• Journal of Electrochemical Science and Technology
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• 제13권2호
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• pp.279-291
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• 2022

In this report the thermochemical conversion of Sm₂O₃ to SmCl₃ using AlCl₃ in LiCl-KCl melt at 773 K is discussed. The final product was a mixture of SmCl₃, Al₂O₃, unreacted Sm₂O₃ and AlCl₃ in the chloride melt. The electrochemical attributes of the mixture was analyzed with cyclic voltammetry (CV) and square wave voltammetry (SWV). The crystallographic phases of the mixture were studied with X-ray diffraction (XRD) technique. The major chemical conversion was optimized by varying the effective parameters, such as concentrations of AlCl₃, duration of reaction and the amount of LiCl-KCl salt. The extent of conversion and qualitative assessment of efficiency of the present protocol were evaluated with fluorescence spectroscopy, UV-Vis spectrophotometry and inductively coupled plasma atomic emission spectroscopy (ICP-AES) studies of the mixture. Thus, a critical assessment of the thermochemical conversion efficiency was accomplished by analysing the amount of SmCl₃ in LiCl-KCl melt. In the process, a conversion efficiency of 95% was achieved by doubling the stoichiometric requirement of AlCl₃ in 50 g of LiCl-KCl salt. The conversion reaction was found to be very fast as the reaction reached equilibrium in 15 min.

• 한국응용과학기술학회지
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• 제28권4호
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• pp.502-507
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• 2011

A voltammetric assay of phenol ions was investigated using three electrode systems of graphite pencil working, reference and counter electrodes. Under optimum analytical parameters, square wave stripping working ranges were attained at a mili range of 10~80 mg/L and a micro range of 20~90 ug/L using seawater electrolyte. The developed sensor was applied to tap water and the human body system of a smoker. It was found that the methods can be applied to in vivo fluid or medicinal diagnosis.

• 한국세라믹학회지
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• 제48권3호
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• pp.205-210
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• 2011

The dependence of sulfur redox behavior and its diffusivity on temperature and composition was studied in mixed alkali silicate melts by means of square wave voltammetry (SWV) at different frequencies in a temperature range of $1000^{\circ}C$ to $1400^{\circ}C$. The voltammograms showed two reduction peaks at high frequency but only one peak at low frequency. Irrespective of $K_2O/(Na_2O+K_2O)$, each peak potential due to reduction of $S^{6+}$ to $S^{4+}$ and $S^{4+}$ to $S^0$ moved toward a negative direction with temperature decrease, and the peak current showed a strong dependence on frequency at a constant temperature. However, the compositional dependence of the peak potential showed an inconsistent behavior with an increase of $K_2O$. The mixed alkali effect was not observed in sulfur diffusion. This inconsistency of both peak potential and diffusion for compositional dependence may be derived from the strong volatilization of sulfur in melts.

• 대한화학회지
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• 제41권11호
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• pp.590-593
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• 1997

Germanium(IV)-Morin 착물에 대한 네모파 양극벗김 전압전류법적 연구를 0.5 M 황산 지지전해질에서 수행하였다. Germanium(IV)-Morin 착물의 피크전위는 - 0.606 V vs. Ag/AgCl에서 나타났다. Germanium(IV)-Morin 착물의 피크전류 크기에 미치는 지지전해질의 황산 농도, Morin의 농도, 축적전위 및 축적시간의 의존성 등에 대하여 논의하였다. 또한, Germanium(IV)-Morin 착물의 피크전류 크기에 영향을 주는 금속 양이온들의 방해효과도 조사하였다. 이 방법을 적용시켜 축적시간을 60초로 하였을 때 Germanium(IV)의 검출한계는 $3.76{\times}10^{-7}M(27 {\mu}g/L)$ 이었으며, 0.4 mg/L($5.5{\times}10^{-6}$ M)의 Germanium(IV) 분석에 대한 상대표준편차(n=8)는 3.2% 이었다.

