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Imidazole as an organocatalyst for the rapid synthesis of 1H-pyrazolo[1,2-b]phthalazine-5,10-diones in aqueous medium 咪唑作为有机催化剂在水介质中快速合成1h -吡唑[1,2-b]酞菁-5,10-二酮
IF 1.7 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-12-05 DOI: 10.1007/s12039-024-02327-w
Pavan D Baviskar, Arun D Kale, Vilas N Mahire, Dipak S Dalal, Pramod P Mahulikar

A facile one-pot multicomponent reaction employing aromatic aldehydes, malononitrile, and phthalhydrazide in H2O and EtOH (1:1) mixture at 80ºC has been innovated for the synthesis of 1H-pyrazolo[1,2-b]phthalazine-5,10-diones. This approach stands out for its simplicity, ease of execution, and high efficiency. The reaction employs 20 mol% of imidazole as an organocatalyst, enhancing its practicality and applicability. A total of 14 compounds were synthesized within 0.5 to 4 h under a greener reaction medium, with the yields of products ranging from 85–94%. The key components of this protocol are the use of H2O:EtOH (1:1) mixture as green solvent, recyclable reaction medium, imidazole as an organocatalyst, mild reaction conditions, easy isolation of products, good to excellent yields, and no column chromatographic purification. Using the microbial dilution method, all the synthesized compounds underwent evaluation for their antibacterial activity against a spectrum of strains, including E. coli, S. aureus, P. aeruginosa, B. subtilis, as well as antifungal activity against A. flavus and A. niger. The synthesized derivatives exhibited diverse inhibitory effects on the growth of both bacterial and fungal strains, showcasing their potential utility across various microbial targets.

Graphical abstract

A simple one-pot multicomponent reaction using substituted aromatic aldehydes, malononitrile, and phthalhydrazide in 10 ml of H2O and EtOH (1:1) mixture at 80ºC for the synthesis of 1H-pyrazolo[1,2-b]phthalazine-5,10-dione derivatives has been developed. This methodology involves the use of greener solvents and imidazole as an organocatalyst which leads to good to excellent yields of the products with less reaction time.

以芳香族醛、丙二腈和邻苯二肼为原料,在水和乙二醇(1:1)的混合物中,在80℃条件下,采用一锅多组分反应合成了1h -吡唑[1,2-b]邻苯二嗪-5,10-二酮。这种方法以其简单、易于执行和高效率而突出。该反应采用20%摩尔的咪唑作为有机催化剂,提高了反应的实用性和适用性。在较绿的反应介质条件下,在0.5 ~ 4 h内合成了14个化合物,产物收率在85% ~ 94%之间。该方案的关键组成部分是使用H2O:EtOH(1:1)混合物作为绿色溶剂,可循环使用的反应介质,咪唑作为有机催化剂,反应条件温和,产物易于分离,收率好至优异,无需柱层析纯化。使用微生物稀释法,对所有合成的化合物进行了抗菌活性评价,包括大肠杆菌、金黄色葡萄球菌、铜绿假单胞菌、枯草芽孢杆菌,以及对黄曲霉和黑曲霉的抗菌活性。合成的衍生物对细菌和真菌菌株的生长都有不同的抑制作用,显示了它们在各种微生物靶点上的潜在效用。以取代芳醛、丙二腈和邻苯二肼为原料,在10 ml水和乙二醇(1:1)的混合物中,在80℃下进行了简单的一锅多组分反应,合成了1h -吡唑[1,2-b]邻苯二嗪-5,10-二酮衍生物。该方法包括使用更环保的溶剂和咪唑作为有机催化剂,从而在更短的反应时间内获得良好的产品收率。
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引用次数: 0
Synthesis and characterization of a composite featuring metal–organic frameworks, titania nanoparticles, and graphene oxide: a dual evaluation as a photocatalyst and electrochemical sensing platform 金属有机框架、二氧化钛纳米粒子和氧化石墨烯复合材料的合成和表征:作为光催化剂和电化学传感平台的双重评价
IF 1.7 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-12-05 DOI: 10.1007/s12039-024-02320-3
Varun Bhatnagar, Deepak Kumar, Anjana Pandey, Ashutosh Pandey

