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GC/MS를 이용한 수질시료 중 2,4-D와 2,4,5-T의 분석에 관한 연구
표희수,신혜승,박송자 한국환경독성학회 2000 환경독성보건학회지 Vol.15 No.3
Chlorophenoxy acid류는 제초제로 폭넓게 사용되고 있는 농약 중의 하나이다. 특히 2,4-D와 2,4,5-T는 내분비계 장애 물질 중의 하나로 알려져 있다. 본 연구에서는 이 두 가지 물질을 산성하에서 액체-액체 추출법으로 추출한 후 유도체화하여 GC/MS로 분석하였다. 추출용매로 methylene chloride와 diethyl ether를 사용하여 추출율을 비교한 결과 ether를 사용한 경우 2,4-D는 약 98% 2,4,5-T는 약 82%의 좋은 회수율을 보였다. 또한 산성기를 유도체화하기 위하여 CH₃I/Acetone-K₂CO₃와 황산/메탄올로 각각 methylation실험을 행하였고, 산성조건에서 triflouroethanlo (TFAA/TFE)과 반응시켜 각각의 검출검도를 비교하였다. 그 결과 TFAA/TFE를 사용하여 반응시킨 결과 감도가 좋을 것으로 나타났다. Chlorophenoxy acids are one of the most useful classes of chlorinated herbicides. Specially 2,4-D and 2,4, 5-T were known to endocrine distruptors. In this study, these pesticides in water samples were extracted by liquid-liquid extration at acidic conditions and then derivatization of acidic group was carried out various esterifications using by CH₃I/Acetone-K₂CO₃, H₂SO₄/Me0H or TFAA/TFE. That result, Sensitivities of TFE derivatized 2,4-D and 2,4,5-T are prior to the others. The recoveries of 2,4-D and 2,4,5-T were 98% and 82% respectively using diethyl ether as an extracting solvent.
비점오염물질 저감을 위한 가정용 소규모 빗물 정원 연구
박희수(Heesoo Park),김성표(Seong-Pyo Kim) 한국산학기술학회 2014 한국산학기술학회 학술대회 Vol.- No.-
도시의 개발사업에 따른 불투수면 확애로 인해 비점오염물질로 인한 4대강의 비점부하율은 1998년에 약 27%에서 2010년에는 약 68%로 증가하였으며 2020년에는 약 72%까지 증가될 것으로 전망된다. 본 연구에서는 이러한 비점오염물질의 증가율을 저감시키기 위해 가정용 소규모 빗물 정원의 연구가 필요하다고 보고 연구를 진행하였다. 본 연구에서 사용된 여재 및 식생은 가정에서 구하기 쉬운 것으 로 선택하였다. 여재는 자갈 5mm/10mm, 톱밥, 모래, peatmoss를 사용하였으며 식생으로는 창포, 잔디 를 선택하였다. 빗물 정원은 자갈 10mm, 톱밥, 모래(Type A), 자갈 5mm, 우드칩, 모래(Type B), 자갈 10mm, 잔디, 모래(Type C), 자갈 10mm, 창포, 모래(Type D), 자갈, 잔디, 모래 + paetmoss(Type E) 로 구성하였고 초기 오염물질의 농도는 T-N 12.6mg/L, T-P 2.5mg/L, COD 9mg/L로 하였다. 오염물 질 제거율이 가장 높은 빗물 정원은 Type E로 확인되었으나 전반적으로 제거율이 낮게 나타나 더 높 은 오염물질 제거율을 위해 추가 실험이 필요하다고 보인다.
