• Environmental Analysis Health and Toxicology
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• 제15권3호
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• pp.107-113
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• 2000

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 $CH_3$I/Acetone -K$_2$CO$_3$와 황산/메탄올로 각각 methylation실험을 행하였고, 산성조건에서 triflouroethanol (TFAA/TEE)과 반응시켜 각각의 검출검도를 비교하였다. 그 결과 TPAA/TEE를 사용하여 반응시킨 결과감도가 좋은 것으로 나타났다.

• 분석과학
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• 제8권4호
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• pp.739-744
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• 1995

The two main methods to prepare water samples for analyzing volatile organic compounds(VOC's) were investigated. One is the purge and trap(PT) method and another is the head space(HS) sampling method. Both methods were effective to transfer the low boiling point components from the water sample onto the capillary column. The cryo-focusing at the top of the main capillary column was an effective way to obtain the sharpness of the chromatographic peaks but could be avoided when a semi-wide bore column was used. The recovery from the same amount of the sample was better in PT than in HS but a larger sample volume in HS method could compensate the lower efficiency. Therefore PT is suitable to the analysis of drinking water where the very low concentration must be determined. HS is suitable to waste water analysis because of the easiness of the operation. The repeatability was good and similar in both methods. For the contamination of the former sample, both methods were tough and could be used without any problems. The matrix effect which could change the equilibrium parameters in HS method was find negligible in many components. The actual samples such as tap water and river water were analyzed with both methods concerning 16 components regulated in Korea.

• Environmental Analysis Health and Toxicology
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• 제18권3호
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• pp.219-224
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• 2003

1,4-Dioxane is used as a solvent for lacquers, paints, varnish removers, dye baths and printing compositions. And it is also used for detergent preparations, cosmetics, deodorants and fumigants. A method is described for the determination of 1,4-dioxane in water samples by GC/MS. The extraction recoveries were studied for some solvents and solvent volume ratio were investigated using r-butyl methyl ether (MTBE). Optimum condition was obtained by the liquid-liquid extraction using the 10 mL of MTBE for 10 mL of water. Method detection limit of 1,4-dioxane in the 20 mL of water samples was 0.05 ng/mL. It could be determined in the range of 0.24∼240 ng/mL in treated water, and in the range of 0.69∼81.9 ng/mL in raw water, respectively. Risk assessments with 1,4-dioxane exposure by drinking water ingestion were carried out. Based on the results of analysis, chronic daily intake of 1,4-dioxane was 2.22${\times}$10$\^$-4/ mg/kg/day and excess cancer risk was calcu-lated to be 2.44${\times}$10$\^$-6/.

• 상하수도학회지
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• 제32권5호
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• pp.389-398
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• 2018

A nationwide survey of 8 N-nitrosamines in finished water samples from drinking water treatment plants (DWTPs) in Korea was conducted. The samples were pre-treated by solid-phase extraction (SPE) and analyzed using a gas chromatography coupled with tandem mass spectrometry (GC-MS/MS). According to the study results, four N-nitrosamines (NDMA, NDEA, NMOR, NDBA) were detected for three consecutive years, NMEA and NPYR were only found in samples collected in 2013. Two of these N-nitrosamines, N-nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA), have received attention and were the most commonly detected. The concentration of NDMA and NDEA in this study ranged from $0.002{\mu}g/L$ to $0.013{\mu}g/L$ and in $0.001{\mu}g/L$ to $0.008{\mu}g/L$, respectively. In comparison to studies performed in EPA(UCMR2), the concentrations of NDMA (from $0.002{\mu}g/L$ to $0.630{\mu}g/L$) and NDEA (from $0.005{\mu}g/L$ to $0.100{\mu}g/L$) observed in the this study were low.

• 상하수도학회지
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• 제18권5호
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• pp.638-648
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• 2004

In many drinking water treatment plants, chlorination process is one of the main techniques used for the disinfection of water. This disinfecting treatment leads to the formation of haloacetic acid (HAAs). In this study, headspace solid-phase microextraction (HS-SPME) was studied as a possible alternative to liquid-liquid extraction for the analysis of HAAs in drinking water. The method involves direct derivatization of the acids to their methyl esters without methyl tert-butyl ether (MTBE) extraction, followed by HS-SPME with a $2cm-50/30{\mu}m$ divinylbenzene/carboxen/polydimethylsiloxane fiber. The effects of experimental parameters such as selection of SPME fiber, the volume of sulphuric acid and methanol, derivatization temperature and time, the addition of salts, extraction temperature and time, and desorption time on the analysis were investigated. Analytical parameters such as linearity, repeatability and limit of detection were also evaluated. The $2cm-50/30{\mu}m$-divinylbenzene/carboxen/polydimethylsiloxane fiber, sulphuric acid of 1ml, methanol of 3ml, derivatization temperature of $50^{\circ}C$ derivatization time of 2hrs, sodium chloride salt of 10g, extraction time of 30 minutes, extraction temperature of $20^{\circ}C$ and desorption time of 1 minute at $260^{\circ}C$ were selected as the optimal experimental conditions for the analysis of HAAs. The linearities ($r^2$), relative standard deviations (%RSD) and limits of detection (LOD) for HAAs were 0.9978~0.9991, 1.1~9.8% and $0.05{\sim}0.2{\mu}g/l$, respectively.

