• Title/Summary/Keyword: Electrochemical Determination

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Ion Conduction Properties of PMMA/PVDF based Polymer Electrolyte for Lithium Polymer Battery (리튬 폴리머전지용 PMMA/PVDF계 고분자 전해질의 이온 전도 특성)

  • 이재안;김종욱;구할본;이헌수;손명모
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2000.11a
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    • pp.347-350
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    • 2000
  • The purpose of this study is to research and develop solid polymer electrolyte(SPE) for Li polymer battery. The temperature dependence of conductivity, impedance spectroscopy and electrochemical properties of PMMA/PVDF electrolytes as a function of a mixed ratio were reported for PMMA/PVDF based polymer electrolyte films, which were prepared by thermal gellification method of preweighed PMMA/PVDF, plasticizer and Li salt. The ion conductivity of PMMA/PVDF electrolytes was 10$\^$-3/S/cm, which may be applicable to a constituent of lithium secondary battery. 5PMMA20PVDFLiC1O$_4$PC$\sub$8/EC$\sub$8/ electrolyte remains stable up to 5V vs. Li/Li$\^$+/. Steady state current method and AC impedance were used for the determination of transference numbers in PMMA/PVDF electrolyte film. The transference number of 5PMMA20PVDFLiC1O$_4$PC$\sub$8/EC$\sub$8/ electrolyte is 0.55.

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Electrochemistry and Direct Conductivity Determination of Thin Films of Prussian Blue

  • 문성배;김영인
    • Bulletin of the Korean Chemical Society
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    • v.16 no.6
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    • pp.511-515
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    • 1995
  • Since much studies have been performed concerning the electrochemical behaviors and the practical applications of PB based devices, little has yet reported to investigate the best condition for the preparation for PB thin films. As considered some factors(peak shape, peak current, and peak separation) from the i-V curves, the optimal condition in the film growth were investigated under various immersion solutions. An electron-transfer processes of Fe2+/Fe3+ and Fe(CN)63-/4- redox couples were considered by measuring the observed currents as a function of the rotation velocity. The standard heterogeneous electron-transfer rates for these films and bare Au disc electrode in 10-3 M Fe2+/Fe3+ solution, applied at +0.65 V vs. SCE, were 6.14 × 10-3 and 7.78 × 10-3 cm/s, respectively, obtained using a rotating disc electrode. In case of the addition of potassium ion, the rate constants for these Fe2+/Fe3+ system on thin films of PB and bare electrode were given a little high values. The electron transfer rate for 10-3 M Fe(CN)63-/4- were 4.55 × 10-3 and 6.84 × 10-3 cm/s, respectively. The conductivity as directly determined during obtained the voltammogram, was 2.2 × 10-7 (Ω·cm)-1. This value is similar magnitude to that calculated from bulk sample.

Analysis of Surface and Thin Films Using Spectroscopic Ellipsometry (Spectroscopic Ellipsometry를 이용한 표면 및 박막의 분석)

  • 김상열
    • Korean Journal of Optics and Photonics
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    • v.1 no.1
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    • pp.73-86
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    • 1990
  • The technique of Spectroscopic Ellipsometry (SE) has been examined with emphasis on its inherent sensitivity to the existence of thin films or surface equivalents. A brief review of related theories like the Fresnel reflection coefficients, the effect of a multilayer upon reflectivities, together with the validity of the effective medium theory and the modelling procedure, is followed by a short description of the experimental setup of a rotating polarizer type SE as well as the necessful expressions which lead to tan and cos. Out of its numerous, successful applications, a few are exampled to convince a reader that SE can be applied to a variety of research fields related to surface, interface and thin films. Specifically, those are adsorption and/or desorption on metals or semiconductors, oxidation process, formation of passivation layers on an electrode, thickness determination, interface between semiconductor and its oxide, semiconductor heterojunctions, surface microroughness, void distribution of dielectric, optical thin films, depth profile of multilayered samples, in-situ or in-vitro characterization of a solid surface immersed in electrolyte during electrochemical, chemical, or biological treatments, and so on. It is expected that the potential capability of SE will be widely utilized in a very near future, taking advantage of its sensitivity to thin films or surface equivalents, and its nondestructive, nonperturbing characteristics.

