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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 December 2022) | Viewed by 28046

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Prof. Dr. Giulio Malucelli

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Department of Applied Science and Technology, Politecnico di Torino, I-10129 Torino, Italy
Interests: hybrid O/I systems; sol–gel processes; biomacromolecules; biopolymers; flame retardance; structure–property–processing relationships; thermal degradation; polymer (nano)composites
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Prof. Dr. Xavier Colom

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Department of Chemical Engineering, Universitat Politècnica de Catalunya Barcelona Tech, 08222 Terrassa, Barcelona, Spain
Interests: rubber waste; ground tire rubber; biogenic composites; FTIR analysis; TGA analysis; microwave devulcanization
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Special Issue Information

Dear Colleagues,

This Special Issue aims at presenting original articles or reviews on Polymer Analysis. Though the characterization of polymer systems is fundamental for any scientific work, irrespective of the covered topic, it seems very important to get high-level contributions from polymer scientists, who have the opportunity to disseminate the current achievements/recent advances in polymer characterization in a specific Special Issue. Potential topics include but are not limited to:

Progresses in photodegradation and photo-oxidation of polymer and polymer composites;
Thermal behavior of polymer and polymer composites;
Advanced spectroscopy methods for the characterization of polymer systems;
Progresses in morphological characterization of polymers and polymer micro- and nano-composites;
Advances in the characterization of polymerization mechanisms;
Progresses in the characterization of surface properties of bulky polymers and films;
Rheological characterization of polymers and polymer micro- and nano-composites;
Morphological characterization of polymers and polymer micro- and nano-composites;
Mechanical characterization of polymers and polymer micro- and nano-composites;
Structural modification and characterization of polymer and polymer composites

Prof. Dr. Giulio Malucelli
Prof. Dr. Xavier Colom
Guest Editors

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Keywords

FT-IR spectroscopy
NMR spectroscopy
Mechanical behavior
Thermal behavior
Morphological characterization
Flame retardance
Surface properties
Crystallization behavior
Permeability
Rheological behavior

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Published Papers (10 papers)

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Research

14 pages, 3305 KiB

Open AccessArticle

Effect of Hemp Hurd Biochar and Humic Acid on the Flame Retardant and Mechanical Properties of Ethylene Vinyl Acetate

by Mattia Di Maro, Maria Giulia Faga, Riccardo Pedraza, Giulio Malucelli, Mattia Bartoli, Giovanna Gomez d’Ayala and Donatella Duraccio

Polymers 2023, 15(6), 1411; https://doi.org/10.3390/polym15061411 - 12 Mar 2023

Cited by 2 | Viewed by 2060

Abstract

In this work, the combination of biochar produced through a pyrolytic process of hemp hurd with commercial humic acid as a potential biomass-based flame-retardant system for ethylene vinyl acetate copolymer is thoroughly investigated. To this aim, ethylene vinyl acetate composites containing hemp-derived biochar at two different concentrations (i.e., 20 and 40 wt.%) and 10 wt.% of humic acid were prepared. The presence of increasing biochar loadings in ethylene vinyl acetate accounted for an increasing thermal and thermo-oxidative stability of the copolymer; conversely, the acidic character of humic acid anticipated the degradation of the copolymer matrix, even in the presence of the biochar. Further, as assessed by forced-combustion tests, the incorporation of humic acid only in ethylene vinyl acetate slightly decreased both peaks of heat release rate (pkHRR) and total heat release (THR, by 16% and 5%, respectively), with no effect on the burning time. At variance, for the composites containing biochar, a strong decrease in pkHRR and THR values was observed, approaching −69 and −29%, respectively, in the presence of the highest filler loading, notwithstanding, for this latter, a significant increase in the burning time (by about 50 s). Finally, the presence of humic acid significantly lowered the Young’s modulus, unlike biochar, for which the stiffness remarkably increased from 57 MPa (unfilled ethylene vinyl acetate) to 155 Mpa (for the composite containing 40 wt.% of the filler). Full article

