• 방사성폐기물학회지
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• 제16권4호
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• pp.397-410
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• 2018

아메리슘(Am)은 사용후핵연료의 장기 방사성 독성에 크게 영향을 주기 때문에 고준위 방사성 폐기물 처분의 장기 안전성 평가에 필수적으로 고려되어야 할 원소이다. 분광학적 방법을 이용한 일부 악티나이드 원소의 화학반응 연구가 활발히 진행되고 있는 반면, 아메리슘에 대한 연구는 아직까지 미비한 상황이다. 이 연구에서는 고순도의 시료를 필요로 하는 화학반응 연구를 위하여 $^{241}Am$ 시료를 정제한 후, 액체섬광계수기와 감마선 및 알파선 스펙트럼을 이용하여 정량과 정성분석을 하였다. 액체 광도파 모세관 셀을 이용한 고감도의 UV-Vis 흡수 분광학과 시간분해 레이저 형광 분광학을 이용하여 Am(III) 가수분해물과 옥살레이트(oxalate, Ox) 착물반응을 조사하였다. 산성조건에서 $Am^{3+}$은 503 nm에서 최대 흡수봉우리를 보이며, 몰흡광계수는 $424{\pm}8cm^{-1}{\cdot}M^{-1}$임을 확인하였다. 중성 이상의 pH 조건에서 형성되는 $Am(OH)_3(s)$ 콜로이드 입자에서는 506-507 nm 파장에서 최대 흡수봉우리가 관측되었다. ${Am(Ox)_3}^{3-}$ 착물은 $Am^{3+}$에 비교하여 흡수 및 발광스펙트럼이 각각 4와 5 nm정도 장파장으로 이동하였고 몰흡광계수와 발광세기도 크게 증가하였다. ${Am(Ox)_3}^{3-}$의 발광수명은 23에서 56ns으로 증가하였고 이는 Am(III)의 내부권에 결합하고 있던 약 여섯 개의 물분자가 옥살레이트의 카르복실기로 치환되었음을 의미한다. 이 결과로부터 ${Am(Ox)_3}^{3-}$은 각 옥살레이트 리간드가 두 자리 결합(bidentate)을 하고 있다는 것을 제안하였다.

• Bulletin of the Korean Chemical Society
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• 제27권9호
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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.

• 한국환경보건학회지
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• 제35권5호
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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.

• 자원환경지질
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• 제28권4호
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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 $Cd_{plant}=0.11245\;Log\;Cd_{soil}+0.13472$.

• 분석과학
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• 제8권1호
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• pp.9-16
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• 1995

본 연구에서는 혈액 중 저농도의 카드뮴 분석을 위하여 시료를 1% Triton X-100으로 5배 희석시킨 다음에 흑연로 원자흡수분광법을 이용하여 분석하였다. 매트릭스 개선제로서 2% $(NH_4)_2HPO_4$와 L'vov platform이 삽입된 pyrocoated 흑연로를 사용하여 비교적 높은 회화온도 ($600^{\circ}C$)에서 카드뮴의 손실을 최대한 억제시키면서, 혈액내의 방해 성분으로 인한 영향을 감소시켰다. 분석의 정확성을 평가하기 위하여 NIST 표준물질(혈청 중 Cd) 및 외부 분석 기관(일본)에서 분석한 결과를 비교 검토하였다. 이 실험에서 얻은 상대 표준편차는 1.0ng/ml 농도에서 10% 정도이며 검출한계값은 0.1ng/ml였다.

• 대한화학회지
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• 제52권1호
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• pp.16-22
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• 2008

예비농축 및 분리를 위한 온라인 시스템을 소개하였다. 이 방법은 활성탄소에 흡착된 메틸티몰 블루로 납(II)의 착체형성을 기저로 한다. 간섭이온의 효과는 물론 수용액상의 산성도, 고상의 용량, 흐름변수와 같은 희석용액으로부터 납(II)의 정량회수와 고상 시약의 준비 상태에 대해 연구되었다. 예비농축 후에 금속이온은 0.5M HNO3 용액의 5 ml에 자동적으로 용출되고 납이온의 양은 불꽃원자 흡수 분광법로 측정하였다. 최적조건하에서, 수용액시료의 납이온은 컬럼에 의해 약 1000배 분리 및 농축되었다. 검출한계는 0.001mg mL-1였다. 납은 강과 수돗물시료에서 98에서 102% 회수율을 보였다.

• Bulletin of the Korean Chemical Society
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• 제31권10호
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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.

• 대한화학회지
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• 제38권3호
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• pp.214-220
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• 1994

금속시료를 직접분석하기 위하여 원자흡수법에 의한 글로우방전시스템을 구성하였다. 방전이 일어나는 양극과 음극은 가공성 세라믹을 이용한 arrestor에 의해 분리하였으며, 방전에 영향을 미치는 전류 및 전압, arrestor의 형태, 가스 압력 그리고 가스 흐름 등을 개인용 컴퓨터와 ADC/DAC board 및 RS-232를 사용하여 자동적으로 제어될 수 있도록 하였다. 여러가지 방전에 미치는 실험변수들을 변화시키면서 시료손실속도, 원자흡광도 등의 변화를 측정하였으며, sputtering 된 후의 시료 표면을 주사형 전자현미경으로 관찰하였다.

• Bulletin of the Korean Chemical Society
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• 제25권9호
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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.

• 한국환경보건학회지
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• 제44권5호
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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.