts: Pigment-to-Binder Ratio. 1.7 Formulation Concepts: Pigment-Volume Concentration. 1.8 Formulation Concepts: Density, Weight Solids and Volume Solids. References. 2 Why Coatings Work and Why They Fail. 2.1 Why Coatings Work. 2.1.1 Adhesion. 2.1.2 Wetting. 2.1.3 Surface Preparation. 2.1.4 Cohesive Strength. 2.1.5 Permeability. 2.2 Why Coatings Fail. 2.2.1 Mechanical Stress. 2.2.2 Internal Stress. 2.2.3 Chemical Attack. 2.2.4 Weathering Stress. 2.2.5 Osmotic Blistering. 2.2.6 Electroendosmotic Blistering. References. 3 Pigments. 3.1 Inorganic Pigments. 3.1.1 Inorganic Colour Pigments – White. 3.1.2 Inorganic Colour Pigments – Yellow. 3.1.3 Inorganic Colour Pigments – Orange. 3.1.4 Inorganic Colour Pigments – Red. 3.1.5 Inorganic Colour Pigments – Blue. 3.1.6 Inorganic Colour Pigments – Green. 3.2 Extender Pigments. 3.2.l Silica/Silicates. 3.2.2 Calcium Carbonate. 3.2.3 Barytes. 3.3 Corrosion-Resistant Pigments. 3.4 Organic Pigments. 3.4.1 Organic Red Pigments. 3.4.2 Organic Yellow Pigments. 3.4.3 Organic Blue Pigments. 3.4.4 Organic Green Pigments. References. 4 Additives and Solvents. 4.1 Additives. 4.1.1 Anti-settling Agents. 4.1.2 Viscosity Modifiers. 4.1.3 Surfactants and Emulsifying Agents. 4.1.4 De-foaming and Anti-foaming Agents. 4.1.5 Driers. 4.1.6 Plasticizers. 4.1.7 Ultraviolet Stabilizers. 4.1.8 Anti-skinning Agents. 4.1.9 Biocides. 4.1.10 Flow-Modifying Agents. 4.2 Solvents. References. 5 Coating Types and Common Failure Modes. 5.1 Natural Resins and Oils. 5.1.1 Natural Resins. 5.1.2 Oils. 5.2 Alkyds and Epoxy Esters. 5.2.1 Alkyds. 5.2.2 Epoxy Esters. 5.3 Epoxies. 5.3.1 Amine and Amide Curing Agents for Epoxy Resins. 5.3.2 Epoxy Failure Modes. 5.4 Modifi ed Epoxies. 5.4.1 Acrylic Epoxies. 5.4.2 Coal Tar Epoxies. 5.4.3 Epoxy Phenolics. 5.5 Phenolics. 5.5.1 Resole Phenolics. 5.5.2 Novolac Phenolics. 5.5.3 Phenolic Failure Modes. 5.6 Amino Resins. 5.7 Acrylics. 5.7.1 Solution Acrylics. 5.7.2 Acrylic Latex Coatings. 5.7.3 Thermoset Acrylics. 5.8 Polyesters. 5.8.1 Saturated Polyesters. 5.8.2 Unsaturated Polyesters. 5.9 Polyurethanes. 5.9.1 Two-Component Polyisocyanate/Polyol Coatings. 5.9.2 Urealkyds. 5.9.3 Moisture-Cured Polyurethanes. 5.9.4 Polyurethane Lacquers and Dispersions. 5.9.5 Two-Component Water-Borne Polyurethanes. 5.10 Vinyls. 5.10.1 Solution Vinyls. 5.10.2 Plastisols and Organosols. 5.10.3 Vinyl Fluorides. 5.10.4 Poly(vinyl butyral). 5.10.5 Vinyl Latexes. 5.11 Bituminous Coatings. 5.12 Inorganic and Silicone-Modifi ed Coatings. 5.12.1 Silicone Coatings. 5.12.2 Silicate Coatings. 5.12.3 Polysiloxane Coatings. 5.13 Polyureas. 5.13.1 Polyaspartic Polyurea Coatings. 5.14 Powder Coatings. References. 6 Application-Related Problems. 6.1 Brush and Roller. 6.2 Spray Applications. 6.2.1 Air (Conventional) Spray. 6.2.2 Airless Spray. 6.2.3 Plural Spray. 6.2.4 Electrostatic Spray. 6.3 Flow Coating. 6.4 Roll Coating. 6.5 Powder Coating. 6.6 Coating Failures Related to Application Problems. References. 7 Field Methods. 8 Analytical Methods. 8.1 Light Microscopy. 8.2 Infrared Spectroscopy. 8.2.1 Theory. 8.2.2 Instrumentation. 8.2.3 Sample Handling. 8.2.4 Applications. 8.3 Gas Chromatography (GC). 8.3.1 Theory of GC. 8.3.2 Instrumentation. 8.3.3 Pyrolysis-GC. 8.3.4 Application of GC. 8.4 Gel Permeation Chromatography (GPC). 8.4.1 Theory. 8.4.2 Instrumentation. 8.4.3 Applications. 8.5 Ion Chromatography. 8.5.1 Theory. 8.5.2 Applications. 8.6 Scanning Electron Microscopy. 8.6.1 Imaging Theory. 8.6.2 Elemental Analysis by X-ray Spectroscopy. 8.6.3 Sample Preparation. 8.6.4 Applications of SEM-EDS. 8.7 Differential Scanning Calorimetry (DSC). 8.7.1 Theory. 8.7.2 Calibration and Sample Preparation. 8.7.3 Applications of DSC. 8.8 Miscellaneous Methods of Analysis. References. 9 Physical Methods. 9.1 Adhesion. 9.2 Flexibility and Impact Resistance. 9.3 Solvent Resistance. 9.4 Weathering Resistance. 9.5 Chemical Resistance. 9.6 Freeze–Thaw. 9.7 Application Variables. References. 10 Examples of Coating Failures. 10.1 Urethane Topcoat Disbonding from Epoxy. 10.2 Blistering of an Epoxy Tank Coating. 10.3 Cracking and Delamination of Epoxy Coating Systems on Masonry Walls. 10.4 Discolouration of Coil-Coated Aluminium Siding. 10.5 Discolouration and Delamination of Plastisol. 10.6 Delamination of Floor Coating. 10.7 Delamination of Dry-Fall Alkyd. 10.8 Coal Tar Epoxy Failure. 10.9 Splitting of Inorganic Zinc-Rich Primer. 10.10 Defects on Electro-Coated Panels. 10.11 Failure of Coated Light Poles. 10.12 Blistering of Coating on Concrete Floor, Number 1. 10.13 Blistering of Coating on Concrete Floor, Number 2. 10.14 Peeling of Paint from Metal Chairs. 10.15 Failure of Railroad Car Liner. 10.16 Failure of Calcium Sulfonate Modifi ed Alkyd Topcoat from a Bridge. 10.17 Discolouration of Furniture Lacquer. 10.18 Failure of Tank Car Lining. References. 11 The Repair of Coating Failures. Index.

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Book SynopsisThermal Convection - Patterns, Stages of Evolution and Stability Behavior provides the reader with an ensemble picture of the subject, illustrating the state-of-the-art and providing the researchers from universities and industry with a basis on which they are able to estimate the possible impact of a variety of parameters. Unlike earlier books on the subject, the heavy mathematical background underlying and governing the behaviors illustrated in the text are kept to a minimum. The text clarifies some still unresolved controversies pertaining to the physical nature of the dominating driving force responsible for asymmetric/oscillatory convection in various natural phenomena and/or technologically important processes and can help researchers in elaborating and validating new, more complex models, in accelerating the current trend towards predictable and reproducible natural phenomena and in establishing an adequate scientific foundation to industrial processes. TherTrade Review“In our opinion, this book will be useful for experts in fluid mechanics, nonlinear dynamics, and applied mathematics, as well as physicists and engineers. The book can be used also by graduate students.” (Mathematical Reviews, 2012) "Undoubtedly, the book can be considered as a mandatory reading for everybody whose research involves thermal convection effects. . . For experts it offers a good overview of the current status of "hot" problems in thermal convection. The book can be strongly recommended for MSc and PhD students whose research includes thermal convection problems, as well as to engineers whose projects involve nonisothermal buoyancy- and thermocapillary-driven flows." (Cryst. Res. Technol, 2011) "Despite the word "convection" appearing in the title, this excellent monograph is not a book on heat transfer . . . Otherwise, this is an excellent text which I recommend for those seriously interested in thermally driven convection." (Computational Thermal Sciences, 2011) "It represents the most comprehensive single volume monograph on convection phenomena available at the present time. I am glad to have the book on my shelf and I will recommend it to anyone with interest in convection as an inspiring guide through its myriad manifestations." (Radostin D. Simitev, October 2010)"This excellent monograph will be warmly welcomed by university teachers and researchers working in the field of thermal convection, and it will be useful for graduate students looking for a short way from basic notions to the current state of the art in that field." (European Journal of Mechanics B/Fluids, September 2010) "It is a treasure-trove of phenomenological details ordered in a systematic way. It represents the most comprehensive single-volume monograph on convection phenomena available at the present time. I am glad to have the book on my shelf and I will recommend it to anyone with interest in convection as an inspiring guide through its myriad manifestations." (Journal of Geophysical and Astrophysical Fluid Dynamics, February 2011)Table of ContentsPreface. Acknowledgements. 1 Equations, General Concepts and Methods of Analysis. 1.1 Pattern Formation and Nonlinear Dynamics. 1.2 The Navier–Stokes Equations. 1.3 Energy Equality and Dissipative Structures. 1.4 Flow Stability, Bifurcations and Transition to Chaos. 1.5 Linear Stability Analysis: Principles and Methods. 1.6 Energy Stability Theory. 1.7 Numerical Integration of the Navier–Stokes Equations. 1.8 Some Universal Properties of Chaotic States. 1.9 The Maxwell Equations. 2 Classical Models, Characteristic Numbers and Scaling Arguments. 2.1 Buoyancy Convection and the Boussinesq Model. 2.2 Convection in Space. 2.3 Marangoni Flow. 2.4 Exact Solutions of the Navier–Stokes Equations for Thermal Problems. 2.5 Conductive, Transition and Boundary-layer Regimes. 3 Examples of Thermal Fluid Convection and Pattern Formation in Nature and Technology. 3.1 Technological Processes: Small-scale Laboratory and Industrial Setups. 3.2 Examples of Thermal Fluid Convection and Pattern Formation at the Mesoscale. 3.3 Planetary Structure and Dynamics: Convective Phenomena. 3.4 Atmospheric and Oceanic Phenomena. 4 Thermogravitational Convection: The Rayleigh–Bénard Problem. 4.1 Nonconfined Fluid Layers and Ideal Straight Rolls. 4.2 The Busse Balloon. 4.3 Some Considerations About the Role of Dislocation Dynamics. 4.4 Tertiary and Quaternary Modes of Convection. 4.5 Spoke Pattern Convection. 4.6 Spiral Defect Chaos, Hexagons and Squares. 4.7 Convection with Lateral Walls. 4.8 Two-dimensional Models. 4.9 Three-dimensional Parallelepipedic Enclosures: Classification of Solutions and Possible Symmetries. 4.10 The Circular Cylindrical Problem. 4.11 Spirals: Genesis, Properties and Dynamics. 4.12 From Spirals to SDC: The Extensive Chaos Problem. 4.13 Three-dimensional Convection in a Spherical Shell. 5 The Dynamics of Thermal Plumes and Related Regimes of Motion. 5.1 Introduction. 5.2 Free Plume Regimes. 5.3 The Flywheel Mechanism: The ‘Wind’ of Turbulence. 5.4 Multiplume Configurations Originated from Discrete Sources of Buoyancy. 6 Systems Heated from the Side: The Hadley Flow. 6.1 The Infinite Horizontal Layer. 6.2 Two-dimensional Horizontal Enclosures. 6.3 The Infinite Vertical Layer: Cats-eye Patterns and Temperature Waves. 6.4 Three-dimensional Parallelepipedic Enclosures. 6.5 Cylindrical Geometries under Various Heating Conditions. 7 Thermogravitational Convection in Inclined Systems. 7.1 Inclined Layer Convection. 7.2 Inclined Side-heated Slots. 8 Thermovibrational Convection. 8.1 Equations and Relevant Parameters. 8.2 Fields Decomposition. 8.3 The TFD Distortions. 8.4 High Frequencies and the Thermovibrational Theory. 8.5 States of Quasi-equilibrium and Related Stability. 8.6 Primary and Secondary Patterns of Symmetry. 8.7 Medium and Low Frequencies: Possible Regimes and Flow Patterns. 9 Marangoni–Bénard Convection. 9.1 Introduction. 9.2 High Prandtl Number Liquids: Patterns with Hexagons, Squares and Triangles. 9.3 Liquid Metals: Inverted Hexagons and High-order Solutions. 9.4 Effects of Lateral Confinement. 9.5 Temperature Gradient Inclination. 10 Thermocapillary Convection. 10.1 Basic Features of Steady Marangoni Convection. 10.2 Stationary Multicellular Flow and Hydrothermal Waves. 10.3 Annular Configurations. 10.4 The Liquid Bridge. 11 Mixed Buoyancy–Marangoni Convection. 11.1 The Canonical Problem: The Infinite Horizontal Layer. 11.2 Finite-sized Systems Filled with Liquid Metals. 11.3 Typical Terrestrial Laboratory Experiments with Transparent Liquids. 11.4 The Rectangular Liquid Layer. 11.5 Effects Originating from the Walls. 11.6 The Open Vertical Cavity. 11.7 The Annular Pool. 11.8 The Liquid Bridge on the Ground. 12 Hybrid Regimes with Vibrations. 12.1 RB Convection with Vertical Shaking. 12.2 Complex Order, Quasi-periodic Crystals and Superlattices. 12.3 RB Convection with Horizontal or Oblique Shaking. 12.4 Laterally Heated Systems and Parametric Resonances. 12.5 Control of Thermogravitational Convection. 12.6 Mixed Marangoni–Thermovibrational Convection. 12.7 Modulation of Marangoni–Bénard Convection. 13 Flow Control by Magnetic Fields. 13.1 Static and Uniform Magnetic Fields. 13.2 Historical Developments and Current Status. 13.3 Rotating Magnetic Fields. 13.4 Gradients of Magnetic Fields and Virtual Microgravity. References. Index.

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Book SynopsisWritten in four parts, this book provides a dedicated and in-depth reference for blending within the pharmaceutical manufacturing industry. It links the science of blending with regulatory requirements associated with pharmaceutical manufacture.Table of ContentsContributor List xv Preface xvii Part I Fundamentals of Mixing 1 1 Mixing Theory 3Chris D. Rielly 1.1 Introduction 3 1.2 Describing Mixtures 5 1.3 Scale of Scrutiny 6 1.4 Quantifying Mixedness for Coarse and Fine‐Grained Mixtures 8 1.4.1 Coarse and Fine‐Grained Mixtures 8 1.4.2 Scale and Intensity of Segregation 9 1.5 Determining the End‐Point of Mixing: Comparison of Mixing Indices 15 1.6 Continuous Flow Mixers 19 1.6.1 Idealized Mixing Patterns 19 1.6.2 Residence Time Distributions 21 1.6.3 Back‐Mixing and Filtering of Disturbances Using a CSTR 23 References 24 2 Turbulent Mixing Fundamentals 27Suzanne M. Kresta 2.1 Introduction 27 2.2 The Velocity Field and Turbulence 28 2.3 Circulation and Macro‐Mixing 29 2.4 Fully Turbulent Limits and the Scaling of Turbulence 32 2.5 The Spectrum of Turbulent Length Scales, Injection of a Scalar (Either Reagent or Additive) and the Macro‐, Meso‐ and Micro‐Scales of Mixing 34 2.6 Turbulence and Mixing of Solids, Liquids, and Gases 37 2.7 Specifying Mixing Requirements for a Process 38 2.8 Conclusions 39 Notation 39 Roman Characters 39 Greek Characters 40 References 40 3 Laminar Mixing Fundamentals 43P.J. Cullen and N.N. Misra 3.1 Laminar Flows 43 3.2 Mixing in Laminar Flows 44 3.2.1 Chaos and Laminar Chaotic Mixing 45 3.2.2 Granular Chaotic Mixing 50 3.3 Recent Advances 53 References 54 4 Sampling and Determination of Adequacy of Mixing 57Rodolfo J. Romañach 4.1 Introduction, Process Understanding, and Regulations 57 4.2 Theory of Sampling 59 4.3 Sampling of Pharmaceutical Powder Blends 63 4.4 Stratified Sampling Approach 65 4.5 Testing 67 4.6 Process Knowledge/Process Analytical Technology 68 4.7 Real Time Spectroscopic Monitoring of Powder Blending 70 4.8 Looking Forward, Recommendations 73 4.9 Conclusion 74 4.10 Acknowledgments 75 References 75 Part II Applications 79 5 Particles and Blending 81Reuben D. Domike and Charles L. Cooney 5.1 Introduction 81 5.2 Particle Geometry 82 5.2.1 Particle Size and Size Distribution 82 5.2.2 Particle Shape and Shape Distribution 83 5.3 Particle Interactions 84 5.3.1 van der Waals Forces 84 5.3.2 Electrostatic Forces 85 5.3.3 Adsorbed Liquid Layers and Liquid Bridges 85 5.3.4 Solid Bridges 86 5.3.5 Use of AFM to Measure Interparticle Forces 87 5.3.6 Interparticle Friction 89 5.4 Empirical Investigations of Particles and Blending 90 5.4.1 Blending of Powders 90 5.4.2 Impact of Particle Geometry on Blending 92 5.4.3 Impact of Interparticle Forces on Blending 93 5.4.4 Impact of Blender Conditions on Blending 95 5.5 Simulation Techniques 95 5.5.1 Full Physics Models Using Discrete Element Modeling 96 5.5.2 Continuum Models 97 5.5.3 Cellular Automata 98 References 98 6 Continuous Powder Mixing 101Juan G. Osorio, Aditya U. Vanarase, Rodolfo J. Romañach, and Fernando J. Muzzio 6.1 Introduction 101 6.2 Overview 102 6.3 Theoretical Characterization 107 6.3.1 Residence Time Distribution (RTD) Modeling 107 6.3.2 Variance Reduction Ratio 108 6.4 Experimental Characterization 108 6.4.1 Hold‐Up 109 6.4.2 Residence Time Distribution (RTD) Measurements 109 6.4.3 Mean Strain 110 6.5 Continuous Mixing Efficiency 110 6.5.1 Variance Reduction Ratio 110 6.5.2 Blend Homogeneity 111 6.6 Effects of Process Parameters on Mixing Behavior and Performance 112 6.6.1 Hold‐Up 113 6.6.2 RTD Measurements 113 6.7 Mixing Performance 118 6.7.1 Modeling 120 6.7.2 PAT, QbD, and Control 122 6.8 Conclusions and Continuing Efforts 124 References 125 7 Dispersion of Fine Powders in Liquids: Particle Incorporation and Size Reduction 129Gül N. Özcan-Taşkın 7.1 Particle Incorporation into Liquids 129 7.1.1 Wetting 130 7.1.2 Stirred Tanks for Particle Incorporation 132 7.1.3 In‐Line Devices Used for Particle Incorporation 140 7.2 Break Up of Fine Powder Clusters in Liquids 143 7.2.1 Mechanisms of Break Up 146 7.2.2 Process Devices for Deagglomeration\Size Reduction of Agglomerates 147 References 150 8 Wet Granulation and Mixing 153Karen P. Hapgood and Rachel M. Smith 8.1 Introduction 153 8.2 Nucleation 154 8.2.1 Drop Penetration Time 156 8.2.2 Dimensionless Spray Flux 158 8.2.3 Nucleation Regime Map 160 8.3 Consolidation and Growth 162 8.3.1 Granule Consolidation 162 8.3.2 Granule Growth Behaviour 164 8.3.3 Granule Growth Regime Map 165 8.4 Breakage 167 8.4.1 Single Granule Strength and Deformation 167 8.4.2 In‐Granulator Breakage Studies 170 8.4.3 Aiding Controlled Granulation via Breakage 172 8.5 Endpoint Control 174 8.5.1 Granulation Time 175 8.5.2 Impeller Power Consumption 176 8.5.3 Online Measurement of Granule Size 176 8.5.4 NIR and Other Spectral Methods 177 References 178 9 Emulsions 183Andrzej W. Pacek 9.1 Introduction 183 9.2 Properties of Emulsions 185 9.2.1 Morphology 185 9.2.2 Volumetric Composition 185 9.2.3 Drop Size Distributions and Average Drop Sizes 186 9.2.4 Rheology 191 9.3 Emulsion Stability and Surface Forces 195 9.3.1 Surface Forces 195 9.3.2 Emulsion Stability 199 9.4 Principles of Emulsion Formation 203 9.4.1 Low Energy Emulsification 204 9.4.2 High Energy Emulsification 205 9.5 Emulsification Equipment 216 9.5.1 Stirred Vessels 216 9.5.2 Static Mixers 218 9.5.3 High Shear Mixers 219 9.5.4 High‐Pressure Homogenizers 223 9.5.5 Ultrasonic Homogenizers 225 9.6 Concluding Remarks 226 Nomenclature 226 Greek symbols 228 References 228 10 Mixing of Pharmaceutical Solid‐Liquid Suspensions 233Mostafa Barigou and Frans L. Muller 10.1 Introduction 233 10.1.1 Linking Solid‐Liquid Processing to Critical Quality Attributes 233 10.1.2 Material Properties and Composition 234 10.1.3 Impact of Blending and Homogenization 234 10.1.4 Impact of Turbulence 237 10.1.5 Impact of Heat Transfer 237 10.2 Scale‐Up of Operations Involving Solid Suspensions 237 10.2.1 The Nature of Suspensions 237 10.2.2 Scale‐Up and Scale‐Down Rules 239 10.2.3 Identification of Agitator Duties 240 10.2.4 Solid‐Liquid Unit Operations 242 10.3 General Principles of Solid‐Liquid Suspensions 243 10.3.1 Rheological Behaviour of the Continuous Phase 243 10.3.2 Rheology of Suspensions 246 10.3.3 Terminal Velocity of Particles 249 10.3.4 Turbulence 254 10.4 Solids Charging 257 10.4.1 Charging to Batch Vessels 257 10.4.2 Charging Difficult Powders 261 10.5 Solid Suspension 261 10.5.1 States of Solid Suspension 261 10.5.2 Prediction of Minimum Speed for Complete Suspension 262 10.6 Solid Distribution 269 10.6.1 Agitator Speed 269 10.6.2 Homogeneity 270 10.6.3 Geometry 271 10.6.4 Practical Guidelines 272 10.7 Blending in Solid‐Liquid Systems 272 10.7.1 Mixing Time 272 10.7.2 Viscoplastic Slurries Yield Stress and Cavern Formation 272 10.8 Mass Transfer 275 10.9 Size Reduction, Deagglomeration and Attrition 277 10.9.1 Breaking Particles through Turbulent Forces 277 10.9.2 Breaking Particles through Impact 278 Nomenclature 281 Greek symbols 281 Abbreviations 282 References 282 Part III Equipment 287 11 Powder Blending Equipment 289David S. Dickey 11.1 Introduction 289 11.2 Blending Mechanisms 290 11.3 Blend Time 290 11.4 Fill Level 291 11.5 Segregation 291 11.6 Powder Processing Difficulties 292 11.7 Blender Classification 292 11.7.1 Tumble Blenders 293 11.7.2 Rotating Element Blenders 298 11.7.3 Granulators 303 11.7.4 Other Blenders – Mullers and Custom Blenders 304 11.8 Continuous Blenders 305 11.9 Blender Selection 306 11.10 Equipment Specifications 307 11.10.1 Materials of Construction 309 11.10.2 Electrical Classification 309 11.10.3 Drives and Seals 309 References 310 12 Fluid Mixing Equipment Design 311David S. Dickey 12.1 Introduction 311 12.2 Equipment Description 312 12.2.1 Laboratory Mixers 312 12.2.2 Development Mixers 313 12.2.3 Portable Mixers 313 12.2.4 Top-Entering Mixers 315 12.2.5 High-Shear Dispersers 318 12.2.6 High Viscosity Mixers 319 12.2.7 Multi-Shaft Mixers 319 12.2.8 Bottom-Entering Mixers 320 12.2.9 Glass-Lined Mixers and Vessels 321 12.2.10 Side-Entering Mixers 322 12.2.11 Vessel Geometry 322 12.2.12 Baffles 323 12.3 Measurements 323 12.3.1 Power 324 12.3.2 Torque 326 12.3.3 Tip Speed 327 12.3.4 Blend Time 327 12.4 Mixing Classifications 328 12.4.1 Liquid Mixing 328 12.4.2 Solids Suspension 330 12.4.3 Gas Dispersion 332 12.4.4 Viscous Mixing 333 12.5 Mechanical Design 334 12.5.1 Shaft Design 334 12.5.2 Shaft Seals 335 12.5.3 Materials of Construction 336 12.5.4 Surface Finish 337 12.5.5 Motors 338 12.5.6 Drives 339 12.6 Static Mixers 339 12.6.1 Twisted Element 339 12.6.2 Structured Element 339 12.6.3 Basic Design 340 12.7 Challenges and Troubleshooting 341 12.7.1 Careful Observations 341 12.7.2 Process Problems 341 Nomenclature 342 Greek 343 References 343 13 Scale‐Up 345David S. Dickey 13.1 Introduction 345 13.2 Similarity and Scale‐Up Concepts 346 13.2.1 Dimensional Analysis 346 13.2.2 Similarity 347 13.2.3 Applied Scale‐Up 349 13.3 Testing Methods 350 13.4 Observation and Measurement 352 13.5 Scale‐Up Methods 354 13.5.1 Scale‐Up with Geometric Similarity 354 13.5.2 Example of Geometric Similarity Scale‐Up 358 13.5.3 Scale‐Up Without Geometric Similarity 359 13.5.4 Example of Non‐Geometric Scale‐Up 361 13.5.5 Scale‐Up for Powder Mixing 364 13.6 Summary 367 Nomenclature 367 Greek 368 References 368 14 Equipment Qualification, Process and Cleaning Validation 369Ian Jones and Chris Smalley 14.1 Introduction 369 14.2 Blending Equipment Commissioning and Qualification 370 14.2.1 Outline of the Verification Approach 370 14.2.2 Requirements Phase 371 14.2.3 Specifications and Design Review Phase 373 14.2.4 Verification Phase 375 14.3 Blending and Mixing Validation 380 14.3.1 Why do You Need to Validate Pharmaceutical Blends/Mixes? 382 14.3.2 When do You Need to Validate Blending/Mixing? 384 14.3.3 Components of Blending/Mixing Validation 385 14.3.4 What to Validate 386 14.4 Blending Cleaning Validation 389 14.4.1 Cleaning Development Studies 389 14.4.2 Cleaning Validation 395 14.5 Conclusion 398 14.6 Acknowledgements 399 References 399 Part IV Optimization and Control 401 15 Process Analytical Technology for Blending 403Nicolas Abatzoglou 15.1 Introduction 403 15.1.1 The Role of PAT in Pharmaceutical Manufacturing: Is PAT Really New? 404 15.1.2 Why PAT is Feasible 405 15.1.3 Where PAT can be Applied in Pharmaceutical Manufacturing 406 15.1.4 The Regulatory Framework 406 15.2 Chemometrics and Data Management 408 15.2.1 PAT Data Management and Interpretation 409 15.3 Near‐Infrared Spectroscopy (NIRS) 412 15.4 Raman Spectroscopy (RS) 419 15.5 Image Analysis 422 15.6 LIF Spectroscopy 424 15.7 Effusivity 426 15.8 Other Potential Sensor Technologies 426 15.9 Comments on PAT in Liquid Formulation Mixing 427 References 427 16 Imaging Fluid Mixing 431Mi Wang 16.1 Introduction 431 16.2 Point Measurement Techniques 433 16.3 Photographic Imaging 435 16.4 Digital Particle Image Velocimetry 439 16.5 Magnetic Resonance Imaging 443 16.6 Positron Emission Particle Tracking Imaging 444 16.7 Electrical Process Tomography 446 References 452 17 Discrete Element Method (DEM) Simulation of Powder Mixing Process 459Ali Hassanpour and Mojtaba Ghadiri 17.1 Introduction to DEM and its Application in Pharmaceutical Powder Processing 459 17.2 DEM Simulation of Powder Mixing 461 17.3 Validation and Comparison with the Experiments 468 17.4 Concluding Remarks 474 References 475 Index 479

