• Bulletin of the Korean Chemical Society
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• 제29권12호
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• pp.2482-2486
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• 2008

• Journal of Dairy Science and Biotechnology
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• 제33권1호
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• pp.27-34
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• 2015

본 연구에서는 dispersive-SPE를 사용하여 간편하고, 신속하며, 경제적인 우유 내 19종 잔류농약의 동시 다성분 분석법을 설정하고자 하였다. Liquid-liquid partitioning method와 low-temperature cleanup method를 적용한 추출방법과 PSA 및 PSA + C18의 sorbent가 사용된 dispersive-SPE를 사용한 정제방법을 비교 실험하였으며, GC/MS의 선택이온 검색법(selected ion monitoring, SIM)으로 정량 분석하였다. matrix-matched standards와 matrix-free standards를 사용하여 분석방법의 matrix enhancement effect를 확인하였고, 분석방법 설정을 위한 비교실험의 결과, low-temperature cleanup 방법으로 추출하여 dispersive-SPE(PSA + C18)로 정제하는 방법이 시료 추출물의 간섭물질을 제거하는데 가장 효과적이고, 첨가한 $1{\mu}g/mL$에 대한 개별 농약 성분의 회수율 또한 전체적으로 가장 높은 수준을 나타내었으며, 모든 농약 성분의 RSD(%)가 20% 이하로서 기준에 적합한 재현성을 나타내었다.

• Korean Chemical Engineering Research
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• 제54권5호
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• pp.636-647
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• 2016

Magnetite nanoparticles ($Fe_3O_4$ NPs) were synthesized by co-precipitating method under optimized condition. The $Fe_3O_4$ NPs coated with sodium dodecyl sulfate-thenoyltrifluoroacetone ($Fe_3O_4$ NPs-SDS-TTFA) were then exerted as the magnetic solid phase extraction (MSPE) adsorbent for the extraction process prior to introducing to a flame atomic adsorption spectrometry (FAAS). The synthesized $Fe_3O_4$ NPs-SDS-TTFA were applied for the extraction of Pb(II) ions from different water samples. The characterization studies of nanoparticles were performed via scanning electron microscopy-energy dispersive micro-analysis (SEM-EDAX), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM) techniques. The substantial parameters affecting the extraction efficiency were surveyed and optimized. A dynamic linear range (DLR) of $10-400{\mu}g\;L^{-1}$ was obtained and the limit of detection (LOD, n=7) and relative standard deviation (RSD%, n= 6, $C=20{\mu}g\;L^{-1}$) were found to be $2.3{\mu}g\;L^{-1}$ and 1.9%, respectively. According to the results, the proposed method successfully applied for the extraction of Pb(II) ions from different environmental water samples and satisfactory results achieved.

• Bulletin of the Korean Chemical Society
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• 제32권12호
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• pp.4265-4269
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• 2011

A method based on ethyl acetate extraction and gas chromatography with tandem mass spectrometry was developed for determining tetraconazole residues in fruits and vegetables. A 10 g homogenized sample was mixed with 10 mL ethyl acetate, shaken vigorously for 3 min, stored at $-20^{\circ}C$ for 15 min, and then vortexed vigorously for 1 min; 1 g NaCl and 4 g anhydrous $MgSO_4$ were added. The clean-up was carried out by applying dispersive solid-phase with 150 mg $MgSO_4$and 50 mg primary secondary amine. Three precursor product ion transitions for tetraconazole were measured and evaluated to provide the maximum degree of confidence. Average recoveries in fruits and vegetables at three levels (0.005, 0.05 and 0.5 mg/kg) ranged from 85.53% to 110.66% with relative standard deviations ($RSD_r$) from 1.3% to 17.5%. The LODs ranged from 0.002 to 0.004 ${\mu}g$/kg, and LOQs ranged from 0.006 to 0.012 ${\mu}g$/kg. This method was also applied to determine tetraconazole residue in cucumber dissipation experiment under field conditions. The half-lives of tetraconazole in cucumber were in the range of 2.1-3.1 days.

