Springer Laboratory – serie

This book introduces the reader to thermal field-flow fractionation and discusses its advantages over the fundamental problems associated with traditional column-based analytical techniques commonly used to characterize polymers and macromolecules.

This Springer Laboratory volume introduces the reader to advanced techniques for the separation and fractionation of polyolefins. It includes detailed information on experimental protocols and procedures, addressing the experimental background of different polyolefin fractionation techniques in great detail. The book summarizes important applications in all major fractionation methods with emphasis on multidimensional analytical approaches. It comprises the most powerful modern techniques, such as high temperature size exclusion chromatography (HT-SEC) for molar mass analysis, temperature rising elution fractionation (TREF) and crystallization analysis fractionation (CRYSTAF) for the analysis of chemical composition and branching, high temperature two-dimensional liquid chromatography (HT-2D-LC), solvent and temperature gradient interaction chromatography (SGIC and TGIC) and crystallization elution fractionation (CEF). Beginners as well as experiencedchromatographers will benefit from this concise introduction to a great variety in instrumentation, separation procedures and applications. With detailed descriptions of experimental approaches for the analysis of complex polyolefins, the readers are offered a toolbox to solve simple as well as sophisticated separation tasks. The book starts with an introduction into the molecular complexity of polyolefins - the most widely used synthetic polymers with rapidly growing production capacities. It systematically discusses crystallization based fractionation techniques including TREF, CRYSTAF and CEF and column chromatographic techniques for molar mass, chemical composition and microstructure, as well as the combination of different fractionations in multidimensional experimental setups. This book also includes basic information on the application of high-temperature field-flow fractionation.

This Springer Laboratory volume is a practical guide for scientists and students dealing with the measurement of mechanical properties of polymers at the nanoscale through AFM force-distance curves.In the first part of the book the reader will find a theoretical introduction about atomic force microscopy, focused on force-distance curves, and mechanical properties of polymers. The discussion of several practical issues concerning the acquisition and the interpretation of force-distance curves will help scientists starting to employ this technique.The second part of the book deals with the practical measurement of mechanical properties of polymers by means of AFM force-distance curves. Several "hands-on" examples are illustrated in a very detailed manner, with particular attention to the sample preparation, data analysis, and typical artefacts. This section gives a complete overview about the qualitative characterization and quantitative determination of the mechanical properties of homogeneous polymer samples, polymer brushes, polymer thin films, confined polymer samples, model blends and microstructured polymer blends through AFM force-distance curves. The book also introduces to new approaches and measurement techniques, like creep compliance and force modulation measurements, pointing out approximations, limitations and issues requiring further confirmation.

This Springer Laboratory volume introduces the reader to advanced techniques for the separation and fractionation of polyolefins. It includes detailed information on experimental protocols and procedures, addressing the experimental background of different polyolefin fractionation techniques in great detail. The book summarizes important applications in all major fractionation methods with emphasis on multidimensional analytical approaches. It comprises the most powerful modern techniques, such as high temperature size exclusion chromatography (HT-SEC) for molar mass analysis, temperature rising elution fractionation (TREF) and crystallization analysis fractionation (CRYSTAF) for the analysis of chemical composition and branching, high temperature two-dimensional liquid chromatography (HT-2D-LC), solvent and temperature gradient interaction chromatography (SGIC and TGIC) and crystallization elution fractionation (CEF). Beginners as well as experiencedchromatographers will benefit from this concise introduction to a great variety in instrumentation, separation procedures and applications. With detailed descriptions of experimental approaches for the analysis of complex polyolefins, the readers are offered a toolbox to solve simple as well as sophisticated separation tasks. The book starts with an introduction into the molecular complexity of polyolefins - the most widely used synthetic polymers with rapidly growing production capacities. It systematically discusses crystallization based fractionation techniques including TREF, CRYSTAF and CEF and column chromatographic techniques for molar mass, chemical composition and microstructure, as well as the combination of different fractionations in multidimensional experimental setups. This book also includes basic information on the application of high-temperature field-flow fractionation.

