Characterization of Synthetic Polymers Applying MALDI-TOF MS and Combined Analysis Techniques PDF Download
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Author: Anja Baumgärtel
Publisher:
ISBN:
Category :
Languages : de
Pages : 0
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Book Description
Zur vollständigen Charakterisierung synthetischer Polymersysteme ist nicht nur der Einsatz von verschiedenen, besonders schonend ionisierenden Massenspektrometrietechniken erforderlich, sondern auch die Verwendung erweiterter chromatographischer Analysemethoden. Zu diesem Zweck eignen sich spezielle Massenspektrometriemethoden wie die matrixunterstützte Laserdesorption-Ionisation (MALDI) und die Elektrospray Ionisation (ESI) (gekoppelt mit einem (Quadrupol- ) Flugzeitanalysator (TOF oder Q-TOF)), welche zusätzliche Informationen über den Polymerisationsverlauf und die zugrundeliegende Molekülstruktur der untersuchten synthetischen Homo- und Copolymere liefern können. Die vorliegende Arbeit befasst sich mit der Charakterisierung von verschiedensten synthetischen Homo- und Copolymeren unter Zuhilfenahme der einfachen MALDI-TOF Massenspektrometrie (MS) sowie der erweiterten Tandem-MS Analysenmethode (MS/MS).
Author: Anja Baumgärtel
Publisher:
ISBN:
Category :
Languages : de
Pages : 0
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Book Description
Zur vollständigen Charakterisierung synthetischer Polymersysteme ist nicht nur der Einsatz von verschiedenen, besonders schonend ionisierenden Massenspektrometrietechniken erforderlich, sondern auch die Verwendung erweiterter chromatographischer Analysemethoden. Zu diesem Zweck eignen sich spezielle Massenspektrometriemethoden wie die matrixunterstützte Laserdesorption-Ionisation (MALDI) und die Elektrospray Ionisation (ESI) (gekoppelt mit einem (Quadrupol- ) Flugzeitanalysator (TOF oder Q-TOF)), welche zusätzliche Informationen über den Polymerisationsverlauf und die zugrundeliegende Molekülstruktur der untersuchten synthetischen Homo- und Copolymere liefern können. Die vorliegende Arbeit befasst sich mit der Charakterisierung von verschiedensten synthetischen Homo- und Copolymeren unter Zuhilfenahme der einfachen MALDI-TOF Massenspektrometrie (MS) sowie der erweiterten Tandem-MS Analysenmethode (MS/MS).
Author: Harald Pasch
Publisher: Springer Science & Business Media
ISBN: 3662050463
Category : Science
Languages : en
Pages : 312
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Book Description
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, the monograph examines experimental protocols for the determination of endgroups, the analysis of copolymers and additives, and the coupling of liquid chromatography and MALDI-TOF in detail.
Author: Liang Li
Publisher: John Wiley & Sons
ISBN: 0470567228
Category : Science
Languages : en
Pages : 325
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Book Description
Principles and Practices of Polymer Mass Spectrometry helps readers acquire the skills necessary for selecting the optimal methods, handling samples, analyzing the data, and interpreting the results of the mass spectrometry of polymers. This guide describes the principles of polymer MS and best practices in polymer characterization. It discusses different approaches, including MALDI, ESI, TOF MS, and FT-MS. It provides a guide to developing appropriate sample preparation protocols for different polymers. Complete with examples of applications and experiments, this is an excellent reference for scientists, researchers, graduate students, and others.
Author: Liang Li
Publisher: Wiley
ISBN: 9780471775799
Category : Science
Languages : en
Pages : 307
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Book Description
Principles and Practices of Polymer Mass Spectrometry helps readers acquire the skills necessary for selecting the optimal methods, handling samples, analyzing the data, and interpreting the results of the mass spectrometry of polymers. This guide describes the principles of polymer MS and best practices in polymer characterization. It discusses different approaches, including MALDI, ESI, TOF MS, and FT-MS. It provides a guide to developing appropriate sample preparation protocols for different polymers. Complete with examples of applications and experiments, this is an excellent reference for scientists, researchers, graduate students, and others.
Author: Christopher Barner-Kowollik
Publisher: John Wiley & Sons
ISBN: 3527641831
Category : Science
Languages : en
Pages : 501
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Book Description
Combining an up-to-date insight into mass-spectrometric polymer analysis beyond MALDI with application details of the instrumentation, this is a balanced and thorough presentation of the most important and widely used mass-spectrometric methods. Written by the world's most proficient experts in the field, the book focuses on the latest developments, covering such technologies and applications as ionization protocols, tandem and liquid chromatography mass spectrometry, gas-phase ion-separation techniques and automated data processing. Chapters on sample preparation, polymer degradation and the usage of mass-spectrometric tools on an industrial scale round off the book. As a result, both entrants to the field and experienced researchers are able to choose the appropriate methods and instrumentations -- and to assess their respective strengths and limitations -- for the characterization of polymer compounds.
