• Environmental Engineering Research
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• 제22권2호
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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.

• Bulletin of the Korean Chemical Society
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• 제32권11호
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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).

• Bulletin of the Korean Chemical Society
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• 제25권8호
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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.

• 대한전기학회논문지:전기물성ㆍ응용부문C
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• 제54권12호
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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.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2013년도 제44회 동계 정기학술대회 초록집
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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.

• Bulletin of the Korean Chemical Society
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• 제21권5호
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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.

• Nuclear Engineering and Technology
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• 제54권1호
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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.

• 분석과학
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• 제9권3호
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• pp.253-261
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• 1996

무기시료 중에 게르마늄의 DPP에 의한 미량 분석법이 연구되었다. 1, 2, 3-트리하이드 록시벤젠이 함유된 과염소산 용액 중에 게르마늄(IV)의 환원 피크가 -0.45V(기준전극 Ag/AgCl)에서 나타났고, 이 피크의 높이는 농도에 직선성을 보였다. 게르마늄 분석시에 감도 및 정밀도에 영향을 주는 인자들이 조사되었고, 최적 조건하에서 검출한계는 1ng/ml였다. 무기물 시료들은 potassium pyrosulfate를 사용한 용융법으로 분해하였다. 게르마늄 검출시 Se(IV), Pb(II), As(III)의 간섭에 대한 조사가 있었고, 이들 간섭은 10M HCl용액 중에서 $CCl_4$로 추출함으로써 해결할 수 있었다. 무기물 시료들 (Pb bf. dust, Cu bf. dust, 편마암, Cu anode slime)중의 게르마늄 함량은 위의 방법으로 정량되었다.

• 대한환경공학회지
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• 제30권6호
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• pp.621-627
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• 2008

본 연구에서는 물속 As(III)와 As(V)의 종 규명분석에 필요한 HPLC와 DRC-ICP-MS의 최적조건을 설정하고, 이를 이용하여 한강 팔당수계 10개 지류 천으로부터 채취한 시료중의 As(III)와 As(V)를 분석 검토하였다. 종 분리를 위한 HPLC의 이동상으로는 10 mM ammonium nitrate와 10 mM ammonium phosphate monobasic을 사용하였으며, flushing solvent로는 5% v/v 메탄올을 사용하였다. 검출기는 DRC-ICP-MS를, 반응기체는 산소를 사용하였다. 최적 분석조건을 설정하기 위하여 이동상의 pH, 유량 및 시료 주입량과 DRC의 산소 유량을 달리하여 검토한 결과, 이동상의 pH는 9.4, 유량은 1.5 mL/min, 시료 주입량은 100 $\mu$L, 산소의 유량은 0.5 mL/min이었을 때 가장 좋은 분석조건으로 나타났다. 검정곡선은 As(III)와 As(V)에 대해 모두 r$^2$ = 0.998 이상의 선형성을 나타냈으며, As(III)의 검출한계는 0.10 $\mu$g/L, 정확도(RSD)는 4.3%, 회수율은 95.2%, As(V)의 검출한계는 0.08 $\mu$g/L, 정확도(RSD)는 3.6%, 회수율은 96.4%로 나타났다. 분석시간은 4분이었다. 설정된 파라미터를 적용하여 한강 팔당수계 유입 10개 지류 천에서 채수한 시료를 분석한 결과, As(III)는 0.10$\sim$0.22 $\mu$g/L, As(V)는 0.44$\sim$1.19 $\mu$g/L의 범위로 나타났으며, 총 비소의 93.5%가 As(V)의 형태인 것을 확인할 수 있었다.

• Korean Chemical Engineering Research
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• 제50권5호
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• pp.933-937
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• 2012

본 연구에서는 환경오염을 발생시키는 주요한 중금속 물질의 하나인 구리를 상대적으로 쉽게 검출하기 위해, CNT 전극 및 벗김전압전류법을 이용하여 구리 금속의 감도 향상을 위한 최적조건 및 민감도를 평가하였다. 또한 구리의 벗김반응이 발생될 때의 반응 메카니즘에 대한 연구도 수행하였다. 이를 위해, 네모파 벗김전압전류법 및 선형주사 전압 전류법등의 전기화학적 분석법이 이용되었다. 평가 결과, 네모파 벗김전압전류법의 최적조건으로, 15 mV의 네모파증폭율, 60 Hz의 주파수, -1.0V vs. Ag/AgCl의 석출전위 및 200초의 석출시간이 결정되었다. 구리 금속의 민감도를 측정한 결과 $1.824{\mu}A/{\mu}M$의 민감도를 얻을 수 있었다. 선형주사 전압전류법을 이용하여 구리의 벗김반응에 영향을 끼치는 인자를 평가하였을 때, 확산반응 보다는 표면반응이 구리의 벗김반응 성능에 영향을 끼치는 것으로 측정되었다. 이러한 전기화학적 분석 결과가 다른 참고문헌들과 비교되어졌고, 구리금속의 민감도 측면에서 본 연구에서 제안한 CNT 전극의 우수함이 입증되었다.