This Springer Laboratory volume is a practical guide for scientists and students dealing with the measurement of mechanical properties of polymers at the nanoscale through AFM force-distance curves.In the first part of the book the reader will find a theoretical introduction about atomic force microscopy, focused on force-distance curves, and mechanical properties of polymers. The discussion of several practical issues concerning the acquisition and the interpretation of force-distance curves will help scientists starting to employ this technique.The second part of the book deals with the practical measurement of mechanical properties of polymers by means of AFM force-distance curves. Several "hands-on" examples are illustrated in a very detailed manner, with particular attention to the sample preparation, data analysis, and typical artefacts. This section gives a complete overview about the qualitative characterization and quantitative determination of the mechanical properties of homogeneous polymer samples, polymer brushes, polymer thin films, confined polymer samples, model blends and microstructured polymer blends through AFM force-distance curves. The book also introduces to new approaches and measurement techniques, like creep compliance and force modulation measurements, pointing out approximations, limitations and issues requiring further confirmation.

Analytical ultracentifugation (AUC) is a powerful method for the characterization of polymers, biopolymers, polyelectrolytes, nanoparticles, dispersions, and other colloidal systems. The method is able to determine the molar mass, the particle size, the particle density and interaction parameters like virial coefficients and association constants. Because AUC is also a fractionation method, the determination of the molar mass distribution, the particle size distribution, and the particle density distribution is possible. A special technique, the density gradient method, allows fractionating heterogeneous samples according to their chemical nature that means being able to detect chemical heterogeneity. The book is divided into chapters concerning instrumentation, sedimentation velocity runs, density gradient runs, application examples and future developments. In particular, the detailed application chapter demonstrates the versatility and power of AUC by means of many interesting and important industrial examples. Thus the book concentrates on practical aspects rather than details of centrifugation theory.Both authors have many years of experience in an industrial AUC research laboratory of a world leading chemical company.

Cosmetic emulsions exist today in many forms for a wide variety of applications, including face and hand creams for normal, dry or oily skin, body milks and lotions, as well as sun-block products. Keeping track of them and their properties is not always easy despite informative product names or partial names (e.g. hand or face cream) that clearly indicate their use and properties. This practical manual provides a detailed overview that describes the key properties and explains how to measure them using modern techniques. Written by an expert in flows and flow properties, it focuses on the application of rheological (flow) measurements to cosmetic and food emulsions and the correlation of these results with findings from other tests.Beginning with a brief history of rheology and some fundamental principles, the manual describes in detail the use of modern viscometers and rheometers, including concise explanations of the different available instruments. But the focus remains on practical everyday lab procedures: how to characterize cosmetic and food emulsions with different rheological tests such as temperature, time, stress and strain, both static and dynamic.Also the critical topic of how the results correlate with other important product characteristics, for instance, skin sensation, pumping performance, stability etc. is carefully explored. Many pictures, illustrations, graphs and tables help readers new to the measurement of cosmetic emulsions in their daily work as well as to the more experienced who seek additional special tips and tricks

Polysaccharide esters (e.g. cellulose and starch) are among the first polymeric materials applied commercially. The way of producing these technically relevant derivatives, mainly the carboxylic acid esters of C2 to C4 acids, have not been changed significantly during their history of manufacture. The investigation of new acylation methods and strategies of analysis was revived during the last decade by the search for tailored, biocompatible material for specific fields of application, e.g., biotechnology, sensor technique and medicine. Unconventional solvents were developed for completely homogeneous acylation reaction applying state of the art techniques of modern organic chemistry for polysaccharide modification. This book will provide a first comprehensive summary of acylation methods in a very practical manner.Detailed structure analysis is indispensable for the evaluation of structure-property-relationships. Spectroscopic methods in particular FTIR- and NMR spectroscopy including two dimensional methods are of increasing importance.

