• Title/Summary/Keyword: metal ion determination

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Studies on Drug Analysis by Metal Chelate Ion. I. Colorimetric Determination of Nicotinamide with Dimethyglyoxime-Fe (II) (금속 chelate ion에 의한 의약품 정량에 관한 연구(I) Dimethylglyoxime-Fe(II)에 의한 Nicotinamide의 비색정량)

  • 이왕규
    • YAKHAK HOEJI
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    • v.13 no.1
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    • pp.22-27
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    • 1969
  • Nicotinamide Complex Compound was not formed in simple alkaline solution under two to one molar ratio of dimethyglyoxime and Fe (II), but it was formed with ammonia or pyridine under the same molar ratio. Based on this fact, nicotinamide solution was added into dimethyglyoxime-Fe (II) complex solution, and the chelation product was extracted with chloroform. The extraction was Completed in a range of pH 8.4-11.0. The chloroform solution shows stability and maximum absorption at 516 m${\mu}$.

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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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Development of Continuous Flow Microwave Digestion Procedures for Analysis of Trace Metal in Water Using Ion Chromatography

  • Youn Doo Kim;Gae Ho Lee;Hyung Seung Kim;Dong Soo Kim;Kwang Kyu Park
    • Bulletin of the Korean Chemical Society
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    • v.15 no.9
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    • pp.786-791
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    • 1994
  • A simple and rapid sample pretreatment process necessary for determination of metal oxides in water was proposed. Samples were injected into the continuous-flow tube installed inside the microwave oven and the treated samples were cooled before entered to the Ion Chromatography (IC) or Inductively Coupled Plasma (ICP). By coupling this microwave digestion system with IC or ICP, a fully automatic analytical procedures may be easily established. In this study, two different types of digestion methods were considered; the open tubing method (OTM) and the restraint tubing method (RTM). The RTM was proved to be 3 times faster in digestion period and 10 times higher in detection range than the OTM. Validation of proposed sample digestion system was carried out by using an ICP. The results showed that both of continuous-flow methods, the OTM and the RTM were comparable in accuracies with the conventional batch-type vessel digestion method.

Determination of Ag(Ⅰ) Ion with a Chemically Modified Carbon Paste Electrode Containing Cinchonidine (Cinchonidine으로 변성된 Carbon Paste 전극을 사용한 은이온의 정량)

  • Kim, Sin Hui;Won, Mi Suk;Sim, Yun Bo
    • Journal of the Korean Chemical Society
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    • v.38 no.10
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    • pp.734-740
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    • 1994
  • Electrochemical determination of Ag(I) ion was carried out by cyclic voltammetry (CV) and differential pulse voltammetry (DPV) with the carbon paste electrode (CPE) containing cinchonidine. The detection limit for Ag(I) ion was shown to be $1.0 {\times}10^{-6}$ M in conventional CV and up to $8.0{\times}10^{-9}$ M (${\pm}$0.6%) using DPV. The optimum analytical condition of Ag(I) ion was determined as follows: pH 7, 20 minutes of deposition time, and 50% (w/w) cinchonidine to carbon powder composition of electrode. The interference effect of various metal ions added to the deposition solution was also studied. The peak current of Ag(I) ion except Hg(II) ion was decreased roughly 25% compare to Ag(I) ion only. When Mn(II) ion was present in sample solution at pH 9, shown a large interference effect.

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Selective determination of mercury (II) ion in aqueous solution by chemiluminescence method (화학발광법에 의한 수용액 중의 선택적 수은(II) 이온 정량)

  • Kim, Kyung-Min;Jang, Taek-Gyun;Kim, Young-Ho;Oh, Sang-Huyb;Lee, Sang-Hak
    • Analytical Science and Technology
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    • v.24 no.4
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    • pp.243-248
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    • 2011
  • A selective determination method of mercury (II) ion in aqueous solution by luminol-based chemiluminescence system (luminol CL system) has been developed. Determination of metal ions such as copper (II), iron (III), chromium (III) ion in solution by the luminol CL system using its catalytic role in the reaction of luminol and hydrogen peroxide has been reported by several groups. In this study, the catalytic activity of mercury (II) ion in the reaction of luminol and hydrogen peroxide was observed by the enhanced CL intensity of the luminol CL system. Based on this phenomenon, experimental conditions of the luminol CL system were investigated and optimized to determine mercury (II) ion in aqueous solution. While mercury (II) ion in mixed sample solution containing mercury (I) and (II) ions highly enhanced the CL intensity of the luminol CL system, the mercury (I) ion could not enhanced the CL intensity. Thus selective determination of the mercury (II) ions in a mixture containing mercury (I) and (II) ions could be achieved. Each concentration of mercury (I) and (II) ions in aqueous solution can be obtained from the results of the CL method that give the concentration of only mercury (II) ion and the inductively coupled plasma (ICP) method that give the total concentration of mercury ions. On the optimized conditions, the calibration curve of mercury (II) ion was linear over the range from $1.25{\times}10^{-5}$ to $2.50{\times}10^{-3}M$ with correlation coefficient of 0.991. The detection limit of mercury (II) ion in aqueous solution was calculated to be $1.25{\times}10^{-7}M$.