• 대한핵의학회지
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• 제34권4호
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• pp.336-343
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• 2000

목적: $[^{201}Tl]$TICI주사액의 제조과정에서 안정동위원소인 $^{201}Tl$ 및 Cu, Pb의 중금속을 함유할 가능성이 있어 이러한 이물질을 확인하기 위한 방법으로 방사성 물질의 대기오염을 일으키지 않는 폴라로그래피의 분석 조건을 설정하고자 하였다. 대상 및 방법: 원자력병원에서 생산하고 있는 $[^{201}Tl]$-TlCl 주사액에 포함될 수 있는 중금속을 대상으로 하였다. 극미량의 중금속을 측정하기 위한 방법으로 BAS-50W 폴라로그래피를 이용하였고, 여기에 사용된 3 전극계는 작업전극인 DME, 기준전극인 Ag/AgCl 그리고 보조전극인 백금선을 이용하였다. 신속하고 재현성있는 분석을 위한 조건으로 기기의 분석 모드, 각 모드에 적합한 전극, 지지전해질, 석출시간 등의 치적 조건을 설정하였다. 결과: 폴라로그래피의 모드는 OSWSV 방법이 재현성과 감도면에서 가장 우수하였고, 작업전극은 DME와 Au 전극을 비교 실험한 결과 재현성 면에서 DME가 보다 좋은 결과를 보였다. 지지전해질은 염기성인 0.50 M KOH 용액, 산성인 1.0 M $HNO_3$, 용액, 중 성인 pH 7 phosphate 완충용액을 비교 실험하여 pH 7 phosphate 완충용액이 $Tl^+$과 $Cu^{2+}$를 분석하는데 가장 적합함을 확인하였다. 이를 바탕으로 중금속을 측정한 결과 $Tl^+$은 -450 mV, $Cu^{2+}$는 -50 mV에서 각각의 피크가 나타났고, 석출시간을 45초로 하였을 때 $Tl^+$의 경우 y=2.05E-$9{\chi}$+5.66E-9이고 $Cu^{2+}$의 경우는 y=1.23E-$8{\chi}$+1.23E-6의 선형 관계식을 얻었다. 결론: 이 방법에 의한 Tl과 Cu의 검출한계는 약 0.05 ppm이다. 이 방법을 현재 원자력병원에서 생산하고 있는 $[^{201}Tl]$TICl 주사액의 정도관리에 도입하여 중금속을 측정한 결과 약전에서 규정하고 있는 2 ppm 미만임을 확인하였고, 그 결과는 재현성, 정확도, 감도 및 간편성에서 모두 만족할 수 있었다. 이 방법은 $[^{201}Tl]$TlCl 주사액 뿐만 아니라 $^{67}Ga$ 주사액 및 기타 방사성의약품과 중금속 분석에도 응용할 수 있다.

• 한국응용과학기술학회지
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• 제29권1호
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• pp.40-46
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• 2012

In vivo nicotine is associated with Alzheimer's, Parkinson's and lung cancer. Diagnostic assays of these diseases depend on very low analytical detection limits. In this study, a sensitive analytical method was examined using a voltammetric graphite pencil electrode (GPE) and a modified carbon nanotube paste electrode (CNE). The optimum analytical conditions for both electrodes were compared using square wave anodic stripping voltammetry (SW) and cyclic voltammetry (CV) obtaining 400 sec accumulation time and oxidation peak. Under optimum parameters, the stripping working range of GPE was $5.0-40.0{\mu}g/L$, CNE: 0.1-0.8 and $5-50{\mu}g/L$. Quantification limits were $5.0{\mu}g/L$ for GPE and $0.1{\mu}g/L$ for CNE, while detection limits were $0.6{\mu}g/L$ for GPE and $0.07{\mu}g/L$ for CNE. A standard deviation of $10.0{\mu}g/L$ was observed for 0.064 GPE and 0.095 CNE (n = 12) using 400 sec accumulation time. The results obtained can be applied to non.treated urine and ex vivo biological diagnostics.