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Book SynopsisThis is a modern introductory book on sensors, combining underlying theory with bang up to date topics such as nanotechnology. The text is suitable for graduate students and research scientists with little background in analytical chemistry. It is user-friendly, with an accessible theoretical approach of the basic principles, and referencesfor further reading. Thebook covers up-to-date advances in the sensor field, e.g. nanotechnology and quantum dots. It includes calculation exercises and solutions, andthe accompanying website contains Powerpoint slides.Trade Review“Summary In conclusion it can be stated that this book is very suitable for students and a sound didactic means of learning the basics of chemo and biosensors . . . The organization of the content and the quantity of material presented are highly suitable for undergraduate and graduate students and for newcomers to this field; it can, therefore, be recommended for those wishing to gain both a first insight into, and a comprehensive overview of, this still growing topic.” (Analytical and Bioanalytical Chemistry, 1 March 2013)Table of Contents1 What are Chemical Sensors? 1 2 Protein Structure and Properties 21 3 Enzymes and Enzymatic Sensors 28 4 Mathematical Modeling of Enzymatic Sensors 50 5 Materials and Methods in Chemical-Sensor Manufacturing 66 6 Affinity-Based Recognition 101 7 Nucleic Acids in Chemical Sensors 118 8 Nanomaterial Applications in Chemical Sensors 135 9 Thermochemical Sensors 157 10 Potentiometric Sensors 165 11 Chemical Sensors Based on Semiconductor Electronic Devices 217 12 Resistive Gas Sensors (Chemiresistors) 246 13 Dynamic Electrochemistry Transduction Methods 258 14 Amperometric Enzyme Sensors 314 15 Mathematical Modeling of Mediated Amperometric Enzyme Sensors 332 16 Electrochemical Affinity and Nucleic Acid Sensors 347 17 Electrical-Impedance-Based Sensors 367 18 Optical Sensors – Fundamentals 404 19 Optical Sensors – Applications 435 20 Nanomaterial Applications in Optical Transduction 454 21 Acoustic-Wave Sensors 473 22 Microcantilever Sensors 507 23 Chemical Sensors Based on Microorganisms, Living Cells and Tissues 518

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Book SynopsisThis book addresses the scientific principles underlying electrochemistry. Starting with basic concepts of electricity, early chapters discuss the physics and chemistry of electrochemical cell materials and the properties that make them appropriate as cell components.Trade Review“Students will find it a good starting point to discover electrochemistry, which was pointed out as the primary objective by the authors. Job well done!.” (Chromatographia, 1 August 2013)Table of ContentsPreface xi 1 Electricity 1 Electric Charge 1 Charges at Rest 3 Capacitance and Conductance 8 Mobilities 18 Electrical Circuits 21 Alternating Electricity 23 Summary 28 2 Chemistry 29 Chemical Reactions 29 Gibbs Energy 30 Activity 33 Ionic Solutions 38 Ionic Activity Coefficients 41 Chemical Kinetics 46 Summary 52 3 Electrochemical Cells 55 Equilibrium Cells 55 Cells not at Equilibrium 60 Cells with Junctions 64 Summary 69 4 Electrosynthesis 71 Metal Production 71 The Chloralkali Industry 74 Organic Electrosynthesis 75 Electrolysis of Water 77 Selective Membranes 79 Summary 83 5 Electrochemical Power 85 Types of Electrochemical Power Source 85 Battery Characteristics 86 Primary Batteries 88 Secondary Batteries 94 Fuel Cells 100 Summary 104 6 Electrodes 105 Electrode Potentials 105 Standard Electrode Potentials 109 The Nernst Equation 111 Electrochemical Series 113 Working Electrodes 117 Summary 123 7 Electrode Reactions 125 Faraday’s Law 125 Kinetics of a Simple Electron Transfer 130 Multi-step Electrode Reactions 137 Summary 144 8 Transport 145 Flux Density 145 Three Transport Modes 148 Migration 149 Diffusion 154 Diffusion and Migration 158 Convection 161 Fluxes at Electrodes and in the Bulk 165 Summary 170 9 Green Electrochemistry 171 Sensors for Pollution Control 171 Stripping Analysis 177 Electrochemical Purification of Water 182 Electrochemistry of Biological Cells 186 Summary 192 10 Electrode Polarization 193 Three Causes of Electrode Polarization 193 Ohmic Polarization 197 Kinetic Polarization 200 Transport Polarization 202 Multiple Polarizations 205 Polarizations in Two- and Three-Electrode Cells 208 Summary 212 11 Corrosion 213 Vulnerable Metals 213 Corrosion Cells 215 Electrochemical Studies 217 Concentrated Corrosion 222 Fighting Corrosion 224 Extreme Corrosion 228 Summary 229 12 Steady-State Voltammetry 231 Features of Voltammetry 232 Microelectrodes and Macroelectrodes 234 Steady-State Potential-Step Voltammetry 237 The Disk Microelectrode 245 Rotating Disk Voltammetry 248 Shapes of Reversible Voltammograms 252 Summary 258 13 The Electrode Interface 259 Double Layers 259 Adsorption 266 The Interface in Voltammetry 271 Nucleation and Growth 281 Summary 285 14 Other Interfaces 287 Semiconductor Electrodes 287 Phenomena at Liquid*Liquid Interfaces 291 Electrokinetic Phenomena 298 Summary 302 15 Electrochemistry With Periodic Signals 303 Nonfaradaic Effects of A.C. 304 Faradaic Effects of A.C. 305 Equivalent Circuits 313 A.C. Voltammetry 318 Fourier-Transform Voltammetry 322 Summary 328 16 Transient Voltammetry 329 Modeling Transient Voltammetry 329 Potential-Step Voltammetry 334 Pulse Voltammetries 339 Ramped Potentials 346 Multiple Electron Transfers 355 Chemistry Combined with Electrochemistry 357 Controlling Current Instead of Potential 362 Summary 364 Appendix 365 Glossary 365 Absolute and Relative Permittivities 382 Properties of Liquid Water 383 Contents ix Conductivities and Resistivities 384 Elements with Major Importance in Electrochemistry 386 Transport Properties 388 Standard Gibbs Energies 390 Standard Electrode Potentials 392 Index 393

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Book SynopsisOver the past two decades, there has been a shift in research and industrial practice, and products traditionally manufactured primarily from wood are increasingly combined with other nonwood materials of either natural or synthetic origin.Table of ContentsSeries Preface xi Preface xiii Acknowledgments xv 1 Wood and Natural Fiber Composites: An Overview 1 1.1 Introduction 1 1.2 What Is Wood? 1 1.3 Natural Fibers 2 1.4 Composite Concept 6 1.5 Cellular Solids 13 1.6 Objectives and Organization of This Book 15 References 16 2 Lignocellulosic Materials 19 2.1 Introduction 19 2.2 Chemical Composition of Lignocellulosic Materials 19 2.3 The Woody Cell Wall as a Multicomponent Polymer System 35 2.4 Anatomical Structure of Representative Plants 40 2.5 Comparison of Representative Plant Stems 57 2.6 Cellular Solids Revisited 57 References 57 3 Wood as a Lignocellulose Exemplar 61 3.1 Introduction 61 3.2 Wood as a Representative Lignocellulosic Material: Important Physical Attributes 61 3.3 Moisture Interactions 61 3.4 Density and Specific Gravity of Wood 74 3.5 Wood: A Cellular Solid 79 3.6 Mechanical Properties 80 3.7 Wood Is the Exemplar: Extending Principles to Other Plant Materials 83 References 83 4 Consolidation Behavior of Lignocellulosic Materials 85 4.1 Introduction 85 4.2 Synthetic Crystalline and Amorphous Polymers 85 4.3 Glass Transition Temperature of Wood Polymers 89 4.4 Viscoelastic Behavior of Lignocellulosic Materials 97 4.5 Heat and Mass Transfer 104 4.6 Consolidation Behavior: Viscoelasticity Manifested During Hot Pressing 112 4.7 Press Cycles 119 4.8 Horizontal Density Distribution 123 References 125 5 Fundamentals of Adhesion 129 5.1 Introduction 129 5.2 Overview of Adhesion as a Science 129 5.3 Adhesion Theories 136 5.4 Surface Interactions 143 5.5 Work of Adhesion: Dupr´e Equation 152 5.6 Lignocellulosic Adherends 153 References 166 6 Adhesives Used to Bond Wood and Lignocellulosic Composites 169 6.1 Introduction 169 6.2 The Nature of Wood Adhesives 169 6.3 Adhesives Used to Bond Wood and Other Natural Fibers 175 6.4 Amino Resins 178 6.5 Phenolic Resins 184 6.6 Resorcinol Resins 188 6.7 Polymeric Isocyanate Adhesives 190 6.8 Epoxy Adhesives 193 6.9 Polyvinyl Acetate Adhesives 196 6.10 Hot Melts and Mastics 197 6.11 Adhesives from Renewable Natural Resources 199 References 206 7 Technology of Major Wood- and Fiber-Based Composites: An Overview 209 7.1 Introduction 209 7.2 Wood and Natural Fiber Composites as a Material Class 210 7.3 Taxonomy of Adhesive-Bonded Composites Technology 210 7.4 A Generic Process Flow 212 7.5 Technology of Adhesive-Bonded Materials Based on Form of Raw Material Input 213 7.6 Laboratory Panel Calculations 219 7.7 Measurement Conventions for Production Capacity and Output 222 7.8 Technology of Inorganic-Bonded Materials 225 References 234 8 Natural Fiber and Plastic Composites 237 8.1 Introduction 237 8.2 Natural Fibers and Their Temperature-Related Performance 242 8.3 Plastic Composite Processing Technology 247 8.4 Overcoming Incompatibility of Synthetic Polymers and Natural Fibers 252 8.5 Melt Compounding Natural Fibers and Thermoplastics 257 8.6 Performance of Natural Fiber and Plastic Composites 263 References 280 Index

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Book SynopsisOne approach to organic synthesis is retrosynthetic analysis. With this approach a chemist will start with the structure of their target molecule and progressively cut bonds to create simpler molecules. Reversing this process gives a synthetic route to the target molecule from simpler starting materials. This disconnection approach to synthesis is now a fundamental part of every organic synthesis course. Organic Synthesis: The Disconnection Approach, 2nd Edition introduces this important technique, to help students to design their own organic syntheses. There are forty chapters: those on the synthesis of given types of molecules alternate with strategy chapters in which the methods just learnt are placed in a wider context. The synthesis chapters cover many ways of making each type of molecule starting with simple aromatic and aliphatic compounds with one functional group and progressing to molecules with many functional groups. The strategy chapters cover Trade Review?The authors have succeeded admirably in the updating of a classic in the pedagogy of organic chemistry.? ( Journal of Medicinal Chemistry , August 2009) ?This book is suitable for advanced undergraduate students, researchers and professional chemists. Both the writing and the diagrams are simple and clear.? ( Reviews, May 2009)Table of ContentsPreface ix General References xi 1. The Disconnection Approach 1 2. Basic Principles: Synthons and Reagents Synthesis of Aromatic Compounds 7 3. Strategy I: The Order of Events 17 4. One-Group C–X Disconnections 23 5. Strategy II: Chemoselectivity 29 6. Two-Group C–X Disconnections 35 7. Strategy III: Reversal of Polarity, Cyclisations, Summary of Strategy 45 8. Amine Synthesis 53 9. Strategy IV: Protecting Groups 61 10. One Group C–C Disconnections I: Alcohols 69 11. General Strategy A: Choosing a Disconnection 77 12. Strategy V: Stereoselectivity A 83 13. One Group C–C Disconnections II: Carbonyl Compounds 93 14. Strategy VI: Regioselectivity 101 15. Alkene Synthesis 107 16. Strategy VII: Use of Acetylenes (Alkynes) 115 17. Two-Group C–C Disconnections I: Diels-Alder Reactions 121 18. Strategy VIII: Introduction to Carbonyl Condensations 129 19. Two-Group C–C Disconnections II: 1,3-Difunctionalised Compounds 133 20. Strategy IX: Control in Carbonyl Condensations 139 21. Two-Group C–C Disconnections III: 1,5-Difunctionalised Compounds Conjugate (Michael) Addition and Robinson Annelation 151 22. Strategy X: Aliphatic Nitro Compounds in Synthesis 161 23. Two-Group Disconnections IV: 1,2-Difunctionalised Compounds 167 24. Strategy XI: Radical Reactions in Synthesis 177 25. Two-Group Disconnections V: 1,4-Difunctionalised Compounds 185 26. Strategy XII: Reconnection 193 27. Two-Group C–C Disconnections VI: 1,6-diCarbonyl Compounds 199 28. General Strategy B: Strategy of Carbonyl Disconnections 207 29. Strategy XIII: Introduction to Ring Synthesis: Saturated Heterocycles 217 30. Three-Membered Rings 229 31. Strategy XIV: Rearrangements in Synthesis 237 32. Four-Membered Rings: Photochemistry in Synthesis 245 33. Strategy XV: The Use of Ketenes in Synthesis 251 34. Five-Membered Rings 255 35. Strategy XVI: Pericyclic Reactions in Synthesis: Special Methods for Five-Membered Rings 261 36. Six-Membered Rings 269 37. General Strategy C: Strategy of Ring Synthesis 279 38. Strategy XVII: Stereoselectivity B 289 39. Aromatic Heterocycles 301 40. General Strategy D: Advanced Strategy 313 Index 325

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Book SynopsisHeterocycles in Life and Society is an introduction to the chemistry of heterocyclic compounds, focusing on their origin and occurrence in nature, biochemical significance and wide range of applications.Trade ReviewNamed CHOICE Outstanding Title for 2012"Summing Up: Highly recommended. All students, researchers/faculty, and professionals." (Choice, 1 January 2012)Table of ContentsPREFACE TO SECOND ENGLISH EDITION. PREFACE TO FIRST ENGLISH EDITION. 1 MOLECULAR RINGS STUDDED WITH JEWELS. 1.1 From Homocycle to Heterocycle. 1.2 Building Heterocycles from Benzene. 1.3 Some More Kinds of Heterocycles. 1.4 Problems. 1.5 Suggested Reading. 2 WHY NATURE PREFERS HETEROCYCLES . 2.1 Reactions for All Tastes. 2.2 Heterocycles as Acids and Bases. 2.3 Heterocycles and Metals. 2.4 ‘There are Subtle Ties of Power„m'. 2.5 Tautomerism: Heterocycles and Their ‘Masks'. 2.6 Problems. 2.7 Suggested Reading. 3 HETEROCYCLES AND HEREDITARY INFORMATION . 3.1 Nucleic Acids. 3.2 The Double Helix. 3.3 How One DNA Doubles Itself. 3.4 Protein Synthesis. Genetic Code and Genome. 3.5 What are Mutations?. 3.6 Mysterious Telomers. 3.7 Gene Expression. 3.8 Problems. 3.9 Suggested Reading. 4 ENZYMES, COENZYMES AND VITAMINS . 4.1 Molecular Robots. 4.2 Coenzymes and Enzymes as ‘Joint Molecular Ventures'. 4.3 Vitamins, the ‘Molecules of Health'. 4.4 Ribozymes: Vestiges of an Ancient World. 4.5 Problems. 4.6 Suggested Reading. 5 HETEROCYCLES AND BIOENERGETICS . 5.1 ATP as the Universal Currency of Energy. 5.2 Breathing. 5.3 Problems. 5.4 Suggested Reading. 6 HETEROCYCLES AND PHOTOSYNTHESIS . 6.1 Chlorophyll: Sunlight-receiving Antenna and Energy Carrier. 6.2 What Daylight can Achieve. 6.3 Photosynthesis without Light. 6.4 Problems. 6.5 Suggested Reading. 7 HETEROCYCLES AND HEALTH. 7.1 Medicines from a Natural Storehouse. 7.2 Heterocycles versus Infectious Microbes. 7.3 Heterocycles and Viral Infections. 7.4 Heterocycles and the Diseases of Our Century. 7.5 Heterocyclic Molecules in Combat with Ulcer and Sexual Disfunctions. 7.6 Problems. 7.7 Suggested Reading. 8 HETEROCYCLES IN AGRICULTURE . 8.1 A Century of Chemical Warfare against Weeds. 8.2 Regulators of Plant Growth. 8.3 The Struggle against Voracious Insects. 8.4 Resisting the Kingdoms of Mustiness and Rot. 8.5 Heterocycles in Animal Husbandry. 8.6 Combinatorial Chemistry and Functional Genomics in the Synthesis of Biologically Active. Heterocyclic Compounds. 8.7 Problems. 8.8 Suggested Reading. 9 HETEROCYCLES IN INDUSTRY AND TECHNOLOGY. 9.1 Heterocycles and Natural Colors. 9.2 Dyes. 9.3 Fluorescent Agents. 9.4 Color Change Compounds. 9.5 Fire Retardancy. 9.6 Photographic Materials and Recorders of Information. 9.7 Heterocycles as Food Additives. 9.8 Heterocycles as Cosmetics and Perfumery Ingredients. 9.9 Other Applications. 9.10 Problems. 9.11 Suggested Reading. 10 HETEROCYCLES AND SUPRAMOLECULAR CHEMISTRY . 10.1 Molecular Recognition and Host-Guest Interactions. 10.2 Self-assembling Molecular Systems. 10.3 Problems. 10.4 Suggested Reading. 11 HETEROCYCLES AND 21st CENTURY CHALLENGES. 11.1 Energy Problems. 11.2 Ecology and Green Chemistry. 11.3 Biotechnology and Related Problems. 11.4 From Molecular Devices to Molecular Computer. 11.5 Problems. 11.6 Suggested Reading. 12 THE ORIGIN OF HETEROCYCLES . 12.1 Origin of the Universe and Appearance of Chemical Elements. 12.2 Iterstellar Molecules. 12.3 Organic Compounds in Comets and Meteorites. 12.4 Do Heterocycles exist on the Moon and Mars?. 12.5 The Atmosphere of Earth and Other Planets. 12.6 Heterocycles and the Origin of the Biosphere. 12.7 Problems. 12.8 Suggested Reading. CONCLUSION. ANSWERS AND REFERENCES TO SELECTED PROBLEMS. INDEX.

