In light of the structural properties of tetradymite-like layered chalcogenide compounds, the mixed-layered compound GeBi3Te4 was predicted and synthesized for the first time, which belongs to the nBi2–mGeBi2Te4 homologous series in the Ge-Te-Bi system. A polycrystal of a new phase was synthesized, and its single crystal was grown by the Bridgman–Stockbarger method. The obtained samples were investigated by differential thermal analysis (DTA) and powder X-ray diffraction (XRD). It was found that the compound melts peritectically at 563 C and has a rhombohedral lattice-type structure with the following lattice parameters: a =4.3625 (5) Å, c = 31.381 (2) Å (sp. gr R3m). The crystal structure of the layered van der Waals compound GeBi3Te4 consists of a repetition of seven-layer GeBi2Te4 packets and two-layer Bi packets in the form of -7-2-7-7-2-7-7-2-7- which differ from the previously discovered GeBi4Te4 phase, which consists of unit cells from only one seven-layer packet. The discovery of a new mixed-layered compound indicates the possibility of the formation of similar compounds in AIV–BV–Te (AIV = Ge, Sn, Pb; BV = Sb, Bi) systems
根据类四白菌层状硫族化合物的结构性质，首次预测并合成了混合层状化合物GeBi3Te4，该化合物属于Ge-Te-Bi体系中的nBi2-mGeBi2Te4同源系。合成了一种新相的多晶，并用Bridgman-Stockbarger法生长了单晶。采用差热分析(DTA)和粉末x射线衍射(XRD)对所得样品进行了表征。结果表明，该化合物在563℃时呈周晶熔化，具有菱形晶格型结构，晶格参数为:a =4.3625 (5) Å， C = 31.381 (2) Å (sp. gr R3m)。层状范德华化合物GeBi3Te4的晶体结构由七层GeBi2Te4包和两层Bi包的重复组成，其形式为-7-2-7- 2-7-7- 7-7-这与先前发现的GeBi4Te4相不同，后者仅由一个七层包的单位细胞组成。新混合层化合物的发现表明AIV - bv - te中有可能形成类似的化合物(AIV = Ge, Sn, Pb;BV = Sb, Bi)系
{"title":"Synthesis and study of a new mixed-layered compound GeBi3Te4 belonging to the nBi2–mGeBi2Te4 homologous series","authors":"F.R. Aliyev, E. Orujlu, D. Babanly","doi":"10.31489/2022ch1/92-98","DOIUrl":"https://doi.org/10.31489/2022ch1/92-98","url":null,"abstract":"In light of the structural properties of tetradymite-like layered chalcogenide compounds, the mixed-layered compound GeBi3Te4 was predicted and synthesized for the first time, which belongs to the nBi2–mGeBi2Te4 homologous series in the Ge-Te-Bi system. A polycrystal of a new phase was synthesized, and its single crystal was grown by the Bridgman–Stockbarger method. The obtained samples were investigated by differential thermal analysis (DTA) and powder X-ray diffraction (XRD). It was found that the compound melts peritectically at 563 C and has a rhombohedral lattice-type structure with the following lattice parameters: a =4.3625 (5) Å, c = 31.381 (2) Å (sp. gr R3m). The crystal structure of the layered van der Waals compound GeBi3Te4 consists of a repetition of seven-layer GeBi2Te4 packets and two-layer Bi packets in the form of -7-2-7-7-2-7-7-2-7- which differ from the previously discovered GeBi4Te4 phase, which consists of unit cells from only one seven-layer packet. The discovery of a new mixed-layered compound indicates the possibility of the formation of similar compounds in AIV–BV–Te (AIV = Ge, Sn, Pb; BV = Sb, Bi) systems","PeriodicalId":9421,"journal":{"name":"Bulletin of the Karaganda University. \"Chemistry\" series","volume":"98 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-03-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76060359","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A. Sarsenbekova, A. Bolatbay, V. Morgun, D. Havlícek, S. Davrenbekov, E. Nasikhatuly
The study of the kinetic parameters of copolymers based on polyethylene glycol fumarates, as well as the external and internal effects on them, is essential for production processes at various levels. This will solve a whole range of issues in the field of the shelf life of materials and storage conditions. All these point to the relevance of this research. The authors of the research attempt to test the most common thermogravimetric data processing methods and to improve them in terms of the quality of the predictive capabilities of the resulting regression equation. Both of them are important for the production of initial components and the manufacture of the final product from the studied materials. Therefore, the study and further use of the numerical data of the TG/DTA curves applies to both theoretical and practical branches of science. Thus, summarizing the experimental data on the thermal stability studies, we assume that p-EGF: AA copolymers with compositions of 21.03:78.97 and 68.96:31.04 wt.