• Title/Summary/Keyword: 고상 추출법

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Evaluation of 226Ra analysis methods using a gamma-ray spectrometer and a liquid scintillation counter (감마선분광분석기와 액체섬광계수기를 이용한 226Ra 분석법 비교 연구)

  • Ju, Byoung Kyu;Kim, Moon Su;Kim, Hyun Koo;Kim, Dong Su;Cho, Sung Jin;Yang, Jae Ha;Park, Sun Hwa;Kim, Hyoung Seop;Kwon, Oh Sang;Kim, Tae Seung
    • Analytical Science and Technology
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    • v.28 no.3
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    • pp.228-235
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    • 2015
  • The efficiency and applicability of the solid phase extraction disk method in a 226Ra analysis were examined by the gamma ray spectrometer (GRS) method using a Marinelli beaker and the liquid scintillation counter (LSC) method for groundwater. The recovered 226Ra, which was filtered by the solid phase extraction disk, was analyzed using gamma ray spectrometer The disks, which were pretreated for caulking the daughter nuclide, were sealed with polyethylene film. Distilled water was used for the blank value of the 226Ra activity. The recovery values of 214Bi and 214Pb in the solid phase extraction disk, which used 226Ra standard material, were 80% (295.21 Kev) and 104% (351.92 Kev), respectively, which were higher than 75% determined by the LSC. The injection of nitrogen gas into the measuring chamber reduced the interference values by about 10%. The detection limits of the 226Ra activity in a blank sample of 5 L were 0.17~0.40 pCi/L after 80,000 seconds of measuring time. The relationship of the 226Ra activity in the solid phase extraction disk method and in the LSC method in seven groundwater samples showed a correlation coefficient value 0.987, which implies the applicability of the solid phase extraction disk method. The results showed that 226Ra activity in groundwater using the solid phase extraction disk method has the following benefits: simple pretreatment, time saving, high recovery values, a low detection limit, and so on. Compared with the LSC method and the GRS method using the Marinelli beaker for the 226Ra analysis, the solid phase extraction disk method could be useful in groundwater samples with low levels of activities of radionuclides because the method is not restricted by the volume of the sample.

울산지역 폐수 중 프탈레이트 에스테르 및 비스페놀 A(환경호르몬)의 GC/MS 분석

  • Han, Yeong-Ju;Park, Jin-Do;Lee, Hak-Seong
    • Proceedings of the Korean Environmental Sciences Society Conference
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    • 2008.11a
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    • pp.248-251
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    • 2008
  • 일반적으로 phthalate esters의 전처리방법에는 액액추출법(liquid-liquid extraction), 고상추출법(Solid-phase Extraction, SPE), 고상미세추출법(Solid-phase micro extraction, SPME) 등의 분석방법이 있다. 그 중에서 본 연구에서는 SPE를 이용하여 간편하고 정확성이 높으며, 적은 양의 유기용제를 사용하여 전처리함으로써 2차적인 환경오염을 줄일 수 있다는 점에서 다른 전처리 방법보다 유용하다고 할 수 있다. 검출감도 측면에서 phthalate esters의 경우는 구조적으로 안정적인 편이나 페놀류의 경우 hydroxy group 때문에 GC/MS 분석시 유도체화 과정이 필수적인데 이번 연구에서 사용한 BSTFA/TMCS는 비교적 쉽고 빠르게 유도체 화할 수 있다는 이점이 있다. 더 많은 연구가 필요하겠지만 앞서서의 결과에서도 알 수 있듯이 전반적으로 검출한계가 0.05$\sim$0.5 $\mu$g/L 정도로 높고, 4-nonyl phenol을 제외하고 80% 이상의 양호한 회수율을 나타낸 것으로 미루어 보아 phthalate esters, phenols의 효율적인 동시분석이 가능함을 알 수 있다.

