Pub Date : 2024-09-19DOI: 10.1007/s10008-024-06071-6
Ronaldo Augusto de S. Santos, Isabela de F. Schaffel, Gabriel Fernandes S. dos Santos, José Guilherme A. Rodrigues, Rafael de Q. Ferreira
Bee honey has gained significant interest as a crucial commodity in Brazilian agribusiness, leading to its increased consumption in recent years because of its nutritional properties in humans. Legislation based on the Codex Alimentarius establishes quality control parameters essential for ensuring the safety and quality of honey. These parameters include the measurement of hydroxymethylfurfural (HMF), an indicator of honey quality. Currently, the primary methods for determining HMF concentration in honey are spectrophotometric and chromatographic tests. This study proposes a simpler alternative electroanalytical methodology that uses a screen-printed carbon electrode to monitor the HMF in honey. This portable technique offers advantages over commonly used methods, such as lower cost, similar efficacy, and requirement of only 70 µL of solution per analysis. Square-wave voltammetry was employed to determine HMF in Britton-Robinson buffer (pH 9.0), and the technique was optimized based on the experimental design, generating statistical chemical prediction results. The optimal values for modulation amplitude, step potential, and frequency were 81.5 mV, 22.5 mV, and 5 Hz, respectively. The recovery rate was within the limits established by AOAC International (80–110%), except for the concentration of 6.0 × 10−7 mol L−1, which showed a 2.07% higher recovery, indicating a minor matrix effect. The calibration curve had an R2 value of 99%, with a limit of detection of 6.76 × 10−8 mol L−1 and a limit of quantification of 2.23 × 10−7 mol L−1. Therefore, a rapid, cost-effective, and efficient methodology was established to quantify HMF in honey.
Graphical Abstract
A simpler and portable electroanalytical methodology based on screen-printed carbon electrodes to determine the HMF in honey
{"title":"Voltammetric determination of hydroxymethylfurfural in honey using screen-printed carbon electrodes: optimization and in-house validation tests","authors":"Ronaldo Augusto de S. Santos, Isabela de F. Schaffel, Gabriel Fernandes S. dos Santos, José Guilherme A. Rodrigues, Rafael de Q. Ferreira","doi":"10.1007/s10008-024-06071-6","DOIUrl":"https://doi.org/10.1007/s10008-024-06071-6","url":null,"abstract":"<p>Bee honey has gained significant interest as a crucial commodity in Brazilian agribusiness, leading to its increased consumption in recent years because of its nutritional properties in humans. Legislation based on the <i>Codex Alimentarius</i> establishes quality control parameters essential for ensuring the safety and quality of honey. These parameters include the measurement of hydroxymethylfurfural (HMF), an indicator of honey quality. Currently, the primary methods for determining HMF concentration in honey are spectrophotometric and chromatographic tests. This study proposes a simpler alternative electroanalytical methodology that uses a screen-printed carbon electrode to monitor the HMF in honey. This portable technique offers advantages over commonly used methods, such as lower cost, similar efficacy, and requirement of only 70 µL of solution per analysis. Square-wave voltammetry was employed to determine HMF in Britton-Robinson buffer (pH 9.0), and the technique was optimized based on the experimental design, generating statistical chemical prediction results. The optimal values for modulation amplitude, step potential, and frequency were 81.5 mV, 22.5 mV, and 5 Hz, respectively. The recovery rate was within the limits established by AOAC International (80–110%), except for the concentration of 6.0 × 10<sup>−7</sup> mol L<sup>−1</sup>, which showed a 2.07% higher recovery, indicating a minor matrix effect. The calibration curve had an <i>R</i><sup>2</sup> value of 99%, with a limit of detection of 6.76 × 10<sup>−8</sup> mol L<sup>−1</sup> and a limit of quantification of 2.23 × 10<sup>−7</sup> mol L<sup>−1</sup>. Therefore, a rapid, cost-effective, and efficient methodology was established to quantify HMF in honey.</p><h3 data-test=\"abstract-sub-heading\">Graphical Abstract</h3><p>A simpler and portable electroanalytical methodology based on screen-printed carbon electrodes to determine the HMF in honey</p>","PeriodicalId":665,"journal":{"name":"Journal of Solid State Electrochemistry","volume":"60 1","pages":""},"PeriodicalIF":2.5,"publicationDate":"2024-09-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142247487","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}