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Mass Spectrometry-Based Analytical Methods of Amatoxins in Biological Fluids to Monitor Amatoxin-Induced Mushroom Poisoning

  • Choi, Jin-Sung;Lee, Hye Suk
    • Mass Spectrometry Letters
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    • v.13 no.4
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    • pp.95-105
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    • 2022
  • Amatoxin-induced mushroom poisoning starts with nonspecific symptoms of toxicity but hepatic damage may follow, resulting in the rapid development of liver insufficiency and, ultimately, coma and death. Accurate detection of amatoxins, such as α-, β-, and γ-amanitin, within the first few hours after presentation is necessary to improve the therapeutic outcomes of patients. Therefore, analytical methods for the identification and quantification of α-, β-, and γ-amanitin in biological samples are necessary for clinical and forensic toxicology. This study presents a literature review of the analytical techniques available for amatoxin detection in biological matrices, and established an inventory of liquid chromatography (LC) techniques with mass spectrometry (MS), ultraviolet (UV) detection, and electrochemical detection (ECD). LC-MS methods using quadrupole tandem mass spectrometry, time-of-flight mass spectrometry, and orbitrap MS are powerful analytical techniques for the identification and determination of amatoxins in plasma, urine, serum, and tissue samples, with high sensitivity, specificity, and reproducibility compared to LC with UV and ECD, enzyme-linked immunoassay, and capillary electrophoresis methods.

Studies on the Spectrophotometric Determination, Electrochemical Behavior of Heavy Lanthanide ions in Nonaqueous System and Heavy Chelates Complexes with Bidendate Ligands (Ⅱ) Electrochemical Behavior of Heavy Lanthanide Ions in Acetonitrile (무거운 란탄이온의 분광학적 정량, 비수용액에서의 전기화학적 거동 및 중금속이온과 두자리 리간드 착물에 관한 연구 (제 2 보))

  • Kang Sam-Woo;Park Chong-Min;Kim Il-Kwang;Do Lee-Mi;Lee Jong-Min
    • Journal of the Korean Chemical Society
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    • v.37 no.5
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    • pp.483-490
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    • 1993
  • Voltammetric behavior of heavy lanthanide ions has been investigated by the DC, DPP and CV in acetonitrile solution. The reduction of $Gd^{3+}, Tb^{3+}, Dy^{3+}, Ho^{3+}, Er^{3+}, Tm^{3+} 및 Lu^{3+} proceed by three-electron change to the metallic state with totally irreversibility in 0.1M tetraethylammonium perchlorate. However, the reduction of Yb(Ⅲ) proceeds in two steps $(Yb^{3+} + e^- \Leftrightarrow Yb^{2+} and Yb^{2+} + 2e^- → Yb^0)$. The first reduction of Yb(Ⅲ) showed quasi reversible behavior, but the second reduction was irreversible in cyclic voltammetry. The cathodic peak current showed adsorptive properties in high concentration with lower sweep rate. The electroreduction of heavy lanthanides in water-acetonitrile mixture has been studied. In water-acetonitrile mixture, the negative shift of the peak potential and the decrease peak current were observed increasing water concentration. Also the Yb(Ⅲ) reduction to Yb(Ⅲ) has been deviated from quasi-reversible character with increase water amount. These results drive from the high solvation abilities of water which has high donor number.

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Electrochemical Behavior of Light Lanthanide Ions in Nonaqueous Solution, Flow Injection Determination and Photochemical Characterization of Eight Coordinated Chelates of Heavy Metal Ions (Part I) Electrochemical Behavior of Light Lanthanide Ions in Nonaqueous Solution (물아닌용매에서 가벼운 란탄족 이온의 전기화학적 거동, 흐름주입에 의한 정량 및 중금속이온의 킬레이트형 8-배위 착물의 광화학적 특성 (제 1 보) 물아닌용매에서 가벼운 란탄족이온의 전기화학적 거동)

