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FLUORESCENCE CHARACTERISTICS OF FLUORESCEIN AND EOSIN Y SOLUTIONS IN WATER-MICELLAR SURFACTANT MEDIA 荧光素和伊红y溶液在水胶束表面活性剂介质中的荧光特性
Pub Date : 2020-01-01 DOI: 10.17721/1728-2209.2020.1(57).6
V. Klovak, L. Nechpai, Serhii Lelyushok, S. Kulichenko
The effect of cationic, anionic and nonionic surfactants on the fluorescence properties of fluorescein and eosin Y aqueous solutions has been investigated. It has been found that sodium dodecyl sulfate does not affect the position of the maximum wavelengths of solutions of fluorescein and eosin Y in the study of the effect of an anionic surfactant on the fluorescence emission intensity of dyes. The intensity of the signal of the dye solutions when changing the concentration of anionic surfactant changes little. As the concentration of non-ionic surfactant increases, the fluorescence emission intensity of the fluorescein solutions decreases. In contrast, with increasing concentration of Triton X-100, there is an increase in the signal intensity of solutions of more hydrophobic eosin Y with subsequent access to the "plateau" at СТХ-100≥5.1·10–2 mol/L. The position of the maxima fluorescence emission wavelengths for the fluorescein solutions in the 0-1.0·10–5 mol/L range of concentrations of cationic surfactant cetylpyridinium chloride remain unchanged. The position of the maxima shifts to the long-wavelength region of the spectrum at higher concentrations of CPC. The nature of the position dependence of the fluorescence emission maxima of eosin Y solutions in the presence of cationic surfactants is similar. The effect of fluorescence quenching has also been shown in the study of the influence of organic substances of cationic nature on the signal intensity of fluorescein solutions. It has been shown that the concentration dependence is linear in the (0.1–4.0)·10–1 mol/L range of isoniazid molecule concentrations. The data obtained can be implemented in the development of conditions and methods for the determination of pharmacologically active substances of cationic nature by reaction with fluorescein in medicines.
研究了阳离子、阴离子和非离子表面活性剂对荧光素和伊红Y水溶液荧光性能的影响。在研究阴离子表面活性剂对染料荧光发射强度的影响时,发现十二烷基硫酸钠不影响荧光素和伊红Y溶液的最大波长位置。改变阴离子表面活性剂的浓度时,染料溶液的信号强度变化不大。随着非离子表面活性剂浓度的增加,荧光素溶液的荧光发射强度降低。相比之下,随着Triton X-100浓度的增加,疏水性较强的伊红Y溶液的信号强度增加,随后进入СТХ-100≥5.1·10-2 mol/L的“平台”。在阳离子表面活性剂十六烷基吡啶氯浓度0 ~ 1.0·10 ~ 5 mol/L范围内,荧光素溶液的最大荧光发射波长位置保持不变。在较高的CPC浓度下,峰值的位置移向光谱的长波长区域。在阳离子表面活性剂的存在下,伊红Y溶液的荧光发射最大值的位置依赖性的性质是相似的。荧光猝灭效应在阳离子性有机物对荧光素溶液信号强度影响的研究中也得到了体现。结果表明,异烟肼分子浓度在(0.1 ~ 4.0)·10-1 mol/L范围内呈线性关系。所得数据可用于开发与荧光素反应测定药物中阳离子性药理活性物质的条件和方法。
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引用次数: 0
OPTICAL AND PHOTOCHEMICAL PROPERTIES OF POLYMERS BASED ON 2-(4-METHACRYOXYSTYRYL)QUINOLINE 2-(4-甲基丙烯氧基苯乙烯基)喹啉聚合物的光学和光化学性质
Pub Date : 2020-01-01 DOI: 10.17721/1728-2209.2020.1(57).15
O. Krupka, V. Smokal, O. Kharchenko, B. Derkowska-Zielinska
The design and synthesis of new polymer materials with controlled and predictable properties is still a challenge. Photoactive chromophore can be incorporated into a polymer in several different ways: guest-host systems, main chain polymers and side chain polymers. While none of these options are not perfect and each has its advantages and disadvantages. However, the chromophore functionalized polymers were found to be more effective due to: high concentration of the chromophores can be introduced; polymers with chromophore moiety show increased stability of poling induced SHG activity and decrease of the orientation relaxation process; absence of phase separation lessens the scattering losses; such techniques as plasma etching, optically induced index changes, laser ablation, electrical poling can be applied; multilayer phormation assists in easy integration with electronic and optical components. The principles of design of various molecular photoswitches and logical devices, in particular, those based on the photoisomerization reaction of diarylethylenes have been actively investigated in recent years. Azasubstituted diarylethylenes (DAE) styrylquinolines containing a central double bond and an endocyclic nitrogen atom, have become the subject of interest due to their ability to reversible transformations (photoisomerization and protonation). In this work, photosensitive polymers were synthesized by radical polymerization of corresponding styrylquinoline derivatives with comonomers methyl methacrylate (MMA) using asobisisobutyronitrile (AIBN) as radical initiator. We present results obtained for thin films of the methacrylic polymers incorporating styrylquinoline side-group as optically active molecule. Synthesis of 2-(4-methacryloxystyryl)quinolone and 2-(4-methacryloxystyryl)-6-methoxyquinoline was described. The polymers were obtained by free radical polymerization of methacrylic monomers in dimethylformamide with azobisisobutyronitrile as initiator. The products of polymerization were characterized and evaluated by 1HNMR, UV spectroscopy. Glass transition temperatures were characterized by DSC method. It was found 133°C, 110°C, 130°C, 112°C for P1, P1MMA, P2, P2MMA respectively. Their optical and photochemical properties as well as temperature dependence of the photoluminescence of diarylethylenes have been investigated.
