• Title/Summary/Keyword: Trace As(V) detection

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Use of hybrid materials in the trace determination of As(V) from aqueous solutions: An electrochemical study

  • Tiwari, Diwakar;Jamsheera, A.;Zirlianngura, Zirlianngura;Lee, Seung Mok
    • Environmental Engineering Research
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    • v.22 no.2
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    • pp.186-192
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    • 2017
  • The carbon paste electrode (CPE) was modified with the pristine bentonite and hybrid material (HDTMA-modified bentonite). The modified-CPEs are then employed as working electrode in an electrochemical detection of As(V) from aqueous solutions using the cyclic voltammetric measurements. Cyclic voltammograms revealed that As(V) showed reversible behavior onto the working electrode. The hybrid material-modified carbon paste electrode showed significantly enhanced electrochemical signal which was then utilized in the low level detection of As(V). Moreover, the studies were conducted at neutral pH conditions. The electrochemical studies were conducted with scan rates (20 to 200 mV/s) to deduce the mechanism of redox processes involved at the electrode surface. The anodic current was linearly increased, increasing the concentration of As(V) from 5.0 to $35.0{\mu}g/g$ using the hybrid material-modified electrode. This provided fairly a good calibration line for As(V) detection. The presence of varied concentrations of As(III) in the determination of total arsenic was studied. The influence of several cations and anions viz., Cu(II), Mn(II), Zn(II), Pb(II), Cd(II), Fe(III), $Cl^-$, $NO_3{^-}$, $PO_4{^{3-}}$, EDTA and glycine in the detection of As(V) from aqueous solution was also studied. Further, in an attempt to simulate the real matrix analysis, the tap water sample was spiked with As(V) and subjected for As(V) detection using the modified-CPE.

Ultra-trace Arsenic Determination in Urine and Whole Blood Samples by Flow Injection-Hydride Generation Atomic Absorption Spectrometry after Preconcentration and Speciation Based on Dispersive Liquid-Liquid Microextraction

  • Shirkhanloo, Hamid;Rouhollahi, Ahmad;Mousavi, Hassan Zavvar
    • Bulletin of the Korean Chemical Society
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    • v.32 no.11
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    • pp.3923-3927
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    • 2011
  • A noble method for pre-concentration and speciation of ultra trace As (III) and As (V) in urine and whole blood samples based on dispersive liquid-liquid microextraction (DLLME) has been developed. In this method, As (III) was complexed with ammonium pyrrolidine dithiocarbamate at pH = 4 and Then, As (III) was extracted into the ionic liquid (IL). Finally, As (III) was back-extracted from the IL with hydrochloric acid (HCl) and its concentration was determined by flow injection coupled with hydride generation atomic absorption spectrometry (FI-HGAAS). Total amount of arsenic was determined by reducing As (V) to As (III) with potassium iodide (KI) and ascorbic acid in HCl solution and then, As (V) was calculated by the subtracting the total arsenic and As (III) content. Under the optimum conditions, for 5-15 mL of blood and urine samples, the detection limit ($3{\sigma}$) and linear range were achieved 5 ng $L^{-1}$ and 0.02-10 ${\mu}g\;L^{-1}$, respectively. The method was applied successfully to the speciation and determination of As (III) and As (V) in biological samples of multiple sclerosis patients with suitable precision results (RSD < 5%). Validation of the methodology was performed by the standard reference material (CRM).

Determination of Trace Amounts of Lead and Copper in Water Samples by Flame Atomic Absorption Spectrometry after Cloud Point Extraction

