Analytical Chemistry Commons^™

The Development Of Novel Carbohydrate-Based Gelators And Their Applications As Advanced Soft Materials, Joedian Morris

Chemistry & Biochemistry Theses & Dissertations

Low molecular weight gelators (LMWGs) are attractive molecules that have been explored extensively due to their practical applications in many disciplines. These small molecules self-assemble forming solid-like gels via three-dimensional cross-linked networks with the solvent as the key component within the matrix. Carbohydrate-based LMWGs are small molecules that can form solid-like gels in water, organic solvents, and aqueous solutions. They have great potential to be utilized in different applications because carbohydrates are biocompatible and can be made from easily accessible and renewable resources. Designing gelators is still a challenge within the field, even though researchers have developed tools to predict …

Electrochemical Surface-Enhanced Raman Spectroscopic Studies On Nickel Ultramicroelectrode, Li-Wen Wu, Wei Wang, Yi-Fan Huang

Journal of Electrochemistry

Nickel (Ni) electrodes are widely used in electrochemical researches. Understanding electrochemical processes on Ni electrodes through in-situ characterization of adsorbed species on their surfaces is helpful for rational optimization and application of Ni electrochemistry. Microelectrochemical surface-enhanced Raman spectroscopy (μEC-SERS) combines the mass transfer feature of ultramicroelectrode with high-sensitivity characterizations of molecular structures, which is a powerful method for studying Ni electrochemistry on polarization and non-equilibrium conditions. The key point of performing μEC-SERS is to make a SERS-active Ni ultramicroelectrode.
Here, we demonstrate a method of preparing a SERS-active Ni ultramicroelectrode through electrochemical deposition of several atomic layers of …

Valorization Of Xylan In Agroforestry Waste Streams, Harrison Appiah

Graduate Theses, Dissertations, and Problem Reports (ETD)

Valorization of Xylan in Agroforestry Waste Streams.

Harrison Appiah

Microwave-assisted deep eutectic solvent and gamma-valerolactone metallic chloride catalyzed conversion of xylan to furfural were investigated using a 2x3 factorial experimental design at two levels of percent microwave power, reaction time, and catalyst concentration. The levels of each factor studied were (20%, 60% microwave power, 2, 4 minutes, and 10, 20mg) respectively. The effect of three metallic chloride catalysts (LiCl, FeCl3.6H20, CuCl2) on the conversion of xylan to furfural was also investigated. The gamma-valerolactone-ferric chloride sent system exhibited the highest mean yield of furfural (56.50%). The next highest furfural yield of …

Synthesis And Raman Study Of Hollow Core-Shell Ni1.2Co0.8P@N-C As An Anode Material For Sodium-Ion Batteries, Jia-Hui Chen, Xiao-Bin Zhong, Chao He, Xiao-Xiao Wang, Qing-Chi Xu, Jian-Feng Li

Journal of Electrochemistry

With the increasing demand for large-scale energy storage, great progress has been made in discovering new advanced energy storage materials. Sodium-ion batteries (SIBs) have attracted much attention in recent years due to their use of abundant sodium resources and their comparable electrochemical capacity to lithium-ion batteries (LIBs). In this paper, we developed novel hollow core-shell Ni-Co bimetallic phosphide nanocubes with N-doped carbon coatings (Ni_1.2Co_0.8P@N-C) as the anode material for SIBs. The material was synthesized through a low-temperature phosphorization method using resorcinol formaldehyde (RF) resin coating with a Ni-Co Prussian blue analogue (PBA) as a template and …

Ordered Mesoporous Carbon/Graphene/Nickel Foam For Flexible Dopamine Detection With Ultrahigh Sensitivity And Selectivity, Lai-Yu Wang, Xin Xi, Dong-Qing Wu, Xiong-Yu Liu, Wei Ji, Rui-Li Liu

Journal of Electrochemistry

Electro-catalytic reduction is an efficient way to achieve resourcable transformation of CO₂, which is one of the important techniques to solve the global environmental problems originated from excessive CO₂ emission. In this study, a membrane electrode assembly(MEA) type CO₂ electro-reduction electrolytic cell was constucted, which enables CO₂ feeding and real-time KHCO₃ aqueous updating on both sides of the cathode gas diffusion electrode (GDE). By means of the electrolytic cell, effects of KHCO₃ concentration and updating inside the liquid electrolytic chamber on CO₂ electro-reduction activity, production distribution and stability were investigated. The experimental …