The study of polymers by electron microscopy (EM) needs special techniques, precautions and preparation methods, including ultramicrotomy. General characteristics of the different techniques of EM, including scanning force microscopy, are given in this hands-on book. The application of these techniques to the study of morphology and properties, particularly micromechanical properties, is described in detail. Examples from all classes of polymers are presented.

NMR Spectroscopy of Polymers places emphasis on the practical use of NMR spectroscopy in polymer chemistry rather than the theoretical treatments. Based on the authors' extensive experimental experience, topics covered include (1) experimental problems such as preparation of sample solution, selection of solvent, internal standard and tube, and contaminants in sample solution, (2) accuracy and precision of NMR measurements required in the analysis of polymer structure such as tacticity, copolymer composition and chain end structures, (3) volume magnetic susceptibility by NMR, (4) stereochemistry of polymer chains, chemical composition and comonomer sequence distribution in copolymers, and end groups and irregular linkages, (5) on-line coupled size exclusion chromatography(SEC) and NMR spectroscopy(SEC/NMR) in which an NMR spectrometer is set in the SEC system as a detector.

Viscometry is an easy, accessible, but at the same time significant, analytical method for the characterization of polymers in solution. This laboratory handbook offers clear guidelines and tips for the practical everyday application of viscosimetry, as well as supplying a comprehensive companion for the interpretation of viscosimetric data from simple to complex polymer solutions. It is written with the premise that general knowledge of the broad behavioral spectrum of polymer solutions is of utmost importance for the correct handling of viscometric equipment and the interpretation of data. Originating from the author’s experience supervising analytical polymer chemistry lab courses, it shows readers how to tackle many practical examples through detailed examples.

MALDI-TOF mass spectrometry is one of the latest and most fascinating new developments in the analysis of organic compounds. Originally developed for the analysis of biomolecules, it has developed into one of the most powerful techniques for the characterization of synthetic polymers. This book describes the fundamentals of the MALDI process and the technical features of MALDI-TOF instrumentation. It reviews the application of MALDI-TOF for identification, chemical and molar mass analysis of synthetic polymers. With many examples, this monograph examines in detail experimental protocols for the determination of endgroups, the analysis of copolymers and additives, and the coupling of liquid chromatography and MALDI-TOF.

Polyelectrolytes, i. e. , water-soluble polymers with a lot of dissociating functional groups, and nanoparticles, i. e. , ?ne particles with diameters on the nanometer scale, are two substance classes of growing interest. Both polyelectrolytes and nanoparticles can be found in many industrial applications such as in paints, - per coatings, cosmetics, and pharmaceuticals. For adjusting the properties of such multicomponent systems, the knowledge of the macromolecular and electroch- ical features of the polyelectrolytes on the one hand, and the size and shape of the nanoparticles on the other hand is essential. Understanding the basic principles involved in the preparation of nanoparticles and control of the interparticle interaction forces by adsorbing polyelectrolytes is therefore crucial, both from a scienti?c and application oriented point of view. Over the last years, the term nanotechnology, which refers to the technology that produces nanosize particles, has been established, and a new fast-growing market has been born. The pioneers in this ?eld were the alchemists, who were already able in the 16th century to produce colloidal gold, however, without kno- edge of the scienti?c background of the formulation process. Today, of course, we know much more about the colloidal metal nanoparticles, but still some questions are open. Therefore, especially the formation, characterization, and stabilization of gold nanoparticles as a nanoscalic model system in presence of polyelectrolytes, is discussed here in more detail.

Polymers are mainly characterized by molar mass, chemical composition, functionality and architecture. The determination of the complex structure of polymers by chromatographic and spectroscopic methods is one of the major concerns of polymer analysis and characterization. This lab manual describes the experimental approach to the chromatographic analysis of polymers. Different chromatographic methods, their theoretical background, equipment, experimental procedures and applications are discussed. The book will enable polymer chemists, physicists and material scientists as well as students of macromolecular and analytical science to optimize chromatographic conditions for a specific separation problem. Special emphasis is given to the description of applications for homo- and copolymers and polymer blends.