设计和合成具有可控制和可预测性能的新型高分子材料仍然是一个挑战。光活性发色团可以通过几种不同的方式加入到聚合物中:主链聚合物、主链聚合物和侧链聚合物。虽然这些选择都不是完美的,每个都有其优点和缺点。然而,由于可以引入高浓度的发色团,因此发现发色团功能化聚合物更有效;具有生色团片段的聚合物具有较高的极性诱导SHG活性稳定性,取向弛豫过程减弱;无相分离减小了散射损失;可采用等离子体刻蚀、光致折射率变化、激光烧蚀、电极化等技术;多层成形有助于与电子和光学元件轻松集成。近年来,各种分子光开关和逻辑器件的设计原理,特别是基于二乙基乙烯光异构反应的光开关和逻辑器件的设计原理得到了积极的研究。偶氮取代二乙基乙烯(DAE)苯基喹啉含有一个中心双键和一个内环氮原子,由于它们具有可逆转化(光异构化和质子化)的能力而成为人们感兴趣的主题。本文以亚二异丁腈(AIBN)为引发剂,用甲基丙烯酸甲酯(MMA)和苯基喹啉衍生物进行自由基聚合,合成了相应的光敏聚合物。我们得到了以苯基喹啉侧基为旋光分子的甲基丙烯酸聚合物薄膜的结果。研究了2-(4-甲基丙烯氧基苯乙烯基)喹诺酮和2-(4-甲基丙烯氧基苯乙烯基)-6-甲氧基喹啉的合成。以偶氮二异丁腈为引发剂,在二甲基甲酰胺中对甲基丙烯酸单体进行自由基聚合。通过核磁共振、紫外光谱对聚合产物进行了表征和评价。用DSC法表征了玻璃化转变温度。P1、P1MMA、P2、P2MMA分别在133°C、110°C、130°C、112°C下存在。研究了二乙基乙烯的光学和光化学性质以及光致发光的温度依赖性。
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引用次数: 0
STRUCTURAL AND SPECTRAL STUDIES OF THE MIXED-LIGAND CATION COMPLEX OF LANTHANUM [Lа(L)2bipy2]BPh4 WITH CARBACYLAMIDOPHOSPHATE (CAPH) TYPE LIGAND AND 2,2'-BIPYRIDINE 镧[l_ (L)2bipy2]BPh4与碳酰基氨基磷酸(CAPH)型配体和2,2′-联吡啶混合配体阳离子配合物的结构和光谱研究
Pub Date : 2020-01-01 DOI: 10.17721/1728-2209.2020.1(57).4
M. Struhatska, I. Olyshevets, V. Dyakonenko, V. Ovchynnikov, S. Shishkina, V. Amirkhanov
A new cationic mixed-ligand complex [Lа(L)2bipy2]BPh4 (where L-= bis(N,N'-diethylamide)(N'-trichloroacetyl)-triamidophosphate anion, bipy = 2,2'-bipyridine) has been synthesized and studied by the means of IR, 1H NMR spectroscopy, thermogravimetric and X-ray structural analyses. Low-frequency shifts of the absorption bands of the carbonyl and phosphoryl groups of phosphorylated ligand in the IR spectra of the complex compared with similar absorption bands in the spectrum of "free" CAPh ligand are Δν(C = O) = 117 cm–1 and Δν(P = O) = 137 cm–1. The analysis of integral signal intensity in the investigated NMR spectra of coordination compounds [Lа(L)2bipy2]BPh4 indicates the molar ratio of ligand : bipyridine : tetraphenylborate anion as a 2:2:1, which corresponds to the proposed structure of the complexes. The compound has been obtained in monocrystalline form. The structure of the complex has been determined by X-ray structural analysis, its ionic structure was proved, and the coordination of two CAPh ligands through the oxygen atoms of the carbonyl and phosphoryl groups was confirmed. Based on the structural data, it was determined that the La3+ ion is octocoordinated (surrounded by four oxygen atoms from two chelated phosphoryl ligands and four nitrogen atoms from two 2,2'-bipyridine molecules). The coordination polyhedron of central ion is interpreted as a square antiprism. Complex cations and tetraphenylborate anions are connected both by electrostatic interaction and by weak intermolecular C – H ∙∙∙ π-contacts between phenyl substituents of BPh4- and molecules of 2,2'-bipyridine. It was established by thermogravimetric analysis that the complex [Lа(L)2bipy2]BPh4 obtained is thermally stable up to a temperature of 150 °C. Significant decomposition of the complex begins at a temperature of 150 °C, occurs in one stage and most intensively continues up to 300 °C. The total weight loss is 78 %.
