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APPLICATIONS OF NMR AND THEORETICAL CALCULATIONS TO STUDY THE O-H∙∙∙N INTRAMOLECULAR HYDROGEN BOND EFFECT ON THE CONFORMATIONAL EQUILIBRIUM OF CIS-3-N-ETHYLAMINOCYCLOHEXANOL AND CIS-3-N,N-DIETHYLAMINOCYCLOHEXANOL 应用核磁共振和理论计算研究o-h∙∙n分子内氢键对顺-3- n -乙基氨基环己醇和顺-3- n, n -二乙基氨基环己醇构象平衡的影响
IF 0.8 4区 化学 Q3 Chemistry Pub Date : 2023-10-09 DOI: 10.21577/0100-4042.20230051
Paulo R. de Oliveira, R. Rittner, Palimécio Guerrero Jr., P. Batista, G. Costa
Textbooks show that in cis-1,3-disubstituted cyclohexane molecule, the conformer with the substituents in the diaxial positions is higher in energy and hence, it presents a low population in the conformational equilibrium. The diaxial conformer is destabilized by the repulsion between the substituent groups and the axial hydrogen atoms on the same side of the ring. This interaction is known as the 1,3-diaxial interaction. In this study, the solvent effect on the conformational equilibria of cis-3-N-ethylaminocyclohexanol (cis-3-EACOL) and cis-3-N,N-diethylaminocyclohexanol (cis-3-DEACOL) has been assessed through the spin-spin coupling constant (3JHH). The results show that the diaxial conformation of cis-3-EACOL decreases from 92% in CCl4 (∆Gee-aa = 1.48 kcal mol-1 ) to 10% in DMSO-d6 (∆Gee-aa = −1.31 kcal mol-1). For cis-3-DEACOL the diaxial conformer decreased from 36% in CCl4 (∆Gee-aa = −0.33 kcal mol-1) to 7% in Pyridine-d5 (∆Gee-aa = −1.55 kcal mol-1). The stabilization of the diaxial conformer in nonpolar solvents takes place due to the O-H···N intramolecular hydrogen bond, which overcomes the 1,3-diaxial steric interactions.
课本表明,在顺式-1,3-二取代环己烷分子中,取代基在二轴位置的构象能量较高,因此在构象平衡中占比较低。取代基与环同侧的轴向氢原子之间的斥力使二轴形构象不稳定。这种相互作用被称为1,3-二轴相互作用。本研究通过自旋-自旋耦合常数(3JHH)评价了溶剂对顺-3- n-乙基氨基环己醇(顺-3- eacol)和顺-3- n, n-二乙基氨基环己醇(顺-3- deacol)构象平衡的影响。结果表明,顺-3- eacol的双轴构象从CCl4(∆Gee-aa = 1.48 kcal mol-1)中的92%下降到DMSO-d6(∆Gee-aa = - 1.31 kcal mol-1)中的10%。顺-3- deacol的双轴构象从CCl4中的36%(∆Gee-aa = - 0.33 kcal mol-1)下降到吡啶-d5中的7%(∆Gee-aa = - 1.55 kcal mol-1)。在非极性溶剂中,由于O-H···N分子内氢键克服了1,3-二轴位相互作用,使得双轴构象稳定。
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引用次数: 0
PREDICTION OF ANTI-DIABETIC ALOGLIPTIN STABILITY BY ISOTHERMAL STUDIES 用等温研究预测抗糖尿病阿格列汀的稳定性
IF 0.8 4区 化学 Q3 Chemistry Pub Date : 2023-10-09 DOI: 10.21577/0100-4042.20230050
C. Bertol, Gabriel Felimberti, Karini da Rosa, E. Rizzon, R. Pereira, L. Kreutz, Pedro Froelich
Alogliptin (ALG) benzoate is an oral hypoglycemic drug that works as a DPP-4 inhibitor to prevent incretin degradation. Forced stability studies use high temperatures to decompose drugs and estimate their behavior at low temperatures. We aimed to evaluate the thermal stability of ALG using two techniques: isothermal thermogravimetry (TGA) and degradation in an oven followed by liquid chromatography (LC-PDA) analysis. ALG was subjected to 150, 155, 160, 165, and 170 °C up to 10% of mass loss in isothermal TGA. In the oven, the drug was submitted to 130, 140, 150, 155, 160, and 170 °C. Kinetic parameters were calculated with the Arrhenius model. ALG followed zero-order kinetics, in which the degradation rate did not depend on reagent concentration. Activation energy ranged from 31.0 to 35.9 kcal mol-1. The degraded drug was less toxic in a cytotoxicity assay in CRIB cells than the undegraded drug. The TGA method is faster and more practical than the oven followed by LC-PDA, and the data present a correlation. Here we described the kinetic parameters of ALG degradation, improving the knowledge about the drug and assisting in developing new formulations from the drug.