Effect Of Post-Consumer Content And Bioplastic Incorporation On Polymeric Resin In Consumer Applications, Shelby Bicknell

Electronic Theses & Dissertations

Controversy surrounds the use of plastic products, primarily due to their potentially negative impact on the environment at the end of their lifecycle. The most widely used plastics are manufactured from petrochemicals such as petroleum, coal or natural gas. Petrochemical plastics are not able to readily breakdown in the environment, which aggravates the existing pollution problems. Fortunately, there are eco-friendly alternatives to petrochemical-based plastics. Bioplastics may be derived from renewable sources, biodegradable, or both. Bio-based plastics are plastics that may be derived from renewable biomass sources including, but not limited to, vegetable oils, cornstarch, straw, woodchips, and food waste. They …

Interfaces In Lead-Free Tin Perovskite Photovoltaics: An Investigation Of Energetics, Ion Mobility, Surface Modification, And Performance, Alex Boehm

Theses and Dissertations--Chemistry

Halide perovskites have generated tremendous interest as low-cost semiconductors for optoelectronics, such as photovoltaics, lasers, and light emitting diodes due to their extraordinary optical and transport properties. Perovskite photovoltaics in particular have demonstrated a meteoric rise in power conversion efficiencies and drawn considerable interest as a next-generation solar energy technology. The rapid development has centered around lead-based derivatives, and concerns regarding the toxicity of lead has sparked interest in low toxicity and more environmentally friendly perovskite derivatives. In this regime tin (Sn) is regarded as a prominent alternative owing to the ideal bandgap and reduced toxicity exhibited by Sn-halide perovskites. …

Transient Electrochemical Surface-Enhanced Raman Spectroscopic Study In Electrochemical Reduction Of P-Nitrothiophenol, Yun Ling, Jing Tang, Guo-Kun Liu, Cheng Zong

Journal of Electrochemistry

P-nitrothiophenol (PNTP) is one of the most common probe molecules studied by surface-enhanced Raman spectroscopy (SERS). The research in electrochemical reduction behavior of PNTP will help understanding the mechanism for the nitrobenzene reduction. In this paper, we used transient electrochemical surface-enhanced Raman spectroscopy (TEC-SERS) to study the SERS of PNTP with cyclic voltammetry and chronoamperometry on gold electrodes. The results show that the TEC-SERS provide a time resolution that equals the transient electrochemical methods, and we concluded that the reaction was so quick that we did not observe the spectral information of intermediate species described in the literatures with a …

Electrochemical Sensor Based On Magnetic Electrode Modified With Magnetic Molecularly Imprinted Nanoparticles Immobilized Hemoglobin For Determination Of Hydrogen Peroxide, Yang Yuan, Jia-Xin Wang, Yu-Hua Cao

Journal of Electrochemistry

In this work, the surface-imprinted technique was used to prepare magnetic hemoglobin (Hb) imprinted nanoparticles, using Fe₃O₄@SiO₂ NPs as the carrier, Hb as the template molecule, and tetraethyl orthosilicate (TEOS) as the imprinted polymer monomer. The nanoparticles had a core-shell structure, with magnetic Fe₃O₄ NPs as the core and Hb imprinted polymers as the shell. Therefore, Hb could be concentrated and fixed on the surface of the magnetic imprinted nanoparticles (MMIPs NPs). Furthermore, MMIPs NPs were immobilized with chitosan (CS) on the surface of a magnetic electrode to constitute Hb enzyme-like biosensor …

Quantitative Detection Of Levofloxacin Hydrochloride By Differential Pulse Stripping Voltammetry With Electrodeposited Bismuth Film Electrodes, Zi-Ying Guo, Zuo-Peng Li, Jiang Li, Jian-Guo Zhao, Feng Feng

Journal of Electrochemistry

In this study, differential pulse stripping voltammetry was developed for the quantitative detection of levofloxacin hydrochloride indirectly. Levofloxacin hydrochloride contains organic amine, which can be precipitated upon interaction with Zn(SCN)₄^2-. By means of differential pulse stripping voltammetry, the concentration of Zn²⁺ can be determined using an in-situ formed bismuth film electrode, which allows determining indirectly the amount of levofloxacine hydrochloride. The linearity equation, I = 1.1401c - 0.5309 with the correlative coefficient R = 0.9979, was presented in the experiment. The results showed that this approach is very sensitive, having a limitation of detection of 3.18 …