合成了一种新型阳离子混合配体配合物[l_ (L)2bipy2]BPh4(其中L-=双(N,N′-二乙基酰胺)(N′-三氯乙酰基)-三氨基磷酸阴离子,bipy = 2,2′-联吡啶),并通过红外光谱、1H NMR、热重和x射线结构分析对其进行了研究。在配合物的红外光谱中,磷酸化配体的羰基和磷基的吸收带与“自由”CAPh配体的吸收带相比,低频位移分别为Δν(C = O) = 117 cm-1和Δν(P = O) = 137 cm-1。配位化合物[lfe (L)2bipy2]BPh4的核磁共振谱积分信号强度分析表明配体:联吡啶:四苯基硼酸盐阴离子的摩尔比为2:2:1,与所提出的配合物结构相对应。该化合物以单晶形式得到。通过x射线结构分析确定了配合物的结构,证实了其离子结构,并通过羰基和磷基的氧原子确定了两个CAPh配体的配位。根据结构数据,确定La3+离子是八配位的(由两个螯合磷酰配体的四个氧原子和两个2,2'-联吡啶分子的四个氮原子包围)。中心离子的配位多面体被解释为一个方形反棱镜。配合物阳离子和四苯基硼酸盐阴离子通过静电相互作用和BPh4-的苯基取代基与2,2'-联吡啶分子之间的弱分子间C - H∙∙π-接触连接。热重分析表明,所制得的配合物[lfe (L)2bipy2]BPh4在150℃温度下是热稳定的。该复合物的显著分解始于150°C的温度,发生在一个阶段,最密集地持续到300°C。总体重减轻了78%。
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引用次数: 0
DETERMINATION OF ORTHOPHOSPHATE IN WATER BY SOLID-PHASE CHEMILUMINESCENT METHOD 固相化学发光法测定水中正磷酸盐
Pub Date : 2020-01-01 DOI: 10.17721/1728-2209.2020.1(57).17
G. Sumarokova, R. Linnik, О. Zaporozhets, L. Zinko
Phosphorus is one of the most important nutrients. Excessive content of its compounds in water objects leads to eutrophication, as well as reduces water quality. Methods based on the formation of molybdophosphate heteropolyacid (HPA) in an acidic medium with its subsequent reduction and spectrophotometric detection of the formed reduced "blue" HPA are most often used to determine phosphorus compounds. These methods are unsuitable for the analysis of waters with a phosphorus content <40 μg /L. The use of the chemiluminescent method (CL) makes it possible to increase the sensitivity of the determination, but CL detection in an acidic medium under the conditions of formation of HPA is limited by the existing indicator systems. To increase the selectivity of the method for determining the microquantities of phosphate relative to metal ions, we used an approach based on the adsorption removal of analyte with next determination using the CL method. Previous removal of phosphate from an aqueous solution in the form of reduced molybdostibiumphosphate HPA was released using batch technique in optimal conditions of its formation in the solution. Silica modified with cetyltrimethylammonium bromide was used as anion exchange adsorbent. Then the concentrate was processed with alkaline lucigenin solution and registration of the CL glow resulting from the reaction. Under optimal conditions of phosphate determination, the calibration curve is linear in the range from 3.7 to 147 μg PO43–/L with a detection limit of 0.8 μg PO43–/L. Cations K+, Na+, Fe(III), Mo(VI), NH4+ and anions Cl–, F–, HCO3–, С4Н4О62–, Asc–, NO2–, SO42–, as well as EDTA, do not interfere. Silicates (SiO32–) do not interfere with the determination of phosphate, even in 100-fold excess. Nitrates at concentrations below the average content in drinking water do not interfere with the determination. The developed technique was tested on a sample of pump room water. The technique is characterized by high sensitivity and a wide range of detectable concentrations. It is not inferior in sensitivity to flow methods using fluorescent or chemiluminescent detection.
磷是最重要的营养物质之一。其化合物在水中的过量含量会导致富营养化,并降低水质。基于磷酸钼杂多酸(HPA)在酸性介质中的形成及其随后的还原和形成的还原“蓝色”HPA的分光光度法检测的方法最常用于测定磷化合物。这些方法不适用于磷含量<40 μg /L的水质分析。化学发光法(CL)的使用使测定灵敏度的提高成为可能,但现有的指示剂体系限制了CL在酸性介质中形成HPA条件下的检测。为了提高该方法相对于金属离子测定微量磷酸盐的选择性,我们采用了一种基于吸附去除分析物的方法,并使用CL法进行下一次测定。在溶液中形成磷酸盐的最佳条件下,采用批处理技术以还原性磷酸钼铋HPA的形式从水溶液中去除磷酸盐。采用十六烷基三甲基溴化铵改性二氧化硅作为阴离子交换吸附剂。然后用碱性lucigenin溶液对浓缩物进行处理,记录反应产生的CL辉光。在最佳条件下,校准曲线在3.7 ~ 147 μg PO43 - /L范围内呈线性关系,检出限为0.8 μg PO43 - /L。阳离子K+、Na+、Fe(III)、Mo(VI)、NH4+和阴离子Cl -、F -、HCO3 -、С4Н4О62 -、Asc -、NO2 -、SO42 -以及EDTA不受干扰。硅酸盐(SiO32 -)不干扰磷酸盐的测定,即使超过100倍。低于饮用水中平均含量的硝酸盐浓度不会干扰测定。该技术已在某泵房水样品上进行了试验。该技术具有灵敏度高、检测浓度范围广的特点。它的灵敏度不低于使用荧光或化学发光检测的流动方法。
{"title":"DETERMINATION OF ORTHOPHOSPHATE IN WATER BY SOLID-PHASE CHEMILUMINESCENT METHOD","authors":"G. Sumarokova, R. Linnik, О. Zaporozhets, L. Zinko","doi":"10.17721/1728-2209.2020.1(57).17","DOIUrl":"https://doi.org/10.17721/1728-2209.2020.1(57).17","url":null,"abstract":"Phosphorus is one of the most important nutrients. Excessive content of its compounds in water objects leads to eutrophication, as well as reduces water quality. Methods based on the formation of molybdophosphate heteropolyacid (HPA) in an acidic medium with its subsequent reduction and spectrophotometric detection of the formed reduced \"blue\" HPA are most often used to determine phosphorus compounds. These methods are unsuitable for the analysis of waters with a phosphorus content <40 μg /L. The use of the chemiluminescent method (CL) makes it possible to increase the sensitivity of the determination, but CL detection in an acidic medium under the conditions of