• 방사성폐기물학회지
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• 제19권2호
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• pp.161-176
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• 2021

In this study, the electrochemical behavior of Sm on the binary liquid Al-Ga cathode in the LiCl-KCl molten salt system is investigated. First, the co-reduction process of Sm(III)-Al(III), Sm(III)-Ga(III), and Sm(III)-Ga(III)-Al(III) on the W electrode (inert) were studied using cyclic voltammetry (CV), square-wave voltammetry (SWV) and open circuit potential (OCP) methods, respectively. It was identified that Sm(III) can be co-reduced with Al(III) or Ga(III) to form Al_zSm_y or Ga_xSm_y intermetallic compounds. Subsequently, the under-potential deposition of Sm(III) at the Al, Ga, and Al-Ga active cathode was performed to confirm the formation of Sm-based intermetallic compounds. The X-ray diffraction (XRD) and scanning electron microscopy-energy dispersive spectroscopy (SEM-EDS) analyses indicated that Ga₃Sm and Ga₆Sm intermetallic compounds were formed on the Mo grid electrode (inert) during the potentiostatic electrolysis in LiCl-KCl-SmCl₃-AlCl₃-GaCl₃ melt, while only Ga₆Sm intermetallic compound was generated on the Al-Ga alloy electrode during the galvanostatic electrolysis in LiCl-KCl-SmCl₃ melt. The electrolysis results revealed that the interaction between Sm and Ga was predominant in the Al-Ga alloy electrode, with Al only acting as an additive to lower the melting point.

• Bulletin of the Korean Chemical Society
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• 제31권7호
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• pp.1897-1901
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• 2010

Multi-wall carbon nanotube (MWNT)-modified glassy carbon electrodes (GCE) were prepared for simultaneous determination of rutin and quercetin. Microbial carbohydrates, $\alpha$-cyclosophorohexadecaose ($\alpha$-C16) and succinoglycan monomer M3 (M3) were doped into MWNTs to prepare a $\alpha$-C16-doped MWNT-modified GCE (($\alpha$-C16 + MWNTs)/GCE) and a M3-doped MWNT-modified GCE ((M3 + MWNTs)/GCE), respectively. The sensitivities of the ($\alpha$-C16 + MWNTs)/GCE to rutin and quercetin were 34.7 ${\mu}A\cdot{\mu}M^{-1}{\cdot}cm^{-2}$ and 18.3 ${\mu}A\cdot{\mu}M^{-1}{\cdot}cm^{-2}$, respectively, in a linear range of $2\sim8{\mu}M$ at pH 7.2. The sensitivities of the (M3 + MWNTs)/GCE was 2.44 ${\mu}A\cdot{\mu}M^{-1}{\cdot}cm^{-2}$ for rutin and 7.19 ${\mu}A\cdot{\mu}M^{-1}{\cdot}cm^{-2}$ for quercetin without interference.

• 한국응용과학기술학회지
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• 제29권2호
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• pp.302-310
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• 2012

Bio assay of mercury and cadmium ions were searched using voltammetric analysis using DNA doped carbon nanotube paste electrodes (DCP). The square-wave stripping voltammetryic optimized results indicated working ranges of 1-10.0 $ngL^{-1}$ and 20-100 $ugL^{-1}$, Hg(II) Cd(II) within an accumulation time of 120 seconds, in 0.1-M phosphate buffer solutions of pH 6.3. The relative standard deviations of 5 $ngL^{-1}$ Hg(II) and Cd(II) that observed were 0.14 and 0.22% (n=12), respectively, using optimum conditions. The low detection limit (S/N) was pegged at 0.1 $ngL^{-1}$ ($4.9{\times}10^{-11}M$) Hg(II) and 0.2 $ngL^{-1}$ ($1.77{\times}10^{-10}M$) Cd(II). The developed methods can be applied to assays in biological fish kidneys and water samples.

• Toxicological Research
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• 제31권2호
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• pp.213-217
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• 2015

A voltammetric toxic metal of cadmium detection was studied using a fluorine doped graphite pencil electrode (FPE) in a seawater electrolyte. In this study, square wave (SW) stripping and chronoamerometry were used for determination of Cd(II) in seawater. Affordable pencils and an auxiliary electrode were used as reference. All experiments in this study could be performed at reasonable cost by using graphite pencil. The application was performed on the tissue of contaminated soil earthworm. The results show that the method can be applicable for vegetables and in vivo fluid or medicinal diagnosis.