  • Shemirani, Farzaneh;Abkenar, Shiva Dehghan;Khatouni, Asieh
    • Bulletin of the Korean Chemical Society
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    • v.25 no.8
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    • pp.1133-1136
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    • 2004
  • The need for highly reliable methods for the determination of trace metals is recognized in analytical chemistry and environmental science. A method based on the cloud-point extraction (CPE) technique for the trace analysis of Pb and Cu in water samples is described in this study. The analytes in the initial aqueous solution are complexed with pyrogallol, and 0.1%(w/v) Triton X-114 is added as surfactant. Following phase separation at $50^{\circ}C$, based on the cloud point of the mixture and dilution of the surfactant-rich phase with acidified methanolic solution, the enriched analytes are determined by flame atomic absorption spectrometry. After optimization of the complexation and extraction conditions, the enrichment factors of Pb and Cu were found to be 72 and 85, respectively. Under optimum conditions, the preconcentration of 60 mL of samples in the presence of 0.1%(w/v) Triton X-114 permitted the detection of 0.4 ${\mu}gL^{?1}$ of Pb and 0.05 ${\mu}gL^{?1}$ of Cu. The proposed method was applied successfully to the determination of Pb and Cu in water samples.

Application of the Ultrasonic Detection System for the Power Transformer (전력용 변압기 초음파 측정시스템 적용)

  • Kweon, Dong-Jin;Koo, Kyo-Sun;Kim, Jae-Chul
    • The Transactions of the Korean Institute of Electrical Engineers C
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    • v.54 no.12
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    • pp.553-557
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    • 2005
  • This paper describes the application results of an ultrasonic detection system for the power transformer. The ultrasonic detection system with 6 sensors was applied to detect partial discharge in a 154kV transformer with a dangerous levels of $C_{2}H_{2},\;C_{2}H_4$ and $CH_{4}$ gases. The ultrasonic detection tests were carried out 2 times, respectively, to confirm the existence and location of the partial discharge in the transformer. As a result of internal inspection, the arc trace between the pressure ring and core due to the partial discharge was found at the estimated position based on the amplitude and arriving time of the ultrasonic signals. Therefore, it was verified that the ultrasonic detection system is effective as a preventive diagnosis method for the power transformer. Also, the reliability of the ultrasonic detection system in detecting partial discharges in the transformer was also confirmed. It is expected, therefore, that the ultrasonic detection system will have beneficial effects on applications and verifications in detecting partial discharges for the power transformer.

Lower the Detection Limits of Accelerator Mass Spectrometry

  • John A., Eliades;Song, Jong-Han;Kim, Jun-Gon;Kim, Jae-Yeol;O, Jong-Ju;Kim, Jong-Chan
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.02a
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    • pp.243-244
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    • 2013
  • Over the past 15 years, several groups have incorporated radio-frequency quadrupole (RFQ) based instruments before the accelerator in accelerator mass spectrometry (AMS) systems for ion-gas interactions at low kinetic energy (<40 eV). Most AMS systems arebased on a tandem accelerator, which requires negative ions at injection. Typically, AMS sensitivity abundance ratios for radioactive-to-stable isotope are limited to Xr/Xs >10^-15, and the range of isotopes that can be analyzed is limited because of theneed to produce rather large negative ion beams and the presence of atomic isobaric interferences after stripping. The potential of using low-kinetic energy ion-gas interactions for isobar suppression before the accelerator has been demonstrated for several negative ion isobar systems with a prototype RFQ system incorporated into the AMS system at IsoTrace Laboratory, Canada (Ontario, Toronto). Requisite for any such RFQ system applied to very rare isotope analysis is large transmission of the analyte ion. This requires proper phase-space matching between the RFQ acceptance and the ion beam phase space (e.g. 35 keV, ${\varphi}3mm$, +-35 mrad), and the ability to control the average ion energy during interactions with the gas. A segmented RFQ instrument is currently being designed at Korea Institute for Science and Technology (한국과학기술연구원, KIST). It will consist of: a) an initial static voltage electrode deceleration region, to lower the ion energy from 35 keV down to <40 eV at injection into the first RFQ segment; b) the segmented quadrupole ion-gas interaction region; c) a static voltage electrode re-acceleration region for ion injection into a tandem accelerator. Design considerations and modeling will be discussed. This system should greatly lower the detection limits of the 6 MV AMS system currently being commissioned at KIST. As an example, current detection sensitivity of 41Ca/Ca is limited to the order of 10^-15 while the 41Ca/Ca abundance in modern samples is typically 41Ca/Ca~10^-14 - 10^-15. The major atomic isobaric interference in AMS is 41K. Proof-of-principal work at IsoTrace Lab. has demonstrated that a properly designed system can achieve a relative suppression of KF3-/41CaF3- >4 orders of magnitude while maintaining very high transmission of the 41CaF3- ion. This would lower the 41Ca detection limits of the KIST AMS system to at least 41Ca/Ca~10^-19. As Ca is found in bones and shells, this would potentially allow direct dating of valuable anthropological archives and archives relevant to our understanding of the most pronounced climate change events over the past million years that cannot be directly dated with the presently accessible isotopes.

