Analytical Chemistry Commons^™

Phenomena Characterization Of Energy Materials By X-Ray Absorption Spectroscopy, Ming-Yao Cheng, Chun-Jen Pan, Ju-Hsiang Cheng, Bing-Joe Hwang

Journal of Electrochemistry

The aim of this review is to introduce the characterization of energy materials by X-ray absorption spectroscopy (XAS) . This technique allows us to probe changes in the valance state and the local environment of the targeted element in the active material; thereby,leading to a better understanding of its electrochemical behavior,and hopefully showing the way to improved performance. Here,electrocatalysts for fuel cells and active electrode materials for Li-ion batteries are taken as the examples that illustrate the capability of XAS and allow observation and theory to be correlated with electrochemical phenomena.

Electrochemical Sers Studies On The Adsorption Of Benzoimidazole And Derivative In Nonaqueous Solution, Ya-Xian Yuan, Feng-Zhu Yang, Wei Liu, Ping-Jie Wei, Jian-Lin Yao, Ren-Ao Gu

Journal of Electrochemistry

The surface adsorption of benzoimidazole (BIMH) and 2-mercaptobenzimidazole(MBI) was investigated by electrochemical in-situ surface enhanced Raman spectroscopy (SERS) and direct electrochemical synthesis on Cu electrode. The influence of the neutral ligand of triphenylphosphine (pph₃) on the adsorption and surface coordination of BIMH and MBI were investigated respectively. BIMH interacted with metal surface by the neutral molecule to form chemical adlayer in the extremely negative potential,while it adsorbed onto metal surface through the N atoms to form a polymer film which may suppress the corrosion of the metal. The introduction of pph₃ destroyed the film formation of BIMH …

Comparative Study Of Nanoporous Pt, Ptru And Ptruir Catalysts Using Electrochemical Ftir Spectroscopy, M. Amussen Robert, Holt-Hindle Peter, Nigro Samantha, Aicheng Chen

Journal of Electrochemistry

In recent years much effort has been put towards developing efficient Pt-based electrocatalysts for applications in fuel cells. With the rising cost of precious metals such as Pt,the need to enhance the activity and to decrease the load of catalysts is prominent. Herein we report on the synthesis and comparative study of nanoporous Pt,PtRu and PtRuIr electrocatalysts. The nanoporous electrodes were fabricated using a hydrothermal method and characterized by scanning electron microscopy (SEM) ,energy dispersive spectroscopy (EDS) ,X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) . The electrocatalytic activity of the fabricated nanopo- rous materials was evaluated using both CO …

Electrochemical Surface-Enhanced Raman Spectroscopy—Current Status And Perspective, Bin Ren, Jian-Feng Li, Yi-Fan Huang, Zhi-Cong Zeng, Zhong-Qun Tian

Journal of Electrochemistry

Electrochemical interface is a very important interface closely related to various energy and life processes. Surface-enhanced Raman scattering was widely used in electrochemistry soon after its discovery to understand the surface bonding,configuration,and orientation of the surface species. In recent 10 years,the fast development of nanoscience and nanotechnology has offered SERS with abundant substrates and characterization methods,which has allowed impressive development of electrochemical SERS. This articles will follow the time line to make systematically overview of SERS on Au and Ag,thin-layer transition-metal SERS,pure transition metal SERS,core-shell SERS and those methods for studying single crystal surfaces,including gap-mode SERS, TERS and SHINERS. Emphasis …

Fabrication Of Electrochemically Activated Glassy Carbon/Bismuth Film Electrodes For Sensitive Analysis Of Pb(2+) And Cd(2+), Kang Shi, Wen-Jing Wang, Kun Hu

Journal of Electrochemistry

The application of electrochemically activated glassy carbon (GC) in the in-situ preparing of bismuth film electrodes (BiFEs) to analyze Pb^{2 +} and Cd^{2 +} was investigated. The glassy carbon electrodes were electrochemically activated by either potentiostic or cyclic polarization in 1 mol·L^-1 NaOH solution. Experimental results show that employment of HCl solution as the analytical solution not only can reproducibly renew the electrochemically activated GC electrode surface with an electrochemical clear procedure, but also can greatly enhance the sensitivity of BiFes method for analysis of Pb^{2 +} and Cd^{2 +}. The test range thus …

