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Solvothermal synthesis of metastable molybdenum, tungsten and vanadium oxides 溶剂热合成亚稳钼、钨、钒氧化物
Pub Date : 2020-03-05 DOI: 10.33581/2520-257x-2020-1-32-39
T. Sviridova
It is shown that under the solvothermal conditions the polycondensation of molybdic, tungstic and vanadic oxoacids yields metastable oxide phases (h-MoO3, h-WO3, xerogel-V2O5 of lamellar structure) in the form of microcrystals 2–10 μm in size, while the hydrates of these oxides formed as the by-products exhibiting conversion as the result of recrystallization during the course of further growing. By changing the concentration of the reaction solution it is possible to exert an effective control over the nucleation to obtain the oxide particles of the similar structure and habitus.
结果表明,在溶剂热条件下,钼酸、钨酸和钒酸的缩聚反应生成了尺寸为2 ~ 10 μm的亚稳氧化物相(h-MoO3、h-WO3、片层结构的xerogel-V2O5),而这些氧化物的水合物在进一步生长过程中由于再结晶而发生转化。通过改变反应溶液的浓度,可以对成核过程进行有效的控制,得到具有相似结构和习性的氧化物颗粒。
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引用次数: 1
The development of methods for the determination of residues of the insecticide pymetrozine in water, soil, cucumber and rape 建立了吡蚜酮在水、土壤、黄瓜和油菜中的残留量测定方法
Pub Date : 2019-08-30 DOI: 10.33581/2520-257x-2019-2-79-87
M. Zayats, S. Leschev
Based on the literature data on the solubility of pymetrozine in water and organic solvents, as well as experimental data on the extraction of pymetrozine from water, soil and plant matrices, the optimal conditions for the extraction of pymetrozine from water; soil; cucumber; rape seeds, oil and green pods were selected. The conditions for cleaning extracts were selected as well. At the first stage, acetonitrile, a mixture of dichloromethane – isopropanol, or a mixture of dichloromethane – methanol in the presence or absence of inorganic salts were used for extraction of the pesticide. Pymetrozine was found to be a highly hydrophilic substance. For the purification of extracts of pymetrozine from plant matrices the extraction systems hexane – 0.02 mol/L aqueous solution of orthophosphoric acid, hexane or chloroform – aqueous solutions of ammonium sulfate were successfully used. The samples, obtained after this treatment, were pure enough to determine the residual amounts of pymetrozine in them at the maximum residue level (MRL), determined in Russia and the countries of the European Union, or lower using widespread liquid chromatography with diode-array (ultraviolet) detection.
根据吡蚜酮在水和有机溶剂中的溶解度数据,以及从水、土壤和植物基质中提取吡蚜酮的实验数据,确定了从水中提取吡蚜酮的最佳工艺条件;土壤;黄瓜;选择油菜种子、油分和绿豆荚。并对提取液的清洗条件进行了选择。在第一阶段,用乙腈、二氯甲烷-异丙醇的混合物或二氯甲烷-甲醇的混合物在存在或不存在无机盐的情况下提取农药。吡蚜酮是一种高度亲水的物质。采用正己烷- 0.02 mol/L正磷酸水溶液、己烷-氯仿-硫酸铵水溶液等萃取体系对植物基质中吡嘧啉的萃取物进行了纯化。经过这种处理后获得的样品纯度足够高,可以在俄罗斯和欧盟国家确定的最大残留水平(MRL)或使用二极管阵列(紫外线)检测的广泛液相色谱法确定的更低残留水平(MRL)来确定其中的吡虫胺残留量。
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引用次数: 0
IR-spectrum of monometallic copper(II) halogenide complexes with 1-tert-butyl-1,2,4-tria zole: experimental and quantum chemical studies 1-叔丁基-1,2,4-三唑单金属卤化铜配合物的红外光谱:实验和量子化学研究
Pub Date : 2019-08-30 DOI: 10.33581/2520-257x-2019-2-12-20
Djennet S. Saparova, A. N. Bogatikov, V. Matulis, M. M. Degtyarik
The crystalline complexes CuL2X2 and CuL4X2 , where X = Cl or X = Br were synthesized by the interaction of copper(II) chloride or bromide with 1-tert-butyl-1,2,4-triazole (L) in water or organic solvents. The structure of metal complexes have been studied by elemental analysis, X-ray analysis and IR-spectroscopy in the medium (4000 –500 cm –1 ) and long-wavelength (400–50 cm –1 ) regions. Quantum chemical calculations of the vibrational spectra of the CuL2Cl2 and CuL4Cl2 complexes have been carried out to perform the assignment of the signals in the IR-spectra. It is shown that the polymer structure of CuL2X2 complexes is formed due to bridging of one of their halide ions. In the CuL4X2 complexes, the halide ions and 1-tert-butyl-1,2,4-triazole form an island type structure. In all metal complexes 1-tert-butyl-1,2,4-triazole is coordinated by N(4) atom of heterocycle.
