• Title/Summary/Keyword: GFAAS

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Preparation and analysis of lyophilized whole blood as external quality control materials for Pb and Cd determination by graphite furnace atomic absorption spectrometry (흑연료 원자흡수 분광법에 의한 혈중의 납, 카드뮴 정량을 위한 외부정도관리 시료제조 및 분석)

  • Lee, Kong-Joo;Lim, H.B.
    • Analytical Science and Technology
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    • v.8 no.3
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    • pp.273-279
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    • 1995
  • Lyophilized whole blood samples containing various concentrations of Pb and Cd have been prepared as external quality control materials. These materials have been characterized with graphite furnace atomic absorption spectrometry(GFAAS), The optimized conditions for the quantitative determination of Ph and Cd in whole blood using GFAAS were obtained at the ashing temperature of $600{\sim}650^{\circ}C$ with 0.1% ammonium dihydrogen phosphate and 0.1% Triton X-100 as matrix modifier. Homogeniety and stability of the prepared whole blood have been studied at the optimized analytical condition.

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Graphite Furnace Atomic Absorption Spectrophotometric Determination of Trace Horseradish Peroxidase Using Nanosilver

  • Jiang, Zhi-Liang;Tang, Ya-Fang;Wei, Lin;Liang, Ai-Hui
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2732-2736
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    • 2011
  • In pH 4.2 HAc-NaAc buffer solution, horseradish peroxidase (HRP) catalyzed $H_2O_2$ oxidation of nanosilver to form $Ag^+$. After centrifugation, $Ag^+$ in the supernatant can be measured by graphite furnace atomic absorption spectrophotometry (GFAAS) at the silver absorption wavelength of 328.1 nm. When HRP concentration increased, the $Ag^+$ concentration in the supernatant increased, and the absorption value enhanced. The HRP concentration in the range of 0.84-50 $ng{\cdot}mL^{-1}$ was linear to the enhanced absorption value (${\Delta}A$), with a regression equation of ${\Delta}A$=0.012C+0.11, correlation coefficient of 0.9988, and detection limit of 0.41 $ng{\cdot}mL^{-1}$ HRP. The proposed GFAAS method was used to detect HRP in waste water samples, with satisfactory results.

Analysis of Cadmium in Blood using SH(Smith-Hieftje) and $D_2$ Arc Background Correction Methods by Graphite Furnace Atomic Absorption Spectrophotometer (Smith-Hieftje(SH) 및 $D_2$ 바탕보정장치가 부착된 흑연로 원자흡수분광법을 이용한 혈액 중 카드뮴 분석)

  • Lee, Seok Ki;Kim, Poong Zag;Joung, Chang Ung
    • Journal of the Korean Chemical Society
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    • v.40 no.3
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    • pp.196-201
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    • 1996
  • The analysis of trace cadmium in blood by using 10 folds diluted samples with 1% Triton X-100 and Fork platform tube at the ashing temperature of 500$^{\circ}C$ has been performed by GFAAS. In this study, good analytical results were obtained from peak area and peak height methods. The detection limits of SH and $D_2$ arc background correction are 0.02 ng/mL and 0.01 ng/mL, respectively. Relative standard deviation is within 5% at the level of 1.0 ng/mL.

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The role of matrix modifier and for the determination of cadmium in blood by graphite furnace atomic absorption spectrometry (흑연로 원자흡수분광법에 의한 혈중 카드뮴 분석시 매트릭스 개선제(matrix modifier)의 역할)

  • Yoo, Kwang-Sik;Kim, Chang-Bok;Kwon, Jin-Kee
    • Analytical Science and Technology
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    • v.8 no.1
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    • pp.9-16
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    • 1995
  • The low concentration of cadmium in the whole-blood was determined by graphite furnace atomic absorption spectrometry(GFAAS) after the sample was diluted five-fold by 1% Triton X-100, 2% $(NH_4)_2HPO_4$ as matrix modifier and pyrocoated graphite tube with L'vov platform was tried remove the interferences of blood matrix and reduce the loss of volatility of cadmium at higher ashing temperature($600^{\circ}C$). The criteria for evaluating the accuracy and precision of this analysis was confirmed by analysis of interlaboratory comparison(Japan) and NIST SRM No. 909(Cd in Serum). The limit of the determination for cadium was 0.1ng/ml and the relative standard deviation(RSD) at 1.0ng/ml level was about 10% for the GFAAS.

