• Title/Summary/Keyword: Solid environmental samples

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Monitoring of Veterinary Antibiotics in Agricultural Soils using Liquid Chromatography Coupled with Tandem Mass Spectrometry (LC-MS/MS를 이용한 농경지 토양 중 항생제 모니터링)

  • Lee, Young-Jun;Choi, Jeong-Heui;Chung, Hyung Suk;Lee, Han Sol;Park, Byung-Jun;Kim, Jang-Eok;Shim, Jae-Han
    • Korean Journal of Environmental Agriculture
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    • v.35 no.3
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    • pp.166-174
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    • 2016
  • BACKGROUND: The current study developed a monitoring method of 6 veterinary antibiotics (amoxicillin, ampicillin, enrofloxacin, tetracycline, chlortetracycline, oxytetracycline) in agricultural soils using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive electrospray ionization mode.METHODS AND RESULTS: Sample preparation was carried out using acidic acetonitrile and citrate salts followed by purification with dispersive solid phase extraction (d-SPE). Separation on Eclipse Plus C18 column was conducted in gradient of the mobile phase, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations expressed as the coefficient of determination was good with R2≥0.9900. The limit of quantifications (LOQs) ranged from 0.5 to 10 μg/kg for all analytes. Analysis of 51 agricultural soil samples taken in the Republic of Korea revealed concentrations less than 1.9 μg/kg for enrofloxacin, 75.5 μg/kg for chlortetracycline.CONCLUSION: The method was successfully applied to monitor 6 veterinary antibiotics from 51 field incurred agricultural soil samples in 17 provincial areas throughout the Republic of Korea. The developed method was simple, easy, and versatile and can be used for monitoring various veterinary antibiotics in soil.

Physicochemical Heterogeneity of the Supply Water Quality depending on Seasonal Changes in the Taejon Area, Korea (대전지역 상수도 물의 계절변화에 따른 물리화학적 불균질)

  • 이현구;이찬희;서호택
    • Economic and Environmental Geology
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    • v.33 no.6
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    • pp.505-517
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    • 2000
  • This study was undertaken to provide a drinking water quality on the basis of physicochemical properties. In this study, the 25 samples of supply waters of the Taejon area were sampled twice (February and August in 1999). Hydrochemistry of the supply water belongs to the $Ca^{2+}$-${HCO_3}^{-1}$ type, whereas the supply water was characterized by the relatively significant enrichment of ${Ca}^{2+}$, ${Na}^{2+}$, ${K}^{2+}$, ${Cl}^{2+}$ ions and heavy metals compared to the original water from the Daecheong lake. Generally, the supply water has a mean values for $10.7^{\circ}C$ of temperature, 6.86 of pH, -12 mV of Eh, 88 ${\mu}S$/cm of EC and 70.379 mg/l of TDS in February, whereas the waters of the same sites in August are a slightly high temperature ($26.1^{\circ}C$), TDS (78.069 mg/l) and extremely high EC (442 ${\mu}S$/cm) value. These values are similar with physicochemical properties of the original lake water depending on the seasonal differences. Results of speciation calculation indicate that potentially toxic ions might exist mainly in the forms of free metal (${Cu}^{2+}$ or ${Zn}^{2+}$) and a small amount of ${CO_3}^{2-}$and ${OH}^{-}$in the supply water. The water seemed to be in equilibrium with kaolinite field of the normal stability diagrams for the natural water. Based on enrichment parameter of the supply water normalized by original lake water composition, the average value of those parameter can be calculated with nearly 1.00, but the those values for Cu+Zn possible source of decrepit pipe lines are 126.75 in February and 115.63 in August samples. The parameter values varied with sampling sites, however, do not exceed by chemistry of drinking water standard. Solid compounds remained on the membrane filter papers after filtration are adhered to pale yellow or yellowish brown colored dissolved solids and precipitates, which are coated by 0.02 to 0.35 mm thick per 500 ml with colloidal particles of about 1 to 2${\mu}m$ size. The particles are mainly Fe-Cu-Zn compounds and partly detected to Mn and Pb.