Electrochemical Detection Of 4-Nitrophenol Based On Glassy Carbon Electrode Modified By Tio2Nps/Rgo Composite, Lin-Na Jiu, Yong-Qiang Cheng

Journal of Electrochemistry

4-nitrophenol (4-NP) has become factitious pollution, and presented a serious threat to the nature and human health. It is necessary to develop a convenient and fast detection method. In this work, the glassy carbon electrode modified by titanium dioxide nanoparticles (TiO₂NPs)/reduced graphene oxide (RGO) composite as an electrochemical sensor was studied for the trace detection of 4-NP. The morphology of the composite was characterized by scanning electron microscopy (SEM). The homogeneous mixing of titanium dioxide nanoparticles and reduced graphene oxide increased the specific surface area of the composite, and facilitated the electrochemical reaction of 4-NP. The electrochemical characteristics …

In Situ/Operando Visualization Of Electrode Processes In Lithium-Sulfur Batteries: A Review, Shuang-Yan Lang, Xin-Cheng Hu, Rui Wen, Li-Jun Wan

Journal of Electrochemistry

Lithium-sulfur (Li-S) batteries have been regarded as one of the most promising candidates for the next-generation energy storage devices. Fundamental understanding of the structure and evolution processes at electrode-electrolyte interfaces is essential to the further development. In this review, we summarize recent advances in the interfacial observations by means of various in situ/operando visualization techniques, including scanning probe microscopy (SPM), electron microscopy (EM), X-ray microscopy (XRM) and optical microscopy (OM). The real-time investigation provides important evidence for the morphology and component changes including S/Li₂S transformation, polysulfide dissolution on cathodes and Li/solid electrolyte interphase (SEI) evolution on anodes, which …

Recent Progress Of Electrochemiluminescence Sensors Based On Electrically Heated Electrode, Hui-Fang Zhang, Yi-Ting Chen, Fang Luo, Zhen-Yu Lin, Guo-Nan Chen

Journal of Electrochemistry

Electrochemiluminescence (ECL) has broad application in the fields of environmental monitoring and biological analysis due to its intrinsic advantages such as excellent versatility, good detection sensitivity, and high specificity. The intensity of ECL can be influenced by temperature variation in the ECL quantum efficiency and the rate of electrochemical reaction. However, traditional temperature control is commonly realized through bulk solutions heating, which is complicated and unfavorable for detection when the volatile and thermally unstable materials existed. In order to address these problems, electrically heated electrodes are used to adjust the temperature desired. The major character of this technique lies in …

A Facile Strategy For Two-Step Fabrication Of Gold Nanoelectrode For In Vivo Dopamine Detection, Li-Hao Guan, Chao Wang, Wang Zhang, Yu-Lu Cai, Kai Li, Yu-Qing Lin

Journal of Electrochemistry

In vivo monitoring neurochemicals with microelectrode is invasive and the damage to brain tissue may inevitably cause disturbance signals physiologically to the measurement. It is of great importance to reduce the electrode size and to decrease the damage. This study demonstrates a novel nanoelectrode preparation methodology for in vivo monitoring dopamine (DA) fluctuation in the living brain of rats with high dependability. The fabrication process of the gold nanoelectrode involving a few minutes consists of only two steps: 1) growing gold nanoseeds on surface of tip of glassy capillary by ion sputtering; 2) wet depositing a continuous conductive gold film …

Graphene-Like Secondary-Laser-Etched Polyimide Film Decorated With CuXO Nanocomposites: A Novel Electrode Substrate For Non-Enzymatic Glucose Sensors, Wan-Lin Dai, Zhi-Wei Lu, Jian-Shan Ye

