gel permeation chromatography
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Pharmaceutics ◽  
2022 ◽  
Vol 14 (1) ◽  
pp. 206
Author(s):  
Alexander Pozdnyakov ◽  
Artem Emel’yanov ◽  
Anastasiya Ivanova ◽  
Nadezhda Kuznetsova ◽  
Tat’yana Semenova ◽  
...  

A new hydrophilic polymeric nanocomposite containing AgNPs was synthesized by chemical reduction of metal ions in an aqueous medium in the presence of the copolymer. A new water-soluble copolymer of 1-vinyl-1,2,4-triazole and vinylsulfonic acid sodium salt (poly(VT-co-Na-VSA)) was obtained by free-radical copolymerization and was used as a stabilizing precursor agent. The structural, dimensional, and morphological properties of the nanocomposite were studied by UV–Vis, FTIR, X-ray diffraction, atomic absorption, transmission and scanning electron microscopy, dynamic and electrophoretic light scattering, gel permeation chromatography, thermogravimetric analysis, and differential scanning calorimetry. Hydrodynamic diameter of macroclubs for the copolymer was 171 nm, and for the nanocomposite it was 694 nm. Zeta potential for the copolymer was −63.8 mV, and for the nanocomposite it was −70.4 mV. The nanocomposite had strong antimicrobial activity towards Gram-negative and Gram-positive microorganisms: MIC and MBC values were in the range of 0.25–4.0 and 0.5–8.0 μg/mL, respectively.


Polymers ◽  
2022 ◽  
Vol 14 (2) ◽  
pp. 285
Author(s):  
Yulia S. Dyuzhikova ◽  
Anton A. Anisimov ◽  
Alexander S. Peregudov ◽  
Mikhail I. Buzin ◽  
Galina G. Nikiforova ◽  
...  

New non-crystallizable low-dispersity star-shaped polydimethylsiloxanes (PDMS) containing stereoregular cis-tetra(organo)(dimethylsiloxy)cyclotetrasiloxanes containing methyl-, tolyl- and phenyl-substituents at silicon atoms and the mixture of four stereoisomers of tetra[phenyl(dimethylsiloxy)]cyclotetrasiloxane as the cores were synthesized. Their thermal and viscous properties were studied. All synthesized compounds were characterized by a complex of physicochemical analysis methods: nuclear magnetic resonance (NMR), FT-IR spectroscopy, gel permeation chromatography (GPC), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), viscometry in solution, rheometry, and Langmuir trough study.


2022 ◽  
Author(s):  
Malwina Niedzwiedz ◽  
Gokhan Demirci ◽  
Nina Kantor-Malujdy ◽  
Peter Sobolewski ◽  
Miroslawa El Fray

Photocurable materials that can be delivered as liquids and rapidly (within seconds) cured in situ using UV light are gaining increased interest in advanced minimally invasive procedures. The aim of this work was to synthesize and characterize fatty-acid-derived ester-urethane telechelic (methacrylate) macromonomers, suitable for photopolymerization. The commonly used dibutyltin dilaurate catalyst was replaced with bismuth neodecanoate, bismuth tris(2-ethylhexanoate), and zinc (II) acetyloacetonate as less-toxic alternative catalysts. Additionally, ethyl acetate was used as a “green” solvent. The progress of the two-step synthesis was monitored with infrared spectroscopy. The chemical structure and molecular weight of the obtained viscous materials was characterized with nuclear magnetic resonance spectroscopy and gel permeation chromatography. Photocrosslinking of the macromonomers into elastomeric films was achieved using 150 s per spot of UV light (20 mW/cm2) exposure. Mechanical tensile testing of the films indicated their elasticity up to 120% and low modulus typical for soft and elastomeric materials. Finally, in vitro cytotoxicity tests showed high cell viability for the case of materials synthesized using bismuth and zinc catalysts. Overall, our results indicate that bismuth and zinc catalysts are excellent alternatives to organotin compounds in the synthesis of photocurable methacrylate ester-urethanes for potential biomedical applications.