% have a relatively high degree of resistance to heating. It was found that the calculation by the FR method agreed well with the results of the KAS method. It should be noted that for the p-EGF: AA copolymer (21.03:78.97 wt.%) at heating rates of 5.0, 10.0, 20.0 °С∙min–1, the average activation energy data obtained for two methods increase in the following series:KAS E = 187.34 kJ /mol
富马酸聚乙二醇共聚物的动力学参数的研究，以及对它们的外部和内部影响，对不同层次的生产工艺至关重要。这将解决材料的保质期和储存条件领域的一系列问题。这些都表明了本研究的相关性。该研究的作者试图测试最常见的热重数据处理方法，并根据所得回归方程的预测能力的质量来改进它们。这两种方法对于用所研究的材料生产初始部件和制造最终产品都很重要。因此，对热重/差热分析曲线数值数据的研究和进一步利用，在理论和实践两方面都有应用。因此，总结热稳定性研究的实验数据，我们认为组成为21.03:78.97和68.96:31.04 wt.%的p-EGF: AA共聚物具有较高的耐热性。结果表明，FR法的计算结果与KAS法的计算结果吻合较好。值得注意的是，对于p-EGF: AA共聚物(21.03:78.97 wt.%)，在5.0、10.0、20.0°С∙min-1的加热速率下，两种方法得到的平均活化能数据增加如下系列:KAS E = 187.34 kJ /mol
{"title":"Study of thermal stability and determination of effective activation energy values during degradation of unsaturated polyester copolymers in the air atmosphere","authors":"A. Sarsenbekova, A. Bolatbay, V. Morgun, D. Havlícek, S. Davrenbekov, E. Nasikhatuly","doi":"10.31489/2022ch1/86-91","DOIUrl":"https://doi.org/10.31489/2022ch1/86-91","url":null,"abstract":"The study of the kinetic parameters of copolymers based on polyethylene glycol fumarates, as well as the external and internal effects on them, is essential for production processes at various levels. This will solve a whole range of issues in the field of the shelf life of materials and storage conditions. All these point to the relevance of this research. The authors of the research attempt to test the most common thermogravimetric data processing methods and to improve them in terms of the quality of the predictive capabilities of the resulting regression equation. Both of them are important for the production of initial components and the manufacture of the final product from the studied materials. Therefore, the study and further use of the numerical data of the TG/DTA curves applies to both theoretical and practical branches of science. Thus, summarizing the experimental data on the thermal stability studies, we assume that p-EGF: AA copolymers with compositions of 21.03:78.97 and 68.96:31.04 wt.% have a relatively high degree of resistance to heating. It was found that the calculation by the FR method agreed well with the results of the KAS method. It should be noted that for the p-EGF: AA copolymer (21.03:78.97 wt.%) at heating rates of 5.0, 10.0, 20.0 °С∙min–1, the average activation energy data obtained for two methods increase in the following series:KAS E = 187.34 kJ /mol","PeriodicalId":9421,"journal":{"name":"Bulletin of the Karaganda University. \"Chemistry\" series","volume":"17 2 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-03-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79357647","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A. Galiyeva, Y. Tazhbayev, T. Zhumagaliyeva, D. Sadyrbekov, D. Kaikenov, B. Karimova, S.S. Shokenova
The research aims to optimize and minimize the number of experiments to obtain polylactide-co-glycolide (PLGA) nanoparticles (NPs) immobilized with antituberculosis (anti-TB) drug — isoniazid (INH) by applying the Taguchi method and Design Expert statistical software. Several experiments were performed with varying parameters, namely polymer/drug ratio, polyvinyl alcohol (PVA) concentration, the ratio of organic solvent to the aqueous phase, and solvent type. Three different levels and a fractional factorial design were derived for each parameter, particularly the standard orthogonal array (OA) L9. Drug-loaded nanoparticles were prepared by the double emulsion method. The results were obtained from 9 runs indicated particle sizes ranging from 152.2±6.4 nm to 496.4±9.5 nm. These results were used to predict the optimum conditions for synthesizing INH-PLGA particles. The calculated data correlate well with the experimental data. INH-PLGA NPs were obtained with a mean size and polydispersity of nanoparticles of 152.2±2.25 nm and 0.279±0.03, respectively. Scanning electron microscopy, thermogravimetric analysis, and differential scanning calorimetry were carried out to characterize the obtained nanoparticles. The degree of drug release from PLGA NPs was studied, and the results showed that PLGA prolonged the release of INH from the polymer matrix
