• Title/Summary/Keyword: Solid environmental samples

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Determination of N-nitrosamines in Water by Gas Chromatography Coupled with Electron Impact Ionization Tandem Mass Spectrometry (EI-GC/MS/MS를 이용한 니트로사민류의 수질분석)

  • Lee, Ki-Chang;Park, Jae-Hyung;Lee, Wontae
    • Journal of Korean Society of Environmental Engineers
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    • v.36 no.11
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    • pp.764-770
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    • 2014
  • This study assessed analysis of N-nitrosamines by separation, identification, and quantification using a gas chromatography (GC) mass spectrometer (MS) with electron impact (EI) mode. Samples were pretreated by a automated solid phase extraction (SPE) and a nitrogen concentration technique to detect low concentration ranges. The analysis results by EI-GC/MS (SIM) and EI-GC/MS/MS (MRM) on standard samples with no pretreatment exhibited similar results. On the other hand, the analysis of pretreated samples at low concentrations (i.e. ng/L levels) were not reliable with a EI-GC/MS due to the interferences from impurity peaks. The method detection limits of eight (8) N-nitrosamines by EI-GC/MS/MS analysis ranged from 0.76 to 2.09 ng/L, and the limits of quantification ranged from 2.41 to 6.65 ng/L. The precision and accuracy of the method were evaluated using spiked samples at concentrations of 10, 20 and 100 ng/L. The precision were 1.2~13.6%, and the accuracy were 80.4~121.8%. The $R^2$ of the calibration curves were greater than 0.999. The recovery rates for various environmental samples were evaluated with a surrogate material (NDPA-$d_{14}$) and ranged 86.2~122.3%. Thus, this method can be used to determine low (ng/L) levels of N-nitrosamines in water samples.

Evaluation of Environmental Toxicities for Priority Water Pollutants in a Small Watershed by Bioassays - Comparision between Lettuce Seed Germination Test and Microtox Bioassay - (생물학적 검정법을 이용한 소규모 수계내 수질 오염물질의 환경독성 평가 -상추씨 발아시험과 Microtox 시험 비교-)

  • 이지나;황인영
    • Environmental Analysis Health and Toxicology
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    • v.14 no.4
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    • pp.135-144
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    • 1999
  • Environmental toxicities of priority water pollutants were evaluated by two selected bioassays, Lettuce seed germination/elongation test and Microtox acute toxicity test. Toxic chemicals (heavy metals, polycyclic aromatic hydrocarbons, and phenolic compounds) inhibited the germination rate and root elongation of Lettuce seed, as well as the bioluminescence of Microtox bacteria. When test biota were exposed to target chemicals, the sensitivity of Lettuce bioassay was relatively lower than that of Microtox bioassay. However, Lettuce bioassay may be a good candidate for prescreening the environmental toxicities of priority water pollutants, since the testing method with Lettuce seed was relatively easier and more economic than with Microtox bacteria. Toxicity tests were conducted to compare the validity and sensitivity of both bioassays for sediment from a small stream passed through urban area as well as leachate from a municipal solid waste landfill. From experimental results, we found that Lettuce test and Microtox test are compensated each other as a battery of bioassay for evaluating the environmental toxicities of field samples obtained from a small stream contaminated by pollutants.

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Characteristics of Level of Perchlorate Pollution near Military Facility Areas (군사시설물 인근지역에서의 퍼클로레이트 오염수준 및 특성)

  • Choi, Jinsu;Um, Chul Yong;Chu, Kyoung Hoon;Ham, Seok Heon;Lee, Jong Hyeok;Yoo, Sung Soo;Ko, Kwang Baik
    • Journal of Korean Society on Water Environment
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    • v.28 no.3
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    • pp.460-466
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    • 2012
  • Perchlorate is used in a number of applications as an oxidizer in solid propellants, munitions and fireworks and is one of the endocrine disrupting chemicals, which interferes with iodide uptake into the thyroid gland. The purpose of this study was to investigate perchlorate occurrence and distribution with a results of analysis of 94 samples collected from military facilities in Korea from October 11 to October 23, 2011. Overall, among all of the 94 samples analyzed, perchlorate was detected in 6.4% of the total number of samples above $4{\mu}g/L$ (minimum reported limit) and the average concentration was $26.1{\mu}g/L$ and the maximum concentration was $107.7{\mu}g/L$ which was observed in surface water near manufacturing site of ammunition. By site classification, perchlorate was detected at one site in 4 manufacturing sites of ammunition and the maximum concentration was $107.7{\mu}g/L$ which was six times higher than that in guideline for perchlorate in Nakdong River and resulted from point source discharge. Perchlorate was detected at 3 sites in 78 measurements for shooting area and the maximum concentration was $12.4{\mu}g/L$ which was collected in dringking water and perchlorate in another sample was detected above MRL in shooting area was collected right away after shooting. These results showed that long term monitoring was needed considering weather conditions and shooting schedules.

