• 한국신재생에너지학회:학술대회논문집
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• 2009.06a
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• pp.880-883
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• 2009

석탄가스화복합발전(IGCC) 시스템에서 합성가스 중에 포함된 황화수소($H_2S$)는 후단의 가스 터빈과 같은 장치의 부식을 방지하고, 합성가스를 이용하는 연료전지 등의 연계 공정에서 요구하는 수준에 맞추어 정제되어야 한다. 본 연구에서는 $H_2S$ 정제공정 추가에 따른 IGCC 시스템의 효율저하를 최소화하기 위하여 고온고압에서 사용가능한 탈황제를 분무건조법을 이용하여 제조하고 제조된 탈황제에 대해 물성 및 황 흡수능 시험을 실시하였다. 형상, 내마모도, 평균입자크기, 충진밀도와 함께 제조된 탈황제가 적용되는 유동층 공정에 적합한 강도를 보유하는지 여부를 미국표준시험방법에 의하여 측정하였다. 황 흡수능은 열중량분석기를 반응기로 사용하여 모사 합성 가스 분위기에서 측정하였다. 분무건조 성형된 탈황제의 일부가 구형이 아닌 타원형 또는 도넛 형태를 나타내고 있어 형상 개선을 위한 제조방법 개선이 필요한 것으로 나타났다. 제조된 탈황제는 기공도가 65% 이상으로 macropore가 기공부피의 대부분을, mesopore가 비표면적의 대부분을 제공하고 있었다. 소성온도를 650 $^{\circ}C$에서 750 $^{\circ}C$로 증가시킴에 따라 대체로 강도가 감소하는 경향을 나타내었다. 열중량분석기로 측정된 황 흡수능은 약 10 wt%로 나타났다. 제조된 탈황제 중 일부는 유동층 공정에 적합한 물성을 보유하고 있었으며 반응성 또한 기존에 개발된 탈황제에 버금가는 성능을 나타내어 향후 공정 적용이 가능할 것으로 분석되었다.

• Korean Journal of Veterinary Service
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• v.34 no.4
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• pp.429-439
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• 2011

This article described the comparison of a quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation and the classical method established by National Veterinary Research and Quarantine Service (NVRQS) for the determination of pesticide residues in livestock products using GC-tandem mass spectrometry. The classical method by NVRQS used liquid-liquid partioning followed by evaporizing. The modified QuEChERS entailed extraction of 2 g sample with 15 ml acetonitrile containing 1% acetic acid followed by addition of 6 g anhydrous magnesium sulfate and 1.5 g sodium acetate. After centrifugation, 6 ml of the extract underwent a cleanup step (in a technique known as column-based solid phase extraction) using 400 mg each of $C_{18}$ and primary secondary amine sorbents plus 1,200 mg magnesium sulfate. The quantitation of individual pesticides by both methods was based on tissue standard calibration curves with a correlation coefficient in excess of 0.98 for the 24 pesticides. The detection limits by the classical method were ranged 1.3~5.0 ${\mu}g$/kg, with mean recoveries between 76.2% and 114.3% except aldrin (59.3%) and deltamethrin (63.6%). The detection limits by modified QuEChERS were ranged 0.3~6.2 ${\mu}g$/kg, with mean recoveries between 68.0% and 114.3% except dimethipin (152.6%), chlorfenvinphos (138.1%), 4,4-DDT (61.5%), aldrin (60.4%) and chinomethionate (30.3%).

• Environmental Engineering Research
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• v.19 no.3
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• pp.289-292
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• 2014

The effect of carbon dioxide ($CO_2$) on global warming is serious problem. The adsorption with solid sorbents is one of the most appropriate options. In this study, the most interesting adsorbent is granular activated carbon (GAC). It is suitable material for $CO_2$ adsorption because of its simple availability, many specific surface area, and low-cost material. Afterwards, GAC was impregnated with chitosan solution as impregnated granular activated carbon (CGAC) in order to improve the adsorption capacity of GAC. This research aims to compare the physical and chemical characteristics of GAC and CGAC. The experiment was carried out to evaluate the efficiency of $CO_2$ adsorption between GAC and CGAC. The results indicated that the iodine number of GAC and CGAC was 137.17 and 120.30 mg/g, respectively. The Brunauer-Emmett-Teller results (BET) of both GAC and CGAC show that specific surface area was 301.9 and $531.3m^2/g$, respectively; total pore volume was 0.16 and $0.29cm^3/g$, respectively; and mean diameter of pore was 2.18 and 2.15 nm, respectively. Finally, the $CO_2$ adsorption results of both GAC and CGAC in single column how the maximum adsorption capacity was 0.17 and 0.25 mol/kg, respectively; how degeneration time was 49.6 and 80.0 min, respectively; and how the highest efficiency of $CO_2$ adsorption was 91.92% and 91.19%, respectively.

