Potentiometry

电位法
  • 文章类型: Journal Article
    研究了尿苷-5'-二磷酸葡萄糖醛酸与铜(II)离子的二元体系。使用计算机数据分析进行了水溶液中的电位测定研究。优势的pH值,总体稳定常数(logβ),并确定了在研究系统中形成的每种配合物的形成反应平衡常数(logKe)。进行了光谱研究以确定所研究化合物中的配位模式。获得的化合物的细胞毒性和代谢活性测试表明,所测试的复合物对游离配体的生物活性增加。当前的研究可能有助于了解人体中发现的生物分子的复杂化合物,也可能有助于表征一组具有潜在抗癌特性的复杂化合物。
    A binary system of uridine-5\'-diphosphoglucuronic acid with copper (II) ions was studied. Potentiometric studies in aqueous solutions using computer data analysis were carried out. The pH of dominance, the overall stability constants (logβ), and the equilibrium constants of the formation reaction (logKe) were determined for each complex compound formed in the studied system. Spectroscopic studies were carried out to determine the mode of coordination in the compounds studied. Cytotoxicity and metabolic activity tests of the compounds obtained showed an increase in the biological activity of the complexes tested against the free ligand. The current research may contribute to the knowledge of complex compounds of biomolecules found in the human body and may also contribute to the characterization of a group of complex compounds with potential anticancer properties.
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  • 文章类型: Journal Article
    碳纳米材料被引入到这项研究中,作为用于单片电极的聚合物膜的改性剂,并以硝酸盐选择性传感器为例研究了它们的特性。石墨烯的使用,炭黑和碳纳米管显着提高电位响应,而没有观察到氧化还原反应。碳纳米材料的使用导致在宽线性范围(从10-1到10-6MNO3-)内对硝酸根离子的近Nernstian响应(54mV/pNO3-)。通过计时电位法和电化学阻抗谱获得的结果表明电阻很小,并且电容参数高达0.9mF(对于基于石墨烯的传感器)。电极的高电容量导致电位响应的良好稳定性和低电位漂移(0.065mV/h)。将碳纳米材料引入到多层膜中,而不是将它们用作单独的层,允许简化传感器的准备过程。使用单片电极,程序的一个步骤可以省略,与制备固体接触电极的程序相比。
    Carbon nanomaterials were introduced into this research as modifiers for polymeric membranes for single-piece electrodes, and their properties were studied for the case of nitrate-selective sensors. The use of graphene, carbon black and carbon nanotubes is shown to significantly improve the potentiometric response, while no redox response was observed. The use of carbon nanomaterials results in a near-Nernstian response (54 mV/pNO3-) towards nitrate ions over a wide linear range (from 10-1 to 10-6 M NO3-). The results obtained by chronopotentiometry and electrochemical impedance spectroscopy reveal little resistance, and the capacitance parameter is as high as 0.9 mF (for graphene-based sensor). The high electrical capacity of electrodes results in the good stability of the potentiometric response and a low potential drift (0.065 mV/h). Introducing carbon nanomaterials into the polymetric membrane, instead of using them as separate layers, allows for the simplification of the sensors\' preparation procedure. With single-piece electrodes, one step of the procedure could be omitted, in comparison to the procedure for the preparation of solid-contact electrodes.