formation of HPA is limited by the existing indicator systems. To increase the selectivity of the method for determining the microquantities of phosphate relative to metal ions, we used an approach based on the adsorption removal of analyte with next determination using the CL method. Previous removal of phosphate from an aqueous solution in the form of reduced molybdostibiumphosphate HPA was released using batch technique in optimal conditions of its formation in the solution. Silica modified with cetyltrimethylammonium bromide was used as anion exchange adsorbent. Then the concentrate was processed with alkaline lucigenin solution and registration of the CL glow resulting from the reaction. Under optimal conditions of phosphate determination, the calibration curve is linear in the range from 3.7 to 147 μg PO43–/L with a detection limit of 0.8 μg PO43–/L. Cations K+, Na+, Fe(III), Mo(VI), NH4+ and anions Cl–, F–, HCO3–, С4Н4О62–, Asc–, NO2–, SO42–, as well as EDTA, do not interfere. Silicates (SiO32–) do not interfere with the determination of phosphate, even in 100-fold excess. Nitrates at concentrations below the average content in drinking water do not interfere with the determination. The developed technique was tested on a sample of pump room water. The technique is characterized by high sensitivity and a wide range of detectable concentrations. It is not inferior in sensitivity to flow methods using fluorescent or chemiluminescent detection.","PeriodicalId":9359,"journal":{"name":"Bulletin of Taras Shevchenko National University of Kyiv. Chemistry","volume":"228 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74094875","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}
引用次数: 0
REACTION OF PYRIDO[2,1-a]ISOINDOLE WITH З (R)- AND (S)- N-α-METHILBENZYLMALEIMIDE 吡啶[2,1-a]异吲哚与З (R)-和(S)- N-α-甲基苄基马来酰亚胺的反应
Pub Date : 2020-01-01 DOI: 10.17721/1728-2209.2020.1(57).11
T. Yegorova, B. Barnych, Z. Voitenko
Selective chemical reactions create new possibilities for controlled synthesis of compounds with pre-designed properties for further use in medical chemistry, material science and other fields. This is especially useful for such synthetic methodology as [4+2] cycloaddition. Current work is dedicated to study of reactions between N-chiral maleinimides with cyclic dienes based on the pyridoisoindol. Pyrido[2,1-a]isoindol turned out to be the most practical object to study the first example of asymmetric variant of the Diels-Alder reaction involving condensed isoindols. Previously, we established that this heterocyclic system, in contrast to other azino- and azoloisoindols, upon undergoing cycloaddition with non-chiral maleinimides gives only rearranged adducts of the first type. This type of compounds have also interesting stereochemistry: in solid state they have twisted double bond (twist angle 7-10°), while in solution they exist as a mixture of athropodiastereomeres due to the asymmetric Carbon atom and hindered rotation around С–С bond between exocyclic double bond and 2-(α-pyridil)phenyl fragment. Initial expectation was that chiral induction would influence the ratio of corresponding athropodiastereomeres. Calculations show that there are four possible athropodiastereomeres due to the chiral center and sterically hindered chiral axis. In case of non-chiral dienophiles, reaction results in two major diastereomeres (for our purposes marked as A and B) with 70:30 ration and two minor isomers (marked С and D respectively), the latter constituting less than 5% of the total amount. Major and minor isomers are in constant complex equilibrium, controlled via slow rotation of around corresponding С-С bond on one hand (which is the reason for athropodiastereomeres between major forms A and B, shown via NMR spectra at different temperatures), and on the other hand – fast equilibrium due to the 1,5-sigmatropic shift (cause for the minor forms C and D). Target reaction was studied under standard conditions for this rearrangement and under the kinetic control in the inert atmosphere at -80°С using TiCl4 as catalyzer. We therefore show that reaction pathway is similar to our previous examples and results in rearranged adducts of the first type. Ratio of athropodiastereomeres (both major and minor forms) is different from previous examples using non-chiral 2-substituted maleimides. Asymmetric induction spontaneously transfers from influencing the Diels-Alder reaction to influencing synchronic sigmatropic rearrangement, which is the final stage in the formation of the rearranged adduct of the first type in condensed isoindol systems.