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Determination of Trace Amounts of Nickel(II) with ${\alpha}-(2-Benzimidazolyl))-{\alpha}'{\alpha}$

  • Park, Chan Il;Kim, Hyeon Su;Cha, Gi Won
    • Bulletin of the Korean Chemical Society
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    • v.21 no.5
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    • pp.483-486
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    • 2000
  • A method is described for the fluorimetric determination of nickel, based on the formation of $Ni(II)-\alpha-(2-Benzimidazolyl)-\alpha'$, $\alpha''$ -(N-5-Nitro-2-Pyridylhydrazone)-toluene complex in the presence of a non-ionic surfactant. The complex has practically no fluorescence in the absence of surfactant, but the addition of Triton X-100 makes possible the fluorimetric determination of low concentrations of Ni(II) as it enhances the fluorescenceintensity of the complex by up to about 5-fold. This method is very sensitive and selectrive for the direct determination of nickel ion. The optimum conditions are a Triton X-100 concentration of 2.0 mL(5.0%, v/v) and pH $9.0\pm0.2(ammonium$ chloride-ammonia buffer). The fluorescence is measured at 337 nm of emission wavelength under 300 nm of excitation wavelength. The fluorescence intensity is a linear function of the concentration of Ni(II) in the range 5-70 ng/mL, and the detection limit is 2.0 nm/mL. The proposed method has been successfully applied to the determination of trace amounts of Ni(II) in food and human hair samples.

Neutronic design of pulsed neutron facility (PNF) for PGNAA studies of biological samples

  • Oh, Kyuhak
    • Nuclear Engineering and Technology
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    • v.54 no.1
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    • pp.262-268
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    • 2022
  • This paper introduces a novel concept of the pulsed neutron facility (PNF) for maximizing the production of the thermal neutrons and its application to medical use based on prompt gamma neutron activation analysis (PGNAA) using Monte Carlo simulations. The PNF consists of a compact D-T neutron generator, a graphite pile, and a detection system using Cadmium telluride (CdTe) detector arrays. The configuration of fuel pins in the graphite monolith and the design and materials for the moderating layer were studied to optimize the thermal neutron yields. Biological samples - normal and cancerous breast tissues - including chlorine, a trace element, were used to investigate the sensitivity of the characteristic γ-rays by neutron-trace material interactions and the detector responses of multiple particles. Around 90 % of neutrons emitted from a deuterium-tritium (D-T) neutron generator thermalized as they passed through the graphite stockpile. The thermal neutrons captured the chlorines in the samples, then the characteristic γ-rays with specific energy levels of 6.12, 7.80 and 8.58 MeV were emitted. Since the concentration of chlorine in the cancerous tissue is twice that in the normal tissue, the count ratio of the characteristic g-rays of the cancerous tissue over the normal tissue is approximately 2.

