• Title/Summary/Keyword: Determination of Fe(III)

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Determination of Trace Mo(VI) in Seawater Samples by Ion Pair Formation and Solvent Extraction (이온쌍 형성-용매추출에 의한 해수 중 극미량 Mo(VI)의 정량)

  • Kim, Young-Sang;Nho, Seung-Gu;Choi, Jong-Moon
    • Analytical Science and Technology
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    • v.6 no.3
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    • pp.329-334
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    • 1993
  • The formation of Mo(VI)-alizarin red S chelate ion its extraction into an organic solvent by ion-pairing for the separarive determination of trace Mo(VI) in natural water was applied in seawater samples. Removed Fe(III) and Zn(II), and Cu(II) by precipitating with anthranilic acid at pH 4.0 and 2.0, seawater 100mL was sampled in 250mL separatory funnel. After Mo(VI)-ARS chelate ion was formed by adding 0.01M alizarin red S solution 1.0mL to the water sample of pH 4.6, 0.6% aliquat-336 chloroform solution 10mL was added and the solution was vigorously shaked for about 30 seconds to form the ion-pair between Mo(VI)-ARS and aliquat-336 perfectly. The solution was stood for about 30 minutes. And the organic phase was taken for the absorbance measurement of the ion-pair at 520nm. The content of Mo(VI) was obtained from the standard calibration curve. Several extraction conditions such as pH, adding amounts of alizarin red S and aliquat-336, and shaking and standing times were optimized and the interferences and release of concomitant ions was also studied. This procedure was applied to the analysis of Eastern and Yellow seawaters. It could be confirmed from the recoveries of over 85% in samples spiked with a given amount of Mo(VI) that this method was also quantitative in the determination of trace Mo(VI) in a seawater.

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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.

Intercomparison and Determination of Sediment by Instrumental Neutron Activation Analysis (중성자방사화분석을 이용한 퇴적물의 정량 및 비교연구)

  • 정용삼;문종화;정영주;박용준;이길용;윤윤열;이수형;김경태
    • Journal of the Korean Society of Groundwater Environment
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    • v.5 no.2
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    • pp.116-121
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    • 1998
  • For the application of study on pollution and conservation of environment determination of 33 elemental concetrations in different sediment samples were carried out using instrumental neutron activation analysis (INAA). For verification and evaluation of the analytical method, three standard reference materials (two NIST SRMs and one NRCC CRM) were chosen and the accuracy and precision of the analysis were estimated by comparison to the certified values. Under the optimum condition, the analytical procedure to apply a practical sample was estimated. Neutron irradiation of sample was done at the irradiation facilities (neutron flux, 1-3${\times}$10$\^$13/n/$\textrm{cm}^2$$.$s) of the TRIGA MARK-III and HANARO research reactor in the Korea Atomic Energy Research Institute. In addition, analysis of two IAEA's sediment was performed according to the pre-established analytical method. The analytical results of elements such as Al, As, Co, Cr, Fe, Sb and Zn by INAA were intercompared with those of WD-XRF, ICP-MS and AAS, and are relatively agreed with each other.

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Mechanism and Activation Parameters $({\Delta}H^{\neq},\;{\Delta}S^{\neq}$ and ${\Delta}V^{\neq})$ of Electron Transfer Reaction Between $Co^{II}CyDTA\;and\;Fe^{III}$CN Complex Ions (Co(II)-CyDTA와 Fe(III)-CN 착이온간의 전자이동반응에서 활성화파라미터 $({\Delta}H^{\neq},\;{\Delta}S^{\neq}$${\Delta}V^{\neq})$ 와 반응메카니즘)