在水或有机溶剂中,氯化铜(II)或溴化铜与1-叔丁基-1,2,4-三唑(L)相互作用,合成了X = Cl或X = Br的结晶配合物CuL2X2和CuL4X2。通过元素分析、x射线分析和红外光谱研究了金属配合物在中波(4000 ~ 500 cm -1)和长波(400 ~ 50 cm -1)区域的结构。对CuL2Cl2和CuL4Cl2配合物的振动光谱进行了量子化学计算,以确定红外光谱中的信号分配。结果表明,CuL2X2配合物的聚合物结构是由于其中一个卤化物离子的桥接而形成的。在CuL4X2配合物中,卤化物离子与1-叔丁基-1,2,4-三唑形成岛状结构。在所有的金属配合物中,1-叔丁基-1,2,4-三唑是由杂环上的N(4)原子配位的。
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引用次数: 1
Compo­sition, structure and properties of electroless deposited nickel – phosphorus – copper coatings 化学沉积镍磷铜镀层的组成、结构和性能
Pub Date : 2019-08-30 DOI: 10.33581/2520-257x-2019-2-62-68
L. S. Tsybul’skaya, S. Perevoznikov, V. Shendyukov
The nickel – phosphorus – copper functional coating was deposited on aluminum alloys substrate by chemical deposition method from malonate­glycinate nickel plating solution. The chemical and phase coatings composition was studied by X­ray fluorescence and X­ray phase analyze. Thermally stimulated phase transitions in deposited Ni – P – Cu coating were detected by differential scanning calorimetry method. The annealing at 250 and 400 °С was shown to lead to the changes in coating structure involving the transition from amorphous to amorphous­crystalline at 250 °С and to crystalline at 400 °С with Ni and Ni3P1 –  δ phases forming. Changes in the structure of Ni–P coating results in the increase of microhardness by 1.6–1.7 times and wear resistance by 3– 4 times. Annealing at 400 °С led to decreasing of corrosion stability of the coatings in 3.5 % sodium chloride solution. The optimum physical, mechanical and protective properties has the attained in the case of Ni – P – Cu coating annealed at 250 °C.
