• Title/Summary/Keyword: solvent recovery

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Process Optimization Using Regression Analysis of Distillation Processes for the Recovery of Propylene Glycol Monomethyl Ether Acetate (PGMEA) Containing Waste Organic Solvent (폐액 중 프로필 글리콜 모노메틸 에테르 아세테이트(PGMEA) 회수하는 증류공정에서 회귀분석을 이용한 공정 최적화)

  • Choi, Yong-Seok;Byun, Hun-Soo
    • Korean Chemical Engineering Research
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    • v.53 no.2
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    • pp.181-192
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    • 2015
  • The aim of this study is to obtain optimum process condition for using two tower distribution to recycle the waste Propylene Glycol Monomethyl Ether Acetate (PGMEA) that is formed after washing LCD. The optimum process condition for the content of PGMEA, which is dependent variable, at 1st distillation was calculated according to Bottom temperature (BTM temperature), Reflux amount, Feed amount, Feed temperatures, and the optimum process conditions and optimum factors for the content of PGMEA at 2nd distillation according to Bottom temperature (BTM temperature), Reflux amount, Feed amount, Feed temperatures. At 1st distillation, Reflux amount, Feed amount, and Feed temperature are significant variables. However, it is found that the BTM temperature range is not significant in the range of process condition used in this study. The optimum process conditions are based on $5700{\ell}$ of Feed amount, $2500{\ell}$ of Reflux amount, $165^{\circ}C$ of BTM temperature, and $130^{\circ}C$ of Feed temperature. For the this condition, the predicted content of PGMEA was calculated as 92.12~94.62%. Significant factors at 2nd distillation are Reflux amount, Feed amount, and BTM temperature. Multicollinearity is between Reflux amount and BTM temperature. BTM was omitted in the multiple regression equation because there is a strong positive correlation between Reflux amount and BTM temperature. Base on $199^{\circ}C$ of BTM temperature, The optimum process conditions are based on $4275{\ell}$ of Feed amount, $6200{\ell}$ of Reflux amount and $130^{\circ}C$ of Feed temperature. In this condition, the predicted content of PGMEA was calculated as 99.0~99.5%.

A Study on the Treatment of Wastewater from Ion Removal Process for Purifying Electrocoat Paint in the Bath by Use of Reverse Osmosis (역삼투압을 이용한 전착도료 정제공정폐수처리에 관한 연구)

  • 김진성
    • Membrane Journal
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    • v.8 no.2
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    • pp.77-85
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    • 1998
  • To treat effectively EDIR (electrodeposition ion removal) wastewater in terms of CO$_{Mn}$ 1,500~2,000 ppm generated from aluminum painting process, a RO (reverse osmosis) process was designed and installed to recover and reuse the concentrated solvent sent back to the electrocodeposition tank while the permeate reused as rinse water. A RO system in which three polyamide-spiral wound modules ($102\Phi \times 1,016L$ mm) connnected in series had been running to treat 20 m$^3$ in waste volume in 3 days batch operation at the condition of system recovery of 30 %, applied pressure 11.5 $kg_f/cm^2$ and room temperature. During 42 hours continuous operation leading to 5-fold decrease in waste volume, nearly constant permeation flux of 390 l/m$^2$-hr was maintained and the permeate with average CO$_{Mn}$, 300 ppm was obtained which could be used for washing the remaining paint solution in ion-exchange tower instead of demineralized water. Also COD$_{Mn}$ rejection as a function of running time was observed to be in the range of 78~87 % and the observed solvent rejections for ethyl cellusolve, buthyl cellusolve and n-butanol were 79 %, 87 % and 70 %, respectively.

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Validation on the Analytical Method of Ginsenosides in Red Ginseng