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울산지역 폐수 중 프탈레이트 에스테르 및 비스페놀 A의 HPLC 분석

  • Han, Yeong-Ju;Park, Jin-Do;Lee, Hak-Seong
    • Proceedings of the Korean Environmental Sciences Society Conference
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    • 2008.11a
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    • pp.272-274
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    • 2008
  • 일반적으로 프탈레이트 에스테르의 전처리방법에는 액액추출법(Liquid Liquid Extraction, LLE), 고상추출법(Solid Phase Extraction, SPE), 고상미세추출법(Solid Phase Micro Extraction, SPME) 등의 분석방법이 있다. 그 중에서 본 연구에서는 간편하고 정확성이 높은 SPE를 이용하였으며, 적은 양의 유기용제를 사용하여 전처리함으로써 2차적인 환경 오염을 줄일 수 있다는 점에서 다른 전처리 방법보다 유용하다고 할 수 있다. 또한 프탈레이트 에스테르의 경우는 구조적으로 안정적인 편이나 페놀류의 경우 hydroxy group 때문에 GC/MS 분석시 유도체화 과정이 필수적이나 이번 연구에서는 HPLC를 이용하므로 별도의 유도체화의 번거로움 없이 바로 분석할 수 있는 이점이 있다. 더 많은 연구가 필요하겠지만 앞서서의 결과에서도 알 수 있듯이 전반적으로 검출한계가 0.1$\sim$0.5$\mu$g/L 정도로 높고, 82% 이상의 양호한 회수율을 나타낸 것으로 미루어 보아 극미량 분석이 아닌 이상, 산업체에서 HPLC의 이용이 더욱 유리할 것이라고 사료된다.

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Quantification of Volatile Organic Compounds in Gas Sample Using Headspace Solid-Phase Microextraction (고상 미세 추출법을 이용한 가스시료 중 휘발성유기화합물의 정량 분석)

  • Kim, Jae Hyuck;Kim, Hyunook
    • Journal of Korean Society of Environmental Engineers
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    • v.35 no.12
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    • pp.906-917
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    • 2013
  • The purpose of this study is to quantify volatile organic compounds (VOCs) in gas sample using headspace solid-phase microextraction (HS-SPME) coupled to GC analysis. The optimal HS-SPME conditions was CAR/PDMS fiber and 30 min absorprion time for the analysis of various VOCs. In optimal conditions, 80 VOCs could be detected within 1 ppbv and even less than 0.0005 ppbv especially in the case of BTEX. However, fiber reproducibility on adsorption efficiency was 1~9.2% (between the same fiber) and 5.9~13.5% (between the other fiber). We successfully determined 35 VOCs in landfill gas with this method and found that VOCs of high concentration are emitting from vent pipe of closed/open landfill site under the HS-SPME conditions. This method may apply to VOCs/odor determination from various atmospheric environmental samples as well as landfills.

Optimization of solid phase extraction and simultaneous determination of trace anions in concentrated hydrofluoric acid by ion chromatography (불산 중 극미량 음이온 분석을 위한 고상 추출법 및 이온크로마토그래프를 이용한 동시분석법 확립)