以丙二酸盐-甘氨酸盐镀镍液为原料,采用化学沉积法在铝合金基体上制备了镍磷铜功能镀层。采用x射线荧光和x射线物相分析研究了涂层的化学成分和物相组成。采用差示扫描量热法对Ni - P - Cu镀层的热激相变进行了检测。250°和400°С退火导致涂层结构发生变化,在250°С从无定形转变为非晶,在400°С转变为结晶,形成Ni和Ni3P1 - δ相。Ni-P镀层组织的改变使镀层显微硬度提高1.6 ~ 1.7倍,耐磨性提高3 ~ 4倍。400°С退火导致涂层在3.5%氯化钠溶液中的腐蚀稳定性下降。在250℃退火条件下,Ni - P - Cu涂层获得了最佳的物理、机械和防护性能。
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引用次数: 0
Synthesis of functionalized polyisobutylene and its block copolymers with D,L-lactide 功能化聚异丁烯及其与D, l -丙交酯嵌段共聚物的合成
Pub Date : 2019-08-30 DOI: 10.33581/2520-257x-2019-2-40-50
P. Nikishau, E. Ksendzov, D. Shiman, L. V. Gaponik, S. Kostjuk
Method of reactive polyisobutylene modification by various alkoxybenzenes (anisole and 4-phenoxybutanol) was proposed to form functionalized polyisobutylenes. Polymerization of D,L-lactide was explored on the 4-phenoxybutanol/1,5,7-triazabicyclo[4.4.0]dec-5-ene system. It led to determination of optimal conditions for gaining of poly(isobutylene-b-D,L-lactide). Such copolymers (Mn = 14 300 g/mol and Mn = 36 600 g/mol, Mw /  Mn ≤ 2.5) which were obtained by the polymerization of D,L-lactide on polyisobutylene macroinitiator shows microphase ordering. Formation of the block copolymers is confirmed by 1Н NMR spectroscopy, gel permeation chromatography, and scanning electron microscopy.
提出了用各种烷氧苯(苯甲醚和4-苯氧丁醇)对聚异丁烯进行反应性改性的方法,得到功能化聚异丁烯。研究了4-苯氧基丁醇/1,5,7-三氮杂环[4.4.0]十二-5-烯体系中D, l -丙交酯的聚合反应。从而确定了合成聚异丁烯-b- d -l -丙交酯的最佳工艺条件。D, l -丙交酯在聚异丁烯高分子引发剂上聚合得到的共聚物(Mn = 14 300 g/mol和Mn = 36 600 g/mol, Mw / Mn≤2.5)具有微相有序性。嵌段共聚物的形成是通过1Н核磁共振波谱,凝胶渗透色谱和扫描电镜证实的。
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引用次数: 0
Biopharmaceutical aspects of techno­logy of wound­healing gels containing silver(I) complex with 2-­(4,6-­di-­tert-­butyl-­2,3-­dihydroxyphenylsulphanyl)acetic acid 含银(I)与2—(4,6—二叔—丁基—2,3—二羟基苯基磺胺基)乙酸配合物的伤口愈合凝胶的生物制药技术
Pub Date : 2019-08-30 DOI: 10.33581/2520-257x-2019-2-29-39
H. Harbatsevich, Sergei I. Stakhevich, N. Loginova, G. Ksendzova, N. Osipovich, I. N. Slabko, V. V. Butkevich, Zhanna A. Makarevich, Lyudmila V. But'ko
The object of the work is to develop optimal composition of a gel with wound­healing ability based on Ag(I) complex with 2­(4,6­di­tert­butyl­2,3­dihydroxyphenylsulphanyl)acetic acid to produce a novel effective remedy. It was found that propylene glycol (PG) favours the formation of more fine suspension of Ag(I) complex, and introduction of polyvinylpyrrolidone (PVP) hinders aggregation of the particles of the complex, thus providing optimal dispersity of the gel suspension. The gels based on methyl cellulose (MC) are characterized by an acceptable degree of release of Ag(I) complex. It is the gels containing PG and PVP that are characterized by the most complete release of the active substance, which is in agreement with the data on the optimal dispersity. It was found that PG and PVP being introduced into the gel composition increase the osmotic activity of the gel considerably. The optimal composition of the ointment base was determined, %: MC – 3.5; PVP – 5.0; 0.1 mol/L citric acid solution – 5.0; PG – 20.0; water for injections – up to 100.0. The gel obtained was shown to surpass «Dermazin» cream and «Levomecol» ointment in wound­healing ability, while the content of the active substance was significantly lower (0.5 %), and to promote wounds to be cleansed of microorganisms fast and completely too. No accumulation of silver in the liver was found when the gel was used medicinally.