This investigation involves synthesizing a new composite, blending graphene oxide (GO), HKUST-1 (copper-based metal–organic frameworks), and titanium dioxide (TiO2) via the hydrothermal method. Following that, the prepared composite is utilized in the design of a photocatalyst and electrochemical sensing platform. Numerous analytical methods, such as XRD, FT-IR, SEM-EDX, TGA, UV-Vis investigations, and suitable electrochemical analyses, were used to examine the morphological and structural characteristics of the crafted material. The tailored composite exhibited remarkable efficiency, showcasing an exceptional degradation efficiency of 97.47% for MB dye within just an hour under sunlight irradiation. On the other hand, the electrochemical sensor developed by fabricating the surface of a glassy carbon electrode (GCE) referred to as GO@HKUST-1@TiO2/GCE exhibited a remarkable catalytic effect on the electrochemical response to imatinib (IMB). The sensor displayed exceptional electrocatalytic performance for detecting IMB under optimized conditions, including solution pH and scan rate. Calibration plots showed linear segments within the concentration range of 2–20 µM, with a significant limit of detection (LOD). The fabricated sensor demonstrated high accuracy, reproducibility, and stability throughout various electrochemical assessments. Thus, the dual functionality of the material has been established.

Graphical abstract

A novel composite comprising graphene oxide (GO), HKUST-1, and titanium dioxide (TiO2) namely GO@HKUST@TiO2 was synthesized and utilized for both photocatalytic degradation of methylene blue (MB) dye and electrochemical sensing of imatinib (IMB). The composite demonstrated exceptional efficiency in both applications, highlighting its potential for dual-functionality.

本研究涉及通过水热法合成氧化石墨烯(GO), HKUST-1(铜基金属有机框架)和二氧化钛(TiO2)的新复合材料。随后,将所制备的复合材料用于光催化剂和电化学传感平台的设计。采用XRD、FT-IR、SEM-EDX、TGA、UV-Vis等多种分析方法,以及合适的电化学分析方法,对制备材料的形态和结构特征进行了研究。该复合材料在太阳光照射下1小时内对MB染料的降解效率达到97.47%。另一方面,通过制造玻璃碳电极(GCE)表面(GO@HKUST-1@TiO2/GCE)开发的电化学传感器对伊马替尼(IMB)的电化学响应表现出显著的催化作用。该传感器在优化的条件下,包括溶液pH和扫描速率,显示出卓越的电催化性能。校正图在2 ~ 20µM浓度范围内呈线性段,检出限(LOD)显著。制造的传感器在各种电化学评估中表现出高精度、可重复性和稳定性。因此,材料的双重功能已经建立。合成了一种由氧化石墨烯(GO)、HKUST-1和二氧化钛(TiO2)组成的新型复合材料GO@HKUST@TiO2,并将其用于亚甲基蓝(MB)染料的光催化降解和伊马替尼(IMB)的电化学传感。这种复合材料在这两种应用中都表现出了卓越的效率,突出了其双重功能的潜力。
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引用次数: 0
Mesomorphic cyanobiphenyl appended thiols as anti-corrosive materials: Electrochemical and theoretical investigations 介形氰联苯附加硫醇作为防腐材料:电化学和理论研究
IF 1.7 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-12-05 DOI: 10.1007/s12039-024-02329-8
S Kshama Shetty, K Swamynathan, Jyoti Roy Choudhuri, K Shwetha, Sadhana H Upadhya, Sandeep Kumar

Cyanobiphenyls are well-known for their liquid crystalline organization. The molecules that can undergo self-assembly on the surface of metal, offer potent corrosion inhibition properties. Herein we report five such cyanobiphenyl derivatives as potential anti-corrosion films on the surface of mild steel immersed in 1M HCl medium. The electrochemical impedance measurements and potentiodynamic polarization measurements reveal that the cyanobiphenyl derivative with shortest chain length out of the five inhibitors under consideration (i.e., 4′-((6-mercaptohexyl)oxy)-[1,1′-biphenyl]-4-carbonitrile) exhibited up to 98% efficiency for the drop cast volume of 25 µL of 1 mg/mL of stock solution as compared to increased chain length molecules. The surface characterization of the corroded and protected mild steel surface was done by using a scanning electron microscope and energy-dispersive X-ray spectroscopic methods which affirms the presence of protective film on the surface of mild steel after exposure to acid medium. The theoretical calculations support experimental observations with respect to trends in the efficiency of short-chain and long-chain functionalized cyanobiphenyls.