Pub Date : 2024-09-19DOI: 10.1007/s10008-024-06078-z
Alisha Mary Manoj, Leema Rose Viannie
This paper presents a comparative study of the electrochemical pH sensing characteristics of N-ZnO on a carbon screen-printed electrode (N-ZnO/C) and a silver screen-printed electrode (N-ZnO/Ag). The surface-morphological properties of the film were evaluated using scanning electron microscopy. Electrochemical evaluation was carried out in the presence of common salts present in physiological fluids like NaCl and KCl. Cyclic voltammetry (CV) and chronoamperometry (CA) were carried out to evaluate the response characteristics of the solution under different pHs. Electrochemical impedance spectroscopy (EIS) was carried out to determine the interfacial parameters ruling the pH sensing mechanism for different electrode configurations. The studies revealed that the carbon-based electrodes exhibit stable behavior, with a sensitivity of 17.8 nA·cm−2/pH and a linear correlation (r2 = 0.996) across a range of acidic to basic conditions, thereby enhancing the sensor’s performance. The carbon electrodes demonstrated superior sensing properties, attributed to their improved stability and conductivity. This advancement in sensor technology offers promising potential for applications requiring reliable and precise measurements.
{"title":"Comparative analysis of pH sensing performance of nitrogen-doped ZnO on screen-printed silver and carbon electrodes","authors":"Alisha Mary Manoj, Leema Rose Viannie","doi":"10.1007/s10008-024-06078-z","DOIUrl":"https://doi.org/10.1007/s10008-024-06078-z","url":null,"abstract":"<p>This paper presents a comparative study of the electrochemical pH sensing characteristics of N-ZnO on a carbon screen-printed electrode (N-ZnO/C) and a silver screen-printed electrode (N-ZnO/Ag). The surface-morphological properties of the film were evaluated using scanning electron microscopy. Electrochemical evaluation was carried out in the presence of common salts present in physiological fluids like NaCl and KCl. Cyclic voltammetry (CV) and chronoamperometry (CA) were carried out to evaluate the response characteristics of the solution under different pHs. Electrochemical impedance spectroscopy (EIS) was carried out to determine the interfacial parameters ruling the pH sensing mechanism for different electrode configurations. The studies revealed that the carbon-based electrodes exhibit stable behavior, with a sensitivity of 17.8 nA·cm<sup>−2</sup>/pH and a linear correlation (<i>r</i><sup>2</sup> = 0.996) across a range of acidic to basic conditions, thereby enhancing the sensor’s performance. The carbon electrodes demonstrated superior sensing properties, attributed to their improved stability and conductivity. This advancement in sensor technology offers promising potential for applications requiring reliable and precise measurements.</p>","PeriodicalId":665,"journal":{"name":"Journal of Solid State Electrochemistry","volume":"18 1","pages":""},"PeriodicalIF":2.5,"publicationDate":"2024-09-19","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142247488","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}
Enormous scientific interests focused on the improvement of the electrocatalytic activity of counter electrodes for their application in dye-sensitized solar cells (DSSCs). In this regards, we have elaborated a novel gold and platinum (AuPt) nanostructures via direct and indirect electrodeposition techniques; the first one is cyclic voltammetric, while the second one is a combination of amperometric and potentiostatic methods. The as-prepared AuPt nanomaterials, which were characterized by XRD, XPS, SEM, and CA, and electrochemical analysis such as cyclic voltammetry, electrochemical impedance spectroscopy, and Tafel polarization were employed as counter electrode in dye sensitized solar cells. The AuPt counter electrode prepared by cyclic voltammetric technique was the best electrocatalytic activity toward ({text{I}}_{3}^{-}/{text{I}}^{-}) reduction, low charge transfer resistance of 9.2 Ω cm2, and good chemical and electrochemical stability in the electrolyte. The assembled cell with the Au/Pt electrode provided a maximum power density of 2.35 mW cm−2 with an efficiency of 2.35% under back illumination of 100 mW cm−2 and AM 1.5 G.
