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Voltammetric performance of nanofiber structured over-oxidized poly(3,4-ethylenedioxythiophene) modified pencil graphite electrodes for dobutamine sensing 纳米纤维结构过氧化聚(3,4-亚乙二氧基噻吩)修饰铅笔形石墨电极的伏安性能,用于多巴酚胺传感
Pub Date : 2023-09-27 DOI: 10.18596/jotcsa.1306564
Ayşegül Özbek, L. Özcan
A modified electrode was developed for the electrochemical sensing of dobutamine (DBT), one of the catecholamines. For this modification process, pencil graphite electrodes (PGE) were modified with over-oxidized nanofiber structured poly (3,4-ethylenedioxythiophene) (PGE/OPEDOTNF) by electropolymerization. The electrochemical performance of PGE/OPEDOTNF was evaluated by cyclic and differential pulse voltammetry. In addition, the performances of non-nanofiber PEDOT-modified PGE electrodes were also examined for comparison. The characterization of the modified electrodes was carried out by scanning electron microscopy and electrochemical methods. The signal of the modified electrodes was observed in a linear range of 0.1-2.0 µM against DBT using the differential pulse voltammetry method. The limit of detection and quantification are calculated as 0.026 µM and 0.086 µM, respectively. The effect of the interfering species was examined. It has been shown that DBT can be detected sensitively and selectively using pencil graphite electrodes modified with nanofiber-structured poly(3,4-ethylenedioxythiophene). The repeatability of PGE/OPEDOTNF electrodes was found to be 5.2%. PGE/OPEDOTNF electrodes remained stable for 15 days without losing their electrochemical activity.
为对儿茶酚胺之一多巴酚丁胺(DBT)进行电化学传感,开发了一种改性电极。在此改性过程中,铅笔石墨电极(PGE)与过氧化纳米纤维结构聚(3,4-乙撑二氧噻吩)(PGE/OPEDOTNF)通过电聚合进行了改性。通过循环伏安法和差分脉冲伏安法评估了 PGE/OPEDOTNF 的电化学性能。此外,还对非纳米纤维 PEDOT 改性 PGE 电极的性能进行了比较研究。改性电极的表征是通过扫描电子显微镜和电化学方法进行的。使用微分脉冲伏安法观察到改性电极的信号与 DBT 的线性范围为 0.1-2.0 µM。计算得出的检测限和定量限分别为 0.026 µM 和 0.086 µM。研究了干扰物的影响。结果表明,使用纳米纤维结构聚(3,4-亚乙二氧基噻吩)修饰的铅笔石墨电极可以灵敏地、选择性地检测 DBT。PGE/OPEDOTNF 电极的重复性为 5.2%。PGE/OPEDOTNF 电极在 15 天内保持稳定,不会丧失其电化学活性。
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引用次数: 0
DFT and Electrochemical Study of Novel Green Corrosion Inhibitor (Pyrantrin) for 1100-H14 Aluminum Corrosion Remediation in 1 M H2SO4 Acidic Environment 新型绿色缓蚀剂(嘧啶)在 1 M H2SO4 酸性环境中修复 1100-H14 铝腐蚀的 DFT 和电化学研究
Pub Date : 2023-08-31 DOI: 10.18596/jotcsa.1234194
B. Ugi
The study on Corrosion Inhibition of 1100-H14 Aluminum in H2SO4 Acidic Deploying pyrantrin as a Green Inhibitor was investigated by adopting different experimental methods, including weight loss, electrochemical impedance spectroscopic, potentiodynamic polarization, and computational methods. It was observed that pyrantrin was a good inhibitor for the 1100–H14–type aluminum. Inhibition efficiency was recorded between 42.5 % and 95.2 % for aluminum at 500 ppm and 1500 ppm concentrations. This high inhibition efficiency was attributed to the strong adsorption of the molecules on both metal surfaces. Electrochemical impedance showed higher and increasing charge transfer resistance values and decreasing values for the double-layer capacitance, indicating better inhibition. From quantum calculations, the EHOMO value was higher than that of the ELUMO, while the energy gap was calculated to be 1.9 with a binding energy of 132.9, indicating stronger adsorption and inhibition.