Graphical Abstract

Five different chain-length cyanobiphenyls appended thiols as anti-corrosive materials on the surface of mild steel in an acidic medium were investigated by electrochemical, theoretical and surface characterization methods. The efficacy of the molecule was as high as 98–99% at a very small drop cast volume of 25 µL.

氰联苯以其液晶组织而闻名。这些分子可以在金属表面进行自组装,具有有效的缓蚀性能。本文报道了五种氰基苯衍生物在浸入1M HCl介质的低碳钢表面作为潜在的防腐膜。电化学阻抗测量和动电位极化测量表明,在考虑的五种抑制剂中,链长最短的氰联苯衍生物(即4 ' -((6-巯基己基)氧)-[1,1 ' -联苯]-4-碳腈)在滴投体积为25 μ L的1 mg/mL原液中,与链长增加的分子相比,效率高达98%。利用扫描电子显微镜和能量色散x射线光谱法对腐蚀防护后的低碳钢表面进行了表征,证实了酸介质作用后的低碳钢表面存在保护膜。理论计算支持关于短链和长链功能化氰联苯效率趋势的实验观察。摘要采用电化学、理论和表面表征等方法,研究了5种不同链长氰联苯在酸性介质中钢表面附加硫醇的防腐材料。在很小的滴注体积为25µL的情况下,该分子的功效高达98-99%。
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引用次数: 0
Role of alkyl chain linker in the conformational preferences of N′-phenylalkylsquaramates and bis-N,N′-diphenylalkylsquaramides 烷基链连接剂在N′-苯烷基角酰胺和双-N,N′-二苯烷基角酰胺构象偏好中的作用
IF 1.7 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-12-04 DOI: 10.1007/s12039-024-02331-0
Aman Pandey, G Naresh Patwari

Conformational space of small molecules can be exploited to deploy the hierarchical nature of intermolecular interactions, such as hydrogen bonding and π-stacking in the crystal structures. Modulation of conformational space was achieved by varying the alkyl chain length in N′-phenylalkylsquaramates and bis-N,N′-diphenylalkylsquaramides, which were synthesized by condensation of dimethyl squarate with the corresponding phenyl alkylamines. In the crystal structures of these compounds, even though the catemeric N–H···O hydrogen bonding is the primary interaction and hierarchy in the secondary interactions consisting of π-stacking and H···H bonding leads to a large variation in molecular structures in the solid state.

Graphical abstract

Conformational variation in the alkyl chain linker connected to central squaramide unit is contingent to the variation in partner chain length.

小分子的构象空间可以用来揭示分子间相互作用的层次性,如晶体结构中的氢键和π堆积。通过改变N′-苯基烷基角酰胺和双N,N′-二苯基烷基角酰胺的烷基链长来调节构象空间。在这些化合物的晶体结构中,虽然N-H··O氢键是主要的相互作用,但在由π堆叠和H··H键组成的二级相互作用中,层次结构导致了固态分子结构的很大变化。图:与中心方酰胺单元相连的烷基链连接体的构象变化取决于伙伴链长度的变化。
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引用次数: 0
Pyrene-tethered self-assembled supramolecular system demonstrating vesicular structures and aggregation-induced emission: synthesis, assembled studies and morphology 展示囊泡结构和聚集诱导发射的芘系结自组装超分子体系:合成、组装研究和形态
IF 1.7 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-12-04 DOI: 10.1007/s12039-024-02316-z
Rajinder Kaur, Ramesh Kataria, Surbhi Sharma

The emergence of aggregation-induced emission luminogens (AIEgens) has significantly stimulated the development of luminescent supramolecular materials because of their strong emissions in the aggregated state. With this inspiration, pyrene tethered Schiff base molecule, namely (Z)-1-(2,4-dinitrophenyl)-2-(pyren-1-ylmethylene), hydrazine was designed and successfully synthesized and well characterized by using proton (1H NMR), Fourier–transform infrared (FT-IR), and electron ionization mass spectrometry (EI-MS). UV-visible absorption and emission studies have been employed to elucidate self-assembled and aggregation properties. It is shown that monomers of synthesized compounds can exhibit emission driven by assembly by forming an H-aggregate, which corresponds to its blue shift tuning to the visible region associated with the extended π-conjugation. Furthermore, to have a more profound understanding of the supramolecular assembly, TEM and confocal microscopy were utilized to verify the aggregate morphology. In both investigations, monomer aggregation into a vesicular structure with monodispersed PDI is preferred.