Although size exclusion chromatography (SEC) is perhaps the most popular and widely used technique for determining the molecular weight distribution of polymeric materials, there have been very few texts written on this topic. During the past decade, SEC has experienced a considerable amount of growth in regard to column and detector technology and new applications. With these advances, SEC can now be used for determining absolute molecular weight, polymer chain conformation and size, and branching, as well as polymer solution properties. This book introduces the reader to the fundamentals of SEC with emphasis on practical aspects of the technique, such as column and mobile selection, calibration, new detector capabilities and guidelines for performing SEC on most types of polymers, especially those of industrial importance. This book is intended for either those new to the field of SEC, or for those research workers who require a more comprehensive background.

Applications of X-ray scattering to soft matter have advanced considerably within recent years, both conceptually and technically – mature high-power X-ray sources, synchrotrons and rotating anodes, as well as high-speed detectors have become readily available. High-quality time-resolved experiments on polymer structure now can be performed with ease, a major advancement due to the genuine power of the scattering method.This manual summarizes the analytical power of modern X-ray scattering in the field of soft matter. Description of simple tools that can elucidate the mechanisms of structure evolution in the studied materials is followed by a step-by-step guide and breakdown of the more advanced methods. Data analysis based on clear, unequivocal results is rendered simple and straightforward – with a stress on the carefully planning of the experiments and adequate recording of all required data. To this end, this book serves as a useful ready-reference guide.

Light scattering is a very powerful method to characterize the structure of polymers and nanoparticles in solution. Recent technical developments have strongly enhanced the possible applications of this technique, overcoming previous limitations like sample turbidity or insufficient experimental time scales. However, despite their importance, these new developments have not yet been presented in a comprehensive form. In addition, and maybe even more important to the broad audience, there lacks a simple-to-read textbook for students and non-experts interested in the basic principles and fundamental techniques of light scattering. As part of the Springer Laboratory series, this book tries not only to provide such a simple-to-read and illustrative textbook about the seemingly very complicated topic of light scattering from polymers and nanoparticles in dilute solution, but also intends to cover some of the newest technical developments in experimental light scattering.

Tis book concentrates on atomic force microscopy (AFM), a method recently - veloped to study the surfaces of synthetic polymeric membranes. AFM is becoming a very important tool for the characterization of synthetic polymeric membranes. Te development of membranes of improved performance depends on the exact kn- ledge of the morphology of a thin selective layer that exists at the surface of the m- brane. Te control of the morphology of the selective layer is crucial for the design of synthetic polymeric membranes. With a relatively short history of only twen- ?ve years, AFM has ?rmly established its position as a method to characterize the membrane surface. Each chapter of this book includes information on basic principles, commercial applications, current research, and guidelines for future research. Each chapter is summarized at the end and contains a comprehensive list of references. Te introductory chapter gives a brief overview of synthetic polymeric m- branes and their applications both in industrial processes and in biomedical ?elds. It also gives an overview of studies on membrane surface morphology by various methods. Chapter ? deals with the synthesis of membranes, the properties of membranes, and the application of membranes. Te beginning also identi?es the three types of membranes (i.e., biological, synthetic, and theoretical) and their applications.

Scope of the Book Synthetic and natural polymers exhibit a complex structural and morphological hierarchy on multiple length scales [1], which determines their performance. Thus, research aiming at visualizing structure and morphology using a multitude of microscopy techniques has received considerable attention since the early days of polymer science and technology. Various well-developed techniques such as optical microscopy and different forms of electron microscopy (Scanning Electron Micr- copy, SEM; Transmission Electron Microscopy, TEM; Environmental Scanning Electron Microscopy, ESEM) allow one to view polymeric structure at different levels of magni?cation. These classical techniques, and their applications to po- mers, are well documented in the literature [2, 3]. The invention of Scanning Tunneling Microscopy (STM) inspired the devel- ment of Atomic Force Microscopy (AFM) and other forms of scanning proximity microscopes in the late 1980s [4, 5]. AFM, unlike STM, can be used to image n- conducting specimens such as polymers. In addition, AFM imaging is feasible in liquids, which has several advantages. Using liquid imaging cells the forces between specimen and AFM probe are drastically reduced, thus sample damage is prevented. In addition, the use of water as imaging medium opened up new applications aiming at imaging, characterizing, and analyzing biologically important systems.

