• Title/Summary/Keyword: Lead determination

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Determination of Lead(II) at Nation-Coated Glassy Carbon Electrodes Modified by Tetren-Glycerol (Nafion-Tetren-Glycerol이 수식된 유리탄소전극에서 납(II) 이온의 정량)

  • 반옥기;박은희;정근호
    • Journal of Environmental Health Sciences
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    • v.29 no.2
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    • pp.62-68
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    • 2003
  • Differential pulse voltammetry (DPV) using nafion-coated glassy carbon electrodes modified with Tetren(tetraethylene pentamine)-glycerol showed sensitivity for determining lead (II) at low concentration. The Lead (II) was accumulated on the electrode surface by the formation of the complex in an open circuit, and the resulting surface was characterized by medium exchange, electrochemical reduction, and differential pulse voltammetry. Various experimental parameters, such as the composition of modifier, preconcentration time, pH of electrolyte (0.1 M acetate buffer), and parameters of differential pulse voltammetry, were optimized. The initial potential was applied for 50 s, the electrode was scanned from -0.9 to -0.3 V, and the anodic peak current was measured at -0.604 V $\pm$ 0.015 V (vs. Ag/AgCl). The calibration plot was obtained in the range 1.0$\times$10$^{-8}$ M~l.0$\times$10$^{-6}$ M with pH 4.5 buffer solution. The detection limit (3$\sigma$) it as low as 5.0$\times$ 10$^{-9}$ M. This method is applied to the determination of lead(II) in a certified reference material and the result agrees satisfactorily with the certified value.

A Fundamental Study on the Pyrometallurgical Debismuthizing of Lead (粗鉛의 乾式 脫蒼鉛에 관한 基礎的 硏究)

  • Koh, Chang-Shik
    • Journal of the Korean Chemical Society
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    • v.6 no.2
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    • pp.143-147
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    • 1962
  • As a part of "the Fundamental Study of Pyrometallurgical Debismuthizing of Lead", the author has studied liquid Pb-Bi, Pb-Na, Bi-Na binaries and Pb-Bi-Na ternary including Pb rich side composition which forms a basis of the Dittmer method. In this study, debismuthizing mechanism of the Dittmer method pertaining to the lead rich corner of the system studied was classified by the results of thermal analysis, solubility determination of Bi and Na in liquid Pb and debismuthizing test by adding metallic sodium. For instance eutectic trough in lead rich corner of Pb-Bi-Na ternary relating to the Dittmer method was determined.

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Indirect Determination of Nitrite by Flame Atomic Absorption Spectrometry Using a Lead(IV) Dioxide Oxidant Microcolumn

  • Noroozifar, Meissam;Khorasani Motlagh, Mozhgan;Taheri, Aboozar;Homayoonfard, Marjan
    • Bulletin of the Korean Chemical Society
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    • v.27 no.6
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    • pp.875-880
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    • 2006
  • A new, simple and fast flow injection analysis (FIA) method has been developed for the indirect determination of nitrite. The proposed indirect automatic method is based on the oxidation of nitrite to nitrate using a lead(IV) dioxide oxidant microcolumn where the flow of the sample through the microcolumn reduces the $PbO_2$ solid phase reagent to Pb(II), which is measured by flame atomic absorption spectrometry. The absorbance of Pb(II) are proportional to the concentration of nitrite in the samples. The calibration curve was linear up to 30 mg $L ^{-1}$, with a detection limit of 0.11 mg $L ^{-1}$ for a 400 mL injected sample volume and a sampling rate of about 80 $h ^{-1}$. The results exhibit no interference from the presence of large amounts of ions. The developed procedure was found to be suitable for the determination of nitrite in foodstuffs and wastewaters. A relative standard deviation better than 0.9% was obtained in a repeatability study. The reliability of the method was established by parallel determination against the standard method.

Matrix Modification for Graphite Furnace Atomic Absorption Spectrophotometric Determination of Volatile Elements (Ⅰ). Determination of Trace Lead by Graphite Furnace Atomization (휘발성 원소들의 원자흡수 분광분석을 위한 매트릭스 개선에 관한 연구 (제 1 보). 흑연로 원자화에 의한 흔적량 납의 정량)