On, Jiwon,Pyo, Heesoo,Myung, Seung-Woon Elsevier 2018 Science of the Total Environment Vol.639 No.-
<P><B>Abstract</B></P> <P>The aim of this study was to optimize the dispersive liquid–liquid microextraction (DLLME) parameters for simultaneous analysis through DLLME-gas chromatography–mass spectrometry (GC–MS) of six iodo-trihalomethanes, four haloacetonitriles, and one halonitromethane, which are residual disinfection products found in drinking water. Eleven disinfection by-product (DBPs) remaining in aqueous samples were extracted and concentrated using a simple, rapid, and environmentally friendly DLLME method, and then analyzed simultaneously by GC–MS. The optimized DLLME parameters were a sample volume of 5 mL, 100 μL of dichloromethane as the extraction solvent, 1 mL of methanol as the dispersion solvent, an extraction time of 60 s, and 1.5 g of sodium chloride for the salting out effect. The enrichment factor values obtained using the established DLLME-GC–MS method were 19.8–141.5, and the limit of detection and limit of quantification were 0.22–1.19 μg/L and 0.75–3.98 μg/L, respectively. The calibration curves had correlation coefficients (r<SUP>2</SUP>) of 0.9958–0.9992 in the concentration range of 0.5–40 μg/L, and they exhibited good linearity in quantitative analysis. This new method could be useful for analyzing eleven DBPs that remain in drinking water.</P> <P><B>Highlights</B></P> <P> <UL> <LI> We established a DLLME-GC–MS method for analyze 11 DBPs in drinking water. </LI> <LI> 11 DBPs include six iodo-THMs, four HANs, and one HNMs. </LI> <LI> DLLME is an environmentally friendly, rapid, and economical LPME method. </LI> <LI> The EF values were 19.8–141.5. </LI> <LI> The LOD and LOQ were 0.22–1.19 μg/L and 0.75–3.98 μg/L. </LI> </UL> </P> <P><B>Graphical abstract</B></P> <P>Scheme. Diagram of the DLLME sample preparation procedure for analysis of 11 Disinfection Byproducts in drinking water.</P> <P>[DISPLAY OMISSION]</P>
기체크로마토그래피/질량분석계에 의한 물시료 중 EDTA와 NTA의 분석 및 위해성 평가
박송자,표희수,홍지은 한국환경독성학회 2000 환경독성보건학회지 Vol.15 No.3
Ethylenediaminetetraacetic acid (EDTA) and nitrilotriacetic acid (NTA) are various applied as chelating agents for metal ions, then they are widely used in many industrial processes and domestic products. A method is described for the determination of EDTA and NTA in water samples by GC/MS. The reaction temperature, reaction time and pH for esterification of EDTA and NTA were investigated using 10% sulfuric acid-methanol, ethanol and propanol. Optimum conditions were obtained by the esterification in 80℃ for 1hr with ethanol. Method detection limits of ethylated EDTA and NTA in the 200 ml of water samples were 0.05ng/ml, respectively. EDTA and NTA could be determined in the range of 0.05~23.6 and 0.05~7.0ng/ml in treated water, and in the range of 0.06~25.0 and 0.05--6.40ng/ml in raw water respectively. Risk assessments with EDTA and NTA exposure by drinking water ingestion were carried out, Based on the results of analysis, chronic daily intakes of EDTA and NTA would be less than the value of acceptable daily intake or tolerable daily intake.
Park, Sung Pyo,Yoon, Doo Hyun,Tak, Young Jun,Lee, Heesoo,Kim, Hyun Jae The Royal Society of Chemistry 2015 Chemical communications Vol.51 No.44
<P>Here, we propose an effective method for improving the resistive switching characteristics of solution-processed gallium-doped zinc oxide (GaZnO<SUB><I>x</I></SUB>) resistive random access memory (RRAM) devices using hydrogen peroxide. Our results imply that solution processed GaZnO<SUB><I>x</I></SUB> RRAM devices could be one of the candidates for the development of low cost RRAM.</P> <P>Graphic Abstract</P><P>Here, we propose an effective method for improving the resistive switching characteristics of solution-processed gallium-doped zinc oxide (GaZnO<SUB><I>x</I></SUB>) resistive random access memory (RRAM) devices using hydrogen peroxide. <IMG SRC='http://pubs.rsc.org/services/images/RSCpubs.ePlatform.Service.FreeContent.ImageService.svc/ImageService/image/GA?id=c4cc10209f'> </P>
Lee, Soojin,Pyo, Heesoo,Chung, Bong Chul,Kim, Haidong,Lee, Jeongae Korean Chemical Society 2014 Bulletin of the Korean Chemical Society Vol.35 No.11
Alkoxyalcohols are used as solvents or preservatives in various consumer products such as wet wipes. The metabolites of alkoxyalcohols are known to be chronically toxic and carcinogenic to animals. Thus, an analytical method is needed to monitor alkoxyalcohols in wet wipes. The aim of this study was to develop a simultaneous analytical method for 14 alkoxyalcohols using headspace gas chromatography coupled with mass spectrometry to analyze the wet wipes. This method was developed by comparing with various headspace extraction parameters. The linear calibration curves were obtained for the method ($r^2$ > 0.995). The limit of detection of alkoxyalcohols ranged from 2 to $200ng\;mL^{-1}$. The precision of the determinative method was less than 18.20% coefficient of variation both intra and inter days. The accuracy of the method ranged from 82.86% to 119.83%. (2-Methoxymethylethoxy)propanol, 2-phenoxyethanol, and 1-phenoxy-2-propanol were mainly detected in wet wipes.