这项工作的目的是开发一种基于银(I)与2 -(4,6 -二叔丁基- 2,3 -二羟基苯基磺胺基)乙酸配合物的具有伤口愈合能力的凝胶的最佳组合,以产生一种新的有效药物。发现丙二醇(PG)有利于银(I)配合物形成更细的悬浮液,而聚乙烯吡咯烷酮(PVP)的引入阻碍了配合物颗粒的聚集,从而提供了最佳的凝胶悬浮液分散性。基于甲基纤维素(MC)的凝胶具有可接受的Ag(I)配合物释放度。含有PG和PVP的凝胶的活性物质释放最完全,这与最佳分散性的数据一致。结果表明,在凝胶组分中加入PG和PVP可显著提高凝胶的渗透活性。确定软膏基质的最佳组成:%:MC - 3.5;PVP - 5.0;0.1 mol/L柠檬酸溶液- 5.0;Pg - 20.0;注射用水-高达100.0。所获得的凝胶在伤口愈合能力上超过了“Dermazin”霜和“左旋美可”软膏,而活性物质的含量明显低于“Dermazin”霜和“左旋美可”软膏(0.5%),并且也能促进伤口微生物的快速彻底清洁。当凝胶作为药物使用时,没有发现银在肝脏中积聚。
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引用次数: 0
Electrodeposition of copper – tin alloys from glycol electrolytes 乙二醇电解液电沉积铜锡合金
Pub Date : 2019-08-30 DOI: 10.33581/2520-257x-2019-2-69-78
T. N. Vorobyova, Maryia G. Haluza, Olga N. Vryblevskaya, A. V. Paniatouski, E. A. Veretennikova
Stable ethylene glycol (EG) and propylene glycol (PG) electrolytes containing СuCl2 · 2H2O, SnCl4 · 5H2O and Trilon B have been developed, which provide electrodeposition of Cu – Sn alloy with tin content varying from 34 to 52 at. % in case of EG and from 51 to 91 at. % in case of PG electrolytes. It is found that the coatings contain phases of Cu6Sn5 и Cu10Sn3 intermetallic compounds, and metallic tin is also present in case of its highest content in the alloy. It is revealed that tin content can be simply varied by the change of current density or concentrations of tin and copper compounds in glycols. The effect of electrolyte composition, deposition conditions, a nature of a substrate on the coatings deposition rate (in the limits of 0.9‒2.9 μm ∙ h‒1), total metal current efficiency (from 40 to 95 %), the ratio of metals in the alloy (from 34 to 91 at. %), its phase composition and microstructure is determined. The conditions for the deposition of Cu – Sn alloy close to the eutectic composition have been found.
研制了含有СuCl2·2H2O、SnCl4·5H2O和Trilon B的稳定的乙二醇(EG)和丙二醇(PG)电解质,可电沉积锡含量在34 ~ 52 at之间的Cu - Sn合金。在EG的情况下,从51到91。%的PG电解质。结果表明,镀层中含有Cu6Sn5和Cu10Sn3金属间化合物相,同时还存在金属锡,锡在合金中含量最高。结果表明,锡的含量可以通过电流密度的变化或乙二醇中锡和铜化合物浓度的变化而简单地改变。电解质组成、沉积条件、衬底性质对镀层沉积速率(在0.9 ~ 2.9 μm∙h-1范围内)、总金属电流效率(从40%到95%)、合金中金属比(从34到91 at)的影响。%),测定其相组成和显微组织。发现了铜锡合金接近共晶成分的沉积条件。
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引用次数: 0
Formation of laterally-oriented monolayers of plasmonic silver nanoplats and their ensembles with cadmium selenide quantum dots on the sur face of thin polymeric film 等离子体银纳米片横向定向单层的形成及其与薄聚合物膜表面硒化镉量子点的集成
Pub Date : 2019-08-30 DOI: 10.33581/2520-257x-2019-2-21-28
P. Malakhovsky, M. Artemyev
We present here a novel method for formation of laterally-oriented monolayers of plasmonic silver nanoplates and their electrostatic ensembles with semiconductor quantum dots. Monolayers were electrostatically deposited on the surface of thin polymeric film containing different amount of tertiary amino groups. This method allows simultaneously investigate optical properties and morphology of silver nanoplates using transmittance electron microscopy. The optical density of films and surface concentration of silver nanoplates is proportional to the percentage of tertiary amino groups in the polymeric film. A surface ligand exchange was used for functionalization of the surface of silver nanoplates toward formation of electrostatic ensembles with colloidal quantum dots. We observed a straight correlation between the red shift of surface plasmon resonances in silver nanoplates and alkyl chain length of ligand molecules.