• 한국물환경학회지
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• 제26권3호
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• pp.446-453
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• 2010

This study was investigated nine nitrosamines in small tributary rivers, sewage treatment plants (STPs) and drinking water treatment plants. They are N-nitrosodimethylamine (NDMA), N-nitrosomethylethylamine (NMEA), N-nitrosodiethylamine (NDEA), N-nitrosopyrrolidine (NPYR), N-nitrosodi-n-propylamine (NDPA), N-nitrosomorpholine (NMOR), N-nitrosopiperidine (NPIP), N-nitrosodi-n-butylamine (NDBA) and N-nitrosodiphenylamine (NDPHA). The nine nitrosamines were analyzed by gas chromatography mass spectrometry (GC/MS) using solid phase extraction (SPE) with a coconut charcoal cartridge. Among the nine nitrosamines, NDMA, NMEA, NDEA, NDPA NDBA and NDPHA were detected in small tributary rivers and sewage tretment plants. In small tributary rivers, NDMA, NMEA, NDEA, NDPA, NDBA and NDPHA were obtained as ND~16.4 ng/L, ND~17.7 ng/L, ND~102.4 ng/L, ND~455.4 ng/L, ND~330.1 ng/L and ND~161.0 ng/L, respectively. Also NDMA, NMEA, NDEA, NDPA and NDBA were investigated ND~821.4 ng/L, 22.5~55.4 ng/L, 53.2~588.5 ng/L, ND~56.6 ng/L and ND~527.9 ng/L in STPs, respectively. In drinking water treatment plants, NMEA and NDEA concentration were increased to as high as 38.8 ng/L after ozonation process. However nitrosamines were decreased subsequent biological activated carbon (BAC) treatment process. It was supposed that nitrosamines were formed by $O_3$ oxidation and were removed by biodegradation of BAC.

• 분석과학
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• 제28권1호
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• pp.58-64
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• 2015

이 연구에서는 농촌지역 마을상수 중에 함유된 trihalomethanes (THMs)의 농도 분포 및 발생 특성을 파악하였다. 농촌지역의 마을상수 시료는 2010년과 2011년 여름에 강원도 춘천시의 40가정에서 두 차례에 걸쳐 채취하였고, 도시상수 시료는 2011년의 같은 기간에 비교 목적으로 20곳의 수도꼭지에서 채취하였다. 현장에서 수온, pH 및 잔류염소(총 및 유리) 농도를 측정하였고, 물 시료는 실험실에서 용존 유기탄소(DOC)와 THMs 농도에 대해 분석하였다. 마을상수 중 DOC의 평균 농도는 원수로 사용된 지하수와 지표수 간에 거의 차이를 보이지 않았다(1.81 vs. 1.91 mg/L). 그러나 마을상수의 지하수에서($9.77{\mu}g/L$)의 총 THMs(TTHMs)의 평균 농도는 지표수보다($2.85{\mu}g/L$) 훨씬 더 높았고, 도시상수 중 TTHMs의 평균 농도($10.8{\mu}g/L$)와 유사하였다. 도시상수와는 다르게, 마을상수(특히 지하수)는 dibromochloromethane (DBCM)과 같은 더 많이 브롬화된 THMs을 함유하였는데, 이는 마을상수의 원수 중에 bromide ion(Br-)이 비교적 높은 수준으로 존재함을 암시하였다. 이 연구를 통해 마을상수는 도시상수와는 다른 THMs 생성 특성을 나타내는 것을 알 수 있었는데, 이것은 아마도 원수의 수질 특성의 차이에서 비롯되는 것으로 생각된다.