Graphical abstract

Pyrene tethered Schiff base molecule, namely (Z)-1-(2,4-dinitrophenyl)-2-(pyren-1-ylmethylene), hydrazine was designed and successfully synthesized. Monomer 1 demonstrating aggregation-induced emission upon increasing the gradual amount of H2O in DMF solution of compound 1 (DMF/H2O, 30/70 (v/v). Pictorial representation is also pasted along with TEM and confocal results of aggregate or supramolecular structures of synthesised compound.

聚集致发射发光物质(AIEgens)的出现极大地促进了发光超分子材料的发展,因为它们在聚集状态下具有很强的发光能力。在此启发下,设计并成功合成了芘系席夫碱分子(Z)-1-(2,4-二硝基苯基)-2-(芘-1-基亚甲基)肼,并利用质子(1H NMR)、傅里叶变换红外(FT-IR)和电子电离质谱(EI-MS)对其进行了表征。紫外可见吸收和发射研究已被用来阐明自组装和聚集性质。结果表明,合成化合物的单体可以通过形成h聚集体而表现出由组装驱动的发光,这对应于其蓝移调谐到与扩展π共轭相关的可见区。此外,为了更深入地了解超分子组装,我们利用TEM和共聚焦显微镜对聚集体形态进行了验证。在这两项研究中,单体聚集成具有单分散PDI的囊泡结构是首选。摘要设计并成功合成了芘系链希夫碱分子(Z)-1-(2,4-二硝基苯)-2-(芘-1-基亚甲基)联氨。单体1在化合物1的DMF溶液中逐渐增加H2O (DMF/H2O, 30/70 (v/v)),表现出聚集诱导发射。图像表示也粘贴与TEM和共聚焦结果的合成化合物的聚集体或超分子结构。
{"title":"Pyrene-tethered self-assembled supramolecular system demonstrating vesicular structures and aggregation-induced emission: synthesis, assembled studies and morphology","authors":"Rajinder Kaur,&nbsp;Ramesh Kataria,&nbsp;Surbhi Sharma","doi":"10.1007/s12039-024-02316-z","DOIUrl":"10.1007/s12039-024-02316-z","url":null,"abstract":"<div><p>The emergence of aggregation-induced emission luminogens (AIEgens) has significantly stimulated the development of luminescent supramolecular materials because of their strong emissions in the aggregated state. With this inspiration, pyrene tethered Schiff base molecule, namely (Z)-1-(2,4-dinitrophenyl)-2-(pyren-1-ylmethylene), hydrazine was designed and successfully synthesized and well characterized by using proton (<sup>1</sup>H NMR), Fourier–transform infrared (FT-IR), and electron ionization mass spectrometry (EI-MS). UV-visible absorption and emission studies have been employed to elucidate self-assembled and aggregation properties. It is shown that monomers of synthesized compounds can exhibit emission driven by assembly by forming an H-aggregate, which corresponds to its blue shift tuning to the visible region associated with the extended <i>π</i>-conjugation. Furthermore, to have a more profound understanding of the supramolecular assembly, TEM and confocal microscopy were utilized to verify the aggregate morphology. In both investigations, monomer aggregation into a vesicular structure with monodispersed PDI is preferred.</p><h3>Graphical abstract</h3><p>Pyrene tethered Schiff base molecule, namely (Z)-1-(2,4-dinitrophenyl)-2-(pyren-1-ylmethylene), hydrazine was designed and successfully synthesized. Monomer <b>1</b> demonstrating aggregation-induced emission upon increasing the gradual amount of H<sub>2</sub>O in DMF solution of compound 1 (DMF/H<sub>2</sub>O, 30/70 (v/v). Pictorial representation is also pasted along with TEM and confocal results of aggregate or supramolecular structures of synthesised compound.</p><div><figure><div><div><picture><source><img></source></picture></div></div></figure></div></div>","PeriodicalId":616,"journal":{"name":"Journal of Chemical Sciences","volume":"136 4","pages":""},"PeriodicalIF":1.7,"publicationDate":"2024-12-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142761701","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A new synthesis of 7H-pyrrolo[3,2-f]quinoxaline derivatives by a one-pot, three-component reaction 用一锅三组分反应合成7h -吡咯[3,2-f]喹啉衍生物
IF 1.7 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-12-04 DOI: 10.1007/s12039-024-02332-z
Xue Wang, Ji Li, Jia-Yan Liu, Dong-Sheng Chen

An acid-catalyzed three-component reaction of arylglyoxals, quinoxalin-6-amine and 4-hydroxycoumarin is described, leading to the synthesis of new functionalized 7H-pyrrolo[3,2-f]quinoxaline derivatives with good yields. It has high synthetic efficiency and operational simplicity, and only water was generated as a byproduct.