A Synthetic Biological Engineering Approach To Secretion- Based Recovery Of Polyhydroxyalkanoates And Other Cellular Products, Elisabeth Linton

All Graduate Theses and Dissertations, Spring 1920 to Summer 2023

The costs associated with cellular product recovery commonly account for as much as 80% of the total production expense. As a specific example, significant recovery costs limit commercial use of polyhydroxyalkanoates (PHA), which comprise a class of microbially-accumulated polyesters. PHAs are biodegradable compounds that are of interest as a sustainable alternative to petrochemically-derived plastics. Secretion-based recovery of PHAs was studied to decrease PHA production costs. Type I and II secretory pathways are commonly used for the translocation of recombinant proteins out of the cytoplasm of E. coli. Proteins were targeted for translocation using four signal peptides (HlyA, TorA, GeneIII, …

A New Green Chemistry Method Based On Plant Extracts To Synthesize Gold Nanoparticles, Milka Odemariz Montes Castillo

Open Access Theses & Dissertations

Extraordinary chemical and physical properties exhibited by nanomaterials, as compared to their bulk counterparts, have made the area of nanotechnology a growing realm in the past three decades. It is the nanoscale size (from 1 to 100 nm) and the morphologies of nanomaterials that provide several properties and applications not possible for the same material in the bulk. Magnetic and optical properties, as well as surface reactivity are highly dependent on the size and morphology of the nanomaterial. Diverse nanomaterials are being widely used in molecular diagnostics as well as in medicine, electronic and optical devices. Among the most studied …

Electrodeposition Of Tin Using Tin (Ii) Methanesulfonate From Mixture Of Ionic Liquid And Methane Sulfonic Acid., Yang Kok Kee

Student Works (2010-2019)

The electrodeposition of tin from Tin(II) Methane Sulfonate (MSA) with varying concentration in air and water stable 1-butyl-1-methyl-pyrrolidinium trifluoromethanesulfonate, (BMPOTF) ionic liquid at room temperature was studied. Cyclic Voltammetry served to characterize the electrochemical behavior of tin reduction and oxidation. The diffusion coefficient of stannous ions in the mixture of BMPOTF ionic liquid and MSA based electrolyte obtained via Randles-Sevcik and Cottrell equation was 2 × 10-7 cm2/s. Electroplating on copper panel was conducted under different current densities to determine BMPOTF based tin plating solution current efficiency. Mixture of BMPOTF and MSA based tin plating solution gave current efficiency as …

Cyclic Voltammetric And In-Situ Ftir Spectroscopic Studies Of Adsorption And Reduction Of No On Electrode Of Pt Nanoparticles, Qian Cheng, Yan-Xia Jiang, Dong-Mei Zeng, Shi-Gang Sun

Journal of Electrochemistry

Adsorption and reduction of NO on electrode of Pt nanoparticles in acid solutions were studied by means of cyclic voltammetry(CV) and in-situ FTIR spectroscopy.The results indicated that the reduction of NO is a complicated process including the adsorption of NO on electrode surface.Two types of surface-bonded NO were determined on Pt nanoparticles.The weakly adsorbed NO was reduced between 0.6 V and-0.05 V,which yielded nitrous oxide(N₂O) and ammonium(NH₄⁺) as products;while the strongly bonded NO was reduced at more negative potentials between-0.05V and-0.15V,producing only NH₄⁺ species.

Factors Affecting Redox Magnetohydrodynamics For Flow In Small Volumes, Matthew D. Gerner

Graduate Theses and Dissertations

Lab-on-a-chip technologies offer the possibility of developing analytical devices that are low-cost, portable, disposable, fast, and operable by non-technical personnel. Such devices require automated methods to manipulate ultra-small volumes (picoliters) of samples and solution, including pumping, stirring, and positioning. Current methods for ultra-small volume microfluidics have limitations that restrict their use including high voltage requirements, disadvantageous flow profiles or rates, and relatively complicated fabrication due to mechanical parts. Redox magnetohydrodyanmics (RMHD) that utilizes permanent magnets for portability shows promise as a micropump with ease of switching flow direction, no moving parts, compatibility with both aqueous and non-aqueous solutions, low voltages …