Journal of Electrochemistry

In this work, a novel electrode substrate with graphene-like surface and Cu_xO nanocomposites derived from secondary-laser-etched polyimide (SLEPI) film was synthesized and applied in non-enzymatic glucose detection for the first time. Characterizations indicate that the as-prepared SLEPI/Cu_xO film electrode (SLEPI/Cu_xO-FE) possessed huge surface area, plentiful active sites and excellent electrocatalytic performance. The obtained sensor exhibited the high sensitivity and selectivity for glucose determination with a linear range of 0.05 mmol·L^-1 to 3 mmol·L^-1 and a detection limit of 1.72 μmol·L^-1 (S/N=3), which provides a simple, flexible and low-cost electrochemical sensor for …

A Dual Nanostructured Approach To Sers Amenable To Large-Scale Production, Kory Brian Castro

Chemistry & Biochemistry Theses & Dissertations

A SERS device was made using a dual-nanostructured surface comprised of silver nanoparticle and silver nanowires. The ability of each nanostructure to produce a uniform surface was characterized and the surface-enhanced Raman scattering (SERS) response of the resulting surfaces were examined using the reporter molecule 4-aminothiolphenol (ATP) and a 638 nm excitation laser.

A synthetic method was developed to produce silver nanowires with lengths of ~20 μm and diameters of ~100 nm with a narrow size distribution. The method utilized a simple, one-pot synthesis that is amenable to large-scale production. A selective precipitation method was used to the isolate the …

The Pilot Application Of Electrochemical Impedance Spectroscopy On Dynamic Proton Exchange Membrane Fuel Cell, Jian-Wei Guo, Jian-Long Wang

Journal of Electrochemistry

By analyzing Electrochemical Impedance Spectroscopy (EIS) in applications of dynamic proton exchange membrane fuel cell (PEMFC), bottlenecks which restrict EIS tool development have been pointed out in this paper. Though the high-frequency resistance in EIS is largely accepted as cell inner-resistance, this can only be applied for cell with low current. The low-frequency resistance is difficult to be realized due to its relation with mass transfer. Furthermore, the improved Randles equivalent circuits are built up preliminarily, thus, penetrating into studies for mass transfer reaction, cell operation/degeneration, and high temperature fuel cell. Inspiringly, EIS is becoming an analyzing tool for stack …

Synthesis Of Keggin Polyoxometalates Modified Carbon Paste Electrode As A Sensor For Dopamine Detection, Peng-Fei Dong, Na Li, Hai-Yan Zhao, Min Cui, Cong Zhang, Ju-Jie Ren, Xue-Ping Ji

Journal of Electrochemistry

Polyoxometalates, a class of anionic clusters with structure diversity and size variability, make them very attractive in many fields such as electrochemistry, catalysis and medicine. The Co(C₁₅N₆H₁₂)₂[PW₁₂O₃₈]·5H₂O(Co[PW₁₂O₃₈]) modified carbon paste electrode was prepared in this work, and its electrochemical performances as the sensor for dopamine detection were characterized with electrochemical impedance spectroscopy, cyclic voltammetry and differential pulse voltammetry. The preparation conditions and test conditions were optimized respectively. Under the optimized conditions, the POMs modified carbon paste electrode exhibited good selectivity and sensitivity …

Photocatalytic Activity: Experimental Features To Report In Heterogeneous Photocatalysis, Md. Ariful Hoque, Marcelo I. Guzman

Chemistry Faculty Publications

Heterogeneous photocatalysis is a prominent area of research with major applications in solar energy conversion, air pollution mitigation, and removal of contaminants from water. A large number of scientific papers related to the photocatalysis field and its environmental applications are published in different journals specializing in materials and nanomaterials. However, many problems exist in the conception of papers by authors unfamiliar with standard characterization methods of photocatalysts as well as with the procedures needed to determine photocatalytic activities based on the determination of “apparent quantum efficiencies” within a wavelength interval or “apparent quantum yields” in the case of using monochromatic …

Carbon Composite Fe3O4 Nanoparticles Based Electrochemical Sensor For Hydrogen Peroxide Detection, Si-Yu Zhang, Hui-Juan Wang, Shu-Fang Li, Jian-Ying Qu

Journal of Electrochemistry

In this work, a novel hydrogen peroxide electrochemical sensor was constructed with ferroferric oxide (Fe₃O₄) magnetic nanoparticles, which demonstrated good electrocatalytic activity for hydrogen peroxide. There existed a good linear relationship between the concentration of hydrogen peroxide and the oxidation peak current in the range of 1.00 × 10^-6 ~ 1.00 × 10^-3 mol·L^-1 (R = 0.9980) with the detection limit of 6.60 × 10-7 mol·L^-1. The sensor exhibited good anti-interference ability, high reproducibility and stability.