• 분석과학
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• 제31권2호
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• pp.96-105
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• 2018

이 연구는 발암 의심 물질인 nitrosamine 화합물의 유기 전구물질인 8종의 이차 지방족 아민 화합물의 분석 방법을 개선한 후, 지표수 및 수돗물에서의 농도 분포를 측정하고자 실시하였다. 여과한 물 시료(200 mL)에 10 M NaOH (8 mL)와benzenesulfonyl chloride (2 mL)를 첨가하고 $80^{\circ}C$에서 30분 동안 교반한 후, 10 M NaOH (10 mL)를 첨가하여 30분 동안 교반하였다. 실온으로 식힌 물 시료에 35 % HCl를 첨가하여 pH를 5.5-6.0로 조절한 후, dichloromethane (50 mL)을 가하여 진탕기로 30분 동안 추출하였고, 이 추출 과정은 한 번 더 반복하였다. 추출액(100 mL)을 0.05 M $NaHCO_3$ 수용액(15 mL)으로 씻어준 후 $Na_2SO_4$(4 g)로 건조하였다. 여과액은 회전증발기와 질소가스를 사용하여 0.1 mL까지 농축한 후, GC-MS로 이차 지방족 아민에 대해 분석하였다. 검량선의 직선성은 결정계수($r^2$)로 0.9969-0.9996이었다. 방법검출한계는 $0.01-0.20{\mu}g/L$이었고, 반복성 및 재현성은 RSD로 나타낼 때 모두 10 % 이내이었다(6.6-9.4 %). 퍼센트 오차로 나타낸 정확도는 $0.6{\mu}g/L$에 대해 2.4-6.1 %이었다. 확립된 분석 방법을 5개의 지표수와 82 개의 수돗물에 대해 분석하였다. Dimethylamine은 모든 물 시료에서 검출되었으며, 농도는 평균 $0.79{\mu}g/L$이었고 범위는 $0.20-2.54{\mu}g/L$이었다. 따라서 본 연구에서는 지표수 및 수돗물 중 이차 지방족 아민에 대한 분석 방법을 개선하였으며, 지역 및 계절별 농도 분포를 파악하였다.

• 대한환경공학회지
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• 제37권5호
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• pp.262-268
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• 2015

본 연구는 on-line micro extraction by packed sorbent (on-line MEPS)와 시료다량주입장치인 programmed temperature vaporizer (PTV) injector를 결합한 가스크로마토그래피 질량분석 시스템을 이용하여 유기인계 농약인 methyldemetone-S, diazinon, fenitrothion, parathion, phentoate, O-ethyl O-(4-nitrophenyl) phenylphosphonothioate (EPN)과 카바이트계인 carbaryl에 대한 동시 수질분석법을 확립하였다. MEPS 내 sorbent는 polystyrene divinylbenzene (PDVB) 재질을 이용하였다. 시료전처리시 추출용매 종류, pH, 추출용매량 및 시료주입왕복횟수가 분석에 미치는 영향과 정도보증(QA/QC), 그리고 환경시료에 대한 각 물질의 회수율을 평가하였다. 추출용매는 acetone과 dichloromethane을 80 : 20 (v/v)으로 혼합하여 사용하였고, 내부표준물질과 황산을 첨가한 시료 1 mL를 대상으로 추출용매량 $30{\mu}L$, 시료주입왕복횟수를 7회로 추출하여 분석조건을 최적화하였다. pH가 낮을수록 Diazinon의 분석감응도는 감소한 반면 carbaryl의 분석감응도는 증가하였다. 정도보증결과 항목별 방법검출한계 및 정량한계는 각각 $0.02{\sim}0.18{\mu}g/L$, $0.08{\sim}0.59{\mu}g/L$로 낮았으며, 농도범위 $0.5{\sim}5.0{\mu}g/L$ 수준에서 정밀도와 정확도 범위는 각각 1.5~11.5%, 83.3~129.8%로 나타났다. 환경시료 중 carbaryl을 제외한 모든 항목의 회수율은 75.7~129.3%로 적합하였다. Carbaryl에 대한 회수율은 수돗물, 지하수, 하천수 분석에서 적합한 범위를 나타냈으나, 하수처리방류수에서는 200% 이상으로 만족하지 못하였다.

• 한국물환경학회지
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• 제16권4호
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• pp.469-477
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• 2000

Bisphenol-A (BPA), a known endocrine disruptor, is a main building block of epoxy resin which is widely used as a coating agent in residential water storage tanks. Therefore, BPA leaching from the epoxy resin may have adverse effects on human health. The possibility of BPA leaching from three epoxy resins were tested with a modified KS D 8502 method at 20, 50, 75 and $100^{\circ}C$ in deionized water and the specified test water, respectively. BPA leached to the test water was identified using GC-MS and quantified with GC-FID after a sequential extraction and concentration. The results showed that BPA leaching has occurred in all three samples tested. The quantify of BPA leaching from unit area of epoxy resin coating was in the range of $10.677{\sim}273.120{\mu}g/m^2$ for sample A, 29.737~1734.045 for sample B and 52.857~548.778 for sample C depending on the test temperature, respectively. In general, the amount of BPA leaching increased as the water temperature increases. This result implies a higher risk of BPA leaching to drinking water during a hot summer season. In addition, microbial growth, measured by colony forming units, in epoxy coated water tanks was higher than that in a stainless steel tank suggesting that compounds leaching from epoxy resin may support the growth of microorganisms in a residential water holding tank.