阿格列汀(ALG)苯甲酸酯是一种口服降糖药物,作为DPP-4抑制剂防止肠促胰岛素降解。强制稳定性研究使用高温来分解药物并估计它们在低温下的行为。采用等温热重法(TGA)和液相色谱法(LC-PDA)对ALG的热稳定性进行了评价。在等温热重分析中,ALG分别在150、155、160、165和170°C下进行了高达10%的质量损失。在烘箱中,将药物置于130、140、150、155、160和170°C。采用Arrhenius模型计算动力学参数。ALG遵循零级动力学,其中降解速率不依赖于试剂浓度。活化能范围为31.0 ~ 35.9 kcal mol-1。在细胞毒性试验中,降解药物在CRIB细胞中的毒性低于未降解药物。TGA法比烤炉法和LC-PDA法更快、更实用,且数据具有相关性。在这里,我们描述了ALG降解的动力学参数,提高了对药物的认识,并协助从药物开发新的配方。
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引用次数: 0
DETERMINATION OF RESIDUAL METHANOL AND ETHANOL IN BIODIESEL BY 1H-NMR 氢核磁共振法测定生物柴油中甲醇和乙醇残留量
IF 0.8 4区 化学 Q3 Chemistry Pub Date : 2023-10-09 DOI: 10.21577/0100-4042.20230046
Samuel Santos, Cassiane Dutra, Luiz Fontoura
Alcohol residues in biodiesel can be present even after the purification steps. It diminishes the flash point, lubricity and cetane number. The standard technique to quantify residual alcohol in biodiesel is the FID-GC with headspace sampling. NMR, although underused for quantitative analyses, requires no special sample preparation, and consumes low volume of solvent. In this work, methodologies for the residual methanol and ethanol contents in soy biodiesel by 1H-NMR in a 9.4 T (400 MHz) spectrometer by standard addition were developed and validated. Quantification limits were found equal to 0.07 and 0.08% respectively, so more than twice lower than the maximum level acceptable, which is 0.2%. Accuracy and precision were considered suitable for the alcohol content around the specification limit.
生物柴油中的酒精残留物即使经过提纯步骤也可能存在。它降低了闪点、润滑性和十六烷值。定量生物柴油中残醇的标准技术是顶空取样FID-GC。核磁共振虽然在定量分析中使用不足,但不需要特殊的样品制备,并且消耗的溶剂量小。本研究建立并验证了在9.4 T (400 MHz)谱仪中标准添加1H-NMR测定大豆生物柴油中残留甲醇和乙醇含量的方法。定量限分别为0.07%和0.08%,比可接受的最大限量0.2%低2倍以上。准确度和精密度被认为适合于酒精含量在规范限度附近。
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引用次数: 0
DIFFUSION STUDY OF NaCl AND KCl AT THE SOLUTION/OLIVE INTERFACE: MATHEMATICAL MODELING USING THE FINITE ELEMENT METHOD AND SELF-ORGANIZING FEATURE MAP (SOFM)-TYPE NEURAL NETWORKS NaCl和KCl在溶液/橄榄界面的扩散研究:使用有限元方法和自组织特征映射(SOFM)型神经网络的数学建模
IF 0.8 4区 化学 Q3 Chemistry Pub Date : 2023-10-09 DOI: 10.21577/0100-4042.20230053
D. Borsato, M. Clemente, Heloisa Silva, Nathan Silva, Júlia Campos, Eduardo Sousa, H. Silva, Karina B. Angilelli, A. Mantovani, Rafael Mantovani
Olive samples were subjected to the salting process in brine containing 1196 mol m-3 of NaCl and 402 mol m-3 of KCl. Samples were collected during 60 h and salt concentration values were determined. With the finite element method (FEM) and the minimization of the errors percentage between the simulated and experimental values, the mass transfer coefficients in the film (hm) were obtained, being 1.0072 × 10-8 and 1.2499 × 10-8 for NaCl and KCl, respectively. The salts concentration at the olive/brine interface was simulated by FEM and analyzed via SOFM. A network with 4 × 4 topology and 10000 training epochs was used. It was observed that the influence of the stationary film formed on the surface of the olives during the salting process depends on the position, the salt involved in the diffusion and that the concentration of the salts, at each point, varies according to the immersion time.
