• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.16 no.4
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• pp.397-410
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• 2018

When considering the long-term safety assessment of spent-nuclear fuel management, americium is one of the most radio-toxic actinides. Although spectroscopic methods are widely used for the study of actinide chemistry, application of those methods to americium chemistry has been limited. Herein, we purified $^{241}Am$ to obtain a highly pure stock solution required for spectroscopic studies. Quantitative and qualitative analyses of purified $^{241}Am$ were carried out using liquid scintillation counting, and gamma and alpha radiation spectrometry. Highly sensitive absorption spectrometry coupled with a liquid waveguide capillary cell and time-resolved laser fluorescence spectroscopy were employed for the study of Am(III) hydrolysis and oxalate (Ox) complexation. $Am^{3+}$ ions under acidic conditions exhibit maximum absorbance at 503 nm, with a molar absorption coefficient of $424{\pm}8cm^{-1}{\cdot}M^{-1}$. $Am(OH)_3(s)$ colloidal particles formed under near neutral pH conditions were identified by monitoring the absorbance at around 506-507 nm. The formation of ${Am(Ox)_3}^{3-}$ was detected by red-shifts of the absorption and luminescence spectra of 4 and 5 nm, respectively. In addition, considerable enhancements of the luminescence intensities were observed. The luminescence lifetime of ${Am(Ox)_3}^{3-}$ increased from 23 to 56 ns, which indicates that approximately six water molecules are replaced by carboxylate ligands in the inner-sphere of the Am(III). These results suggest that ${Am(Ox)_3}^{3-}$ is formed through the bidentate coordination of the oxalate ligands.

• Bulletin of the Korean Chemical Society
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• v.27 no.9
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• pp.1293-1296
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• 2006

In this study, a solid phase extraction method has been developed for the preconcentration and separation of the elements Cr(III), Fe(III), Co(II) and Pb(II) at trace levels by using a column packed with Amberlite XAD-1180 resin loaded with 4-(2-pyridylazo)-resorcinol (PAR) reagent. After preconcentrating, the metals retained on the column were eluted with 20 mL of 3 mol/L $HNO_3$ and then determined by flame atomic absorption spectrometry (FAAS). The factors affecting the recovery of the elements, such as pH, type and concentration of eluent, volume of sample and elution solution, and matrix components, were also ascertained. The recoveries of Cr(III), Fe(III), Co(II) and Pb(II) were found to be $99\;{\pm}\;4,\;97\;{\pm}\;3,\;95\;{\pm}\;3$ and $98\;{\pm}\;4$%, respectively, under the optimum conditions at 95% confidence level and the relative standard deviations found by analyzing of nine replicates were $\leq4.4$%. The preconcentration factors for Cr(III), Fe(III), Co(II) and Pb(II) were found as 75, 125, 50 and 75 respectively. The detection limits (DL, 3s/b) were 3.0 $\mu g/L$ for Cr(III), 1.25 $\mu g/L$ for Fe(III), 3.3 $\mu g/L$ for Co(II), and 7.2 $\mu g/L$ for Pb(II). The recoveries achieved by adding of metals at known concentrations to samples and the analysis results of Buffalo river sediment (RM 8704) show that the described method has a good accuracy. The proposed method was applied to tap water, stream water, salt and street dust samples.

• Journal of Environmental Health Sciences
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• v.35 no.5
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• pp.402-410
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• 2009

This study was carried out to examine the optimal analytical method for determination of urinary toxic arsenic (inorganic arsenic and its metabolites) by HG-AAS (hydride generation-atomic absorption spectrometry). In the analysis of SRMs (standard reference materials), method E (addition of 0.4% L-cysteine to pre-reductant and use 0.04M HCl as carrier acid) showed the most accurate results compared with the reference values. In the analysis of 30 urinary samples, analytical results were significantly different depend on the component of pre-reductant and the concentration of carrier acid. When the concentration of carrier acid was higher, the analytical result was lower. The recovery rates of MMA (monomethylarsonic acid) and DMA (dimethylarsenic acid) were varied by the concentration of pre-treatment acid and carrier acid and hydride generation reagents. When the concentration of carrier acid was 1.62 M (5% HCl), the recovery rates of DMA was 1%. The recovery rates of MMA and DMA in method E (=V) were 102% and 100%, respectively. The results of this study suggest that the component and concentration of pre-reductant and carrier acid must be carefully adjusted in the analysis of urinary arsenic, and method E is recommendable as the most precise analytical method for determination of urinary toxic arsenic.