Graphical abstract

A new procedure for the synthesis of pyrrolo[3,2-f]quinoxaline derivatives.

本文报道了芳基乙二醛、喹啉-6-胺和4-羟基香豆素的酸催化三组分反应,合成了新的功能化7h -吡咯[3,2-f]喹啉衍生物,收率高。该工艺合成效率高,操作简单,只产生水作为副产物。图示摘要:合成吡咯[3,2-f]喹诺啉衍生物的新方法。
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引用次数: 0
Formation of dicyano ruthenium(II) complex mediated by triethylamine via deprotonation of hydrazonochroman-2,4-dione 在三乙胺介导下通过肼基二氢苯并二氢吡喃-2,4-二酮的去质子化作用形成二氰基钌(II)络合物
IF 1.7 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-29 DOI: 10.1007/s12039-024-02307-0
Reena Ravindran, Minitha R, Shiji Fazil, A. Sarau Devi

New ruthenium(II) complex containing cyanide anions has been isolated from the hydrazonochromandione ligand 3-(2-(4-chlorophenyl)hydrazono)chroman-2,4-dione in the presence of acetonitrile along with triethylamine from Ru(III) salt. This method is a one-pot synthetic approach for preparing dicyano Ru(II) complex. Using physicochemical and spectral techniques, the synthesized compound [Ru(CN)2L2]·2Et3N+H was structurally described. The monoanionic bidentate character of the hydrazone ligand and coordination through carbonyl oxygen and deprotonated hydrazonochroman-2,4-dione nitrogen atom were revealed by single crystal X-ray diffraction investigation of the Ru(II) complex. Ru(II) complex is a member of the P21/n space group and monoclinic system. Ru(II) chelate rings were stabilized by intermolecular hydrogen bonds and ππ stacking interactions between ligands and triethylammonium molecules. A single phase with rod-like morphologies is imaged by SEM. The quasi-reversible single electron transfer property is exhibited by the Ru(II) complex.

在乙腈和三乙胺的作用下,从氢氮铬二酮配体 3-(2-(4-氯苯基)氢氮)铬-2,4-二酮中分离出了新的含氰阴离子的钌(II)络合物。这种方法是一种制备二氰基 Ru(II) 复合物的单锅合成方法。利用物理化学和光谱技术,对合成的化合物 [Ru(CN)2L2]-2Et3N+H 进行了结构描述。通过对 Ru(II) 复合物的单晶 X 射线衍射研究,发现了腙配体的单阴离子双齿特性以及通过羰基氧和去质子化腙-2,4-二酮氮原子的配位。Ru(II) 复合物属于 P21/n 空间群和单斜晶系。配体和三乙基铵分子之间的分子间氢键和 π-π 堆积相互作用稳定了 Ru(II) 螯合环。扫描电子显微镜(SEM)对具有棒状形态的单相进行了成像。Ru(II) 复合物表现出准可逆的单电子转移特性。
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引用次数: 0
AgNO3-anchored Prussian blue-derived porous Ag/α-Fe2O3 heterostructure with enhanced electrochemical sensing performance towards methylparaben 锚定 AgNO3 的普鲁士蓝衍生多孔 Ag/α-Fe2O3 异质结构可提高对苯甲酸甲酯的电化学传感性能
IF 1.7 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-29 DOI: 10.1007/s12039-024-02323-0
Ho Van Minh Hai, Van Cuong Nguyen, The Ky Vo