(This article belongs to the Special Issue Feature Papers in Polymer Analysis)

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22 pages, 5893 KiB

Open AccessArticle

Damping Properties of Large-Scale Overlap Joints Bonded with Epoxy Hybrid Resin or Polyurethanes: Experimental Characterisation and Analytical Description

by Jannis Damm and Matthias Albiez

Polymers 2023, 15(5), 1102; https://doi.org/10.3390/polym15051102 - 22 Feb 2023

Cited by 1 | Viewed by 1660

Abstract

Structures in various industries are exposed to dynamic loads. The dissipative properties of adhesively bonded joints can contribute to the damping of dynamically stressed structures. Dynamic hysteresis tests are carried out to determine the damping properties of adhesively bonded overlap joints by varying the geometry and test boundary conditions. The dimensions of the overlap joints are full-scale and thus relevant for steel construction. Based on the results of experimental investigations, a methodology is developed for the analytic determination of the damping properties of adhesively bonded overlap joints for various specimen geometries and stress boundary conditions. For this purpose, dimensional analysis is carried out using the Buckingham Pi Theorem. In summary, it can be stated that the loss factor of adhesively bonded overlap joints investigated within this study is in the range between 0.16 and 0.41. The damping properties can particularly be increased by increasing the adhesive layer thickness and reducing the overlap length. The functional relationships of all the test results shown can be determined by dimensional analysis. An analytical determination of the loss factor considering all identified influencing factors is enabled by derived regression functions with a high coefficient of determination. Full article

(This article belongs to the Special Issue Feature Papers in Polymer Analysis)

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12 pages, 4297 KiB

Open AccessArticle

Rubber-Composite-Nanoparticle-Modified Epoxy Powder Coatings with Low Curing Temperature and High Toughness

by Run Zhang, Haosheng Wang, Xiaoze Wang, Jian Guan, Meiqi Li and Yunfa Chen

Polymers 2023, 15(1), 195; https://doi.org/10.3390/polym15010195 - 30 Dec 2022

Cited by 6 | Viewed by 2315

Abstract

In this study, a rubber-composite-nanoparticle-modified epoxy powder composite coating with low curing temperature and high toughness was successfully fabricated. The effects of N,N-dimethylhexadecylamine (DMA) carboxy-terminated nitrile rubber (CNBR) composite nanoparticles on the microstructure, curing behavior, and mechanical properties of epoxy-powder coating were systematically investigated. SEM and TEM analysis revealed a uniform dispersion of DMA-CNBR in the epoxy-powder coating, with average diameter of 100 nm. The curing temperature of the epoxy-composite coatings had reduced almost 19.1% with the addition of 1phr DMA-4CNBR into the coating. Impact strength tests confirmed that DMA-CNBR-modified epoxy-composite coatings showed significant improvements compared with the neat EP coating, which was potentially attributed to the nanoscale dispersion of DMA-CNBR particles in epoxy coatings and their role in triggering microcracks. Other mechanical properties, including adhesion and cupping values, were improved in the same manner. In addition, thermal and surface properties were also studied. The prepared epoxy composite powder coating with the combination of low curing temperature and high toughness broadened the application range of the epoxy coatings. Full article

(This article belongs to the Special Issue Feature Papers in Polymer Analysis)

