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

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Extraction of Water-Soluble Porphyrin and Metalloporphyrins into Acetonitrile by Salting-out

  • Tabata, Masaaki;Kumamoto, Midori
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.511-517
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    • 1995
  • A cationic water soluble porphyrin (5,10,15,20-tetrakis (l-methyl-pyridinium-4-yl)porphyrin, $H_2tmpyp^{4+}$) and its metalloporphyrins (MP) were easily extracted into acetonitrile separated by addition of sodium chloride ($4mol\;dm^{-3}$) in the presence of sodium perchlorate, where M denotes $Zn^{2+}$, $Cu^{2+}$, $Co^{3+}$, $Fe^{3+}$, and $Mn^{3+}$ and $P^{2-}$ is porphyrinate ion. The extracted ion-pair complexes were completely dissociated to $[MP(ClO_4)_3]^+$, and $[MP(ClO_4)_2]^{2+}$. The extraction and the dissociation constants were determined by taking into account of the partition constant of sodium perchlorate ($K_D=1.82{\pm}0.01$). The chemical properties of the separated acetonitrile phase as $E_{T(30)}$ and $D_{II,I}$ were determined and compared with other water miscible solvents (acetone, actonitrile, 1,4-dioxane, tetrahydrofuran, 1-propanol and 2-propanol). Furthermore, a sensitive and selective method was proposed for the determination of a subnanogram amount of copper(II) in natural water samples by using the present salting-out method and the porphyrins.

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IS CALCIUM II TRIPLET A GOOD METALLICITY INDICATOR OF GLOBULAR CLUSTERS IN EARLY-TYPE GALAXIES?

  • CHUNG, CHUL;YOON, SUK-JIN;LEE, SANG-YOON;LEE, YOUNG-WOOK
    • Publications of The Korean Astronomical Society
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    • v.30 no.2
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    • pp.489-490
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    • 2015
  • We present population synthesis models for the calcium II triplet (CaT), currently the most popular metallicity indicator, based on high-resolution empirical spectral energy distributions (SEDs). Our new CaT models, based on empirical SEDs, show a linear correlation below [Fe/H] ~ -0.5, but the linear relation breaks down in the metal-rich regime by converging to the same equivalent width. This relation shows good agreement with the observed CaT of globular clusters (GCs) in NGC 1407 and the Milky Way. However, a model based on theoretical SEDs does not show this feature of the CaT and fails to reproduce observed GCs in the metal-rich regime. This linear relation may cause inaccurate metallicity determination for metal-rich stellar populations. We have also confirmed that the effect of horizontal-branch stars on the CaT is almost negligible in models based on both empirical and theoretical SEDs. Our new empirical model may explain the difference between the color distributions and CaT distributions of GCs in various early-type galaxies. Based on our model, we claim that the CaT is not a good metallicity indicator for simple stellar populations in the metal-rich regime.

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).

Determination of Mefenamic Acid with Fe(II)-Dipyridyl-Mefenamic Acid Ternary Complex as Ion-exchagner (철-디피리딜-메페남산 삼원착물을 이용한 메페남산의 정량)

  • Nam, Su Ja;Moon, Hyun Sook;Lee, Mi Na;Jung, Moon Mo;Hur, Moon Hye;Ahn, Moon Kyu
    • Analytical Science and Technology
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    • v.14 no.1
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    • pp.59-63
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    • 2001
  • A PVC membrane electrodes based on Fe(II)-dipyridyl-mefenamic acid ternary complex as ion exchanger were prepared using o-nitrophenyl octyl ether as a plasticizer. The 2,2'-dipyridyl, 4,4'-dipyridyl and 4,4'-dipyridyl-2,2'-dipyridyl were used as dipyridyl derivative ligand. The electrode dxhibits a fast stable and linear response for $10^{-5}-10^{-3}mol/L$ mefenamate with an anionic slope of -55.98, -49.47, -59.35mV/decade in pH 8.9 borate buffer solution respectively. Potentiometric selectivity measurements revealed negligible interferences from aromatic and aliphatic carboxylic acid salts.

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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.