  • Cho B. G.;Nho K. B.;Shon H. J.;Choi K. J.;Lee S. K.;Kim S. C;Ko S. R.;Xie P. S.;Yan Y. Z.;Yang J. W.
    • Proceedings of the Ginseng society Conference
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    • 2002.10a
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    • pp.491-501
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    • 2002
  • A cross-examination between KT&G Central Research Institute and Guangzhou Institute for Drug Control was carried out in order to select optimum conditions for extraction, separation and determination of ginsenosides in red ginseng and to propose a better method for the quantitative analysis of ginsenosides. The optimum extraction conditions of ginsenosides from red ginseng were as follows: the extraction solvent, $70\%$ methanol; the extraction temperature, $100^{\circ}C;$ the extraction time, 1 hour for once; and the repetition of extraction, twice. The optimum separation conditions of ginsenosides on the SepPak $C_{18}$ cartridge were as follows: the loaded amount, 0.4 g of methanol extract; the washing solvents, distilled water of 25 ml at first and then $30\%$ methanol of 25 ml; the elution solvent, $90\%$ methanol of 5 ml. The optimum HPLC conditions for the determination of ginsenosides were as follows: column, Lichrosorb $NH_2(25{\times}0.4cm,$ 5${\mu}m$, Merck Co.); mobile phase, a mixture of acetonitrile/water/isopropanol (80/5/15) and acetonitrile/water/isopropanol (80/20/15) with gradient system; and the detector, ELSD. On the basis of the optimum conditions a method for the quantitative analysis of ginsenosides were proposed and another cross-examination was carried out for the validation of the selected analytical method conditions. The coefficient of variances (CVs) on the contents of ginsenoside-$Rg_{1}$, -Re and $-Rb_1$ were lower than $3\%$ and the recovery rates of ginsenosides were $89.4\~95.7\%,$ which suggests that the above extraction and separation conditions may be reproducible and reasonable. For the selected HPLC/ELSD conditions, the CVs on the detector responses of ginsenoside-Rg, -Re and $-Rb_1$) were also lower than $3\%$, the regression coefficients for the calibration curves of ginsenosides were higher than 0.99 and two adjacent ginsenoside peaks were well separated, which suggests that the above HPLC/ELSD conditions may be good enough for the determination of ginsenosides.

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Characterization of Microemulsion of Crude Oil Using Alkali-Surfactant Solution (알칼리-계면활성제 용액을 이용한 인도네시아 A원유의 마이크로에멀전 특성)

  • Lee, Sang Heon;Kim, Sang Kyum;Bae, Wisup;Rhee, Young Woo
    • Applied Chemistry for Engineering
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    • v.26 no.3
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    • pp.259-264
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    • 2015
  • For the enhanced oil recovery, one of the most important factors is to determine the surfactant formulation in chemical flood. The objective of this study is to analyze the microemulsion formed between the alkali-surfactant (AS) solution and A crude oil for screening surfactants. The alkali-surfactant solution was manufactured by using the surfactant purchased from AK ChemTech. $C_{16}-PO_7-SO_4$ and sodium carbonate solution were used as surfactant and alkaline, respectively. Both TEGBE and IBA were used as a co-solvent. The AS solution and A crude oil can form a Type III middle phase microemulsion at the salinity from 0.0 wt%~3.6 wt%. Increasing the salinity causes the phase transition of microemulsion from the lower (Type I) to middle (Type III) to upper (Type II) phase. Interfacial tension (IFT) values calculated by Huh's equation were in good agreement with ultralow IFT. According to this characteristic, the surfactant purchased from a domestic company can be applied to the enhanced oil recovery.

Analysis of Vitamin K1 in Commonly Consumed Foods in Korea (국내에서 소비되는 상용 식품의 비타민 K1 함량 분석)

  • Lee, Seongeung;Sung, Jeehye;Choi, Youngmin;Kim, Youngwha;Jeong, Heon-Sang;Lee, Junsoo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.8
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    • pp.1194-1199
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    • 2015
  • Vitamin $K_1$ (phylloquinone) content of commonly consumed foods in Korea were determined by solvent extraction followed by reversed-phase liquid chromatography using post-column derivatization and fluorescence detection. Samples were obtained in the years of 2013 and 2015. In this study, 46 vegetables, 14 fruits, and 6 legumes were analyzed. Relatively higher amounts of vitamin $K_1$ were found in sweet potato leaves, green kiwi, and mung beans among vegetables, fruits, and legumes, respectively. The content of vitamin $K_1$ in vegetables including spinach, broccoli, and potato ranged from non-detectable (ND) to $1,467.3{\mu}g/100g$. The content of vitamin $K_1$ in fruits ranged from ND to $42.7{\mu}g/100g$. The content of vitamin $K_1$ in legumes, including soybeans, mung beans and peas ranged from 1.7 to $63.4{\mu}g/100g$. In addition, the analytical method validation parameters including recovery, reproducibility, repeatability, peak purity, and linearity were calculated to ensure the method's validity. The results showed high linearity with a correlation coefficient of 0.9999. Overall recovery was close to 100% (n=5). This study revealed reliable vitamin K content in commonly consumed foods in Korea for a nutritional information and food composition database.

