• 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.

• 약학회지
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• 제25권4호
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• pp.193-197
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• 1981

Germanium (Ge) content in Zingiberis Rhizoma was determined by flameless atomic absorption spectrometry with a graphite tube atomizer. The Ge content of the cortical layer was 65.mu.g/g, the central cylinder, $98\mu$g/g and the total, $87\mu$g/g. In the effect of the extraction of Ge by various solvents, polar solvent was more effective than the nonpolar one, Especially, water was the most effective solvent. The water extract of Zingiberis Rhizoma, separated by sephadex G-25 gel filtration, was fractionated into 2 peaks at 254nm. Both the peaks showed atomic absorptions of Ge. It may be concluded that the Ge components of Zingiberis Rbizoma exist as the form of an aqueous organic compounds or associated forms with proteins.

• 한국환경보건학회지
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• 제47권5호
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• pp.496-503
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• 2021

Background: Considering the expenses of and difficulties in arsenic speciation by high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS), alternative measurement methods should be useful, especially for large-scale research and projects. Objectives: A measurement method was developed for arsenic speciation using HPLC-atomic fluorescence spectrometry (HPLC-AFS) as an alternative to HPLC-ICP-MS. Methods: Total arsenic and toxic arsenic species in some seafoods were determined by atomic absorption spectrometry coupled with hydride vapor generation (AAS-HVG) and HPLC-AFS, respectively. Recovery rate of arsenic species in seafood was evaluated by ultra sonication, microwave and enzyme (pepsin) for the optimal extraction method. Results: Limits of detection of HPLC-AFS for As³⁺, dimethylarsinate (DMA), monomethylarsonate (MMA) and As⁵⁺ were 0.39, 0.53, 0.60 and 0.64 ㎍/L, respectively. The average accuracy ranged from 97.5 to 108.7%, and the coefficient of variation was in the range of 1.2~16.7%. As³⁺, DMA, MMA and As⁵⁺ were detected in kelp, the sum of toxic arsenic in kelp was 40.4 mg/kg. As³⁺, DMA, MMA and As⁵⁺ were not detected in shrimp and squid, but total arsenic (iAS and oAS) content in shrimp and squid analyzed by AAS-HVG were 18.1 and 24.7 mg/kg, respectively. Conclusions: HPLC-AFS was recommendable for the quantitative analysis method of arsenic species. As toxic arsenic species are detected in seaweeds, further researches are needed for the contribution degree of seafood in arsenic exposure.

• 방사선산업학회지
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• 제8권1호
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• pp.17-22
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• 2014

In this study, we prepared CdTe/CdS solar cells using a thermal vacuum evaporation method. In particular, $CdCl_2$ treatment was attempted using this same method at $400^{\circ}C$ for 30 min. The prepared CdTe/CdS solar cells were investigated using Fouier transform infrared spectrometry (FTIR), field emission scanning electron microscopy (FE-SEM), and a solar simulator system including light absorption properties, morphological properties, and power conversion efficiency (PCE). In addition, we investigated the gamma-irradiation treatment at dose rates of 0 Gy, 500 Gy, 1 kGy, 10 kGy, and 30 kGy. The characteristics of gamma-irradiation treatment were studied based on the same method described above. In particular, it showed increased values as 0.826% higher than the non-irradiation of 0.448% from PCE analysis.

• 대한화학회지
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• 제36권2호
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• pp.273-281
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• 1992

원자흡수분광법을 위한 글로우방전 분광 장치를 sputtering된 시료원자가 기저상태의 원자가 최대이며 여기 상태의 원자가 최소가 되는 지역을 측정하도록 설계 개발하였다. 빠른 속도의 가스 jet는 방전의 육안 및 전기적 변화 뿐만 아니라 시료표면의 변화에서 처럼 시료가 원자화되는 양을 현저히 증가시킨다. 가스 jet는 원자흡수분광법으로 시료를 직접할 수 있는 가능성을 보여주었다. 감도와 재현성에 영향을 끼치는 여러 가지 요인들에 관하여 연구하였다.

• 한국환경보건학회지
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• 제41권5호
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• pp.289-298
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• 2015

Objectives: The method of analyzing urinary arsenic by flow injection hydride generation atomic absorption spectrometry (FI-HG-AAS) is generally used because it shows relatively greater sensitivity, low detection limits, low blocking action, and is simple to operate. In this study, the results of analysis according to three pre-reductants commonly used in the FI-HG-AAS method were compared with each other. Methods: To analyze urinary arsenic, nineteen urine samples were collected from adults aged 43-79 years old without occupational arsenic exposure. Analysis equipment was FI-HG-AAS (AAnalyst 800/FIAS 400, Perkin- Elmer Inc., USA). The three pre-reductants were potassium iodide (KI/AA), C3H7NO2S (L-cysteine), and a mixture of KI/AA and L-cysteine (KI/AA&L-cysteine). Results: In the results of the analysis, the recovery rate of the method using KI/AA was 82.3%, 95.7% for Lcysteine, and 123.5% for KI/AA and L-cysteine combined. When compared with the results by use of high performance liquid chromatography inductively-coupled plasma mass spectrometry (HPLC-ICP-MS), the method using L-cysteine was the closest to those using HPLC-ICP-MS ($98.57{\mu}g/L$ for HPLC-ICP-MS; $74.96{\mu}g/L$ for L-cysteine; $69.23{\mu}g/L$ for KI/AA and L-cysteine; $13.06{\mu}g/L$ for KI/AA) and were significantly correlated (R2=0.882). In addition, they showed the lowest coefficient of variation in the results between two laboratories that applied the same method. Conclusion: The efficiency of hydride generation is considered highly important to the analysis of urinary arsenic via FI-HG-AAS. This study suggests that using L-cysteine as a pre-reductant may be suitable and the most rational among the FI-Hg-AAS methods using pre-reductants.

