• Title/Summary/Keyword: 고상미세추출법

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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.

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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Quantification of Odorants from Animal Husbandry using Solid-phase Microextraction (고상(固相) 미세 추출법에 의한 축산 관리시설에서 발생하는 악취성 가스 화합물의 정량적 평가)

  • Kim, Jae-Hyuck;Choi, Hong-Lim;Kown, So-Young;Lim, Hong-Lae;McConnell, Laura L.;Arispe, Susana;Park, Chul-Hwi;Kim, Hyun-Ook
    • Journal of Korean Society of Environmental Engineers
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    • v.28 no.2
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    • pp.158-164
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    • 2006
  • Offensive odor from CAFO(concentrated animal feeding operation) and its control have become a significant issue in Korea. Control of odors from the CAFO requires to identify major odorant and their generation mechanisms. In this study, an easy method to collect gas sample and to quantify its odorants is proposed. The method involves on-site odorant extraction with solid-phase microextraction and quantitation with GC/MSD or GC/FID. Analytes of the current study include: trimethylamine(TMA), carbon disulfide($CS_2$), dimethyl sulfide(DMS), dimethyl disulfide(DMDS), acetic acid(AA), propionic acid(PA) and n-butyric acid(BA). The resulting linearity($R^2$) of calibration curve for each analyte was good over the range from several ppbv to ppmv; 0.984 for TMA(0.056-1.437), 0.996 for $CS_2$(0.039-0.999), 0.994 for DMS(0.029-0.756), 0.995 for DMDS(0.024-0.623), 0.992 for AA(0.068-1.314), 0.955 for PA(0.047-0.940), and 0.976 for BA(0.036-0.712). Method detection limits were 5.67, 6.39, 5.78, 25.2, 0.098, 0.363 and 0.099 ppbv for AA, PA, BA, TMA, DMS, $CS_2$, and DMDS, respectively. With the developed method, odorants from poultry, swine, and cattle barns were analysed. All the compounds but DMDS were detected from the sample collected in the poultry barn, and their levels exceeded the representative published human olfactory threshold.

Synthesis and Biocompatibility of the Hydroxyapatite Ceramic Composites from Tuna Bone(I) - The Sintering Properties of Hydroxyapatite and Hydroxyapatite- Containing Wollastonite Crushed with Dry Milling Process - (참치 뼈를 이용한 Hydroxyapatite 세라믹 복합체의 합성 및 생체 친화성(제1보)-건식법으로 분쇄한 Hydroxyapatite 및 Wollastonite가 첨가된 소결체의 특성-)

  • Kim, Se-Kwon;Lee, Chang-Kook;Byun, Hee-Guk;Jeon, You-Jin;Lee, Eung-Ho;Choi, Jin-Sam
    • Applied Chemistry for Engineering
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    • v.8 no.6
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    • pp.994-999
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    • 1997
  • The sintering properties of hydroxyapatite isolated from tuna bone and hydroxyapatite-containing wollastonite sintered by solid-state reaction was investigated. As the sinterability of hydroxyapatite dependent upon the particle size by dry milling, it showed a sintering. But the hydroxyapatite-containing wollastonite was appeared good sinterability. On X-ray measurements, the major phases of hydroxyapatite-containing wollastonite by solid state reaction at $1250^{\circ}C$ were identified as hydroxyapatite and pseudowollastonite(${\alpha}-CaSiO_3$). And the phases appeared as whitlockite [$Ca_3(PO_4)_2$] by decomposition of hydroxyapatite at higher temperature above $1250^{\circ}C$. The shapes of microstructure on SEM images changed from porous to dense bulk by elevating temperature. The mean bending strength of hydroxyapatite-containing wollastonite sintered by solid-state reaction at $1300^{\circ}C$ was about 18 MPa, it was close to the cancellous bone's maximum strength, 20 MPa.

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Synthesis and Biocompatibility of the Hydroxyapatite Ceramic Composites from Tuna Bone(II) - The Sintering Properties of Hydroxyapatite Treated with Wet Milling Process - (참치 뼈를 이용한 Hydroxyapatite 세라믹 복합체의 합성 및 생체 친화성(제2보)-습식법에 의한 Hydroxyapatite 소결체의 특성-)

  • Kim, Se-Kwon;Choi, Jin-Sam;Lee, Chang-Kook;Byun, Hee-Guk;Jeon, You-Jin;Lee, Eung-Ho
    • Applied Chemistry for Engineering
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    • v.8 no.6
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    • pp.1000-1005
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    • 1997
  • The properties of ceramics by solid-state reaction with hydroxyapatite[$Ca_{10}(PO_4)_6(OH)_2$], which was isolated from tuna bone by wet milling process were investigated. The bulk density $2.93g/cm^3$ at $1350^{\circ}C$ was close to the calculated density $3.21g/cm^3$. On X-ray measurements, the major phases were identified as hydroxyapatite at below $1300^{\circ}C$, but the whitlockite [$Ca_3(PO_4)_2$] phases were appeared due to a decomposition of hydroxyapatite with temperature. The microstructures of sintering specimens were shown as small closed pores between grain boundaries. The mean bending strength of the sintered hydroxyapatite by solid-state reaction is about 58 MPa and this value is higher than that of the articular cartilage maximum strength, 40MPa.