Simple Semiquantitative Determination and Selective Preconcentration of Trace Heavy Metals in Environmental Pollutants : Determination of Chromium (VI) with DPC Gel (環境汚染 重金屬의 選擇的 濃縮 및 簡易分析法 : DPC 겔의 의한 크롬 (VI) 의 定量)

  • Yong Keun Lee;Kyu Ja Whang;In Hwa Woo
    • Journal of the Korean Chemical Society
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    • v.25 no.4
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    • pp.275-282
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    • 1981
  • A simple semiquantitative procedure was developed for the determination of sub-ppm level of chromium(VI) in aquatic samples by using an analytical micro-column packed with diphenylcarbazide(DPC) gel beads. DPC gel beads were prepared by swelling XAD-2 resin(115∼150 mesh in dry condition) in ethanol for 10min, packing into a glass column(1.5 mm bore, 65nm length) and adsorbing 1ml of ethanol solution of $2{\times}10^{-3}M$ DPC for 20min at room temperature. When 0.5ml of ethanol solution containing chromium(VI) was passed through the DPC gel column for 40min, the original white color of the reagent gel turned to red-violet from the up-stream of the column. As the length of colored band was proportional to the total amount of chromium(VI) in the sample solution passed through the column, the concentration of chromium(VI) could be determined from the calibration line which had been prepared by using the standard solution. Chromium(VI) ion as small as from 0.1 to 0.8 ppm could be determined with ${\pm}5{\sim}{\pm}15{\%}$ relative errors. Since other interfering cations were few, 100-fold excess of Fe(III), 50-fold excess of Cu(II) could be masked with EDTA. This method was successfully applied to the analysis of chromium(VI) in industrial effluents.

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Studies on X-Ray Fluorescence Analysis of Sulfide Ores by Solution Technique (II). Analysis of Iron, Copper and Cobalt (용액법을 이용한 황화광석의 X-선 형광분석에 관한 연구 (제2보). 철, 구리 및 코발트의 분석)

  • Young-Sang Kim;Kee-Chae Park
    • Journal of the Korean Chemical Society
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    • v.26 no.5
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    • pp.320-325
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    • 1982
  • Utilyzing the solution prepared for the sulfur determination, the amounts of iron, copper and cobalt in the sulfide ore were determined by X-ray fluorescence spectrometry. The samples were dissolved with the mixed solutions of ,$Br_2\;and\;HNO_3$ and a major constituent of $SiO_2$was repelled from the solution by HF treatment several times. The analytical results agreed with the data obtained by conventional methods within ${\pm}$1.5% for Fe of the range of 20 to 50%, ${\pm}$1.0% for Cu of 10 to 15%, and ${\pm}$0.4% for Co of 1 to 5%. The present method was tolerably found to be reproducible.

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Biochemical Characterization of the Dual Positional Specific Maize Lipoxygenase and the Dependence of Lagging and Initial Burst Phenomenon on pH, Substrate, and Detergent during Pre-steady State Kinetics

  • Cho, Kyoung-Won;Jang, Sung-Kuk;Huon, Thavrak;Park, Sang-Wook;Han, Ok-Soo
    • BMB Reports
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    • v.40 no.1
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    • pp.100-106
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    • 2007
  • The wound-inducible lipoxygenase obtained from maize is one of the nontraditional lipoxygenases that possess dual positional specificity. In this paper, we provide our results on the determination and comparison of the kinetic constants of the maize lipoxygenase, with or without detergents in the steady state, and characterization of the dependence of the kinetic lag phase or initial burst, on pH, substrate, and detergent in the pre-steady state of the lipoxygenase reaction. The oxidation of linoleic acid showed a typical lag phase in the pre-steady state of the lipoxygenase reaction at pH 7.5 in the presence of 0.25% Tween-20 detergent. The reciprocal correlation between the induction period and the enzyme level indicated that this lag phenomenon was attributable to the slow oxidative activation of Fe (II) to Fe (III) at the active site of the enzyme as observed in other lipoxygenase reactions. Contrary to the lagging phenomenon observed at pH 7.5 in the presence of Tween-20, a unique initial burst was observed at pH 6.2 in the absence of detergents. To our knowledge, the initial burst in the oxidation of linoleic acid at pH 6.2 is the first observation in the lipoxygenase reaction. Kinetic constants (Km and kcat values) were largely dependent on the presence of detergent. An inverse correlation of the initial burst period with enzyme levels and interpretations on kinetic constants suggested that the observed initial burst in the oxidation of linoleic acid could be due to the availability of free fatty acids as substrates for binding with the lipoxygenase enzyme.