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Book SynopsisMacrocyclic molecules contain rings made up of seven or more atoms. They are interesting because they provide building blocks for synthesizing precise two or three dimensional structures an important goal in nanotechnology. For example, they can be used to develop nanosized reaction vessels, cages, switches and shuttles, and have potential as components in molecular computers. They also have applications as catalysts and sensors. Macrocycles: Construction, Chemistry and Nanotechnology Applications is an essential introduction this important class of molecules and describes how to synthesise them, their chemistry, how they can be used as nanotechnology building blocks, and their applications. A wide range of structures synthesised over the past few decades are covered, from the simpler cyclophanes and multi-ring aromatic structures to vases, bowls, cages and more complex multi-ring systems and 3D architectures such as pumpkins, interlocking chains and knots. ToTrade Review“Macrocycles : Construction, Chemistry and Nanotechnology Applications distils the essence of this important topic for undergraduate and postgraduate students, and for researchers in other fields who are interested in getting a general insight into this increasingly important class of molecules.” (Chimie Nouvelle, 1 March 2013) “Figures aside, the book provides a good introduction to novices in the field and points readers to the key references in the macrocyclic chemistry.” (Chemistry World, 2012) Table of ContentsPreface. 1. Introduction. 1.1. Simple ring compounds. 1.2. Three dimensional aliphatic carbon structures. 1.3. Annulenes. 1.4. Multi-ring aromatic structures. 1.5. Porpyrins and phthalocanines. 1.6. Conclusions. References. 2. Cyclophanes. 2.1. Introduction to cyclophanes. 2.2. Cyclophanes with one aromatic system and aliphatic chain. 2.3. Cyclophanes with more than 1 aromatic ring. 2.4. Napthalenophanes and other aromatic systems. 2.5. Cyclophanes containing heteroaromatic systems. 2.6. Ferrocenophanes. References. 3. Crown ethers, cryptands and other compounds. 3.1. Introduction. 3.2. Crown ethers. 3.3. Simple complexes with crown ethers. 3.4. Azacrowns, cyclens and cyclams. 3.5. Crowns containing other heteroatoms. 3.6. Lariat and bibracchial crown ethers. 3.7. Cryptands. 3.8. Spherands. 3.9. Combined and multiple systems. 3.10. Applications of crown ethers and related compounds. 3.11. Conclusions. References. 4. Calixarenes. 4.1. Introduction to calixarenes. 4.2. History of the calixarenes. 4.3. Structures of calixarenes. 4.4. Chemical modification of calixarenes. 4.5. Complexes with calixarenes. 4.6. Bis- and multicalixarenes. 4.7. Oxacalixarenes, azacalixarenes and thiacalixarenes. 4.8. Resorcinarenes - synthesis and structure. 4.9. Cavitands and carcerands. 4.10. Uses of calixarenes and conclusions. References. 5. Heterocalixarenes and calixnaphthalenes. 5.1. Introduction to heterocalixarenes and calixnaphthalenes. 5.2. Calixnaphthalenes. 5.3. Tropolone based macrocycles. 5.4. Calixfurans. 5.5. Calixpyrroles. 5.6. Calixindoles, calixpyridines and calixthiophenes. 5.7. Conclusions. References. 6. Cyclodextrins. 6.1. Introduction to cyclodextrins. 6.2. Complex formation by cyclodextrins. 6.3. Cyclodextrins of other sizes. 6.4. Modification reactions of cyclodextrins. 6.5. Selectivity of cyclodextrins. 6.6. Multiple cyclodextrin systems. 6.7. Polymeric cyclodextrins. 6.8. Cyclodextrins combined with other macrocyclic systems. 6.9. Therapeutic uses of cyclodextrins. 6.10. Other uses of cyclodextrins. 6.11. Conclusions. References. 7. Cyclotriveratylenes and cryptophanes. 7.1. Introduction to cyclotriveratrylenes and cryptophanes. 7.2. Synthesis of cyclotriveratrylenes. 7.3. Modification of cyclotriveratrylenes. 7.4. Synthesis of optically active cyclotriveratrylenes. 7.5. Modification of the bridging groups. 7.6. Modification of the aromatic rings with organometallic groups. 7.7. Selective binding applications of cyclotriveratrylenes. 7.8. Analogues of CTV. 7.9. Cryptophanes - synthesis and structure. 7.10. Cryptophanes - chemical modification. 7.11. Complexes with cryptophanes. 7.12. Cryptophane/Xenon complexes. 7.13. Other uses of cryptophanes. 7.14. Hemicryptophanes. 7.15. Conclusions. References. 8. Cucurbiturils. 8.1. Introduction to cucurbiturils. 8.2. Complexation behaviour of simple cucurbiturils. 8.3. Modification of cucurbiturils. 8.4. Uses of cucurbiturils. 8.5. Hemicucurbiturils. 8.6. Conclusions. References. 9. Rotaxanes and catenanes. 9.1. Introduction to rotaxanes and catenanes. 9.2. Rotaxanes. 9.3. Rotaxanes as molecular machines. 9.4. Thin films of rotaxanes. 9.5. Polyrotaxanes. 9.6. Catenanes. 9.7. Switchable catenanes. 9.8. Catenanes on surfaces. 9.9. Polycatenanes and catenated polymers. 9.10. Natural catenanes. 9.11. Conclusions. References. 10. Other supermolecular systems, molecular motors, machines and nanotechnological applications. 10.1. Introduction. 10.2. Other molecular systems. 10.3. Molecular devices, motors and machines. 10.4. Conclusions. References.

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Book SynopsisProcess Analytical Technology explores the concepts of this technology and its application in the chemical and pharmaceutical industry from the point of view of the analytical chemist.Trade Review"Overall, this excellent compilation is highly recommended." (Organic Process Research and Development, January 2011) Table of ContentsPreface to the Second Edition xvii List of Contributors xix List of Abbreviations xxi 1 Overview of Process Analysis and PAT 1 Jason E. Dickens 1.1 Introduction 1 1.1.1 Historical perspective 3 1.1.2 Business drivers 4 1.2 Execution of Process Analysis Projects 5 1.2.1 Wisdoms 5 1.2.2 Team structure 6 1.2.3 Project life cycle 6 1.2.4 Project scoping 9 1.2.5 Common challenges and pitfalls 10 1.3 Process Instrumentation 12 1.3.1 Process instrumentation types 12 1.3.2 Novel process instrumentation 12 1.4 Conclusions 13 1.5 Glossary of Acronyms and Terms 14 References 14 2 Implementation of Process Analytical Technologies 17 Robert Guenard and Gert Thurau 2.1 Introduction to Implementation of Process Analytical Technologies (PAT) in the Industrial Setting 17 2.1.1 Definition of process analytics 18 2.1.2 Differences between process analyzers and laboratory analysis 19 2.1.3 General industrial drivers for PA 19 2.1.4 Types of applications (R&D versus manufacturing) 20 2.1.5 Organizational considerations 20 2.2 Generalized Process Analytics Work Process 23 2.2.1 Project identification and definition 24 2.2.2 Analytical application development 26 2.2.3 Design, specify and procure 26 2.2.4 Implementation in production 28 2.2.5 Routine operation 29 2.2.6 Continuous improvement 30 2.3 Considerations for PAT Implementation in the Pharmaceutical Industry 30 2.3.1 Introduction 30 2.3.2 Business model 30 2.3.3 Technical differences 31 2.3.4 Regulatory Aspects of Process Analytics in the Pharmaceutical Industry –the Concept of Quality by Design 33 2.4 Conclusions 36 References 36 3 Process Sampling: Theory of Sampling – the Missing Link in Process Analytical Technologies (PAT) 37 Kim H. Esbensen and Peter Paasch-Mortensen 3.1 Introduction 37 3.2 Theory of Sampling – Introduction 39 3.2.1 Heterogeneity 41 3.2.2 Constitutional heterogeneity 41 3.2.3 Distributional heterogeneity 42 3.2.4 Structurally correct sampling 45 3.2.5 Incorrect sampling error 45 3.2.6 Increment delimitation error 45 3.2.7 Increment extraction error 46 3.2.8 Increment preparation error 46 3.2.9 Increment weighing error 47 3.2.10 Total sampling error 48 3.2.11 Global estimation error 48 3.3 Mass Reduction as a Specific Sampling Procedure 48 3.4 Fundamental Sampling Principle 51 3.5 Sampling – a Very Practical Issue 51 3.5.1 Sampling unit operations 52 3.5.2 Understanding process sampling: 0-D versus 1-D LOTS 52 3.5.3 Grab sampling – 0-D and 1-D 54 3.5.4 Correct process sampling: increment delimitation/extraction 56 3.5.5 PAT versus correct process sampling – what is required? 58 3.6 Reactors and Vessels – Identical Process Sampling Issues 60 3.6.1 Correct process sampling with existing process technology 62 3.6.2 Upward flux – representative colocated PAT sampling 62 3.6.3 Upstream colocated PAT sampler 64 3.7 Heterogeneity Characterization of 1-D lots: Variography 66 3.7.1 Process sampling modes 67 3.7.2 The experimental variogram 67 3.7.3 Sampling plan simulation and estimation of TSE 71 3.7.4 TSE estimation for 0-D lots – batch sampling 72 3.7.5 Corporate QC benefits of variographic analysis 73 3.8 Data Quality – New Insight from the TOS 75 3.9 Validation in Chemometrics and PAT 76 3.10 Summary 78 References 79 4 UV-visible Spectroscopy for On-line Analysis 81 Marcel A. Liauw, Lewis C. Baylor and Patrick E. O’Rourke 4.1 Introduction 81 4.2 Theory 82 4.2.1 Chemical concentration 82 4.2.2 Color 84 4.2.3 Film thickness 85 4.2.4 Turbidity 85 4.2.5 Plasmons/nanoparticles 85 4.3 Instrumentation 85 4.4 Sample Interface 86 4.4.1 Cuvette/vial 87 4.4.2 Flow cells 87 4.4.3 Insertion probe 87 4.4.4 Reflectance probe 89 4.5 Implementation 89 4.5.1 A complete process analyzer 89 4.5.2 Troubleshooting 89 4.6 Applications 91 4.6.1 Gas and vapor analysis 92 4.6.2 Liquid analysis 92 4.6.3 Solid analysis 96 4.6.4 Other applications 99 4.7 Detailed Application Notes 100 4.7.1 Gas and vapor analysis: toluene 100 4.7.2 Liquid analysis: breakthrough curves 101 4.7.3 Solids analysis: extruded plastic color 101 4.7.4 Film thickness determination: polymer 103 4.8 Conclusion 104 References 104 5 Near-infrared Spectroscopy for Process Analytical Technology: Theory, Technology and Implementation 107 Michael B. Simpson 5.1 Introduction 107 5.2 Theory of Near-infrared Spectroscopy 112 5.3 Analyser Technologies in the Near-infrared 114 5.3.1 Light sources and detectors for near-infrared analyzers 114 5.3.2 The scanning grating monochromator and polychromator diode-array 119 5.3.3 The acousto-optic tunable filter (AOTF) analyzer 123 5.3.4 Fourier transform near-infrared analyzers 127 5.3.5 Emerging technologies in process NIR analyzers 134 5.4 The Sampling Interface 136 5.4.1 Introduction 136 5.4.2 Problem samples: liquids, slurries and solids 142 5.4.3 The use of fiber optics 145 5.5 Practical Examples of Near-infrared Analytical Applications 147 5.5.1 Refinery hydrocarbon streams 148 5.5.2 Polyols, ethoxylated derivatives, ethylene oxide/propylene oxide polyether polyols 149 5.5.3 Oleochemicals, fatty acids, fatty amines and biodiesel 151 5.6 Conclusion 152 References 153 6 Infrared Spectroscopy for Process Analytical Applications 157 John P. Coates 6.1 Introduction 157 6.2 Practical Aspects of IR Spectroscopy 161 6.3 Instrumentation Design and Technology 163 6.4 Process IR Instrumentation 166 6.4.1 Commercially available IR instruments 167 6.4.2 Important IR component technologies 172 6.4.3 New technologies for IR components and instruments 176 6.4.4 Requirements for process infrared analyzers 178 6.4.5 Sample handling for IR process analyzers 185 6.4.6 Issues for consideration in the implementation of process IR 187 6.5 Applications of Process IR Analyzers 189 6.6 Process IR Analyzers: a Review 191 6.7 Trends and Directions 192 References 193 7 Raman Spectroscopy 195 Nancy L. Jestel 7.1 Attractive Features of Raman Spectroscopy 195 7.1.1 Quantitative information 195 7.1.2 Flexible sample forms and sizes used as accessed without damage 196 7.1.3 Flexible sample interfaces 196 7.1.4 Attractive spectral properties and advantageous selection rules 197 7.1.5 High sampling rate 197 7.1.6 Stable and robust equipment 198 7.2 Potential Issues with Raman Spectroscopy 198 7.2.1 High background signals 198 7.2.2 Stability 198 7.2.3 Too much and still too little sensitivity 199 7.2.4 Personnel experience 199 7.2.5 Cost 200 7.3 Fundamentals of Raman Spectroscopy 200 7.4 Raman Instrumentation 203 7.4.1 Safety 203 7.4.2 Laser wavelength selection 204 7.4.3 Laser power and stability 204 7.4.4 Spectrometer 205 7.4.5 Sample interface (probes) 206 7.4.6 Communications 208 7.4.7 Maintenance 209 7.5 Quantitative Raman 209 7.6 Applications 212 7.6.1 Acylation, alkylation, catalytic cracking, and transesterification 213 7.6.2 Bioreactors 213 7.6.3 Blending 214 7.6.4 Calcination 214 7.6.5 Catalysis 215 7.6.6 Chlorination 216 7.6.7 Counterfeit pharmaceuticals 217 7.6.8 Extrusion 218 7.6.9 Forensics 218 7.6.10 Hydrogenation 218 7.6.11 Hydrolysis 219 7.6.12 Medical diagnostics 219 7.6.13 Microwave-assisted organic synthesis 219 7.6.14 Mobile or field uses 220 7.6.15 Natural products 220 7.6.16 Orientation, stress, or strain 221 7.6.17 Ozonolysis 222 7.6.18 Polymerization 222 7.6.19 Polymer curing 224 7.6.20 Polymorphs (crystal forms) 225 7.6.21 Product properties 228 7.6.22 Purification: distillation, filtration, drying 229 7.6.23 Thin films or coatings 229 7.7 Current State of Process Raman Spectroscopy 230 References 231 8 Near-infrared Chemical Imaging for Product and Process Understanding 245 E. Neil Lewis, Joseph W. Schoppelrei, Lisa Makein, Linda H. Kidder and Eunah Lee 8.1 The PAT Initiative 245 8.2 The Role of Near-infrared Chemical Imaging (NIR-CI) in the Pharmaceutical Industry 246 8.2.1 Characterization of solid dosage forms 246 8.2.2 ‘A picture is worth a thousand words’ 247 8.3 Evolution of NIR Imaging Instrumentation 247 8.3.1 Spatially resolved spectroscopy – mapping 247 8.3.2 The infrared focal-plane array 247 8.3.3 Wavelength selection 248 8.3.4 The benefits of NIR spectroscopy 248 8.3.5 NIR imaging instrumentation 249 8.4 Chemical Imaging Principles 251 8.4.1 The hypercube 251 8.4.2 Data analysis 251 8.4.3 Spectral correction 252 8.4.4 Spectral preprocessing 253 8.4.5 Classification 253 8.4.6 Image processing – statistical 255 8.4.7 Image processing – morphology 257 8.5 PAT Applications 257 8.5.1 Content uniformity measurements – ‘self calibrating’ 258 8.5.2 Quality assurance – imaging an intact blister pack 260 8.5.3 Contaminant detection 261 8.5.4 Imaging of coatings – advanced design delivery systems 263 8.6 Processing Case Study: Estimating ‘Abundance’ of Sample Components 267 8.6.1 Experimental 268 8.6.2 Spectral correction and preprocessing 268 8.6.3 Analysis 268 8.6.4 Conclusions 273 8.7 Processing Case Study: Determining Blend Homogeneity Through Statistical Analysis 273 8.7.1 Experimental 273 8.7.2 Observing visual contrast in the image 274 8.7.3 Statistical analysis of the image 274 8.7.4 Blend uniformity measurement 276 8.7.5 Conclusions 276 8.8 Final Thoughts 277 Acknowledgements 278 References 278 9 Acoustic Chemometric Monitoring of Industrial Production Processes 281 Maths Halstensen and Kim H. Esbensen 9.1 What is Acoustic Chemometrics? 281 9.2 How Acoustic Chemometrics Works 282 9.2.1 Acoustic sensors 282 9.2.2 Mounting acoustic sensors (accelerometers) 283 9.2.3 Signal processing 284 9.2.4 Chemometric data analysis 284 9.2.5 Acoustic chemometrics as a PAT tool 284 9.3 Industrial Production Process Monitoring 285 9.3.1 Fluidized bed granulation monitoring 285 9.3.2 Pilot scale studies 286 9.3.3 Monitoring of a start-up sequence of a continuous fluidized bed granulator 291 9.3.4 Process monitoring as an early warning of critical shutdown situations 295 9.3.5 Acoustic chemometrics for fluid flow quantification 296 9.4 Available On-line Acoustic Chemometric Equipment 299 9.5 Discussion 301 9.5.1 Granulator monitoring 301 9.5.2 Process state monitoring 301 9.5.3 Ammonia concentration monitoring 301 9.6 Conclusions 302 References 302 10 Process NMR Spectroscopy: Technology and On-line Applications 303 John C. Edwards and Paul J. Giammatteo 10.1 Introduction 303 10.2 NMR Spectroscopy Overview 305 10.2.1 The NMR phenomenon 305 10.2.2 Time–domain-NMR: utilization of the FID and spin relaxation 309 10.2.3 High-resolution NMR: obtaining a spectrum with resolved chemical shift information 312 10.3 Process NMR Instrumentation 313 10.3.1 Spectrometer and magnet design 313 10.3.2 Sampling and experimental design 316 10.4 Postprocessing Methodologies for NMR Data 317 10.5 Advantages and Limitations of NMR as a Process Analytical Technology 320 10.5.1 Advantages 320 10.5.2 Limitations 321 10.6 On-line and At-line Applications 321 10.6.1 Time–domain NMR 322 10.6.2 High-resolution NMR: chemometric applications 323 10.7 Current Development and Applications 330 10.8 Conclusions 331 References 332 11 Fluorescent Sensing and Process Analytical Applications 337 Jason E. Dickens 11.1 Introduction 337 11.2 Luminescence Fundamentals 338 11.2.1 Luminescence nomenclature 338 11.2.2 Luminescence processes 338 11.2.3 Fluorophore classification 338 11.3 LIF Sensing Fundamentals 341 11.3.1 LIF sensing classification 341 11.3.2 Luminescence spectroscopy 342 11.3.3 LIF signal response function 343 11.4 LIF Sensing Instrumentation 343 11.4.1 LIF photometric instrument specification 345 11.4.2 LIF Instrument selection 347 11.5 Luminescent Detection Risks 347 11.6 Process Analytical Technology Applications 348 11.6.1 Petrochemical, chemical and nuclear field applications 349 11.6.2 Pharmaceutical PAT applications 349 11.7 Conclusions 350 References 351 12 Chemometrics in Process Analytical Technology (PAT) 353 Charles E. Miller 12.1 Introduction 353 12.1.1 What is chemometrics? 353 12.1.2 Some history 354 12.1.3 Some philosophy 355 12.1.4 Chemometrics in analytical chemistry? 355 12.1.5 Chemometrics in process analytical chemistry? 356 12.2 Foundations of Chemometrics 356 12.2.1 Notation 356 12.2.2 Some basic statistics 358 12.2.3 Linear regression 359 12.2.4 Multiple linear regression 361 12.2.5 Principal components analysis (PCA) 362 12.2.6 Design of experiments (DOE) 366 12.3 Chemometric Methods in PAT 368 12.3.1 Data preprocessing 369 12.3.2 Quantitative model building 377 12.3.3 Qualitative model building 389 12.3.4 Exploratory analysis 397 12.4 Overfitting and Model Validation 407 12.4.1 Overfitting and underfitting 407 12.4.2 Test set validation 408 12.4.3 Cross validation 410 12.5 Outliers 413 12.5.1 Introduction to outliers 413 12.5.2 Outlier detection and remediation 413 12.6 Calibration Strategies in PAT 416 12.6.1 The ‘calibration strategy space’ 417 12.6.2 Strategies for direct versus inverse modeling methods 418 12.6.3 Hybrid strategies 419 12.7 Sample and Variable Selection in Chemometrics 420 12.7.1 Sample selection 420 12.7.2 Variable selection 421 12.8 Troubleshooting/Improving an Existing Method 425 12.8.1 Method assessment 425 12.8.2 Model improvement strategies 425 12.9 Calibration Transfer and Instrument Standardization 426 12.9.1 Slope/intercept adjustment 428 12.9.2 Piecewise direct standardization (PDS) 428 12.9.3 Generalized least squares (GLS) weighting 429 12.9.4 Shenk–Westerhaus method 429 12.9.5 Other transfer/standardization methods 429 12.10 Chemometric Model Deployment Issues in PAT 430 12.10.1 Outliers in prediction 430 12.10.2 Deployment software 432 12.10.3 Data systems, and control system integration 432 12.10.4 Method updating 433 12.11 People Issues 433 12.12 The Final Word 434 References 434 13 On-line PAT Applications of Spectroscopy in the Pharmaceutical Industry 439 Brandye Smith-Goettler 13.1 Background 439 13.2 Reaction Monitoring 441 13.3 Crystallization 442 13.4 API Drying 443 13.5 Nanomilling 444 13.6 Hot-melt Extrusion 445 13.7 Granulation 446 13.7.1 Wet granulation 446 13.7.2 Roller compaction 449 13.8 Powder Blending 450 13.8.1 Lubrication 451 13.8.2 Powder flow 451 13.9 Compression 452 13.10 Coating 452 13.11 Biologics 453 13.11.1 Fermentation 453 13.11.2 Freeze-drying 454 13.12 Cleaning Validation 454 13.13 Conclusions 455 References 455 14 NIR spectroscopy in Pharmaceutical Analysis: Off-line and At-line PAT Applications 463 Marcelo Blanco Romía and Manel Alcalá Bernárdez 14.1 Introduction 463 14.1.1 Operational procedures 464 14.1.2 Instrument qualification 466 14.2 Foundation of Qualitative Method Development 466 14.2.1 Pattern recognition methods 467 14.2.2 Construction of spectral libraries 468 14.2.3 Identification and qualification 470 14.3 Foundation of Quantitative Method Development 471 14.3.1 Selection and preparation of samples 472 14.3.2 Preparation and selection of samples 473 14.3.3 Determination of reference values 474 14.3.4 Acquisition of spectra 474 14.3.5 Construction of the calibration model 475 14.3.6 Model validation 476 14.3.7 Prediction of new samples 476 14.4 Method Validation 476 14.5 Calibration Transfer 476 14.6 Pharmaceutical Applications 478 14.6.1 Identification of raw materials 478 14.6.2 Homogeneity 478 14.6.3 Moisture 480 14.6.4 Determination of physical parameters 481 14.6.5 Determination of chemical composition 483 14.7 Conclusions 485 References 486 15 Near-infrared Spectroscopy (NIR) as a PAT Tool in the Chemical Industry: Added Value and Implementation Challenges 493 Ann M. Brearley and Susan J. Foulk 15.1 Introduction 493 15.2 Successful Process Analyzer Implementation 494 15.2.1 A process for successful process analyzer implementation 494 15.2.2 How NIR process analyzers contribute to business value 497 15.2.3 Issues to consider in setting technical requirements for a process analyzer 498 15.2.4 Capabilities and limitations of NIR 499 15.2.5 General challenges in process analyzer implementation 500 15.2.6 Approaches to calibrating an NIR analyzer on-line 502 15.2.7 Special challenges in NIR monitoring of polymer melts 505 15.3 Example Applications 506 15.3.1 Monitoring monomer conversion during emulsion polymerization 506 15.3.2 Monitoring a diethylbenzene isomer separation process 508 15.3.3 Monitoring the composition of copolymers and polymer blends in an extruder 509 15.3.4 Rapid identification of carpet face fiber 512 15.3.5 Monitoring the composition of spinning solution 514 15.3.6 Monitoring end groups and viscosity in polyester melts 516 15.3.7 In-line monitoring of a copolymerization reaction 518 References 520 16 Future Trends for PAT for Increased Process Understanding and Growing Applications in Biomanufacturing 521 Katherine A. Bakeev and Jose C. Menezes 16.1 Introduction 521 16.2 Regulatory Guidance and its Impact on PAT 522 16.3 Going Beyond Process Analyzers Towards Solutions 524 16.3.1 Design of experiments for risk-based analysis 526 16.3.2 Sample and process fingerprinting with PAT tools 527 16.3.3 Design and Control Spaces 528 16.3.4 Chemometrics and process analysis 528 16.4 Emerging Application Areas of PAT 529 16.4.1 Biofuels 529 16.4.2 Biomanufacturing 530 16.5 New and Emerging Sensor and Control Technologies 531 16.5.1 Terahertz spectroscopy 531 16.5.2 Integrated sensing and processing 532 16.5.3 Dielectric spectroscopy 533 16.5.4 Process chromatography 533 16.5.5 Mass spectrometry 534 16.5.6 Microwave resonance 534 16.5.7 Novel sensors 535 16.5.8 Inferential sensors 536 16.6 Advances in Sampling: NeSSI 537 16.7 Challenges Ahead 537 16.7.1 Continuous process validation 538 16.7.2 Data challenges: data handling and fusion 539 16.7.3 Regulatory challenges 539 16.7.4 Enterprise systems for managing data 539 16.8 Conclusion 540 References 540 Index 545