Electrochemical Properties Of Functionalized Carbon Nanotubes And Their Applications In Analysis Of 6-Mercaptopurine, Bao-Yi Lu, Yan-Yan Lai, Hong Li

Journal of Electrochemistry

The electrochemical behaviors and adsorption properties of single-walled carbon nanotubes such as SWNT,SWNT-COOH,and SWNT-OH and multi-walled carbon nanotubes including MWNT,MWNT-COOH,and MWNT-OH modified at a graphite electrode have been investigated by using [Fe(CN)₆]^3-anion and [Co(phen)₃]³⁺ cation.It was shown that shows good redox reversibility of [Fe(CN)₆]^3-/4-reactions on the existed carbon nanotubes(CNT) modified electrode.Based on the strong adsorptive property of [Co(phen)₃]³⁺ on the CNT surface,the [Co(phen)₃]³⁺/CNT modified graphite electrode can be obtained by progressive potential sweeping and developed to monitor quantitatively 6-mercaptopurine(6-MP).The adsorption capacity of …

Yttrium And Hydrogen Superstructure And Correlation Of Lattice Expansion And Proton Conductivity In The Bazr0.9y0.1o2.95 Proton Conductor, A. Braun, A. Ovalle, V. Pomjakushin, A. Cervellino, S. Erat, Wayne C. Stolte, T. Graule

Chemistry and Biochemistry Faculty Research

Bragg reflections in Y-resonant x-ray diffractograms of BaZr_0.9Y_0.1O_2.95 (BZY10) reveal that Y is organized in a superstructure. Comparison with neutron diffraction superstructure reflections in protonated/deuterated BZY10 suggests that both superstructures are linked, and that protons move in the landscape imposed by the Y. The thermal lattice expansion decreases abruptly for protonated BZY10 at T≥648±20 K, coinciding with the onset of lateral proton diffusion and suggesting a correlation of structural changes and proton conductivity. The chemical shift in the Y L₁-shell x-ray absorption spectra reveals a reduction from Y³⁺ toward Y²⁺ upon …

Corrosion Inhibition Of Self-Assembled Films On Iron By Electrochemical Impedance Spectroscopy, Yuan-Yuan Feng, Shen-Hao Chen, Juan-Juan Zhou, Wen-Juan Guo

Journal of Electrochemistry

The self-assembled films of tetradecylamine were formed on iron surface, and the inhibition ability of which for iron corrosion in 0.5 mol/L H₂SO₄ solutions was studied by electrochemical impedance spectroscopy technique. Results indicated that longer immersion time would result in stronger inhibition ability of the films. The maximal inhibition efficiency(IE) of the tetradecylamine films was 68.7%. When the tetradecylamine films were modified by dodecylthiol, the mixed films became denser and more stable, thus the inhibition ability increased remarkably. The η of the mixed films increased to 78.2%.

Cyclic Voltammetry And In Situ Ftir Studies Of Cyanide Adsorption On Nanostructured Au Film Electrode In Alkaline Solutions, Chun-Hua Zhen, Chun-Jie Fan, Shi-Gang Sun

Journal of Electrochemistry

The adsorption of cyanide(CN^-) on electrodes of nanometer scale thin film of gold supported on glassy carbon(nm-Au/GC) in alkaline solutions were investigated using cyclic voltammetry and in situ FTIR spectroscopy.It has revealed that the electrodeposited nanostructured Au thin film exhibited AIREs(abnormal infrared effects) for CN^-adsorption,which manifested 3 nonlinear IR spectral features: inversion of the direction of CN^-band,enhancement of IR absorption of adsorbed CN-species(about 39.2 folds) and increase in the FWHM(full width at half maximum) of CN^-band.