Herein, we report on facile fabricating sensors based on Ag/α-Fe2O3 nanocubes harvesting by one-step pyrolyzing Prussian blue (PSB) template anchored AgNO3 at different temperatures (300~500°C) and exploiting them for electrochemical sensing of methylparaben (MP). The Ag/Fe2O3 nanocubes had crystallite sizes ranging from 300~400 nm and incorporated reduced Ag nanoparticles (AgNPs) ranging from 10.5~15.3 nm. Notably, the harvested Ag/Fe2O3 composites were constructed hetero-interfacial Ag–Fe2O3 structures inside the porous α-Fe2O3 cubes with interconnected pore matrix resulting from the thermal conversion of PSB. The carbon glass electrode (GCE) coated with an Ag/Fe2O3 sensor prepared at 400°C showed the highest oxidation peak at 0.84 V towards MP. In addition, the Ag/α-Fe2O3@GCE interface achieved an excellent detection of MP with a low LOD of 0.14 µM and a linear response range of 10~38 µM. The sensor also depicted good selectivity and stability during 10 days, demonstrating a suitable sensor for detecting and analyzing MP. This study provides a facile strategy for constructing a porous Ag/Fe2O3 heterostructural composite as an efficient electrochemical sensing material.

Graphical abstract

Sensors based on Ag/α-Fe2O3 nanocube harvesting by one-step pyrolyzing Prussian blue (PSB) template anchored AgNO3 and exploited for the electrochemical sensing of methylparaben. The results suggest that Ag/α-Fe2O3 nanocube crystals comprise heterointerfaces and interconnected pores. The Ag/α-Fe2O3@GCE interface exhibited excellent detection of methylparaben, good stability, and selectivity.

在此,我们报告了在不同温度(300~500°C)下一步热解普鲁士蓝(PSB)模板锚定的 AgNO3,从而方便地制造出基于 Ag/α-Fe2O3 纳米立方体的传感器,并将其用于对羟基苯甲酸甲酯(MP)的电化学传感。Ag/Fe2O3 纳米立方体的结晶尺寸为 300~400 nm,并含有 10.5~15.3 nm 的还原型 Ag 纳米颗粒(AgNPs)。值得注意的是,收获的 Ag/Fe2O3 复合材料是在多孔 α-Fe2O3 立方体内部构建的异质界面 Ag-Fe2O3 结构,其孔隙矩阵是由 PSB 热转换产生的。在 400°C 下制备的涂有 Ag/Fe2O3 传感器的碳玻璃电极 (GCE) 对 MP 的氧化峰值最高,为 0.84 V。此外,Ag/α-Fe2O3@GCE 界面实现了对 MP 的出色检测,LOD 低至 0.14 µM,线性响应范围为 10~38 µM。该传感器还具有良好的选择性和 10 天的稳定性,证明是一种适用于检测和分析 MP 的传感器。该研究为构建多孔 Ag/Fe2O3 异质结构复合材料作为高效电化学传感材料提供了一种简便的策略。图解摘要通过一步热解普鲁士蓝(PSB)模板锚定 AgNO3,获得基于 Ag/α-Fe2O3 纳米立方体的传感器,并将其用于苯甲酸甲酯的电化学传感。结果表明,Ag/α-Fe2O3 纳米立方体晶体由异质界面和相互连接的孔隙组成。Ag/α-Fe2O3@GCE 界面对苯甲酸甲酯具有良好的检测性能、稳定性和选择性。
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引用次数: 0
LED-based broadband cavity-enhanced spectrometer for high-sensitive optical detection of diacetyl in gas phase 基于 LED 的宽带空腔增强光谱仪,用于气相双乙酰的高灵敏度光学检测
IF 1.7 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-29 DOI: 10.1007/s12039-024-02324-z
Ardhendu Pal, Koushik Mondal, Soumen Mandal, Soumyadipta Chakraborty, Indrayani Patra, Manik Pradhan

Diacetyl (C4H6O2) is an important organic diketone that is widely used as flavoring agent and food additive. It is toxic when inhaled or exposed to high concentrations and may lead to chronic respiratory disease and neurodegenerative disorders. But, a viable optical detection method for rapid and quantitative estimation of diacetyl molecules in gas phase does not currently exist. Here, we report the design and development of a simple, compact and cost-effective robust optical technique exploiting incoherent broadband cavity-enhanced absorption spectroscopy (IBBCEAS) technique for high-sensitive selective detection and quantitative estimation of gas-phase diacetyl levels in real-time using a visible light emitting diode (LED) operating at 450 nm. The IBBCEAS method demonstrates an effective optical-path length of 4.5 km within an optical cavity (Finesse ~15706) composed of two high-reflective mirrors. A typical detection limit of ~190 parts-per-billion (ppb) for diacetyl was achieved with an optimum acquisition time of ~4 s at an optimal cavity pressure of 100 Torr. LED-based diacetyl sensor system was optimized, calibrated and demonstrated for trace detection of gaseous diacetyl at the ppb levels in various food products and liquor samples as a few representative applications, thus paving the way for development of future optical monitors.