选择性化学反应为控制合成具有预先设计性能的化合物创造了新的可能性,这些化合物可进一步用于医学化学、材料科学和其他领域。这对于[4+2]环加成等合成方法特别有用。目前主要研究n -手性马来酰亚胺与吡啶异吲哚类环二烯的反应。Pyrido[2,1-a]异吲哚被证明是研究Diels-Alder反应不对称变体中涉及缩合异吲哚的第一个例子中最实用的对象。在此之前,我们确定了该杂环体系,与其他氮基和偶氮异吲哚相比,在与非手性马来酰亚胺进行环加成后,只得到第一类重排加合物。这类化合物还具有有趣的立体化学性质:在固体状态下,它们具有扭曲的双键(扭转角为7-10°),而在溶液中,由于碳原子的不对称和绕С -С外环双键和2-(α-吡啶)苯基片段的旋转受阻,它们以脂肪脚非对映体的混合物存在。最初的预期是手性诱导会影响相应的肌足异体的比例。计算表明,由于手性中心和位阻手性轴的存在,有四种可能的肌足非对映体。对于非手性亲二烯亲和物,反应产生两个比例为70:30的主要非对映异构体(为我们的目的标记为A和B)和两个次要异构体(分别标记为С和D),后者占总量不到5%。主要异构体和次要异构体处于恒定的复杂平衡状态,一方面通过相应С-С键的缓慢旋转来控制(这就是主要形式A和B之间的肌脚非对映体的原因,通过不同温度下的核磁共振光谱显示);在-80°С的惰性气氛中,以TiCl4为催化剂,在动力学控制下,研究了这种重排的标准条件下的目标反应。因此,我们表明反应途径与我们前面的例子相似,并导致第一类加合物的重排。肌足非对映体的比例(包括主要形式和次要形式)与先前使用非手性2-取代马来酰亚胺的例子不同。不对称诱导自发地从影响Diels-Alder反应转变为影响同步信号型重排,这是缩合异吲哚体系中第一类重排加合物形成的最后阶段。
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引用次数: 0
GAS SENSITIVE SEMICONDUCTOR NANOMATERIALS FOR CREATION OF HYDROGEN SENSORS 用于制造氢传感器的气敏半导体纳米材料
Pub Date : 2020-01-01 DOI: 10.17721/1728-2209.2020.1(57).10
I. Matushko, L. Oleksenko, N. Maksymovych, Galina Skolyar, O. Roik, G. Fedorenko, L. Lutsenko, Oleksandr Ripko
Co-precipitaion method and sol-gel technique were used to prepare semiconductor microcrystalline and nanosized SnO2/Sb2O5 and Со/SnO2/Sb2O5 (0.15 wt.% Sb) materials aimed to create high sensitive hydrogen sensors. Morphology and phase composition of the obtained samples were studied by SEM, TEM and XRD methods. It was found that microcrystalline SnO2/Sb2O5 material with particle size of 1–30 μm was obtained by a co-precipitation method and nanosized SnO2/Sb2O5 material with particle size of 5–25 μm (an average size – 12 nm) was obtained by a zol-gel method. Only cassiterite phase was detected for both microcrystalline and nanosized materials. Sensitivity measurements of the sensors were carried out with using of air-hydrogen mixtures in the concentration range of 40 – 1145 ppm Н2, and dynamic characteristics (response time and relax time) were evaluated for 40 ppm Н2 at different heater power consumptions – 0.25 and 0.35 W. To increase sensitivities of the sensors, cobalt oxide, a known catalyst for hydrogen oxidation, was added to the resulting SnO2/Sb2O5 materials. It was shown that the sensors obtained by a zol-gel method demonstrate more significant sensitivity to hydrogen concentration in comparison with the sensors obtained by a co-precipitation method. It is probably associated with a higher surface area of the nanomaterial that agrees with its smaller particles as compared with the particles of the microcrystalline material. The Co-containing sensors based on the nanosized SnO2/Sb2O5 material are established to reveal higher sensitivity to Н2 than microcrystalline Co/SnO2/Sb2O5 sensors. The Co-containing sensors based on the nanosized SnO2/Sb2O5 material were found to have better dynamic characteristics than microcrystalline Co/SnO2/Sb2O5 sensors. The sensitivities increase and the response and recovery time decrease were found for both sensor materials at increasing of the sensors heater power consumption. The obtained results can be explained with different degree of energy surface heterogeneity of the used materials. The sensor response time is determined by the time of dynamic equilibrium establishment of the hydrogen oxidation reaction on the sensor surface and the recovery time is determined by the time of desorption of the H2 oxidation reaction products (H2O) from the sensor surface. Because of the processes, the sensor with a gas sensitive layer based on the nanosized material possessing with more homogeneous structure of its surface (according to the obtained TEM data) demonstrates improved gas sensitive properties in comparison with the sensor based on the microcrystalline material. The obtained results concerning the sensitivities to H2 and the dynamic parameters of the created sensors point to possibility of effective usage of the sensors based on the nanomaterial to detect H2 in air in the practice.
采用共沉淀法和溶胶-凝胶技术制备了半导体微晶和纳米级SnO2/Sb2O5和Со/SnO2/Sb2O5 (0.15 wt.% Sb)材料,旨在制造高灵敏度的氢传感器。采用SEM、TEM和XRD等方法研究了样品的形貌和相组成。结果表明,共沉淀法可获得粒径为1 ~ 30 μm的SnO2/Sb2O5微晶材料,zol-gel法可获得粒径为5 ~ 25 μm(平均粒径为- 12 nm)的SnO2/Sb2O5纳米材料。在微晶和纳米材料中只检测到锡石相。在40 - 1145 ppm Н2的空气-氢混合物浓度范围内对传感器的灵敏度进行了测量,并在不同的加热器功率消耗(0.25和0.35 W)下,对40 ppm Н2的动态特性(响应时间和放松时间)进行了评估。为了提高传感器的灵敏度,将已知的氢氧化催化剂氧化钴添加到所得的SnO2/Sb2O5材料中。结果表明,与共沉淀法相比,zol-gel法获得的传感器对氢浓度的灵敏度更高。这可能与纳米材料的高表面积有关,与微晶材料的颗粒相比,纳米材料的颗粒更小。基于纳米SnO2/Sb2O5材料的含Co传感器对Н2的灵敏度高于微晶Co/SnO2/Sb2O5传感器。基于纳米SnO2/Sb2O5材料的含Co传感器比微晶Co/SnO2/Sb2O5传感器具有更好的动态特性。随着传感器加热器功耗的增加,两种传感器材料的灵敏度均增加,响应时间和恢复时间均减少。所得结果可以用所用材料不同程度的能量表面非均质性来解释。传感器响应时间由传感器表面氢氧化反应建立动态平衡的时间决定,恢复时间由传感器表面氢氧化反应产物(H2O)解吸的时间决定。由于这些工艺,基于纳米材料的气敏层传感器具有更均匀的表面结构(根据获得的TEM数据),与基于微晶材料的传感器相比,具有更好的气敏性能。所获得的传感器对氢气的灵敏度和动态参数的结果表明,基于纳米材料的传感器在实际中有效应用于空气中氢气的检测是可能的。
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引用次数: 0
FEATURES OF COMPONENT INTERACTION IN LIQUID ALLOYS OF TERNARY Al-Ge-3d-Me (Me = Mn, Fe, Ni, Cu) SYSTEMS 三元Al-Ge-3d-Me (Me = Mn, Fe, Ni, Cu)体系液态合金中组分相互作用的特征
Pub Date : 2020-01-01 DOI: 10.17721/1728-2209.2020.1(57).9
