• 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.

• 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.

• 분석과학
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• 제23권1호
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• pp.1-14
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• 2010

모든 전기전자제품에 대한 유해 중금속 규제법(RoHS)이 유럽과 중국 등 세계 각 나라에서 시작 되면서 이에 대한 중요성이 대두되고 있다. 이와 관련하여, 현재 세계 전기전자 협회(IEC)에서 발표된 IEC 62321 문건은 기존의 표준 분석 규격들과 마찰이 있을 수 있다. 반면에, IEC기술위원회(TC 111) 에서 발표된 시료 채취 및 처리 방법(sampling)에 관한 일반공개규격(Publicly Accessible Specification: PAS)은 기존 규격들과 상호보완적으로 응용될 수 있다. 이 실험에서는 PAS에 준하여 휴대폰시료를 분리 및 분해하는 방법을 찾고, 기존의 분석장치를 이용한 스크리닝방법과 비교하고자 하였다. X선 형광분석법(XRF)은 시료의 전 처리가 필요 없어서, 신속한 분석이 가능하므로 스크리닝에 탁월한 기능을 보여준다. 하지만 이 방법은 표면의 유해물질 정보만 알 수 있으며, 심각한 매트릭스 간섭과 정량을 위한 다양한 표준물질이 없다는 제약이 따르기 때문에, 이를 보완할 수 있는 방법이 필요하다. 본 연구에서는 레이저 박리 유도결합플라스마 질량분석장치(LA-ICP-MS), 에너지 분산형 XRF (ED-XRF) 와 전자주사현미경 에너지분산 X선분광기(SEM-EDX)를 휴대폰 스크리닝에 적용하여 보았으며, 유해중금속이 검출된 일부 부품의 경우에는 흑연로 원자흡수분광분석법(GF-AAS)을 수행하여 농도를 측정하였다. 이 실험결과, 배터리 일부 부품의 경우, GF-AAS와 XRF의 Pb 측정결과는 각각 0.92%와 5.67%로서 차이가 많이 나는 것을 알 수 있었다. 또한, XRF의 상대편차 범위 23-168%는 LA-ICP-MS의 편차 범위인 1.9-92.3% 보다 월등히 큰 것으로 나타났다. 결론적으로, 스크리닝 목적으로 XRF 분석방법을 이용하였다 할지라도, 정확한 함량을 얻기 위하여 GF-AAS의 분석을 수행해야 할 것으로 판단된다. 그리고, 기존 IEC 문건의 스크리닝 방법에는 언급되어 있지 않으나, 본 연구에서는 LA-ICP-MS가 전기전자제품 내에 있는 유해물질들에 대한 정보를 신속하게 얻을 수 있는 스크리닝 방법으로 활용될 수 있음을 확인하였다.

• 분석과학
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• 제17권1호
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• pp.1-7
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• 2004

N-nitroso-N-phenylhydroxylamineammonium salt(cupferron)과 tetrabutylammonium ion ($TBA^+$)을 사용하여 수용액 중 미량 Mn(II)을 상승 용매 추출하는 법에 대해서 연구하였다. $TBA^+$가 존재할 때 cupferron으로 수용액 중의 Mn(II)을 추출하면 용액의 pH 4-10 범위에서 95% 이상이 추출되지만 $TBA^+$가 존재하지 않으면 거의 추출되지 않았다. 이런 조건에서 Mn(II)의 추출은 $CH_2Cl_2$나 $CHCl_3$와 같은 유기용매를 사용 할 때가 다른 비극성 용매를 사용할 때 보다 현저히 잘 추출되었으므로 여기서는 chloroform을 사용하였다. 그리고 수용액의 pH는 5로 조절하였다. 실제시료 중 존재하는 극미량의 Mn(II)을 정량하기 위해서는 chloroform에 추출된 Mn(II)을 다시 0.1 mol/L $HNO_3$용액에 역 추출하여 GF-AAS로 Mn(II)의 흡광도를 측정하였다. 본 방법으로 얻은 Mn(II)의 검출한계는 0.37 ng/mL이었고, 이 방법을 응용하여 실험실 수돗물 중 Mn(II)을 정량한 결과는 0.4-1.01 ng/mL로 얻어졌다. 이 시료에 일정량의 Mn(II)용액을 첨가하여 얻은 회수율은 94-107%이었다. 그리고 Cu(II), Ca(II), Fe(III) 등 공존하는 다른 원소는 10 내지 $20{\mu}g/mL$까지 Mn(II) 정량에 방해를 하지 않았다. 이로서 본 방법이 극미량 Mn(II)의 새로운 분석법으로 사용될 수 있을 것으로 생각된다.

