• 한국환경보건학회지
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• 제45권3호
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• pp.258-266
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• 2019

Objectives: In this study, blood lead was analyzed using graphite furnace atomic absorption spectrometry (GF-AAs) and inductively coupled plasma mass spectrometry (ICP-MS). We tried to examine the difference and consistency of the analytical values and the applicability of the analytical method. Methods: We selected 57 people who agreed to participate in this study. After confirming the linearity of the calibration standard curves in GF-AAs and ICP-MS, the concentrations of lead in quality control material and samples were measured, and the degree of agreement was compared. Results: The detection limit of the ICP-MS was lower than that of GF-AAs. The coefficient of variation of reference materials was shown to be stable in the ICP-MS and GF-AAs. When the correspondence between the two equipments was verified by bias of the analysis values, a concordance was shown, and approximately 98% of the ideal reference lines were present within ${\pm}40%$ of the deflection. Conclusion: GF-AAs showed high sensitivity to single heavy metal analysis, but it took much time and showed higher detection limit than ICP-MS. Therefore, it would be considered necessary to switch to ICP-MS analysis method, considering that the level of lead exposure is gradually decreasing.

• 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.

• 분석과학
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• 제16권2호
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• pp.152-158
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• 2003

본 연구는 인체의 골중 납 농도를 측정하는데 필요한 시료 전처리법과 기기 분석법을 평가하기 위하여 수행되었다. 절단한 인간 사체 다리의 뼈를 상온에서의 산 분해법과 마이크로웨이브 분해법 (microwave oven method)을이용하여 납을 추출하였으며, 유도결합 플라즈마 질량분석법 (ICP-MS)과 흑연로 원자 흡수 분광 광도법 (GF-AAS)으로 납 농도를 측정하였다. 표준시료를 이용하여 회수율을 조사한 결과, 산분해 후 ICP-MS로 측정한 경우 높은 회수율을 보였으나, 산분해 후 GF-AAS로 측정한 것은 표준 농도보다 낮은 값을 보였으며, 마이크로웨이브 분해한 경우는 두 측정기기 모두 표준 농도보다 높은 값을 보였다. 뼈 시료의 경우, 산분해 후 ICP-MS로 측정한 납 농도는 GF-AAS의 값과 높은 상관성을 보였으나 (상관계수 = 0.983), GF-AAS가 ICP-MS보다 계통적으로 높은 값을 측정하였다. 마이크로웨이브 분해 역시 두 분석방법이 높은 상관성을 보였으나 (상관계수 = 0.950), 대체로 산분해에 의한 값보다 높은 농도를 보였다. 결론적으로, 상온에서 질산으로 분해 후 ICP-MS를 이용하여 측정한 것이 골중 납 농도를 결정하는데 편이성과 정확성 면에서 가장 효율적인 방법으로 보인다.

• 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.

• 분석과학
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• 제5권4호
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• pp.349-358
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• 1992

본 연구에서는 흑연로 원자흡수분광법을 이용하여 혈액을 1% Triton X-100을 5배 희석시킨 다음 납 함량을 직접 측정하였다. 혈액내 방해 성분을 제거하기 위하여 매트릭스 변형제를 사용하여 최적의 분석 조건을 조사하였다. 매트릭스 변형제로서 1% $(NH_4)_2HPO_4$와 0.1% $PdCl_2$를 같이 사용하고 700도에서 회화시켰을 때에, 일본 비교 분석 프로그램에 의해 제공된 혈중 납 함량에 대한 정도관리용 표준시료(우혈)의 공인값과 비교적 잘 일치하였다. 이 실험에서 얻은 표준편차는 $31{\mu}gPb/l$에서 $624{\mu}gPb/l$ 범위에서는 1% $(NH_4)_2HPO_4$ 및 1% $(NH_4)_2HPO_4$와 0.1% $PdCl_2$를 매트릭스 변형제로서 사용했을 경우 각각 2.2~6.3%, 3.1~9.1%였다.

• 분석과학
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• 제7권4호
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• pp.427-434
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• 1994

GFAAS(graphite furnace atomic absorption spectrophotometer)를 이용하여 혈액 중 납을 분석할 때, 납은 비교적 휘발성 원소인 관계로 바탕선이 높아지므로 희화 온도를 일정 온도 이상으로 높일 수 없었다. 그래서 종래에는 매트릭스 변형제를 사용하여 희화 온도를 $700^{\circ}C$까지 올려서 희화시켜야 바탕선이 안정되었다. 본 연구에서는 광온도 및 전류 제어 장치가 부착된 기기(Shimadzu, AA-6501S)를 사용하여 온도조절을 단시간에 정확히 함으로써 매트릭스 변형제를 사용하지 않고 Triton X-100으로만 희석하여 분석해도 희화 온도 $550^{\circ}C$ 부근에서 바탕선이 안정됨을 알았다. 또한 자동 바탕 보정 장치인 $D_2$ arc형과 SR(self reversal)법을 비교해 본 결과, 같은 농도에서의 흡광도는 $D_2$ arc형이 높았으나 BGC(background correction)값은 SR법이 높음을 알았다.