Author: Giorgio Montaudo
Publisher: CRC Press
ISBN: 1420037757
Category : Science
Languages : en
Pages : 601
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Book Description
Mass Spectrometry (MS) has rapidly become an indispensable tool in polymer analysis, and modern MS today complements in many ways the structural data provided by Nuclear Magnetic Resonance (NMR) and Infrared (IR) methods. Recent advances have sparked a growing interest in this field and established a need for a summary of progress made and results
Author: Madalis Casiano-Maldonado
Publisher:
ISBN:
Category : Biodegradation
Languages : en
Pages : 178
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Book Description
The characterization of synthetic polymers and complex oligomeric mixtures by a combination of different mass spectrometry (MS) techniques is the main topic of this dissertation. Ion mobility (IM) separation and/or tandem mass spectrometry (MS2) were interfaced with single stage mass spectrometry for the fast, complete, precise and accurate characterization of different polymers, biopolymers, and biodegradation products. Additionally, the development of a mass spectrometry protocol for the quantitation of proteins adsorbed on different polymer surfaces was accomplished in this dissertation. Over the passed years, synthetic routes for the creation of PEGs have been modified by the elimination of organic catalysts and solvents and the application of green chemistry for the generation of new polymers. In Chapter 4 of this dissertation, MS and MS2 were employed, as the main analytical techniques, for the structural elucidation of enzyme-catalyzed, functionalized PEG and tetraethylene glycol (TEG) biomaterials. The samples analyzed were synthesized by two different processes, transesterification and Michael addition reactions, both of them using CALB as the catalyst. In Chapter 5 of this dissertation, polylactide was degraded using Proteinase K and its biodegradation products were analyzed by MS and MS2. Elucidation of its degradation products is important to the biomedical community; knowledge of these products helps to see any toxicity problems with the use of this polymer. The MS and MS2 results showed that the degradation products are short polylactide chains, down to the monomer. No other, potentially dangerous organics were detected. In the following chapter of this dissertation (Chapter 6), the adsorption of three model proteins onto two different surfaces was evaluated over a pH range. The results were explained on terms of polymer chemistry, surface morphology, proteins' isoelectricpoints and molecular dimensions. Finally, Chapter 7 reports how derivatization, degradation, or chromatographic separation can be avoided for the analysis of complex systems, if multidimensional mass spectrometry methods combining ion mobility separation and different ionization techniques are employed. Using this new approach complex poly([alpha]-peptoid) samples were characterized. The results showed that the main product in the system contained the N-heterocyclic carbene (NHC) moiety that served as ring-opening polymerization catalyst. Furthermore, it was demonstrated that elimination of the NHC segment leads to cyclic poly([alpha]-peptoid)s that have very similar conformations with comparably sized polypeptides.
Author: Sarah Charlotte Crotty
Publisher:
ISBN:
Category :
Languages : en
Pages :
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Book Description
The focus of this thesis was to gain in-depth structural information of synthetic polymers by the application of several combined techniques. The second chapter provides an overview about the influence of the polymer architecture on its characterization by mass spectrometry and complementary methods. In the third chapter, we demonstrate the use of MS, more specifically MALDI-ToF MS, which provides molar masses and dispersity values for poly(furfuryl glycidyl ether) (PFGE). The second example is the study of poly(N-isopropyl acrylamide) (PNiPAm) copolymers with glyco-monomers with specific combinations of matrices and cationization agents. The fourth chapter will combine three different examples regarding linear, star-shaped and hybrid polymers, which were analyzed by advanced techniques. The linear copolymers were analyzed by separating them according to their chemical heterogeneity using liquid absorption chromatography at critical conditions (LACCC) of poly(2-ethyl-2-oxazoline) (PEtOx), followed by automated spotting onto a MALDI target, which was subsequently analyzed by MALDI. Secondly, star-shaped polymers: [poly(ethylene oxide) (PEO)-b-PEtOx]8 were monitored firstly by using LACCC of linear PEO as first separation dimension and furthermore injected onto an SEC column confirming the molar mass. Lastly, a hybrid PEO star-shaped polymer was investigated using MALDI to verify the complete functionality of the core with PEO arms. Finally, the last chapter will focus on the creation of a software to obtain information regarding average composition, overcoming isotopic, overlapping peaks and isobaric species from MS spectra. Moreover, the quantitative studies were carried out by correction of the mass discrimination and isotopic abundance. Consequently, advanced analytical techniques such as different ionization techniques within MS, a range of chromatographic hyphenation and computational methods are implemented for elucidating the complexity of synthetic polymers.