  • Yu Chul Park;Seong Su Kim
    • Journal of the Korean Chemical Society
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    • v.33 no.3
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    • pp.273-280
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    • 1989
  • The spectra of the $Co^{II}CyDTA$(CyDTA: cyclohexyldiaminetetraacetic acid) complex have been measured in aqueous solution of pH = 6-13.2. The red shift of the spectrum in the more basic solution was ascribed to the transformation of $CoCyDTA^{2-}$ into $CoCyDTA(OH)^{3-}$. The equilibrium constant, $K_{OH} = [CoCyDTA(OH)^{3-}]/[CoCyDTA^{2-}][OH^-]$ was $75M^{-1}$ at $40^{\circ}C$. The electron transfer reactions of $CoCyDTA^{2-}$ and $CoCyDTA(OH)^{3-}$ with $Fe(CN)_6^{3-}$ have been studied using spectrophotometric technique in the range of pH applied to the determination of equilibrium constant. The pseudo first-order rate constants observed ($k_{obs}$) were not changed upto pH = 10.8, but increased with increasing pH in the range of pH = $10.8{\sim}13.0$. The rate law reduced in the range of pH = 6-13 was $k_{obs} = (k_3[CoCyDTA^{2-}] + k_4[CoCyDTA(OH)^{3-}])/(1+K_1[CoCyDTA^{2-}])$. The rate constants of the reactions (3a) and (3b), $k_3$ and $k_4$ respectively have been determined to be 0.529 and $4.500M^{-1}sec^{-1}$ at $40^{\circ}C$. The activation entropies (147{\pm}1.1JK^{-1} mol^{-1}$ at pH = 10.8) and activation volumes $(6.25cm^3mol^{-1}, pH = 10.8)$ increased with increasing pH, while the activation enthalpy (12.44 ${\pm}$ 0.20 kcal/mole) was independent of pH. Using the pH effect on the rate constants, the activation entropies and the activation volumes, the mechanism of the electron transfer reaction for $Co^{II}-Fe^{III}$ system was discussed.

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Determination of Chromium(VI) by Differential-Pulse Polarography with a Sodium Borate Supporting Electrolyte

  • Hong, Tae-kee;Czae, Myung-Zoon
    • Bulletin of the Korean Chemical Society
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    • v.9 no.2
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    • pp.77-80
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    • 1988
  • A suituable choice of supporting electrolyte medium for trace level determinations of chromium(VI) by differential pulse polarography is described. A comparative study suggests that sodium borate buffer is superior to ammonium acetate, ammonium tartrate, and especially to NaF which was recently known to be one of the most proper medium for the purpose. With 0.01 M borate, the best combination of high sensitivity, well-defined base line, and freedom from common interferents was attained. With $5.0{\times}10^{-7}$M Cr(VI), tenfold excesses of Cu(II) and Fe(III), and a five hundred-fold excess of $Cl^-$ do not change the peak current by more than about 1%. And the detection limit was $5.0{\times}10^{-8}$M Cr(VI).

X-Ray Absorption Spectroscopy: A Complementary Tool for Structural and Electronic Characterization of Solids

  • Jean Etourneau
    • Bulletin of the Korean Chemical Society
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    • v.19 no.1
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    • pp.5-21
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    • 1998
  • The purpose of this paper is to show that X-ray absorption spectroscopy (XANES and EXAFS) is a powerful technique for characterizing both crystalline and amorphous solids from structural (local order) and electronic point of view. The principle of this technique is briefly described by showing the main factors which must be considered for recording and fitting the experimental results. Some non-trivial examples have been selected for demonstrating that XAS spectroscopy is the only technique for bringing a definitive answer as for example: the determination of the local distortion of the $NiO_6$ octahedra in the $Li_{1-z}Ni_{1+z}O_2$ layered oxides and the evidence of the presence of copper pairs in the NASICON-type phosphate $CuZr_2 (PO_4)_3$. Are also reported some significant examples for which XAS spectroscopy is decisive with other characterization methods as (i) Raman spectroscopy for glasses (ii) Mossbauer spectroscopy for $LiNi_{1+z-t}Fe_To_2$ oxides (iii) magnetic measurements for Ce-based intermetallic compounds.

Studies on Copper (II)-Oxamidoxime Complex by Spectrophotometric Method (分光光度法에 依한 Cu(II)-Oxamidoxime의 錯物에 關한 硏究)

  • Oh, Sang O.;Do, Che-Chul
    • Journal of the Korean Chemical Society
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    • v.9 no.1
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    • pp.45-48
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    • 1965
  • Stability constant, composition of copper (II)-oxamidoxime complex were determined by spectrophotometric method. The ratio of copper (II) and oxamidoxime in the above complex was 1 : 1, and its stability constant was calculated to be $2.4{\times}10^{22}$. The complex solution gave constant absorbancy between the pH range of 4.5 to 6 at 600 $m{\mu}$ in which Beer's law applicable in the concentration range of 0.3 to 2.0 ppm studied in this work. It was noted that some metals such as Fe(III), Ni(II), Co(II), U(VI) interfere copper determination by this method.