• 분석과학
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• 제11권4호
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• pp.271-280
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• 1998

국내에서 재배 생산된 현미로 부터 표준물질을 가공하여 원소별 검정분석을 실시하였다. 주요 오염원소의 농도가 서로 다른 2종의 쌀분말 표준물질을 제조하였는데 1종은 정상치시료로서 분말 시료를 그대로 처리하였으며, 1종은 제조과정중에 As, Cu, Pb, Hg, Cr, Cd등 6개의 중금속원소를 건조중량기준 $1.0{\mu}g/g$씩 첨가한 고농도 오염시료로서 제조하였다. 제조된 시료는 중성자방사화분석법 (NAA)과 불꽃원자흡수분광법(FAAS)으로 Cd, Cu, Fe, Mn, Zn등 5개 원소에 대한 균질도 분석을 실시하여 기준불질로서의 균질성을 확인하였다. 쌀시료의 분해 및 전처리에는 고온가압법과 마이크로파분 해법을 사용하였으며, NAA, FAAS, 흑연로원자흡수분광법(GFAAS), 유도플라즈마방출분광법(ICP-AES), 동위원소희석질량분석법(IDMS), 증기발생법 등을 이용하여 쌀분말표준물질 소재의 원소별 정량 분석을 실시하였다. 이들 각 방법의 원소별 분석결과를 이용하여 P, K, Mg, As, Ca, Cd, Cr, Cu, Fe, Mn, Mo, Na, Zn, Pb, Se, Hg등 16개 원소에 대한 검정값 및 참고값을 확정하였다.

• 분석과학
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• 제13권2호
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• pp.179-188
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• 2000

대기환경시료인 도시분진시료와 인공적으로 준비한 휠터상 도시분진시료중의 미량원소를 중성자방사화분석법을 사용하여 비파괴 분석하였다. 분석정도관리를 위하여 미국 표준기술원의 인증표준시료 (Urban Dust, NIST SRM 1648)를 이용하였다. 37종의 검출된 원소의 상대오차와 상대 표준편차를 계산하였으며 각각 10%와 15%이내이었다. 도시분진시료로부터 29종의 원소, 휠터상 도시분진시료로부터 21종의 원소를 정량하였다. 측정결과의 신뢰도 및 숙련도 평가를 위하여, 중성자방사화분석법, 하전입자유도 X-선방출분광법, X-선 형광분석법과 원자흡수분광법을 이용한 세계 39개 실험실이 참여한 실험실간 비교시험에 참여하였으며 수집된 결과를 통계처리하였다. 평균값과 표준편차로 계산한 z-score는 몇개의 원소를 제외하고 모두 -1

• 한국재료학회지
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• 제21권10호
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• pp.525-531
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• 2011

Two dimensional (2D) arrays of noble metal nanoparticles are widely used in the sensing of nanoscale biological and chemical events. Research in this area has sparked considerable interest in many fields owing to the novel optical properties, e.g., the localized surface plasmon resonance, of these metallic nanoarrays. In this paper, we report successes in fabricating 2D arrays of gold nano-islands using nanosphere lithography. The reproducibility and the effectiveness of the nano-patterning method are tested by means of spin coating and capillary force deposition. We found that the capillary force deposition method was more effective for nanospheres with diameters greater than 600 nm, whereas the spin coating method works better for nanospheres with diameters less than 600 nm. The optimal deposition parameters for both methods were reported, showing about 80% reproducibility. In addition, we characterize gold nano-island arrays both geometrically with AFM as well as optically with UV-VIS spectrometry. The AFM images revealed that the obtained nano-arrays formed a hexagonal pattern of truncated tetrahedron nano-islands. The experimental and theoretical values of the geometric parameters were compared. The 2D gold nano-arrays showed strong LSPR in the absorption spectra. As the nano-islands increased in size, the LSPR absorption bands became red-shifted. Linear dependence of the plasmon absorption maximum on the size of the gold nano-islands was identified through the increment in the plasmon absorption maximum rate for a one nanometer increase in the characteristic length of the nano-islands. We found that the 2D gold nano-arrays showed nearly seven-fold higher sensitivity of the absorption spectrum to the size of the nano-islands as compared to colloidal gold nano-particles.

• 분석과학
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• 제24권6호
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• pp.443-450
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• 2011

ICP-AES와 AAS를 이용하여 세라믹, 금속 및 플라스틱 소재에 함유된 니켈을 정량하기 위한 조건을 연구하였다. 니켈 정량을 위해 산분해하여 조제된 시험 용액을 직접 ICP-AES 또는 AAS로 분석할 때 철이나 크로뮴 등의 원소가 방해하므로, 니켈을 dimethylglyoxime으로 착화시키고 $CHCl_3$로 추출하여 방해원소로부터 분리한 후 $CHCl_3$을 제거하고 염산으로 용해하여 측정하였다. 니켈에 대한 측정 회수율이 우수하였고, 방해를 일으키는 매질원소를 효율적으로 제거할 수 있어 본 방법은 인증표준물질(BAM-376 및 PACS-2)에 대한 용매추출시험에서 matrix의 영향을 받지 않고 니겔을 정량할 수 있었다.