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  • 文章类型: Journal Article
    离子选择电极(ISE)在临床和环境分析领域具有广泛的应用。四氢呋喃(THF)是现代ISE制备中最常用的溶剂,配备离子选择膜(ISM)。直到现在,THF中杂质对基于离子选择性膜的ISE的电位不稳定性的影响可能与残留水或过氧化物的存在有关。为了解决这个问题,大多数文献推荐在用于制备电位膜之前再蒸馏THF。目前的研究表明,造成ISM中潜在不稳定性的实际THF杂质包括THF氧化产物,它含有羟基和可能的羰基,沸点高于200℃。密度泛函理论计算支持THF氧化化学反应的途径,因此,预测了不确定杂质的化学结构。提出了ISE潜在稳定性恶化的根本原因,因为这些杂质的显着亲水性会影响膜中离子传感组件的分配。从而增强膜组分从膜相的浸出。这一发现解释了为什么建议再蒸馏老化的THF。
    Ion-selective electrodes (ISEs) have widespread use in the fields of clinical and environmental analyses. Tetrahydrofuran (THF) is the most used solvent for the preparation of modern ISEs, equipped with ion-selective membranes (ISMs). Until now, the influence of impurities in THF toward potentiometric instability of ion-selective membrane based ISEs was probably associated with the presence of either residual water or peroxide. To address this issue, most literature recommends redistilling THF prior to use in the preparation of the potentiometric membranes. Current study reveals that the actual THF impurity that is responsible for potential instability in the ISM includes products from the oxidation of THF, which contains the hydroxyl group and possibly carbonyl group with a boiling point of above 200 °C. The density functional theory calculation supported pathway of the chemical reaction of THF oxidation, hence, the chemical structure of the uncertain impurities was predicted. The underlying reason for the deteriorating potential stability of the ISEs is proposed as the significant hydrophilicity of these impurities that affect the partitioning of the ion sensing components in the membrane, thus enhancing the leaching of the membrane components from the membrane phase. This finding explains why redistillation of aged THF is advised.
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  • 文章类型: Journal Article
    电位传感器系统的小型化和批量生产为分布式环境传感铺平了道路,身体测量和工业过程监测。喷墨印刷作为一种高度适应性和可扩展的生产技术而越来越受欢迎。本文提出了一种通过喷墨印刷制造柔性固体接触铵离子选择性电极的可扩展且低成本的路线。利用喷墨印刷的三聚氰胺插层石墨烯纳米片作为固体接触材料显着改善了电荷传输,同时避免有害的水层形成。研究了外部极化作为改善电极间再现性的一种手段:电极极化后E0值的标准偏差降低,响应的线性区域扩展到NH4Cl的10-1-10-6M范围,LOD降低到0.88±0.17μM。最后,我们已经表明,电极是足够的测量在一个复杂的真实的样品:铵浓度被确定在垃圾渗滤液的水,与参考方法的偏差小于4%。
    Miniaturization and mass-production of potentiometric sensor systems is paving the way towards distributed environmental sensing, on-body measurements and industrial process monitoring. Inkjet printing is gaining popularity as a highly adaptable and scalable production technique. Presented here is a scalable and low-cost route for flexible solid-contact ammonium ion-selective electrode fabrication by inkjet printing. Utilization of inkjet-printed melamine-intercalated graphene nanosheets as the solid-contact material significantly improved charge transport, while evading the detrimental water-layer formation. External polarization was investigated as a means of improving the inter-electrode reproducibility: the standard deviations of E0 values were reduced after electrode polarization, the linear region of the response was extended to the range 10-1-10-6 M of NH4Cl and LODs reduced to 0.88 ± 0.17 μM. Finally, we have shown that the electrodes are adequate for measurements in a complex real sample: ammonium concentration was determined in landfill leachate water, with less than 4 % deviation from the reference method.
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  • 文章类型: Journal Article
    在理想条件下,具有固定负管壁电荷的纳米管将拒绝阴离子和仅传输阳离子。由于许多提出的纳米流体装置在这种理想的阳离子选择渗透状态下进行了优化,知道产生理想反应的实验条件是很重要的。一个名为Ccrit的参数,接触溶液中的最高盐浓度仍然产生理想的阳离子选择性,是特别重要的。使用静电模型解释了对金纳米管的开创性电位研究,该模型指出,当接触盐溶液中的德拜长度等于管半径时,应该发生Ccrit。由于这个“双层重叠模型”(DLOM),将所有相同电荷的离子视为相同的点电荷,它预测所有相同电荷的阳离子应该产生相同的Ccrit。然而,从未研究过阳离子对金纳米管中Ccrit的影响。这种知识差距已经变得重要,因为最近对聚合物阳离子选择性渗透纳米孔膜的研究表明,DLOM对于所研究的每种阳离子都失败了。要解决此问题,我们对10nm直径的金纳米管膜的盐阳离子对Ccrit的影响进行了电位研究。研究的所有阳离子的Ccrit,在实验误差内,相同和相同,值由DLOM预测。DLOM对于金纳米管盛行但对于聚合物纳米孔失败的原因源于这两种膜的固定负电荷之间的化学差异。
    Under ideal conditions, nanotubes with a fixed negative tube-wall charge will reject anions and transport-only cations. Because many proposed nanofluidic devices are optimized in this ideally cation-permselective state, it is important to know the experimental conditions that produce ideal responses. A parameter called Ccrit, the highest salt concentration in a contacting solution that still produces ideal cation permselectivity, is of particular importance. Pioneering potentiometric studies on gold nanotubes were interpreted using an electrostatic model that states that Ccrit should occur when the Debye length in the contacting salt solution becomes equivalent to the tube radius. Since this \"double-layer overlap model\" (DLOM), treats all same-charge ions as identical point charges, it predicts that all same-charged cations should produce the same Ccrit. However, the effect of cation on Ccrit in gold nanotubes was never investigated. This knowledge gap has become important because recent studies with a polymeric cation-permselective nanopore membrane showed that DLOM failed for every cation studied. To resolve this issue, we conducted potentiometric studies on the effect of salt cation on Ccrit for a 10 nm diameter gold nanotube membrane. Ccrit for all cations studied were, within experimental error, the same and identical, with values predicted by DLOM. The reason DLOM prevailed for the gold nanotubes but failed for the polymeric nanopores stems from the chemical difference between the fixed negative charges of these two membranes.