采用不同的实验方法,包括失重法、电化学阻抗光谱法、电位极化法和计算法,研究了吡咯烷酮作为绿色缓蚀剂在 H2SO4 酸性溶液中对 1100-H14 型铝的缓蚀作用。结果表明,吡咯烷酮对 1100-H14 型铝具有良好的抑制作用。在浓度为 500 ppm 和 1500 ppm 时,对铝的抑制效率分别为 42.5% 和 95.2%。这种高抑制效率归因于分子在两种金属表面的强吸附性。电化学阻抗显示电荷转移电阻值越来越高,而双层电容值则越来越低,这表明抑制效果更好。通过量子计算,EHOMO 值高于 ELUMO 值,能隙为 1.9,结合能为 132.9,表明吸附和抑制作用更强。
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引用次数: 0
Carbon Paste Electrode Modified by Dibenzo 18-crown-6 for the Determination of Pb in Carrot Using Differential Pulse Voltammetry 二苯并18-冠-6修饰碳糊电极差分脉冲伏安法测定胡萝卜中的铅
Pub Date : 2023-08-17 DOI: 10.18596/jotcsa.1120078
Irdhawati Irdhawati, Ayu Jyostosya Yotirani Arya Wijana, Emmy Sahara, Manuntun Manurung
In this research, the modification of carbon paste electrode (CPE) using dibenzo 18-crown-6 was carried out to detect Pb level in carrot. The purpose of this electrode modification is to increase the sensitivity of the measurement. The optimized parameters were scan rate, composition of dibenzo 18-crown-6 in carbon paste, and supporting electrolyte. Measurements were validated by determining the linear concentration range, detection limit (LoD), quantification limit (LoQ), repeatability, selectivity, and recovery. At the best measurement conditions, the modified CPE (CPE-Dbc) was applied to determine Pb in carrot. The optimum measurements conditions were obtained the optimum concentration of crown ether in carbon paste was 0.8%, the scan rate using CPE at 15 mV/s, increased to 20 mV/s, and H2SO4 solution as supporting electrolyte. The linear concentration was found in the range of 5-100 µg/L using CPE and became wider to 5-2000 µg/L using CPE-Dbc. The values of LoD and LoQ measurement using CPE were 0,3575 µg/L and 0,3583 µg/L, and decreased to 0,1265 µg/L and 0,1266 µg/L using CPE-Dbc. CPE and CPE-Dbc had good precision with Horwitz ratio values were 0,2231 and 0,2183, which is smaller than two. The percentage of recovery of Pb in the mixture of standard and sample solutions was (88,97 ± 2,76)%. The presence of Cu, Cd and Na in the solution did not interfere the measurement of Pb. The concentration of Pb in carrot sample was (1,8423 ± 0,0002) mg/kg, which was higher than the acceptable concentration according to SNI No. 7387:2009, which is 0,5 mg/kg.