The study of polymers by electron microscopy (EM) needs special techniques, precautions and preparation methods, including ultramicrotomy. General characteristics of the different techniques of EM, including scanning force microscopy, are given in this hands-on book. The application of these techniques to the study of morphology and properties, particularly micromechanical properties, is described in detail. Examples from all classes of polymers are presented.

NMR Spectroscopy of Polymers places emphasis on the practical use of NMR spectroscopy in polymer chemistry rather than the theoretical treatments. Based on the authors' extensive experimental experience, topics covered include (1) experimental problems such as preparation of sample solution, selection of solvent, internal standard and tube, and contaminants in sample solution, (2) accuracy and precision of NMR measurements required in the analysis of polymer structure such as tacticity, copolymer composition and chain end structures, (3) volume magnetic susceptibility by NMR, (4) stereochemistry of polymer chains, chemical composition and comonomer sequence distribution in copolymers, and end groups and irregular linkages, (5) on-line coupled size exclusion chromatography(SEC) and NMR spectroscopy(SEC/NMR) in which an NMR spectrometer is set in the SEC system as a detector.

Viscometry is an easy, accessible, but at the same time significant, analytical method for the characterization of polymers in solution. This laboratory handbook offers clear guidelines and tips for the practical everyday application of viscosimetry, as well as supplying a comprehensive companion for the interpretation of viscosimetric data from simple to complex polymer solutions. It is written with the premise that general knowledge of the broad behavioral spectrum of polymer solutions is of utmost importance for the correct handling of viscometric equipment and the interpretation of data. Originating from the author’s experience supervising analytical polymer chemistry lab courses, it shows readers how to tackle many practical examples through detailed examples.

MALDI-TOF mass spectrometry is one of the latest and most fascinating new developments in the analysis of organic compounds. Originally developed for the analysis of biomolecules, it has developed into one of the most powerful techniques for the characterization of synthetic polymers. This book describes the fundamentals of the MALDI process and the technical features of MALDI-TOF instrumentation. It reviews the application of MALDI-TOF for identification, chemical and molar mass analysis of synthetic polymers. With many examples, this monograph examines in detail experimental protocols for the determination of endgroups, the analysis of copolymers and additives, and the coupling of liquid chromatography and MALDI-TOF.

Polyelectrolytes, i. e. , water-soluble polymers with a lot of dissociating functional groups, and nanoparticles, i. e. , ?ne particles with diameters on the nanometer scale, are two substance classes of growing interest. Both polyelectrolytes and nanoparticles can be found in many industrial applications such as in paints, - per coatings, cosmetics, and pharmaceuticals. For adjusting the properties of such multicomponent systems, the knowledge of the macromolecular and electroch- ical features of the polyelectrolytes on the one hand, and the size and shape of the nanoparticles on the other hand is essential. Understanding the basic principles involved in the preparation of nanoparticles and control of the interparticle interaction forces by adsorbing polyelectrolytes is therefore crucial, both from a scienti?c and application oriented point of view. Over the last years, the term nanotechnology, which refers to the technology that produces nanosize particles, has been established, and a new fast-growing market has been born. The pioneers in this ?eld were the alchemists, who were already able in the 16th century to produce colloidal gold, however, without kno- edge of the scienti?c background of the formulation process. Today, of course, we know much more about the colloidal metal nanoparticles, but still some questions are open. Therefore, especially the formation, characterization, and stabilization of gold nanoparticles as a nanoscalic model system in presence of polyelectrolytes, is discussed here in more detail.