Graphical Abstract
大量科学兴趣集中在提高对电极的电催化活性上,以便将其应用于染料敏化太阳能电池(DSSC)。为此,我们通过直接和间接电沉积技术制备了一种新型金铂(AuPt)纳米结构;第一种是循环伏安法,第二种是安培法和电位法相结合的方法。制备的 AuPt 纳米材料通过 XRD、XPS、SEM 和 CA 以及电化学分析(如循环伏安法、电化学阻抗光谱法和 Tafel 极化法)进行了表征,并被用作染料敏化太阳能电池的对电极。通过循环伏安技术制备的金铂对电极对({text{I}}_{3}^{-}/{text{I}}^{-})还原具有最佳的电催化活性,电荷转移电阻低至 9.2 Ω cm2,并且在电解液中具有良好的化学和电化学稳定性。在 100 mW cm-2 和 AM 1.5 G 的背光照明下,使用金/铂电极组装的电池可提供 2.35 mW cm-2 的最大功率密度和 2.35% 的效率。
{"title":"Effect of electrodeposition of AuPt nanostructure thin films on the electrocatalytic activity of counter electrodes: DSSCs application","authors":"Hayet Lallali, Abdelhadi Bentouami, Fatma Zohra Tighilt, Samia Belhousse, Kahina Lasmi, Khaled Hamdani, Sabrina Sam, Amar Manseri","doi":"10.1007/s10008-024-06074-3","DOIUrl":"https://doi.org/10.1007/s10008-024-06074-3","url":null,"abstract":"<p>Enormous scientific interests focused on the improvement of the electrocatalytic activity of counter electrodes for their application in dye-sensitized solar cells (DSSCs). In this regards, we have elaborated a novel gold and platinum (AuPt) nanostructures via direct and indirect electrodeposition techniques; the first one is cyclic voltammetric, while the second one is a combination of amperometric and potentiostatic methods. The as-prepared AuPt nanomaterials, which were characterized by XRD, XPS, SEM, and CA, and electrochemical analysis such as cyclic voltammetry, electrochemical impedance spectroscopy, and Tafel polarization were employed as counter electrode in dye sensitized solar cells. The AuPt counter electrode prepared by cyclic voltammetric technique was the best electrocatalytic activity toward <span>({text{I}}_{3}^{-}/{text{I}}^{-})</span> reduction, low charge transfer resistance of 9.2 Ω cm<sup>2</sup>, and good chemical and electrochemical stability in the electrolyte. The assembled cell with the Au/Pt electrode provided a maximum power density of 2.35 mW cm<sup>−2</sup> with an efficiency of 2.35% under back illumination of 100 mW cm<sup>−2</sup> and AM 1.5 G.</p><h3 data-test=\"abstract-sub-heading\">Graphical Abstract</h3>","PeriodicalId":665,"journal":{"name":"Journal of Solid State Electrochemistry","volume":"9 1","pages":""},"PeriodicalIF":2.5,"publicationDate":"2024-09-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142247489","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}
Pub Date : 2024-09-17DOI: 10.1007/s10008-024-06079-y
Guilherme P. Oliveira, Lucas V. de Faria, Natalia M. Caldas, Amanda G. Batista, Suéllen F. L. do Nascimento, Murillo N. T. Silva, Fernanda N. Feiteira, Edson Nossol, Diego P. Rocha, Felipe S. Semaan, Wagner F. Pacheco, Rafael M. Dornellas
Developing new sensors presenting low-cost, portability, and disposability features is of paramount in the electrochemical field. Thus, this work proposes the fabrication of lab-made composite electrodes using acrylonitrile butadiene styrene, graphite, and aluminum oxide. In this investigation, the amount of aluminum oxide (0 to 12.25 w/w) was carefully optimized, and its impact on the electrochemical performance of the electrode was observed using the ferri-ferro redox probe and dopamine (DOP) as a proof of concept. This innovative electrode was characterized by spectroscopy, morphological, elemental, and electrochemical techniques. Using the alumina-loaded electrode, significantly improved cyclic voltammetric responses regarding peak currents and peak-to-peak separation were obtained for both evaluated species. This sensor was integrated into the batch injection analysis system for amperometric monitoring of DOP in synthetic biological fluids (saliva and urine) and tap water. The developed method showed a wide linear range (10 to 1000 µmol L−1), a low detection limit (2.6 µmol L−1), and a high analytical frequency (182 analyses per hour). Furthermore, it was precise (RSD < 5%), accurate (recoveries between 90.5 and 107.3%), and selective. Therefore, it can be considered a low-cost alternative analytical tool for electrochemical sensing of DOP in samples of clinical and environmental interest.