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Book SynopsisUntil recently the low-coordinate compounds of the heavier elements of group 14 were known only as transient, unstable species which were difficult to isolate. However recent developments have led to the stabilisation of these compounds and today heavier group 14 element cations, radicals, anions, carbene analogues, alkene and alkyne analogues and aromatics have all been prepared as highly reactive, stable, fully characterizable and readily available organometallic reagents. Organometallic Compounds of Low-Coordinate Si, Ge, Sn and Pb describes the chemistry of this exciting new class of organometallics, with an emphasis on their major similarities and differences with the analogous species in organic chemistry. Topics covered include include the synthesis, structure, reactions and synthetic applications of : Si-, Ge-, Sn and Pb-centered cations, radicals and anions heavy analogues of carbenes: silylenes, germylenes, stannylenes and plumbylenes Trade Review“In effect, the body of work described constitutes one of the cornerstones of modern main group chemistry and this account provides a highly useful reference source for the specialist as well as a non-intimidating guide for the beginner.” (Applied Organometallic Chemistry, 6 March 2015) Table of ContentsPreface. Abbreviations. 1. Heavy Analogs of Carbenium Ions: Si-, Ge-, Sn- and Pb-Centered Cations. 1.1 Introduction. 1.2 Synthesis of RR'R"E+Cations (E = Si-Pb). 1.3 Reactions and Synthetic Applications of RRRE+ Cations16. 1.4 Theoretical Studies. 1.5 Early Studies of RR'R"E+ Cations: Free or Coordinated? 1.6 Stable RR'R"E+ Cations. 1.7 Summary and Outlook. 1.8 References. 2. Heavy Analogs of Organic Free Radicals: Si-, Ge-, Sn- and Pb-Centered Radicals. 2.1 Introduction. 2.2 Early Studies: Transient Species RR'R"E. 2.3 Persistent Radicals (Generation and Identification). 2.4 Stable Radicals. 2.5 Summary and Outlook. 2.6 References. 3. Heavy Analogs of Carbanions: Si-, Ge-, Sn- and Pb-Centered Anions. 3.1 Introduction. 3.2 Synthesis. 3.3 Structure. 3.4 Reactions and Synthetic Applications. 3.5 Recent Developments. 3.6 Summary and Outlook. 3.7 References. 4. Heavy Analogs of Carbenes: Silylenes, Germylenes, Stannylenes and Plumbylenes. 4.1 Introduction. 4.2 Generation. 4.3 Spectroscopic Identification. 4.4 Structure. 4.5 Reactions of Transient Species. 4.6 Stable/Persistent Silylenes, Germylenes, Stannylenes and Plumbylenes. 4.7 Summary and Outlook. 4.8 References. 5. Heavy Analogs of Alkenes, 1,3-Dienes, Allenes and Alkynes: Multiply Bonded Derivatives of Si, Ge, Sn and Pb. 5.1 Introduction. 5.2 Early Studies: Generation and Identification. 5.3 Stable Derivatives (Synthesis and Structure). 5.4 Summary and Outlook. 5.5 References. 6. Heavy Analogs of Aromatic Compounds. 6.1 Introduction. 6.2 Early Studies. 6.3 Stable Compounds (Synthesis and Structure). 6.4 Summary and Outlook. 6.5 References. Index.

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Book SynopsisFocusing on spectroscopic properties of molecular systems, Quantum Modeling of Molecular Materials presents the state-of-the-art methods in theoretical chemistry that are used to determine molecular properties relevant to different spectroscopies.Table of ContentsPreface xi 1 Introduction 1 2 Quantum Mechanics 11 2.1 Fundamentals 11 2.1.1 Postulates of Quantum Mechanics 11 2.1.2 Lagrangian and Hamiltonian Formalisms 11 2.1.3 Wave Functions and Operators 18 2.2 Time Evolution of Wave Functions 22 2.3 Time Evolution of Expectation Values 25 2.4 Variational Principle 27 Further Reading 29 3 Particles and Fields 31 3.1 Microscopic Maxwell’s Equations 32 3.1.1 General Considerations 32 3.1.2 The Stationary Case 34 3.1.3 The General Case 38 3.1.4 Electromagnetic Potentials and Gauge Freedom 39 3.1.5 Electromagnetic Waves and Polarization 41 3.1.6 Electrodynamics: Relativistic and Nonrelativistic Formulations 45 3.2 Particles in Electromagnetic Fields 48 3.2.1 The Classical Mechanical Hamiltonian 48 3.2.2 The Quantum-Mechanical Hamiltonian 52 3.3 Electric and Magnetic Multipoles 57 3.3.1 Multipolar Gauge 57 3.3.2 Multipole Expansions 59 3.3.3 The Electric Dipole Approximation and Beyond 63 3.3.4 Origin Dependence of Electric and Magnetic Multipoles 64 3.3.5 Electric Multipoles 65 3.3.5.1 General Versus Traceless Forms 65 3.3.5.2 What We Can Learn from Symmetry 68 3.3.6 Magnetic Multipoles 69 3.3.7 Electric Dipole Radiation 70 3.4 Macroscopic Maxwell’s Equations 72 3.4.1 Spatial Averaging 72 3.4.2 Polarization and Magnetization 73 3.4.3 Maxwell’s Equations in Matter 77 3.4.4 Constitutive Relations 79 3.5 Linear Media 81 3.5.1 Boundary Conditions 82 3.5.2 Polarization in Linear Media 86 3.5.3 Electromagnetic Waves in a Linear Medium 92 3.5.4 Frequency Dependence of the Permittivity 96 3.5.4.1 Kramers–Kronig Relations 97 3.5.4.2 Relaxation in the Debye Model 98 3.5.4.3 Resonances in the Lorentz Model 101 3.5.4.4 Refraction and Absorption 105 3.5.5 Rotational Averages 107 3.5.6 A Note About Dimensions, Units, and Magnitudes 110 Further Reading 111 4 Symmetry 113 4.1 Fundamentals 113 4.1.1 Symmetry Operations and Groups 113 4.1.2 Group Representation 117 4.2 Time Symmetries 120 4.3 Spatial Symmetries 125 4.3.1 Spatial Inversion 125 4.3.2 Rotations 127 Further Reading 134 5 Exact-State Response Theory 135 5.1 Responses in Two-Level System 135 5.2 Molecular Electric Properties 145 5.3 Reference-State Parameterizations 151 5.4 Equations of Motion 156 5.4.1 Time Evolution of Projection Amplitudes 157 5.4.2 Time Evolution of Rotation Amplitudes 159 5.5 Response Functions 163 5.5.1 First-Order Properties 166 5.5.2 Second-Order Properties 166 5.5.3 Third-Order Properties 169 5.5.4 Fourth-Order Properties 174 5.5.5 Higher-Order Properties 179 5.6 Dispersion 179 5.7 Oscillator Strength and Sum Rules 183 5.8 Absorption 185 5.9 Residue Analysis 190 5.10 Relaxation 194 5.10.1 Density Operator 195 5.10.2 Liouville Equation 196 5.10.3 Density Matrix from Perturbation Theory 200 5.10.4 Linear Response Functions from the Density Matrix 201 5.10.5 Nonlinear Response Functions from the Density Matrix 204 5.10.6 Relaxation in Wave Function Theory 204 5.10.7 Absorption Cross Section 207 5.10.8 Einstein Coefficients 210 Further Reading 211 6 Electronic and Nuclear Contributions to Molecular Properties 213 6.1 Born–Oppenheimer Approximation 213 6.2 Separation of Response Functions 216 6.3 Molecular Vibrations and Normal Coordinates 221 6.4 Perturbation Theory for Vibrational Wave Functions 225 6.5 Zero-Point Vibrational Contributions to Properties 227 6.5.1 First-Order Anharmonic Contributions 227 6.5.2 Importance of Zero-Point Vibrational Corrections 231 6.5.3 Temperature Effects 234 6.6 Pure Vibrational Contributions to Properties 235 6.6.1 Perturbation Theory Approach 235 6.6.2 Pure Vibrational Effects from an Analysis of the Electric-Field Dependence of the Molecular Geometry 238 6.7 Adiabatic Vibronic Theory for Electronic Excitation Processes 244 6.7.1 Franck–Condon Integrals 248 6.7.2 Vibronic Effects in a Diatomic System 250 6.7.3 Linear Coupling Model 252 6.7.4 Herzberg–Teller Corrections and Vibronically Induced Transitions 252 Further Reading 253 7 Approximate Electronic State Response Theory 255 7.1 Reference State Parameterizations 255 7.1.1 Single Determinant 255 7.1.2 Configuration Interaction 263 7.1.3 Multiconfiguration Self-Consistent Field 266 7.1.4 Coupled Cluster 268 7.2 Equations of Motion 271 7.2.1 Ehrenfest Theorem 271 7.2.2 Quasi-Energy Derivatives 275 7.3 Response Functions 276 7.3.1 Single Determinant Approaches 276 7.3.2 Configuration Interaction 281 7.3.3 Multiconfiguration Self-Consistent Field 281 7.3.4 Matrix Structure in the SCF, CI, and MCSCF Approximations 281 7.3.5 Coupled Cluster 285 7.4 Residue Analysis 288 7.5 Relaxation 291 Further Reading 293 8 Response Functions and Spectroscopies 295 8.1 Nuclear Interactions 296 8.1.1 Nuclear Charge Distribution 296 8.1.2 Hyperfine Structure 301 8.1.2.1 Nuclear Magnetic Dipole Moment 301 8.1.2.2 Nuclear Electric Quadrupole Moment 305 8.2 Zeeman Interaction and Electron Paramagnetic Resonance 310 8.3 Polarizabilities 317 8.3.1 Linear Polarizability 317 8.3.1.1 Weak Intermolecular Forces 321 8.3.2 Nonlinear Polarizabilities 325 8.4 Magnetizability 326 8.4.1 The Origin Dependence of the Magnetizability 328 8.4.2 Magnetizabilities from Magnetically Induced Currents 331 8.4.3 Isotropic Magnetizabilities and Pascal’s Rule 332 8.5 Electronic Absorption and Emission Spectroscopies 335 8.5.1 Visible and Ultraviolet Absorption 338 8.5.2 Fluorescence Spectroscopy 343 8.5.3 Phosphorescence 344 8.5.4 Multiphoton Absorption 347 8.5.4.1 Multiphoton Absorption Cross Sections 348 8.5.4.2 Few-State Models for Two-Photon Absorption Cross Section 350 8.5.4.3 General Multiphoton Absorption Processes 351 8.5.5 X-ray Absorption 354 8.5.5.1 Core-Excited States 355 8.5.5.2 Field Polarization 358 8.5.5.3 Static Exchange Approximation 360 8.5.5.4 Complex or Damped Response Theory 362 8.6 Birefringences and Dichroisms 364 8.6.1 Natural Optical Activity 366 8.6.2 Electronic Circular Dichroism 372 8.6.3 Nonlinear Birefringences 375 8.6.3.1 Magnetic Circular Dichroism 376 8.6.3.2 Electric Field Gradient-Induced Birefringence 379 8.7 Vibrational Spectroscopies 381 8.7.1 Infrared Absorption 381 8.7.1.1 Double-Harmonic Approximation 381 8.7.1.2 Anharmonic Corrections 383 8.7.2 Vibrational Circular Dichroism 384 8.7.3 Raman Scattering 388 8.7.3.1 Raman Scattering from a Classical Point of View 388 8.7.3.2 Raman Scattering from a Quantum Mechanical Point of View 392 8.7.4 Vibrational Raman Optical Activity 402 8.8 Nuclear Magnetic Resonance 408 8.8.1 The NMR Experiment 408 8.8.2 NMR Parameters 413 Further Reading 417 Appendicies A Abbreviations 419 B Units 421 C Second Quantization 423 C.1 Creation and Annihilation Operators 423 C.2 Fock Space 425 C.3 The Number Operator 426 C.4 The Electronic Hamiltonian on Second-Quantized Form 427 C.5 Spin in Second Quantization 429 D Fourier Transforms 431 E Operator Algebra 435 F Spin Matrix Algebra 439 G Angular Momentum Algebra 441 H Variational Perturbation Theory 445 I Two-Level Atom 451 I.1 Rabi Oscillations 452 I.2 Time-Dependent Perturbation Theory 454 I.3 The Quasi-energy Approach 455 Index 457

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Book SynopsisPractical Cell Analysis serves as a guide for researchers interested in adding cell analyses to their repertoire. This book covers the basics of setting up a cell culture-capable laboratory, as well as sources and types of cells.Trade Review"It is a valuable means to get started in the field and targets mainly scientists without prior experience in cell biology . . . In summary, the book has earned its place on the bench in an interdisciplinary life science environment." (Anal Bioanal Chem, 2010)Table of ContentsChapter 1: Getting Starting (and Getting the Cells) 1.1 Introduction 1.2 The Driving Need 1.3 Primary and Cultured Cells 1.4 Choosing a Cultured Cell 1.5 Choosing Primary Cells 1.6 Easily Obtainable Primary Cells 1.7 Primary Cells from Tissues 1.8 Purifying Primary Cells 1.9 How Long do Primary Cells Remain Primary? 1.10 Obtaining Primary Cells from a Commercial Source 1.11 Bacteria and Yeast 1.12 Practical Aspects of Cell Culture 1.13 Safety Aspects of Primary and Transformed Cell Lines 1.14 Transfection of Primary and Transformed Cell Lines 1.15 Conclusion References Chapter 2: The Cell Culture Laboratory (Tools of the Trade) 2.1 Introduction 2.2 Issues Concerning a Cell Laboratory 2.3 Setting up a Cell Culture Laboratory 2.4 Cell Line Storage 2.5 Personal Protective Equipment 2.6 Cell and Sample Handling 2.7 Common Analytical Instrumentation for Cell Culture 2.8 Considerations when Setting up a Cell Culture Laboratory 2.9 Establishing and Regulating A Culture Facility 2.10 Conclusion References Chapter 3. Maintaining Cultures 3.1 Introduction 3.2 Medium 3.3 The Use of Medium in Analysis, and Alternatives 3.4 Culturing Cells Protocol 3.1: Sub-Culture of Adherent Cells 3.5 Growing Cells in Three Dimensions 3.6 Sterility and Contamination of Culture 3.7 Storage of Cell Samples and Cell Lines Protocol 3.2: Cryopreservation of Mammalian Cells Protocol 3.3: Retrieval of Cells from Liquid Nitrogen Storage 3.8 Conclusion References Chapter 4. Microscopy of Cells 4.1 Introduction 4.2 Microscope Types 4.3 Culturing Cells for Microscopy 4.4 Signals, Background, and Artifacts in Optical Microscopy 4.5 Staining Cells for Fluorescence Microscopy 4.6 Multiple Labels 4.7 Viability and Two-Photon Microscopy 4.8 Spatial Resolution in Optical Microscopy 4.9 Image Saturation and Intensity 4.10 Atomic Force and Environmental Scanning Electron Microscopy 4.11 Conclusion References Chapter 5: Separating Cells 5.1 Introduction 5.2 The Cell Sample 5.3 Label-Free (Intrinsic) Separations 5.4 Immunomagnetic Sorting 5.5 Cell Affinity Chromatography 5.6 Affinity Chemistry Considerations in CAC and MACS Separations Protocol 5.1: Screening of Antibody Clones 5.7 Elution in Cell Affinity Chromatography 5.8 Nonspecific Binding in Cell Separations 5.9 Separation of Rare Cells 5.10 Fluorescence Activate Cell Sorting 5.11 Sorting Parameters 5.12 Other Separation Techniques and Considerations 5.13 Conclusion References Chapter 6. Flow Cytometry: Cell Analysis in the Fast Lane 6.1 Introduction 6.2 The Cell Sample 6.3 Flow Cytometer Function 6.4 Obtaining or Finding a Flow Cytometer 6.5 Using Flow Cytometers 6.6 Setting up a Flow Cytometer for Multi-Color Staining 6.7 Analyzing Flow Cytometry Data 6.8 Example Flow Cytometry Assays 6.9 No-Flow Cytometry 6.10 Conclusion References Chapter 7: Analyzing Cells with Microfluidic Devices 7.1 Introduction 7.2 Advantages of Microfluidics 7.3 Considerations of Microfluidics and Cells 7.4 Obtaining Microfluidic Cell Devices 7.5 Microfluidic Flow Cytometry 7.6 Cell Separations 7.7 Analysis of Cell Products 7.8 Cell Culture Protocol 7.1: Low-shear Cell Culture Chip 7.9 Conclusion References Chapter 8: Statistical Considerations 8.1 Introduction 8.2 Types of Error 8.3 Figures of Merit in Statistical Analysis of Cells 8.4 Limits of Detection and Quantitation (of Cell) 8.5 Methods to Improve Cell Statistics 8.6 Comparing Analytical Values 8.7 Rejecting Data: Proceed With Caution 8.8 Conclusion References Chapter 9 Protocols, Probes, and Standards 9.1 Introduction 9.2 Cell Transfection and Immortalization (Chapter 1) Protocol 9.1: Transfecting Cells with Polyamine Reagents Protocol 9.2: Stable Transfection using Polyamine Delivery Protocol 9.3: Transfection Using Electroporation Optimizing Electroporation Parameters Protocol 9.4: Cell Immortalization using hTERT Transfection 9.3 Calculating Relative Centrifugal Force (RCF) and Centrifuge Rotor Speed (Chapter 2) 9.4 Fluorescence Methods (Chapter 4 & 6) Protocol 9.4: Apoptosis Detection Using Fluorophore-Conjugated Annexin-V and a Viability Dye Protocol 9.5: Apoptosis Detection Using Fluorogenic Caspase Probes 9.5 Surface Modifications for Cell Analysis (Chapter 5 & 7) Protocol 9.6: Covalent Linkage of Proteins (non-Antibody) to Glass by Microcontact Imprinting Protocol 9.7: Covalent Linkage of Antibodies to Glass Protocol 9.8: Noncovalent Attachment of Antibodies to Glass #1 Protocol 9.9: Noncovalent Attachment of Antibodies to Glass or PDMS #2 Protocol 9.10: Blocking Endogenous Biotin 9.6 Flow Cytometry and Cell Separations (Chapter 5 & 6) Protocol 9.11: Cell Cycle Measurements by Flow Cytometry Protocol 9.12: Antigen Density Measurements in Flow Cytometry Protocol 9.13: Antigen Density Measurements using Fluorescence Correlation Spectroscopy. Protocol 9.14: Cell Proliferation using Anti-CD71 staining (Chapter 4 & 6). 9.7 Fluorescent Labels and Fluorogenic Probes (Chapter 4, 6 & 7) References