• Carbon letters
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• 제26권
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• pp.43-50
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• 2018

In this research, a novel and efficient quinoline thioacetamide functionalized magnetic graphene oxide composite ($GO@Fe_3O_4@QTA$) was synthesized and utilized for dispersive magnetic solid phase preconcentration of Cd(II) and Ni(II) ions in urine and various food samples. A number of diverse methods were employed for characterization of the new nanosorbent. The design of experiments approach and response surface methodology were applied to monitor and find the parameters that affect the extraction performance. After sorption and elution steps, the concentrations of target analytes were measured by employing FAAS. The highest extraction performance was achieved under the following experimental conditions: pH, 5.8; sorption time, 6.0 min; $GO@Fe_3O_4@QTA$ amount, 17 mg; 2.4 mL $1.1mol\;L^{-l}$ $HNO_3$ solution as the eluent and elution time, 13.0 min. The detection limit is 0.02 and $0.2ng\;mL^{-1}$ for Cd(II), and Ni(II) ions, respectively. The accuracy of the new method was investigated by analyzing two certified reference materials (sea food mix, Seronorm LOT NO 2525 urine powder). The interfering study revealed that there are no interferences from commonly occurring ions on the extractability of target ions. Finally, the new method was satisfactorily employed for rapid extraction and determination of target ions in urine and various food samples.

• 환경생물
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• 제36권3호
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• pp.345-351
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• 2018

An efficient, quick and low-cost extraction and clean up method for the determination of 14 polycyclic aromatic hydrocarbons (PAHs) in the agricultural water samples was optimized using gas chromatography-tandem mass spectrometry (GC-MS/MS). The extraction of the target compounds in water sample was carried out with acetonitrile, followed by partitioning promoted by the addition of salt. As a clean-up procedure, dispersive solid phase extraction was employed to purify the analytes of interest for GC-MS/MS analysis. This method was successfully applied for the quantification of PAHs in real water samples collected for the purpose of monitoring from the waterways located in Chungbuk (15 sites) and Gyeongbuk (6 sites), S. Korea. Phenanthrene (0.54 to $2.53{\mu}gL^{-1}$) was detected in all the water samples collected from both the sites. Fluoranthene was detected in the water samples collected from the two sites in Gyeongbuk province, but other PAHs were not determined in these water sampling sites. Based on these results, the determined PAHs were conducted using an environmental risk assessment. The risk characterization ratios (RCRs) for phenanthrene ranged from 0.37 to 3.21. These RCR values referred to as risk was not controlled because RCR values of some sites were greater than 1. In conclusion, it is proposed that the optimized method in combination with GC-MS/MS could be successfully employed for the determination of PAHs in any environmental samples including water samples.

• Advances in concrete construction
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• 제12권6호
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• pp.507-515
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• 2021

To evaluate the influence of slag on the alkalinity of pore solution and microstructure of concrete, this paper performs a leaching experiment on hardened cement-slag pastes (HCSP) slice specimens with different slag content in purified water. The pH value of pore solution, average porosity, morphology, phase composition and Ca/Si of HCSP specimens in the leaching process are measured by solid-liquid extraction, saturated-dried weighing, scanning electron microscopy-energy dispersive spectrometry (SEM-EDS) and X-ray diffraction (XRD). Results shows that the addition of slag can mitigate an increase in porosity and a decrease in Ca/Si of HCSP in the leaching process. Besides, an appropriate slag content can improve the microstructure so as to obtain the optimum leaching resistance of HCSP, which can guarantee the suitable alkalinity of pore solution to prevent a premature corrosion of reinforced bar. The optimum slag content is 40% in HCSP with a water-binder ratio of 0.45, and an excessive slag causes a significant decrease in the alkalinity of pore solution, resulting in a loss of protection on reinforced bar in HCSP.