{"title":"Polylactide-co-glycolide nanoparticles immobilized with isoniazid: optimization using the experimental Taguchi method","authors":"A. Galiyeva, Y. Tazhbayev, T. Zhumagaliyeva, D. Sadyrbekov, D. Kaikenov, B. Karimova, S.S. Shokenova","doi":"10.31489/2022ch1/69-77","DOIUrl":"https://doi.org/10.31489/2022ch1/69-77","url":null,"abstract":"The research aims to optimize and minimize the number of experiments to obtain polylactide-co-glycolide (PLGA) nanoparticles (NPs) immobilized with antituberculosis (anti-TB) drug — isoniazid (INH) by applying the Taguchi method and Design Expert statistical software. Several experiments were performed with varying parameters, namely polymer/drug ratio, polyvinyl alcohol (PVA) concentration, the ratio of organic solvent to the aqueous phase, and solvent type. Three different levels and a fractional factorial design were derived for each parameter, particularly the standard orthogonal array (OA) L9. Drug-loaded nanoparticles were prepared by the double emulsion method. The results were obtained from 9 runs indicated particle sizes ranging from 152.2±6.4 nm to 496.4±9.5 nm. These results were used to predict the optimum conditions for synthesizing INH-PLGA particles. The calculated data correlate well with the experimental data. INH-PLGA NPs were obtained with a mean size and polydispersity of nanoparticles of 152.2±2.25 nm and 0.279±0.03, respectively. Scanning electron microscopy, thermogravimetric analysis, and differential scanning calorimetry were carried out to characterize the obtained nanoparticles. The degree of drug release from PLGA NPs was studied, and the results showed that PLGA prolonged the release of INH from the polymer matrix","PeriodicalId":9421,"journal":{"name":"Bulletin of the Karaganda University. \"Chemistry\" series","volume":"11 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-03-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82654800","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-01-01DOI: 10.31489/2022ch4/4-22-17
S. Zulfugarova, G. Azimova, Z. Aleskerova, Y. Litvishkov, D. Tagiyev
This review considers recent work on the synthesis of transition metal ferrites (Co, Cu, Ni, Mn) by sol-gel method with combustion, as well as the effect of microwave radiation. Ferrites are interesting not only for magnetic and optical properties, but also for their catalytic properties. In recent years, there has been an in-creasing amount of literature, which investigates the catalytic properties of transition metal ferrites in various reactions, including oxidative reactions. Given the fact that various organic components are used as complex-ing agents and as a fuel in the sol-gel method with combustion, the review considers the influence of the or-ganic reagent nature, its ratio to precursors, the pH of the medium, the power and time of microwave expo-sure to the process of ferrite formation as factors influencing the size of formed particles and their textural characteristics, which are of great importance in the catalysis. Recently, the attention of chemists working in the field of catalysis has been attracted by studies of the effect of physical fields, to which the microwave field belongs, on various chemical processes, including the nanocatalysts synthesis. The use of microwave ra-diation in sol-gel synthesis of ferrite allows obtaining nanoferrites with high specific surface area. From this point of view, this paper considers the works of recent years devoted to the study of microwave sol-gel syn-thesis of ferrite.