  • Kang, Sam-Woo;Pak, Chong-Min;Do, Lee-Mi;Song, Myoung-Kyu;Kim, Il-Kwang
    • Analytical Science and Technology
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    • v.7 no.3
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    • pp.361-369
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    • 1994
  • Voltammetric behavior of some light lanthanide ions($La^{3+}$, $Pr^{3+}$, $Nd^{3+}$, $Sm^{3+}$ and $Eu^{3+}$) in acetonitrile(AN) and dimethylformamide(DMF) has been investigated by direct current, differential pulse polarography and cyclic voltammetry. The reduction of $La^{3+}$, $Pr^{3+}$ and $Nd^{3+}$ in 0.1M TEAP proceeded directly to the metallic state through three-electron charge transfer of irreversible process where as $Sm^{3+}$ and $Eu^{3+}$ proceeded by charge transfer of two steps. As the results of the cyclic voltammetric investigation, the first step reduction of $Sm^{3+}$ and $Eu^{3+}$ were a quasireversible reaction, the second step reductions were an irreversible reaction. The cathodic peak currents of the differential pulse polarogram showed adsorptive properties at lower sweep rates and high concentrations of these metal ions. The peak potenital was shifted to a negative petential and the peak current decreased with the increase of percentage of water in AN. On the other hand, the peak potential was shifted to a positive potential and the peak current decreased with an increased percentage of water in DMF.

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Determination of cimetidine injection by square wave voltammetry (네모파 전압전류법에 의한 Cimetidine 주사액의 정량분석)

  • Lee, Soo-Jung;Hahn, Young-Hee
    • Analytical Science and Technology
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    • v.23 no.1
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    • pp.68-73
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    • 2010
  • In order to develop the square wave voltammetric method determining cimetidine in an ampoule for injection, $5.00{\times}10^{-4}\;M$ cimetidine HCl solutions prepared with phosphate buffers of various pH values (3.01~8.97) were investigated by SWV. The well defined single peak due to the electrochemical reduction of -C=N-C$\equiv$N- in the structure of cimetidine moved towards the cathodic direction by -0.051V/pH as the pH values were increased indicating the involvement of hydrogen in its reduction. The calibration curves of cimetidine HCl in the concentration range between $1.00{\times}10^{-5}\;M$ and $5.00{\times}10^{-3}\;M$ prepared using three phosphate buffers yielded the slopes of 127,407nA/M (pH 3.01), 115,125nA/M (pH 5.00) and 111,287nA/M(pH 7.00) with excellent linearities of $R^2{\geqq}0.9997$. When one ampoule of Tagma Inj.$^{(R)}$ was analyzed by standard addition method by SWV, the within-day precision study (n=4) on the day of sample preparation resulted in the contents of cimetidine as $203{\pm}3.8\;mg$ (102% of the specified contents, RSD of 1.9%) and the inter-day precision (n=4) through 5 days was reasonable as 1.3% of RSD.

Determination of Properties of Ionomer Binder Using a Porous Plug Model for Preparation of Electrodes of Membrane-Electrode Assemblies for Polymer Electrolyte Fuel Cells

  • Park, Jin-Soo;Park, Seok-Hee;Park, Gu-Gon;Lee, Won-Yong;Kim, Chang-Soo;Moon, Seung-Hyeon
    • Journal of the Korean Electrochemical Society
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    • v.10 no.4
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    • pp.295-300
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    • 2007
  • A new characterization method using a porous plug model was proposed to determine the degree of sulfonation (DS) of ionomer binder with respect to the membrane used in membrane-electrode assemblies (MEAs) and to analyze the fraction of proton pathways through ionomer-catalyst combined electrodes in MEAs for polymer electrolyte fuel cells (PEFCs). Sulfonated poly(ether ether ketone) was prepared to use a polymeric electrolyte and laboratory-made SPEEK solution (5wt.%, DMAc based) was added to catalyst slurry to form catalyst layers. In case of the SPEEK-based MEAs in this study, DS of ionomer binder for catalyst layers should be the same or higher than that of the SPEEK membrane used in the MEAs. The porous plug model suggested that most of protons were via the ionomer binder (${\sim}92.5%$) bridging the catalyst surface to the polymeric electrolyte, compared with the pathways through the alternative between the interstitial water on the surface of ionomer binder or catalyst and the ionomer binder (${\sim}7.3%$) and through only the interstitial water on the surface of ionomer or catalyst (${\sim}0.2%$) in the electrode of the MEA comprising of the sulfonated poly(ether ether ketone) membrane and the 5wt.% SPEEK ionomer binder. As a result, it was believed that the majority of proton at both electrodeds moves through ionomer binder until reaching to electrolyte membrane. The porous plug model of the electrodes of MEAs reemphasized the importance of well-optimized structure of ionomer binder and catalyst for fuel cells.