橄榄样品在含1196 mol m-3 NaCl和402 mol m-3 KCl的盐水中进行腌制。60 h内采集样品,测定盐浓度。采用有限元法(FEM),尽量减小模拟值与实验值之间的误差百分比,得到了NaCl和KCl在膜内的传质系数hm,分别为1.0072 × 10-8和1.2499 × 10-8。采用有限元法模拟了橄榄/卤水界面的盐浓度,并用SOFM法对其进行了分析。使用4 × 4拓扑和10000个训练epoch的网络。观察到,在腌制过程中,橄榄表面形成的固定膜的影响取决于扩散所涉及的盐的位置,并且在每个点上盐的浓度随浸泡时间而变化。
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引用次数: 0
FUNCTIONAL AND TECHNOLOGICAL PROPERTIES OF COFFEE MUCILAGE (Coffea arabica) AND ITS APPLICATION IN EDIBLE FILMS 咖啡胶浆(阿拉比卡咖啡)的功能、工艺特性及其在食用薄膜中的应用
IF 0.8 4区 化学 Q3 Chemistry Pub Date : 2023-10-09 DOI: 10.21577/0100-4042.20230052
Daiane Machado, R. D. de Oliveira
Brazil is the largest coffee producer in the world, and together with the millions of tons produced, millions of tons of residues are also generated. The generated residues are a source of environmental contamination depending on the chosen processing route. One of the main applications of food industry waste is in the production of raw materials to produce edible films and coatings. Coffee mucilage is a pectin-rich liquid residue from the coffee sector that can be used in the production of value-added products. Given this, the objective of this work was to characterize and evaluate the potential of functional and technological properties of coffee mucilage and your applicability in the production of edible films. The filmogenic mixture was obtained by casting from 10% (w/v) lyophilized coffee mucilage and solvent (water). The films produced from the coffee mucilage presented good homogeneity, continuity (absence of ruptures or fragile regions), flexibility, ease of detachment of the support and handling, without the need to add adjuvant to its formation. In addition, they presented uniformity in thickness, high light barrier and medium water vapor barrier. Thus, it can be concluded that mucilage is a potential product to be used in the cosmetic, pharmaceutical and food industries.
巴西是世界上最大的咖啡生产国,在生产数百万吨咖啡的同时,也产生了数百万吨的残留物。根据所选择的加工路线,所产生的残留物是环境污染源。食品工业废弃物的主要应用之一是生产可食用薄膜和涂料的原料。咖啡胶是一种富含果胶的液体残渣,来自咖啡行业,可用于生产增值产品。鉴于此,本工作的目的是表征和评估咖啡粘液的功能和技术特性的潜力,以及它们在可食用薄膜生产中的适用性。以10% (w/v)的冻干咖啡胶浆和溶剂(水)为原料,通过浇铸得到成膜混合物。由咖啡粘液制成的薄膜具有良好的均匀性、连续性(没有破裂或脆弱区域)、柔韧性、易于脱离支撑和处理,而不需要添加佐剂来形成。此外,它们还具有厚度均匀性、高光阻隔性和中等水汽阻隔性。因此,可以得出结论,粘液是一种潜在的产品,可用于化妆品,制药和食品工业。
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引用次数: 0
GUIA DETALHADO PARA MONTAGEM PRÓPRIA DE IMPRESSORAS 3D 自己组装3D打印机的详细指南
IF 0.8 4区 化学 Q3 Chemistry Pub Date : 2023-10-09 DOI: 10.21577/0100-4042.20230057
M. Pereira, R. Quero, Dosil Pereira De Jesus, Juliano Bonacin
DETAILED GUIDE TO OWN ASSEMBLY OF 3D PRINTERS. In recent years, there has been an increase in the use of 3D printing for the manufacture of three-dimensional objects. Thus, it is clear that 3D printers have presented as a tool with high potential for applications in several fields, including chemistry. However, despite its popularity, it is notable that some 3D printers have a relatively high cost, in addition to not favoring optimizations or repairs, making users dependent on the manufacturers of such tools. Therefore, this article aims to present, particularly to the chemistry community, a detailed guide for assembling a low-cost FDM-type 3D printer with good performance. Consequently, we hope that this guide can contribute to increasing the 3D printing popularization in the field of chemistry because of the various possibilities of applications in this area.
