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Polymers
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Polymer Mass Spectrometry
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Polymer Mass Spectrometry

A special issue of Polymers (ISSN 2073-4360). This special issue belongs to the section "Polymer Analysis and Characterization".

Deadline for manuscript submissions: closed (20 March 2019) | Viewed by 30130

Special Issue Editors

Prof. Dr. Marek M. Kowalczuk

E-Mail Website
Guest Editor
Centre of Polymer and Carbon Materials Polish Academy of Sciences, PL-41819 Zabrze, Poland
Interests: biocompatible and biodegradable polymer systems; polymer mass spectrometry; bioactive oligomers; controlled drug delivery systems; ring-opening polymerization; forensic engineering of advanced polymeric materials
Special Issues, Collections and Topics in MDPI journals
Prof. Dr. Grażyna Adamus

E-Mail Website
Guest Editor
Centre of Polymer and Carbon Materials, Polish Academy of Sciences, M. Curie-Skłodowskiej 34, 41-819 Zabrze, Poland
Interests: polymers from renewable resources; synthesis of functional polymers; structure–property relationships; novel polymeric materials of controlled biodegradability; application of mass spectrometry techniques to the structural study of synthetic polymers at the molecular level
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Mass spectrometry (MS) represents a powerful toolset for the structural characterization of polymers. Progress in this area has been tremendous ever since covers the novel mass spectrometry characterization methods as well as the polymers that have been analysed. MS can be successfully applied for the characterization of natural polymers, as well as their derivatives, and may also be helpful in the synthesis of (co)polymers from natural and non-renewable sources. Moreover, mass spectrometry is currently needed for the evaluation and understanding of the relationships among structure, properties, and behavior (before, during and after practical applications) of advanced polymeric materials important for civilization and social function.

The development of soft ionization techniques in MS have helped to solve the difficult question regarding the molecular structure of (co)polymers. Application of “such” ionization techniques, generating predominantly quasi-molecular or adduct ions, enables sequence analysis of natural and synthetic macromolecules. It permits the production of gas-phase ions from a wide variety of polymers, with little or no fragmentation during ionization.

Polymer scientists have been unfamiliar with the advances made in the field of modern mass spectrometry for a long time. However, MS sequence analysis of synthetic macromolecules can be helpful for the specific area of applied research on polymeric materials. Multistage mass spectrometry (MSn) enables the structural analysis of mass selected macromolecular ions of (co)polymers at the molecular level. Therefore, it may be expected that MSn will become a routine and accurate analytical technique of (co)polymers for years to come.

In this Special Issue, we aim to present a contemporary overview of recent developments in the field of polymer mass spectrometry. Reviews, full papers, and short communications of the current trends in this area of knowledge are all welcome.

Prof. Marek M. Kowalczuk
Prof. Grazyna Adamus
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Polymers is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2700 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • New ionization techniques in polymer mass spectrometry
  • Ion mobility mass spectrometry for polymers
  • MS for polymerization reaction mechanisms
  • DESI-MS in polymer analysis
  • Sequence analysis of synthetic macromolecules
  • Decoding of polymeric materials molecular labeling

Published Papers (6 papers)