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Book SynopsisMedicinal Natural Products: A Biosynthetic Approach, Third Edition , provides a comprehensive and balanced introduction to natural products from a biosynthetic perspective, focussing on the metabolic sequences leading to various classes of natural products.Trade Review"Students should be empowered for a deductive analysis of the presented substances." (Arzneimittelforschung, December 2009) "This new edition is an excellent text that is unrivaled in both its scope and overall coverage of natural products biosynthesis." (Journal of Medicinal Chemistry, August 2009) "There is no question that this is the best book available on the biosynthesis and bio-organic chemistry of medicinally important natural products." (Education in Chemistry, September 2009)Table of Contents1 About this book, and how to use it 1 The subject 1 The aim 1 The approach 2 The topics 2 The figures 2 Further reading 3 What to study 3 What to learn 3 Nomenclature 3 Conventions regarding acids, bases, and ions 4 Some common abbreviations 4 Further reading 5 2 Secondary metabolism: the building blocks and construction mechanisms 7 Primary and secondary metabolism 7 The building blocks 8 The construction mechanisms 11 Alkylation reactions: nucleophilic substitution 12 Alkylation reactions: electrophilic addition 12 Wagner–Meerwein rearrangements 15 Aldol and Claisen reactions 15 Imine formation and the Mannich reaction 18 Amino acids and transamination 20 Decarboxylation reactions 22 Oxidation and reduction reactions 24 Dehydrogenases 24 Oxidases 26 Monooxygenases 26 Dioxygenases 26 Amine oxidases 27 Baeyer–Villiger monooxygenases 27 Phenolic oxidative coupling 28 Halogenation reactions 28 Glycosylation reactions 31 Elucidating biosynthetic pathways 34 Further reading 38 3 The acetate pathway: fatty acids and polyketides 39 Fatty acid synthase: saturated fatty acids 39 Unsaturated fatty acids 44 Uncommon fatty acids 53 Prostaglandins 58 Thromboxanes 64 Leukotrienes 64 Polyketide synthases: generalities 66 Polyketide synthases: macrolides 68 Polyketide synthases: linear polyketides and polyethers 90 Diels–Alder cyclizations 96 Polyketide synthases: aromatics 96 Cyclizations 99 Post-polyketide synthase modifications 103 Starter groups 116 Further reading 131 4 The shikimate pathway: aromatic amino acids and phenylpropanoids 137 Aromatic amino acids and simple benzoic acids 137 Phenylpropanoids 148 Cinnamic acids and esters 148 Lignans and lignin 152 Phenylpropenes 156 Benzoic acids from C6 C3 compounds 157 Coumarins 161 Aromatic polyketides 166 Styrylpyrones, diarylheptanoids 166 Flavonoids and stilbenes 167 Flavonolignans 173 Isoflavonoids 174 Terpenoid quinones 178 Further reading 184 5 The mevalonate and methylerythritol phosphate pathways: terpenoids and steroids 187 Mevalonic acid and methylerythritol phosphate 188 Hemiterpenes (C5) 192 Monoterpenes (C10) 193 Irregular monoterpenes 204 Iridoids (C10) 206 Sesquiterpenes (C15) 210 Diterpenes (C20) 223 Sesterterpenes (C25) 234 Triterpenes (C30) 234 Triterpenoid saponins 242 Steroids 247 Stereochemistry and nomenclature 247 Cholesterol 248 Phytosterols 251 Vitamin d 256 Steroidal saponins 259 Cardioactive glycosides 265 Bile acids 275 Adrenocortical hormones/corticosteroids 277 Semi-synthesis of corticosteroids 277 Progestogens 287 Oestrogens 290 Androgens 296 Tetraterpenes (C40) 298 Higher terpenoids 306 Further reading 306 6 Alkaloids 311 Alkaloids derived from ornithine 311 Polyamines 311 Pyrrolidine and tropane alkaloids 312 Pyrrolizidine alkaloids 324 Alkaloids derived from lysine 326 Piperidine alkaloids 326 Quinolizidine alkaloids 328 Indolizidine alkaloids 330 Alkaloids derived from nicotinic acid 331 Pyridine alkaloids 331 Alkaloids derived from tyrosine 336 Phenylethylamines and simple tetrahydroisoquinoline alkaloids 336 Modified benzyltetrahydroisoquinoline alkaloids 346 Phenethylisoquinoline alkaloids 359 Terpenoid tetrahydroisoquinoline alkaloids 363 Amaryllidaceae alkaloids 365 Alkaloids derived from tryptophan 366 Simple indole alkaloids 366 Simple β-carboline alkaloids 369 Terpenoid indole alkaloids 369 Quinoline alkaloids 380 Pyrroloindole alkaloids 385 Ergot alkaloids 387 Alkaloids derived from anthranilic acid 395 Quinazoline alkaloids 395 Quinoline and acridine alkaloids 396 Alkaloids derived from histidine 398 Imidazole alkaloids 398 Alkaloids derived by amination reactions 400 Acetate-derived alkaloids 401 Phenylalanine-derived alkaloids 401 Terpenoid alkaloids 406 Steroidal alkaloids 406 Purine alkaloids 413 Caffeine 413 Saxitoxin and tetrodotoxin 416 Further reading 417 7 Peptides, proteins, and other amino acid derivatives 421 Peptides and proteins 421 Ribosomal peptide biosynthesis 422 Peptide hormones 426 Thyroid hormones 426 Hypothalamic hormones 427 Anterior pituitary hormones 429 Posterior pituitary hormones 430 Pancreatic hormones 432 Interferons 433 Opioid peptides 434 Ribosomal peptide toxins 434 Enzymes 438 Non-ribosomal peptide biosynthesis 438 Modified peptides: penicillins, cephalosporins, and other β-lactams 458 Penicillins 458 Cephalosporins 465 Other β-lactams 469 Cyanogenic glycosides 476 Glucosinolates 477 Cysteine sulfoxides 480 Further reading 481 8 Carbohydrates 485 Monosaccharides 485 Oligosaccharides 490 Polysaccharides 493 Aminosugars and aminoglycosides 498 Further reading 507 Index 509

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Book SynopsisThis book describes nerve agents and vesicants, their decomposition and their degradation products' chemistry as well as their toxicity including a list of detection techniques of nerve agents and their degradation products.Trade Review“The strength of the book “Analysis of chemical warfare degradation products” is that it gives a short introduction to CWAs in general and provides the reader with a large number of analytical examples.” (Anal Bioanal Chem, 21 February 2012)Table of ContentsPreface. 1 Historical Milieu. 1.1 Organophosphorus Nerve Agents. 1.2 Blister Agents. 1.3 Sternutator Agents. 1.4 Chemical Weapons Convention (CWC). 1.4.1 Schedule of Chemicals. 1.4.2 Destruction of Chemical Weapons. References. 2 Toxicity of Chemical Warfare Agents and their Degradation Products. 2.1 Organophosphorus Nerve Agent Toxicity. 2.1.1 Toxicity Mechanism – Acetylcholinesterase Inhibition. 2.1.2 Exposure. 2.1.3 Response, Treatment and Prevention. 2.2 Toxicity of Nerve Agent Degradation Products. 2.2.1 Toxicity of GA (Tabun) Degradation Products. 2.2.2 Toxicity of GB (Sarin) Degradation Products. 2.2.3 Toxicity of GD (Soman) Degradation Products. 2.2.4 Toxicity of GF (Cyclosarin) Degradation Products. 2.2.5 Toxicity of VX Degradation Products. 2.3 Toxicity of Blister Agents. 2.4 Toxicity of Sternutator Agents. 2.4.1 Toxicity of Degradation Products of Sternutator Agents. References. 3 Analysis of Chemical Warfare Agents. 3.1 Introduction. 3.2 Minimally Invasive Detection Techniques. 3.3 Separation and Detection Techniques. 3.3.1 Capillary Electrophoresis. 3.3.2 Ion Mobility Spectrometry. 3.3.3 Gas Chromatography (GC)/Gas Chromatography-Mass Spectrometry (GC-MS). 3.3.4 Liquid Chromatography (LC)/Liquid Chromatography-Mass Spectrometry (LC-MS). 3.3.5 Desorption Electrospray Ionization and Direct Analysis in Real Time Mass Spectrometry. References. 4 Chemical Warfare Agent Degradation Products. 4.1 Analysis of Nerve Agent Degradation Products. 4.1.1 Sample Preparation. 4.1.2 Liquid–Liquid Extraction (Pre-concentration). 4.1.3 Solid Phase Extraction (SPE). 4.1.4 Solid Phase Microextraction (SPME). 4.1.5 Stir Bar Sorptive Extraction (SBSE). 4.1.6 Derivatization. 4.2 Analytical Techniques. 4.2.1 Gas Chromatography (GC). 4.2.2 Liquid Chromatography (LC). 4.2.3 Elemental Speciation. 4.2.4 Ion Mobility. 4.2.5 Capillary Electrophoresis. 4.3 Analysis of Sulfur Mustard Degradation Products. 4.4 Analysis of Sternutator Degradation Products. References. Appendix. Index.

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Book Synopsis* Membrane-based separation is among the fastest growing methods for gas and vapor separations in a wide variety of applications * Includes approximately 24 contributions that cover all the aspects of contemporary membrane gas separation dealing with both fundamental results and applied achievements.Table of ContentsPreface. Contributors. I. Novel Membrane Materials and Transport in Them. 1 Synthesis and Gas Permeability of Hyperbranched and Cross-linked Polyimide Membranes (Shinji Kanehashi, Shuichi Sato and Kazukiyo Nagai). 1.1 Introduction. 1.2 Molecular Designs for Membranes. 1.3 Synthesis of Hyperbranched Polyimides. 1.4 Gas Permeation Properties. 1.5 Concluding Remarks. References. 2 Gas Permeation Parameters and Other Physicochemical Properties of a Polymer of Intrinsic Microporosity (PIM-1) (Peter M. Budd, Neil B. McKeown, Detlev Fritsch, Yuri Yampolskii and Victor Shantarovich). 2.1 Introduction. 2.2 The PIM concept. 2.3 Gas Adsorption. 2.4 Gas Permeation. 2.5 Inverse Gas Chromatography. 2.6 Positron Annihilation Lifetime Spectroscopy. 2.7 Conclusions. Acknowledgements. References. 3 Addition-type Polynorbornene with Si(CH3)3 Side Groups: Detailed Study of Gas Permeation, Free Volume and Thermodynamic Properties (Yuri Yampolskii, Ludmila Starannikova, Nikolai Belov, Maria Gringolts, Eugene Finkelshtein and Victor Shantarovich). 3.1 Introduction. 3.2 Experimental. 3.3 Results and Discussion. 3.4 Conclusions. References. 4 Amorphous Glassy Perfl uoropolymer Membranes of Hyfl on AD: Free Volume Distribution by Photochromic Probing and Vapour Transport Properties (Johannes Carolus Jansen, Karel Friess, Elena Tocci, Marialuigia Macchione, Luana De Lorenzo, Matthias Heuchel, Yuri P. Yampolskii and Enrico Drioli). 4.1 Introduction and Scope. 4.2 Membrane Preparation. 4.3 Free Volume Analysis. 4.4 Molecular Dynamics Simulations. 4.5 Transport Properties. 4.6 Correlation of Transport and Free Volume. 4.7 Conclusions. References. 5 Modelling Gas Separation in Porous Membranes (Aaron W. Thornton, James M. Hill and Anita J. Hilli). 5.1 Introduction. 5.2 Background. 5.3 Surface Diffusion. 5.4 Knudsen Diffusion. 5.5 Membranes: Porous Structures? 5.6 Transition State Theory (TST). 5.7 Transport Models for Ordered Pore Networks. 5.8 Pore Size, Shape and Composition. 5.9 The New Model. 5.10 Conclusion. List of Symbols. References. II. Nanocomposite (Mixed Matrix) Membranes. 6 Glassy Perfl uorolymer–Zeolite Hybrid Membranes for Gas Separations (Giovanni Golemme, Johannes Carolus Jansen, Daniela Muoio, Andrea Bruno, Raffaella Manes, Maria Giovanna Buonomenna, Jungkyu Choi and Michael Tsapatsis). 6.1 Introduction. 6.2 Materials and Methods. 6.3 Results and Discussion. 6.4 Conclusions. Acknowledgements. References. 7 Vapor Sorption and Diffusion in Mixed Matrices Based on Tefl on® AF 2400 (Maria Chiara Ferrari, Michele Galizia, Maria Grazia De Angelis and Giulio Cesare Sarti). 7.1 Introduction. 7.2 Theoretical Background. 7.3 Experimental. 7.4 Results and Discussion. 7.5 Conclusions. Acknowledgements. References. 8 Physical and Gas Transport Properties of Hyperbranched Polyimide–Silica Hybrid Membranes (Tomoyuki Suzuki, Yasuharu Yamada, Jun Sakai and Kumi Itahashi). 8.1 Introduction. 8.2 Experimental. 8.3 Results and Discussion. 8.4 Conclusions. References. 9 Air Enrichment by Polymeric Magnetic Membranes (Zbigniew J. Grzywna, Aleksandra Rybak and Anna Strzelewicz). 9.1 Introduction. 9.2 Formulation of the Problem. 9.3 Experimental. 9.4 Results and Discussion. 9.5 Conclusions. Acknowledgements. List of Symbols. References. III. Membrane Separation of CO2 from Gas Streams. 10 Ionic Liquid Membranes for Carbon Dioxide Separation (Christina R. Myers, David R. Luebke, Henry W. Pennline, Jeffery B. Ilconich and Shan Wickramanayake). 10.1 Introduction. 10.2 Experimental. 10.3 Results. 10.4 Discussion. 10.5 Conclusions. References. 11 The Effects of Minor Components on the Gas Separation Performance of Polymeric Membranes for Carbon Capture (Colin A. Scholes, Sandra E. Kentish and Geoff W. Stevens). 11.1 Introduction. 11.2 Sorption Theory for Multiple Gas Components. 11.3 Minor Components. 11.4 Conclusions. References. 12 Tailoring Polymeric Membrane Based on Segmented Block Copolymers for CO2 Separation (Anja Car, Wilfredo Yave, Klaus-Viktor Peinemann and Chrtomir Stropnik). 12.1 Introduction. 12.2 Tailoring Block Copolymers with Superior Performance. 12.3 Block Copolymers and their Blends with Polyethylene Glycol. 12.4 Composite Membranes. 12.5 Conclusions and Future Aspects. 13 CO2 Permeation with Pebax-based Membranes for Global Warming Reduction (Quang Trong Nguyen, Julie Sublet, Dominique Langevin, Corinne Chappey, Stéphane Marais, Jean-Marc Valleton and Fabienne Poncin-Epaillard). 13.1 Introduction. 13.2 Experimental. 13.3 Results and Discussions. 13.4 Conclusions. References. IV. Applied Aspects of Membrane Gas Separation. 14 Membrane Engineering: Progress and Potentialities in Gas Separations (Adele Brunetti, Paola Bernardo, Enrico Drioli and Giuseppe Barbieri). 14.1 Introduction. 14.2 Materials and Membranes Employed in GS. 14.3 Membranes Applications in GS. 14.4 New Metrics for Gas Separation Applications. 15 Evolution of Natural Gas Treatment with Membrane Systems (Lloyd S. White). 15.1 Introduction. 15.2 Market for Natural Gas Treatment. 15.3 Amine Treaters. 15.4 Contaminants and Membrane Performance. 15.5 Cellulose Acetate versus Polyimide. 15.6 Compaction in Gas Separations. 15.7 Experimental. 15.8 Laboratory Tests of Cellulose Acetate Membranes. 15.9 Field Trials of Cellulose Acetate Membranes. 15.10 Strategies for Reduced Size of Large-scale Membrane Systems. 15.11 Research Directions. 15.12 Summary. Acknowledgements. References. 16 The Effect of Sweep Uniformity on Gas Dehydration Module Performance (Pingjiao Hao and G. Glenn Lipscomb). 16.1 Introduction. 16.2 Theory. 16.3 Results and Discussion. 16.4 Conclusion. List of Symbols. References. Index.

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Book SynopsisOver the past two decades the benefits of label-free biosensor analysis have begun to make an impact in the market, and systems are beginning to be used as mainstream research tools in many drug discovery laboratories. Label-Free Technologies For Drug Discovery summarises the latest and emerging developments in label-free detection systems, their underlying technology principles and end-user case studies that reveal the power and limitations of label-free in all areas of drug discovery. Label-free technologies discussed include SPR, NMR, high-throughput mass spectrometry, resonant waveguide plate-based screening, transmitted-light imaging, isothermal titration calorimetry, optical and impedance cell-based assays and other biophysical methods. The technologies are discussed in relation to their use as screening technologies, high-content technologies, hit finding and hit validation strategies, mode of action and ADME/T, access to difficult target classes, cell-based reTrade Review"Label-Free Technologies For Drug Discovery summarises the latest and emerging developments in label-free detection systems, their underlying technology principles and end-user case studies that reveal the power and limitations of label-free in all areas of drug discovery." (Laboratory Journal, 10 March 2011)Table of ContentsPreface. List of Contributors. 1 The Revolution of Real-Time, Label-Free Biosensor Applications (Rebecca L. Rich and David G. Myszka). 2 Design and Implementation of Vertically Emitting Distributed Feedback Lasers for Biological Sensing (Meng Lu, Steven S. Choi, Chun Ge, Clark J. Wagner, J. Gary Eden, and Brian T. Cunningham). 2.1 Introduction. 2.2 DFB Laser Biosensor Design. 2.3 Fabrication and Instrumentation. 2.4 Experimental Results. 2.5 Conclusions. 3 SPR Screening of Chemical Microarrays for Fragment Based Discovery (Thomas Neumann and Renate Sekul). 3.1 Introduction. 3.2 Key Features of Fragment Screening. 3.3 SPR Fragment Screening. 3.4 Synthesis of Library Compounds. 3.5 Library Design and Array Content. 3.6 Chemical Microarray Production. 3.7 Surface Plasmon Resonance. 3.8 SPR Imaging. 3.9 Array Visualization and Analysis. 3.10 Follow-up. 3.11 Applications: MMP case study. 3.12 Search for New Binding Modes. 3.13 Selectivity Studies. 3.14 Other Target Classes. 3.15 Conclusions. 4 The CellKey System: A Label-Free Cell-Based Assay Platform for Early Drug Discovery Applications (Ryan P. McGuinness, Debra L. Gallant, Yen-Wen Chen, Trisha A. Tutana, Donna L. Wilson, John M. Proctor, H. Roger Tang). 4.1 Introduction. 4.2 Cellular Impedance Technology. 4.3 Target Identification and Validation. 4.4 Screening and Lead Optimization. 4.5 Conclusion. 5 Dynamic and Label-Free Cell-Based Assays using the xCELLigence System (Yama A. Abassi, Alexander Sieler, Manfred Watzele, Xiaobo Wang and Xiao Xu). 5.1 Introduction. 5.2 The xCELLigence system. 5.3 Principle of Detection. 5.4 Applications. 5.5 Functional Assays for G Protein-Coupled Receptors. 5.6 Conclusion. 6 Selecting the Best HTS Hits to Move Forward: ITC Ligand Binding Characterization Provides Guidance (Ronan O'Brien & Richard Brown). 6.1 Introduction. 6.2 Principles of Isothermal Titration Calorimetry (ITC). 6.3 Applications of ITC in Hit Validation. 6.4 Applications of ITC in Fragment-Based Drug Discovery. 6.5 Applications of ITC in Mechanism of Action Studies. 6.6 Applications of ITC in Lead Optimization. 6.7 ITC as an Enzyme Activity Monitor. 6.8 Conclusion. 7 Incorporating Transmitted Light Modalities into High-Content Analysis Assays (Robert Graves). 7.1 Introduction. 7.2 Transmitted Light (Bright Field) Imaging. 7.3 Image Analysis of Phase Contrast Images. 7.4 Conclusion. 8 Nonradioactive Rubidium Efflux Assay Technology for Screening of Ion Channels (Georg C. Terstappen). 8.1 Introduction. 8.2 Ion Channels as Drug Targets. 8.3 Ion Channel Assays and Screening. 8.4 Nonradioactive Rubidium Efflux Assay Based on Atomic Absorption Spectrometry. 8.5 A Typical Assay Protocol. 8.6 Conclusions. 9 Expanding the Scope of HTMS Methods (Tom G. Holt, Jun Wang, Xun Chen, Bernard K. Choi, Neil S. Geoghagen, Kristian K. Jensen, Maxine Jonas, Qi Luo, William A. LaMarr, Lorraine Malkowitz, Can C. Ozbal, Yusheng Xiong, Claude Dufresne, Ming-Juan Luo). 9.1 Introduction. 9.2 Development of Htms Method for Underivatized Cystathionine in Biological Samples Spanning In Vitro, Cell Culture, and Ex Vivo Assays. 9.3 Development of 2D HTMS Method for Plasma-Bound Small Molecules. 9.4 Conclusion. 10 A Novel Multiplex SPR Array for Rapid Screening and Affinity Determination of Monoclonal Antibodies: The ProteOn XPR36 Label Free System: Kinetic Screening of Monoclonal Antibodies (Vered Bronner, Oded Nahshol and Tsafrir Bravman). 10.1 Introduction. 10.2 Optimized Assay Configuration. 10.3 Selection of the Optimal Capture Agent. 10.4 Kinetic Analysis of 192 Human Anti-Il-12 Supernatants. 10.5 Kinetic Analysis of 243 Human Hemoglobin Supernatants. 10.6 Conclusions. 11 Biophysics/Label-Free Assays in Hit Discovery and Verification (Johannes Ottl). 11.1 Introduction. 11.2 Why biophysics? 11.3 Biophysics/Label-Free Toolbox. 11.4 Which Biophysical Measurement at Which Stage of a Drug Discovery Project Flowchart? 11.5 Conclusion. 11.6 Outlook. 12 Harnessing Optical Label-free on Microtiter Plates for Lead Finding From Binding to Phenotypes (Julio Martin). 12.1 Introduction. 12.2 Value Proposition and Advantages Of Label-Free Methodologies. 12.3 Detection Principle of an Optical Label-Free Resonant Grating Sensor. 12.4 Biological Applications of Optical Label-Free In Lead Discovery. 12.5 Current and Future Challenges. 12.6 Conclusion. 13 Use of Label-Free Detection Technologies in the Hit-to-Lead Process: Surface Optical Detection of Cellular Processes (F. Stuhmeier, J. Bradley, E. Fairman, E. Gbekor, P. Hayter, S. Ramsey). 13.1 Introduction. 13.2 Overview of Label-Free Assay Platforms. 13.3 Surface Optical Detection of Cellular Processes. 13.4 Discussion. 14 Cellular Screening for 7TMs Using Label-Free Detection (Jeffrey C. Jerman, Jason Brown and Magalie Rocheville). 14.1 Introduction. 14.2 Results and Discussion. 14.3 Conclusions and Perspective. 14.4 Materials and Methods. 14.5 Acknowledgements. 15 Novartis Evaluation of the ForteBio Octet RED: A Versatile Instrument for Direct-Binding Experiments (Eric Martin, John Wang, Isabel Zaror, Jiamin Yu, Kelly Yan, Mike Doyle, Paul Feucht, Kevin Shoemaker, Bob Warne, Mike Chin, Blisseth Sy, Lukas Leder, Marco Meyerhofer, Charles Wartchow, Danfeng Yao). 15.1 Introduction. 15.2 Methods. 15.3 Results and Discussion. 15.4 Conclusion. 16 The Pyramid Approach to Fragment-Based Biophysical Screening (Glyn Williams). 16.1 Introduction. 16.2 Summary and Conclusions. 16.3 Acknowledgements. 17 Characterisation of Antibodies Against the Active Conformation of Gαi1 Using the SRU-BIND­® Label-Free Detection System (Melanie Leveridge, Chun-Wa Chung and Trevor Wattam). 17.1 Introduction. 17.2 Materials and Methods. 17.3 Results and Discussion. 17.4 Conclusions. 17.5 Acknowledgements. 18 SPR Based Direct Binding Assays in Drug Discovery (Walter Huber). 18.1 Introduction. 18.2 Screening Using SPR-Based Direct Binding Assay. 18.3 Lead Selection using SPR Based Binding Assay. 18.4 Conclusion. 18.5 Acknowledgements. 19 Kinetic Binding Mechanisms: Their Contribution to an Optimal Therapeutic Index (David C. Swinney). 19.1 Introduction. 19.2 Why are Binding Mechanisms and Kinetics Important to Drug Action? 19.3 How Can Kinetics Contribute to an Optimal Mechanism? 19.4 Binding Kinetics Differentiate Physiological Responses. 19.5 Utilization of Binding Kinetics in Drug Discovery. How to get Maximum Value out of Kinetic Analysis? 19.6 Conclusion. 20 ITC: More Than Just Binding Affinities (Ernesto Freire). 20.1 Introduction. 20.2 Why should We Care About Enthalpy and Entropy? 20.3 Conclusion. Acknowledgements. Index.