Preparation of Biodegradable Polymer Microparticles Containing 5-FU Using Supercritical Carbon Dioxide (초임계 이산화탄소를 이용한 5-FU 함유 생분해성 고분자 미세입자 제조)

  • Jung, Ju-Hee;Jung, In-Il;Joo, Hyun-Jae;Shin, Jae-Ran;Lim, Gio-Bin;Ryu, Jong-Hoon
    • KSBB Journal
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    • v.23 no.5
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    • pp.452-459
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    • 2008
  • To obtain maximal efficacy with minimal systemic side-effects, many studies have been carried out to achieve the controlled release of 5-fluorouracil (5-FU). In this study, biodegradable poly(L-lactide) (L-PLA) microparticles containing 5-FU were prepared by a process, called aerosol solvent extraction system (ASES), utilizing supercritical carbon dioxide. The effects of various organic solvents, drug/polymer feeding ratio, polymer molecular weight, and blending with the same polymers with different molecular weights on the formation of 5-FU loaded microparticles were investigated under a predetermined operating condition from our previous study. The drug recovery, entrapment efficiency, and in vitro drug release kinetics were determined by HPLC assays. The drug recovery obtained from the ASES process was found to be very high, whereas the drug entrapment efficiency was considerably low in all the experiments due to the poor affinity between L-PLA and 5-FU. These results indicated that the precipitation rate of L-PLA might be quite different from that of 5-FU so that there was little chance to form 5-FU loaded L-PLA microparticles.

Improved Radiochemical Yields, Reliability and Improvement of Domestic $^{18}F$-FDG Auto Synthesizer (국산 $^{18}F$-FDG Auto Sysnthesizer의 수율 향상과 성능 개선)

  • Park, Jun-Hyung;Im, Ki-Seop;Lee, Hong-Jin;Jeong, Kyung-Il;Lee, Byung-Chul;Lee, In-Won
    • The Korean Journal of Nuclear Medicine Technology
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    • v.13 no.3
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    • pp.147-151
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    • 2009
  • Purpose: 2-[$^{18}F$]Fluoro-2-deoxy-D-glucose ([$^{18}F$]FDG) particularly plays as a important role in Positron Emission Tomography (PET) imaging in nuclear medicine. Domestic [$^{18}F$]FDG auto synthesizers are installed in Seoul National University Bundang Hospital (SNUBH) at June 2008, these modules were known that it's synthetic yields were guaranteed in average $45{\pm}5%$ so far. To improve yields and convenience of domestic [$^{18}F$]FDG auto synthesizer, numerous trials in reaction time, base concentration, pressure and temperature were performed to increase [$^{18}F$]FDG yields. Materials and Methods: Several synthetic factors (temperature, time and pressure) and shortcoming were corrected based on many evaporation test. Syringe dispensing of tetra-butylammonium bicarbonate (TBAB) was replaced with micro pipette to prepare tetrabutyl ammonium fluoride salt ([$^{18}F$]TBAF). Troublesome refill of liquid nitrogen every 2 hours which was used to protect vacuum system was changed to charcoal cartridge, base guard filter. To monitor the volume of delivered $[^{18}O]OH_2$ from cyclotron by surveillance camera, we set up the volumetric vial on the cover of the module. In addition to, the recovery vial was added in [$^{18}F$]FDG production system to recover [$^{18}F$]FDG loss due to the leak of valve ($V_{13,14}$) in [$^{18}F$]FDG purification process. Results: When we used micro pipette for adding TBAB ($30\;{\mu}L$ in 12% $H_2O$ in acetonitrile), this quantitative dispensation has enabled to improve $5.5{\pm}1.7%$ residual fluorine-18 activity in fluorine separation cartridge compared to syringe adding. Besides, the synthetic yields of [$^{18}F$]FDG has increased $58{\pm}2.6%$ (n=19), $58{\pm}2.9%$ (n=14), $60%{\pm}2.5%$ (n=17) for 3 months. The life cycle of charcoal cartridge and base vacuum was 3 months prior to filling liquid nitrogen every 2 hours and additional side separator can prevent pump corrosion by organic solvent. After setting of volumetric indicator vial, the operator can easily monitor the total volume of irradiated $[^{18}O]OH_2$ from cyclotron. The recovery vial can be used for the stabilizer when an irregular [$^{18}F$]FDG loss was generated by the leak of valves ($V_{13,14}$). Conclusions: We has optimized appropriate synthetic conditions (temperature, time, pressure) in domestic [$^{18}F$]FDG auto synthesizer. In addition to, the remodeling with several accessories improve yields of domestic [$^{18}F$]FDG auto synthesizer with reliable reproducibility.