• 한국식품위생안전성학회지
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• 제36권4호
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• pp.281-288
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• 2021

GF-AAS와 수은분석기를 이용하여 납, 비소, 카드뮴 및 수은의 회수율로 정확도를 측정한 결과 92.67-102.56% 범위에서 측정되었고, 정밀도를 측정한 결과 0.21-6.00 RSD%의 재현성을 보였으며, CODEX guideline에서 규정하는 범위에 적합하였다. 또한, FAPAS QC material을 검증결과, 회수율은 96.7-102.0%, 재현성은 0.33-4.93 RSD%로 우수한 결과를 나타냈다. 한약재 430건의 평균 Pb 함량은 254.9 ㎍/kg(N.D.-2,515.2)이었고, 평균 As 함량은 171.0 ㎍/kg (N.D.-2,465.2)이었으며, 평균 Cd 함량은 99.2 ㎍/kg (N.D.-797.1), 평균 Hg 함량은 6.0 ㎍/kg (N.D.-83.6)이었다. 분석 결과 우리나라에 유통되는 한약재 20종은 식품의약품안전처에서 규정하는 한약재의 중금속 함량에 대한 허용기준 이내의 결과로 모두 안전한 수준의 한약재로 나타났다. 이를 토대로 한약 규격품 제조업소를 품질관리의 기준으로 하여 유통되기 직전의 가공 포장 과정에서의 한약재 중 납, 비소, 카드뮴 및 수은의 함량을 조사하여 한약재 내 중금속 함량 실태를 파악하고, 국민에게 안전하고 우수한 한약재를 공급하기 위한 기초자료로 활용할 수 있을 것으로 사료된다.

• 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.

• Bulletin of the Korean Chemical Society
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• 제23권10호
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• pp.1381-1391
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• 2002

The solvent sublation using ion pairs of metal-2-naphthoate(2-HNph) and tetrabutyl ammonium ($TBA^+$) ion has been studied for the concentration and determination of ultra trace Bi(III), In(III) and Tl(Ⅲ) ions in water samples. The partition coefficients ($K_p$) and the extraction percentages of 2-HNph and the ion pairs to methyl isobutyl ketone (MIBK) were obtained as basic data. After the ion pair $TBA^+$·M$(Nph)_4^-$ was formed in water samples, the analytes were concentrated by the solvent sublation and the elements were determined by GF-AAS. The pH of the sample solution, the amount of the ligand and counter ion added and stirring time were optimized for the efficient formation of the ion pair. The type and amount of optimum surfactant, bubbling time with nitrogen and the type of solvent were investigated for the solvent sublation as well. 10.0 mL of 0.1 M 2-HNph and 2.0 mL of 0.1 M $TBA^+$ were added to a 1.0 L sample solution at pH 5.0. After 2.0 mL of 0.2%(w/v) Triton X-100 was added, the ion pairs were extracted into 20.0 mL MIBK in a flotation cell by bubbling. The analytes were determined by a calibration curve method with measured absorbances in MIBK, and the recovery was 80-120%.

• Bulletin of the Korean Chemical Society
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• 제21권9호
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• pp.855-859
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• 2000

An application of synergistic solvent extraction for the etermination of trace lithium in sea water has been studied by forming an adduct complex of thenoyltrifluoroacetone (TTA) and trioctylphosphine oxide (TOPO) in a solvent. The interference by major constituents in sea water was eliminated by phosphate precipitation. Ex-perimental conditions such as solution pH, concentrations of TTA and TOPO etc. were optimized in synthetic sea water with similar compositionto its natural counterpart. To eliminate the interference, 1.38g of ammoni-um dihydrogen phosphate and 2.5 mL of ammonia water were added into 100 mL of thediluted solution at $60^{\circ}C$ to form the phosphate precipitates of Ca2+ and Mg2+ ions. After the pH of this filtrate was adjusted to 8.0, 10.0 mL of m-xylene containing 0.1 M TTA and 0.05 M TOPO was added to the solution in a separatory funnel, and the solution was shaken vigorously for 20 minutes. The solvent was separated from the aqueous solution, and 20 uL of m-xylene solution was injected into a gaphite tube to measure the absorbance by GF-AAS. The detection limit was 0.42 ng/mL. Lithium was determined within the range of 146 to 221 ng/mLin Korean coast-al sea waters, and the recoveries in the spiked samples were 94 to 106%.