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A Study on the Synthesis and the Electrochemical Properties of $LiNi_{1-y}$${Co_y}{O_2}$from $Li_2$$CO_3$, ${NiCO_3}$, and $CoCO_3$ ($Li_2$$CO_3$, ${NiCO_3}$, $CoCO_3$로부터 $LiNi_{1-y}$${Co_y}{O_2}$의 합성 및 전극특성 연구)

  • Rim, Ho;Kang, Seong-Gu;Chang, Soon-Ho;Song, Myoung-Youp
    • Journal of the Korean Ceramic Society
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    • v.38 no.6
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    • pp.515-521
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    • 2001
  • 출발 물질로서 L $i_2$C $O_3$, NiC $O_3$, CoC $O_3$를 사용하고 조성과 합성 온도를 변화시켜, 고온 고상법에 의하여 LiN $i_{1-y}$ $Co_{y}$ $O_2$(y=0.1, 0.3, 0.5)를 합성하였다. 합성과 시료들의 결정구조, 미세구조 그리고 전기화학적 특성을 조사하였다. 80$0^{\circ}C$와 8$50^{\circ}C$에서 제조한 L $i_{x}$N $i_{1-y}$ $Co_{y}$ $O_2$는, 삼방정계(space group: R3m)의 $\alpha$-NaFe $O_2$구조로 결정화되어 있는 층상 구조를 형성하였다. LiN $i_{1-y}$ $Co_{y}$ $O_2$(y=0.1, 0.3, 0.5)는 Co의 양이 증가함에 따라 a축과 c축의 크기가 감소하였는데, 이는 코발트 이온의 크기가 니켈 이온의 크기보다 작은데 기인하는 것이다. 그러나 c축과 a축의 크기의 비(c/a)가 증가하였음은 이차원적 구조가 잘 발달됨을 보여준다. 니켈에 대한 코발트의 치환량에 따른 리튬 이온의 삽입/추출 가역성은 코발트의 치환량이 증가하면서 증가하여 y=0.3인 LiN $i_{0.9}$ $Co_{0.1}$ $O_2$에서 대체로 우수하였고 그 이상으로 y값이 증가하면 가역성이 나빠졌다. 80$0^{\circ}C$에서 합성한 LiN $i_{0.9}$ $Co_{0.1}$ $O_2$가 가장 큰 초기 방전 용량 146 mAh/g을 나타내었으며, 싸이클링 성능도 비교적 우수하였다. 8$50^{\circ}C$에서 합성한 LiN $i_{0.9}$ $Co_{0.1}$ $O_2$와 LiN $i_{0.7}$ $Co_{0.3}$ $O_2$가 우수한 싸이클링 성능을 보였다.다. 싸이클링 성능을 보였다.다.보였다.다.

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Preparation and Characterization of Tungsten Carbide Using Products of Hard Metal Sludge Recycling Process (초경합금 슬러지 재활용 공정 산물을 활용한 텅스텐 탄화물 제조 및 특성 평가)

  • Kwon, Hanjung;Shin, Jung-Min
    • Resources Recycling
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    • v.31 no.4
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    • pp.19-25
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    • 2022
  • In this study, tungsten carbide (WC) powder was prepared using a novel recycling process for hard metal sludge that does not use ammonium paratungstate. Instead of ammonia, acid was used to remove the sodium and crystallized tungstate, resulting in the formation of tungstic acid (H2WO4). The WC powder was successfully synthesized by the carbothermal reduction of tungstic acid through H2O decomposition, reduction of WO3 to W, and formation of WC. The carbon content and holding time at the carbothermal reduction temperature were optimized to remove free carbon from the WC powder. As a result, most of the free carbon in the WC powder prepared from sludge was removed, and the content of free carbon in the synthesized WC powder was lower than that in commercial WC powder. Moreover, the crystallite size of WC prepared from H2WO4 was much smaller than that of commercial micron-sized WC powder produced from APT. The small crystallite size of WC induces grain growth during the sintering of the WC-Co composite; thus, a WC-Co composite with large WC grains was fabricated using the WC powder prepared from H2WO4. The large WC grains affected the mechanical properties of the WC-Co composite. Further, due to the large grain size, the WC-Co composite fabricated from H2WO4 exhibited a higher toughness than that of the WC-Co composite prepared from commercial WC powder.