• Title/Summary/Keyword: Determination of metal ions

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Chemiluminescence System with Air Pump as a Sensor for Determination of Metal Levels in Rain

  • Hong, Hyuck-Gi;Lim, H.B.
    • Bulletin of the Korean Chemical Society
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    • v.26 no.12
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    • pp.1937-1940
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    • 2005
  • A lab-made chemiluminescence system with air pump was developed for monitoring of some metal levels in rain. The air pump enabled injection of 17.7 $\mu$g samples into a glass cell filled with luminol-$H_2O_2$ reagent of typically 300 $\mu$L for chemiluminescence measurement. The monitored trend of total metal ions in the rain collected in our campus was compared with analytical results of each metal ion from GFAAS. The system was also demonstrated to determine $Cr^{6+}$ by reduction to $Cr^{3+}$ using $SnCl_2$. The limit of detection for $Cr^{6+}$ obtained by 4 measurements was 85.0 pg $mL^{-1}$ with a relative standard deviation of 3.4%. Although this system doesn’t have selectivity due to the characteristics of chemiluminescence, application of it to environmental monitoring as a sensor for some transition metal ions was demonstrated.

NMR Studies of Metal-binding Luteinizing Hormone Releasing Hormone

  • Won, Ho-Shik
    • Bulletin of the Korean Chemical Society
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    • v.32 no.11
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    • pp.4021-4026
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    • 2011
  • Functions of the luteinizing hormone releasing hormone (LHRH) and its induced release by divalent metal ions have received great attention because this neurotransmitter subsequently regulates the secretion of luteinizing hormone (LH). Metal-LHRH complexes were synthesized by addition of various Cu(II),Ni(II),Zn(II) ions into LHRH in order to understand how the induced release of LHRH is possible. The degree of complexation was monitored by $^1H$, $^{13}C$-NMR chemical shifts, and final products were identified by Mass spectrometry. Solutionstate structure determination of Zn(II)-LHRH out of metal-complexes was accomplished by using NMR and NMR-based distance geometry (DG). Interproton distance information from nuclear Overhauser effect spectroscopy was utilized for structure determination. Structure obtained in this study has a cyclic conformation exhibiting a specific ${\alpha}$-helical turn with residue numbers His[2]-Leu[7] out of 10 amino acids. Comparison of chemical shifts and EPR studies of Ni(II),Cu(II)-LHRH complexes exhibit that these metal complexes have 4-coordination geometry.

Study on Determination of Seven Transition Metal Ions in Water and Food by Microcolumn High-Performance Liquid Chromatography

  • Hu, Qiufen;Yang, Guangyu;Li, Haitao;Tai, Xi;Yin, Jiayuan
    • Bulletin of the Korean Chemical Society
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    • v.25 no.5
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    • pp.694-698
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    • 2004
  • A new method for the simultaneous determination of seven transition metal ions in water and food by microcolumn high-performance liquid chromatography has been developed. The lead, cadmium, mercury, nickel, cobalt, silver and tin ions were pre-column derivatized with tetra-(4-aminophenyl)-porphyrin ($T_4$-APP) to form the colored chelates which were then enriched by solid phase extraction with $C_{18}$ cartridge. The enrichment factor of 50 was achieved by eluted the retained chelates from the cartridge with tetrahydrofuran (THF). The chelates were separated on a ZORBAX Stable Bound microcolumn ($2.0{\times}50\;mm,\;1.8\;{\mu}m$)with methanol-tetrahydrofuran (95 : 5, v/v, containing 0.05 mol/L pyrrolidine-acetic acid buffer salt, pH = 10.0) as mobile phase at a flow rate of 0.5 mL/min and detected with a photodiode array detector from 350-600 nm. The seven chelates were separated completely within 2.0 min. The detection limits of lead, cadmium, mercury, nickel, cobalt, silver and tin are 4 ng/L, 3 ng/L, 6 ng/L, 5 ng/L, 5 ng/L, 6 ng/L, 4 ng/L respectively in the original samples. This method was applied to the determination of the seven transition metal in water and food samples with good results.

A Study on the Alkalimetric Titration with Gran Plot in Noncomplexing Media for the Determination of Free Acid in Spent Fuel Solutions

  • 서무열;이창헌;손세철;김정숙;엄태윤
    • Bulletin of the Korean Chemical Society
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    • v.20 no.1
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    • pp.59-64
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    • 1999
  • Based on the study of hydrolysis behaviour of U(Ⅵ) ion and major fission product metal ions such as Cs(Ⅰ), Ce(Ⅲ), Nd(Ⅲ), Mo(Ⅵ), Ru(Ⅱ), and ZR(Ⅳ) in the titration media, the performance of noncomplexing-alkalimetric titration method for the determination of free acid in the presence of these metal ions was investigated and its results were compared to those from the completing methods. The free acidities could be determined as low as 0.05 meq in uranium solutions in which the molar ratio of U(Ⅵ)/H+ was less than 5, when the end-point of titration was estimated by Gran plot. The biases in the determinations were less than 1% and about +3% respectively for 0.4 meq and 0.05 meq of free acid at the U(Vl)/H+ molar ratio of up to 5. Applicability of this method to the determination of free acid in spent fuel solutions was confirmed by the analysis of nitric acid content in simulated spent fuel solutions and in a real spent fuel solution.