  • Yoon, Suk-Hwan;Jo, Dong-ho;Kim, Hyun-Ji;Shin, Ho-Sang
    • Analytical Science and Technology
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    • v.29 no.5
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    • pp.219-224
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    • 2016
  • 불산 중 극미량 음이온의 고상추출과 이온크로마토그래프를 이용한 고감도 분석법이 개발되었다. 불산 중 불소이온이 고상에 의해 제거하였고 이어서 음이온 (F, CH3COO, Cl, Br, NO3, PO43−, SO42−)들이 이온크로마토그래프를 이용하여 연속적으로 분리하였다. 고상 추출법에 영향을 주는 각 인자들 (흡착제의 선택, 시료의 부피 및 pH, 용출 용액과 용출용액의 부피)을 결정하였으며 그 결과 흡착제로서 Oasis WAX 컬럼이 가장 우수하였고 1.0 mL의 시료부피, 용출용액으로 50 mM 초산암모늄염 5 mL가 분리능에서 가장 우수하였다. 개발한 방법에 의한 음이온 (Cl, Br, NO3, PO43−, SO42−)들의 방법검출한계는 25 % 불산용액 (w/w) 중에 0.04~0.30 µg/L의 범위를 보였고 정밀도는 20.0와 40.0 µg/L의 농도에서 5 % 이내를 보였다. 한 제조회사에 의한 25 % 불산 중 음이온의 4.2에서 47.5 µg/L의 범위로 모두 검출되었다. 이 방법은 시험절차가 간단하고, 재현성 및 감도가 좋아서 반도체회사에서 불산 중 음이온 불순물을 정도 관리하는데 매우 유용한 방법이 될 것으로 판단된다.

Isolation and Analysis of Micro-Regions Having Possibly Higher Tc in Oxide Superconductors (산화물계 초전도체의 고변이 송도부근의 곡출과 이의 성분 분석에 관한 연구)

  • 이규용
    • Journal of the Korean Society of Fisheries and Ocean Technology
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    • v.25 no.3
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    • pp.143-153
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    • 1989
  • In conclusion, a high-Tc superconducting YBa sub(2) Cu sub(3) O sub(y) phase with zero resistance at about 90K was successfully prepared by nitrate solution method with densed micro structure. The result of the EDAX analysis on the isolated particles using the microscopic meissner effect showed that the particles were isolated at higher temperature due to the differences in O vacances rather than the differences in chemical compositions. The composition of the isolated particles were almost identical to the starting compositions on the samples prepared by the solid reaction and nitrate solution method but the Ba-rich composition were seen in the coprecipitated sample. The isolation process on Bi system was not successful due to the weak dimagnetism even though its high Tc above the liquid nitrogen temperature.

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Characterization of Adsorbents for the Simultaneous Solid-Phase Extraction of Trace $\beta$-Blockers from Biological Samples (생체시료로부터 미량 $\beta$-Blockers의 동시고상추출에 사용될 흡착제들의 특성)

  • Kim, Kyoung Rae;Kim, Do Jeong
    • Analytical Science and Technology
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    • v.6 no.4
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    • pp.375-381
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    • 1993
  • The efficiencies of four different solid absorbents were evaluated for the simultaneous solid-phase extraction of six ${\beta}$-blockers from biological sample. Chromosorb 107 using methanol as the eluting solvent gave the highest solid-phase extraction yield. From the breakthrough studies of ${\beta}$-blockers, the excellent sorption and desorption properties of the Chromosorb 107 column were verified. The usefulness of Chromosorb 107/methanol was examined for the simultaneous solid-phase extraction of the ${\beta}$-blockers from serum in the concentration range of 2~8ppm.

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The Study on the Rapid Screening of Schedule Chemicals in Aqueous Solution Using SPE-ACF (수용액에서 SPE-ACF를 이용한 특정화학물질의 신속 스크리닝 기법 연구)

  • Park, Hoon;Jung, Chang-Hee;Lee, Yong-Han;Hong, Dea-Sik
    • Journal of the Korean Chemical Society
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    • v.52 no.3
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    • pp.239-248
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    • 2008
  • study of the solid phase extraction (SPE) technique using activated carbon fiber (ACF) as a sorbent was carried out on the schedule chemicals in water. 14 different schedule chemicals, which are the hydrolysis products and simulants of chemical agents such as alkylphosphonate, thiodiglycol etc. were selected for the study. Pyridine was used as a promoter to increase the derivatization efficiency, especially to improve silylation of 3-quinuclidinol. To improve the recovery efficiency of amines in the water solution, 1 mL of 5% Et3N/MeOH was introduced into SPE-ACF before the water sample loading. Throughout this study, the optimum condition was established to detect rapidly above chemicals in water.