• Bulletin of the Korean Chemical Society
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• v.25 no.8
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• pp.1125-1129
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• 2004

This work assesses the potential of natural Analcime Zeolite as an adsorbent for preconcentration of lead (II) traces. Lead is quantitatively retained on 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol by column method with Analcime in the pH range of 5-6.5 and 2 mL $min^{?1}$ flow rate. Lead was removed from the column with 10.0 mL of 4 M hydrochloric acid and was determined by anodic stripping differential pulse voltammetry. 0.5ppb detection limit was obtained and linear dynamic range was 3 to $1.2{\times}10^5$ ppb in final solution with correlation coefficient of 0.999 and relative standard deviation of ${\pm}$ 1.2% (for eight replicate determination of 2.5 ${\mu}g\;mL^{?1}$ of lead). Various parameters such as the effect of pH, flow rate, instrumental conditions and interferences of some ions on the determination of lead have been studied in detail for optimization of conditions. The method was successfully applied for determination of lead in various samples.

• Journal of Industrial and Engineering Chemistry
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• v.67
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• pp.461-468
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• 2018

A highly sensitive, selective and rapid method for the determination of lead based on the reaction of lead (II) with 5-(4'-chlorophenylazo)-6-hydroxypyrimidine-2,4-dione (CPAHPD) and the solid phase extraction of the Pb(II)-CPAHPD complex with Amberlite XAD-2000 was developed, in the presence of pH 5.6 buffer solution and Triton X-114 medium. CPAHPD reacts with lead to form a violet complex with a molar ratio of 2:1 (CPAHPD to lead). This complex was enriched by the solid phase extraction with Amberlite XAD-2000. An enrichment factor of 500 was obtained by elution of the complex from the resin with a minimal amount of isopentyl alcohol(0.2 mL). In isopentyl alcohol medium,the molar absorptivity of the complex is $1.13{\times}10^6L\;mol^{-1}cm^{-1}$ at 647 nm. Beer's law is obeyed in the range of $5.0-160ng\;mL^{-1}$ in the measured solution. The relative standard deviation for 10 replicate samples of $50ng\;mL^{-1}$ level is 1.26%. The detection and quantification limits reaches 1.5 and $4.7ng\;mL^{-1}$ in the original samples. The presented procedure was successfully applied for determination of lead content in real samples such as vegetables, waters, biological and soil samples with satisfactory results.

• Proceedings of the Korean Environmental Health Society Conference
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• 2003.06a
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• pp.204-207
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• 2003

Determination of Lead(II) using nafion-DTPA (diethylene triamine pentaacetic acid)-glycerol-modified glassy carbon electrodes is described. Lead(II) is accumulated at the electrode by complexing with the DTPA, reduced, and detected by differential pulse voltammetry. In this study, we demonstrate that at a preconcentration time of 5min the nafion-DTPA-glycerol-modified glassy carbon electrode has a linear calibration curve at range 1.0${\times}$10$\^$-9/M∼1.0${\times}$10$\^$-7/M in pH 4.0 buffer solution. The detection limit(3$\sigma$) is as low as 5.0${\times}$10$\^$-6/M. This method is applied to the determination of lead(II) in certified reference material and the result agrees satisfactorily with the certified value.

• Analytical Science and Technology
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• v.10 no.4
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• pp.240-245
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• 1997

An accurate analysis method for the determination of lead in whole blood by ICP/MS was developed. Whole blood samples were decomposed in microwave digestion system without any contamination and loss of lead. The 96 samples were analyzed by ICP/MS using mass$^{208}$ isotope of lead. Lead concentrations of human whole blood were ranged of $2.50{\sim}22.8{\mu}g/dL$. The accuracy of this analysis method was verified by analyzing of NIST SRM 955a series(lead in blood).

• Journal of Environmental Health Sciences
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• v.28 no.5
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• pp.53-58
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• 2002

A method for the determination of lead(II) ion using a nafion-EDTA(ethylene diamine tetraacetic acid)-glycerol modified glassy carbon electrode was proposed. Lead(II) ion is accumulated at the electrode by complexation and electrostatic attraction with nafion-EDTA-glycerol and detected at -0.560$\pm$0.015V (vs. Ag/AgCl) by differential pulse voltammetry. For the determination of lead(II) ion, a standard calibration curve if obtained from 10$^{-9}$ M lead(II) ion to 10$^{-7}$ M, and the detection limit(3s) is as low as 5.0$\times$10$^{-10}$ M.