Determination of Trace Metals in Waters by FAAS after Enrichment as Metal-HMDTC Complexes Using Solid Phase Extraction

  • Tokalioglu, Serife;Kartal, Senol;Elci, Latif
    • Bulletin of the Korean Chemical Society
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    • v.23 no.5
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    • pp.693-698
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    • 2002
  • A method has been described for the determination of Cu(Ⅱ), Pb(Ⅱ), Ni(Ⅱ), Cd(Ⅱ), Mn(Ⅱ) and Fe(Ⅲ) by flame atomic absorption spectrometry (FAAS) after preconcentration on Amberlite XAD-16 resin, using hexamethyleneammonium-hexamethylenedithiocarbamate (HMA-HMDTC) as a chelating agent, and NH3/NH4Cl buffer solution (pH 9). Influences of various analytical parameters such as pH, concentration of nitric acid, amount of analytes, diverse ions and sample volume were investigated. The relative standard deviation (RSD) and the detection limit (LOD) were found in the range of 0.8-2.9% and 0.006-0.277 ㎍/mL,respectively. Recoveries obtained by the column method were quantitative ( >95%) at optimum conditions.The method was applied to the determination of some metal ions in seawater and wastewater samples. A high preconcentration factor (about 150 for seawater and 75 for wastewater samples) and simplicity are the main advantages of this suggested method.

Property about Extraction of Metal Ion in the Synthesized Crown Ether Model Compounds (합성한 crown ether 모델 화합물에서 금속이온의 추출 특성 연구)

  • Lee, Yong-Hee;Suh, Myung-Gyo;Roh, Jong-Su;Lee, Kook-Eui;Lee, Young-Sei
    • Journal of the Korean Society of Industry Convergence
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    • v.6 no.3
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    • pp.165-169
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    • 2003
  • To extract alkali metal ions and heavy metal ions, search for crown ether model compounds (4a-b, 5a-b, 6a-b) bearing side arm has led to achieve in 5~6 steps starting from 2,6-dimethylaniline. The determination of structure in their compound derivatives were on the basis of melting point and nuclear magnetic resonance spectroscopy. In the solvent extraction of metal ions from the synthesized derivatives, we observed that silver ion has only high selectivity for synergistic ligation of crown ether.

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Voltammetric Determination of Copper(II) at Chemically Modified Carbon Paste Electrodes Containing Alga

  • Bae, Zun-Ung;Kim, Young-Lark;Chang, Hye-Young
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.611-615
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    • 1995
  • The design of appropriate chemically modified electrodes should allow development of new voltammetric measurement schemes with enhanced selectivity and sensitivity. Microorganism like algae has high ability to trap toxic and heavy metal ions and different affinities for metal ions. A copper(II) ion-selective carbon paste electrode was constructed by incorporating alga Anabaena into a conventional carbon paste mixture, and then the film of 10% Nafion was coated to avoid the swelling of the electrode surface. Copper ion could be deposited at the 25% algamodified electrode for 15 min without the applied potential while stirring the solution by only immersing the electrode in a buffer (pH 4.0) cot1taining copper(II). Temperature was controlled at $35^{\circ}C$. After preconcentration was carried out the electrode was transferred to a 0.1 M potassium chloride solution and was reduced at -0.6 volt at $25^{\circ}C$. The differential pulse anodic stripping voltammetry was employed. A well-defined oxidation peak could be obtained at -0.1 volt (vs SCE). In five deposition / measurement / regeneration cycles, the responses were reproducible and relative standard deviations were 3.3% for $8.0{\times}10^{-4}M$ copper(II). Calibration curve for copper was linear over the range from $2.0{\times}10^{-4}M$ to $1.0{\times}10^{-3}M$. The detection limit was $7.5{\times}10^{-5}M$. Studies of the effect of diverse ions showed that the coexisting metal ions had little or no effect for the determination of copper. But anions such as cyanide. oxalate and EDTA seriously interfered.

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Pulsed Amperometric Detection of Metal Ions Complexing with EDTA in a Flow Injection System

  • 이준우;여인형;편종홍
    • Bulletin of the Korean Chemical Society
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    • v.18 no.3
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    • pp.316-318
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    • 1997
  • A general and universal detection method, which can be used in high performance liquid chromatography (HPLC) and flow injection analysis (FIA) system for the determination of any metal ions complexing with ethylenediaminetetraacetic acid (EDTA), is demonstrated. Pulsed amperometric detection scheme is applied in a flow-through thin layer electrochemical cell at an Au working electrode. Fluctuation of peak current level at the same flow rate of carrier solution is minimized at this solid working electrode, whereas not at a dropping mercury electrode. Removal of dissolved oxygen can be omitted with this detection method, which is a required step for cathodic detection methods. Also, a group of metal ions can be determined selectively and indirectly with this detection scheme.