Green flow injection spectrophotometric system for lead ion (II) evaluation in vegetables samples using new azo reagent

  • Fatimah Lateef Al-Zubaidi;Khdeeja Jabbar Ali
    • Analytical Science and Technology
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    • v.36 no.1
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    • pp.1-11
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    • 2023
  • A new, sensitive, and reliable flow injection methodology was investigated for the determination of lead ion (II) in vegetables' samples using a laboratory-prepared reagent 2-[(6-methoxy-2-benzothiazoly)azo]-4-methoxy phenol (6-MBTAMP). Infrared spectroscopy, UV-visible spectrophotometry, Energy dispersive X-ray spectroscopy (EDX), Elemental Analysis (CHN), nuclear magnetic resonance spectroscopy 1HNMR, and 13CNMR techniques were used to characterize the reagent and lead (II) complex. The method is based on lead ion (II) reacting with the reagent (6-MBTAMP) in a neutral solution to produce a green-red complex with a maximum absorbance at 670 nm. The optimum conditions, such as flow rate, lead ion (II) volume, reagent volume, medium pH, reagent concentration, and reaction coil length were thoroughly examined. The limits of detection (LOD) and quantification (LOQ) were determined to be 0.621 mg·L-1 and 2.069 mg·L-1 , respectively, while Sandell's sensitivity was determined to be 0.345 ㎍·cm-2.

Reversed-Phase Ion-Pair High Performance Liquid Chromatographic Elution Behavior of Noble Metal-Thiacrown Ether Complexes (귀금속-티아크라운에테르 착물들의 역상 이온쌍 고성능 액체크로마토그래피 용리거동)

  • Chung, Yong Soon;Kim, Dong Won;Lee, Kang Woo;Kim, Chang Seok
    • Journal of the Korean Chemical Society
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    • v.42 no.4
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    • pp.416-421
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    • 1998
  • In the reversed-phase ion-pair high performance liquid chromatographic (RPIP-HPLC) elution behavior of noble metal-thiacrown ether complexes, the effects of the concentration of ion-pairing reagent and kind of ligands were studied. It was found that the less the number of atoms in the ring of the thiacrown ether molecule was, the larger the selectivity was, and the elution mechanism of the complexes was explained due to the formation of ion-pair when the concentration of sodium dodecyl sulfate (SDS) in mobile phase was lower than 10 mM and due to the formation of micelle when the SDS concentration was higher than 10 mM. As a conclusion, separations of the noble metal-thiacrown ether complexes in an optimum separation condition were accomplished successfully and the method was proved to be an useful one for the separation and determination of Ag (Ⅰ) ion in a black-white photographic fixing solution.

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Spectrophotometric Determination of Antihistamines by Using Metal Indicators NN, EBT and Calcon as Color Developing Agents. (항 히스타민제의 흡광광도정량법)

  • 옥지원
    • YAKHAK HOEJI
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    • v.18 no.2
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    • pp.133-144
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    • 1974
  • The metal indicator, acidic azo dyes NN, EBT and Calcon are utilized to analyse quantitatively chlorpheniramine, tripelenamine and diphenhydramine forming insoluble ion pair in aqueous solution at proper pH values between the acidic azo dyes and the sample molecules, these compexes are extracted by organic polar solvents, and organic layer is determined spectrophotometrically. Generally, the absorption maxima of the complexes are shifted to longer wavelengths compare to the absorption maxima of the dyes themselves. The binding ratio of the ion pair forming complex molecules in chloroform soln, are as follows ; NN-antihistamines (chlorpheniramine, tripelennamine, diphenhydramine) are NN-1 to antihisamine-1, EBT-antihistamines are EBT-2 to antithistamines a and Calcon-antihistamines are Calcon-3 to antithistamines-1. These coomplexes in chloroform soln. are very stable, and show higher absorbance than the other organic polar solvents. The binding state of complexes were presumed intermolecular hydrogen bond by their infrared spectra. In the mixture solution of three samples, the aqueous phase is buffered at pH 1.0, and benzene is used to extract ion pair of diphenhydramine EBT complex selectively. At pH 1.0 of aqueous layer, Calon-diphenhydramine complex is also extracted selectively by benzene. However, in this case very small amount of chlorpheniramine-calcon calcon simultaneously. The binding state of diphenhydramine-EBT and diphenhydramine-calcon in benzene are smae as the complexes in chloroform. But the absorption maxima of the complexes in benzene are shifted to shorter wavelenlgths than the complexes in chloroform.

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Determination of measuring time for decision of heavy metal ion concentration in Square Wave Voltammetry with FPGA (FPGA를 이용한 네모파 전압전류법의 계측시간 분석)

  • Lee, Jaechoon
    • Journal of Korea Society of Digital Industry and Information Management
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    • v.12 no.4
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    • pp.25-31
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    • 2016
  • In this research, to analyze the concentration of heavy metal ions in water, we tried to find the measuring time at which the faradaic electric currents flowing by the pure oxidation-reduction reaction from the pushing up mercury electrode of the stripping scan square wave voltammetry(SV+SWV) methods system becomes larger than the capacitance electric current. In order to do this, a method for analyzing signals using FPGA has been designed and we conducted 120 experiments using it. As a result, when the frequency of the square wave is 40Hz, The valid potential-current signal was measured from 96.6667% to 96.7155% of the end of the pulse of the forward and reverse, and the optimal signal was measured at 96.6667%. In addition, the experiment was carried out 40 times by changing the pulse height of the square wave from 10Mv to 40Mv. As a result, at a size smaller than 40Mv, there is little change in the magnitude of the potential-current, and an invalid signal was generated when it is out of this size.