A Study on the Trace Analysis of Germanium in Inorganic Matrices by Differential Pulse Polarography (Differential Pulse Polarography에 의한 무기물 시료 중 Germanium의 미량 분석에 관한 연구)

  • Shin, Ho-Sang;Oh, Yun-Suk;Shin, Hak-Soo
    • Analytical Science and Technology
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    • v.9 no.3
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    • pp.253-261
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    • 1996
  • Analytical method for the determination of trace germanium in inorganic matrices by differential pulse polarography(DPP) was studied. The reduction peak of germanium(IV) in perchloric acid solution containing 1, 2, 3-trihydroxy benzene appeared at -0.45V(vs. Ag/AgCl) and the peak current for germanium complex varied linearly with concentration variation. Factors affecting sensitivity and precision for germanium quantification were studied and detection limit under the investigated parameters was 1ng/ml. Inorganic samples were decomposed by fusion with potassium pyrosulfate. Serious interferences of Se(IV), Pb(II), As(III) for the determination of germanium were discussed. Interferences of these elements could be avoided by extraction of germanium from decomposed matrices by $CCl_4$ in 10M HCl solution. The germanium contents of inorganic samples(Pb bf. dust, Cu bf. dust, gneiss, Cu anode slime) were determined by the above method.

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Speciation Analysis of Arsenic Species in Surface Water (수중의 비소 종 분리 분석)

  • Jeong, Gwan-Jo;Kim, Dok-Chan
    • Journal of Korean Society of Environmental Engineers
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    • v.30 no.6
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    • pp.621-627
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    • 2008
  • In this study, a technique of speciation and determination of the trace inorganic arsenic(As(III) and As(V)) in water sample using HPLC-DRC-ICP-MS has been developed. Isocratic mobile phase of 10 mM ammonium nitrate and 10 mM ammonium phosphate monobasic was used and methanol(5 v/v%) was used as flushing solvent. Selection of the best flow rate of reaction gas, O$_2$, and optimization of the parameters such as pH and flow rate of mobile phase, and injection volume of sample for the separation and detection of arsenic species were carried out. The oxygen flow rate of 0.5 mL/min, pH of 9.4 and flow rate of 1.5 mL/min of mobile phase, and injection volume of sample of 100 $\mu$L were found to be the best parameters for the speciation and determination of arsenic species. The analytical features of the method were detection limit 0.10 and 0.08 $\mu$g/L, precision(RSD) 4.3% and 3.6%, and recovery 95.2% and 96.4% for As(III) and As(V), respectively. Analysis time was 4 minutes per sample. Linear calibration graphs with r$^2$ = 0.998 were obtained for both As(III) and As(V). Speciation analysis of arsenic species in the raw water samples collected from the tributary streams to Han River and main stream of Paldnag were performed by the proposed method. The concentrations of As(III) ranged from 0.10 to 0.22 $\mu$g/L and As(V) concentrations ranged from 0.44 to 1.19 $\mu$g/L, and 93.5% of total arsenic was found to be As(V).

Analysis of Trace Copper Metal at The Electrode Consisting of Carbon Nanotube using Stripping Voltammetry (벗김전압전류법을 이용한 카본나노튜브 전극에서의 구리 분석)

  • Choi, Chang-Kun;Jung, Young-Sam;Kim, Nack-Joo;Pak, Dae-Won;Chung, Kun-Yong;Kim, Lae-Hyun;Kwon, Yong-Chai
    • Korean Chemical Engineering Research
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    • v.50 no.5
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    • pp.933-937
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    • 2012
  • In the present study, we evaluate the sensitivity and optimal stripping voltammetry (SV) conditions of copper (Cu), which is one of the main trace heavy metals inducing the environmental contamination, using carbon nanotube (CNT) electrode. In addition, the reaction mechanism of stripping reaction of Cu is investigated. The electrochemical analyses such as squarewave stripping voltammetry (SWSV) and linear scan voltammetry (LSV) are used for the evaluations. As a result of that, the best SWSV conditions like squarewave amplitude of 15 mV, frequency of 60 Hz, deposition potential of -1.0V vs. Ag/AgCl and deposition time of 200s are determined with the measured Cu sensitivity of $1.824{\mu}A/{\mu}M$. As a driving force affecting the stripping reaction of Cu, surface reaction is more dominant one than diffusion. These results are compared with other reference results and it is confirmed that our suggested CNT electrode gives rise to better Cu sensitivity result than other references.