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Book SynopsisEnergy production and storage are central problems for our time. In principle, abundant energy is available from the sun to run the earth in a sustainable way. Solar energy can be directly harnessed by agricultural and photovoltaic means, but the sheer scale of the energy demand poses severe challenges, for example any major competition between biomass production and food production would simply transfer scarcity from energy to food. Indirect use of solar energy in the form of wind looks also promising, especially for those regions not blessed with abundant sunlight. Other modes such as tidal and wave energy may well become important niche players. Inorganic chemistry plays a decisive role in the development of new energy technologies and this Volume covers some promising modes of alternative energy production and storage that minimize the atmospheric burden of fossil-derived carbon monoxide. No one production or storage mode is likely to dominate, at least at first, and numerous Trade Review"The breadth of subjects covered is both the strength and weakness of this book. There are very few scientists who will have interest across the range of topics covered. At the same time, these reviews are written for the very knowledgeable reader." (Chemistry World, 1 April 2011) Table of ContentsContributors. Series Preface. Volume Preface. PART 1: ENERGY PRODUCTION. H2 Production from Renewables (Rufino M. Navarro, M. Cruz Sanchez-Sanchez, M. Consuelo Alvarez-Galvan, Jose Luis G. Fierro and Saeed M. Al-Zaharani). Energy Conversion in Photosynthesis (Gozde Ulas and Gary W. Brudvig). Molecular Catalysts for Oxygen Production from Water (Antoni Llobet and Sophie Romain). Dye-Sensitized Solar Cells: an Overview (Luisa Andrade, Helena Aguilar Ribeiro and Adelio Mendes). Enzymes and Microbes for Energy Production by Fuel Cells (Frederic Barriere). Proton Exchange Membranes for Fuel Cells (Ram Devanathan). Methane-to-Methanol Conversion (Brian G. Hashiguchi, Claas H. H¨ovelmann, Steven M. Bischof, Kapil S. Lokare, Chin Hin Leung and Roy A. Periana). Photocatalytic Hydrogen Production from Water (Shamindri M. Arachchige and Karen J. Brewer). Intermediate-Temperature Solid Oxide Fuel Cells (Alan Atkinson, John Kilner, Stephen Skinner, Nigel P. Brandon and Dan J. L. Brett). Some Computational Challenges in Energy Research (Victor S. Batista). Toward Solar Fuels Using a Biomimetic Approach: Progress in the Swedish Consortium for Artificial Photosynthesis (Sascha Ott, Stenbj¨orn Styring, Leif Hammarstr¨om and Olof Johansson). Direct Ethanol Fuel Cells (Zhi Wen Chia and Jim Yang Lee). Molecular Catalysis for Fuel Cells (Kenichi Oyaizu). Recent Advances in Photo-Initiated Electron-Transfer at the Interface between Anatase TiO2 Nanocrystallites and Transition-Metal Polypyridyl Compounds (Shane Ardo and Gerald J. Meyer). Electrochemical and Photoelectrochemical Conversion of CO2 to Alcohols (Robert H. Crabtree). PART 2: ENERGY STORAGE. Hydrogen Economy (Stephen A. Wells, Asel Sartbaeva, Vladimir L. Kuznetsov and Peter P. Edwards). Thermal Stability of Lithium Ion Battery Electrolytes (Brett L. Lucht, Tippawan Markmaitree and Li Yang). Supercapacitors: Electrode Materials Aspects (Li Li Zhang, Zhibin Lei, Jintao Zhang, Xiaoning Tian and Xiu Song Zhao). Thermochemical Water-Splitting (Ali T-Raissi). Lithium Ion Batteries for Transportation and Electrical Energy Storage Applications: Nuclear Magnetic Resonance Studies of Structure and Function (Jordi Cabana and Clare P. Grey). Index.

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Book SynopsisStandards, technologies, and requirements for computer validation have changed dramatically in recent years, and so have the interpretation of the standards and the understanding of the processes involved. International IT Regulations and Compliance brings together current thinking on the implementation of standards and regulations in relation to IT for a wide variety of industries. The book provides professionals in pharmaceutical and semiconductor industries with an updated overview of requirements for handling IT systems according to various Quality Standards and how to ?translate? these requirements in the regulations.Trade Review“This book is a good reference for everyone dealing with IT systems in a regulated environment. The style and content are targeted to entry- and middle-level professionals. The author provides readers with a broad picture and strong overall understanding of IT systems.” (Pharmaceutical Technology, June 2009)Table of ContentsPreface and Acknowledgements. 1. Quality Standards. 1.1 What Quality is. 1.2 Mandatory and Voluntary Standards. 1.3 Pharmaceutical Industry Regulations. 1.4 US GXP Regulations. 1.5 European GXP Regulations. 1.6 Other GXP Regulations. 1.7 Good Manufacturing Practice - GMP. 1.8 Good Laboratory Practice - GLP. 1.9 Good Clinical Practice - GCP. 1.10 Medical Device Standards. 1.11 It Systems in The GXP And Medical Device Regulations. 1.12 GAMP. 1.13 Mandatory Quality Standards in Other Industries. 1.14 Legal Issues. 1.15 ISO. 1.16 ASTM. 1.17 IEEE. 1.18 TASKS. 2. Regulatory Requirements for IT Systems. 2.1 Introduction. 2.2 US Requirements. 2.3 EU Requirements. 2.4 21 CFR Part 11. 2.5 The "Part 11 Project". 2.6 EU GMP Annex 11. 2.7 PIC Document PI 011 Recommendation on Computerised Systems In Regulated "GXP" Environments. 2.8 GAMP. 2.9 ISO 9000-Series. 2.10 Comparison Between the Standards. 2.11 Conclusion. 2.12 Tasks. 3. IT Security. 3.1 Introduction. 3.2 Continuous Connections - Wireless Networks. 3.3 Threats. 3.4 Security Policy. 3.5 Tasks. 4. Quality Management Systems. 4.1 Introduction to QMS. 4.2 Definitions. 4.3 Principles for Quality Management. 4.4 Quality Management System Levels. 4.5 Creating a QMS. 4.6 Roles and Responsibilities. 4.7 Work Processes. 4.8 Controlled Documents. 4.9 Quality Policy--QP. 4.10 Quality Manual--QM. 4.11 Standard Operating Procedures. 4.12 The Art of Writing an SOP. 4.13 Tasks. 5. IT Integrated In the QMS in a User Organization. 5.1 Introduction. 5.2 How to Integrate the IT Systems in the QMS. 5.3 Generic Standard Operating Procedures (SOPS). 5.4 Procedures for Each System. 5.5 Tasks. 6. IT Integrated in the Supplier’s QMS. 6.1 Introduction. 6.2 Which Standards to Use? 6.3 Quality Management System. 6.4 System Development Models. 6.5 Documents for the Software Development. 6.6 Customer-Supplier Relationship. 6.7 Tasks. 7. Organization for an IT System. 7.1 Introduction. 7.2 Roles and Responsibilities for a Live System. 7.3 Groups in the IT System Organization. 7.4 Roles and Responsibilities for an IT Validation Project. 7.5 Outsourcing. 1.1 Service Level Agreement for Outsourcing. 7.6 Consultants. 8. The Legal Implications of an IT System. 8.1 Introduction. 8.2 Pharmaceutical Regulations. 8.3 Financial Systems. 8.4 Patent Systems. 8.5 Human Resource (HR) Systems. 8.6 Healthcare Systems. 8.7 Systems for Legal Information. 9. Advanced Quality Management Systems. 9.1 Introduction. 9.2 The Live QMS is a Good QMS. 9.3 Changes. 9.4 How to Keep the QMS Updated. 9.5 Training and Understanding. 9.6 How to Use A QMS Effectively As A Tool In The Organization - Not As a Straightjacket. 9.7 Tasks. 10. Audits. 10.1 Introduction. 10.2 ISO 9000 Series. 10.3 Tickit. 10.4 Why Audit? 10.5 Audit In A Risk-Based Environment. 10.6 Audit Scope. 10.7 Supplier Audit Preparations. 10.8 During the Audit. 10.9 What To Look For. 10.10 Other Issues. 10.11 Findings/Discrepancies. 10.12 Closing Meeting/Wash-Up Meeting. 10.13 Audit Report. 10.14 Conducting an Audit from the Receiving End Of The Table. 10.15 Tasks. 11. Validation of IT Systems. 11.1 Introduction. 11.2 External Requirements for Validation. 11.3 Internal Requirements for Validation. 11.4 Validation Cost. 11.5 Inspectors. 11.6 Validation Scope Is Changing. 11.7 Computer Validation Project. 11.8 Which Hardware and Software Shall Be Validated. 11.9 Network. 11.10 Software. 11.11 Risks and System Categories. 11.12 Qualifications. 11.13 DQ - Development Qualification. 11.14 IQ - Installation Qualification. 11.15 OQ - Operation Qualification. 11.16 PQ - Performance / Process Qualification. 11.17 Validation Master Plan VMP. 11.18 Validation Plan VP. 11.19 Validation Report. 11.20 Tasks. 12. Risk Assessment and Risk Management. 12.1 Introduction. 12.2 Addressing Risks. 12.3 Risk Assessment Tools. 12.4 Risk Assessment. 12.5 Risk Management. 12.6 Tasks. 13. Development Qualification. 13.1 Introduction. 13.2 User’s Point Of View. 13.3 Supplier’s Point of View. 13.4 Project: The New System in the User Organization. 13.5 The Four Assessments of System Selection. 13.6 Functional Specification and System Implementation. 13.7 Tasks. 14. Installation Qualification. 14.1 Introduction. 14.2 IQ Organizational Issues. 14.3 IQ Plan. 14.4 IQ Testing. 14.5 IQ Report. 14.6 Tasks. 15. Operational Qualification. 15.1 Introduction. 15.2 OQ Framework. 15.3 What If The Supplier Has Done OQ? 15.4 OQ Plan. 15.5 OQ Testing. 15.6 Documentation of the Testing. 15.7 OQ Report. 15.8 Tasks. 16. Process/Performance Qualification. 16.1 Introduction. 16.2 PQ Plan. 16.3 PQ Test Plans. 16.4 Documentation During the Testing. 16.5 PQ Report. 16.6 Ongoing PQ. 16.7 Tasks. 17. Laboratory Instrument Systems. 17.1 Introduction. 17.2 Instruments. 17.3 Analytical Instruments in the Laboratory. 17.4 Raw Data and Meta Data. 17.5 Devices. 17.6 Biometric Devices. 17.7 Electronic Lab Notebooks ELN. 17.8 Validation of Computerized Instrument Systems. 17.9 Pure Computer Systems. 17.10 Computerized Instruments That Can Run ‘Barefoot’. 17.11 Integrated Computerized Instruments. 17.12 Qualification of Laboratory Instruments. 18. Laboratory Information Management Systems. 18.1 Introduction. 18.2 Build or Buy a New LIMS? 18.3 The Real Cost Of LIMS. 18.4 Differences Between Commercial LIMS Systems. 18.5 Static and Dynamic Data. 18.6 Static Data. 18.7 Dynamic Data. 18.8 LIMS Functionality. 18.9 Types of Production. 18.10 Analytical Methods. 18.11 Calculations in Analytical Methods. 18.12 Specifications and Limits. 18.13 Standards, Solutions and Chemicals Used In the Lab. 18.14 Instrument Connections and Definitions. 18.15 Instrument Information. 18.16 Do We Store The Data In The Instrument System Or In LIMS? 18.17 Stability Studies and Stability Testing. 18.18 Pharmacokinetic Studies and Testing. 18.19 Dissolution Testing. 18.20 Patients/Animals Information. 18.21 Customer Information. 18.22 Bar Coded Labels. 18.23 RFID. 18.24 Chain of Custody. 18.25 Sample Scheduling and Workload. 18.26 Status. 18.27 Security. 18.28 Specifying and Choosing the New LIMS. 18.29 Trace Matrix. 18.30 List of Sops for a LIMS. 18.31 Tasks. 18.32 Further Reading. 19. Building Management System (BMS) and Heating, Ventilation, Air Conditioning. 19.1 Introduction. 19.2 BMS Systems. 19.3 PLC. 19.4 SCADA. 19.5 Control Parameters and Instrumentation. 19.6 Sterile Facilities. 19.7 Regulatory Requirements and Validation Enforcement. 19.8 Validation of Old HVAC / BMS Systems. 19.9 New Systems. 19.10 Risk Assessment. 19.11 Electronic Records in the BMS. 19.12 Validation. 19.13 IQ. 19.14 OQ/PQ. 19.15 Standard Operating Procedures. 19.16 Tasks. Appendix 1 Regulation comparisons. Appendix 2 Terminology. Index.

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Book SynopsisThis workbook accompanies Organic Synthesis: Strategy and Control , the bestselling advanced organic chemistry textbook. The workbook provides a complete course for advanced organic chemistry students and includes a graded set of problems, solutions, and discussions to illustrate and develop the themes of each of the chapters in the textbook.Trade Review?This is a must-read for any final year undergrad or PhD? student in organic chemistry, but it's more than that?it's a book for experienced chemists too.? (Reviews, May 2009)Table of ContentsPreface vii A: Introduction: Selectivity 1 1. Planning Organic Syntheses: Tactics, Strategy and Control 3 2. Chemoselectivity 7 3. Regioselectivity: Controlled Aldol Reactions 19 4. Stereoselectivity: Stereoselective Aldol Reactions 35 5. Alternative Strategies for Enone Synthesis 47 6. Choosing a Strategy: The Synthesis of Cyclopentenones 57 B: Making Carbon–Carbon Bonds 69 7. The Ortho Strategy for Aromatic Compounds 71 8. σ-Complexes of Metals 91 9. Controlling the Michael Reaction 103 10. Specific Enol Equivalents 115 11. Extended Enolates 123 12. Allyl Anions 135 13. Homoenolates 147 14. Acyl Anion Equivalents 155 C: Carbon–Carbon Double Bonds 169 15. Synthesis of Double Bonds of Defined Stereochemistry 171 16. Vinyl Anions 191 17. Electrophilic Attack on Alkenes 203 18. Vinyl Cations 221 19. Allyl Alcohols: Allyl Cation Equivalents (and More) 241 D: Stereochemistry 257 20. Control of Stereochemistry–Introduction 259 21. Diastereoselectivity 269 22. Resolution 283 23. The Chiral Pool: Asymmetric Synthesis with Natural Products as Starting Materials 295 24. Asymmetric Induction I: Reagent-Based Strategy 309 25. Asymmetric Induction II: Asymmetric Catalysis: Formation of C–O and C–N Bonds 321 26. Asymmetric Induction III: Asymmetric Catalysis: Formation of C–H and C–C Bonds 335 27. Asymmetric Induction IV: Substrate-Based Strategy 351 28. Kinetic Resolution 365 29. Enzymes: Biological Methods in Asymmetric Synthesis 377 30. New Chiral Centres from Old: Enantiomerically Pure Compounds and Sophisticated Syntheses 391 31. Strategy of Asymmetric Synthesis 405 E: Functional Group Strategy 417 32. Functionalisation of Pyridine 419 33. Oxidation of Aromatic Rings and of Enol(ate)s 433 34. Functionality and Pericyclic Reactions: Nitrogen Heterocycles by Cycloadditions and Sigmatropic Rearrangements 447 35. Synthesis and Chemistry of Azoles and other Heterocycles with Two or more Heteroatoms 459 36. Tandem Organic Reactions 473 Index 483

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Book SynopsisSurfacants from Renewable Resources is a comprehensive text that meets scientists' demand for information on new biodegradable surfacants with safer properties for modern industrial formulations. This edited volume explores the current status of the research and applications of "green" surfactant chemistry.Trade Review"The book is highly concentrated on technical aspects with big expertise in the different production technologies, it aims to be used as a chemical and technical reference for industrial and academic researchers in this field." (Encyclopedia of Industrial Biotechnology, 30 August 2011)Table of ContentsSeries Preface xi Preface xiii Acknowledgements xvii List of Contributors xix Part 1 Renewable Hydrophobes 1 1 Surfactants Based on Natural Fatty Acids 3 Martin Svensson 1.1 Introduction and History 3 1.2 Fats and Oils as Raw Materials 4 1.3 Fatty Acid Soaps 5 1.4 Polyethylene Glycol Fatty Acid Esters 10 1.5 Polyglycerol Fatty Acid Esters 11 1.6 Conclusions 13 References 15 2 Nitrogen Derivatives of Natural Fats and Oils 21 Ralph Franklin 2.1 Introduction 21 2.2 Manufacture of Fatty Nitrogen Derivatives 22 2.3 Production Data 30 2.4 Ecological Aspects 30 2.5 Biodegradation 31 2.6 Properties of Nitrogen-Based Surfactants 33 2.7 Applications 35 2.8 Conclusions 39 References 40 3 Surface-Active Compounds as Forest-Industry By-Products 45 Bjarne Holmbom, Anna Sundberg and Anders Strand 3.1 Introduction 45 3.2 Resin and Fatty Acids 46 3.3 Sterols and Sterol Ethoxylates 54 3.4 Hemicelluloses 56 Acknowledgements 58 References 59 Part 2 Renewable Hydrophiles 63 4 Surfactants Based on Carbohydrates and Proteins for Consumer Products and Technical Applications 65 Karlheinz Hill 4.1 Introduction 65 4.2 Raw Materials 65 4.3 Products and Applications 67 4.4 Conclusion 81 Acknowledgements 81 References 81 5 Amino Acids, Lactic Acid and Ascorbic Acid as Raw Materials for Biocompatible Surfactants 85 Carmen Moran, Lourdes Perez, Ramon Pons, Aurora Pinazo and Maria Rosa Infante 5.1 Introduction 85 5.2 Production of Raw Materials 86 5.3 Lysine-Based Surfactants 87 5.4 Lactic Acid-Based Surfactants 94 5.5 Ascorbic Acid-Based Surfactants 97 References 100 Part 3 New Ways of Making Renewable Building Blocks 109 6 Ethylene from Renewable Resources 111 Anna Lundgren and Thomas Hjertberg 6.1 Introduction 111 6.2 Why Produce Ethylene from Renewable Resources? 113 6.3 Production of Ethylene from Renewable Feedstock 115 6.4 Commercialization of Bioethylene 121 6.5 Environmental Impact of Bioethylene 123 6.6 Certificate of Green Carbon Content 124 6.7 Concluding Remarks 125 References 125 7 Fermentation-Based Building Blocks for Renewable Resource-Based Surfactants 127 Kris Arvid Berglund, Ulrika Rova and David B. Hodge 7.1 Introduction 127 7.2 Existing and Potential Classes of Surfactants from Biologically Derived Metabolites 129 7.3 Fermentation-Based Building Blocks with Large Existing Markets 131 7.4 New Fermentation-Based Building Blocks 133 7.5 Conclusion 138 References 138 Part 4 Biosurfactants 143 8 Synthesis of Surfactants Using Enzymes 145 Patrick Adlercreutz and Rajni Hatti-Kaul 8.1 Introduction 145 8.2 Enzymes as Catalysts for Synthesis of Surfactants 146 8.3 Enzymatic Synthesis of Polar Lipids Useful as Surfactants 147 8.4 Carbohydrate Esters 148 8.5 Fatty Amide Surfactants 151 8.6 Amino Acid-Based Surfactants 155 8.7 Alkyl Glycosides 158 8.8 Future Prospects 160 Acknowledgements 161 References 161 9 Surfactants from Waste Biomass 167 Flor Yunuen García-Becerra, David Grant Allen and Edgar Joel Acosta 9.1 Introduction 167 9.2 Surfactants Obtained from Biological Transformation of Waste Biomass 168 9.3 Surfactants Obtained from Chemical Transformation of Waste Biomass 177 9.4 Summary and Outlook 185 References 185 10 Lecithin and Other Phospholipids 191 Willem van Nieuwenhuyzen 10.1 Introduction 191 10.2 Sources and Production 191 10.3 Composition 195 10.4 Quality and Analysis of Lecithins 196 10.5 Modification 198 10.6 Emulsifying Properties 203 10.7 Applications 206 10.8 Legislation and Reach 209 10.9 Conclusion 211 References 211 11 Sophorolipids and Rhamnolipids 213 Dirk W. G. Develter and Steve J. J. Fleurackers 11.1 Sophorolipids 213 11.2 Derivatives of Native Sophorolipids 224 11.3 Biosynthesis of Novel Sophorolipids 227 11.4 Rhamnolipids 230 11.5 Cleaning Applications Using Sophorolipids and Rhamnolipids 234 References 236 12 Saponin-Based Surfactants 239 Wieslaw Oleszek and Arafa Hamed 12.1 Introduction 239 12.2 Molecular Properties 240 12.3 Sources of Saponins 242 12.4 Saponins as Emulsifiers and Surfactants 242 12.5 Application of Saponins as Surfactants and Emulsifiers 245 Acknowledgements 248 References 248 Part 5 Polymeric Surfactants/Surface-Active Polymers 251 13 Surface-Active Polymers from Cellulose 253 Leif Karlson 13.1 Introduction 253 13.2 Structure and Synthesis of Cellulose Ether 254 13.3 Cellulose Ethers in Aqueous Solution 257 13.4 Interaction with Surfactants 262 13.5 Clouding 263 References 265 14 New Developments in the Commercial Utilization of Lignosulfonates 269 Rolf Andreas Lauten, Bernt O. Myrvold and Stig Are Gundersen 14.1 Introduction 269 14.2 Lignosulfonates 269 14.3 Lignosulfonate Production 271 14.4 Environmental Issues 272 14.5 Lignosulfonates as Stabilizers for Emulsions and Suspoemulsions 274 14.6 Superplasticizers for Concrete 279 14.7 Summary 280 Acknowledgements 281 References 281 15 Dispersion Stabilizers Based on Inulin 285 Tharwat Tadros and Bart Levecke 15.1 Introduction 285 15.2 Solution Properties of Long-Chain Inulin and Hydrophobically Modified Inulin (HMI) 288 15.3 Interfacial Aspects of HMI at Various Interfaces 289 15.4 Emulsions Stabilized Using HMI 290 15.5 Emulsion Polymerization Using HMI 293 15.6 Use of HMI for Preparation and Stabilization of Nanoemulsions 295 References 300 Index 303