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10 pages, 2752 KiB

Open AccessArticle

On the Applicability of Electrophoresis for Protein Quantification

by Karina Dome, Zoya Akimenko, Aleksey Bychkov, Yuri Kalambet and Oleg Lomovsky

Polymers 2021, 13(22), 3971; https://doi.org/10.3390/polym13223971 - 17 Nov 2021

Viewed by 2672

Abstract

Polyacrylamide gel electrophoresis is widely used for studying proteins and protein-containing objects. However, it is employed most frequently as a qualitative method rather than a quantitative one. This paper shows the feasibility of routine digital image acquisition and mathematical processing of electropherograms for protein quantification when using vertical gel electrophoresis and Chrom & Spec software. Both the well-studied model protein molecules (bovine serum albumin) and more complex real-world protein-based products (casein-containing isolate for sports nutrition), which were subjected to mechanical activation in a planetary ball mill to obtain samples characterized by different protein denaturation degrees, were used as study objects. Protein quantification in the mechanically activated samples was carried out. The degree of destruction of individual protein was shown to be higher compared to that of the protein-containing mixture after mechanical treatment for an identical amount of time. The methodological approach used in this study can serve as guidance for other researchers who would like to use electrophoresis for protein quantification both in individual form and in protein mixtures. The findings prove that photographic imaging of gels followed by mathematical data processing can be applied for analyzing the electrophoretic data as an affordable, convenient and quick tool. Full article

(This article belongs to the Special Issue Feature Papers in Polymer Analysis)

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17 pages, 2370 KiB

Open AccessArticle

Structure of Polytetrafluoroethylene Modified by the Combined Action of γ-Radiation and High Temperatures

by Alexander Sergeevich Smolyanskii, Ekaterina Dmitrievna Politova, Ol’ga Alekseevna Koshkina, Mikhail Aleksandrovich Arsentyev, Pavel Prokof’evich Kusch, Lev Vladimirovich Moskvitin, Sergei Vital’evich Slesarenko, Dmitrii Pavlovich Kiryukhin and Leonid Izrailevich Trakhtenberg

Polymers 2021, 13(21), 3678; https://doi.org/10.3390/polym13213678 - 25 Oct 2021

Cited by 14 | Viewed by 3533

Abstract

By means of X-ray computed microtomography (XCMT), the existence of a developed porous structure with an average pore diameter of ~3.5 μm and pore content of ~1.1 vol.% has been revealed in unirradiated polytetrafluoroethylene (PTFE). It has been found that the combined action of gamma radiation (absorbed dose per PTFE of ~170 kGy) and high temperatures (327–350 °C) leads to the disappearance of the porous structure and the formation of several large pores with sizes from 30 to 50 μm in the bulk of thermal-radiation modified PTFE (TRM-PTFE). It has been established by X-ray diffraction (XRD) analysis that the thermal-radiation modification of PTFE leads to an increase in the interplanar spacings, the degree of crystallinity and the volume of the unit cell, as well as to a decrease in the size of crystals and the X-ray density of the crystalline phase in comparison with the initial polymer. It is assumed that the previously-established effect of improving the deformation-strength and tribological properties of the TRM-PTFE can be due not only to the radiation cross-linking of polymer chains but also to the disappearance of the pore system and to the ordering of the crystalline phase of PTFE. Full article

(This article belongs to the Special Issue Feature Papers in Polymer Analysis)

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14 pages, 2796 KiB

Open AccessArticle

Manipulating Crystallization for Simultaneous Improvement of Impact Strength and Heat Resistance of Plasticized Poly(l-lactic acid) and Poly(butylene succinate) Blends

by Todsapol Kajornprai, Supakij Suttiruengwong and Kalyanee Sirisinha

Polymers 2021, 13(18), 3066; https://doi.org/10.3390/polym13183066 - 10 Sep 2021

Cited by 9 | Viewed by 3314

Abstract

Crystalline morphology and phase structure play a decisive role in determining the properties of polymer blends. In this research, biodegradable blends of poly(l-lactic acid) (PLLA) and poly(butylene succinate) (PBS) have been prepared by melt-extrusion and molded into specimens with rapid cooling. The crystalline morphology (e.g., crystallinity, crystal type and perfection) is manipulated by annealing the molded products from solid-state within a short time. This work emphasizes on the effects of annealing conditions on crystallization and properties of the blends, especially impact toughness and thermal stability. Phase-separation morphology with PBS dispersed particles smaller than 1 μm is created in the blends. The blend properties are successfully dictated by controlling the crystalline morphology. Increasing crystallinity alone does not ensure the enhancement of impact toughness. A great improvement of impact strength and heat resistance is achieved when the PLLA/PBS (80/20) blends are plasticized with 5% medium molecular-weight poly(ethylene glycol), and simultaneously heat-treated at a temperature close to the cold-crystallization of PLLA. The plasticized blend annealed at 92 °C for only 10 min exhibits ten-fold impact strength over the starting PLLA and slightly higher heat distortion temperature. The microscopic study demonstrates the fracture mechanism changes from crazing to shear yielding in this annealed sample. Full article