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Synergistic Solvent Extraction of Manganese(II) by using Cupferron and Tetrabutylammonium ion (Cupferron과 Tetrabutylammonium ion을 이용한 Mn(II)의 상승용매 추출에 관한 연구)

  • In, Gyo;So, Jin-Hwan;Choi, Jong-Moon;Kim, Young-Sang
    • Analytical Science and Technology
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    • v.17 no.1
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    • pp.1-7
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    • 2004
  • The synergistic solvent extraction of Mn(II) by N-nitroso-N-phenylhydroxylamineammonium salt (cupferron) and tetrabutylammonium ion ($TBA^+$) has been studied. In the presence of $TBA^+$, over 95% Mn(II) was extracted from an aqueous solution into chloroform by the cupferron in the pH range of 4 to 10. But a part of Mn(II) was extracted with only cupferron. The ternary complex of Mn(II) was more efficiently extracted into $CH_2Cl_2$ and $CHCl_3$ than other nonpolar solvents. The extracted Mn(II) was determined in the back-extracted $HNO_3$ solution by GF-AAS. This fixed procedure was applied to the determination of trace Mn(II) in tap water samples of pH 5.0. The detection limit equivalent to 3 times standard deviation of the background absorption was 0.37 ng/mL and Mn(II) was determined with the range of 0.4 to 1.01 ng/mL in our laboratory's tap water. And the recovery was 94 to 107% in samples in which 2.0 ng/mL Mn(II) was spiked. The interferences of common concomitant elements such as Cu(II), Ca(II), Fe(III) and so on were not shown up to $10{\sim}20{\mu}g/mL$. From these results, this procedure could be concluded to be applied for the determination of trace Mn(II) in other environmental water samples.

Spectrophotometric Determination of Iron with 2-Hydroxybenzaldehyde-5-nitro-pyridylhydrazone after Separation with Amberlite XAD-7 Nonionic Resin (Amberlite XAD-7 비이온성 수지로 분리 후 2-Hydroxybenzaldehyde-5-nitro-pyridylhydrazone을 이용한 철의 분광학적 정량)

  • Park, Chan Il;Chung, Byung Doo;Jung, Duck Chae;Cha, Ki Won
    • Journal of the Korean Chemical Society
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    • v.43 no.5
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    • pp.522-526
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    • 1999
  • 2-Hydroxybenzaldehyde-5-nitro-pyridylhydrazone (2HB-5NPH) was synthesized and its application to the spectrophotometric determination of iron was studied. The reagent reacts with iron in the pH range 6.0-7.5 to form a yellow coIored 1:2 chelate which is very stable in methanol solution. Beer's law is obeyed in the concentration range 0.05∼2.0 ${\mu}gmL^{-1}$ iron and separation procedure using a short column filled with Amberlite XAD-7 nonionic chelating resin is proposed for the spectrophotometric determination of traces of iron. The influence of several ions as interference was discussed. The separation of Fe(III) ion from the mix-ture solution were carried out with the buffer solution (pH 5.0) and 0.25M HCl as eluents.

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Trace Element Analysis by Neutron Activastion Analysis in the Human Cancer Tissue (폐암조직에서 중성자 방사화 분석법을 이용한 미량 원소 분석)

  • Lim, Sang-Moo;Zo, Jae-Il;Shim, Young-Mog;Chung, Young-Ju;Cho, Seung-Yeon;Chung, Yong-Sam
    • The Korean Journal of Nuclear Medicine
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    • v.27 no.1
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    • pp.104-111
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    • 1993
  • Trace elements are important components in the biological system, as a structural material and metabolic controller. Neutron activation analysis (NAA) with high neutron flux and high energy resolution Ge (Li) detector coupled to multichannel analyzer (MCA) has been one of the most accurate method for the determination of ultra-trace level components, and is applicable to biological material. In human body, the NAA can be used for quantitation of trace elements in various organs and tissue with endocrinological and metabolic disease and industrial metal poisoning. In this study, Triga Mark III nuclear reactor in Korea Atomic Research Institute was used for quantitation of trace eleement in human lung cancer tissues by neutron activation analysis. In the squamous cell carcinoma tissues, Br, Hg, La, Sb, Sc, Cl, Fe and I content were lower than normal lung tissues, and K, Rb and Se content were higher. In the adenocarcinoma tissues, Fe, Au, La, Sc and Zn content were lower than normal lung tissues, and Rb, Co and Se content were higher. Rb content was higher in the adenocarcinoma tissues than in the squamous cell carcinoma tissues. Fe and Na content were higher in the squamous cell carcinoma tissues than in the adenocarcinoma tissues.

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