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Book SynopsisThis book provides a comprehensive and up-to-date picture of sludge minimization and reuse with a focus on process fundamentals, feasibility, and cost evaluation.Table of ContentsPreface xvii Contributors xxi 1 Fundamentals of Biological Processes for Wastewater Treatment 1 Jianlong Wang 1.1 Introduction, 1 1.2 Overview of Biological Wastewater Treatment, 2 1.2.1 The Objective of Biological Wastewater Treatment, 2 1.2.2 Roles of Microorganisms in Wastewater Treatment, 3 1.2.3 Types of Biological Wastewater Treatment Processes, 4 1.3 Classification of Microorganisms, 4 1.3.1 By the Sources of Carbon and Energy, 4 1.3.2 By Temperature Range, 6 1.3.3 Microorganism Types in Biological Wastewater Treatment, 7 1.4 Some Important Microorganisms in Wastewater Treatment, 8 1.4.1 Bacteria, 8 1.4.2 Fungi, 12 1.4.3 Algae, 15 1.4.4 Protozoans, 16 1.4.5 Rotifers and Crustaceans, 18 1.4.6 Viruses, 20 1.5 Measurement of Microbial Biomass, 21 1.5.1 Total Number of Microbial Cells, 21 1.5.2 Measurement of Viable Microbes on Solid Growth Media, 22 1.5.3 Measurement of Active Cells in Environmental Samples, 23 1.5.4 Determination of Cellular Biochemical Compounds, 24 1.5.5 Evaluation of Microbial Biodiversity by Molecular Techniques, 24 1.6 Microbial Nutrition, 24 1.6.1 Microbial Chemical Composition, 25 1.6.2 Macronutrients, 27 1.6.3 Micronutrients, 28 1.6.4 Growth Factor, 29 1.6.5 Microbial Empirical Formula, 31 1.7 Microbial Metabolism, 31 1.7.1 Catabolic Metabolic Pathways, 32 1.7.2 Anabolic Metabolic Pathway, 38 1.7.3 Biomass Synthesis Yields, 39 1.7.4 Coupling Energy-Synthesis Metabolism, 41 1.8 Functions of Biological Wastewater Treatment, 42 1.8.1 Aerobic Biological Oxidation, 42 1.8.2 Biological Nutrients Removal, 45 1.8.3 Anaerobic Biological Oxidation, 50 1.8.4 Biological Removal of Toxic Organic Compounds and Heavy Metals, 55 1.8.5 Removal of Pathogens and Parasites, 58 1.9 Activated Sludge Process, 59 1.9.1 Basic Process, 60 1.9.2 Microbiology of Activated Sludge, 61 1.9.3 Biochemistry of Activated Sludge, 66 1.9.4 Main Problems in the Activated Sludge Process, 67 1.10 Suspended- and Attached-Growth Processes, 69 1.10.1 Suspended-Growth Processes, 69 1.10.2 Attached-Growth Processes, 70 1.10.3 Hybrid Systems, 71 1.10.4 Comparison Between Suspended- and Attached-Growth Systems, 72 1.11 Sludge Production, Treatment and Disposal, 74 1.11.1 Sludge Production, 74 1.11.2 Sludge Treatment Processes, 76 1.11.3 Sludge Disposal and Application, 78 References, 79 2 Sludge Production: Quantification and Prediction for Urban Treatment Plants and Assessment of Strategies for Sludge Reduction 81 Mathieu Spe´randio, Etienne Paul, Yolaine Bessie`re, and Yu Liu 2.1 Introduction, 81 2.2 Sludge Fractionation and Origin, 82 2.2.1 Sludge Composition, 82 2.2.2 Wastewater Characteristics, 83 2.3 Quantification of Excess Sludge Production, 88 2.3.1 Primary Treatment, 88 2.3.2 Activated Sludge Process, 90 2.3.3 Phosphorus Removal (Biological and Physicochemical), 97 2.4 Practical Evaluation of Sludge Production, 99 2.4.1 Sludge Production Yield Variability with Domestic Wastewater, 99 2.4.2 Influence of Sludge Age: Experimental Data Versus Models, 100 2.4.3 ISS Entrapment in the Sludge, 103 2.4.4 Example of Sludge Production for a Different Case Study, 104 2.5 Strategies for Excess Sludge Reduction, 106 2.5.1 Classification of Strategies, 106 2.5.2 Increasing the Sludge Age, 107 2.5.3 Model-Based Evaluation of Advanced ESR Strategies, 109 2.6 Conclusions, 111 2.7 Nomenclature, 112 References, 114 3 Characterization of Municipal Wastewater and Sludge 117 Etienne Paul, Xavier Lefebvre, Mathieu Sperandio, Dominique Lefebvre, and Yu Liu 3.1 Introduction, 117 3.2 Definitions, 119 3.3 Wastewater and Sludge Composition and Fractionation, 120 3.3.1 Wastewater COD Fractions, 121 3.3.2 WAS COD Fractions, 122 3.3.3 ADS Organic Fractions, 122 3.4 Physical Fractionation, 123 3.4.1 Physical State of Wastewater Organic Matter, 123 3.4.2 Methods for Physical Fractionation of Wastewater Components, 123 3.5 Biodegradation Assays for Wastewater and Sludge Characterization, 124 3.5.1 Background, 124 3.5.2 Methods Based on Substrate Depletion, 125 3.5.3 Methods Based on Respirometry, 125 3.5.4 Anaerobic Biodegradation Assays, 128 3.6 Application to Wastewater COD Fractionation, 131 3.6.1 Global Picture of Fractionation Methods and Wastewater COD Fractions, 131 3.6.2 Application of Physical Separation for Characterization of Wastewater COD Fractions, 132 3.6.3 Biodegradable COD Fraction, 133 3.6.4 Relation Between Physical and Biological Properties of Organic Fractions, 136 3.6.5 Unbiodegradable Particulate COD Fractions, 137 3.7 Assessment of the Characteristics of Sludge and Disintegrated Sludge, 143 3.7.1 Physical Fractionation of COD Released from Sludge Disintegration Treatment, 143 3.7.2 Biological Fractionation of COD Released from Sludge Disintegration Treatment, 145 3.7.3 Biodegradability of WAS in Anaerobic Digestion, 145 3.7.4 Unbiodegradable COD in Anaerobic Digestion, 146 3.8 Nomenclature, 147 References, 149 4 Oxic-Settling-Anaerobic Process for Enhanced Microbial Decay 155 Qingliang Zhao and Jianfang Wang 4.1 Introduction, 155 4.2 Description of the Oxic-Settling-Anaerobic Process, 156 4.2.1 Oxic-Settling-Anaerobic Process, 156 4.2.2 Characteristics of the OSA Process, 157 4.3 Effects of an Anaerobic Sludge Tank on the Performance of an OSA System, 158 4.3.1 Fate of Sludge Anaerobic Exposure in an OSA System, 158 4.3.2 Effect of Sludge Anaerobic Exposure on Biomass Activity, 160 4.4 Sludge Production in an OSA System, 161 4.5 Performance of an OSA System, 162 4.5.1 Organic and Nutrient Removal, 162 4.5.2 Sludge Settleability, 163 4.6 Important Influence Factors, 164 4.6.1 Influence of the ORP on Sludge Production, 164 4.6.2 Influence of the ORP on Performance of an OSA System, 164 4.6.3 Influence of SAET on Sludge Production, 166 4.6.4 Influence of SAET on the Performance of an OSA System, 166 4.7 Possible Sludge Reduction in the OSA Process, 166 4.7.1 Slow Growers, 167 4.7.2 Energy Uncoupling Metabolism, 167 4.7.3 Sludge Endogenous Decay, 169 4.8 Microbial Community in an OSA System, 171 4.8.1 Staining Analysis, 172 4.8.2 FISH Analysis, 173 4.9 Cost and Energy Evaluation, 174 4.10 Evaluation of the OSA Process, 175 4.11 Process Development, 176 4.11.1 Sludge Decay Combined with Other Sludge Reduction Mechanisms, 176 4.11.2 Improved Efficiency in Sludge Anaerobic Digestion, 177 4.11.3 Combined Minimization of Excess Sludge with Nutrient Removal, 178 References, 179 5 Energy Uncoupling for Sludge Minimization: Pros and Cons 183 Bo Jiang, Yu Liu, and Etienne Paul 5.1 Introduction, 183 5.2 Overview of Adenosine Triphosphate Synthesis, 184 5.2.1 Electron Transport System, 184 5.2.2 Mechanisms of Oxidative Phosphorylation, 185 5.3 Control of ATP Synthesis, 187 5.3.1 Diversion of PMF from ATP Synthesis to Other Physiological Activities, 187 5.3.2 Inhibition of Oxidative Phosphorylation, 187 5.3.3 Uncoupling of Electron Transport and Oxidative Phosphorylation, 188 5.4 Energy Uncoupling for Sludge Reduction, 189 5.4.1 Chemical Uncouplers Used for Sludge Reduction, 189 5.4.2 Uncoupling Activity, 198 5.5 Modeling of Uncoupling Effect on Sludge Production, 200 5.6 Sideeffects of Chemical Uncouplers, 202 5.7 Full-Scale Application, 204 References, 204 6 Reduction of Excess Sludge Production Using Ozonation or Chlorination: Performance and Mechanisms of Action 209 Etienne Paul, Qi-Shan Liu, and Yu Liu 6.1 Introduction, 209 6.2 Significant Operational Results for ESP Reduction with Ozone, 210 6.2.1 Options for Combining Ozonation and Biological Treatment, 210 6.2.2 ESP Reduction Performance, 212 6.2.3 Assessing Ozone Efficiency for Mineral ESP Reduction, 215 6.3 Side Effects of Sludge Ozonation, 216 6.3.1 Outlet SS and COD, 216 6.3.2 N Removal, 218 6.4 Cost Assessment, 221 6.5 Effect of Ozone on Sludge, 222 6.5.1 Synergy Between Ozonation and Biological Treatment, 222 6.5.2 Some Fundamentals of Ozone Transfer, 222 6.5.3 Sludge Composition, 224 6.5.4 Effect of Ozone on Activated Sludge: Batch Tests, 226 6.5.5 Effect of Ozone on Biomass Activity, 228 6.5.6 Competition for Ozone in Mixed Liquor, 231 6.6 Modeling Ozonation Effect, 233 6.7 Remarks on Sludge Ozonation, 236 6.8 Chlorination in Water and Wastewater Treatment, 236 6.8.1 Introduction, 236 6.8.2 Chlorination-Assisted Biological Process for Sludge Reduction, 237 6.8.3 Effect of Chlorine Dosage on Sludge Reduction, 239 6.8.4 Chlorine Requirement, 240 6.9 Nomenclature, 242 References, 244 7 High-Dissolved-Oxygen Biological Process for Sludge Reduction 249 Zhi-Wu Wang 7.1 Introduction, 249 7.2 Mechanism of High-Dissolved-Oxygen Reduced Sludge Production, 251 7.2.1 High-Dissolved-Oxygen Decreased Specific Loading Rate, 251 7.2.2 High-Dissolved-Oxygen Uncoupled Microbial Metabolism Pathway, 252 7.2.3 High-Dissolved-Oxygen Shifted Microbial Population, 254 7.3 Limits of High-Dissolved-Oxygen Process for Reduced Sludge Production, 255 References, 256 8 Minimizing Excess Sludge Production Through Membrane Bioreactors and Integrated Processes 261 Philip Chuen-Yung Wong 8.1 Introduction, 261 8.2 Mass Balances, 262 8.3 Integrated Processes Based on Lysis-Cryptic Growth, 266 8.3.1 Mass Balance Incorporating Sludge Disintegration and Solubilization, 268 8.3.2 Thermal and Thermal-Alkaline Treatment, 274 8.3.3 Ozonation, 276 8.3.4 Sonication, 279 8.4 Predation, 283 8.5 Summary and Concluding Remarks, 285 References, 286 9 Microbial Fuel Cell Technology for Sustainable Treatment of Organic Wastes and Electrical Energy Recovery 291 Shi-Jie You, Nan-Qi Ren, and Qing-Liang Zhao 9.1 Introduction, 291 9.2 Fundamentals, Evaluation, and Design of MFCs, 293 9.2.1 Principles, 293 9.2.2 Performance Evaluation, 293 9.2.3 MFC Configurations, 294 9.3 Performance of Anodes, 295 9.3.1 Electrode Materials, 295 9.3.2 Microbial Electron Transfer, 296 9.3.3 Electron Donors, 298 9.4 Cathode Performances, 299 9.4.1 Electron Acceptors, 300 9.4.2 Electrochemical Fundamentals of the Oxygen Reduction Reaction, 302 9.4.3 Air-Cathode Structure and Function, 303 9.4.4 Electrocatalyst, 304 9.5 Separator, 306 9.6 pH Gradient and Buffer, 307 9.7 Applications of MFC-Based Technology, 309 9.7.1 Biosensors, 309 9.7.2 Hydrogen Production, 310 9.7.3 Desalination, 310 9.7.4 Hydrogen Peroxide Synthesis, 312 9.7.5 Environmental Remediation, 312 9.8 Conclusions and Remarks, 314 References, 315 10 Anaerobic Digestion of Sewage Sludge 319 Kuan-Yeow Show, Duu-Jong Lee, and Joo-Hwa Tay 10.1 Introduction, 319 10.2 Principles of Anaerobic Digestion, 320 10.2.1 Hydrolysis and Acidogenesis, 321 10.2.2 Methane Formation, 323 10.3 Environmental Requirements and Control, 324 10.3.1 pH, 324 10.3.2 Alkalinity, 325 10.3.3 Temperature, 326 10.3.4 Nutrients, 326 10.3.5 Toxicity, 327 10.4 Design Considerations for Anaerobic Sludge Digestion, 329 10.4.1 Hydraulic Detention Time, 329 10.4.2 Solids Loading, 330 10.4.3 Temperature, 331 10.4.4 Mixing, 331 10.5 Component Design of Anaerobic Digester Systems, 331 10.5.1 Tank Configurations, 331 10.5.2 Temperature Control, 333 10.5.3 Sludge Heating, 333 10.5.4 Auxiliary Mixing, 334 10.6 Reactor Configurations, 336 10.6.1 Conventional Anaerobic Digesters, 336 10.6.2 Anaerobic Contact Processes, 338 10.6.3 Other Types of Configurations, 340 10.7 Advantages and Limitations of Anaerobic Sludge Digestion, 343 10.8 Summary and New Horizons, 344 References, 345 11 Mechanical Pretreatment-Assisted Biological Processes 349 He´le`ne Carre`re, Damien J. Batstone, and Etienne Paul 11.1 Introduction, 349 11.2 Mechanisms of Mechanical Pretreatment, 350 11.2.1 From Sludge Disintegration to Cell Lysis and Chemical Transformation, 350 11.2.2 Specific Energy, 350 11.2.3 Sonication, 351 11.2.4 Grinding, 353 11.2.5 Shear-Based Methods: High-Pressure and Collision Plate Homogenization, 353 11.2.6 Lysis Centrifuge, 353 11.3 Impacts of Treatment: Rate vs. Extent of Degradability, 353 11.3.1 Grinding, 354 11.3.2 Ultrasonication, 354 11.4 Equipment for Mechanical Pretreatment, 354 11.4.1 Sonication, 355 11.4.2 Grinding, 357 11.4.3 Shear-Based Methods: High-Pressure and Collision Plate Homogenization, 358 11.4.4 Lysis Centrifuge, 359 11.5 Side Effects, 359 11.6 Mechanical Treatment Combined with Activated Sludge, 360 11.7 Mechanical Treatment Combined with Anaerobic Digestion, 361 11.7.1 Performances, 361 11.7.2 Dewaterability, 363 11.7.3 Full-Scale Performance and Market Penetration, 364 11.7.4 Energy Balance, 365 11.7.5 Nutrient Release and Recovery/Removal, 366 11.8 Conclusion, 367 References, 368 12 Thermal Methods to Enhance Biological Treatment Processes 373 Etienne Paul, He´le`ne Carre`re, and Damien J. Batstone 12.1 Introduction, 373 12.2 Mechanisms, 374 12.2.1 Effects of Heating on Cells, 374 12.2.2 Effect of Heating on Sludge, 376 12.2.3 Mechanisms of Thermal Pretreatment, 388 12.3 Devices for Thermal Treatment, 388 12.3.1 Low-Temperature Pretreatment, 389 12.3.2 High-Temperature Pretreatment, 390 12.4 Applications of Thermal Treatment, 390 12.4.1 Thermal Treatment Combined with Activated Sludge, 390 12.4.2 Thermal Pretreatment to Anaerobic Digestion, 394 12.5 Conclusions, 398 References, 399 13 Combustion, Pyrolysis, and Gasification of Sewage Sludge for Energy Recovery 405 Yong-Qiang Liu, Joo-Hwa Tay, and Yu Liu 13.1 Introduction, 405 13.2 Characteristics and Dewatering of Sewage Sludge, 406 13.3 Energy Recovery from Sludge, 408 13.3.1 Incineration, 408 13.3.2 Pyrolysis and Gasification, 416 13.3.3 Wet Oxidation, 419 13.3.4 Thermal Plasma Pyrolysis and Gasification, 420 References, 421 14 Aerobic Granular Sludge Technology for Wastewater Treatment 429 Bing-Jie Ni and Han-Qing Yu 14.1 Introduction, 429 14.2 Technological Starting Points: Cultivating Aerobic Granules, 431 14.2.1 Substrate Composition, 431 14.2.2 Organic Loading Rate, 433 14.2.3 Seed Sludge, 433 14.2.4 Reactor Configuration, 433 14.2.5 Operational Parameters, 434 14.3 Mechanisms of the Aerobic Granulation Process, 436 14.3.1 Granulation Steps, 436 14.3.2 Selective Pressure, 437 14.4 Characterization of Aerobic Granular Sludge, 438 14.4.1 Biomass Yield and Sludge Reduction, 438 14.4.2 Formation and Consumption of Microbial Products, 440 14.4.3 Microbial Structure and Diversity, 441 14.4.4 Physicochemical Characteristics, 442 14.5 Modeling Granule-Based SBR for Wastewater Treatment, 447 14.5.1 Nutrient Removal in Granule-Based SBRs, 447 14.5.2 Multiscale Modeling of Granule-Based SBR, 450 14.6 Bioremediation of Wastewaters with Aerobic Granular Sludge Technology, 452 14.6.1 Organic Wastewater Treatment, 452 14.6.2 Biological Nutrient Removal, 452 14.6.3 Domestic Wastewater Treatment, 454 14.6.4 Xenobiotic Contaminant Bioremediation, 454 14.6.5 Removal of Heavy Metals or Dyes, 455 14.7 Remarks, 456 References, 457 15 Biodegradable Bioplastics from Fermented Sludge, Wastes, and Effluents 465 Etienne Paul, Elisabeth Neuhauser, and Yu Liu 15.1 Introduction, 465 15.1.1 Context of Poly(hydroxyalkanoate) Production from Sludge and Effluents, 465 15.1.2 Industrial Context for PHA Production, 467 15.2 PHA Structure, 469 15.3 Microbiology for PHA Production, 469 15.4 Metabolism of PHA Production, 471 15.4.1 PHB Metabolism, 472 15.4.2 Metabolism for Other PHA Production, 475 15.4.3 Nutrient Limitations, 476 15.4.4 PHA Metabolism in Mixed Cultures, 477 15.4.5 Effect of Substrate in Mixed Cultures, 478 15.5 PHA Kinetics, 479 15.6 PHA Storage to Minimize Excess Sludge Production in Wastewater Treatment Plants, 481 15.7 Choice of Process and Reactor Design for PHA Production, 482 15.7.1 Criteria, 482 15.7.2 Anaerobic–Aerobic Process, 483 15.7.3 Aerobic Dynamic Feeding Process, 485 15.7.4 Fed-Batch Process Under Nutrient Growth Limitation, 486 15.8 Culture Selection and Enrichment Strategies, 487 15.9 PHA Quality and Recovery, 489 15.10 Industrial Developments, 490 References, 492 Index 499