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  • 文章类型: Journal Article
    PdRuO2/PVP纳米材料使用简单的方法合成,并使用先进的分析方法如TEM,XRD,XPS,元素测绘和扫描电镜。合成的PdRuO2/PVP纳米材料被用作电位传感器电极中的离子载体,并成功地适应了大量含水样品中的Cr3离子检测。PdRuO2/PVP传感器的几个实验参数,如电位行为,选择性,重复性,响应时间,pH值,滴定,并对实际样品中的回收率进行了调查。在1×10-6-1.0×10-1M的浓度范围内进行电位测定行为特征。进行了六次重复实验表明,测量结果没有偏差。PdRuO2/PVP电位传感器的检测限非常低,值为8.6×10-8M。电位测量表明,合成的PdRuO2/PVP离子载体在宽pH范围内检测Cr3非常有效。2.0-8.0,发现保质期超过1年。因此,发现合成的PdRuO2/PVP电极材料具有高选择性,稳定,适用于Cr3+检测。
    PdRuO2/PVP nanomaterial was synthesized using a straightforward method and characterized using advanced analytical methods such as TEM, XRD, XPS, elemental mapping and SEM. The synthesized PdRuO2/PVP nanomaterial was used as an ionophore in potentiometric sensor electrodes and successfully adapted to Cr3+ ion detection in a large number of aqueous samples. Several experimental parameters of the PdRuO2/PVP sensor such as potentiometric behavior, selectivity, repeatability, response time, pH, titration, and recovery in real samples were investigated. Potentiometric behavioral characteristics were performed in the concentration range 1 × 10-6-1.0 × 10-1 M. The repeated experiments performed six times showed that there was no deviation in the measurements. The limit of detection of the PdRuO2/PVP potentiometric sensor was very low with a value of 8.6 × 10-8 M. The potentiometric measurements showed that the synthesized PdRuO2/PVP ionophore was highly effective in detecting Cr3+ in a wide pH range of 2.0-8.0 and was found to have a shelf life of over 1 year. As a result, the synthesized PdRuO2/PVP electrode material was found to be highly selective, stable, and applicable for Cr3+ detection.