• 자원환경지질
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• 제25권2호
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• pp.145-151
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• 1992

In order to study the optimum depth for the soil geochemical exploration in the area which is affected by agricultural activities and waste disposal of metal mine, the soil samples were sampled from the B layer of residual soil and vertical 7 layers up to 250 cm in the rice field and 3 layers up to 90 cm in the ordinary field. They were analyzed for Au, As, Cu, Pb and Zn by AAS, AAS-graphite furnace and ICP. To investigate the proper depth for the soil sampling in the contaminated area, the data were treated statistically by applying correlation coefficient, factor analysis and trend analysis. It is conclude that soil geochemical exploration method could be applied in the farm-land and a little contaminated area. The optimum depth of soil sampling is 60 cm in the ordinary field, and 150~200 cm in the rice field. Soil sampling in the area of a huge mine waste disposal is not recommendable. Plotting of geochemical map with factor scores as a input data shows a clear pattern compared with the map of indicater element such as As or Au. The second or third degree trend surface analysis is effective in inferring the continuity of vein in the area where the outcrop is invisible.

• Bulletin of the Korean Chemical Society
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• 제19권1호
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• pp.50-56
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• 1998

A solvent sublation was studied for the determination of trace Cd, Co, Cu and Ni in water samples. Ammonium pyrrolidine dithiocarbamate (APDC) was used as a complexing agent. Experimental conditions such as pH of solution, amounts of APDC, the type and amount of surfactant, the type of solvent, etc. were optimized for the effective sublation of analytes. After metal-PDC complexes were formed in sample solutions of pH 2.5, the precipitate-type complexes were floated in a flotation cell with an aid of sodium lauryl sulfate as a surfactant and by bubbling with nitrogen gas. The precipitates were dissolved and separated into the surface layer of methyl iso-butyl ketone (MIBK). The analytes preconcentrated were determined by a graphite furnace atomic absorption spectrophotometry (GF-AAS). Extractability of each element was 88% for Cd(Ⅱ), 86% for Co(Ⅱ), 95% for Cu(Ⅱ) and 76% for Ni(Ⅱ), respectively. And this procedure was applied to the analysis of real samples. From the recoveries of more than 92%, it was concluded that this method could be simple and applicable for the determination of trace elements in various water samples of a large volume.

• 한국환경보건학회지
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• 제42권6호
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• pp.450-464
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• 2016

Objectives: This study developed and validated reference materials (RMs) to analyze metal compounds in blood. Methods: We referred to KoNEHS (Korea National Environmental Health Survey) to estimate concentrations of blood metals (cadmium, Cd; lead, Pb; mercury, Hg) and applied analytical methods (inductively coupled plasma - mass spectroscopy, ICP-MS, for Cd and Pb; graphite furnace - atomic absorption spectrometry, GF-AAS, for Cd and Pb; and direct mercury analyzer, DMA, for Hg). Homogeneity and stability tests were carried out. In addition, certified values and uncertainties of RMs were calculated through internal and external experiments. All RMs were developed and assessed in various forms according to element, analytical method, and two types of concentration levels high concentration for occupational exposure and low concentration for environmental exposure. Results: All samples showed acceptable homogeneity, except for low concentration of Cd in the GF-AAS method. Short- and long-term stabilities were satisfied by ANOVA testing. In the inter-laboratory comparison, robust medians were lower than the certified values of all RMs (robust median/reference value; $1.301/1.327{\mu}g/L$ for Cd, ICP-MS, low concentration; $3.152/3.388{\mu}g/L$ for Cd, ICP-MS, high concentration; $1.219/1.301{\mu}g/L$ for Cd, GF-AAS, low concentration; $3.074/3.321{\mu}g/L$ for Cd, GF-AAS, high concentration; $14.473/14.516{\mu}g/L$ for Pb, ICP-MS, low concentration; $50.069/50.114{\mu}g/L$ for Pb, ICP-MS, high concentration; $12.881/14.147{\mu}g/L$ for Pb, GF-AAS, low concentration; $47.015/47.591{\mu}g/L$ for Pb, GF-AAS, high concentration; $4.059/4.218{\mu}g/L$ for Hg, DMA, low concentration; $11.474/11.181{\mu}g/L$ for Hg, DMA, high concentration). Conclusion: This study demonstrates procedures for developing and validating RMs for biomonitoring in the field of the environmental health.

• Journal of Magnetics
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• 제11권2호
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• pp.98-102
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• 2006

It was examined in this study that magnetic beads, which are assumed to be environmentally functional, could be effective in processing heavy metals that are water pollutants. For the purpose, magnetic beads containing carboxyl groups, which has strong binding force with heavy metals, are mixed with each Cd, Pb, Ni, Cu and Cr(III) solution, then stirred in pH 6. As a results of the process, it was proven that heavy metals bind quickly with magnetic beads through the reaction. In order to analyze heavy metal concentration, magnetic beads bind with heavy metal were collected by external magnetic force and dissolved in acid. The graphite furnace AAS was used to get heavy metal concentration melted in the acid solution. The results showed that heavy metal extractions by magnetic beads were influenced by the type and the concentration of a heavy metal, and over 90% of a heavy metal can be extracted in ppm level save for Cr(III). It was also examined in the study whether heavy metal extraction is influenced when other ions exist in each heavy metal solution. According to experiment, adding other heavy metals to a solution did have little influence on extracting an intended heavy metal. But in case salt or heavy metal chelate was added, Ni extraction changed sensitively although extracting other heavy metals were influenced only when the concentration of an added substance is high. In conclusion, it was shown that magnetic beads could be used to treat wastewater with relatively high heavy metal concentration.