详细指南自己组装3d打印机。近年来,使用3D打印制造三维物体的情况有所增加。因此,很明显,3D打印机在包括化学在内的多个领域都具有很高的应用潜力。然而,尽管它很受欢迎,值得注意的是,一些3D打印机的成本相对较高,而且不支持优化或维修,使得用户依赖于这些工具的制造商。因此,本文旨在为化学界提供一个组装性能良好的低成本fdm型3D打印机的详细指南。因此,我们希望本指南能够促进3D打印在化学领域的普及,因为这一领域的应用有多种可能性。
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引用次数: 0
UMA ANÁLISE DO PROCESSO DE ELABORAÇÃO DE PERGUNTAS PRODUZIDAS POR LICENCIANDOS EM QUÍMICA A PARTIR DA LITERATURA DE DIVULGAÇÃO CIENTÍFICA 对化学本科生提出的问题的阐述过程进行了分析,并从科学文献中进行了分析
IF 0.8 4区 化学 Q3 Chemistry Pub Date : 2023-10-09 DOI: 10.21577/0100-4042.20230047
Pedro Paulo Da Silva, Flávio Schifino, C. Sirtori, C. Passos, N. Simon
AN ANALYSIS OF THE PROCESS OF DEVELOPING QUESTIONS PRODUCED BY CHEMISTRY STUDENTS IN A TEACHING PROGRAM BASED ON SCIENTIFIC COMMUNICATION LITERATURE. The objective of the present investigation was to evaluate the use of scientific dissemination literature (SDL) in the process of formulating questions developed by chemistry students in a Teaching Program in Chemistry. To this end, the book entitled The Disappearing Spoon was analyzed in terms of categories referring to format and content, while the 18 questions produced by these students about the chapters read were analyzed in terms of presupposition and request. The investigation was carried out with 16 undergraduates who were taking a theoretical course on “Introduction to Chemistry”, as part of the Teaching Program in Chemistry. According to the analysis carried out, some particularities of format, such as the scarcity of visual resources, the autonomous structure of the chapters and the language, may have influenced the elaborated presentations. It is interesting to note that almost half of the questions produced were of an investigative nature, demonstrating the potential of SDL to stimulate high cognitive skills. In addition, the questions with investigative requests were mostly opinion questions, which may have been motivated by characteristics of the text read, such as the content with a controversial approach used by the author, when reporting on some aspects of scientific activity.
基于科学传播文献的教学方案中化学学生提出问题的过程分析。本研究的目的是评估化学教学计划中化学学生在制定问题过程中使用科学传播文献(SDL)的情况。为此,我们对《消失的勺子》这本书从形式和内容的分类上进行了分析,对这些学生提出的关于所读章节的18个问题从预设和请求上进行了分析。调查对象是16名正在上“化学导论”理论课的本科生,这是化学教学计划的一部分。根据分析,格式的一些特殊性,如视觉资源的稀缺性,章节的自治结构和语言,可能影响了详细的陈述。有趣的是,几乎一半的问题都是调查性的,这表明SDL有可能激发高认知技能。此外,有调查要求的问题大多是意见问题,这些问题可能是由所读文本的特征引起的,例如作者在报道科学活动的某些方面时使用了有争议的方法的内容。
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引用次数: 0
A BIOQUÍMICA POR TRÁS DA COVID-19: DESENVOLVIMENTO E APLICAÇÃO DE WEBQUEST DIRECIONADA AO ENSINO REMOTO EMERGENCIAL COVID-19背后的生物化学:针对紧急远程学习的WEBQUEST开发和应用
IF 0.8 4区 化学 Q3 Chemistry Pub Date : 2023-10-09 DOI: 10.21577/0100-4042.20230044
N. Silva, Carolina Sotério, Fernanda Canduri, S. Queiroz
THE BIOCHEMISTRY BEHIND COVID-19: WEBQUEST DEVELOPMENT AND APPLICATION FOR EMERGENCY REMOTE TEACHING. WebQuests are inquiry-oriented activities structured in such a way that almost all resources used come from the web. The present study aims to investigate to what extent a WebQuest focusing on Biochemistry and COVID-19 can be used as an instructive tool to enhance undergraduate students’ media and information literacy (MIL). Students’ opinions on the use of the WebQuest were also discussed. The WebQuest was implemented in a BSc in Physical and Biomolecular Sciences course in the context of the COVID-19 pandemic. Based on the results of this study, the WebQuest has improved the MIL competence of students and motivated them towards learning Biochemistry.