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Book SynopsisThe content of this volume has been added to eMagRes (formerly Encyclopedia of Magnetic Resonance) - theTable of ContentsContributors ix Series Preface xiii Volume Preface xv Part A: Surface Coils 1 1 An Historical Introduction to Surface Coils: The Early Days 3 Joseph J. H. Ackerman 2 Radiofrequency Coils for NMR: A Peripatetic History of Their Twists and Turns 9 Eiichi Fukushima 3 Quadrature Surface Coils 17 Christopher M. Collin and, Andrew G. Webb 4 Double-Tuned Surface Coils 27 Barbara L. Beck 5 Nested Surface Coils for Multinuclear NMR 39 Arthur W. Magill and Rolf Gruetter 6 Quadrature Transverse Electromagnetic (TEM) Surface Coils 51 Nikolai I. Avdievich Part B: Array Coils 63 7 Receiver Loop Arrays 65 Steven M. Wright 8 Coil Array Design for Parallel Imaging: Theory and Applications 81 Daniel K. Sodickson, Michael A. Ohliger, Riccardo Lattanzi and Graham C. Wiggins 9 Transceiver Loop Arrays 101 Randy Duensing 10 Characterization of Multichannel Coil Arrays on the Benchtop 111 Mark A Griswold Part C: Volume Coils 121 11 Birdcage Volume Coil Design 123 Nicola De Zanche 12 Double-Tuned Birdcage Coils: Construction and Tuning 137 Joseph Murphy-Boesch 13 TEM Body Coils 147 J. Thomas Vaughan 14 TEM Transceiver Head Array Coils for Ultra High Magnetic Fields 169 Gregor Adriany 15 TEM Arrays, Design and Implementation 175 Carl Snyder 16 Transverse Electromagnatic (TEM) Coils for Extremities 185 Nikolai I. Avdievich 17 Antennas as Surface Array Elements for Body Imaging at Ultra-high Field Strengths 197 A. J. E. Raaijmakers and C. A. T. van den Berg Part D: Special Purpose Coils 209 18 Catheter Coils 211 Ergin Atalar 19 Microcoils 225 Andrew G. Webb 20 Cryogenic and Superconducting Coils for MRI 233 Sven Junge 21 Litz Coils for High Resolution and Animal Probes, Especially for Double Resonance 245 F. David Doty, George Entzminger Jr 22 Millipede Coils 259 Ernest W. H. Wong Part E: Coil Interface Circuits 269 23 Receiver Design for MR 271 David I. Hoult 24 Radiofrequency Power Amplifiers for NMR and MRI 299 Daniel P. Myer 25 Impedance Matching and Baluns 315 David M. Peterson Part F: Coil Modeling and Evaluation 325 26 Radiofrequency MRI Coil Analysis: A Standard Procedure 327 Rostislav A. Lemdiasov, Reinhold Ludwig 27 Practical Electromagnetic Modeling Methods 339 Jian-Ming Jin 28 Radiofrequency Fields and SAR for Bird Cages 363 Tamer S. Ibrahim 29 RF Field Modeling for Double-Tuned Volume Coils 377 Wanzhan Liu 30 Radiofrequency Fields and SAR for Transverse Electromagnetic (TEM) Surface Coils 387 Can Eyup Akgun 31 TEM Coil Fields and SAR 397 Jinfeng Tian Part G: RF Safety 407 32 RF Device Safety and Compatibility 409 John Nyenhuis 33 Radiofrequency Heating Models and Measurements Devashish Shrivastava, J. Thomas Vaughan 425 Index 437

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Book SynopsisStable radicals - molecules with odd electrons which are sufficiently long lived to be studied or isolated using conventional techniques - have enjoyed a long history and are of current interest for a broad array of fundamental and applied reasons, for example to study and drive novel chemical reactions, in the development of rechargeable batteries or the study of free radical reactions in the body. In Stable Radicals: Fundamentals and Applied Aspects of Odd-Electron Compounds a team of international experts provide a broad-based overview of stable radicals, from the fundamental aspects of specific classes of stable neutral radicals to their wide range of applications including synthesis, materials science and chemical biology. Topics covered include: triphenylmethyl and related radicals polychlorinated triphenylmethyl radicals: towards multifunctional molecular materials phenalenyls, cyclopentadienyls, and other carbon-centered radicals<Trade Review"This is a worthwhile and insightful anthology and leaves the reader with the impression that novel prospects and discoveries could surface at any moment from junctions on the stable radical chemical topology." (Angewandte Chemie, 2011) Table of ContentsPreface xv List of Contributors xvii 1. Triarylmethyl and Related Radicals 1 Thomas T. Tidwell 1.1 Introduction 1 1.1.1 Discovery of the triphenylmethyl radical 1 1.1.2 Bis(triphenylmethyl) peroxide 3 1.2 Free radical rearrangements 4 1.3 Other routes to triphenylmethyl radicals 5 1.4 The persistent radical effect 7 1.5 Properties of triphenylmethyl radicals 8 1.6 Steric effects and persistent radicals 9 1.7 Substituted triphenylmethyl radicals and dimers 9 1.8 Tris(heteroaryl)methyl and related triarylmethyl radicals 12 1.9 Delocalized persistent radicals: analogues of triarylmethyl radicals 14 1.10 Tetrathiatriarylmethyl (TAM) and related triarylmethyl radicals 16 1.11 Perchlorinated triarylmethyl radicals 20 1.12 Other triarylmethyl radicals 23 1.13 Diradicals and polyradicals related to triphenylmethyl 24 1.14 Outlook 28 Acknowledgements 28 References 28 2. Polychlorotriphenylmethyl Radicals: Towards Multifunctional Molecular Materials 33 Jaume Veciana and Imma Ratera 2.1 Introduction 33 2.2 Functional molecular materials based on PTM radicals 35 2.2.1 Materials with magnetic properties 37 2.2.2 Materials with electronic properties 53 2.2.3 Materials with optical properties 65 2.3 Multifunctional switchable molecular materials based on PTM radicals 69 2.3.1 Photo switchable molecular systems 69 2.3.2 Redox switchable molecular systems 70 2.4 Conclusions 75 References 76 3. Phenalenyls, Cyclopentadienyls, and Other Carbon-Centered Radicals 81 Yasushi Morita and Shinsuke Nishida 3.1 Introduction 81 3.2 Open shell graphene 82 3.3 Phenalenyl 84 3.4 2,5,8-Tri-tert-butylphenalenyl radical 86 3.5 Perchlorophenalenyl radical 92 3.6 Dithiophenalenyl radicals 94 3.7 Nitrogen-containing phenalenyl systems 97 3.7.1 Molecular design and topological isomers 97 3.7.2 2,5,8-Tri-tert-butyl-1,3-diazaphenalenyl 97 3.7.3 Hexaazaphenalenyl derivatives 102 3.7.4 β-Azaphenalenyl derivatives 103 3.8 Oxophenalenoxyl systems 106 3.8.1 Molecular design and topological isomers 106 3.8.2 3-Oxophenalenoxyl (3OPO) system 108 3.8.3 4- and 6-Oxophenalenoxyl (4OPO, 6OPO) systems 110 3.8.4 Redox-based spin diversity 114 3.8.5 Molecular crystalline secondary battery 115 3.8.6 Spin-center transfer and solvato-/thermochromism 117 3.9 Phenalenyl-based zwitterionic radicals 119 3.10 π-Extended phenalenyl systems 122 3.10.1 Triangulenes 122 3.10.2 Trioxytriangulene with redox-based spin diversity nature 125 3.10.3 Bis- and tris-phenalenyl system and singlet biradical characters 125 3.11 Curve-structured phenalenyl system 130 3.12 Non-alternant stable radicals 131 3.12.1 Cyclopentadienyl radicals 131 3.12.2 Cyclopentadienyl radicals within a larger π-electronic framework 135 3.13 Stable triplet carbenes 136 3.14 Conclusions 139 Acknowledgements 139 References 140 4. The Nitrogen Oxides: Persistent Radicals and van der Waals Complex Dimers 147 D. Scott Bohle 4.1 Introduction 147 4.2 Synthetic access 149 4.3 Physical properties 149 4.4 Structural chemistry of the monomers and dimers 150 4.4.1 Nitric oxide and dinitrogen dioxide 150 4.4.2 Nitrogen dioxide and dinitrogen tetroxide 152 4.5 Electronic structure of nitrogen oxides 153 4.6 Reactivity of nitric oxide and nitrogen dioxide and their van der Waals complexes 155 4.7 The kinetics of nitric oxide’s termolecular reactions 156 4.8 Biochemical and organic reactions of nitric oxide 158 4.9 General reactivity patterns 160 4.9.1 Oxidation 160 4.9.2 Reduction 161 4.9.3 Coordination 162 4.9.4 Addition of nucleophiles 162 4.9.5 General organic reactions 165 4.9.6 Reactions with other nucleophiles 165 4.10 The colored species problem in nitric oxide chemistry 166 4.11 Conclusions 166 References 166 5. Nitroxide Radicals: Properties, Synthesis and Applications 173 Hakim Karoui, François Le Moigne, Olivier Ouari and Paul Tordo 5.1 Introduction 173 5.2 Nitroxide structure 174 5.2.1 Characteristics of the aminoxyl group 174 5.2.2 X-ray structures of nitroxides 175 5.2.3 Quantum mechanical (QM), molecular dynamics (MD) and molecular mechanics (MM) calculations 177 5.2.4 Influence of solvent polarity on the EPR parameters of nitroxides 180 5.3 Nitroxide multiradicals 181 5.3.1 Electron spin–spin exchange coupling 182 5.3.2 Miscellaneous aspects of di- and polynitroxides 184 5.4 Nitronyl nitroxides (NNOs) 185 5.4.1 Synthesis of nitronyl nitroxides 186 5.4.2 Nitronyl nitroxide as a nitric oxide trap 186 5.4.3 Nitronyl nitroxides as building blocks for magnetic materials 188 5.5 Synthesis of nitroxides 191 5.5.1 Oxidation of amines 191 5.5.2 Oxidation of hydroxylamines 191 5.5.3 Chiral nitroxides 191 5.5.4 Nitroxide design for nitroxide mediated polymerization (NMP) 193 5.6 Chemical properties of nitroxides 196 5.6.1 The Persistent Radical Effect 197 5.6.2 Redox reactions 197 5.6.3 Approaches to improve the resistance of nitroxides toward bioreduction 198 5.6.4 Hydrogen abstraction reactions 199 5.6.5 Cross-coupling reactions 200 5.6.6 Nitroxides in synthetic sequences 200 5.7 Nitroxides in supramolecular entities 206 5.7.1 Interaction of nitroxides with cyclodextrins 207 5.7.2 Interaction of nitroxides with calix[4]arenes 209 5.7.3 Interaction of nitroxides with curcubiturils 210 5.7.4 Interaction of nitroxides with micelles 211 5.7.5 Fullerene-linked nitroxides 212 5.8 Nitroxides for dynamic nuclear polarization (DNP) enhanced NMR 213 5.8.1 DNP for biological NMR and real-time metabolic imaging 213 5.8.2 Nitroxides as polarizing agents for DNP 214 5.9 Nitroxides as pH-sensitive spin probes 216 5.10 Nitroxides as prefluorescent probes 217 5.11 EPR-spin trapping technique 217 5.11.1 Immuno spin trapping 219 5.11.2 Conclusion 219 5.12 Conclusions 220 References 220 6. The Only Stable Organic Sigma Radicals: Di-tert-Alkyliminoxyls 231 Keith U. Ingold 6.1 Introduction 231 6.2 The discovery of stable iminoxyls 232 6.2.1 Synthesis of di-tert-butyl ketoxime 233 6.2.2 Synthesis of di-tert-butyliminoxyl 234 6.2.3 Stability of di-tert-butyliminoxyl 235 6.3 Hydrogen atom abstraction by di-tert-butyliminoxyl 236 6.3.1 The O−H bond dissociation enthalpy (BDE) in (Me 3 C) 2 C=NOH 236 6.3.2 Oxidation of hydrocarbons with di-tert-butyliminoxyl 237 6.3.3 Oxidation of phenols with di-tert-butyliminoxyl 238 6.3.4 Oxidation of amines with di-tert-butyliminoxyl 239 6.3.5 Oxidation of di-tert-butylketoxime with di-tert-butyliminoxyl 239 6.4 Other reactions and non-reactions of di-tert-butyliminoxyl 241 6.5 Di-tert-alkyliminoxyls more sterically crowded than di-tert-butyliminoxyl 241 6.6 Di-(1-Adamantyl)iminoxyl: a truly stable σ radical 242 References 243 7. Verdazyls and Related Radicals Containing the Hydrazyl [R 2 N−NR] Group 245 Robin G. Hicks 7.1 Introduction 245 7.2 Verdazyl radicals 246 7.2.1 Synthesis of verdazyls 246 7.2.2 Stability, physical properties and electronic structure of verdazyls 250 7.2.3 Verdazyl radical reactivity 256 7.2.4 Inorganic verdazyl analogues 264 7.3 Tetraazapentenyl radicals 265 7.4 Tetrazolinyl radicals 266 7.5 1,2,4-Triazolinyl radicals 268 7.6 1,2,4,5-Tetrazinyl radicals 269 7.7 Benzo-1,2,4-triazinyl radicals 270 7.8 Summary 273 References 273 8. Metal Coordinated Phenoxyl Radicals 281 Fabrice Thomas 8.1 Introduction 281 8.2 General properties of phenoxyl radicals 282 8.2.1 Electronic structure and stabilization 282 8.2.2 Electrochemistry of phenoxyl radicals 283 8.2.3 Structure of non-coordinated phenoxyl radicals 284 8.2.4 UV-Vis spectroscopy 284 8.2.5 EPR spectroscopy 284 8.3 Occurrence of tyrosyl radicals in proteins 285 8.4 Complexes with coordinated phenoxyl radicals 287 8.4.1 General ligand structures 287 8.4.2 Vanadium complexes 290 8.4.3 Chromium complexes 291 8.4.4 Manganese complexes 292 8.4.5 Iron complexes 294 8.4.6 Cobalt complexes 297 8.4.7 Nickel complexes 299 8.4.8 Copper complexes 303 8.4.9 Zinc complexes 310 8.5 Conclusions 313 8.6 Abbreviations 313 References 313 9. The Synthesis and Characterization of Stable Radicals Containing the Thiazyl (SN) Fragment and Their Use as Building Blocks for Advanced Functional Materials 317 Robin G. Hicks 9.1 Introduction 317 9.2 Radicals based exclusively on sulfur and nitrogen 319 9.2.1 NS• and SNS• 319 9.2.2 S3 N3• 320 9.2.3 S3 N2•+ and related radical cations 320 9.2.4 Poly(thiazyl), (SN)X 322 9.3 “Organothiazyl” radicals 323 9.3.1 Thioaminyl radicals 323 9.3.2 1,2,3,5-Dithiadiazolyl radicals 329 9.3.3 1,3,2,4-Dithiadiazolyl radicals 336 9.3.4 1,3,2-Dithiazolyl radicals 339 9.3.5 1,2,3-Dithiazolyl radicals 342 9.3.6 Bis(1,2,3-dithiazole) and related radicals 345 9.3.7 1,2,4-Thiadiazinyl radicals 348 9.3.8 1,2,4,6-Thiatriazinyl and -selenatriazinyl radicals 349 9.3.9 Larger cyclic thiazyl radicals 355 9.4 Thiazyl radicals as “advanced materials” 355 9.4.1 Charge transport properties of thiazyl radicals 356 9.4.2 Thiazyl radical-based charge transfer salts 360 9.4.3 Magnetic properties of thiazyl radicals 364 9.5 Conclusions 373 References 373 10. Stable Radicals of the Heavy p-Block Elements 381 Jari Konu and Tristram Chivers 10.1 Introduction 381 10.2 Group 13 element radicals 382 10.2.1 Boron 382 10.2.2 Aluminum, gallium, and indium 384 10.3 Group 14 element radicals 388 10.3.1 Cyclic group 14 radicals 389 10.3.2 Acyclic group 14 radicals 391 10.4 Group 15 element radicals 395 10.4.1 Phosphorus 395 10.4.2 Arsenic, antimony, and bismuth 400 10.5 Group 16 element radicals 400 10.5.1 Sulfur 400 10.5.2 Selenium and tellurium 401 10.6 Group 17 element radicals 402 10.7 Summary and future prospects 403 References 404 11. Application of Stable Radicals as Mediators in Living-Radical Polymerization 407 Andrea R. Szkurhan, Julie Lukkarila and Michael K. Georges 11.1 Introduction 407 11.2 Living polymerizations 408 11.2.1 Living-radical polymerization background 408 11.3 Stable free radical polymerization 409 11.3.1 Background of the work performed at the Xerox Research Centre of Canada 409 11.3.2 General considerations and mechanism 410 11.3.3 Unimolecular initiators 411 11.3.4 Persistent radical effect 413 11.3.5 Requirements of stable radicals as mediating agents 413 11.3.6 Nitroxides as mediating agents 414 11.3.7 Nitroxides and their ability to moderate polymerizations 414 11.3.8 Rate enhancement of stable free radical polymerization through the use of additives 416 11.4 Non-nitroxide-based radicals as mediating agents 416 11.4.1 Triazolinyl radicals 416 11.4.2 Verdazyl radicals 417 11.4.3 Other radicals as mediators 418 11.5 Aqueous stable free radical polymerization processes 420 11.5.1 Living-radical miniemulsion polymerization 421 11.5.2 Emulsion polymerization 422 11.5.3 Other aqueous polymerization processes 423 11.6 The application of stable free radical polymerization to new materials 423 11.6.1 Statistical copolymers 423 11.6.2 Block copolymers 424 11.7 Conclusions 425 List of abbreviations 425 References 425 12. Nitroxide-Catalyzed Alcohol Oxidations in Organic Synthesis 433 Christian Brückner 12.1 Introduction 433 12.2 Mechanism of TEMPO-catalyzed alcohol oxidations 434 12.3 Nitroxides used as catalysts 435 12.3.1 Monomeric nitroxides 435 12.3.2 Ionic liquid nitroxides 436 12.3.3 Supported nitroxides 436 12.4 Chemoselectivity: oxidation of primary vs secondary alcohols 437 12.5 Chemoselectivity: oxidation of primary vs benzylic alcohols 438 12.6 Oxidation of secondary alcohols to ketones 439 12.7 Oxidations of alcohols to carboxylic acids 439 12.7.1 Oxidations leading to linear carboxylic acids 439 12.7.2 (Diol) oxidations leading to lactones 443 12.8 Stereoselective nitroxide-catalyzed oxidations 444 12.9 Secondary oxidants used in nitroxide-catalyzed reactions 446 12.9.1 Elemental halogens 446 12.9.2 Sodium hypochlorite (bleach) 446 12.9.3 Bis(acetoxy)iodobenzene (BAIB) 447 12.9.4 Oxygen (air) 448 12.9.5 Peroxides 449 12.9.6 Other organic secondary oxidants 450 12.9.7 Anodic, electrochemical oxidation 451 12.10 Use of nitroxide-catalyzed oxidations in tandem reactions 451 12.11 Predictable side reactions 453 12.11.1 Oxidations of sulfur 453 12.11.2 Oxidations of nitrogen 453 12.11.3 Oxidations of carbon 454 12.12 Comparison with other oxidation methods 454 12.13 Nitroxide-catalyzed oxidations and green chemistry 455 Acknowledgements 456 References 456 13. Metal–Nitroxide Complexes: Synthesis and Magnetostructural Correlations 461 Victor Ovcharenko 13.1 Introduction 461 13.2 Two types of nitroxide for direct coordination of the metal to the nitroxyl group 462 13.2.1 Complexes containing only >N−•O as a coordinating group 462 13.2.2 Complexes containing >N−•O and other functional groups as donor fragments 464 13.3 Ferro- and ferrimagnets based on metal–nitroxide complexes 465 13.3.1 Molecular magnets based on 1-D systems 470 13.3.2 Molecular magnets based on 2-D systems 474 13.3.3 Molecular magnets based on 3-D systems 480 13.4 Heterospin systems based on polynuclear compounds of metals with nitroxides 483 13.4.1 Reactions whose products retain both the multinuclear fragment and nitroxide 484 13.4.2 Transformation of polynuclear fragments in reactions with nitroxides 487 13.4.3 Transformation of both the polynuclear fragment and the starting nitroxide 489 13.5 Breathing crystals 490 13.6 Other studies of metal–nitroxides 494 13.6.1 Analytical applications 494 13.6.2 NMR spectroscopy 494 13.6.3 Stabilization of nitroxides with β-hydrogen atoms 496 13.6.4 Increased reactivity 496 13.6.5 Hidden exchange interactions 497 13.6.6 Contrast agents 499 13.7 Conclusions 500 References 500 14. Rechargeable Batteries Using Robust but Redox Active Organic Radicals 507 Takeo Suga and Hiroyuki Nishide 14.1 Introduction 507 14.2 Redox reaction of organic radicals 508 14.3 Mechanism and performance of an organic radical battery 509 14.4 Molecular design and synthesis of redox active radical polymers 512 14.4.1 Poly(methacrylate)s and poly(acrylate)s 512 14.4.2 Poly(vinyl ether)s and poly(allene)s 514 14.4.3 Poly(cyclic ether)s 514 14.4.4 Poly(norbornene)s 514 14.4.5 Poly(acetylene)s 514 14.4.6 Poly(styrene)s 515 14.4.7 Combination of radicals with biopolymers and ionic liquids 515 14.5 A totally organic-based radical battery 515 14.6 Conclusions 517 References 518 15. Spin Labeling: A Modern Perspective 521 Lawrence J. Berliner 15.1 Introduction 521 15.2 The early years 522 15.3 Advantages of nitroxides 523 15.4 Applications of spin labeling to biochemical and biological systems 524 15.4.1 Stoichiometry and specificity: proteins and enzymes 524 15.4.2 The reporter group approach: who makes the news? 525 15.5 Distance measurements 526 15.5.1 Metal–spin label distance measurements 526 15.5.2 Spin label–spin label distance measurements 526 15.5.3 Example of strong dipolar interactions 527 15.5.4 Multiple-quantum EPR and distance measurements 528 15.6 Site directed spin labeling (SDSL): how is it done? 529 15.6.1 The SDSL paradigm 530 15.6.2 SDSL parameters 530 15.7 Other spin labeling applications 531 15.7.1 pH sensitive spin labels 532 15.7.2 Spin labeled DNA – structure, dynamics and sequence analysis 532 15.8 Conclusions 534 References 534 16. Functional in vivo EPR Spectroscopy and Imaging Using Nitroxide and Trityl Radicals 537 Valery V. Khramtsov and Jay L. Zweier 16.1 Introduction 537 16.2 Nitroxyl radicals 538 16.3 Triarylmethyl (trityl) radicals 539 16.4 In vivo EPR oximetry using nitroxyl and trityl probes 539 16.4.1 Magnetic resonance approaches for in vivo oximetry 540 16.4.2 Nitroxide probes for EPR oximetry 540 16.4.3 TAM oximetric probes 545 16.5 EPR spectroscopy and imaging of pH using nitroxyl and trityl probes 547 16.5.1 pH-sensitive nitroxyl radicals 547 16.5.2 Dual function pH- and oxygen-sensitive trityl radicals 553 16.6 Redox- and thiol-sensitive nitroxide probes 556 16.6.1 Nitroxides as redox-sensitive EPR probes 556 16.6.2 Disulfide nitroxide biradicals as GSH-sensitive EPR probes 558 16.7 Conclusions 562 Acknowledgements 563 References 563 17. Biologically Relevant Chemistry of Nitroxides 567 Sara Goldstein and Amram Samuni 17.1 Introduction 567 17.2 Mechanisms of nitroxide reactions with biologically relevant small radicals 569 17.3 Nitroxides as SOD mimics 571 17.4 Nitroxides as catalytic antioxidants in biological systems 573 17.5 Conclusions 576 Acknowledgements 576 References 576 Index 579

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