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  • 文章类型: Journal Article
    最近,儿童日常消费的一些产品,如谷物和糖果,一直在上升,这为确定可能存在的任何金属物质提供了令人信服的理由。监测某些金属的浓度,像镍一样,在这些产品是必要的,由于医疗问题,在人类经常食用。所以,在这项工作中,制备了一种新型的高选择性碳糊作为Ni(II)离子选择性传感器,并使用陶瓷镁铝尖晶石纳米颗粒作为离子载体和磷酸三甲苯酯(TOCP)作为增塑剂进行了研究。采用改进的共沉淀法合成尖晶石纳米粒子。X射线衍射,扫描电子显微镜与EDAX,透射电子显微镜,和BET表面积用于确定相组成,微观结构,毛孔大小,颗粒大小,和合成的纳米颗粒的表面积。发现尖晶石纳米颗粒具有立方晶系的纳米微晶尺寸,粒径范围为17.2至51.52nm,介孔性质(平均孔径=8.72nm),和大的表面积(61.75m2/g)。基于电位法检测,在5.0×10-8至1.0×10-2molL-1的浓度下,石墨碳作为基质:TOCP作为粘合剂:脊柱作为离子载体的组成比为67.3:30.0:2.7(wt%)。-1,LOD为5.0×10-8molL-1。对于Nernstian斜率,在pH2.0-7.0下测量为29.22±0.12mVdecade-1。该传感器在9周内表现出良好的可重复性和8s的快速响应。在许多干扰物中,Ni(II)离子具有良好的选择性。三-,di-,和一价阳离子。加标实际样品中的Ni(II)含量,包括可卡因,糖果,古柯,巧克力,碳酸饮料,谷物,和包裹,被测量。根据F和t检验数据,所获得的结果表明,拟议的电位滴定法与官方报告的ICP方法之间没有显着差异。除了利用方差分析统计分析,验证程序已经实施,结果超过了ICP-MS方法。
    Lately, children\'s daily consumption of some products, such as cereals and candies, has been rising, which provides a compelling rationale for determining any metallic substances that may be present. Monitoring the concentration of certain metals, like nickel, in these products is necessary due to medical issues in humans when consumed regularly. So, in this work, a novel and highly selective carbon paste as a Ni(II) ion-selective sensor was prepared and investigated using ceramic magnesium aluminum spinel nanoparticles as the ionophore and tritolyl phosphate (TOCP) as a plasticizer. A modified co-precipitation method was used to synthesize the spinel nanoparticles. X-ray diffraction, scanning electron microscope with EDAX, transmission electron microscope, and BET surface area were used to determine the phase composition, microstructure, pores size, particle size, and surface area of the synthesized nanoparticles. The spinel nanoparticle was found to have a nano crystallite size with a cubic crystal system, a particle size ranging from 17.2 to 51.52 nm, mesoporous nature (average pore size = 8.72 nm), and a large surface area (61.75 m2/g). The composition ratio of graphite carbon as a base: TOCP as binder: spinal as ionophore was 67.3:30.0:2.7 (wt%) based on potentiometric detections over concentrations from 5.0 × 10-8 to 1.0 × 10-2 mol L-1 with LOD of 5.0 × 10-8 mol L-1. A measurement of 29.22 ± 0.12 mV decade-1 over pH 2.0-7.0 was made for the Nernstian slope. This sensor demonstrated good repeatability over nine weeks and a rapid response of 8 s. A good selectivity was shown for Ni(II) ions across many interferents, tri-, di-, and monovalent cations. The Ni(II) content in spiked real samples, including cocaine, sweets, coca, chocolate, carbonated drinks, cereals, and packages, were measured. The results obtained indicated no significant difference between the proposed potentiometric method and the officially reported ICP method according to the F- and t-test data. In addition to utilizing ANOVA statistical analysis, validation procedures have been implemented, and the results exceed the ICP-MS methodology.
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  • 文章类型: Journal Article
    固体接触离子选择电极(SC-ISEs)具有易于小型化的优点,甚至芯片集成,携带方便,稳定性强,以及在复杂环境中更有利的检测。它们已广泛用于便携式,可穿戴,和智能检测设备,以及在环境领域的现场分析和及时监测,工业,和医学。本文对基于氧化还原电容和双层电容SC-ISEs的传感器的组成进行了全面的综述,以及固体接触(SC)层中的离子-电子转导机制,特别关注过去三年(自2021年以来)提出的优化SC-ISE绩效的战略。这些策略包括构建离子选择性膜,SC层,和导电基板。最后,并对该领域未来的研究方向和可能性进行了探讨和展望。
    Solid-contact ion-selective electrodes (SC-ISEs) have the advantages of easy miniaturization, even chip integration, easy carrying, strong stability, and more favorable detection in complex environments. They have been widely used in conjunction with portable, wearable, and intelligent detection devices, as well as in on-site analysis and timely monitoring in the fields of environment, industry, and medicine. This article provides a comprehensive review of the composition of sensors based on redox capacitive and double-layer capacitive SC-ISEs, as well as the ion-electron transduction mechanisms in the solid-contact (SC) layer, particularly focusing on strategies proposed in the past three years (since 2021) for optimizing the performance of SC-ISEs. These strategies include the construction of ion-selective membranes, SC layer, and conductive substrates. Finally, the future research direction and possibilities in this field are discussed and prospected.