{"title":"Synthesis of Transition Metal Ferrites (Co, Cu, Ni, Mn) by the Sol-Gel Method with Combustion and the Use of Microwave Processing","authors":"S. Zulfugarova, G. Azimova, Z. Aleskerova, Y. Litvishkov, D. Tagiyev","doi":"10.31489/2022ch4/4-22-17","DOIUrl":"https://doi.org/10.31489/2022ch4/4-22-17","url":null,"abstract":"This review considers recent work on the synthesis of transition metal ferrites (Co, Cu, Ni, Mn) by sol-gel method with combustion, as well as the effect of microwave radiation. Ferrites are interesting not only for magnetic and optical properties, but also for their catalytic properties. In recent years, there has been an in-creasing amount of literature, which investigates the catalytic properties of transition metal ferrites in various reactions, including oxidative reactions. Given the fact that various organic components are used as complex-ing agents and as a fuel in the sol-gel method with combustion, the review considers the influence of the or-ganic reagent nature, its ratio to precursors, the pH of the medium, the power and time of microwave expo-sure to the process of ferrite formation as factors influencing the size of formed particles and their textural characteristics, which are of great importance in the catalysis. Recently, the attention of chemists working in the field of catalysis has been attracted by studies of the effect of physical fields, to which the microwave field belongs, on various chemical processes, including the nanocatalysts synthesis. The use of microwave ra-diation in sol-gel synthesis of ferrite allows obtaining nanoferrites with high specific surface area. From this point of view, this paper considers the works of recent years devoted to the study of microwave sol-gel syn-thesis of ferrite.","PeriodicalId":9421,"journal":{"name":"Bulletin of the Karaganda University. \"Chemistry\" series","volume":"10 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74780878","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A. Houbi, A. Zharmenov, Yomen Atassi, Z. Bagasharova, S. Mirzalieva, B. Karibayev
In this work, ternary composites of NiZn ferrite/carbonyl iron/carbon black (Ni0.5Zn0.5Fe2O4/CI/CB) were prepared via two stages. Firstly, Ni0.5Zn0.5Fe2O4 was prepared by a self-combustion method using sucrose as a fuel. After that, the operation was continued via mixing CB, CI, and Ni0.5Zn0.5Fe2O4 through grinding balls. Three various weight ratios of Ni0.5Zn0.5Fe2O4/CI/CB (1:1:1, 1:1:2, and 2:1:1) with various thicknesses (2–4–6 mm) were prepared. The absorbers were prepared by dispersing (Ni0.5Zn0.5Fe2O4/CI/CB) composites with a weight ratio within a paraffin wax matrix of 40 % w/w. X-ray diffractometry and FTIR spectroscopy were used in order to characterize the samples. The morphology of the powders was investigated by SEM. The functional characterization was accomplished by measuring the microwave absorption properties in the fre-quency band of 8.8–12 GHz. The microwave absorption materials (MAMs) showed wide bandwidths under –10 dB in the range of 2.81–3.20 GHz and reasonable surface density in the range of 3.625–4.041 kg/m2. The absorber of 3.20 GHz bandwidth had a minimal reflection loss of –19.4 dB at the matching frequency of 9.92 GHz with a thickness of 6 mm.