• Korean Chemical Engineering Research
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• v.61 no.4
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• pp.619-626
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• 2023

Primary and secondary amine-based sorbents were synthesized to investigate the operation capacity for the carbon dioxide separation TSA process. (3-Aminopropyl) triethoxysilane was used as a primary amine precursor as a crosslinking agent to synthesize a secondary amine precursor in which amine groups were crosslinked with a crosslinking agent. Carbon dioxide absorbed by primary amines is completely separated above 170 ℃. The working capacity of the primary amine absorbent was less than 2% when regenerated at 130℃. The secondary amine absorbent has a higher carbon dioxide separation capacity at a lower regeneration temperature than the primary amine absorbent. The secondary amine absorbent could predict process operation performance of about 6.5% with 2% carbon dioxide absorption and 100% carbon dioxide regeneration conditions. Therefore, it was found that the working capacity of the secondary amine absorbent was higher than that of the primary amine.

• Korean Chemical Engineering Research
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• v.50 no.3
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• pp.492-498
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• 2012

In this study, hydrodynamics such as solid circulation rate and voidage in the desulfurizer and the reaction characteristics of Zn-based solid sorbents were investigated using lab-scale high pressure and high temperature desulfurization process. The continuous HGD (Hot Gas Desulfurization) process consist of a fast fluidized bed type desulfurizer (6.2 m tall pipe of 0.015 m i.d), a bubbling fluidized bed type regenerator (1.6 m tall bed of 0.053 m i.d), a loop-seal and the pressure control valves. The solid circulation rate was measured by varying the slide-gate opening positions, the gas velocities and temperatures of the desulfurizer and the voidage in the desulfurizer was derived by the same way. At the same gas velocities and the same opening positions of the slide gate, the solid circulation rate, which was similar at the temperature of $300^{\circ}C$ and $550^{\circ}C$, was low at those temperatures compared with a room temperature. The voidage in the desulfurizer showed a fast fluidized bed type when the opening positions of the slide gate were 10~20% while that showed a turbulent fluidized bed type when those of slide gate were 30~40%. The reaction characteristics of Zn-based solid sorbent were investigated by different desulfurization temperatures at 20 atm in the continuous operation. The $H_2S$ removal efficiency tended to decrease below the desulfurization temperature of $450^{\circ}C$. Thus, the 10 hour continuous operation has been performed at the desulfurization temperature of $500^{\circ}C$ in order to maintain the high $H_2S$ removal efficiency. During 10 hour continuous operation, the $H_2S$ removal efficiency was above 99.99% because the $H_2S$ concentration after desulfurization was not detected at the inlet $H_2S$ concentration of 5,000 ppmv condition using UV analyzers (Radas2) and the detector tube (GASTEC) which lower detection limit is 1 ppmv.

• Analytical Science and Technology
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• v.21 no.5
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• pp.412-423
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• 2008

A procedure based on solid-phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry has been developed for the simultaneous analysis of 55 basic drugs in equine urine. The test scope covers diversified classes of drugs including some ${\beta}$-blockers, ${\beta}$-agonists, antihypotensives, CNS stimulants, sedatives, tranquilizers, antidepressants, antihypertensives and so on. LC-MS/MS separation and quantification was carried out in positive electrospray ionization and multiple reaction monitoring (MRM) mode. Four different brands of mixed mode cation exchange SPE sorbents; UCT XTRACT$^{(R)}$ XRDAH, Supelco DSC-MCAX$^{(R)}$, Varian Bond Elut Certify$^{(R)}$ and Waters Oasis$^{(R)}$ MCX were compared. The UCT XTRACT$^{(R)}$ XRDAH sorbent provided the best results in the preconcentration of samples, yielding relative recoveries higher than 80% except for terbutaline (41.3%), salbutamol (71.5%), heptaminol (70.7%), phenylpropanolamine (66.3%). Detection limits of the target drugs provided by the proposed analytical procedure were between 0.2~8.3 ng/mL.

• Journal of Korean Society for Atmospheric Environment
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• v.30 no.6
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• pp.586-599
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• 2014

During the last two decades, indoor air quality and volatile organic compounds (VOCs) have been of concern in Korean society due to their nature of potential health impacts. In order to investigate the pollution levels of VOCss in indoor environments, establishment of a solid test method for monitoring the airborne VOCss is essential. In Korea, a method based on adsorbent sampling and GC analysis coupled with thermal desorption was proclaimed as the Korea Standard Method for Indoor Air Quality Test. This study was carried out to examine some inherent problems of the VOCs measurement method. The VOCs method does not describe in detail preparing the standard samples. The standard samples may be prepared by impregnation of either liquid standard solutions or a mixture of standard gases. In this study, we investigated the optimal temperature condition for transferring the liquid standards onto a standard adsorbent tube. As a result, keeping the impregnation temperature at $250^{\circ}C$ will be recommended in regard of the boiling points of multiple target analytes and the thermal stability of the adsorbent. We also demonstrated some problems associated with handling of a syringe used for transferring the standard solutions onto the adsorbent tubes, and a best way to get rid of the syringe problems was suggested. Finally, a number of field works were conducted to evaluate the performance of adsorbent sampling methods. Comparison of different adsorbent tubes, i.e. tube packed with single sorbent (Tenax) and double sorbents (Tenax with Carbotrap), revealed that 30 to 40% differences between the two groups, implying that sampling efficiency is depending on the volatility and the strength of adsorbents. However, duplicate precisions for VOCs sampling with a same type of adsorbent and at same flow rates appeared to be satisfactory to be all within 20%, which is a quality control guideline. Distributed volume precisions were also found to be within a guideline value, 25%, although the precision was in general inferior to the duplicate precision. The Korea indoor VOCs test method should be more refined and improved in many aspects, particularly procedure and instrumentation for preparing the standard samples and specification of quality control assessment.

