Poly(acrylic acid) (PAA) microspheres is one of the widely-used polymeric materials for the bio-field application and the electric materials. For the synthesis of PAA microspheres, the polymerization technique using surfactants is applied. After the synthesis, the purification and separation processes are required for the removal of surfactant. When general organic solvents were used, many problems, such as huge amount of waste solvent, additional separation processes, and the possibility of residual media, were occurred. Thus, High-pressure Soxhlet extraction using liquid $CO_2$ was developed to solve these problems. In this study, High-pressure Soxhlet extraction of the synthesized PAA microspheres using liquid $CO_2$ was conducted for the removal of Monasil PCA which is used for the dispersion polymerization of acrylic acid in compressed liquid Dimethyl ether (DME). The morphology of the extracted PAA particles was checked by field emission scanning electron microscopy (FE-SEM) and the residual concentration of Monasil PCA was analyzed by inductively coupled plasma - Optical Emission Spectrometer (ICP-OES). For studying the effect of the solvent effect, Soxhlet extraction was conducted using n-hexane, liquid DME, and liquid $CO_2$. In case of n-hexane, some extracted PAA microspheres were produced. However, deformation was also occurred due to the high thermal energy of n-hexane vapor. Liquid DME could not remove Monasil PCA. When using liquid $CO_2$, the extracted PAA microspheres which were free for the residual solvent were produced without deformation. For finding the optimum operating condition, high-pressure Soxhlet extraction was conducted for 8 hours with changing the temperature of reboiler and condenser. When the extractor temperature is $19.6{\pm}0.2^{\circ}C$ and the pressure is $51.5{\pm}0.5$ bar, the best removal efficiency was obtained.
Byung Gyu, Park;Jong Heon, Kim;Jin Hee, Im;Kyoung Chul, Lee
Journal of the Society of Cosmetic Scientists of Korea
/
v.30
no.2
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pp.181-187
/
2004
Preparations of mesoporous materials using various templates and their applicability have been intensively investigated for many years. We studied on synthesizing mesoporous Ti02 with pores in which sensitive compounds having weak physico-chemical properties such as thermal or UV irradiation and low solubility in solvent are trapped. Prior to trapping OMC in the pores of mesoporous titania, OMC was nano-emulsified in O/W system using Lecithin. Thereafter the OMC was trapped in the pores of mesoporous titania using sol-gel method. Main focus of this work is to prepare OMC-trapped mesoporous titania and to trace the stability and solubility of nano-emulsified OMC in the pores of mesoporous titania, and compared with that of mesoporous silica. OMC-trapped mesoporous Inorganic-Organic hybrid titania showed higher factors in sun protecting and a skin penetration phenomenon was reduced.
Choi, Seong Dae;Jeon, Sang Kwon;Park, Geun Woo;Yang, Jin Young;Kim, Geon-Joong
Applied Chemistry for Engineering
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v.25
no.5
/
pp.503-509
/
2014
The carbon/porous silica composite membrane was fabricated in a simple manner, which could be successfully for the simultaneous separation and production of chiral epoxides and 1,2-diols, based on their differences in hydrophilic/hydrophobic natures. The chiral Co(III)-$BF_3$ salen catalyst adopted in the membrane reactor system has given the very high enantioselectivity and recyclability in hydrolysis of terminal epoxides such as ECH, 1,2-EB, and SO. The optically pure epoxide and the chiral catalyst were collected in the organic phase after hydrolysis reaction. The hydrophilic water-soluble 1,2-diol product hydrolyzed by chiral salen diffused into the aqueous phase through the SBA-16 or NaY/SBA-16 silica composite layer during the reaction. The water acted simultaneously as a reactant and a solvent in the membrane system. One optical isomer was obtained with high purity and yield, and furthermore the catalysts could be recycled without observable loss in their activity in the continuous flow-type membrane reactor.
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
/
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.
Kim, Ye Jin;Lee, Sung Hae;Hong, Sung Kyu;Kim, Min;Park, Sang Jin
Korean Chemical Engineering Research
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v.48
no.1
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pp.121-127
/
2010
This study is to optimize the enzyme(lipase) activity for biodiesel production. The ion-exchanged non-woven fabrics(EtA, DEA-EtA non-woven fabric) containing ethanolamine, diethylamine groups are used by radiation induced grafted polymerization onto a non-woven fabric for more effective immobilization of lipase. Since the porous hollow fiber membranes are showed the low throughputibehe non-woven fabric membranes are used for biodiesel production. The physical charateristics of enzyme immobilized and the enzyme activity to EtA and DEA-EtA non-woven fabrics are studied. The EtA non-woven fabrics are quite similar to DEA-EtA non-woven fabric for the amount of enzyme immobilized(EtA non-woven fabric:15.69 mg/g, DEA-EtA non-woven fabric:14.45 mg/g) but DEA-EtA non-woven fabrics have shown the lower permeabiliquite the organic solvent than the EtA non-woven fabrics(EtA non-woven fabric:$3.50mol/h{\cdot}kg$, DEA-EtA non-woven fabric:$0.38mol/h{\cdot}kg$). Optimum characteristics of ehe non-woven fabric membranes and the limilaractivity are also investigated for the effective biodiesel production.