本研究利用二苯并18-冠-6对碳糊电极(CPE)进行修饰,测定胡萝卜中铅的含量。这种电极修饰的目的是为了提高测量的灵敏度。优化参数为扫描速率、碳糊中二苯并18-冠-6的组成、支撑电解质。通过确定线性浓度范围、检出限(LoD)、定量限(LoQ)、重复性、选择性和回收率来验证测量结果。在最佳测定条件下,应用改性CPE (CPE- dbc)测定胡萝卜中的铅。得到了碳糊中冠醚的最佳浓度为0.8%,CPE扫描速率从15 mV/s提高到20 mV/s,以H2SO4溶液为支撑电解质的最佳测量条件。CPE的线性浓度范围为5-100µg/L, CPE- dbc的线性浓度范围为5-2000µg/L。CPE测得的LoD和LoQ分别为0.3575µg/L和0.3583µg/L, CPE- dbc测得的LoD和LoQ分别为0.1265µg/L和0.1266µg/L。CPE和CPE- dbc具有较好的精度,Horwitz比值分别为0.2231和0.2183,均小于2。标准溶液和样品溶液的铅回收率为(88,97±2,76)%。溶液中Cu、Cd和Na的存在对Pb的测量没有干扰。胡萝卜样品中Pb的浓度为(18423±0.0002)mg/kg,高于SNI No. 7387:2009规定的0.5 mg/kg的可接受浓度。
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引用次数: 0
Synthesis, Antiproliferative Activity and In Silico Studies of Chalcones Derived From 4-(Imidazole-1-yl)Acetophenone 4-(咪唑-1-基)苯乙酮衍生查尔酮的合成、抗增殖活性及硅研究
Pub Date : 2023-08-05 DOI: 10.18596/jotcsa.1313595
Bedriye Seda KURŞUN AKTAR, Abdulraheem Mustafa Alkarabash, A. ŞAHİN YAĞLIOĞLU, E. E. Oruç-Emre
In this study, the synthesis of chalcone compounds (1-11) derived from 4-(imidazol-1-yl)acetophenone and the structure determination of these compounds by various spectroscopic methods were carried out. The anticancer activities of compounds 1-11 were examined against HeLa and PC-3 cancer cells at four different concentrations (100, 50, 25, and 5 µM) using the BrdU ELISA assay. It was determined that all molecules except compounds 1 and 6 in HeLa cancer cells and compounds 2 and 8 against PC-3 cancer cells were more active against HeLa and PC-3 than the standard drug 5-fluorouracil (5-FU). The best activity against PC-3 cancer cells was compound 4 (IC50: 1.39±0.00 µM). In addition, compound 11 (IC50: 1.58±0.01 µM) was found to have the highest activity against HeLa cancer cells. Compound 4 against PC-3 cancer cell and compound 11 against HeLa cancer cell displayed cell selective activity. The ADME properties and drug similarities of the molecules 1-11 using the SwissADME software were investigated. According to these properties, compounds 1-11 were found to obey Lipinski rules.
本研究合成了由4-(咪唑-1-基)苯乙酮衍生的查尔酮类化合物(1-11),并利用各种光谱方法对其结构进行了测定。采用BrdU ELISA法检测化合物1-11在不同浓度(100、50、25和5µM)下对HeLa和PC-3癌细胞的抗癌活性。结果表明,除HeLa癌细胞中的化合物1、6和PC-3癌细胞中的化合物2、8外,其他分子对HeLa和PC-3的活性均高于标准药物5-氟尿嘧啶(5-FU)。化合物4对PC-3癌细胞的抑制活性最高(IC50: 1.39±0.00µM)。化合物11 (IC50: 1.58±0.01µM)的抗HeLa癌细胞活性最高。化合物4对PC-3癌细胞和化合物11对HeLa癌细胞表现出细胞选择性活性。利用SwissADME软件对分子1-11的ADME性质和药物相似性进行了研究。根据这些性质,化合物1-11符合利平斯基规则。
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引用次数: 0
3- and 4-Arm Star Polymers (PEG3 and PEG4) via Metal-Free Azide-Alkyne Click Reaction 3臂和4臂星形聚合物(pegg3和PEG4)的无金属叠氮-炔点击反应
Pub Date : 2023-08-01 DOI: 10.18596/jotcsa.1324025
U. Günay
Star polymers are known for their different structural and functional properties. Depending on their structure, they may display a wide range of characteristics. Star polymers can be synthesized using either a core-first or arm-first strategy. Numerous synthetic approaches can be used in both cases. In this work, 3- and 4-arm star polymers were prepared via the metal-free azide-alkyne click reaction. Trifunctional and tetrafunctional propiolate (acetylenecarboxylate) ester-containing cores were prepared and then subjected to a metal-free azide-alkyne reaction with azide end-functionalized PEG (PEG-N3) to yield A3 and A4-type star polymers, respectively. All the structures were characterized using 1H and 13C NMR spectroscopy and GPC.