  • Choi, Jong Moon;Choi, Ho Sung;Kim, Young Sang
    • Journal of the Korean Chemical Society
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    • v.39 no.3
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    • pp.204-212
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    • 1995
  • The graphite furnace atomic absorption spectrophotometric determination of trace lead in water samples was studied using matrix modifiers. In order to modify the sample matrix, the type and optimum amount of the modifier were investigated with a given concentration of Pb solution. In fact, if the matrix is not modified, lead has low ashing and atomization temperatures as to give a low absorbance with bad reproducibility because of its volatility. Therefore, optimum modifiers should be used to stabilize the atomization. In this work, the ashing and atomization temperatures were raised from 400 and $1800^{\circ}C$, to 1,000 and $2000^{\circ}C$, by the addition of palladium to 50 ng/mL lead solution as a modifier. The concentration of palladium was 5.0 ${\mu}g/mL$ in the modified solution. Furthermore, if 1.5 ${\mu}g/mL$ of aluminum was mixed with the palladium modifier as an auxiliary modifier, the ashing temperature could be increased $150^{\circ}C$ additionally. With such a treatment, the sensitivity was improved more than 5 times of the solution unmodified and the reproducible results of less than 5% RSD were obtained in the samples of university's waste water and pipe-washing tap water. It could be concluded that this procedure was quantitative in the determination of trace lead from the recoveries of more than 88% obtained in the samples in which a given amount of lead was spiked.

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X-Ray Diffractometric Study on Modification Mechanism of Matrixes for Electrothermal AAS Determination of Volatile Lead and Bismuth

  • Kim, Yeong Sang;Choe, Jong Mun
    • Bulletin of the Korean Chemical Society
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    • v.21 no.1
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    • pp.56-60
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    • 2000
  • The mechanism of a matrix modification for the trace determination of volatile lead and bismuth by an electro-thermal atomic absorption spectrophotometry was studied by a X-ray diffractometry (XRD). For the investigation of structures, the ash products of the elements were produced by using a palladium as a matrix modifier with or without aluminum or nickel as an auxiliary modifier. The same charring conditions as in the analysis of samples were applied together with much concentrated solution of analytical elements and modifiers in a graphite furnace to get a large amount of the product for XRD. The XRD patterns showed PbPd3 for lead and BiPd3 for bismuth. These mean that the reaction procedures through the charring and atomization were changed from $Pb^{2+}$ ${\rightarrow}$ PbO ${\rightarrow}$$Pb^0$ to $Pb^{2+}$ ${\rightarrow}$ PbO ${\rightarrow}PbPd_3$ ${\rightarrow}$ Pb o for lead and from $Bi^{3+}$ ${\rightarrow}$ BiO ${\rightarrow}$ Bi o to $Bi^{3+}$ ${\rightarrow}$ BiO ${\rightarrow}$ $BiPd_3$ ${\rightarrow}$ $Bi^0$ for bismuth by the addition of modifiers. The volatile elements were stabilized by the formation of palladium alloys through a charring process. Charring temperatures were raised about 500 $^{\circ}C$ by the alloying and the atomization was also stabilized for the enhancement of sensitivities.

Studies on the Micro-determination of Metals by Spetrophotometry (II) Micro-determination of pb by Dithizone Method (Spectrophotometer에 의한 금속의 최상정량법에 관한 연구 (제 2 보) Dithizone에 의한 Pb의 미량정량법)

  • 노일협
    • YAKHAK HOEJI
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    • v.5 no.1
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    • pp.24-26
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    • 1960
  • Micro-determination of Lead by Dithizone Method was studied as follows: 1) Max. absorption wave length of Dithizone-pb complex in CC $l_{4}$ soln. is 510m.mu., 2) at the range of 5.gamma.-120.gamma. pb content, Bourguer-Beer's law hold good, 3) co-existence of F $e^{++}$ Z $n^{++}$, and C $u^{++}$ interfere.rfere.

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Preparation of L-cysteine Salicylaldehyde Schiff-base Modified Macroporous Polystyrene Resin and Its Application to Determination of Trace Cadmium and Lead in Environmental Water Samples

  • Xie, Fazhi;Zhang, Fengjun;Xuan, Han;Ge, Yejun;Wang, Yin;Li, Guolian;Zhu, Lei;Oh, Won-Chun
    • Journal of the Korean Ceramic Society
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    • v.51 no.5
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    • pp.472-476
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    • 2014
  • In this work, a new method that utilizes L-cysteine salicylaldehyde Schiff-base modified macroporous polystyrene resin (PS-CSC) as an effective sorbent has been developed for preconcentration of trace cadmium and lead in environmental water samples. The effect of pH, the contact time, the elution conditions, the flow rate, the initial concentration of target metal ions, and the effects of interfering ions on the preconcentration of the analytes were investigated. The maximum adsorption capacity of PS-CSC under optimum conditions for cadmium and lead were found to be 6.03 - 18.17 mg/g and 12.58 - 36.13 mg/g when the initial concentration of metal ions between 5.0 - 90 mg/L. The limits of detection for cadmium and lead were 2.46 ng/L and $0.52{\mu}g/L$, with a preconcentration factor of 200. The developed method has been validated by analyzing certified reference material and successfully applied for the enrichment and determination of trace cadmium and lead from environmental water samples.