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Analysis of Lead in Blood using SR(self-reversal) and $D_2$ Arc Background Correction Methods (SR 바탕보정법과 $D_2$ 바탕보정법에 의한 혈액 중 Pb 분석)

  • Lee, Seokki;Kim, Poongzag
    • Analytical Science and Technology
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    • v.7 no.4
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    • pp.427-434
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    • 1994
  • For the analysis of the relatively volatile lead in blood by GFAAS(graphite furnace atomic absorption spectrophotometer), one can not raise the ashing temperature beyond certain degree due to the elevation of the baseline. Previous investigations showed that background is stabilized when the ashing temperature is raised to $700^{\circ}C$ using a matrix modifier. In this study, same result was obtained at the ashing temperature of around $550^{\circ}C$ even when the matrix modifier is not used and only Triton X-100 is used as a diluent, on an instrument which is equipped with both temperature and current controller(Shimadzu, AA-6501S) and thus the temperature control is fast and accurate. Background correction methods of $D_2$ arc and SR(self reversal) were reviewed. The results show that the absorbance is higher for the $D_2$ arc method, but the background correction is higher for the SR method.

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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.

A Comparative Analysis of Whole Blood Cadmium by Atomic Absorption Spectrophotometry with a Graphite Furnace (흑연로 원자흡수분광법에 의한 혈액중 카드뮴 정량분석)

  • Park, Jong An;Oh, Hye Jeong;Lee, Jong Hwa
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.6 no.2
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    • pp.301-312
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    • 1996
  • This study was performed to search a optimal analyzing method of cadmium in whole-blood. Cadmium was determined by graphite furnace atomic absorption spectrometry(GFAAS). We investigated the effect of ashing temperature on the absorbance of cadmium in a simple dilution(ten-fold) method with triton X-100 and matrix modifier methods treated with $NH_4H_2PO_4$(1 and 3%) and $Pd(NO_3)_2$(0.00l and 0.005%) as matrix modifier. We also compared the reported reference values of standard blood with values resulted from optimal analyzing conditions of this study. In case of a simple dilution method, when ashing temperature was set at $450^{\circ}C$, the absorbance of sample and background were $0.334{\pm}0.012$ and $1.382{\pm}0.245$, respectively. Background level was higher than the value(0.8) that can be corrected by $D_2$ background correction method. As ashing temperature was rised to $500^{\circ}C$, the absorbance of sample and background were $0.178{\pm}0.008$ and $0.711{\pm}0.223$ respectively. The higher ashing temperature($450^{\circ}C-650^{\circ}C$) was, the lower the absorbance of sample was. In case of a matrix modifier method with $NH_4H_2PO_4$(1 and 3%), when ashing temperature was rised from $500^{\circ}C$ to $650^{\circ}C$, the absorbance of sample slightly changed. The absorbances of sample at $600^{\circ}C$ were $0.230{\pm}0.017$ and $0.137{\pm}0.012$, respectively. These values were larger than that of simple dilution method. But the absorbance of background was higher than the level that can be corrected by $D_2$ method. In case of a matrix modifier method with $Pd(NO_3)_2$(0.001 and 0.005%), the absorbance of sample and background were higher than those of other methods and were stable and reproducible. When ashing temperature was over $550^{\circ}C$, the absorbance of sample was significantly decreased. In case of 0.005% $Pd(NO_3)_2$ carbon residue remained in graphite tube affected the absorbance of sample and background. From these results, We propose that in case of a simple dilution(ten-fold) method with triton X-100 ashing temperature must be maintained below $400^{\circ}C$. In order to diminish the absorbance of background, the alternative method is attenuation of injection volume or multiplication of dilution ratio. We recommend $Pd(NO_3)_2$ than $NH_4H_2PO_4$ as a matrix modifier. In case of a matrix modifier method with $Pd(NO_3)_2$ ashing temperature might be maintained below $550^{\circ}C$.