Simulation Analysis In Dynamic Performance Of Proton Exchange Membrane Fuel Cell Under Starting Condition, Yan Xiao, Ying-Jie Chang, Wei Zhang, Qiu-Hong Jia

Journal of Electrochemistry

Based on the equivalent circuit model, by considering both the dynamic gas pressure model and the dynamic heat transfer model, a lumped parameter model is developed. The start process of the fuel cell is simulated by using SIMULINK software. The undershoot of the voltage is observed from the simulation results, and the response time of the voltage is basically the same as that of the fuel cell temperature, which indicates that the temperature has great influence on the dynamic performance of the fuel cell. From the perspective of the temperature, the dynamic responses of the thermodynamic potential, the activation overvoltage, …

Technology Development For Detection Of Circulating Disease Biomarkers From Liquid Biopsies Using Multifunctional Nanomaterials, Mustafa Balcioglu

Legacy Theses & Dissertations (2009 - 2024)

Despite the advance health care, devastating health conditions such as cancer and infectious diseases that affect populations worldwide are too often not diagnosed until morbid symptoms become apparent in the late phase. Obtaining an early and accurate diagnosis that reveal a hidden lethal threat before the disease becomes complicated may dramatically reduce the severity of its impact on the patient’s life and increase the probability of survival. For example, in the case of ovarian cancer, which is the fifth most common malignancy and the fifth leading cause of cancer mortality in women in the US, the 5-year relative survival is …

Interfacial Corrosion Of Copper And The Formation Of Copper Hydroxychloride, Mary Teague, Shengxi Li, Hongbo Cong

Williams Honors College, Honors Research Projects

Electrical circuitry is an industry, among many others, heavily using the element of copper. Ensuring the mechanical integrity of Cu is crucial, especially in salt environments, for the multifaceted composition of circuits. 4N NaCl solution (equilibrium concentration in ~84% RH) simulated this three-phase system. Rectangular Cu samples were partially immersed in both ambient and continuous lab air sparging atmospheres to understand waterline corrosion of the metal. Open circuit potentials (OCP) were continuously taken during the immersion testing for a maximum of 5 days. A scanning electron microscopy (SEM) equipped with an energy dispersive X-ray spectrometer (EDS), Raman spectroscopy, and 3-D …

Plasmon-Enhanced Optical Sensing By Engineering Metallic Nanostructures, Peng Zheng

Graduate Theses, Dissertations, and Problem Reports (ETD)

The world’s booming population projected to reach 10 billion by 2050 causes enormous stresses on environmental safety, food supply, and healthcare, which in return threatens human civilizations. One of the most promising solutions lies at innovating point-of-care (POC) sensing technologies to conduct detection of environmental hazards, monitoring of food safety, and early diagnosis of diseases in a timely and accurate manner. The discovery of surface-enhanced spectroscopy in the 1970s has significantly stimulated research on light-matter interaction which gives rise to enhanced optical phenomena such as surface-enhanced Raman scattering (SERS), plasmon-enhanced fluorescence (PEF), and particularly, they have found enormous applications in …

Capacity Fading Analyses Of Lini0.5Co0.2Mn0.3O2And Lini0.5Co0.2Mn0.3O2/Lifepo4 Cathode Materials For Lithium-Ion Battery, Yi Hu, Xiang-Zhu He, Zhong-De Deng, Ling-Yong Kong, Wei-Li Shang

Journal of Electrochemistry

The LiNi _0.5Co _0.2Mn _0.3O₂/LiFePO₄ (NMC532/LFP) composite cathode material for lithium-ion battery was prepared by wet ball-milling. The capacity fading behaviors of LiNi _0.5Co _0.2Mn _0.3O₂ (NMC532) and LiNi _0.5Co _0.2Mn _0.3O₂/LiFePO₄ (NMC532/LFP) were analyzed by X-ray diffraction (XRD), scanning electron microscope (SEM), charge/discharge and electrochemical impedance spectroscopy (EIS) tests. The results indicated that the capacity retention values of NMC532/LFP were 97.80% and 86.48%, respectively, after 50 cycles and 60℃ high temperature storage. The NMC532/LFP exhibited better cycle performance and high temperature storage performance. …