In Situ Measurement Of Chloride Concentration And Ph Distribution In The Crevice During The Crevice Corrosion Of Copper Electronic Board, Min Zhang, Xiang-Dong Zhuo, Chang-Jian Lin

Journal of Electrochemistry

Although the crevice corrosion of metals had been extensively studied in the past years,it remained lack of direct experimental information of the micro chemical environments and electrochemical conditions inside the corroding crevice.The distribution of chloride concentration and local pH in the occluded area are the most crucial factors in development of crevice corrosion.The array probes in one dimension of Ag/AgCl and IrO₂ array were developed in this work to in situ follow the distribution of chloride concentration and local pH in the occluded area during the crevice corrosion propagation.Based on a designed simulated crevice corrosion system in 0.5mol/L NaCl …

Improved High-Temperature Stability And Sun-Light-Driven Photocatalytic Activity Of Sulfur-Doped Anatase Tio2, Suresh Pillai, Declan Mccormack, Pradeepan Periyat, John Colreavy, Steve Hinder

Articles

No abstract provided.

Study On Electrochemical Impedance Spectroscopy Of Carbon Steel Eroded In Methyldiethanolamine Solution, Dong-Ping Wei, Rong-Zong Hu, Dan-Mei Pan, Wei-Xiong Huang, Rui Dong

Journal of Electrochemistry

Corrosion behavior of carbon steel in methyldiethanolamine(MDEA) solution was investigated by Electrochemical Impedance Spectroscopy(EIS).The results were showed that the corrosion rate of carbon steel in solution containing dissolved oxygen is higher than that in solution removed of dissolved oxygen before cathodic activation.They were reversed after cathodic activation.The corrosion rate is increased at first and then decreased when the concentration of MDEA is increased in the blank solutions.In the simulated solutions containing quantities of!heat-stable salts(HSS),the corrosion rate is decreased monotonously with increase of the MDEA concentration.As anodic polarization potential is increased,the EIS of carbon steel in HSS simulated solution showed characteristics …

Determination Of Tetracyclines Based On The Flow-Through Electrochemical Detection Cell With Nickel Electrode, Dan-Mei Pan, Rong-Zong Hu, Dong-Ping Wei, Hao-Dong Ding

Journal of Electrochemistry

The electrochemical responses to tetracycline at the nickel electrode in alkaline solution were compared with that of gold and glassy carbon electrode by voltammetry.The electrocatalytic oxidation characteristics of tetracycline at nickel electrode were discussed.Subsequently a flow-through amperometric detection cell with nickel as the working electrode was designed to detect tetracycline,oxytetracycline,and doxycycline.Standard calibration graphs for the tetracyclines yielded linear ranges of 0.1~15 mg/L.Detection limits(S/N=3)of 35,45 and 43 μg/L were obtained for tetracycline,oxytetracycline and doxycycline,respectively.The system was applied for the determination of the three antibiotics in single-component drug formulations.

Stm Tip-Induced Nanostructuring-Replacement Method To Construct Pt Surface Nanostructures, Jin-Gang Wang, Jing Tang, Zhao-Bin Chen, Bing-Wei Mao

Journal of Electrochemistry

STM tip-induced surface nanostructuring based on "Jump-to-contact" mechanism is a nanostructuring technique that has the highest resolution in aqueous solutions.However,for metals that have high cohesive energy,atoms would transfer from surface to tip instead,which limits the wide application of this technique.In this paper,we present a two-step Nanostructuring-Replacement method to construct metal nanoclusters that cannot be obtained directly via the "Jump-to-contact" mechanism.The method is demonstrated to construct Pt nanoclusters that are of great interest in catalysis and electrocatalysis but cannot be constructed via the "Jump-to-contact" mechanism.Since Cu is the most intensively studied and successful system in the tip-induced nanostructuring,it is utilized as …

Pre-Oxidative Amperometric Glucose Biosensor Incorporated With Carbon Nanotube And Pbo2, Hong-Lan Qi, Cheng-Xiao Zhang

Journal of Electrochemistry

A pre-oxidative amperometric glucose biosensor incorporated with carbon nanotube,ferrocenemonocarboxylic acid and PbO₂ was designed.The interferences coming from reduced substances,such as ascoribic acid and urine acid were eliminated by PbO₂.The oxidative current is linear at the potential of +0.40 V(vs.SCE) to the concentration of glucose in the range from 0.50 to 20 mmol·L^-1,and the detection limit of glucose is 0.1 mol L^-1.The relative standard deviation is 3.3% for seven successive assays at 5.0 mmol·L^-1glucose.This biosensors have been applied to determination of the glucose in serum with satisfying results.