• Conservation and Restoration of Cultural Heritage
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• 제1권1호
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• pp.9-22
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• 2012

The most widely excavated iron artifacts used as weapons or farm tools from central southern regions of Korea were subjects of non-metallic inclusion analysis through metallographic examination, microhardness measurement, and scanning electron microscopy with energy dispersive X-ray spectroscopy. Through metallographic interpretation and study of the analyzed results, the steel manufacturing and iron smelting using heat processing in the iron artifacts excavated from the central southern region of the ancient Korean peninsula was studied, and the analysis of the non-metallic inclusions mixed within the metallic structures was interpreted as the ternary phase diagram of the oxide to infer the type of iron ores for the iron products and the temperature of the furnace used to smelt them. Most of the ancient forged iron artifacts showed $Al_2O_3/SiO_2$ with high $SiO_2$ contents and relatively low $Al_2O_3$ contents for iron ore, indicating t hat for $Al_2O_3$ below 5%, it is presumed that magnetic iron ores were reduced to bloom iron (sponge iron) with direct-reduction process for production. The temperature for extraction of wustite for $Al_2O_3$ below 1% was found to be $1,020{\sim}1,050^{\circ}C$. Considering the oxide ternary constitutional diagram of glassy inclusions, the steel-manufacturing temperature was presumed to have been near $1,150{\sim}1,280^{\circ}C$ in most cases, and minimum melting temperature of casting iron part excavated in Daeseong-ri. Gyeonggi was near $1,400^{\circ}C$, and it is thought that hypoeutectic cast iron of about 2.3% carbon was casted and fragility of cast iron was improved by decarburizing in solid state.

• 환경생물
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• 제34권3호
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• pp.216-221
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• 2016

다환방향족탄화수소류 (PAHs, Polycyclic aromatic hydrocarbons)는 열분해 또는 불완전연소 과정에서 발생하는 방향족 고리를 포함하고 있는 유기화합물질로서 생물 및 인간에 해를 입힐 수 있는 독성물질들로 알려져 있다. 이에 본 연구는 경기도 20곳 및 강원도 15곳에서 농업용수를 채취하여, 시료 중 PAHs 농도와 분포 특성을 규명하였다. 쉽고 간단하고 효과적인 케처스 추출법 및 d-SPE 정제법을 이용해 분석 시료를 준비한 후에 GC-MS/MS를 이용해 14종의 PAHs 분석하였다. 경기도 강원도 지역에서 채취한 모든 시료에서 Phenanthrene이 검출되었으며 경기도 지역의 phenanthrene 농도는 $0.82{\sim}2.56{\mu}g\;L^{-1}$였고 강원도 지역의 phenanthrene 농도는 $0.83{\sim}1.62{\mu}g\;L^{-1}$였다. 경기도 한 곳에서만 fluoranthene ($0.26{\mu}g\;L^{-1}$)이 검출되었다. 분석법의 효율과 신뢰성을 확신하기 위한 회수율 시험에서 60~110%의 회수율을 얻었다. 상대표준편차는 PAHs 14종 모두 20% 이하였다.

• 한국환경농학회지
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• 제35권3호
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• pp.166-174
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• 2016

농경지 토양에서 대상항생제 6종(amoxicillin, ampicillin, chlortetracycline, enrofloxacin, oxytetracycline, tetracycline을 아세트산 함유 아세토니트릴, Na₂Cit.5H₂O, Na₃Cit.2H₂O과 Na₂-EDTA로 추출 후 C₁₈으로 정제하여 LC-MS/MS로 분석하는 모니터링을 수행하였다. 그 중 2종의 항생제, chlortetracycline과 enrofloxacin이 국내 농경지 토양에서 검출되었다. 제안한 분석법은 토양 중 잔류 항생제 모니터링을 위한 빠르고 간편한 시험법이었고 다양한 활용이 가능할 것으로 보인다.