Direct Electrochemistry Of Glucose Oxidase Based On Ws2 Quantum Dots And Its Biosensing Application, Chen-Lu Li, Hua-Ping Peng, Zhong-Nan Huang, Yi-Lun Sheng, Pei-Wen Wu, Xin-Hua Lin

Journal of Electrochemistry

In this study, a novel electrochemical glucose biosensor has been developed by immobilizing glucose oxidase (GOx) on tungsten disulfide quantum dots (WS₂ QDs) on the surface of glassy carbon electrode (GCE). Transmission electron microscopy, UV-vis spectroscopy and cyclic voltammetry were employed to characterize the morphology, structure, and electrochemical behaviors of the as-prepared WS₂ QDs and the biofilm modified electrode. The results suggested that the WS₂ QDs could accelerate the electron transfer between the electrode and the immobilized enzyme, which enabled the direct electrochemistry of GOx without any electron mediator. Besides, the immobilized GOx in WS₂ QDsfilm …

Application Of Adamantane Schiff Base Nickel Complexes/Graphene Oxide/Glassy Carbon Modified Electrode In Detection Of Carmine, Peng Guo, Zheng Liu, Hai-Ying Li, Li-Ming Ma

Journal of Electrochemistry

The Schiff base nickel complexes/graphene oxide/glassy carbon electrodes were prepared by embedded method and electrodeposition on which were used to quantitatively detect the contents of carmine. Cyclic voltammetry, chronoamperometry, scanning electron microscopy (SEM) and other methods were employed to characterize properties and morphologies of the modified electrodes. The results show that the adamantane double Schiff base nickel complexes/graphene oxide/glassy carbon electrode had high electric catalytic activity toward carmine oxidation reaction, and might provide an easy and quick way to detect carmine content with good reproducibility.

Stm Investigation Of Oxygen Reduction Reaction On Solid Interface In Fuel Cell, Zhen-Feng Cai, Bing Sun, Wen-Jie Jiang, Ting Chen, Dong Wang, Li-Jun Wan

Journal of Electrochemistry

An electrocatalyst for oxygen reduction reaction (ORR) is an important component for fuel cells. An investigation at interfacial electrochemical reactions toward ORR at a molecular scale benefits mechanistic understanding as well as rational design of catalysts. Scanning tunneling microscopy (STM) has been proven to be a powerful tool to monitor chemical reactions and to provide in-situ information about the interfacial electrochemical reactions at a molecular level. This review summarizes the recent STM studies in monitoring the interface processes such as morphological changes, molecular changes, reaction intermediates, and oxidation products. The prospects of future development in this field are outlined.

Synthesis Of Ultrathin Co3O4 Nanoflakes Film Material For Electrochemical Sensing, Hui-Juan Wang

Journal of Electrochemistry

Ultrathin cobalt oxide (Co₃O₄) nanoflakes film material was synthesized by using an electro-deposited cobalt layer as a raw material through a simple oxidation method and followed by a heat treatment at 350 ^oC. The physical characterizations of the Co₃O₄ nanoflakes film were performed by scanning electron microscopy (SEM), X-ray diffraction (XRD) and transmission electron microscopy (TEM) technologies, and the electrochemical activity was measured by cyclic voltammetry (CV). As a promising material for electrochemical sensing, the as-synthesized ultrathin Co₃O₄ nanoflakes film material exhibited excellent electrochemical activity for H₂O …

The Study Of Dynamical Electrochemical Impedance Spectroscopy For Oxygen Reduction Reaction On Pt/C Catalyst, Kun-Ming Shi, Jian-Wei Guo, Jia Wang

Journal of Electrochemistry

With joint techniques of rotating disc electrode(RDE) and electrochemical impedance spectroscopy(EIS), and further establishment on equivalent circuit model, this paper studied oxygen reduction reaction(ORR) on commercial Pt/C catalyst in acid medium. Our results found that the dynamical interface on Pt/C consists of two independent processes: 1) the PtO reduction from Pt surface, 2) the new PtO formation from ORR, thus providing key clues for catalyst stability and activity. This also implied that the dynamical interface facilitates reconstruction for porous electrode, and matches with mass transfer. One important issue is discovered that at high overpotential, the high reaction rate for ORR …