• Economic and Environmental Geology
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• v.28 no.4
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• pp.389-394
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• 1995

Yugu-Kwangcheon Au-Ag Province is connected to the southwestern part of the Cheonan Province and includes the Gubong (one of the biggest gold mine in past), Daebong and Samgwang mines. Cadmium concentrations in sphalerite of Yugu-Kwancheon Province is higher than those of other Au-Ag provinces and could be the source of the heavy metal contaminations. Heavy metals are present in rock-soil-plant-human system from natural geological materials, and dietary intake through this system makes a significant contribution to the ingestion of heavy metals by man. In order to examine the degree and extent of heavy metal contaminations in the Gubong, Daebong and Samgwang mine areas of Yugu-Kwangcheon Province, soil, stream water, sediment and crop plant samples were taken and analyzed for Cd, Cu, Pb and Zn by Atomic Absorption Spectrometry (AAS) and Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). Cadmium and Pb concentrations in paddy/farm soils and stream sediments from the Gubong and Samgwang mine areas are higher than those in uncontaminated soils. Lead concentrations in crop plants cultivated in these soils are high up to $0.38{\mu}g/g$ in rice grain and $4.5{\mu}g/g$ in sesame. In these mine areas, regular consumption of crop plants by the local population would seem to pose a potential health problems from long-term Pb exposure. The biological absorption coefficient in rice grain for heavy metals varies in the order $C_d=Zn>Cu>Pb$ and the relationship between Cd concentrations in soils and crop plants is expressed by the equation $Cd_{plant}=0.11245\;Log\;Cd_{soil}+0.13472$.

• 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.

• Journal of the Korean Chemical Society
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• v.52 no.1
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• pp.16-22
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• 2008

on-line system for preconcentration and separation of lead(II) is presented. The method is based on the complex formation of Pb(II) with adsorbed Methyl thymol blue on activated carbon. The conditions of preparing the solid phase reagent and of quantitative recovery of Pb(II) from diluted solutions, such as acidity of aqueous phase, solid phase capacity, and flow variables were studied as well as effect of potential interfering ions. After preconcentration step, the metal ions are eluted automatically by 5 ml of 0.5 M HNO3 solution and the lead ions content was determined by flame atomic absorption spectrometry. Under the optimum conditions, the lead ions in aqueous samples were separated and preconcentrated about 1000-fold by the column. The detection limit was 0.001 g mL-1. Lead has been determined in river and tap water samples, with recovery of 98 to 102%.

• Bulletin of the Korean Chemical Society
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• v.31 no.10
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• pp.2813-2818
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• 2010

A novel method was developed for the speciation of chromium in natural water samples based on homogeneous liquid-liquid extraction and determination by flame atomic absorption spectrometry (FAAS). In this method, Cr(III) reacts with a new Schiff's base ligand to form the hydrophobic complex, which is subsequently entrapped in the sediment phase, whereas Cr(VI) remained in aqueous phase. The Cr(VI) assay is based on its reduction to Cr(III) by the addition of sodium sulfite to the sample solution. Thus, separation of Cr(III) and Cr(VI) could be realized. Homogeneous liquid-liquid extraction based on the pH-independent phase-separation process was investigated using a ternary solvent system (water-tetrabutylammonium ion ($TBA^+$)-chloroform) for the preconcentration of chromium. The phase separation phenomenon occurred by an ion-pair formation of TBA and perchlorate ion. Then sedimented phase was separated using a $100\;{\mu}L$ micro-syringe and diluted to 1.0 mL with ethanol. The sample was introduced into the flame by conventional aspiration. After the optimization of complexation and extraction conditions such as pH = 9.5, [ligand] = $1.0{\times}10^{-4}\;M$, [$TBA^+$] = $2.0{\times}10^{-2}\;M$, [$CHCl_3$] = $100.0\;{\mu}L$ and [$ClO_4$] = $2.0{\times}10{-2}\;M$, a preconcentration factor (Va/Vs) of 100 was obtained for only 10 mL of the sample. The relative standard deviation was 2.8% (n = 10). The limit of detection was sufficiently low and lie at ppb level. The proposed method was applied for the extraction and determination of chromium in natural water samples with satisfactory results.