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Research

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20 pages, 5629 KiB  
Article
Mass Spectrometry Reveals Molecular Structure of Polyhydroxyalkanoates Attained by Bioconversion of Oxidized Polypropylene Waste Fragments
by Brian Johnston, Iza Radecka, Emo Chiellini, David Barsi, Vassilka Ivanova Ilieva, Wanda Sikorska, Marta Musioł, Magdalena Zięba, Paweł Chaber, Adam A. Marek, Barbara Mendrek, Anabel Itohowo Ekere, Grazyna Adamus and Marek Kowalczuk
Polymers 2019, 11(10), 1580; https://doi.org/10.3390/polym11101580 - 27 Sep 2019
Cited by 33 | Viewed by 5130
Abstract
This study investigated the molecular structure of the polyhydroxyalkanoate (PHA) produced via a microbiological shake flask experiment utilizing oxidized polypropylene (PP) waste as an additional carbon source. The bacterial strain Cupriavidus necator H16 was selected as it is non-pathogenic, genetically stable, robust, and [...] Read more.
This study investigated the molecular structure of the polyhydroxyalkanoate (PHA) produced via a microbiological shake flask experiment utilizing oxidized polypropylene (PP) waste as an additional carbon source. The bacterial strain Cupriavidus necator H16 was selected as it is non-pathogenic, genetically stable, robust, and one of the best known producers of PHA. Making use of PHA oligomers, formed by controlled moderate-temperature degradation induced by carboxylate moieties, by examination of both the parent and fragmentation ions, the ESI-MS/MS analysis revealed the 3-hydroxybutyrate and randomly distributed 3-hydroxyvalerate as well as 3-hydroxyhexanoate repeat units. Thus, the bioconversion of PP solid waste to a value-added product such as PHA tert-polymer was demonstrated. Full article
(This article belongs to the Special Issue Polymer Mass Spectrometry)
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12 pages, 3118 KiB  
Article
Sequencing of Side-Chain Liquid Crystalline Copolymers by Matrix-Assisted Laser Desorption/Ionization Tandem Mass Spectrometry
by Savannah R. Snyder, Wei Wei, Huiming Xiong and Chrys Wesdemiotis
Polymers 2019, 11(7), 1118; https://doi.org/10.3390/polym11071118 - 01 Jul 2019
Cited by 5 | Viewed by 4550
Abstract
Polyether based side-chain liquid crystalline (SCLC) copolymers with distinct microstructures were prepared using living anionic polymerization techniques. The composition, end groups, purity, and sequence of the resulting copolymers were elucidated by matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) and tandem mass spectrometry (MS/MS). MALDI-MS [...] Read more.
Polyether based side-chain liquid crystalline (SCLC) copolymers with distinct microstructures were prepared using living anionic polymerization techniques. The composition, end groups, purity, and sequence of the resulting copolymers were elucidated by matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) and tandem mass spectrometry (MS/MS). MALDI-MS analysis confirmed the presence of (CH3)3CO– and –H end groups at the initiating (α) and terminating (ω) chain end, respectively, and allowed determination of the molecular weight distribution and comonomer content of the copolymers. The comonomer positions along the polymer chain were identified by MS/MS, from the fragments formed via C–O and C–C bond cleavages in the polyether backbone. Random and block architectures could readily be distinguished by the contiguous fragment series formed in these reactions. Notably, backbone C–C bond scission was promoted by a radical formed via initial C–O bond cleavage in the mesogenic side chain. This result documents the ability of a properly substituted side chain to induce sequence indicative bond cleavages in the polyether backbone. Full article
(This article belongs to the Special Issue Polymer Mass Spectrometry)
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13 pages, 1622 KiB  
Article
One Step Further in the Characterization of Synthetic Polymers by Ion Mobility Mass Spectrometry: Evaluating the Contribution of End-groups
by Quentin Duez, Romain Liénard, Sébastien Moins, Vincent Lemaur, Olivier Coulembier, Jérôme Cornil, Pascal Gerbaux and Julien De Winter
Polymers 2019, 11(4), 688; https://doi.org/10.3390/polym11040688 - 16 Apr 2019
Cited by 10 | Viewed by 3143
Abstract
Several families of polymers possessing various end-groups are characterized by ion mobility mass spectrometry (IMMS). A significant contribution of the end-groups to the ion collision cross section (CCS) is observed, although their role is neglected in current fitting models described in literature. Comparing [...] Read more.
Several families of polymers possessing various end-groups are characterized by ion mobility mass spectrometry (IMMS). A significant contribution of the end-groups to the ion collision cross section (CCS) is observed, although their role is neglected in current fitting models described in literature. Comparing polymers prepared from different synthetic procedures might thus, be misleading with the current theoretical treatments. We show that this issue is alleviated by comparing the CCS of various polymer ions (polyesters and polyethers) as a function of the number of atoms in the macroion instead of the usual representation involving the degree of polymerization. Finally, we extract the atom number density from the spectra which gives us the possibility to evaluate the compaction of polymer ions, and by extension to discern isomeric polymers. Full article
(This article belongs to the Special Issue Polymer Mass Spectrometry)
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9 pages, 1504 KiB  
Article
Evaluating Phthalate Contaminant Migration Using Thermal Desorption–Gas Chromatography–Mass Spectrometry (TD–GC–MS)
by Yukihiro Ouchi, Hiroyuki Yanagisawa and Shigehiko Fujimaki
Polymers 2019, 11(4), 683; https://doi.org/10.3390/polym11040683 - 15 Apr 2019
Cited by 16 | Viewed by 5756
Abstract
This study describes a methodology for evaluating regulatory levels of phthalate contamination. By collecting experimental data on short-term phthalate migration using thermal desorption–gas chromatography–mass spectrometry (TD–GC–MS), the migration of di(2-ethylhexyl) phthalate (DEHP) from polyvinyl chloride (PVC) to polyethylene (PE) was found to be [...] Read more.
This study describes a methodology for evaluating regulatory levels of phthalate contamination. By collecting experimental data on short-term phthalate migration using thermal desorption–gas chromatography–mass spectrometry (TD–GC–MS), the migration of di(2-ethylhexyl) phthalate (DEHP) from polyvinyl chloride (PVC) to polyethylene (PE) was found to be expressed by the Fickian approximation model, which was originally proposed for solid (PVC)/liquid (solvent) migration of phthalates. Consequently, good data correlation was obtained using the Fickian approximation model with a diffusion coefficient of 4.2 × 10−12 cm2/s for solid (PVC)/ solid (PE) migration of DEHP at 25 °C. Results showed that temporary contact with plasticized polymers under a normal, foreseeable condition may not pose an immediate risk of being contaminated by phthalates at regulatory levels. However, as phthalates are small organic molecules designed to be dispersed in a variety of polymers as plasticizers at a high compounding ratio, the risk of migration-related contamination can be high in comparison with other additives, especially under high temperatures. With these considerations in mind, the methodology for examining regulatory levels of phthalate contamination using TD–GC–MS has been successfully demonstrated from the viewpoint of its applicability to solid (PVC)/solid (PE) migration of phthalates. Full article
(This article belongs to the Special Issue Polymer Mass Spectrometry)
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9 pages, 1774 KiB  
Article
Mass Spectrometric Characterization of Epoxidized Vegetable Oils
by Ákos Kuki, Tibor Nagy, Mahir Hashimov, Stella File, Miklós Nagy, Miklós Zsuga and Sándor Kéki
Polymers 2019, 11(3), 394; https://doi.org/10.3390/polym11030394 - 28 Feb 2019
Cited by 7 | Viewed by 4089
Abstract
Matrix-assisted laser desorption ionization and electrospray ionization mass spectrometry (MALDI-MS and ESI-MS) were used for the characterization of epoxidized soybean and linseed oils, which are important raw materials in the biopolymer production. The recently invented data mining approach, mass-remainder analysis (MARA), was implemented [...] Read more.
Matrix-assisted laser desorption ionization and electrospray ionization mass spectrometry (MALDI-MS and ESI-MS) were used for the characterization of epoxidized soybean and linseed oils, which are important raw materials in the biopolymer production. The recently invented data mining approach, mass-remainder analysis (MARA), was implemented for the analysis of these types of complex natural systems. Different epoxidized triglyceride mass spectral peak series were identified, and the number of carbon atoms and epoxide groups was determined. The fragmentation mechanisms of the epoxidized triglyceride (ETG) adducts formed with different cations (such as H+, Na+, Li+, and NH4+) were explored. As a novel approach, the evaluation of the clear fragmentation pathways of the sodiated ETG adducts enabled the estimation of the epoxidized fatty acid compositions of these types of oils by MS/MS. Full article
(This article belongs to the Special Issue Polymer Mass Spectrometry)
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Review