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Simultaneous Determination of B Group Vitamins in Supplemented Food Products by High Performance Liquid Chromatography-Diode Array Detection

  • Suh, Joon-Hyuk;Yang, Dong-Hyug;Lee, Byung-Kyu;Eom, Han-Young;Kim, Un-Yong;Kim, Jung-Hyun;Lee, Hye-Yeon;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • v.32 no.8
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    • pp.2648-2656
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    • 2011
  • A simple HPLC-DAD method was developed and validated to determine B group vitamin content (thiamine, riboflavin, nicotinamide, pantothenic acid, pyridoxine and folic acid) in supplemented food samples, i.e., infant formula, cereal, low-calorie food, a multi-vitamin pill and a vitamin drink. In this study, the most significant advantages were simultaneous determination of the six B group vitamins in various food matrices and a small number of sample treatment steps that required only an organic solvent, acetonitrile. Moreover, this method prevents reduction of column durability, because the mobile phase does not contain ion-pairing reagents. Analytes were separated on a Develosil RPAQUEOUS $C_{30}$ (4.6 mm ${\times}$ 250 mm, 5 ${\mu}M$ particle size) column with a gradient elution of acetonitrile and 20 mM phosphate buffer (pH 3.0) at a flow rate between 0.8 and 1.0 mL/min. Detection was performed at 275 nm, except for that of pantothenic acid (205 nm). The calibration curves for all six vitamins showed good linearity with correlation coefficients ($r^2$) higher than 0.995. The developed method was validated with respect to linearity, intra- and inter-day accuracy and precision, limit of quantification (LOQ), recovery and stability. The method showed good precision and accuracy, with intra- and inter-assay coefficients of variation less than 15% at all concentrations. The recovery was carried out according to the standard addition procedure, with yields ranging from 89.8 to 104.4%. This method was successfully applied to the determination of vitamin B groups in supplemented food products.

Separation and Purification of 2,6-dimethylnaphthalene in the Light Cycle Oil(I) -Concentration of a mixture of dimethylnaphthalene isomers in the light cycle oil- (접촉분해경유에 함유된 2,6-dimethylnaphthalene의 분리, 정제(I) -접촉분해경유에 함유된 dimethylnaphthalene이성체 혼합물의 농축-)

  • Kim, Su-Jin;Kim, Sang-Chai;Kawasaki, Junjiro
    • Applied Chemistry for Engineering
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    • v.7 no.1
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    • pp.162-170
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    • 1996
  • Light cycle Oil(LCO) contains 2,6-dimethylnaphthalene (2,6-DMNA) which is used as the basic material for high performance engineering plastics and liquid crystal polymer. This study was experimentally investigated to concentrate a mixture of dimethylnaphthalene(DMNA) isomers in the LCO by extraction-distillation combination as a pretreatment for separation and purification of 2,6-DMNA in the LCO. Furthermore, concentration of a mixture of DMNA isomers in the LCO compared between distillation and extraction-distillation combination. The recovery of aromatics in the LCO was performed by batch cocurrent multistage extraction with dimethylsulfoxide and water mixture as solvent. The concentration of naphthalene group(carbon number 10-12) in the extracted mixture is higher than that in the LCO. The yield for naphthalene group increased with decreasing carbon number. The yield for a mixture of DMNA isomers obtained in 5 equilibrium extration runs was about 65%. the separation of individual components with extractedmixture was tested by batch distillation. Futhermore, for recovery of a mixture of DMNA isomers of high concentration, distillate containing DMNA was distilled. As a result, a mixture of DMNA isomers with high concentration such as 60wt% was recovered. The extraction-distillation combination was more effective than the distillation to concentration a mixture of DMNA isomer in the LCO.

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The Effect of Dispersion Medium on Intensity of Volatile Flavor Components and Recovery of Essential Oil from Capsella bursa-pastoris by Steam Distillation (수증기 증류시 분산매의 조성이 냉이의 휘발성 향기성분의 강도 및 정유 회수율에 미치는 영향)

  • Choi, Hyang-Sook;Lee, Mie-Soon
    • Korean Journal of Food Science and Technology
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    • v.28 no.5
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    • pp.827-833
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    • 1996
  • Along with the increased necessity for an efficient utilization of Korean wild edible plants growing in fields and mountains, attempts were made to investigate the patterns of flavor changes accompanied hy various conditions of dispersion medium. The effect of various pH values and concentration of sucrose or NaCl of dispersion medium on volatile flavor patterns was investigated to evaluate the applicability of flavor components extracted from Capsella bursa-pastoris for food industry. Essential oils from this wild plant were isolated by simultaneous steam distillation-extraction (SDE) method using diethyl ether as solvent. Concentrated samples were analyzed s chromatography (GC) and combined gas chromatography-mass spectrometry (GC-MS). Most volatile flavor components of Capsella bursa-pastoris showed good recovery when steam distilled at pH 7 by SDE method. Increasing concentration of sucrose and 15% by NaCl, resulted in greater numbers of identified flavor components from Capsella bursa-pastoris.

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