• Title/Summary/Keyword: 고상추출

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Sample Preparation for Quantitative Determination of Bisphenols in Canned Beverages Coated with Epoxy by RP-HPLC (RP-HPLC 에 의한 에폭시 통조림관 음료 중 비스페놀류의 분석을 위한 시료의 전처리)

  • Kang, Kyung-Mo;Lim, Heung-Youl;Shin, Hyo-Sun
    • Korean Journal of Food Science and Technology
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    • v.32 no.5
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    • pp.1029-1034
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    • 2000
  • A suitable method of sample treatments to minimize the analytical interferences was presented in order to determine bisphenols [bisphenol F (BPF), bisphenol A (BPA), bisphenol F diglycidyl ether (BFDGE), and bisphenol A diglycidyl ether (BADGE)] in various canned beverages coated with epoxy resin by the reversephase high performance liquid chromatography (RP-HPLC) equipped with a fluorescence detector and the gas chromatography with mass selective detection. The recovery test of bisphenols was performed using 1, 5, and 10 ${\mu}g/L$ bisphenols spiked beverages with the combined technique of the solid-phase extraction (SPE) and the liquid-phase extraction (LPE). Both BPA and BADGE showed quite adequate resolutions in HPLC-chromatograms. The recoveries of BPA obtained by LPE with diethyl ether were higher than those obtaind with methylene chloride on coffee, shikhye and fruit juice. For cola and tea, the recoveries of BPA obtaind by SPE were higher than those by LPE with diethyl ether. The recoveries of BADGE were less than those of BPA for all beverage samples treated by either SPE or LPE method. In survey of bisphenols for eighteen commercial canned beverage samples, BPA contents of coffee, cola, tea, shikhye, and fruit juice were in the range of $1.3{\sim}11.6,\;0.5{\sim}0.9,\;1.0{\sim}1.3,\;2.4{\sim}7.9$, and $3.0{\sim}3.4\;{\mu}g/L$, respectively, but there was no detection of BPA in beer sample.

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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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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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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.

Feasibility of Fibrous Solid Phase Extraction to Alkylphenols Analysis (섬유상 고상 추출물질을 이용한 알킬페놀 화합물 분석 가능성)

  • Jung, Yong Jun
    • Journal of Korean Society on Water Environment
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    • v.27 no.3
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    • pp.329-333
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    • 2011
  • p-phenylene-2,5-benzobisoxazole (PBO; Zylon$(R)$) fibers as an adsorbent were employed for solid phase extraction of aqueous alkylphenols. The removal ratios for 10 kinds of alkylphenols at initial concentration of $100{\mu}gL^{-1}$ were in the range of 16.8-96.3% and the removals increased with the increase of the phase ratio (fiber weight/solution volume). The plots of the logarithm of partition coefficient (log K) were correlated with the logarithm of the n-octanol/water partition coefficient (log P). The adsorbed alkylphenols were completely desorbed with the mixture of acetonitrile and dichloromethane.