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Synthesis of a New α-Dioxime Derivative and Its Application for Selective Homogeneous Liquid-Liquid Extraction of Cu(II) into a Microdroplet Followed by Direct GFAAS Determination

  • Ghiasvand, A. R.;Shadabi, S.;Kakanejadifard, A.;Khajehkoolaki, A.
    • Bulletin of the Korean Chemical Society
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    • v.26 no.5
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    • pp.781-785
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    • 2005
  • A fast and reliable method for the selective separation and preconcentration of $Cu^{2+}$ ions using homogeneous liquid-liquid extraction was developed. A new $\alpha$-dioxime derivative (2H-1,4-benzothioazine-2,3(4H)dionedioxime, Dioxime I) was synthesized and investigated as a suitable selective complexing ligand for $Cu^{2+}$ ions. Zonyl FSA (FSA) was applied as a phase-separator agent under the slightly acidic pH conditions. Under the optimal experimental conditions ([FSA] = 3.2% w/v, [THF] = 19.5% v/v, [Dioxime I] = 1.9 ${\times}\;10^{-3}$ M, and pH = 4.7), 10 ${\mu}g\;of\;Cu^{2+}$ in 5.2 mL aqueous phase could be extracted quantitatively into 80 $\mu$L of the sedimented phase. The maximum concentration factor was 65-fold. The limit of detection of the proposed method was 0.005 ng $mL^{-1}$. The reproducibility of the proposed method, on the 10 replicate measurements, was 1.3%. The influence of the pH, type and volume of the water-miscible organic solvent, concentration of FSA, concentration of the complexing ligand and the effect of different diverse ions on the extraction and determination of $Cu^{2+}$ ions were investigated. The proposed method was applied to the extraction and determination of $Cu^{2+}$ ion in different synthetic and natural water samples.

Micro Pre-concentration and Separation of Metal Ions Using Microchip Column Packed with Magnetic Particles Immobilized by Aminobenzyl Ethylenediaminetetraacetic Acid

  • Kim, Y.H.;Kim, G.Y.;Lim, H.B.
    • Bulletin of the Korean Chemical Society
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    • v.31 no.4
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    • pp.905-909
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    • 2010
  • Magnetic beads (Dynabeads$^{(R)}$) embedded in ~1 micron size polystyrene beads bearing surface carboxylic acid groups were modified with aminobenzyl ethylenediaminetetraacetic acid (ABEDTA) to concentrate or separate metal ions using pH gradients on micro and nano scales. The immobilization of ABEDTA was achieved by amide formation. The presence of the metal chelating functional group in the fully deprotonated form was confirmed by FT-IR. The chelation efficiency of beads was tested by determining metal ions in supernatant using GFAAS when pH gradients from 3 to 7. Mixtures of Cu and Mg and of Cd and Mn (at 10 ng/mL of metal) were separated as the difference in formation constant with the functional group of ABEDTA. The separation was repeated twice with relative standard deviation of <18%. A polydimethylsiloxane (PDMS) microchip column packed with EDTA-coated magnetic beads was optimized to concentrate metal ion for practical applications by eluting a Cu solution of micro scale at pH 3.

Analysis of Mobile Lead in Soil Using Carboxylated Magnetic Particle

  • So, Hyung-Suk;Shin, Hyun-Chul;Yoo, Yeong-Seok;Schaeffer Andreas
    • Journal of Magnetics
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    • v.10 no.3
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    • pp.89-92
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    • 2005
  • The analytic possibility of mobile lead contained in soil has been studied using carboxylated magnetic beads. Extraction of heavy metal was performed to contaminated soil that has been collected and supplied for tests. As experiment materials, soil sample, distilled water and magnetic beads were only used. It means that the lead was extracted under neutral condition. In this condition, only the mobile fraction of lead could be extracted by magnetic beads. The mobile lead in the soil was quickly combined with magnetic beads in the mixture process. Then, the magnetic beads were dissolved into acids after collection by external magnetic force, and the lead combined with the beads was eluted and analyzed by Graphite Furnace Atomic Absorption Spectroscopy (GFAAS). In the results of extraction experiments for 3 sandy soils, the efficiency using beads was similar to or higher than that of EDTA (Ethylendiamintetraacetic acid), which is normally used for analyzing mobile heavy metal concentration in soil. With this, it was shown that this method is a more accurate and simple method to analyze mobile lead when analyzing mobile heavy metal concentration in sandy soil, rather than conventional method using EDTA.