Understanding of a Korean Standard for the Analysis of Hexavalent Chromium in Soils and Interpretation of their Results (토양오염공정시험기준 6가크롬 분석의 이해와 결과 해석)

  • Kim, Rog-Young;Jung, Goo-Bok;Sung, Jwa-Kyung;Lee, Ju-Young;Jang, Byoung-Choon;Yun, Hong-Bae;Lee, Yee-Jin;Song, You-Seong;Kim, Won-Il;Lee, Jong-Sik;Ha, Sang-Keun
    • Korean Journal of Soil Science and Fertilizer
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    • v.44 no.5
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    • pp.727-733
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    • 2011
  • A new Korean standard for the determination of Cr(VI) in soils has been officially published as ES 07408.1 in 2009. This analytical method is based on the hot alkaline digestion and colorimetric detection prescribed by U.S. EPA method 3060A and 7196A. The hot alkaline digestion accomplished using 0.28 M $Na_2CO_3$ and 0.5 M NaOH solution (pH 13.4) at $90{\sim}95^{\circ}C$ determines total Cr(VI) in soils extracting all forms of Cr(VI), including water-soluble, adsorbed, precipitated, and mineral-bound chromates. This aggressive alkaline digestion, however, proved to be problematic for certain soils which contain large amounts of soluble humic substances or active manganese oxides. Cr(III) could be oxidized to Cr(VI) by manganese oxides during the strong alkaline extraction, resulting in overestimation (positive error) of Cr(VI). In contrast, Cr(VI) reduction by dissolved humic matter or Fe(II) could occur during the neutralization and acidic colorimetric detection procedure, resulting in underestimation (negative error) of Cr(VI). Futhermore, dissolved humic matter hampered the colorimetric detection of Cr(VI) using UV/Vis spectrophotometer due to the strong coloration of the filtrate, resulting in overestimation (positive error) of Cr(VI). Without understanding the mechanisms of Cr(VI) and Cr(III) transformation during the analysis it could be difficult to operate the experiment in laboratory and to evaluate the Cr(VI) results. For this reason, in this paper we described the theoretical principles and limitations of Cr(VI) analysis and provided useful guidelines for laboratory work and Cr(VI) data analysis.

Quantitative Elemental Analysis in Soils by using Laser Induced Breakdown Spectroscopy(LIBS) (레이저유도붕괴분광법을 활용한 토양의 정량분석)

  • Zhang, Yong-Seon;Lee, Gye-Jun;Lee, Jeong-Tae;Hwang, Seon-Woong;Jin, Yong-Ik;Park, Chan-Won;Moon, Yong-Hee
    • Korean Journal of Soil Science and Fertilizer
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    • v.42 no.5
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    • pp.399-407
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    • 2009
  • Laser induced breakdown spectroscopy(LIBS) is an simple analysis method for directly quantifying many kinds of soil micro-elements on site using a small size of laser without pre-treatment at any property of materials(solid, liquid and gas). The purpose of this study were to find an optimum condition of the LIBS measurement including wavelengths for quantifying soil elements, to relate spectral properties to the concentration of soil elements using LIBS as a simultaneous un-breakdown quantitative analysis technology, which can be applied for the safety assessment of agricultural products and precision agriculture, and to compare the results with a standardized chemical analysis method. Soil samples classified as fine-silty, mixed, thermic Typic Hapludalf(Memphis series) from grassland and uplands in Tennessee, USA were collected, crushed, and prepared for further analysis or LIBS measurement. The samples were measured using LIBS ranged from 200 to 600 nm(0.03 nm interval) with a Nd:YAG laser at 532 nm, with a beam energy of 25 mJ per pulse, a pulse width of 5 ns, and a repetition rate of 10 Hz. The optimum wavelength(${\lambda}nm$) of LIBS for estimating soil and plant elements were 308.2 nm for Al, 428.3 nm for Ca, 247.8 nm for T-C, 438.3 nm for Fe, 766.5 nm for K, 85.2 nm for Mg, 330.2 nm for Na, 213.6 nm for P, 180.7 nm for S, 288.2 nm for Si, and 351.9 nm for Ti, respectively. Coefficients of determination($r^2$) of calibration curve using standard reference soil samples for each element from LIBS measurement were ranged from 0.863 to 0.977. In comparison with ICP-AES(Inductively coupled plasma atomic emission spectroscopy) measurement, measurement error in terms of relative standard error were calculated. Silicon dioxide(SiO2) concentration estimated from two methods showed good agreement with -3.5% of relative standard error. The relative standard errors for the other elements were high. It implies that the prediction accuracy is low which might be caused by matrix effect such as particle size and constituent of soils. It is necessary to enhance the measurement and prediction accuracy of LIBS by improving pretreatment process, standard reference soil samples, and measurement method for a reliable quantification method.