• Journal of the Korean Chemical Society
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• v.38 no.3
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• pp.214-220
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• 1994

A glow discharge atomic absorption system for the direct analysis of conducting solid samples has been designed and constructed. An arrestor made of machinable ceramic which is a main component for confining the discharge between cathode and anode is modified to have a better stability in discharge. Discharge voltage or current, shape of arrestor, pressure, and gas flow rate can be controlled by an ADC/DAC board with a personal computer. The effect of discharge parameters such as discharge voltage, pressure, and gas flow rate on the sample loss rate, absorbance, and the surface morphology of sample by SEM has been studied to find optimum discharge conditions.

• Bulletin of the Korean Chemical Society
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• v.25 no.9
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• pp.1309-1313
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• 2004

A simple and reliable method has been developed to selectively separate and concentrate trace amounts of thallium ion from real samples for the subsequent measurement by flame atomic absorption spectrometry (FAAS). Thallium ions are absorbed quantitatively during passage of aqueous real samples through an octadecyl bonded silica membrane disk modified by 4-(4-Chloro-phenylazo)-2-[(4-hydroxy-phenylamino)-methyl]-phenol. The retained $Tl^+$ ions are then stripped from the disk quantitatively with a minimal amount of thiosulfate solution as eluent. The proposed method permitted large enrichment factors of about 130 and higher. The relative standard deviation for ten replicate extraction of thallium from 1 L samples containing 5 ${\mu}g$ thallium is 1.2%. The break through volume for 5 ${\mu}g$ thallium is 1000 mL. The limit of detection of the proposed method is 11.2 ng of $Tl^+$ per 1000 mL. The effects of various cationic interferences on the recovery of thallium in binary mixtures were studied. The method was applied to the recovery of $Tl^+$ ions from natural water and human hair samples.

• Journal of Environmental Health Sciences
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• v.44 no.5
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• pp.491-501
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• 2018

Objectives: The aims of this study were to compare concentrations and the correspondence of human blood cadmium by using graphite furnace atomic absorption spectrometry (GF-AAS) and inductively coupled plasma-mass spectrometry (ICP-MS), which are representative methods of heavy metal analysis. Methods: We randomly selected 79 people who agreed to participate in the research project. After confirming the linearity of the calibration curves for GF-AAS and ICP-MS, the concentrations of cadmium in a quality control standard material and blood samples were measured, and the correlation and the degree of agreement were compared. Results: The detection limit of ICP-MS (IDL: $0.000{\mu}g/L$, MDL: $0.06{\mu}g/L$) was lower than that of GF-AAS (IDL: $0.085{\mu}g/L$, MDL: $0.327{\mu}g/L$). The coefficient of variation of the quality control standard material showed stable values for both ICP-MS (clinchek-1: 5.35%, clinchek-2: 6.22%) and GF-AAS (clinchek-1: 7.92%, clinchek-2: 5.22%). Recovery was relatively high for both ICP-MS (clinchek-1: 95.1%, clinchek-2: 92.8%) and GF-AAS (clinchek-1: 91.4%, clinchek-2: 98.8%), with more than 90%. The geometric mean, median, and percentile of blood samples were all similar. The agreement of the two instruments compared with the bias of the analytical values found that about 81% of the analytical values were within ${\pm}30%$ of the deviation from the ideal reference line (y=0). As a result of the agreement limit, the value included in the confidence interval was about 94%, which shows high agreement. Conclusion: In this study, we confirmed there was no significant difference in concentrations of a quality control standard material and blood samples. Since ICP-MS showed lower concentrations than GF-AAS at concentrations below the method detection limit of GF-AAS, it is expected that more precise results will be obtained by analyzing blood cadmium with ICP-MS.