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Potential Element Retention by Weathered Pulverised Fuel Ash : I. Batch Leaching Experiments (풍화 석탄연소 고형폐기물(Pulverised Fuel Ash)의 중금속 제거가능성 : I. 뱃치 용출실험)

  • Lee, Sanghoon
    • Economic and Environmental Geology
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    • v.28 no.3
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    • pp.251-257
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    • 1995
  • Three PEA (Pulverised Fuel Ash) samples, which were fresh, 17 and some 40 years weathered, were collected from two major British power plants. Batch leaching tests with these samples using distilled water and simulated industrial leachate showed higher amounts of element liberation from fresh ash, including Ca, Na, K, S (as $SO^{2-}_4$, $Cr_{total}$, Cu, Li Ni, Mo and CI and this seems to indicate their surface association and easier dissolution when contact with water. On the contrary Mg, Al, Ba, Si, V, As and Se do not show such readily leachable concentrations and these elements might be more associated with glass fraction in PFA particle rather than surface. Although element concentrations in the weathered ash are much lower than those in the initial leachate from the fresh ash, elements are still detected as resonable concentrations, with rather constant levels and this seems to demonstrate the element release from unstable glass phase of PFA particle. Fe, Ca, $Cr_{total}$, Cu, Ni, Zn and Hg were removed from the synthetic leachate by PFA and this is also confirmed by gain in solid PFA. The order of element retention is Meaford weathered ash > Drax weathered ash > Drax fresh ash in decreasing order and this conforms with the degree of weathering. Namely, the more wethered, the more wethered, the more effective in metal retention from the synthetic leachate.

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Concrete Deterioration Near Coastal Area and Characteristics of Associated Secondary Mineral Formation (해안지역 콘크리트의 성능저하 현상과 이에 수반되는 이차광물의 형성 특징)

  • 이효민;황진연;진치섭
    • Economic and Environmental Geology
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    • v.36 no.5
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    • pp.365-374
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    • 2003
  • Various deleterious chemicals can be introduced to existing concrete structures from various external sources. The deterioration of concrete by seawater attack is involved in complex processes due to various elements contained in seawater. In the present study, attention was paid to the formation of secondary minerals and characteristics of mineralogical and micro-structural changes involved in concrete deterioration caused by the influence of major seawater composition. The characteristics of deterioration occurred in existing concrete structures was carefully observed and samples were collected at many locations of coastal areas in Busan-Kyungnam. The petrographic, XRD, SEM/EDAX analyses were conducted to determine chemical, mineralogical and micro-structural changes in the aggregate and cement paste of samples. The experimental concrete deteriorations were performed using various chloride solutions (NaCl, CaCl, $MgCl_2$ and $Na_2SO_4$ solution. The experimental results were compared with the observation results in order to determine the effect of major elements in seawater on the deterioration. The alkalies in seawater appear to accelerate alkali-silica reaction (ASR). The gel formed by ASR is alkali-calcium-silica gel which known to cause severe expansion and cracking in concrete. Carbonation causes the formation of abundant less-cementitious calcite and weaken the cement paste. Progressive carbonation significantly affects on the composition and stability of some secondary minerals. Abundant gypsum generally occurs in concretes subjected to significant carbonation, but thaumasite ({$Ca_6/[Si(OH)_6]_2{\cdot}24H_2O$}${\cdot}[(SO_4)_2]{\cdot}[(CO_3))2]$) occurs as ettringite-thaumasite solid solution in concretes subjected to less significant carbonation. Experimentally, ettringite can be transformed to trichloroaluminate or decomposed by chloride ingress under controlled pH conditions. Mg ions in seawater cause cement paste deterioration by forming non-cementitious brucite and magnesium silicate hydrate (MSH).

Development of Matrix for the Immobilization of High Level Radioactive Waste : Study on the Synthesis of Ce-pyrochlore (고준위 핵페기물의 고정화를 위한 메트릭스 개발 : Ce파이로클로어 합성 연구)

  • ;;;Yudintsev, S. V²
    • Economic and Environmental Geology
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    • v.35 no.2
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    • pp.97-102
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    • 2002
  • Ce-pyrochlore (CaCe $Ti_2 $O_7)was synthesized to study its properties and phase relations in CaO-Ce $O_2$-Ti $O_2$ system because Ce-pyrochlore was known as a promising material for the immobilization of radioactive actinide. The samples were prepared from the high purity starling materials under the pressure of 200~400 kg/$\textrm{cm}^2$ at room temperature, and annealed at 1000~ 150$0^{\circ}C$. The Synthesized samples were analysed and indentified with XRD and SEM/EDS methods. The optimal formation condition of Ce-pyrochlore was at 130$0^{\circ}C$ under $O_2$ atmosphere and the chemical composition of it wasCa$Ca_{1-x}Ti_{2-y}O_{7-x-2y}$(x=0.03-0.05, y=0.02~0.04) At temperature between 130$0^{\circ}C$ 140$0^{\circ}C$, Ce-pyrochlore underwent rapidly the incongruent decomposition to perovskite. Ce-perovskite, a partial solid solution between perovskite and loparite (C $e_{0.66}$Ti $O_3$), was observed as a major phase above 140$0^{\circ}C$.>.