(This article belongs to the Special Issue Feature Papers in Polymer Analysis)

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16 pages, 2822 KiB

Open AccessArticle

The Relationship between Free Volume and Cooperative Rearrangement: From the Temperature-Dependent Neutron Total Scattering Experiment of Polystyrene

by Zehua Han, Guisheng Jiao, Changli Ma, Taisen Zuo, Charles C. Han and He Cheng

Polymers 2021, 13(18), 3042; https://doi.org/10.3390/polym13183042 - 9 Sep 2021

Cited by 1 | Viewed by 2152

Abstract

Although many theories have been proposed to describe the nature of glass formation, its microscopic picture is still missing. Here, by a combination of neutron scattering and molecular dynamics simulation, we present the temperature-dependent atomic structure variation of polystyrene at the glass formation, free volume and cooperative rearrangement. When it is close to glass formation, the polymer is confined in tubes, whose diameter is the main chain–main chain distance, in a “static cage” from its neighbors. This definition can not only account for the kinetic pathway dependence of Williams-Landel-Ferry (WLF) free volume, but also be testified in a set of six polymers. However, the free volume which allows a monomer to move cannot be found in any frame of its real-space image. Monomers, thus, have to move cooperatively to be out of the cage. During glass formation, dynamic heterogeneity develops, and string-like cooperative rearrangement region (CRR) grows over a long range of time and length scales. All of these CRRs tend to walk through loose “static cages”. Our observation unifies the concepts of free volume and cooperative rearrangement. The former is a statistical average leading to a polydisperse “static cage” formation; while a loose “static cage” provides the way that CRRs move. Full article

(This article belongs to the Special Issue Feature Papers in Polymer Analysis)

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12 pages, 2945 KiB

Open AccessArticle

Quantitative Analysis of Blended Asian Lacquers Using ToF–SIMS, Py–GC/MS and HPLC

by Hye Hyun Yu, Jung-Ah Lim, Seung Wook Ham, Kang-Bong Lee and Yeonhee Lee

Polymers 2021, 13(1), 97; https://doi.org/10.3390/polym13010097 - 29 Dec 2020

Cited by 9 | Viewed by 3444

Abstract

Asian lacquer is a special polymeric material tapped from lacquer trees. The tree’s sap is a complex mixture of compounds, such as catechol lipids, polysaccharides, glycoproteins, enzymes, and water. Researchers have not yet quantitatively analyzed blended lacquers. We evaluated the compositions of Japanese and Vietnamese lacquers, and blends of the two, using time-of-flight secondary ion mass spectrometry (ToF–SIMS), pyrolysis–gas chromatography/mass spectrometry (Py–GC/MS), and high-performance liquid chromatography (HPLC). ToF–SIMS provided quantitative results for blended lacquers; provided structural information on polymeric lacquer films; and indicated the presence of dimers of urushiol–urushiol, urushiol–laccol, and laccol–laccol derivatives. We used Py–GC/MS and HPLC to obtain linear calibration curves. The specific peak intensity was a linear function of the ratio of Japanese to Vietnamese lacquer in the blends. For an unknown mixture, all three techniques gave essentially the same results. These quantitative methods will be useful for improving the physical properties of polymeric lacquer films, and evaluating the lacquer quality in industry and historic conservation. Full article

(This article belongs to the Special Issue Feature Papers in Polymer Analysis)