In-Situ Detection Of The Effect Of Brighter In The Solution For Nickel And Phosphor Alloy, Jian Zheng, Ning Li, De-Yu Li, Guo-Feng Cui

Journal of Electrochemistry

In this work,the gold-plated mica was used for the substrate,the concentration of 5% of normal plating solution for the nickel was used as the mother solution,and the effect for the deposition by the brighter with ECSTM was in-situ detected.The solution for deposition without the brighter has no brightness,though the values of the roughness and the H_(A-V) have reduced in evidence after deposition;the solution for deposition with the complete brighter although has great brightness,the values of the roughness and the H_(A-V) have increased(after) deposition;the solution for deposition with the half brighter has a moderate effect on the H_(A-V) and (brightness).Hence,the brighter …

The Application Of Astm C1202-93 On Evaluating The Performance Of Anti-Corrosion Of Concrete, Yuan-Chen Yuan, Tsung-Yueh Tu, Chao-Lung Hwang

Journal of Electrochemistry

The test of chloride ion penetration based on the standards of ASTM C1202-93 is applied to evaluate the anti-corrosion performance of concrete in this research. Concrete specimens were produced according to ACI 318-89 mixture proportioning design and the Desenfied Mixture Design Algorithm (DMDA) and were measured the 6-hour coulombs at the age of 91 days. Results show that w/b is not the factor influencing chloride penetration of ACI concrete, as the ion penetration of ACI specimens is all higher than 2 000 Coulombs and can even be poorer than 10 000 Coulombs. With a proper amount of pozzolanic material, the …

Surface-Enhanced Raman Spectra Of Cytosine Adsorbed On A Roughened Gold Electrode, Yuan-Fei Wu, Jian-Feng Li, De-Yin Wu, Bin Ren, Zhong-Qun Tian

Journal of Electrochemistry

Cytosine adsorbed on a roughened gold electrode has been investigated by using electrochemical cyclic voltammetry and surface-enhanced Raman spectroscopy (SERS). The results indicate that cytosine was adsorbed on the Au electrode in a perpendicular orientation via the N3 position. As the maximum enhancement of ring breathing mode appears at negative potentials compared with other modes, both the electromagnetic enhancement and the charge transfer mechanism were considered to contribute to the SERS intensity. The binding interaction between cytosine and the gold electrode was weakened when the potential was negatively moved. The result also indicates that the SERS technique can be used …

Cyclic Voltammetry And Surface Enhanced Raman Spectroscopy Of Dissociative Adsorption Of Ethanol On Pt-Ru Electrodes, Bin Zhang, Hai-Hui Zhou, Zu-Biao Wen, Qi-Ling Zhong, Peng Huang, Xiong-Yuan Yang, Bin Ren, Tian

Journal of Electrochemistry

The behaviors of dissociative adsorption of ethanol on roughened platinum-ruthenium electrode with high activity of SERS were studied by using cyclic voltammetry and in-situ surface enhanced Raman spectroscopy, surface enhanced Raman spectra of dissociative adsorption of ethanol on Pt electrode in acid was obtained for the first time. It is shown that the Pt-Ru could lower the over-potential of CO oxidation when compared to Pt electrode. The results show that the ethanol in acid medium can be self-dissociated at Pt-Ru electrode to produce CO, which discourage the further oxidation of ethanol, some information of Pt-C and Pt-C-Pt stretching vibration from …

Investigation, On The Accelerated Dissolution Of Metal Induced By Afm Tip Scratching And Suppressed By Inhibitors, Jun-E Qu, Xing-Peng Guo