{"title":"Synthesis and Microwave Absorption Properties of (Ni0.5Zn0.5Fe2O4/CI/CB) Ternary Composites","authors":"A. Houbi, A. Zharmenov, Yomen Atassi, Z. Bagasharova, S. Mirzalieva, B. Karibayev","doi":"10.31489/2022ch4/4-22-9","DOIUrl":"https://doi.org/10.31489/2022ch4/4-22-9","url":null,"abstract":"In this work, ternary composites of NiZn ferrite/carbonyl iron/carbon black (Ni0.5Zn0.5Fe2O4/CI/CB) were prepared via two stages. Firstly, Ni0.5Zn0.5Fe2O4 was prepared by a self-combustion method using sucrose as a fuel. After that, the operation was continued via mixing CB, CI, and Ni0.5Zn0.5Fe2O4 through grinding balls. Three various weight ratios of Ni0.5Zn0.5Fe2O4/CI/CB (1:1:1, 1:1:2, and 2:1:1) with various thicknesses (2–4–6 mm) were prepared. The absorbers were prepared by dispersing (Ni0.5Zn0.5Fe2O4/CI/CB) composites with a weight ratio within a paraffin wax matrix of 40 % w/w. X-ray diffractometry and FTIR spectroscopy were used in order to characterize the samples. The morphology of the powders was investigated by SEM. The functional characterization was accomplished by measuring the microwave absorption properties in the fre-quency band of 8.8–12 GHz. The microwave absorption materials (MAMs) showed wide bandwidths under –10 dB in the range of 2.81–3.20 GHz and reasonable surface density in the range of 3.625–4.041 kg/m2. The absorber of 3.20 GHz bandwidth had a minimal reflection loss of –19.4 dB at the matching frequency of 9.92 GHz with a thickness of 6 mm.","PeriodicalId":9421,"journal":{"name":"Bulletin of the Karaganda University. \"Chemistry\" series","volume":"53 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85395374","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Z. Nurmaganbetov, S. Fazylov, K. M. Turdybekov, O. Nurkenov, D. M. Turdybekov, G.K. Mukusheva, Ye.V. Minayeva, G. Khabdolda
The article presents results on the synthesis and investigation of the structural features of a number of 1,4-disubstituted 1H-1,2,3-triazole derivatives of the alkaloid lupinine. Lupinine modification reactions were carried out at the hydroxymethylene group in the C-1 position of the quinolysine backbone. It has been shown that (octahydro-2H-quinolysine-1-ylmethyl)methanesulfonate in high yield (93%) is formed by the interaction of lupinine with methanesulfonyl chloride in methylene chloride. Subsequent treatment of this compound with sodium azide in dimethylformamide on heating leads to the formation of 1-(azidomethyl)octahydro-2H-quinolysine in 61% yield. It has been found that the reaction of a new azide with terminal alkynes of various nature in the presence of aqueous СuSO4 and sodium ascorbate in dimethylformamide can form the corresponding 4-substituted (1S,9aR)-1-[(1,2,3-triazol-1-yl)methyl]octahydro-1H-quinolysines. New 1,2,3-triazole derivatives of lupinine containing various aryl substituents at the C-4 position of the triazole ring have been obtained. The high selectivity of the reaction is explained by the action mechanism of the Sharpless catalyst. The spatial structure of the molecules of lupinine methanesulfonate, 4-aryltriazolylmethyl-octahydro-quinolysines has been established by X-ray diffraction analysis. X-ray structural analysis data of new compounds have been deposited in the form of CIF files at the Cambridge Crystallographic Data Center.