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  • 文章类型: Journal Article
    痕量铁的定量在各个领域都非常重要。在工业部门,监测铁的腐蚀释放是至关重要的,酸洗处理,和钢铁制造业,以应对潜在的环境和经济挑战。在生物系统中,尽管它不可或缺,必须将铁浓度保持在特定阈值以下。电化学(EC)方法由于其简单性而提供了显着的分析能力,易用性,和成本效益。本文综述了EC铁检测方法的基本原理,包括电位计,安培法,库仑法,伏安法,和电化学阻抗谱(EIS)。它进一步解释了获得校准曲线的过程,随后,确定未知离子的浓度。此外,介绍了选择初始信号值的技术说明,减少测试的持续时间,不包括非法拉第信号,并扩展具有最低检测限的线性区域。这些说明得到了相关案例研究的关键发现的支持。
    Quantification of trace amounts of iron is of great importance in various fields. In the industrial sector, it is crucial to monitor the release of iron out of corrosion, pickling treatment, and steel manufacturing to address potential environmental and economic challenges. In biological systems, despite its indispensability, it is essential to maintain iron concentration below a specific threshold. Electrochemical (EC) methods provide significant analytical capabilities due to their simplicity, ease of use, and cost-effectiveness. This review focuses on the fundamental principles of EC methods for iron detection, including potentiometry, amperometry, coulometry, voltammetry, and electrochemical impedance spectroscopy (EIS). It further explains the process of obtaining calibration curves, and subsequently, determining the concentration of unknown ions. Additionally, technical notes are presented on selecting the initial signal value, reducing the duration of tests, excluding non-faradaic signals, and extending the linear region with the lowest detection limit. These notes are supported by key findings from relevant case studies.
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  • 文章类型: Journal Article
    氟,取决于它的浓度和化学形式,对人类和动物是必需的或有毒的。因此,能够可靠地确定它是至关重要的。在这项研究中,用HCl(胃液模拟)提取后测定动物饲料中的氟。采用了氟化物选择电极(ISE)的标准电位法和新开发的高分辨率连续源石墨炉分子吸收光谱法(HR-CSGFMAS)。饲料样品被证明是HR-CSGFMAS的挑战。化学干扰(竞争分子的形成,CaF,GaCl,和GaP,而不是目标GaF分子)和光谱效应(包括磷分子光谱和原子线)被鉴定。试剂污染F和记忆效应引起了额外的困难。困难被消除/减少。对ISE分析的质量进行了多方向验证(包括全面的能力测试)。在低F浓度下存在不准确的风险,其中校准关系是非线性的,被调查。两种方法的结果一致,这证实了方法的准确性,并告知提取的氟是氟化物形式。2021-2023年在波兰进行的广泛的ISE测试结果表明,在大多数情况下,氟含量明显低于阈值。
    Fluorine, depending on its concentration and chemical form, is essential or toxic to humans and animals. Therefore, it is crucial to be able to determine it reliably. In this study, fluorine was determined in animal feed after extraction with HCl (gastric juice simulation). The standard potentiometric method with a fluoride-selective electrode (ISE) and newly developed high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GFMAS) method was applied. Feed samples turned out to be a challenge for HR-CS GFMAS. Chemical interferences (formation of competing molecules, CaF, GaCl, and GaP, instead of the target GaF molecule) and spectral effects (including a phosphorous molecule spectrum and atomic lines) were identified. An additional difficulty was caused by reagent contamination with F and memory effects. Difficulties were eliminated/reduced. The quality of ISE analysis was multi-directionally verified (including comprehensive proficiency testing). A risk of inaccuracy at low F concentration, where the calibration relationship is nonlinear, was investigated. The results of both methods were consistent, which confirms the accuracy of the methods and informs that the extracted fluorine is in fluoride form. The results of extensive ISE tests conducted in Poland in 2021-2023 have shown that, in most cases, the fluoride content is significantly lower than the threshold values.
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