Journal of Electrochemistry

The accelerated dissolution behavior of Cu-Ni alloy induced by AFM tip scratching and the inhibition effect of corrosion inhibitors were investigated. The results showedthat, with a tip loading of 750nN, continuous scan for 30 min in a contact mode on 4×4 μm² of copper-nickel alloy in 1.5mol/L NaCl and 0.01mol/L HCl could enhance the dissolution of the sample and produced pits on the scratched area. Adding inorganic inhibitors, sodium chromateand organic inhibitor dodecylamine, to the solution suppressed the dissolution of copper-nickel alloyinduced by tip scratching, respectively, by improving the surface passivationperformance of metal surface and forming adsorption films on …

Fundamental Chemistry Of U And Pu In The Tbp-Dodecane-Nitric Acid System: Quaterly Report January - March, 2005, Kenneth Czerwinski, Cynthia-May Gong, Amber Wright

Separations Campaign (TRP)

The speciation of hexavalent U and tetravalent Pu will be examined in the TBP-dodecane-nitric acid systems. This topic is chosen based on data needs for separation modeling identified by the AFCI. Emphasis will be placed on studying the influence of nitrate and acetohydroxamic acid on U and Pu speciation as well as conditions where a third phase forms in the organic phase. The organic phase will be 30% TBP in dodecane. Equal volumes of aqueous and organic phase will be used. The speciation of the actinides in the aqueous and organic phase will be determined by a number of different …

Fundamental Chemistry Of U And Pu In The Tbp-Dodecane-Nitric Acid System: Quarterly Report, Kenneth Czerwinski, Cynthia-May Gong, Amber Wright

Separations Campaign (TRP)

The speciation of hexavalent U and tetravalent Pu will be examined in the TBPdodecane- nitric acid systems. This topic is chosen based on data needs for separation modeling identified by the AFCI. Emphasis will be placed on studying the influence of nitrate and acetohydroxamic acid on U and Pu speciation as well as conditions where a third phase forms in the organic phase. The organic phase will be 30 % TBP in dodecane. Equal volumes of aqueous and organic phase will be used. The speciation of the actinides in the aqueous and organic phase will be determined by a number …

Development Of A Systems Engineering Model Of The Chemical Separations Process, Yitung Chen, Sean Hsieh

Separations Campaign (TRP)

The whole chemical separation process is complex to the point that definitely requires certain level of systematic coordination. To perform smoothly and meet the target extraction rates among those processes, this research proposed a general-purpose systems engineering model.

A general purposed systems engineering model, Transmutation Research Program System Engineering Model Project (TRPSEMPro), was developed based on the above design concept. The system model includes four main parts: System Manager, Model Integration, Study Plan, and Solution Viewer. System Manager supervises all the case (problem) creation, and functionality definition. Model Integration identifies chemical extraction processes and their execution sequence. Study Plan is …

Study On Reduction Process Of Electrolyic Manganese Dioxide In Situ By Ultraviolet-Visible Absorption Spectroscopy, Li-Cai Zhu, Zhong-Zhi Yuan, Wei-Shan Li

Journal of Electrochemistry

The concentrationsof soluble Mn(Ⅲ) species, during the reduction ofelectrolytic MnO₂ (EMD) in alkaline solution,have been monitored in situ by UV-visible spectroscopy. The concentration of Mn(Ⅲ) ion in solution changes with discharge time. The first electron discharge process of EMD can be described by three different steps: 1) the reduction of Mn⁴⁺ ions on the surface of EMD particles and the structural defect regions within the EMD, 2) the reduction of Mn⁴⁺ ions in ramsdellite, 3)the reduction of Mn⁴⁺ ions in pyrolusite. During the second electron discharge of EMD, the soluble Mn(Ⅲ) is reduced to Mn(Ⅱ) , …

Fundamental Chemistry Of U And Pu In The Tbp-Dodecane-Nitric Acid System, Kenneth Czerwinski, Byron Bennett

Separations Campaign (TRP)

The speciation of hexavalent U and tetravalent Pu will be examined in the TBP-dodecane-nitric acid systems. This topic is chosen based on data needs for separation modeling identified by the AFCI. Emphasis will be placed on studying the influence of nitrate and acetohydroxamic acid on U and Pu speciation as well as conditions where a third phase forms in the organic phase. The organic phase will be 30% TBP in dodecane. Equal volumes of aqueous and organic phase will be used. The speciation of the actinides in the aqueous and organic phase will be determined by a number of different …