• Journal of Preventive Medicine and Public Health
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• v.7 no.2
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• pp.377-381
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• 1974

Determination of lead in urine is important in industrial hygiene and toxicology. Dithizone method has been principally used for the determination of lead in urine, which gives accurate results in skilful hands but is usually complex and time-consuming. Atomic absorption spectrophotometry is a new simple method and several procedures have been described. However, the influences of pH and the presence of chelating agents during treatment of lead poisoning are not clear. The purpose of this study was to find out the effect of pH and chelating agents on the determination of lead using Shimadzu atomic absorption/flame spectrophotometer, model AA-610. The results obtained were as follows: 1. The atomic absorption spectrophotometry(AAS) could be applied without prior acid digestion to specimens in the absence of chelating agents. The absorbance at $2,170\;{\AA}$, though more sensitive, was more noisy electronically. Therefore, we selected the wavelength of $2,833\;{\AA}$ plus scale expansion. 2. The optimal pH was in the range from 2 to 3. 3. The sensitivity was $0.075{\mu}g/ml/%$ and detection limit was about $0.2{\mu}g/ml$. 4. In the presence of EDTA, lead could not be completely determined without prior acid digestion. 5. On specimens from patients receiving penicillamine therapy, a comparison was made between the values obtained with dithizone method and AAS method with prior acid digestion. The results of comparison showed a very good agreement.

• Journal of the Korean Chemical Society
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• v.7 no.2
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• pp.186-188
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• 1963

An attempt to improve the method of volumetric determination of tungsten developed by Luke has been made successfully. Using amalgam coated lead instead of pure metallic lead in the reduction procedure. W(VI)-W(III) reduction has been found to be quantitative in rather concentrated hydrochloric acid. Since there was no excessive dissolution of lead via reduction of hydrogen ion, lead surface was totally accessible for the reduction of tungsten and no trouble was caused by dereposition of $PbCl_2$ crystals at the nozzle of Jones reductor. Furthermore, it has been confirmed that almost 100 mg. of $WO_3$ can be handled easily if the chloride concentration of the HCl is increased by adding solid $NH_4Cl$.

• Journal of Environmental Health Sciences
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• v.2 no.1
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• pp.29-31
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• 1975

This experiment Was carried out under two points of view, from May 1st to the end of 1973. One was the comparative determination of the activation factor of Lead dioxide by kinds in measuring of Sulfur oxides concentration by $PbO_2$ cylinder method, and the other was the comparison that result with the record of auto analyzer. Five measuring sites were selected out of Seoul City. Three kinds of Lead dioxide made in Japan (B,C and D) were compared with Standard $PbO_2$ (A for use in Determination of Sulphur in the atmosphere, purity 99% up) made in British Institution, and monthly measuring was conducted at every sampling site. The recording by auto analyzer (Beckman Model 906-A $SO_2$ Analyzer) was conducted once or twice a month for 24 hours at each sampling site during the same period. And some significant results were obtained. 1. In comparative experiments to determine the activation degree of three kinds of Lead dioxide (B,C and D), the obtained correction factor of B reagent was 1.09, 1.16 in C and 1.30 in D against Standard $PbO_2$ (A). Therefore, it should be in need of standardization or clear statement about the reagents for use, in determination sulfur oxides by $PbO_2$ cylinder method. 2. Generally, the concentration of Sulfur dioxide by wilkins' convertion method from $SO_3$ showed about 20-30% higher than those by Auto analyzer.

• Journal of the Korean Chemical Society
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• v.13 no.4
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• pp.313-316
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• 1969

In this paper a simple and rapid method is described for the determination of lead in monazite. A monazite sample was dissolved with hot concentrated sulfuric acid and diluted to 200 ml with distilled water. Lead is quatitatively separated by coprecipitating with strontium. Lead-strontium sulfate is dissolved in 3N NaOH soluion. An excess Zn-EDTA is added. The remaining zinc ion is titrated with standard 0.01 M EDTA solution using xylenol orange as indicator at pH 5 in the presence of KCN and acetyl acetone as masking agents.

• Journal of the Korean Chemical Society
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• v.46 no.5
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• pp.407-411
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• 2002

A method to determine lead ion in aqueous media using an optical sensor loaded on a fluorescent optode membrane incoporating a metal ion-selective ionophore, a proton-selective chromoionophore and lipophilic anionic sites has been studied. The effects of pH and thickness of membrane on the fluorescence intensity were investigated. The effects of foreign ions such as $Na^+$, $K^+$, $Mn^{2+}$ and $Zn^{2+}$ on the determination of lead ion were also studied. The linear range in the calibration curve for the determination of lead ion was found to be 5.0${\times}10^-7$ to 5.0${\times}$$10^-3$M and the correlation coefficient in this range was -0.99107 under the optimal experimental conditions. The relative standard deviation of the blank signals was 3.0% and the detection limit of lead ion was 5.0${\times}$$10^-9$M.