{"title":"Synthesis and structure of 4-substituted (1S,9aR)-1-[(1,2,3-triazol-1-yl)methyl]octahydro-1H-quinolysines of lupinine","authors":"Z. Nurmaganbetov, S. Fazylov, K. M. Turdybekov, O. Nurkenov, D. M. Turdybekov, G.K. Mukusheva, Ye.V. Minayeva, G. Khabdolda","doi":"10.31489/2022ch2/2-22-5","DOIUrl":"https://doi.org/10.31489/2022ch2/2-22-5","url":null,"abstract":"The article presents results on the synthesis and investigation of the structural features of a number of 1,4-disubstituted 1H-1,2,3-triazole derivatives of the alkaloid lupinine. Lupinine modification reactions were carried out at the hydroxymethylene group in the C-1 position of the quinolysine backbone. It has been shown that (octahydro-2H-quinolysine-1-ylmethyl)methanesulfonate in high yield (93%) is formed by the interaction of lupinine with methanesulfonyl chloride in methylene chloride. Subsequent treatment of this compound with sodium azide in dimethylformamide on heating leads to the formation of 1-(azidomethyl)octahydro-2H-quinolysine in 61% yield. It has been found that the reaction of a new azide with terminal alkynes of various nature in the presence of aqueous СuSO4 and sodium ascorbate in dimethylformamide can form the corresponding 4-substituted (1S,9aR)-1-[(1,2,3-triazol-1-yl)methyl]octahydro-1H-quinolysines. New 1,2,3-triazole derivatives of lupinine containing various aryl substituents at the C-4 position of the triazole ring have been obtained. The high selectivity of the reaction is explained by the action mechanism of the Sharpless catalyst. The spatial structure of the molecules of lupinine methanesulfonate, 4-aryltriazolylmethyl-octahydro-quinolysines has been established by X-ray diffraction analysis. X-ray structural analysis data of new compounds have been deposited in the form of CIF files at the Cambridge Crystallographic Data Center.","PeriodicalId":9421,"journal":{"name":"Bulletin of the Karaganda University. \"Chemistry\" series","volume":"8 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87827015","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-01-01DOI: 10.31489/2022ch3/3-22-20
V. Zhinzhilo, A.Yu. Litvinova, V.M. Lyamina, G. Dzhardimalieva, I. Uflyand
Metal-organic frameworks (MOFs) are crystalline compounds consisting of metal ions coordinated by bridg-ing organic ligands. Depending on the coordination geometry of the metal and the direction of the bond of donor atoms, as well as on the geometry of the bridging ligand, 1D, 2D, or 3D polymer structures are formed. The characteristic features of metal-organic frameworks are low density, high porosity and crystallinity, and large specific surface. Wide attention is paid to the technological aspects of creating such materials and their integration into various devices. To obtain MOFs, various synthetic approaches have been developed based on precipitation reactions at room temperature and under convective heating, including hydrothermal and sol-vothermal syntheses. In this work metal organic framework structures based on nickel and cobalt trimesinates were synthesized by a modified procedure by reacting nickel acetate and cobalt nitrate with trimesic acid in the presence of alkali. The obtained compounds were used to study the adsorption of Congo Red and Meth-ylene blue organic dyes from their aqueous solutions. The degree of adsorption depends on temperature and reaches a value of 97% for Congo Red, while for Methylene blue it is 83%. The mechanisms and characteris-tic parameters of the adsorption process were analyzed using empirical models of Langmuir, Temkin, and Freundlich isotherms, of which the adsorption process was optimally described by the Freundlich model. The calculated thermodynamic parameters indicate the spontaneity of the process and its insignificant endother-mic character.
{"title":"Coordinating Polymers Based on Nickel(II) and Cobalt(II) Trimesinates as Promising Adsorbents of Organic Dyes","authors":"V. Zhinzhilo, A.Yu. Litvinova, V.M. Lyamina, G. Dzhardimalieva, I. Uflyand","doi":"10.31489/2022ch3/3-22-20","DOIUrl":"https://doi.org/10.31489/2022ch3/3-22-20","url":null,"abstract":"Metal-organic frameworks (MOFs) are crystalline compounds consisting of metal ions coordinated by bridg-ing organic ligands. Depending on the coordination geometry of the metal and the direction of the bond of donor atoms, as well as on the geometry of the bridging ligand, 1D, 2D, or 3D polymer structures are formed. The characteristic features of metal-organic frameworks are low density, high porosity and crystallinity, and large specific surface. Wide attention is paid to the technological aspects of creating such materials and their integration into various devices. To obtain MOFs, various synthetic approaches have been developed based on precipitation reactions at room temperature and under convective heating, including hydrothermal and sol-vothermal syntheses. In this work metal organic framework structures based on nickel and cobalt trimesinates were synthesized by a