Development and Validation of a Simultaneous Analytical Method for the Detection of Mefentrifluconazole and Triticonazole Fungicide in Agricultural Crops (농산물 중 메펜트리플루코나졸 및 트리티코나졸 살균제의 동시 분석법 개발 및 검증)

  • Park, Ji-Su;Lee, Han Sol;Lee, Su Jung;Shin, Hye-Sun;Shim, Jae-Han;Yun, Sang Soon;Jung, Yong-hyun;Oh, Jae-Ho
    • Korean Journal of Environmental Agriculture
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    • v.39 no.2
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    • pp.130-137
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    • 2020
  • BACKGROUND: Mefentrifluconazole and triticonazole are the triazole fungicides. The maximum residue levels for agricultural products need to be set up. Therefore, development of the official analytical method for determination of mefentrifluconazole and triticonazole residues from agricultural crops was necessary due to safety management, and then a simultaneous analytical method was developed for the determination of mefentrifluconazole and triticonazole in agricultural crops. METHODS AND RESULTS: Samples were extracted using acetonitrile and purified using dispersive solid phase extraction, and then detected with liquid chromatograph-tandem mass spectrometry (LC-MS/MS). Matrix-matched calibration curves (0.0025-0.25 ㎍/mL) were linear into a sample extract with r2>0.99. For validation, the recovery test was carried out at three fortification levels (LOQ, 10 LOQ and 50 LOQ) from agricultural samples. The results for mefentrifluconazole and triticonazole ranged between 92.3 to 115.3% and 91.4 to 108.5%, respectively and RSD (relative standard deviation) values were also below 6.0%. Furthermore, inter-laboratory was conducted to validate the method. CONCLUSION: All values were corresponded with the criteria ranges requested by both the CODEX (CAC/GL 40-1993, 2003) and MFDS guidelines (2016). Therefore, the proposed method can be used as an official analytical method for determination of mefentrifluconazole and triticonazole (triazole fungicides) in the Republic of Korea.

Full validation of high-throughput bioanalytical method for the new drug in plasma by LC-MS/MS and its applicability to toxicokinetic analysis

  • Han, Sang-Beom
    • Proceedings of the Korean Society of Toxicology Conference
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    • 2006.11a
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    • pp.65-74
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    • 2006
  • Modem drug discovery requires rapid pharmacokinetic evaluation of chemically diverse compounds for early candidate selection. This demands the development of analytical methods that offer high-throughput of samples. Naturally, liquid chromatography / tandem mass spectrometry (LC-MS/MS) is choice of the analytical method because of its superior sensitivity and selectivity. As a result of the short analysis time(typically 3-5min) by LC-MS/MS, sample preparation has become the rate- determining step in the whole analytical cycle. Consequently tremendous efforts are being made to speed up and automate this step. In a typical automated 96-well SPE(solid-phase extraction) procedure, plasma samples are transferred to the 96-well SPE plate, internal standard and aqueous buffer solutions are added and then vacuum is applied using the robotic liquid handling system. It takes only 20-90 min to process 96 samples by automated SPE and the analyst is physically occupied for only approximately 10 min. Recently, the ultra-high flow rate liquid chromatography (turbulent-flow chromatography)has sparked a huge interest for rapid and direct quantitation of drugs in plasma. There is no sample preparation except for sample aliquotting, internal standard addition and centrifugation. This type of analysis is achieved by using a small diameter column with a large particle size(30-5O ${\mu}$m) and a high flow rate, typically between 3-5 ml/min. Silica-based monolithic HPLC columns contain a novel chromatographic support in which the traditional particulate packing has been replaced with a single, continuous network (monolith) of pcrous silica. The main advantage of such a network is decreased backpressure due to macropores (2 ${\mu}$m) throughout the network. This allows high flow rates, and hence fast analyses that are unattainable with traditional particulate columns. The reduction of particle diameter in HPLC results in increased column efficiency. use of small particles (<2 urn), however, requires p.essu.es beyond the traditional 6,000 psi of conventional pumping devices. Instrumental development in recent years has resulted in pumping devices capable of handling the requirements of columns packed with small particles. The staggered parallel HPLC system consists of four fully independent binary HPLC pumps, a modified auto sampler, and a series of switching and selector valves all controlled by a single computer program. The system improves sample throughput without sacrificing chromatographic separation or data quality. Sample throughput can be increased nearly four-fold without requiring significant changes in current analytical procedures. The process of Bioanalytical Method Validation is required by the FDA to assess and verify the performance of a chronlatographic method prior to its application in sample analysis. The validation should address the selectivity, linearity, accuracy, precision and stability of the method. This presentation will provide all overview of the work required to accomplish a full validation and show how a chromatographic method is suitable for toxirokinetic sample analysis. A liquid chromatography/tandem mass spectrometry (LC-MS/MS) method developed to quantitate drug levels in dog plasma will be used as an example of tile process.