星形聚合物以其不同的结构和功能特性而闻名。根据它们的结构不同,它们可能表现出各种各样的特征。星形聚合物的合成可以采用核优先或臂优先的策略。在这两种情况下都可以使用许多综合方法。本文通过无金属叠氮-炔咔嗒反应制备了3臂和4臂星形聚合物。制备了含三官能团和四官能团的丙酸(乙乙甲酸酯)酯核,并与叠氮化物端功能化的聚乙二醇(PEG- n3)进行无金属叠氮化物-炔反应,分别得到A3型和a4型星型聚合物。所有结构均通过1H、13C NMR和GPC进行了表征。
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引用次数: 0
Synthesis and Photodegradation of Bi2O3 and Pb-Bi2O3 Nanoparticles and Their Kinetic Study Bi2O3 和 Pb-Bi2O3 纳米粒子的合成、光降解及其动力学研究
Pub Date : 2023-07-25 DOI: 10.18596/jotcsa.1164065
Farzana Hai̇der, Zakia Gul, Kafeel AHMAD KHAN
The green synthesis method synthesized the bismuth oxide and lead-doped bismuth oxide nanoparticles using Ferula Asafoetida leaves extract. The lead-doped bismuth oxide showed greater degradation efficiency than undoped bismuth oxide. This greater efficiency was due to decreases in the band gap energy between the valence band and the conduction band of the metal oxide and reduced the chances of electron-hole pair recombination with the metal oxide catalyst. The synthesized nanoparticles were characterized by TGA, SEM, FT-IR, EDX, XRD, and UV- visible Spectrometer. XRD diffraction of Bi2O3 nanoparticles reflected a strong and sharp peak at 32.8˚ shows that Bi2O3 nanoparticles are in crystalline phase. The crystallite size of Bi2O3 nanoparticles is 13.433 nm, and Pb-doped Bi2O3 is 9.6 nm, calculated from the Debye-Scherrer equation. The synthesized Bi2O3 nanoparticles are round in shape with average size of ~ 90-100 nm While Pb doped Bi2O3 is ~ 75 f- 100 nm. The EDX spectra showed no additional peak for any impurities. The degradation rate of Malachite Green dye (MG) increased with the increase in contact time and temperature, while it decreased with increasing dye initial concentration and pH. Initially, the degradation efficiency of the bismuth oxide catalyst is increased with increasing catalyst amount, but after a certain amount of catalyst, it started decreasing as the catalyst amount was further increased. The irradiation time on photodegradation is deliberate, keeping other parameters steady at catalyst quantity 0.01 g at specific reaction conditions. Moreover, the dye showed an increase in degradation at 50 oC. The utmost degradation of 92% was observed for lead-doped bismuth oxide (Bi2O3) and 76% for undoped bismuth oxide (Bi2O3).
该绿色合成方法利用阿魏叶提取物合成了氧化铋和掺杂铅的氧化铋纳米粒子。与未掺杂的氧化铋相比,掺铅的氧化铋具有更高的降解效率。这种更高的降解效率是由于金属氧化物价带和导带之间的带隙能减小,减少了电子-空穴对与金属氧化物催化剂重组的机会。TGA、SEM、傅立叶变换红外光谱、EDX、XRD 和紫外可见光谱仪对合成的纳米粒子进行了表征。Bi2O3 纳米粒子的 XRD 衍射在 32.8˚ 折射出一个强烈而尖锐的峰,表明 Bi2O3 纳米粒子处于结晶相。根据 Debye-Scherrer 方程计算,Bi2O3 纳米粒子的晶粒尺寸为 13.433 nm,掺杂 Pb 的 Bi2O3 纳米粒子的晶粒尺寸为 9.6 nm。合成的 Bi2O3 纳米粒子呈圆形,平均尺寸约为 90-100 nm,而掺杂铅的 Bi2O3 则约为 75 f-100 nm。EDX 光谱显示没有任何杂质的附加峰。孔雀石绿染料(MG)的降解率随着接触时间和温度的增加而增加,但随着染料初始浓度和 pH 值的增加而降低。最初,氧化铋催化剂的降解效率随着催化剂用量的增加而提高,但在催化剂用量达到一定程度后,随着催化剂用量的进一步增加,降解效率开始下降。在特定反应条件下,催化剂用量为 0.01 克时,其他参数保持稳定,辐照时间对光降解的影响是经过深思熟虑的。此外,染料在 50 oC 时的降解率有所上升。掺杂铅的氧化铋(Bi2O3)和未掺杂的氧化铋(Bi2O3)的降解率分别达到 92% 和 76%。
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引用次数: 0