Polymers ◽  
2022 ◽  
Vol 14 (1) ◽  
pp. 213
Author(s):  
Jihua Duan ◽  
Guichang Jiang

Novel physically crosslinked polyurethane (PUII), based on isophorone diisocyanates, was prepared by a conventional two-step method. The chemical structures of the PUII were characterized by fourier transform infrared (FTIR), proton nuclear magnetic resonance (1H NMR), gel permeation chromatography (GPC), scanning electron microscopy (SEM) and DSC. The PUII hydrogels were subjected to solvent-induced self-assembly in THF + water to construct a variety of morphologies. The self-assembly morphology of the PUII was observed by scanning electron microscopy (SEM). The PUII films with different amounts (0.2%, 0.4%, 0.6%, 0.8%, 1.0%) of 1,3,5-Tris(2-hydroxyethyl)hexahydro-1,3,5-triazine (TNO) were challenged with Escherichia coli, Staphylococcus aureus, Bacillus subtilis and Gray mold. The results showed that when a small amount of antibacterial agent were added, the antibacterial effect of films on Botrytis cinerea was more obvious. The mechanical evaluation shows that the antimicrobial polyurethane films exhibit good mechanical properties.


Materials ◽  
2022 ◽  
Vol 15 (1) ◽  
pp. 380
Author(s):  
Jiangang Yang ◽  
Luhua Luo ◽  
Jie Gao ◽  
Jing Xu ◽  
Chengping He

China’s highway asphalt pavement has entered the stage of major repair, and improving the utilization rate of recycled asphalt pavement (RAP) is the main issue. The key link affecting the performance of recycled asphalt mixtures is the regeneration of aged asphalt, and the effect of the regenerant dosing on the high-temperature performance and viscosity of aged asphalt is the main content to be studied in this research. The aging behavior of asphalt seriously affects the roadworthiness of asphalt mixtures. In this study, we investigated the effect of changes in the microscopic properties of the aged asphalt on its viscosity properties during regeneration using gel permeation chromatography (GPC), Fourier-transform infrared spectroscopy (FTIR), and atomic force microscopy (AFM) as well as Brinell viscosity tests. This study simulated asphalt aging by the RTFOT test, and then we obtained an aged asphalt with a needle penetration of 30. We prepared different regenerated asphalts by adding regeneration agent with doses of 2%, 4%, and 6% to the aged asphalt. The results showed that the regeneration agent could effectively reduce the viscosity of the aged asphalt, which can play a positive role in improving the construction and ease of the aged asphalt. Rejuvenation agents affected the aging asphalt sulfoxide and carbon group indices. Moreover, rejuvenation agents can also significantly reduce the intensities of their characteristic functional group indices. The results of the AFM test showed that the increase in the dose of regeneration agent increased the number of the asphalt bee-like structures and decreased the area of individual bee-like structures. The results of the GPC test were consistent with the results of the AFM test, and the increase in the dose of regeneration agent reduced the asphalt macromolecule content. The viscosity properties and microstructure of the aged asphalt changed positively after the addition of the regeneration agent, indicating that the regeneration agent had a degrading and diluting effect on macromolecules.


Materials ◽  
2022 ◽  
Vol 15 (1) ◽  
pp. 346
Author(s):  
Yeong-Heum Yeon ◽  
Ha-Eun Shim ◽  
Jin-Hyung Park ◽  
Nam-Ho Lee ◽  
Jae-Yeon Park ◽  
...  

The scission rates of polystyrene and fluorinated polystyrene irradiated in an irradiation facility with Co-60 γ-rays were determined using molecular dynamics simulation and gel permeation chromatography (GPC) molecular weight distributions. The prediction was based on the assumption that γ-ray energy is transferred to the initial velocity of the primary knock-on atom. We employed a molecular dynamics simulation procedure to compute the changes in bond length between the connections for selected values of the absorbed dose and compared the calculated values with measurements made on the irradiated samples. The samples were exposed to four different absorbed doses of 25, 50, 75, and 100 kGy. The scission process and scission ratio were simulated with LAMMPS with ReaxFF potential for each bond, and we compared the simulation results with the experimental data especially measuring average molecular weight to evaluate the effect of fluorination on radiation enhancement.


Molecules ◽  
2022 ◽  
Vol 27 (1) ◽  
pp. 266
Author(s):  
Valentina S. Borovkova ◽  
Yuriy N. Malyar ◽  
Irina G. Sudakova ◽  
Anna I. Chudina ◽  
Andrey M. Skripnikov ◽  
...  