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14 pages, 3103 KiB

Open AccessArticle

Probing Effect of Papirindustriens Forskningsinstitut (PFI) Refining on Aggregation Structure of Cellulose: Crystal Packing and Hydrogen-Bonding Network

by Kunpeng Li, Lihong Zhao and Beihai He

Polymers 2020, 12(12), 2912; https://doi.org/10.3390/polym12122912 - 4 Dec 2020

Cited by 6 | Viewed by 2360

Abstract

Supramolecular structure is the critical factor that affects the properties of cellulosic fibers. This article studied the action of Papirindustriens forskningsinstitut (PFI) refining on the molecular aggregation and hydrogen bonding network, and tried to explore the relationship between the crystal packing and hydrogen-bonding network in cellulosic fibers. The results showed that the polymorph, H-bonding distance, and H-bonding energy of various H-bonds remained almost unchanged, while the crystalline index, crystallite size, and content of various H-bonds changed with refining. Therein, the content of the inter-molecular O(6)H⋯O(3′) H-bonds was significantly correlated with the crystalline index that was obtained in intensities of the XRD peaks. The Pearson correlation coefficient between them was 0.888 (p < 0.05) for softwood fibers and 0.889 (p < 0.05) for hardwood fibers, respectively. It can be concluded that the variations of accessibility, swelling, and fibrillation were closely related to the supramolecular structure and the intermolecular H-bonds play an important role in the crystal packing of cellulose. Full article

(This article belongs to the Special Issue Feature Papers in Polymer Analysis)

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20 pages, 4970 KiB

Open AccessArticle

Application Properties Analysis as a Dielectric Capacitor of End-of-Life Tire-Reinforced HDPE

by Marc Marín-Genescà, Jordi García-Amorós, Ramon Mujal-Rosas, Lluís Massagués Vidal and Xavier Colom Fajula

Polymers 2020, 12(11), 2675; https://doi.org/10.3390/polym12112675 - 12 Nov 2020

Cited by 10 | Viewed by 2731

Abstract

The purpose of the present research is to obtain waste of polymeric composite as an insulator capacitive application. Rubber materials, once they end their useful life, may be difficult to reuse or recycle. At present, research only uses one tire recycling method, which involves grinding and separating steel and fibers from vulcanized rubber, and then using the rubber particles for industrial capacitors. The methodology for this research is to compare the permittivity (ε′ and ε″) between high-density polyethylene (HDPE) and the polymer matrix compound, consisting of an HDPE polymeric matrix blended with end-of-life tire particles (ground tire rubber (GTR)), to analyze the feasibility of using such tires as electrically insulating materials (dielectrics). The incorporation of carbon black in the GTR compounds modifies conductivity; GTRs carry a significant amount of carbon black, and therefore some electrical properties may change significantly compared to highly insulating polymer substrates. The performed experimental study is based on a dynamic electric analysis (DEA) test developed in the frequency range of 10⁻² Hz to 3 MHz and at different temperatures (from 35 to 70 °C) of different samples type: HDPE neat and HDPE compounds with 10%, 20% and 40% of GTR loads. A sample’s electrical behavior is checked for its dependence on frequency and temperature, focused on the permittivity property; this is a key property for capacitive insulators and is key for examining the possible applications in this field, for HDPE + GTR blends. Results for the permittivity behavior and the loss factor show different electrical behavior. For a neat HDPE sample, no dependence with frequency nor temperature is shown. However, with the addition of 10%, 20%, and 40% amount of GTR the HDPE compounds show different behaviors: for low frequencies, interfacial polarization relaxation is seen, due to the Maxwell–Wagner–Sillars (MWS) effect, performed in heterogeneous materials. In order to analyze thermal and morphological properties the differential scanning calorimetry (DSC) test and scanning electron microscopy (SEM) have been used. Results obtained show that adding waste tire particles in an HDPE matrix allows HDPE + 40% GTR blends to act as a dielectric in capacitors, increasing the capacitor dielectric efficiency in the low frequencies due to the MWS effect, which increases the dielectric constant. Full article

(This article belongs to the Special Issue Feature Papers in Polymer Analysis)

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