Hydration Processes in HCl and Aqueous Salt Solutions 盐酸和盐水溶液中的水化过程
Pub Date : 2023-07-21 DOI: 10.18596/jotcsa.1201298
Gunel Shahbazova, E. A. Masimov
In this work, the number of hydration of ions (K+ and Cl-, K+ and Br-, K+ and I-, H+ and Cl-, Li+ and Cl-, Cs+ and Cl-, Na+ and Cl-) in dilute aqueous solutions of some electrolytes of KCl, KBr, KI, HCl, LiCl, CsCl, and NaCl was studied by the proposed refractometric method. Further, the effect of polyethylene glycol (PEG-6000) on the hydration processes for ions in aqueous solutions of KCl and KBr was studied. It turned out that when the polymer is introduced into the solution, the hydration numbers of ions decrease, which is apparently due to the role of the PEG oxygen atom competing with ions in interaction with water molecules.
本文用提出的折射法研究了KCl、KBr、KI、HCl、LiCl、CsCl、NaCl等电解质的稀水溶液中离子(K+与Cl-、K+与Br-、K+与I-、H+与Cl-、Li+与Cl-、Cs+与Cl-、Na+与Cl-)的水化次数。进一步研究了聚乙二醇(PEG-6000)对KCl和KBr水溶液中离子水化过程的影响。结果表明,当聚合物被引入到溶液中时,离子的水化数减少,这显然是由于PEG氧原子在与水分子相互作用时与离子竞争的作用。
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引用次数: 0
3-Hydroxypyridine and 3-(Hydroxymethyl)pyridine in the Synthesis of Salts of Aryldithiophosphonic Acids on the Basis of Monoterpenyl Alcohols 基于单萜醇合成芳基巯基膦酸盐中的 3-羟基吡啶和 3-(羟甲基)吡啶
Pub Date : 2023-07-20 DOI: 10.18596/jotcsa.1290931
I. Nizamov, A. Yakovlev, I. Nizamov, M. Shulaeva
3-Hydroxypyridinium and 3-(hydroxymethyl)pyridinium O-terpenyl aryldithiophosphonates were obtained by the reactions of 3-hydroxypyridine and 3-(hydroxymethyl)pyridine with O-terpenyl aryldithiophosphonic acids on the basis of (1R,2S,5R)-(−)-menthol, (1S)-endo-(–)-borneol, racemic isoborneol, and carvacrol. The obtained salts possess high antimicrobial activity against Bacillus cereus and Candida albicans.
以(1R,2S,5R)-(-)-薄荷醇、(1S)-内-(-)-香薄荷醇、外消旋异龙脑和香芹醇为基础,通过 3-羟基吡啶和 3-(羟甲基)吡啶与 O-叔戊基芳基二硫代磷酸反应,获得了 3-羟基吡啶鎓和 3-(羟甲基)吡啶鎓 O-叔戊基芳基二硫代磷酸盐。获得的盐类对蜡样芽孢杆菌和白色念珠菌具有很强的抗菌活性。
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引用次数: 0
Eco-friendly dyeing of fabric and wool yarn samples with Morus nigra leaf extracts 用黑桑叶提取物对织物和毛纱样品进行环保染色
Pub Date : 2023-07-12 DOI: 10.18596/jotcsa.1286585
Adem Önal, Oguz Özbek, Pakize Düzgün, Sama Nached
Morus nigra L. is a biologically important plant. In addition to the biological importance of the extracts obtained from its various parts, it is used as a material in various fields. In this work, dyeing properties of the cotton fabrics and the wool yarns with Morus nigra L. leaf extracts were investigated. In dyeing studies using Morus nigra L. leaf extracts, yellow tones were obtained in dyeing cotton fabrics, and green and yellow tones were obtained in dyeing wool yarns. Washing, rubbing and light fastness of dyed textile products were examined. According to the results, cotton fabrics showed better dyeing potential than wool yarns. As a result, Morus nigra L. leaf can be used as a natural dyeing agent in the dyeing of textile products.