{"title":"Effortless lab-manufactured carbon and alumina-based composite sensors for enzymeless sensitive amperometric detection of dopamine in clinical and environmental samples","authors":"Guilherme P. Oliveira, Lucas V. de Faria, Natalia M. Caldas, Amanda G. Batista, Suéllen F. L. do Nascimento, Murillo N. T. Silva, Fernanda N. Feiteira, Edson Nossol, Diego P. Rocha, Felipe S. Semaan, Wagner F. Pacheco, Rafael M. Dornellas","doi":"10.1007/s10008-024-06079-y","DOIUrl":"https://doi.org/10.1007/s10008-024-06079-y","url":null,"abstract":"<p>Developing new sensors presenting low-cost, portability, and disposability features is of paramount in the electrochemical field. Thus, this work proposes the fabrication of lab-made composite electrodes using acrylonitrile butadiene styrene, graphite, and aluminum oxide. In this investigation, the amount of aluminum oxide (0 to 12.25 w/w) was carefully optimized, and its impact on the electrochemical performance of the electrode was observed using the ferri-ferro redox probe and dopamine (DOP) as a proof of concept. This innovative electrode was characterized by spectroscopy, morphological, elemental, and electrochemical techniques. Using the alumina-loaded electrode, significantly improved cyclic voltammetric responses regarding peak currents and peak-to-peak separation were obtained for both evaluated species. This sensor was integrated into the batch injection analysis system for amperometric monitoring of DOP in synthetic biological fluids (saliva and urine) and tap water. The developed method showed a wide linear range (10 to 1000 µmol L<sup>−1</sup>), a low detection limit (2.6 µmol L<sup>−1</sup>), and a high analytical frequency (182 analyses per hour). Furthermore, it was precise (RSD < 5%), accurate (recoveries between 90.5 and 107.3%), and selective. Therefore, it can be considered a low-cost alternative analytical tool for electrochemical sensing of DOP in samples of clinical and environmental interest.</p>","PeriodicalId":665,"journal":{"name":"Journal of Solid State Electrochemistry","volume":"106 1","pages":""},"PeriodicalIF":2.5,"publicationDate":"2024-09-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142268148","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}
Pub Date : 2024-09-17DOI: 10.1007/s10008-024-06075-2
Mahsa Sadat Sarmalek, Mehdi Adelifard, Seyed Ahmad Nabavi Amri
This research focused on the synthesis of gallium oxide (γ-Ga2O3) nanoparticles using sol–gel and hydrothermal techniques. X-ray diffraction (XRD), field emission electron microscopy (FESEM), UV–Vis spectrophotometer, Fourier transform infrared spectroscopy (FTIR), cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), calculation of specific capacitance (SC), and specific capacitance (Q) techniques were used. XRD patterns showed the formation of the cubic phase of gallium oxide (γ-Ga2O3). The polyhedral and spherical grains can be seen in the FESEM images of the synthesized nanostructures. The band gap values were determined between 4.29 and 4.42 eV. The FTIR results indicate the formation of a gallium oxide structure. The cyclic voltammetry (CV) results are consistent with the redox reactions performed. Samples produced by sol–gel and hydrothermal synthesis, then microwave-annealed, have the highest capacity (SC). They show values of 1172.6 mAh g−1 and 1261.9 mAh g−1, respectively. These results show that these nanoparticles are effective anodes for lithium-ion batteries.