Electrochemical Determination of Bisphenol A Concentrations using Nanocomposites Featuring Multi-walled Carbon Nanotube, Polyelectrolyte and Tyrosinase (다중벽 탄소 나노 튜브, 전도성고분자 및 티로시나아제 효소로 구성된 나노복합체를 이용한 비스페놀A 맞춤형의 전기화학적 검출법)

  • Ku, Nayeong;Byeon, Ayeong;Lee, Hye Jin
    • Applied Chemistry for Engineering
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    • v.32 no.6
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    • pp.684-689
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    • 2021
  • In this paper, we develop a cost effective and disposable voltammetric sensing platform involving screen-printed carbon electrode (SPCE) modified with the nanocomposites composed of multi-walled carbon nanotubes, polyelectrolyte, and tyrosinase for bisphenol A. This is known as an endocrine disruptor which is also related to chronic diseases such as obesity, diabetes, cardiovascular and female reproductive diseases, precocious puberty, and infertility. A negatively charged oxidized multi-walled carbon nanotubes (MWCNTs) wrapped with a positively charged polyelectrolyte, e.g., polydiallyldimethylammonium, was first wrapped with a negatively charged tyrosinae layer via electrostatic interaction and assembled onto oxygen plasma treated SPCE. The nanocomposite modified SPCE was then immersed into different concentrations of bisphenol A for a given time where the tyrosinase reacted with OH group in the bisphenol A to produce the product, 4,4'-isopropylidenebis(1,2-benzoquinone). Cyclic and differential pulse voltammetries at the potential of -0.08 V vs. Ag/AgCl was employed and peak current changes responsible to the reduction of 4,4'-isopropylidenebis(1,2-benzoquinone) were measured which linearly increased with respect to the bisphenol A concentration. In addition, the SPCE based sensor showed excellent selectivity toward an interferent agent, bisphenol S, which has a very similar structure. Finally, the sensor was applied to the analysis of bisphenol A present in an environmental sample solution prepared in our laboratory.

Determination of individual sugars in different varieties of persian grape using Near Infrared spectroscopy

  • Kargosha, Kazem;Azad, Jila;Lary, Abas Motamed
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.1527-1527
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    • 2001
  • Glucose, fructose and sucrose being the main sugars that can be found in natural fruit juice. Many instrumental methods, such as GC, LC, electrochemical or spectrometric methods provide information about both the total content of sugars and the specific concentration of each carbohydrate[1]. The simplicity of sample handling and measurement in the near IR(NIR) wavelength region, which allows the use of long pathlength, optical glass cells and optical fibers, makes NIR a good alternative for sugar determination [2]. In the present study, six varieties of persian grapes were harvested at intervals through august to october and analysed for sugars by NIR. The results were processed by principal component regression (PCR) and partial least squares (PLS) analysis. Sample juice was prepared by squeezing through gauze from crashed grape. This solution was treated by zinc ferrocyanide prior to analysis in order to eliminate colored compounds and all optically active nonsugar substances. For glucose and fructose the most characteristic wavelengths were 1456nm corresponding to the first harmonic O-H stretching and the second at 2062nm corresponding to O-H stretching and deformation; secondary characteristic combination bands were also seen at 2265 nm (O-H and C-C stretching) and at 2240 nm (C-H and C-C stretching). However these spectra were taken over a wavelength range from 1100-2500nm at room temperature of 25-$30^{\circ}C$. To test the accuracy of the described procedure, samples of six varieties of grape were analysed by the proposed NIR and a standard method[2]. Good agreement were found between these two sets of the results. To perform the recovery studies , samples of grape juices previously analysed by the proposed method, were spiked with known amounts of each individual sugars and then analysed again. Relative standard deviations varied from 1.4 to 1.8% for six independent measurements of individual and total sugar concentration. In the analysis of real and synthetic samples, precise and accurate results were obtained , providing accuracy errors lower than 1.9% in all cases. Average recoveries of ${97}{\pm}{4%}$ for total sugar and between ${95}{\pm}{5%}$ and ${99}{\pm}{2%}$ for sing1e sugars demonstrate the applicability of the methodology developed to the direct analysis of grape Juice.

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