Although size exclusion chromatography (SEC) is perhaps the most popular and widely used technique for determining the molecular weight distribution of polymeric materials, there have been very few texts written on this topic. During the past decade, SEC has experienced a considerable amount of growth in regard to column and detector technology and new applications. With these advances, SEC can now be used for determining absolute molecular weight, polymer chain conformation and size, and branching, as well as polymer solution properties. This book introduces the reader to the fundamentals of SEC with emphasis on practical aspects of the technique, such as column and mobile selection, calibration, new detector capabilities and guidelines for performing SEC on most types of polymers, especially those of industrial importance. This book is intended for either those new to the field of SEC, or for those research workers who require a more comprehensive background.

Applications of X-ray scattering to soft matter have advanced considerably within recent years, both conceptually and technically – mature high-power X-ray sources, synchrotrons and rotating anodes, as well as high-speed detectors have become readily available. High-quality time-resolved experiments on polymer structure now can be performed with ease, a major advancement due to the genuine power of the scattering method.This manual summarizes the analytical power of modern X-ray scattering in the field of soft matter. Description of simple tools that can elucidate the mechanisms of structure evolution in the studied materials is followed by a step-by-step guide and breakdown of the more advanced methods. Data analysis based on clear, unequivocal results is rendered simple and straightforward – with a stress on the carefully planning of the experiments and adequate recording of all required data. To this end, this book serves as a useful ready-reference guide.

Light scattering is a very powerful method to characterize the structure of polymers and nanoparticles in solution. Recent technical developments have strongly enhanced the possible applications of this technique, overcoming previous limitations like sample turbidity or insufficient experimental time scales. However, despite their importance, these new developments have not yet been presented in a comprehensive form. In addition, and maybe even more important to the broad audience, there lacks a simple-to-read textbook for students and non-experts interested in the basic principles and fundamental techniques of light scattering. As part of the Springer Laboratory series, this book tries not only to provide such a simple-to-read and illustrative textbook about the seemingly very complicated topic of light scattering from polymers and nanoparticles in dilute solution, but also intends to cover some of the newest technical developments in experimental light scattering.

Tis book concentrates on atomic force microscopy (AFM), a method recently - veloped to study the surfaces of synthetic polymeric membranes. AFM is becoming a very important tool for the characterization of synthetic polymeric membranes. Te development of membranes of improved performance depends on the exact kn- ledge of the morphology of a thin selective layer that exists at the surface of the m- brane. Te control of the morphology of the selective layer is crucial for the design of synthetic polymeric membranes. With a relatively short history of only twen- ?ve years, AFM has ?rmly established its position as a method to characterize the membrane surface. Each chapter of this book includes information on basic principles, commercial applications, current research, and guidelines for future research. Each chapter is summarized at the end and contains a comprehensive list of references. Te introductory chapter gives a brief overview of synthetic polymeric m- branes and their applications both in industrial processes and in biomedical ?elds. It also gives an overview of studies on membrane surface morphology by various methods. Chapter ? deals with the synthesis of membranes, the properties of membranes, and the application of membranes. Te beginning also identi?es the three types of membranes (i.e., biological, synthetic, and theoretical) and their applications.

This book presents the principle ideas of combining different analytical techniques in multi-dimensional analysis schemes. It reviews the basic principles and instrumentation of multi-dimensional chromatography and the hyphenation of liquid chromatography with selective spectroscopic detectors and presents experimental protocols for the analysis of complex polymers.It is the consequent continuation of "HPLC of Polymers" from 1999 by the same authors. Like its 'predecessor', this book discusses the theoretical background, equipment, experimental procedures and applications for each separation technique, but in contrast treats multi-dimensional and coupled techniques. "Multidimensional HPLC of Polymers" intends to review the state of the art in polymer chromatography and to summarize the developments in the field during the last 15 years. With its tutorial and laboratory manual style it is written for beginners as well as for experienced chromatographers, and will enable its readers (polymer chemists, physicists and material scientists, as well as students of polymer and analytical sciences) to optimize the experimental conditions for their specific separation problems.