N. Kotova, Natalia Usenko, N. Golovata
The features of the component interaction in liquid alloys of ternary Al-Ge-3d-Me systems (Me = Mn, Fe, Ni, Cu) are described. A joint analysis of the concentration dependences of the enthalpies of mixing of liquid alloys previously obtained by the authors via high-temperature calorimetry, and also of the phase diagrams of the constituent binary systems was carried out. The relationship between the enthalpy values and the type of short-range ordering in liquid alloys of the studied systems was established. The visual similarity of the topology of the projections of ΔmH isolines of the Al-Ge-Fe (Ni, Cu) liquid alloys and a completely different course of the isolines of the enthalpies of mixing for the liquid Al-Ge-Mn alloys are established. The changes in the absolute values of the ΔmHmin from system to system are observed. The enthalpies are approximately the same for the Al-Ge-Mn and Al-Ge-Fe systems (about -20 kJ⋅mol-1), they increase significantly from Al-Ge-Fe to Al-Ge-Ni (-50 kJ⋅mol-1), and then decrease substantially towards the Al-Ge-Cu system (-15 kJ⋅mol-1). For the Al-Ge-Mn (Fe, Ni, Cu) liquid alloys the lines of extreme interaction are located near the 3d-corner of the concentration triangle. These lines connect the compositions of the most stable intermetallic compounds in binary Al(Ge)-Mn(Fe, Ni, Cu) systems. It has been shown that the thermodynamic properties of Al-Ge-Fe (Ni, Cu) liquid alloys are mainly determined by the pair interaction of the components of the constituent binary Al-Fe(Ni, Cu) and Ge-Fe(Ni, Cu) systems, the influence of Al-Fe(Ni, Cu) systems being prevailed. For the Al-Ge-Mn system, the interaction of components in the Ge-Mn binary system gives the main contribution to the thermodynamic properties of the ternary system. The Al-Ge-Mn (Fe, Cu) systems are characterized by significantly lower absolute values of the heats of alloy formation compared to the Al-Ge-Ni one. The specified characteristics of component interaction in the ternary systems under consideration and different values of the enthalpies of mixing are determined by the peculiarities and regular changes of the electronic structure of 3d metals across the 3d series from Mn to Cu.
描述了Al-Ge-3d-Me三元体系(Me = Mn, Fe, Ni, Cu)液态合金中组分相互作用的特征。对作者先前通过高温量热法得到的液态合金混合焓的浓度依赖性和二元体系的相图进行了联合分析。建立了所研究体系中液相合金的焓值与短程有序类型之间的关系。建立了Al-Ge-Fe (Ni, Cu)液态合金ΔmH等值线投影拓扑的视觉相似性和Al-Ge-Mn液态合金混合焓等值线的完全不同的过程。观察了系统间ΔmHmin绝对值的变化。Al-Ge-Mn和Al-Ge-Fe体系的焓值基本相同(约为-20 kJ·mol-1),从Al-Ge-Fe到Al-Ge-Ni体系的焓值显著增加(-50 kJ·mol-1),然后向Al-Ge-Cu体系的焓值大幅下降(-15 kJ·mol-1)。Al-Ge-Mn (Fe, Ni, Cu)液态合金的极端相互作用线位于浓度三角形的3d角附近。这些线连接了二元Al(Ge)-Mn(Fe, Ni, Cu)体系中最稳定的金属间化合物的组成。结果表明,Al-Ge-Fe (Ni, Cu)液态合金的热力学性质主要由二元Al-Fe(Ni, Cu)体系和Ge-Fe(Ni, Cu)体系组分的对相互作用决定,其中Al-Fe(Ni, Cu)体系的影响更大。对于Al-Ge-Mn体系,Ge-Mn二元体系中组分的相互作用对三元体系的热力学性质起主要作用。Al-Ge-Mn (Fe, Cu)体系的合金形成热绝对值明显低于Al-Ge-Ni体系。所考虑的三元体系中组分相互作用的特定特征和不同的混合焓值是由三维金属在从Mn到Cu的三维系列中电子结构的特殊性和规律性变化决定的。
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引用次数: 0
REACTION OF 2-HETARYL-2-(DIHYDROFURAN-2(3H)-ILIDEN)ACETONITRILES WITH AROMATIC AMINES 2-己基-2-(二氢呋喃-2(3h)-苯胺)乙腈与芳香胺的反应
Pub Date : 2020-01-01 DOI: 10.17721/1728-2209.2020.1(57).12
R. Shemehen, O. Khilya, Y. Volovenko
This article reports on the reaction of 2-hetaryl-2-(furanyl-2-ylidene)acetonitriles with aromatic amines as N-nucleophiles. 2-Hetaryl-2-(furanyl-2-ylidene)acetonitriles represent versatile building blocks in syntheses of ω-(N-aryl)alkyl substituted heterocycles due to the presence of 1,3-bielectrophilic acrylonitrile fragment functionalized with unsaturated heterocyclic ring and nucleophilic azaheterocyclic moiety. The carbonyl group masked within the N-arylpyrrolidinylidene fragment which undergoes a ring opening through the reaction with nucleophiles. So, a method for the synthesis of 2-hetaryl-6-hydroxy-3-(arylamino)hex-2-enenitriles and 2-hetaryl-2-(N-arylpyrrolidin-2-ylidene)acetonitriles has been developed by us. The proposed scheme is based on the available reagents using. As a result of Michael addition, the aromatic amines to 2-hetaryl-2-(furanyl-2-ylidene)acetonitriles followed by ring transformations has formed two types of products, depending on the reaction conditions. The reaction of substituted furanylylideneacetonitriles with aromatic amines proceeds in good to high yields affording the corresponding 3-(arylamino)hex-2-enenitriles and 2-(N-arylpyrrolidin-2-ylidene)acetonitriles derivatives. The stereochemistry of the ring-opening reaction follows the rules of a classical SN2 mechanism. The resulting linear products can be cyclized to 2-hetaryl-2-(furanyl-2-ylidene)acetonitriles in high yields by treatment with the catalytic amount of acid or the equimolar amount of aromatic amines. Under these conditions 2-hetaryl-6-hydroxy-3-(arylamino)hex-2-enenitriles arising from reaction gives the ring closure. Since both ring-opening and cyclisation occur with fixed stereochemistry the reaction appears a valuable modification to the preparation of acetonitriles derivatives.