Author:
Publisher:
ISBN: 9789491407178
Category :
Languages : en
Pages : 157
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Book Description
"Polymers vary in terms of the monomer/s used; the number, distribution and type of linkage of monomers per molecule; and the side chains and end groups attached. Given this diversity, traditional single-technique approaches to characterization often give limited and inadequate information about a given polymer. Multi-technique but polymer-specific approach was found to be an appropriate alternative. This strategy was applied in characterizing polymers of a wide range of properties from simple polyethylene gylcol, to polycationic chitosan and aminopropyl based oligosiloxanes, and to polydiverse polyfluorinated polyethoxylates. Mass Spectrometry (MS) was used to characterize the different polymers. Different modes of sample introduction, ionization, mass analysis and detection were surveyed. The nature of the monomer units, the size and the polydispersity of polymers are the important factors that affect the detection and quantification of the polymer moieties using MS. MS gave information not just on the molecular weight but also about the repeating units of the polymers. Traditional techniques like size exclusion chromatography and infrared spectroscopy were also used to obtain complementary information on the properties of polymers. Chemometric techniques like partial least squares aided in the statistical evaluation of experimental data. The research works included in this thesis have demonstrated that polymer characterization can be accomplished with the use of a combination of different instrumental and statistical techniques. This strategy allows the researcher to explore additional information about the polymer formulation and correlate these to some observed behaviors or activities."--Samenvatting auteur.
Author: Kittisak Chaicharoen
Publisher:
ISBN:
Category : Chemistry
Languages : en
Pages : 183
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Book Description
Matrix Assisted Laser Desorption Ionization (MALDI) time of flight (ToF) mass spectrometry is a technique that has been used widely to characterize synthetic polymers. Mass spectrometric characterization is an essential tool in the determination of the comonomer composition and functionality distribution of synthetic polymers. Tandem mass spectrometry (MS/MS) is a two-dimensional technique that characterizes synthetic polymers in more detail. In this dissertation, poly (methyl methacrylate) (PMMA) and poly (methyl acrylate) (PMA) were examined by mass spectrometry (MS) and tandem mass spectrometry (MS/MS). Particular emphasis was devoted to the elucidation of MS/MS fragmentation mechanisms. Such knowledge is a prerequisite for interpreting MS/MS spectra correctly, so that structural information can be deduced from them with confidence. Within the MS/MS studies, a nomenclature was developed to classify MS/MS fragments in a meaningful manner. [Image: Nomenclature for fragments from PMMA chains] Briefly, terminal fragments are labeled by one of the letter codes given in the chart, while internal fragments are labeled by J, K, L, etc. A radical site is indicated by · and the number of repeat units by the subscript. Both, PMMA and PMA chain ionized by alkali metal addition dissociate in the mass spectrometer by homolytic cleavages along the backbone which produce the incipient radical ions a[subscript n]·, b[subscript n]·, y [subscript n]· and z [subscript n]·. These radical ions undergo consecutive, radical-induced reactions which lead to the ultimately observed MS/MS fragments. Radical ions from PMMA as well as PMA dissociate by [beta]-scissions; those from PMA also dissociate by backbiting reactions which produce abundant internal fragments. Hyperbranched acrylate polymers were analyzed by MALDI mass spectrometry and MS/MS. The MALDI-MS data reveal the composition of the polymer, while the MALDI-MS/MS data provide information about the branching architecture. Upon MS/MS, linear as well as hyperbranched polymers dissociate through 1,5-hydrogen rearrangement over the ester group, as also found for polyesters. This reaction leads to unique products from branched isomers, thereby permitting their differentiation from linear isomers. A centrally functionalized polyethylene glycol (f-PEG) star has been investigated by MALDI-MS and MS/MS methods. The mass spectra confirm the repeating unit of 44,Da corresponding to [C2H4O1], and reveal identity of the functionality distributions generated in the synthesis. The fragmentation patterns observed in the MALDI-MS/MS experiments provide information about the lengths of the PEG chains attached to the central substituent. Polyesters are used in many applications, for example, in adhesives, coatings and for packaging. A polyester produced from an aliphatic diacid and an aliphatic diol was analyzed by MALDI mass and tandem mass spectrometry. The MS/MS data show that such polyesters mainly decompose by 1,5-H rearrangement along the ester bond. This behavior is very similar with that found for polyacrylates, where ester moieties are located in the side chains (pendants) instead of the polymer chain. The discovery of this unique dissociation feature, which has been overlooked thus far, opens the possibility to analyze copolymer sequences and branching geometries in ester-containing polymers based on the fragments generated from competitive and consecutive 1,5-H rearrangements. Tung oils were also examined by MALDI-MS and MALDI-MS/MS methods. The mass spectra indicate a triglyceride structure with three fatty acid ester groups, mainly C-18 eleostearates. From the MALDI-MS/MS results, it is possible to determine how the fatty acid chains have been derivatized by the Diel-Alder reaction.