modified procedure by reacting nickel acetate and cobalt nitrate with trimesic acid in the presence of alkali. The obtained compounds were used to study the adsorption of Congo Red and Meth-ylene blue organic dyes from their aqueous solutions. The degree of adsorption depends on temperature and reaches a value of 97% for Congo Red, while for Methylene blue it is 83%. The mechanisms and characteris-tic parameters of the adsorption process were analyzed using empirical models of Langmuir, Temkin, and Freundlich isotherms, of which the adsorption process was optimally described by the Freundlich model. The calculated thermodynamic parameters indicate the spontaneity of the process and its insignificant endother-mic character.","PeriodicalId":9421,"journal":{"name":"Bulletin of the Karaganda University. \"Chemistry\" series","volume":"74 Supplement_1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84002585","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-01-01DOI: 10.31489/2022ch3/3-22-21
G. Mamytbekov, Zh.I. Beksultanov, V. Bannykh, I.V. Dan’ko
A systematic study of the synthesis of hybrid composite materials based on synthetic (poly-N-vinylpyrrolidone) and natural (agar-agar) macromolecules in the presence of plasticizers (PEG-400, glycerin) and mineral filler bentonite has been performed by the method of electron irradiation. The methods of X-ray diffraction analysis and SEM showed that the structure of the resulted hybrid compositions is defined as an interpenetrating network with the distributed intercalated particles of mineral component inside its volume. It has been established that mechanical properties of the hybrid composition are determined mainly by the struc-tural organization of the interpenetrating polymer network, formed during electron irradiation of the initial polymer mixture in the presence of plasticizers, as well as by the conditions for intercalation of polymer seg-ments into the interpacket layers of the mineral matrix. During the process of crazing of the sample under ten-sion the shear stress is concentrated in the central part of the sample from the periphery of the fastening. It is shown that the degree of swelling for hybrid composition strongly depends on concentration of a low molecu-lar plasticizer in the polymeric interpenetrating network, which can easily impregnate into the interplanar lay-ers of bentonite.
{"title":"Synthesis, Structure and Properties of Hybrid Composite Bentonite-Based Materials","authors":"G. Mamytbekov, Zh.I. Beksultanov, V. Bannykh, I.V. Dan’ko","doi":"10.31489/2022ch3/3-22-21","DOIUrl":"https://doi.org/10.31489/2022ch3/3-22-21","url":null,"abstract":"A systematic study of the synthesis of hybrid composite materials based on synthetic (poly-N-vinylpyrrolidone) and natural (agar-agar) macromolecules in the presence of plasticizers (PEG-400, glycerin) and mineral filler bentonite has been performed by the method of electron irradiation. The methods of X-ray diffraction analysis and SEM showed that the structure of the resulted hybrid compositions is defined as an interpenetrating network with the distributed intercalated particles of mineral component inside its volume. It has been established that mechanical properties of the hybrid composition are determined mainly by the struc-tural organization of the interpenetrating polymer network, formed during electron irradiation of the initial polymer mixture in the presence of plasticizers, as well as by the conditions for intercalation of polymer seg-ments into the interpacket layers of the mineral matrix. During the process of crazing of the sample under ten-sion the shear stress is concentrated in the central part of the sample from the periphery of the fastening. It is shown that the degree of swelling for hybrid composition strongly depends on concentration of a low molecu-lar plasticizer in the polymeric interpenetrating network, which can easily impregnate into the interplanar lay-ers of bentonite.","PeriodicalId":9421,"journal":{"name":"Bulletin of the Karaganda University. \"Chemistry\" series","volume":"103 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80721929","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2022-01-01DOI: 10.31489/2022ch3/3-22-16
H. Shinohara, H. Nishide
Electrocatalytic water oxidation for oxygen gas evolution has been widely studied from the perspective of sustainable technology. However, the use of organic polymers as catalyst layers for this reaction remains un-developed. We discuss, here, the prerequisites, characteristics, and advantages of π-conjugated polymers as electrochemical catalysts to modify anodic current collectors for water oxidation, including some examples by citing the previous works in literature. In section 3, we present our latest results, the use of an organic pol-ymer complex of poly(ethylenedioxythiophene) and phytic acid supported by a hydrophilic poly(hydroxy-ethyl methacrylate) platform, which efficiently generates oxygen gas through anodic water oxidation.