本文报道了2-己基-2-(呋喃基-2-酰基)乙腈与芳香胺作为n -亲核试剂的反应。2-己基-2-(呋喃基-2-酰基)乙腈是合成ω-(n -芳基)烷基取代杂环的通用构件,因为它含有1,3-亲二电的丙烯腈片段,并被不饱和杂环和亲核的氮杂环部分功能化。羰基隐藏在n -芳基吡咯烷二基片段内,该片段通过与亲核试剂的反应开环。因此,我们提出了一种合成2-己基-6-羟基-3-(芳基)六-2-烯腈和2-己基-2-(n-芳基吡咯烷-2-芳基)乙腈的方法。提出的方案是基于可用的试剂使用。由于Michael加成,芳香胺对2-己基-2-(呋喃基-2-乙基)乙腈进行环转化,根据反应条件的不同,形成了两类产物。取代呋喃基吡啶乙腈与芳香胺的反应收率较高,得到相应的3-(芳胺)六-2-烯腈和2-(n-芳基吡啶-2-基)乙腈衍生物。开环反应的立体化学反应遵循经典SN2反应机理的规律。用催化量的酸或等摩尔量的芳胺处理,所得线性产物可以高收率地环化成2-己基-2-(呋喃基-2-乙基)乙腈。在这些条件下,由反应产生的2-己基-6-羟基-3-(芳胺)己基-2-烯腈使环闭合。由于开环和环化都是在固定的立体化学条件下发生的,因此该反应是制备乙腈衍生物的一种有价值的改性反应。
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引用次数: 0
STRUCTURE OF THE ZINC COMPLEX WITH CYCLOHEXYL AСETOACETATE 锌与环己基配合物的结构aСetoacetate
Pub Date : 2020-01-01 DOI: 10.17721/1728-2209.2020.1(57).16
O. Shtokvysh, L. Koval, V. Dyakonenko, V. Pekhnyo
Binuclear complex of Zn(II) with cyclohexyl acetoacetate was obtained and structurally characterized for the first time. According to structural data, the crystal system is triclinic, space group P-1; a = 7.6530(4), b = 12.2412(8), c = 12.9102(9) Å; α = 90.198(5), β = 101.071(5), γ = 96.937(5) deg. The molecular structure corresponds to the formula [Zn2(C10H15O3)4(C2H5OH)2]. The complex is located in a special position to the symmetry center of the unit cell. The coordination polyhedrons of the Zn atoms are the same distorted octahedrons formed by six oxygen atoms. Each formed by 4 oxygen atoms in the equatorial position, which belong to three ligand molecules: terminal ligand (2 oxygen atoms) and bridged ligand (1 oxygen atom) which chelate the zinc atom of the named polyhedron and 1 oxygen atom belong to a bridged ligand that chelates the other nucleus and monodentantly coordinated to mentioned one. Two oxygen atoms occupy an axial position, one of which belongs to the terminal ligand, mentioned above and the other to the coordinated ethanol molecule. The bond between the complex nuclei is stabilized by two hydrogen bonds formed by the hydrogen atoms from hydroxyl groups of ethanol molecules and the enol oxygen atoms of the terminal ligands of the other nucleus. The compound was also characterized by IR-spectroscopy, characteristic bands (сm-1) are: ν(C–H) - 2936, 2860, ν(C=O) & ν(C=C) – 1612, ν(C=O) + δ(C–H) – 1532, ν(C=C) & ν(C-CH3)– 1252, δ(C–H) – 1172, π(C–H) – 784, ν(M–O) – 456, 416. IR spectroscopy data confirm the bidentate coordination of cyclohexyl acetoacetate to zinc atoms in deprotonated form with the formation of chelated metallocycles. The structure of the complex is similar to the structures of cobalt and nickel complexes with cyclohexyl acetoacetate. Analysis of XRD-data (which are supplemented with this work) for Co(II), Ni(II) and Zn(II) complexes with acetoacetic acid esters shows that their structure, in particular the number of metal centers in the structures, regardless of the nature of the central atom or the alcohol fragment, but determined the presence of components capable of complementing the coordination sphere of the metal in reaction media.