• Analytical Science and Technology
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• v.24 no.3
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• pp.200-211
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• 2011

In this study, 13 compounds including four volatile fatty acids (VFA) and nine volatile organic compounds (VOC) were analyzed by cryogenic trapping-thermal desorption technique. In order to evaluate the analytical method for VFA, calibration experiments were performed using five different sorbent materials. When the calibration results are compared between different sorbents, sampling tube filled with Carbopack X showed the highest response factor (RF) for both VFA and VOC. To validate this new analytical method for VFA using cryogenic trapping-thermal desorption technique, this method was compared with alkali absorption method recommended by the odor prevention law of the Korea Ministry of Environment (KMOE). For this purpose, unknown samples were analyzed by two different methods, i.e., cryogenic trapping-thermal desorption (TD) and alkali absorption with solid phase microextraction (SPME). When the results of two different methods were compared, ratios of concentrations determined by the two analytical methods (TD/SPME) was found as 0.46 (valeric acid) ~ 0.71 (isovaleric acid). Therefore, additional study is required to properly establish and find stable analytical conditions for VFA analysis. Furthermore, comparison between two different methods should be made with more reliable calibration approaches.

• Korean Journal of Environmental Agriculture
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• v.39 no.3
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• pp.246-252
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• 2020

BACKGROUND: Pesticides are broadly used to control weeds and pests, and the residues remaining in crops are managed in accordance with the MRLs (maximum residue limits). Therefore, an analytical method is required to quantify the residues, and we conducted a series of analyses to select and validate the quick and simple analytical method for tolpyralate in five agricultural products using QuEChERS (quick, easy, cheap, effective, rugged and safe) method and LC-MS/MS (liquid chromatography-tandem mass spectrometry). METHODS AND RESULTS: The agricultural samples were extracted with acetonitrile followed by addition of anhydrous magnesium sulfate, sodium chloride, disodium hydrogencitrate sesquihydrate and trisodium citrate dihydrate. After shaking and centrifugation, purification was performed with d-SPE (dispersive-solid phase extraction) sorbents. To validate the optimized method, its selectivity, linearity, LOD (limit of detection), LOQ (limit of quantitation), accuracy, repeatability, and reproducibility from the inter-laboratory analyses were considered. LOQ of the analytical method was 0.01 mg/kg at five agricultural products and the linearity of matrix-matched calibration were good at seven concentration levels, from 0.0025 to 0.25 mg/L (R²≥0.9980). Mean recoveries at three spiking levels (n=5) were in the range of 85.2~112.4% with associated relative standard deviation values less than 6.2%, and the coefficient of variation between the two laboratories was also below 13%. All optimized results were validated according to the criteria ranges requested in the Codex Alimentarius Commission (CAC) and Ministry of Food and Drug Safety (MFDS) guidelines. CONCLUSION: In conclusion, we suggest that the selected and validated method could serve as a basic data for detecting tolpyralate residue in imported and domestic agricultural products.

• Journal of Food Hygiene and Safety
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• v.34 no.2
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• pp.115-123
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• 2019

An analytical method was developed for the determination of fenpropimorph, a morpholine fungicide, in hulled rice, potato, soybean, mandarin and green pepper using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) sample preparation and LC-MS/MS (liquid chromatography-tandem mass spectrometry). The QuEChERS extraction was performed with acetonitrile followed by addition of anhydrous magnesium sulfate and sodium chloride. After centrifugation, d-SPE (dispersive solid phase extraction) cleanup was conducted using anhydrous magnesium sulfate, primary secondary amine sorbents and graphitized carbon black. The matrix-matched calibration curves were constructed using seven concentration levels, from 0.0025 to 0.25 mg/kg, and their correlation coefficient ($R^2$) of five agricultural products were higher than 0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.001 and 0.0025 mg/kg, respectively, and the limits of quantification for the analytical method were 0.01 mg/kg. Average recoveries spiked at three levels (LOQ, $LOQ{\times}10$, $LOQ{\times}50$, n=5) and were in the range of 90.9~110.5% with associated relative standard deviation values less than 5.7%. As a result of the inter-laboratory validation, the average recoveries between the two laboratories were 88.6~101.4% and the coefficient of variation was also below 15%. All optimized results were satisfied the criteria ranges requested in the Codex guidelines and Food Safety Evaluation Department guidelines. This study could serve as a reference for safety management relative to fenpropimorph residues in imported and domestic agricultural products.