桑是一种重要的生物植物。除了从其各个部分获得的提取物具有重要的生物学意义外,它还被用作各种领域的材料。研究了桑叶提取物对棉织物和毛纱的染色性能。在桑叶提取物染色研究中,棉织物染色得到黄色调,毛纱染色得到绿色调和黄色调。对染色纺织品的洗涤、摩擦和耐光牢度进行了测试。结果表明,棉织物比毛纱具有更好的染色潜力。结果表明,桑叶可作为天然染色剂用于纺织品的染色。
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引用次数: 0
Improvement of corrosion resistance for brass in 3.5% NaCl media by using 4- fluorophenyl-2, 5-dithiohydrazodicarbonamide 4-氟苯基- 2,5 -二硫代肼二酰胺提高黄铜在3.5% NaCl介质中的耐蚀性
Pub Date : 2023-07-12 DOI: 10.18596/jotcsa.1268115
Mothana Ghazi Kadhim AlFalah, Ahmed Elid, Amgad Ahmed ABDO ALİ, E. Kamberli, Bahar Nazli, Sevilay Koyun, Alihan Tosun, Muhammed Kadi̇rli̇oğlu, Fatma Elkassum, Saleh Quddus Saleh, Abdulrahman Obied, Fatma Kandemi̇rli̇
Corrosion poses a significant challenge for numerous industries. The use of corrosion inhibitors is essential within these industries. The efficacy of environmentally friendly corrosion inhibitors should remain high even when used at low concentrations. In the present study, the compound 4- fluorophenyl-2,5- dithiohydrazodicarbonamide (FTSC) was used as a corrosion inhibitor for brass in 3.5% NaCl solution. The inhibitor efficiency was determined by using a series of electrochemical techniques such as open circuit potential (OCP), potential dynamic polarisation (PDP), linear polarisation resistance (LPR), and electrochemical impedance spectroscopy (EIS). All experimental tests have been done in stagnant conditions. The findings of the experiments revealed that the compound FTSC looked to be of the cathodic type. Furthermore, the maximum inhibitor efficiency was reached at 98.28% at 1 × 10-3 and at an immersion time of 1 h. The current density was reduced from 16.5 to 0.284 A.cm-2. The adsorption of compound on the brass surface in 3.5% NaCl solution obeyed the Langmuir isotherm with a low negative value of the standard Gibbs free energy of adsorption (-33.8 kJ/mol ΔGads (chemisorption and physisorption). The results confirmed that the compound FTSC can be used as a corrosion inhibitor for brass in 3.5% NaCl.
腐蚀是许多行业面临的重大挑战。在这些行业中,使用缓蚀剂是必不可少的。即使在低浓度下使用,环保型缓蚀剂的效果也应保持高。在3.5% NaCl溶液中,用化合物4-氟苯基-2,5-二硫代肼二碳酰胺(FTSC)作为黄铜的缓蚀剂。通过开路电位(OCP)、电位动态极化(PDP)、线性极化电阻(LPR)和电化学阻抗谱(EIS)等一系列电化学技术来确定缓蚀剂的效率。所有的实验测试都是在停滞的条件下进行的。实验结果表明,化合物FTSC看起来是阴极型的。在1 × 10-3、浸泡时间为1 h的条件下,阻垢剂的效率最高可达98.28%,电流密度从16.5降低到0.284A.cm-2。化合物在3.5% NaCl溶液中在黄铜表面的吸附服从Langmuir等温线,吸附的标准吉布斯自由能为-33.8 kJ/mol ΔGads(化学吸附和物理吸附)。结果表明,化合物FTSC在3.5% NaCl中可作为黄铜的缓蚀剂。
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引用次数: 0
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Journal of the Turkish Chemical Society Section A: Chemistry
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