首次合成了锌(II)与乙酰乙酸环己基的双核配合物,并对其结构进行了表征。结构资料表明,该晶体体系为三斜晶系,空间群P-1;A = 7.6530(4), b = 12.2412(8), c = 12.9102(9) Å;α = 90.198(5), β = 101.071(5), γ = 96.937(5)度,分子式为[Zn2(C10H15O3)4(C2H5OH)2]。这个复合物位于一个特殊的位置,相对于细胞的对称中心。锌原子的配位多面体是由6个氧原子组成的畸变八面体。每一个都由4个氧原子在赤道位置形成,它们属于3个配体分子:末端配体(2个氧原子)和桥接配体(1个氧原子),它们螯合所述多面体的锌原子和1个氧原子,属于桥接配体,它们螯合另一个核并与所述核单齿配位。两个氧原子占据一个轴向位置,其中一个属于上述末端配体,另一个属于配位乙醇分子。由乙醇分子羟基上的氢原子和另一个核末端配体上的烯醇氧原子形成的两个氢键稳定了复合体核之间的键。用红外光谱对该化合物进行了表征,特征波段为:ν(C- h) - 2936,2860, ν(C=O) & ν(C=C) - 1612, ν(C=O) + δ(C - h) - 1532, ν(C=C) & ν(C- ch3) - 1252, δ(C - h) - 1172, π(C - h) - 784, ν(M-O) - 456,416。红外光谱数据证实了乙酰乙酸环己基与去质子形式锌原子的双齿配位,并形成螯合金属环。该配合物的结构类似于钴和镍与乙酰乙酸环己基配合物的结构。对Co(II)、Ni(II)和Zn(II)与乙酰乙酸酯配合物的xrd数据分析(补充了本工作)表明,它们的结构,特别是结构中金属中心的数量,与中心原子或醇片段的性质无关,而是决定了在反应介质中能够补充金属配位球的组分的存在。
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引用次数: 0
CATECHOLASE ACTIVITY OF A COPPER(II) COMPLEX WITH THE 2-(5-(1,2,4)TRIAZOLE-1-ILMETHYL-1H-(1,2,4)-TRIAZOLE-3-IL)-PYRIDYL 2-(5-(1,2,4)三唑-1- il -甲基-1- 1- 2,4)三唑-3- il)-吡啶配合物铜(ii)的儿茶酚酶活性
Pub Date : 2020-01-01 DOI: 10.17721/1728-2209.2020.1(57).5
D. Khomenko, Roman O. Doroschuk, I. Odarych, I. Raspertova, R. Lampeka
Methods of the synthesis of 2-(5-(1,2,4)triazol-1-ylmethyl-1H-(1,2,4)-triazol-3-yl)-pyridine and a binuclear copper complex are described. The structure of the complex is established by X-ray structural analysis. The complex is a centrosymmetric [Cu2(L)2(NO3)2·2H2O]·H2O dimer. The Cu-Cu distance is 4.0408 (3) Å. In the complex the ligand is in a deprotonated state. Due to this, the triazole fragment acts as a bridge between the two metal centers. Copper ions are in an octahedral environment. The equatorial plane is formed by three triazole nitrogen atoms and one pyridyl nitrogen atom. The axial positions are occupied by a water molecule and a nitrate ion. Isotropic patterns corresponding to binuclear copper particles of the [Cu2L2-H]+ composition were registered in the ESI mass spectra of the solution of the [Cu2(L)2(NO3)2(H2O)2]·H2O complex. These data confirm the presence of a binuclear complex in solution. The catecholoxidase activity of the binuclear copper (II) complex based on 2-(5-(1,2,4)triazol-1-ylmethyl-1H-(1,2,4)-triazol-3-yl)-pyridine was studied. The kinetics of model reactions of the catecholase type were investigated by the method of initial velocities using a model substrate of 3,5-di-tert-butyl catechol (3,5-DTBK). At low concentrations of 3,5-DTBK, the dependence of the initial oxidation rate on the concentration of the substrate is linear, which corresponds to the first order of the reaction on the substrate. However, the dependence graph at higher concentrations of 3,5-DTBK is nonlinear and indicates the saturation of the catalyst with the substrate. The form of the dependence of the initial reaction rate on the substrate concentration is explained within the framework of the Michaelis-Menten model, which well describes the behavior of natural metaloenzymes.
介绍了2-(5-(1,2,4)三唑-1-基甲基- 1h -(1,2,4)三唑-3-基)吡啶和双核铜配合物的合成方法。通过x射线结构分析确定了配合物的结构。该配合物为中心对称的[Cu2(L)2(NO3)2·2H2O]·H2O二聚体。Cu-Cu距离为4.0408 (3)Å。在配合物中,配体处于去质子化状态。因此,三唑碎片在两个金属中心之间起着桥梁的作用。铜离子处于八面体环境中。赤道面由三个三唑氮原子和一个吡啶氮原子组成。轴向位置由一个水分子和一个硝酸盐离子占据。在[Cu2(L)2(NO3)2(H2O)2]·H2O配合物溶液的ESI质谱中,发现了[Cu2L2-H]+组成的双核铜粒子对应的各向同性模式。这些数据证实了溶液中双核配合物的存在。研究了2-(5-(1,2,4)三唑-1-基甲基- 1h -(1,2,4)-三唑-3-基)吡啶双核铜(II)配合物的儿茶酚氧化酶活性。以3,5-二叔丁基儿茶酚(3,5- dtbk)为模型底物,采用初速度法研究了儿茶酚酶型模型反应的动力学。在低浓度的3,5- dtbk下,初始氧化速率与底物浓度呈线性关系,对应于底物上的一级反应。然而,在较高浓度的3,5- dtbk下,依赖图是非线性的,表明催化剂与底物的饱和。在Michaelis-Menten模型的框架内解释了初始反应速率对底物浓度的依赖形式,该模型很好地描述了天然金属酶的行为。
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Bulletin of Taras Shevchenko National University of Kyiv. Chemistry
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