Spruce (Piceaabies) wood hemicelluloses have been obtained by the noncatalytic and catalytic oxidative delignification in the acetic acid-water-hydrogen peroxide medium in a processing time of 3–4 h and temperatures of 90–100 °C. In the catalytic process, the H2SO4, MnSO4, TiO2, and (NH4)6Mo7O24 catalysts have been used. A polysaccharide yield of up to 11.7 wt% has been found. The hemicellulose composition and structure have been studied by a complex of physicochemical methods, including gas and gel permeation chromatography, Fourier-transform infrared spectroscopy, and thermogravimetric analysis. The galactose:mannose:glucose:arabinose:xylose monomeric units in a ratio of 5:3:2:1:1 have been identified in the hemicelluloses by gas chromatography. Using gel permeation chromatography, the weight average molar mass Mw of hemicelluloses has been found to attain 47,654 g/mol in noncatalytic delignification and up to 42,793 g/mol in catalytic delignification. Based on the same technique, a method for determining the α and k parameters of the Mark–Kuhn–Houwink equation for hemicelluloses has been developed; it has been established that these parameters change between 0.33–1.01 and 1.57–472.17, respectively, depending on the catalyst concentration and process temperature and time. Moreover, the FTIR spectra of the hemicellulose samples contain all the bands characteristic of heteropolysaccharides, specifically, 1069 cm−1 (C–O–C and C–O–H), 1738 cm−1 (ester C=O), 1375 cm−1 (–C–CH3), 1243 cm−1 (–C–O–), etc. It has been determined by the thermogravimetric analysis that the hemicelluloses isolated from spruce wood are resistant to heating to temperatures of up to ~100 °C and, upon further heating, start destructing at an increasing rate. The antioxidant activity of the hemicelluloses has been examined using the compounds simulating the 2,2-diphenyl-2-picrylhydrazyl free radicals.


Polymers ◽  
2021 ◽  
Vol 14 (1) ◽  
pp. 16
Author(s):  
Jesus Valcarcel ◽  
José Antonio Vázquez ◽  
Uxía R. Varela ◽  
Rui L. Reis ◽  
Ramon Novoa-Carballal

Styela clava is an edible sea squirt farmed in Korea that has gradually invaded other seas, negatively impacting the ecology and economy of coastal areas. Extracts from S. clava have shown wide bioactivities, and ascidians have the unique capability among animals of biosynthesizing cellulose. Thus, S. clava is a relevant candidate for valorization. Herein, we aimed at surveying and characterizing polysaccharides in both tunic and flesh of this ascidian. To this end, we enzymatically hydrolyzed both tissues, recovering crystalline cellulose from the tunic with high aspect ratios, based on results from microscopy, X-ray diffraction, and infrared spectroscopy analyses. Alkaline hydroalcoholic precipitation was applied to isolate the polysaccharide fraction that was characterized by gel permeation chromatography (with light scattering detection) and NMR. These techniques allowed the identification of glycogen in the flesh with an estimated Mw of 7 MDa. Tunic polysaccharides consisted of two fractions of different Mw. Application of Diffusion-Ordered NMR allowed spectroscopically separating the low-molecular-weight fraction to analyze the major component of an estimated Mw of 40–66 kDa. We identified six different sugar residues, although its complexity prevented the determination of the complete structure and connectivities of the residues. The two more abundant residues were N-acetylated and possibly components of the glycosaminoglycan-like (GAG-like) family, showing the remaining similarities to sulfated galactans. Therefore, Styela clava appears as a source of nanocrystalline cellulose and GAG-like polysaccharides.


Holzforschung ◽  
2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Saeid Nikafshar ◽  
Mojgan Nejad

Abstract Susceptibility of wood to UV degradation decreases the service life of wood products outdoors. Organic UV absorbers (UVAs) and hindered amine light stabilizers (HALSs), as well as inorganic UVAs, are added to coatings to improve the UV stability of coated-wood products. Although about 85% of UV radiation is absorbed by lignin in the wood, it is unclear which UV stabilizers can minimize lignin degradation. In this study, the photodegradation of softwood organosolv lignin was monitored over 35 days of UV exposure. Changes in lignin properties were assessed using Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), gel permeation chromatography (GPC), and phosphorus-31 nuclear magnetic resonance spectroscopy (31P NMR). It was found that the aromatic rings of lignin underwent significant degradation, resulting in increased glass transition temperature and molecular weight of lignin. Subsequently, 18 different additives were mixed with lignin and exposed to UV irradiation. The analysis of samples before and after UV exposure with FTIR revealed that inorganic UVAs (cerium oxide and zinc oxide) and a mixture of organic UVAs and HALSs (T-479/T-292, T-5248, and T-5333) were the most effective additives in reducing lignin degradation. This study can help coating scientists to formulate more durable transparent exterior wood coatings.


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