{"title":"Polymer Complexes for Electrocatalytic Oxygen Evolution","authors":"H. Shinohara, H. Nishide","doi":"10.31489/2022ch3/3-22-16","DOIUrl":"https://doi.org/10.31489/2022ch3/3-22-16","url":null,"abstract":"Electrocatalytic water oxidation for oxygen gas evolution has been widely studied from the perspective of sustainable technology. However, the use of organic polymers as catalyst layers for this reaction remains un-developed. We discuss, here, the prerequisites, characteristics, and advantages of π-conjugated polymers as electrochemical catalysts to modify anodic current collectors for water oxidation, including some examples by citing the previous works in literature. In section 3, we present our latest results, the use of an organic pol-ymer complex of poly(ethylenedioxythiophene) and phytic acid supported by a hydrophilic poly(hydroxy-ethyl methacrylate) platform, which efficiently generates oxygen gas through anodic water oxidation.","PeriodicalId":9421,"journal":{"name":"Bulletin of the Karaganda University. \"Chemistry\" series","volume":"46 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87274588","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
S. Gandhi, A. R. Gawhane, S. Kapse, D. Nagore, S. Chitlange
Simple, sensitive high performance thin layer chromatography method for the estimation of gallic acid and quercetin in in-house polyherbal blend has been developed and validated. Methanolic solution of herbal blend comprising of Emblica officinalis, Camellia sinensis and Garcinia cambogia was used for analysis. The sepa-ration was performed on TLC aluminum plates precoated with silica gel G60 F254 and toluene : ethyl ace-tate : formic acid (5:1.5:1 v/v/v) at 254 nm scanning wavelength. The system gave well resolved peaks for gallic acid and quercetin at Rf 0.14 and Rf 0.29 respectively. The method validated as per ICH Q2R1 guide-lines which shows regression co-efficient 0.9939 for gallic acid and 0.9988 for quercetin in range of 2–6 μg/ml. Recovery of gallic acid and quercetin was found in range of 98–102 % which confirms the accuracy of method. Precision study (interday & intraday) showed that the relative standard deviation is less than 2 %, showing method is well precise. Proposed validated HPTLC method is simple, precise, specific, robust and accurate, and could find application in routine quality-control analysis. The method was used for quantitative estimation of gallic acid and quercetin in the polyherbal blend and was found as 1.648 % w/w and 3.165 % w/w respectively.
{"title":"Validated High Performance Thin Layer Chromatography Method for Simultaneous Estimation for Gallic Acid and Quercetin in Polyherbal Blend and Their Quantitative Estimation","authors":"S. Gandhi, A. R. Gawhane, S. Kapse, D. Nagore, S. Chitlange","doi":"10.31489/2022ch4/4-22-4","DOIUrl":"https://doi.org/10.31489/2022ch4/4-22-4","url":null,"abstract":"Simple, sensitive high performance thin layer chromatography method for the estimation of gallic acid and quercetin in in-house polyherbal blend has been developed and validated. Methanolic solution of herbal blend comprising of Emblica officinalis, Camellia sinensis and Garcinia cambogia was used for analysis. The sepa-ration was performed on TLC aluminum plates precoated with silica gel G60 F254 and toluene : ethyl ace-tate : formic acid (5:1.5:1 v/v/v) at 254 nm scanning wavelength. The system gave well resolved peaks for gallic acid and quercetin at Rf 0.14 and Rf 0.29 respectively. The method validated as per ICH Q2R1 guide-lines which shows regression co-efficient 0.9939 for gallic acid and 0.9988 for quercetin in range of 2–6 μg/ml. Recovery of gallic acid and quercetin was found in range of 98–102 % which confirms the accuracy of method. Precision study (interday & intraday) showed that the relative standard deviation is less than 2 %, showing method is well precise. Proposed validated HPTLC method is simple, precise, specific, robust and accurate, and could find application in routine quality-control analysis. The method was used for quantitative estimation of gallic acid and quercetin in the polyherbal blend and was found as 1.648 % w/w and 3.165 % w/w respectively.","PeriodicalId":9421,"journal":{"name":"Bulletin of the Karaganda University. \"Chemistry\" series","volume":"40 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85079367","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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