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15 pages, 2768 KiB  
Review
Potential of Liquid Extraction Surface Analysis Mass Spectrometry (LESA—MS) for the Characterization of Polymer-Based Materials
by Ambre Issart and Joanna Szpunar
Polymers 2019, 11(5), 802; https://doi.org/10.3390/polym11050802 - 05 May 2019
Cited by 6 | Viewed by 5050
Abstract
Liquid extraction surface analysis mass spectrometry (LESA -MS) is a direct analysis method suitable for the analysis of polymers. It is based on a fast and efficient extraction of polymer components, such as non-intentionally added species (NIAS), post-polymerization residues, or additives, and residues [...] Read more.
Liquid extraction surface analysis mass spectrometry (LESA -MS) is a direct analysis method suitable for the analysis of polymers. It is based on a fast and efficient extraction of polymer components, such as non-intentionally added species (NIAS), post-polymerization residues, or additives, and residues resulting from specific uses followed by their MS detection. In comparison with batch methods, it is a “green” method, using negligible volumes of organic solvents, and it is cost-effective, avoiding lengthy sample preparation procedures. It can be used for the detection of known molecules (targeted analysis), identification of unknown species (exploratory analysis requiring MS/MS) and semi-quantative analysis, if standards are available. The to-date applications of LESA-MS in the field of polymer science are reviewed and critically discussed taking into account the hands-on experience from the authors’ laboratory. Future possibilities of LESA applications are highlighted. Full article
(This article belongs to the Special Issue Polymer Mass Spectrometry)
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