covid-19背后的生物化学:紧急远程教学的webquest开发和应用。webquest是面向查询的活动,其结构使得几乎所有使用的资源都来自web。本研究旨在探讨以生物化学和COVID-19为重点的WebQuest在多大程度上可以作为提高大学生媒体和信息素养(MIL)的指导性工具。讨论了学生对WebQuest使用的看法。WebQuest是在2019冠状病毒病大流行背景下,在物理和生物分子科学理学士课程中实施的。本研究结果显示,WebQuest提高了学生的多媒体素养,并激发了学生学习生物化学的积极性。
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引用次数: 0
ATR-FTIR AND UV-VIS AS TECHNIQUES FOR METHANOL ANALYSIS IN BIODIESEL-WASHING WASTEWATER after - ftir和uv-vis技术在生物柴油洗涤废水中甲醇分析中的应用
IF 0.8 4区 化学 Q3 Chemistry Pub Date : 2023-08-28 DOI: 10.21577/0100-4042.20230041
Methanol present in wastewater from the biodiesel industry can become an atmospheric pollutant and an environmental liability of effluents. This article proposes the development and performance evaluation of two spectroscopic methods, ATR-FTIR and UV-Vis, to identify and quantify methanol in aqueous media. The results of both ways exhibited remarkable linear detection, with a coefficient of determination (r2) > 0.99, wide working range, and relative standard deviation (RSD) < 12%. In the ATR-FTIR method, the detection and quantification limits were 0.064 and 0.128% m V-1, respectively. The UV-Vis method presented lower limits (0.005 and 0.008% m V-1, respectively). Finally, the methods were successfully applied to quickly and sensitively quantify the methanol present in wastewater from biodiesel-washing in a wide concentration range of 0.008-0.641% m V-1. Therefore, we evidenced the feasibility of spectroscopic methods in quality control for identifying and quantifying methanol in aqueous solution, with potential for application in biodiesel production industries and research laboratories. Mainly by ATR-FTIR, in the region of 1300-900 cm-1, as it proved to be more environmentally friendly, faster, and cheaper than the GC-FID method.
生物柴油工业废水中存在的甲醇可能成为大气污染物和废水的环境负担。本文提出了ATR-FTIR和UV-Vis两种光谱方法的发展和性能评价,用于鉴别和定量水介质中的甲醇。两种方法均具有良好的线性检测效果,检测系数(r2)均为0.99,工作范围宽,相对标准偏差(RSD) < 12%。在ATR-FTIR方法中,检测限和定量限分别为0.064和0.128% m V-1。紫外可见法的下限分别为0.005 m V-1和0.008% m V-1。最后,这些方法成功地用于快速、灵敏地定量生物柴油洗涤废水中存在的甲醇,浓度范围为0.008-0.641% m V-1。因此,我们证明了光谱方法在鉴别和定量水溶液中甲醇的质量控制中的可行性,具有应用于生物柴油生产行业和研究实验室的潜力。主要是通过ATR-FTIR,在1300-900 cm-1范围内,因为它被证明比GC-FID方法更环保,更快,更便宜。
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引用次数: 0
BOAS PRÁTICAS SUSTENTÁVEIS DE GESTÃO DE RESÍDUOS QUÍMICOS EM INSTITUIÇÕES PÚBLICAS DE ENSINO SUPERIOR 公立高等教育机构化学废物管理的可持续良好做法
IF 0.8 4区 化学 Q3 Chemistry Pub Date : 2023-08-28 DOI: 10.21577/0100-4042.20230034
Marcus Arantes, W. Günther
THE BEST SUSTAINABLE PRACTICES FOR CHEMICAL WASTE MANAGEMENT IN PUBLIC HIGHER EDUCATION INSTITUTIONS. This work proposes the minimum items for the composition of the best sustainable practices for chemical waste management in higher education institutions (HEI). It was made a bibliographical and documentary review of the Brazilian legislation applicable to the management of chemical waste, with the aim of supporting the elaboration of the best sustainable practices for chemical waste management and propose to assist the technical managers of HEI in the implementation of sustainable and safe management of chemical waste.
公立高等教育机构化学废物管理的最佳可持续做法。这项工作提出了构成高等教育机构化学废物管理最佳可持续做法的最低项目。它对巴西适用于化学废物管理的立法进行了书目和文献审查,目的是支持拟订化学废物管理的最佳可持续做法,并建议协助高等教育机构的技术管理人员对化学废物实施可持续和安全的管理。
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引用次数: 0
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Quimica Nova
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