The Raman Spectroscopy, XRD, SEM, and AFM Study of Arabinogalactan Sulfates Obtained Using Sulfamic Acid

Кузнецов, Б. Н.; Vasilyeva, Natalya Yu.; Levdansky, Alexander V.; Karacharov, Anton; Крылов, А. С.; Mazurova, E. V.; Бондаренко, Г. Н.; Levdansky, Vladimir A.; Kazachenko, Аleksandr S.

doi:10.1134/s106816201707010x

Cited by 10 publications

(12 citation statements)

References 4 publications

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“…numerical aperture, provides a focal spot diameter of about 3 μm on the sample [66,67]. Singlemode argon 457.9 nm line from a Spectra-Physics Stabilite 2017 Ar + laser of 1 mW on the sample was used as an excitation light source.…”

Section: Experimental Methodsmentioning

confidence: 99%

Exploration of structural, thermal and spectroscopic properties of self-activated sulfate Eu2(SO4)3 with isolated SO4 groups

Denisenko

Aleksandrovsky

Atuchin

et al. 2018

Journal of Industrial and Engineering Chemistry

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Eu2(SO4)3 was synthesized by chemical precipitation method and the crystal structure was determined by Rietveld analysis. The compound crystallizes in monoclinic space group С2/с. In the air environment, Eu2(SO4)3 is stable up to 670°C. The sample of Eu2(SO4)3 was examined by Raman, Fourier-transform infrared absorption and luminescence spectroscopy methods. The low site symmetry of SO4 tetrahedra results in the appearance of the IR inactive ν1 mode around 1000 cm-1 and ν2 modes below 500 cm-1. The band intensities redistribution in the luminescent spectra of Eu 3+ ions is analyzed in terms of the peculiarities of its local environment.

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Section: Experimental Methodsmentioning

confidence: 99%

Exploration of structural, thermal and spectroscopic properties of self-activated sulfate Eu2(SO4)3 with isolated SO4 groups

Denisenko

Aleksandrovsky

Atuchin

et al. 2018

Journal of Industrial and Engineering Chemistry

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“…Current methods of AG sulfates producing are based on the use of aggressive and environmentally hazardous sulfating agents such as sulfuric anhydride and chlorosulfonic acid [ 13 , 14 , 15 , 22 , 23 , 24 , 26 ]. We also developed a new, simple and environmentally friendly than known, method for the synthesis of sulfated arabinogalact by sulfation of arabinogalactan with sulfamic acid in dioxane in the presence of the main catalyst—urea [ 25 ]—and studied the physicochemical properties of the sulfated arabinogalactan obtained by this method [ 34 ]. Samples of sulfated arabinogalactan with different sulfur content were isolated depending on the process conditions.…”

Section: Introductionmentioning

confidence: 99%

“…Samples of sulfated arabinogalactan with different sulfur content were isolated depending on the process conditions. Therefore, controlling the characteristics of sulfated polysaccharides with a specified molecular weight as anticoagulants during their synthesis is of great practical importance in the continuation of these studies [ 25 , 34 ].…”

Section: Introductionmentioning

confidence: 99%

Modification of Arabinogalactan Isolated from Larix sibirica Ledeb. into Sulfated Derivatives with the Controlled Molecular Weights

et al. 2021

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The process of sulfation of arabinogalactan—a natural polysaccharide from Larix sibirica Ledeb.—with sulfamic acid in 1,4-dioxane using different activators has been studied for the first time. The dynamics of the molecular weight of sulfated arabinogalactan upon variation in the temperature and time of sulfation of arabinogalactan with sulfamic acid in 1,4-dioxane has been investigated. It has been found that, as the sulfation time increases from 10 to 90 min, the molecular weights of the reaction products grow due to the introduction of sulfate groups without significant destruction of the initial polymer and sulfation products. Sulfation at 95 °C for 20 min yields the products with a higher molecular weight than in the case of sulfation at 85 °C, which is related to an increase in the sulfation rate; however, during the further process occurring under these conditions, sulfation is accompanied by the destruction and the molecular weight of the sulfated polymer decreases. The numerical optimization of arabinogalactan sulfation process has been performed. It has been shown that the optimal parameters for obtaining a product with a high sulfur content are a sulfamic acid amount of 20 mmol per 1 g of arabinogalactan, a process temperature of 85 °C, and a process time of 2.5 h.

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“…The synthesized sulfated galactomannan films are studied by the AFM technique (Fig. 5),which allows one to measure not only the lateral dimensions of nanoscale objects but also their height with the high (up to 0.1 nm) accuracy [39,40]. According to the AFM data, the sulfated galactomannan film surface consists of homogeneous spherical particles with an average diameter from 200 to 300 nm.…”

Section: Atomic Force Microscopymentioning

confidence: 99%

“…7) [38,42,43]. It is well-known [37,[40][41][42] that the pyrolysis of polysaccharides is initiated by random destruction of glycosidic bonds with the subsequent decomposition. Thermograms contain peaks at 254°C and 209°C for the GM and SGM, respectively.…”

Section: Thermal Analysismentioning

confidence: 99%

«Green» synthesis and characterization of galactomannan sulfates obtained using sulfamic acid

Kazachenko

Malyar

Vasilyeva

et al. 2020

Biomass Conv. Bioref.

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The "green" synthesis of galactomannan sulfates using a sulfamic acid-urea mixture has been studied for the first time. The effect of the time and temperature of the galactomannan sulfation process on the degree of substitution of galactomannan sulfates has been investigated. It is shown that, at a temperature of 70°C with an increase in the process time up to 120 min, the degree of substitution increases up to 0.70. An increase in the process temperature up to 80°C leads to the production of galactomannan sulfates with a degree of substitution of 1.67. With a further increase in the process temperature to 90°C, the galactomannan structure is partially destructed, and the degree of substitution decreases. Embedding of the sulfate groups into the galactomannan structure has been confirmed by elemental analysis and Fourier-transform infrared spectroscopy. In addition, the initial and sulfated galactomannans have been characterized by X-ray diffraction, scanning electron microscopy, atomic force microscopy, and gel permeation chromatography. The thermal analysis shows that the initial galactomannan exhibits endothermic peaks at 254 and 294°C and an exothermic peak at 315°C, while sulfated galactomannan exhibits endothermic peaks at 209 and 275°C and an exothermic peak at 281°C. Using atomic force microscopy, it has been shown that the sulfated galactomannan film consists of spherical particles with an average diameter of 200-300 nm; according to the phase contrast data, it has the uniform composition without extraneous impurities.

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The Raman Spectroscopy, XRD, SEM, and AFM Study of Arabinogalactan Sulfates Obtained Using Sulfamic Acid

Cited by 10 publications

References 4 publications

Exploration of structural, thermal and spectroscopic properties of self-activated sulfate Eu2(SO4)3 with isolated SO4 groups

Exploration of structural, thermal and spectroscopic properties of self-activated sulfate Eu2(SO4)3 with isolated SO4 groups

Modification of Arabinogalactan Isolated from Larix sibirica Ledeb. into Sulfated Derivatives with the Controlled Molecular Weights

«Green» synthesis and characterization of galactomannan sulfates obtained using sulfamic acid

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