Determination of antibiotics by SPE-LC-MS/MS in wastewater and risk assessment

  • Aydin, Senar;Aydin, Mehmet E.;Ulvi, Arzu;Kilic, Havva
    • Advances in environmental research
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    • v.7 no.3
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    • pp.201-212
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    • 2018
  • In this study, conditions of solid phase extraction (SPE) for determination of some antibiotics such as trimethoprim, oxytetracycline, erythromycin, clarithromycin, azythromycin, doxycycline, sulfamethazine, ciprofloxacin, chlortetracycline, sulfamethoxazole in wastewaters were optimized. After the optimum volume and pH of the sample were determined, the effect of the concentration of the compounds and matrix were investigated. The highest recovery rates for antibiotic compounds were determined between 82% and 105% in 200 mL sample volume and pH 2.5. Then, antibiotic compounds were investigated in influent and effluent samples taken from Konya Urban Wastewater Treatment Plant. The concentration of the antibiotics was detected range of 0.11-101 ng/L in influent waters and

The Assessment of Stabilization of Open-dumping Landfill Leachate - A Case Study of Noeun Landfill - (비위생매립지 침출수의 안정화 평가 - 노은매립지 사례연구 -)

  • Hong, Sang-Pyo
    • Journal of Environmental Impact Assessment
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    • v.13 no.3
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    • pp.115-124
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    • 2004
  • To utilize a closed municipal solid waste landfill site in environmentally secure conditions, it is necessary to verify the stabilization level of landfill leachate. To assess leachate stabilization of an open-dumping municipal solid waste landfill (Noeun Landfill) which is located at the upper drainage basin of Namhan River which flows into Lake Paldang utilized for Seoul Metropolitan water supplies, the surrounding characteristics of the landfill site was surveyed. After then, leachate, groundwater and soil samples from this landfill were chemically analyzed, and the analysis results were evaluated by "The Criteria of Landfill Waste Stabilization(CLWS)", "Discharge Criteria of Landfill Leachate", "The Criteria of Domestic Use in Groundwater Quality", and "Soil Contamination Criteria" promulgated by Korean Ministry of Environment. The closed open-dumping landfill was equipped with the final soil cover, 3 groundwater monitoring wells and poor landfill gas extraction devices for the post-closure management of the landfill. BOD/CODcr ratios in leachate were less than or slightly higher than 1/10. This results seemed to imply that the leachate stabilization level of this landfill based on the CLWS was almost completed. Qualities of groundwater sampled from monitoring wells located at outside of landfill were adequate for "The Criteria of Domestic Use in Groundwater Quality". Finally, concentrations of soil contaminants that were likely to be influenced by this landfill site were adequate to "Soil Contamination Criteria".

Environmental Pollutants Drained From Highway Pavement Road

  • Takemura, Shinsaku;Goto, Naoshige;Mitamura, Osamu
    • Korean Journal of Ecology and Environment
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    • v.38 no.spc
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    • pp.58-61
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    • 2005
  • Environmental polluting materials from road surface drainage are a significant nonpoint source influenced to the eutrophication of lake and ecosystems with a transport development in recent years. To elucidate the discharge characteristics, the changing patterns in concentrations of polluting materials such as suspended solid (SS), chemical oxygen demand (COD), nitrogenous and phosphorus nutrients in drainage waters, were investigated during rainfall. Load variation of COD concentration in drainage water samples was closely related to that of SS concentration. This indicates that SS contained a greater part of organic matter. A quite difference between the past pavement and the new well-drainage pavement system was observed in the concentrations of SS and COD in drainage waters. Appreciable concentrations of nitrite and nitrate were determined in drainage waters. The present results indicate that the drainage water from road surfaces is a significant nonpoint source, and that the well-drainage pavement system introduced to skid prevention has an effect on the decreases of pollutants.

The Optimal Analytical Method for the Determination of PCE and TCE by GC/FID with SPME technieque (고체상미량분석법(SPME)을 이용한 GC/FID에서 PCE 및 TCE 최적 분석법)

  • Ahn Sang-Woo;Lee Si-Jin;Chang Soon-Woong
    • Journal of Environmental Science International
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    • v.13 no.10
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    • pp.903-909
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    • 2004
  • A new method based on solid phase microextraction(SPME), coupled with GC/FID, has been developed for the determination of PCE and TCE in water samples. The experimental parameters affecting the SPME process (i.e, kinds of fibers, extraction time, desorption time, extraction temperature, volume ratio of sample to headspace, salt addition, and magnetic stirring) were optimized. The coefficients of determination ($R^2$) for PCE and TCE were 0.9951 and 0.9831, respectively when analytes concentration ranges from 10 to 300$\mu$g/L. The relative standard deviations were 3.4 and $2.1\%$ for concentration of 10$\mu$g/L(n=5), respectively. The detection limits of PCE and TCE were 0.5 and l.3$\mu$g/L, respectively.