本研究的重点是利用溶胶-凝胶和水热技术合成氧化镓(γ-Ga2O3)纳米粒子。研究采用了 X 射线衍射 (XRD)、场发射电子显微镜 (FESEM)、紫外可见分光光度计、傅立叶变换红外光谱 (FTIR)、循环伏安法 (CV)、电化学阻抗光谱 (EIS)、比电容 (SC) 和比电容 (Q) 计算等技术。XRD 图谱显示形成了氧化镓的立方相(γ-Ga2O3)。从合成纳米结构的 FESEM 图像中可以看到多面体和球形晶粒。带隙值在 4.29 和 4.42 eV 之间。傅立叶变换红外光谱结果表明形成了氧化镓结构。循环伏安法(CV)结果与氧化还原反应一致。通过溶胶-凝胶法和水热法合成,然后进行微波退火的样品具有最高的容量(SC)。它们的值分别为 1172.6 mAh g-1 和 1261.9 mAh g-1。这些结果表明,这些纳米粒子是锂离子电池的有效阳极。
{"title":"Comparative study of the structural, optical, and electrochemical properties of γ-Ga2O3 synthesized by microwave hydrothermal and sol–gel techniques","authors":"Mahsa Sadat Sarmalek, Mehdi Adelifard, Seyed Ahmad Nabavi Amri","doi":"10.1007/s10008-024-06075-2","DOIUrl":"https://doi.org/10.1007/s10008-024-06075-2","url":null,"abstract":"<p>This research focused on the synthesis of gallium oxide (γ-Ga<sub>2</sub>O<sub>3</sub>) nanoparticles using sol–gel and hydrothermal techniques. X-ray diffraction (XRD), field emission electron microscopy (FESEM), UV–Vis spectrophotometer, Fourier transform infrared spectroscopy (FTIR), cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), calculation of specific capacitance (SC), and specific capacitance (Q) techniques were used. XRD patterns showed the formation of the cubic phase of gallium oxide (γ-Ga<sub>2</sub>O<sub>3</sub>). The polyhedral and spherical grains can be seen in the FESEM images of the synthesized nanostructures. The band gap values were determined between 4.29 and 4.42 eV. The FTIR results indicate the formation of a gallium oxide structure. The cyclic voltammetry (CV) results are consistent with the redox reactions performed. Samples produced by sol–gel and hydrothermal synthesis, then microwave-annealed, have the highest capacity (SC). They show values of 1172.6 mAh g<sup>−1</sup> and 1261.9 mAh g<sup>−1</sup>, respectively. These results show that these nanoparticles are effective anodes for lithium-ion batteries.</p>","PeriodicalId":665,"journal":{"name":"Journal of Solid State Electrochemistry","volume":"119 1","pages":""},"PeriodicalIF":2.5,"publicationDate":"2024-09-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142268145","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}
Pub Date : 2024-09-17DOI: 10.1007/s10008-024-06051-w
Marina Medina, Vinícius José Carvalho, Leanderson Araujo da Silva, Gabriel Gonçalves Borges, Thiago Capelupi, Arthur Piani, Pedro Paes Mauriz, João Vitor Gomes, Juliana Ferreira de Brito
Our energy generation and other industrial processes on which our current lifestyle is based cause significant environmental impacts. Some widely employed industrial processes are major contributors to CO2 emissions. A prime example is ammonia production, which represents a high energy consumption, utilizes natural gas, and generates hundreds of millions of tons of CO2 annually. Proper waste treatment, alternatives to fossil fuels, and chemical compound production processes are crucial to address these issues. In this regard, (photo)electrochemical techniques such as electrocatalysis (EC) and photoelectrocatalysis (PEC) can aid in the clean and cost-effective treatment of wastewater while also generating new fuels and commercially valuable chemical compounds. Reduction reactions can be specifically applied to (i) CO2 molecules, producing fuels; (ii) N2 molecules, generating NH3; and (iii) H + species, producing H2. Oxidation reactions can be employed for organic and inorganic molecules present in real effluents, aiming to treat contaminated water. Electrocatalytic Brazilian research groups have been contributing not only to those redox reaction investigations but also to the synthesis of electrocatalysts for both reactions, making them more cost-effective, specific, and efficient, opening new perspectives in the generation of environmentally friendly chemical compounds with added value, clean energy conversion (non-petroleum energy), and minimizing the economic impact of environmental wastewater treatments. Thus, this work offers for the first time insights into the strengths, challenges, and prospects of electrochemical applications in the fields of energy and environmental remediation in Brazil, highlighting the country’s significance as a source of scientific knowledge on a global scale.