Graphical abstract

This work represents the development of a LED-based optical setup for the detection of diacetyl molecule in gas phase.

二乙酰(C4H6O2)是一种重要的有机二酮,被广泛用作调味剂和食品添加剂。吸入或暴露于高浓度时会中毒,可能导致慢性呼吸道疾病和神经退行性疾病。但是,目前还没有一种可行的光学检测方法来快速、定量地估计气相中的双乙酰分子。在此,我们报告了利用非相干宽带空腔增强吸收光谱(IBBCEAS)技术设计和开发的一种简单、紧凑、高性价比的稳健光学技术,该技术利用工作波长为 450 纳米的可见光发光二极管(LED)对气相中的双乙酰水平进行高灵敏度的选择性检测和实时定量估算。IBBCEAS 方法在由两个高反射镜组成的光腔(Finesse ~15706)内的有效光路长度为 4.5 千米。在最佳腔压为 100 托时,最佳采集时间为 4 秒,双乙酰的典型检测限为十亿分之 190 (ppb)。对基于 LED 的双乙酰传感器系统进行了优化、校准和演示,可用于痕量检测各种食品和酒类样品中ppb级的气态双乙酰,从而为开发未来的光学监测器铺平了道路。 图文摘要 这项工作展示了基于 LED 的光学装置的开发,用于检测气相中的双乙酰分子。
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引用次数: 0
Synthesis and characterization of a new coordination polymer of copper (II): Catalytic application for reductive degradation of dyes under dark 一种新的铜(II)配位聚合物的合成与表征:黑暗条件下染料还原降解的催化应用
IF 1.7 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY Pub Date : 2024-11-26 DOI: 10.1007/s12039-024-02313-2
Aieshri Swargiary, Tanmoy Kumar Ghosh, Arunendu Mondal

A new copper (II) coordination polymer [{Cu(TMDP)(2,3-pydc)}.2H2O]n (A) has been synthesized successfully by solvolysis method using ligands 4,4′-trimethylenedipyridine (TMDP) and 2,3-pyridinedicarboxylic acid (2,3-pydc). The structure of the synthesised coordination polymer is confirmed by the single crystal X-ray diffraction study and also supported by CHN analysis. FTIR, UV-visible spectroscopy, thermogravimetric analysis (TGA) and powder XRD study are used to characterize A. The polymer in aqueous solution is applied as effective catalyst for reductive degradation of methyl orange (MO) and Congo red (CR) dyes with reducing agent sodium borohydride (NaBH4) under dark. The detail study of the catalytic reaction and its kinetic study reveals 97% and 76% degradation of MO and CR with rate constants of 0.061 min−1 and 0.005 min−1, respectively. This is the first example where a coordination polymer has been used for reductive degradation of dyes under dark condition.

Graphical abstract

A newly synthesized copper (II) coordination polymer [{Cu(TMDP)(2,3-pydc)}.2H2O]n (A) has been developed and studied by different analytical methods. The polymer (A) is then used as catalyst for degradation of anionic (MO and CR) dyes.

利用配体 4,4′-三亚甲基二吡啶(TMDP)和 2,3-吡啶二羧酸(2,3-ydc),通过溶解法成功合成了一种新的铜(II)配位聚合物 [{Cu(TMDP)(2,3-pydc)}.2H2O]n(A)。单晶 X 射线衍射研究证实了合成配位聚合物的结构,CHN 分析也证明了这一点。傅立叶变换红外光谱、紫外-可见光谱、热重分析 (TGA) 和粉末 XRD 研究用于表征 A。对催化反应及其动力学的详细研究表明,MO 和 CR 的降解率分别为 97% 和 76%,速率常数分别为 0.061 min-1 和 0.005 min-1。这是配位聚合物在黑暗条件下用于还原降解染料的第一个实例。图解摘要 一种新合成的铜(II)配位聚合物[{Cu(TMDP)(2,3-pydc)}.2H2O]n (A) 已被开发出来,并通过不同的分析方法进行了研究。聚合物 (A) 随后被用作降解阴离子(MO 和 CR)染料的催化剂。
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Journal of Chemical Sciences
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