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Development of Porous Support with Mine Waste Materials (광산 폐기물을 활용한 다공성 담체 개발)

  • 정문영;정명채;최연왕
    • Economic and Environmental Geology
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    • v.37 no.1
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    • pp.143-151
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    • 2004
  • This study focused on examining the possibility of recycling mine solid waste as environmental materials, especially for porous media. Basic properties including mineralogical compositions, chemical compositions, and particle size distribution of the tailings from the Sangdong W mine were checked. The mineralogical and chemical compositions of the tailings samples were not much different in depth. According to Korean Standard Leaching Test for Wastes(KSLT), concentrations of heavy metals leached from the tailings were below the standard values. As a result of particle size analysis, the median diameter (d$_{50}$) of the tailings was in the range of 10 to 30 ${\mu}{\textrm}{m}$. The stable tailings slurry made up of 3 ${\mu}{\textrm}{m}$ in d$_{50}$ was prepared using Attrition Mill. The milling condition was 40 vol% in slurry concentration, 700 rpm in stirring speed, and 1 hour in milling time. PEI was added as dispersing agent. Concentrated slurry was extended to 3 times by foaming method. In the case of 3 times foamed slurry, the total and open porosity of ceramic supports sintered at 1,075$^{\circ}C$ for 90 minutes was about 80% and 72%, respectively. Pore size was in the range of 30∼350${\mu}{\textrm}{m}$. Therefore, the tailings could be recycled starting material for environmental materials such as macroporous ceramic support.

SRF Conversion Potential of Biomass and Mixed Plastic Waste Generated in D City (D시 내에서 발생하는 바이오매스 및 폐플라스틱 혼합 폐기물의 SRF 전환 포텐셜 분석)

  • Yang, Han-Sol;Kim, Ki-Kwang;Lim, Chae-Wook;Hyun, Jae-Hyuk
    • Journal of the Korea Organic Resources Recycling Association
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    • v.26 no.3
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    • pp.55-61
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    • 2018
  • This study evaluated if the selected samples meets the Solid Refuse Fuel quality criteria in Korea. Biomass and plastic wastes generated in D City were mixed in diverse ratio. When the biomass content was about 40%, the moisture content was close to the SRF criteria and was measured to be 9.8%. The ash contents were analyzed up to 4.19%, and the lower calorific values based on Steuer, Dulong Equation and Bomb Calorimeter were at least 4,851, 4,181 and 3,847 kcal/kg, respectively. As a result of the elemental analysis, sulfur and chloride content were measured up to 0.05%. Those values satisfied the SRF criteria. Also, heavy metals(Hg, Cd, Pb, As) were analyzed to be below the SRF criteria. This makes it possible to use efficiently the wood byproducts abandoned in the woods, and the physical properties of wood being weak to moisture can be supplemented with plastics. Consequently, if plastic and biomass were well mixed and made into SRF, it would overcome the problem of shortening the life span of incineration facilities due to the high temperature of plastic wastes in the incinerator.

Size Distribution and Physicochemical Characteristics of MSW for Design of Its Mechanical Biological Treatment Process (폐기물전처리(MBT)시설 설계를 위한 생활폐기물의 입도분포 및 물리화학적 특성에 관한 연구)

  • Park, Jin-Kyu;Song, Sang-Hoon;Jeong, Sae-Rom;Jung, Min-Soo;Lee, Nam-Hoon;Lee, Byoung-Chul
    • Journal of the Korea Organic Resources Recycling Association
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    • v.16 no.1
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    • pp.62-69
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    • 2008
  • There has been a recent trend in Korea that treatments for combustible wastes among municipal solid waste (MSW) by those methods, such as incineration and landfill are restricted as much as possible and Mechanical Biological Treatment (MBT) are encouraged actively in order to promote resource recovery. To build and operate properly these facilities, the physicochemical characteristics of MSW should be analyzed precisely beforehand. In particular, designing a crusher or separator properly which is the main process in MBT facilities of MSW. require the information on the size distribution characteristics of MSW, but they are nor sufficient in the qualities and quantities yet as of now. Accordingly, this study aims to evaluate size distribution characteristics of MSW and its physicochemical characteristics by size. The samples of MSW were collected from detached dwelling area, apartment area, business area, and commercial area of A city in Korea. According to the result of analysis, paper records 29.78~60.02% by wet weight basis, so it was the most regardless of the regions where the wastes were generated. And in terms of element analysis, Carbon(C) was 34.77~44.39%, the largest friction, and Oxygen(O) was the next occupying 19.46~33.71%. As indices of RDFs, Chlorine(Cl) was 0.39~0.83%, so it was less than the standard, 2.0%(by dry weight basis); moreover, Sulfur(S) did not exceed the standard, 0.6%, either. In the size distribution of MSW, waste fraction ranging 50~80mm in diameter was the most in combustible waste while 30~50mm was in incombustible waste.

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