Method Development and Cross Validation of Analysis of Hydroxylated Polycyclic Aromatic Hydrocarbons (OH-PAHs) in Human Urine (소변 중 다환방향족탄화수소 대사체의 분석법 확립 및 교차분석)

  • Park, Na-Youn;Jeon, Jung-Dae;Koo, Hyeryeong;Kim, Jung Hoan;Lee, Eun-Hee;Lee, Kyungmu;Mun, Cheoljin;Kho, Younglim
    • Journal of Environmental Health Sciences
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    • v.41 no.5
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    • pp.358-367
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    • 2015
  • Objectives: This study was performed to evaluate the analytical method for PAH metabolites in human urine using enzyme hydrolysis and solid-phase extraction coupled with LC-(ESI)-MS/MS technique. Methods: We employed HPLC tandem mass spectrometry techniques with appropriate pre-treatment for analysis of 16 OH-PAHs in human urine. Samples were hydrolysis by ${\beta}$-flucuronidase/Aryl sulfatase, and target compounds were extracted by solid-phase extraction with a strata-x cartridge. Cross-validation was performed between Eulji University and Green Cross laboratories with 200 human urine samples. Results: The accuracies were between 90.3% and 118.8%, and precisions (relative standard deviations) were lower than 10%. The linearity obtained was satisfying for the 16 OH-PAH compounds, with a coefficient of determination ($r^2$) higher than 0.99. The results of cross-validation at the two organizations were compared by ICC (interclass correlation coefficient) values. The cross-validation results were excellent or good for all compounds. Conclusion: An analytical method was validated for low nanogram levels of 16 OH-PAHs in human urine. Also, satisfying results were obtained for method validation such as accuracy, precision and ICC of cross-validation.

Synthesis of CoTiOx and Its Catalytic Activity in Continuous Wet TCE Oxidation (CoTiOx의 합성 및 연속 습식 TCE 산화반응에서의 촉매활성)

  • Kim, Moon-Hyeon
    • Journal of Environmental Science International
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    • v.16 no.12
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    • pp.1431-1437
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    • 2007
  • Cobalt titanates($CoTiO_x$), such as $CoTiO_3$ and $Co_2TiO_4$, have been synthesized via a solid-state reaction and characterized using X-ray diffraction(XRD) and X-ray photoelectron spectroscopic(XPS) measurement techniques, prior to being used for continuous wet trichloroethylene(TCE) oxidation at $36^{\circ}C$, to support our earlier chemical structure model for Co species in 5 wt% $CoO_x/TiO_2$(fresh) and(spent) catalysts. Each XRD pattern for the synthesized $CoTiO_3$ and $Co_2TiO_4$ was very close to those obtained from the respective standard XRD data files. The two $CoTiO_x$ samples gave Co 2p XPS spectra consisting of very strong main peaks for Co $2p_{3/2}$ and $2p_{1/2}$ with corresponding satellite structures at higher binding energies. The Co $2p_{3/2}$ main structure appeared at 781.3 eV for the $CoTiO_3$, and it was indicated at 781.1 eV with the $Co_2TiO_4$. Not only could these binding energy values be very similar to that exhibited for the 5 wt% $CoO_x/TiO_2$(fresh), but the spin-orbit splitting(${\Delta}E$) had also no noticeable difference between the cobalt titanates and a sample of the fresh catalyst. Neither of all the $CoTiO_x$ samples were active for the wet TCE oxidation, as expected, but a sample of pure $Co_3O_4$ had a good activity for this reaction. The earlier proposed model for the surface $CoO_x$ species existing with the fresh and spent catalysts is very consistent with the XPS characterization and activity measurements for the cobalt titanates.

Determination of Antibiotic Residues: II. Extraction and Clean-up Methods for Liquid Samples_A Review (시료 중 잔류 항생제 분석 방법: II. 액상 시료 전처리 방법)

  • Kim, Chansik;Ryu, Hong-Duck;Chung, Eu Gene;Kim, Yongseok;Rhew, Doug Hee
    • Journal of Korean Society on Water Environment
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    • v.32 no.6
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    • pp.628-648
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    • 2016
  • Increased attention has been paid to the presence of veterinary antibiotics in various environmental matrices due to their toxicological behavior in the ecosystem and development of antibiotic-resistant strains of pathogenic bacteria. In the this review, 37 target antimicrobials were selected based on annual sales of antibiotics for livestock in South Korea 2014. Also, extraction and clean-up methods for the determination of the antibiotic residues in liquid samples including water, milk, and honey were comprehensively reviewed in the literature. Solid-phase extraction (SPE) was commonly used as a pre-treatment method for the samples. Most of the analytes were extracted in acidic conditions (2.5~4.0) except for aminoglycosides, which were extracted in neutral conditions (7.0~8.0). ${\beta}-Lactams$ showed the highest recoveries in neutral pH due to their degradation characteristics in acidic media. Starta-X, Oasis HLB, and Oasis MCX were frequently applied as an SPE cartridge and Oasis HLB showed the highest recoveries for the majority of antibiotic classes. The homogenized honey and milk were extracted by mixing with acids for deproteinization. Solids and other interfering substances in the extract were eliminated by centrifugation followed by membrane filtration or SPE before injection into HPLC.