我们提出了一种新的方法来形成横向定向的等离子体银纳米板单层及其与半导体量子点的静电系综。在含有不同数量叔胺基的聚合物薄膜表面静电沉积单层膜。该方法允许使用透射电子显微镜同时研究银纳米片的光学性质和形貌。薄膜的光密度和银纳米片的表面浓度与聚合物薄膜中叔氨基的百分比成正比。利用表面配体交换对银纳米片表面进行功能化,使其与胶体量子点形成静电系综。我们观察到银纳米片表面等离子体共振的红移与配体分子的烷基链长度之间存在直接的相关关系。
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引用次数: 0
Study of structure and properties of platinum(II) chloride complexes with (2-alkyltetrazol-5-yl)acetic acid by quantum chemistry and NMR-spectroscopy methods 用量子化学和核磁共振光谱方法研究氯化铂与(2-烷基四唑-5-基)乙酸配合物的结构和性质
Pub Date : 2019-08-30 DOI: 10.33581/2520-257x-2019-2-3-11
V. Matulis, Ekaterina G. Ragoyja, T. V. Serebryanskaya, Yuri V. Grigoriev, O. Ivashkevich
It has been shown that the WP04 functional in combination with moderate basic sets 6-31G(d) and SDD allows to calculate characteristics of 1H NMR-spectrum of metal complexes with ligands based on tetrazole derivatives with high accuracy, which can be used to assign signals in the NMR-spectra. The process of hydrolysis of the isomeric platinum(II) chloride complexes with (2-isopropyltetrazol-5-yl)acetic acid has been investigated using the methods of quantum chemistry and NMR-spectroscopy. An explanation of the changes of signals in the 1H NMR-spectra of the considered complexes during their hydrolysis is given.
研究表明,WP04官能团与6-31G(d)和SDD相结合,可以高精度地计算基于四唑衍生物配体的金属配合物的1H核磁共振光谱特征,并可用于核磁共振光谱中的信号分配。采用量子化学和核磁共振光谱的方法研究了(2-异丙基四唑-5-基)乙酸水解异构体铂(II)氯配合物的过程。给出了所考虑的配合物在水解过程中1H核磁共振光谱信号变化的解释。
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引用次数: 0
Electrochemical synthesis of Sn–Ag alloy coatings in sulphate solution 硫酸盐溶液中Sn-Ag合金镀层的电化学合成
Pub Date : 2019-08-15 DOI: 10.33581/2520-257x-2019-2-51-61
O. Vrublevskaya, M. Shikun
The optimal conditions for the electrochemical synthesis in the sulfate electrolyte of low-melting Sn–Ag alloy coatings used in the assembly of electronic equipment containing 7.1–8.3 at. % of silver and with total current yield of metals equal to 88.8–87.0 % are determined. It is established that electrochemical reduction of Sn(II) and Ag(I) on the surface of the alloy is accompanied by the process of contact displacement of Ag(I) with tin included into the coating. The process of contact displacement is intensified with the electrolyte temperature growth and leads to the increase in silver content in the alloy, to the appearance of dendrites on the surface of the coating due to its passivation.
研究了在硫酸盐电解液中电化学合成含7.1-8.3 at电子设备装配用低熔点Sn-Ag合金镀层的最佳条件。测定银的总电流收率为88.8 - 87.0%。结果表明,合金表面Sn(II)和Ag(I)的电化学还原伴随着Ag(I)与镀层中锡的接触位移过程。接触位移过程随着电解液温度的升高而加剧,导致合金中银含量的增加,导致镀层钝化后表面出现枝晶。
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引用次数: 0
期刊
Journal of the Belarusian State University. Chemistry
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