The antibiotic bacterium JS7901, one of the eighty three antibiotic microorganisms which have been is elated in the surburbs of CheongJu-city, showed the most effective antimicrobial activities against test organisms, both bacteria and fungi. Among the different culture media Soytone Sugar medium was the most effective for growth and activity of the JS7901 antibiotic bacterium a against both Escherichia coli and Staphyllococcus aureus by the cylinder plate method. The higher the sugar content, was, the greater the antibiotic amount of substances of JS7901 were produced in the soytone sugar media. The antibiotic bacterium, JS7901 appeared to have a broad activity spectrum showing inhibition in Vitro against gram positive and negative bacteria and plant disease fungi. In general, the active substances were not transferred into organic solvents. Only a small portion of the activity was transferred into ethyl ether and was also adsorbed to active carbon when the cultured broth was also adsorbed to active carbon when the cultured broth was at $pH\;2.0\~4.0$. On adjusting at pH 8.0, the activity disappeared. The crude active substances could be obtained by means of vacuum drying method and still shelved strong activity. The dried active rake was solved by solvents and crystallized into various shapes. The active substances were developed on the silica gel plate in the solvent system of n-butanol-acetic acid-water(3 : 1 : 1) and gave 5 pinkish colored spots when sprayed with $0.2\%$ ninhydrine in ethanol. The upper 5th spot, which was the result of using disc plate method with Escherichia coli was the strongest of these spots.
Kim, Jin-Sook;Song, Hee-Sang;Chung, Nam-Hyun;Bang, Won-Gi
Applied Biological Chemistry
/
v.48
no.2
/
pp.109-114
/
2005
A bacterium capable of emulsifying hydrocarbon, n-hexadecane, and decreasing surface tension of the culture media using oil collapsing method was isolated. The bacterium was partially identified as Bacillus sp. and named BJS-51. n-Hexadecane was the most effective carbon source for production of biosurfactant. Surface tension was decreased from 76 dyne/cm to 31 dyne/cm and CMD (critical micelle dilution) had the highest value of 5.7 at 3% n-hexadecane. Ammonium phosphate was the most effective nitrogen source, when C/N ratio was 60, surface tension and CMD were 29 dyne/cm and 9.2, respectively. Optimum pH and temperature were 7.2 and $30^{\circ}C$, respectively. Produced biosurfactant was extracted and purified using organic solvent extraction method and preparative HPLC systems. After analysis by various color reaction, this biosurfactant was identified as lipopolysaccharide. Surface tension and CMC (critical micelle concentration) of purified biosurfactant were 27 dyne/cm and 0.08 g/l, repectively. CMD was 9.2, so the yield of biosurfactant was about 0.74 g/l at the optimal conditions. The biosurfactant was very stable at wide range of $pH\;2{\sim}12$ with surface tension $29{\sim}31\;dyne/cm$ and showed $29{\sim}30\;dyne/cm$ of surface tension after heat treatment at $100^{\circ}C$ for 60 min.
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.
In order to find out proper PVdF gel polymer electrolyte for Li/S battery, we investigated PVdF gel polymer electrolytes with various glyme type plasticizer such as polyglyme, tetraglyme, triglyme. The organic solvents as triglyme, tetraglyme, polyglyme (Mn = 250, 500) has different chain length of ethylene oxide(EO) in solvent of glyme system. ionic conductivity decreased as increasing chain length of EO in plasticizers. Ionic conductivity of PVdF gel electrolyte with tetraglyme, triglyme, polyglyme (Mn = 250, 500) at room temperature was $5{\times}10^{-4},\;3{\times}10^{-4},\;6{\times}10^{-5},\;3{\times}10^{-5}\;S/cm$, respectively. Li/S cell with PVdF gel polymer electrolyte using tetraglyme plasticizer had low interfacial resistance and the highest initial discharge capacity of 1232 mAh/g of active sulfur, which was about 70% utilization of theoretical value.
Residual solvents in foods are defined as organic volatile chemicals used or produced in manufacturing of extracts or additives, or functional foods. The solvents are not completely eliminated by practical manufacturing techniques and they also may become contaminated by solvents from packing, transportation or storage in warehouses. Because residual solvents have no nutritional value but may be hazardous to human health, there is a need to remove them from the final products or reduce their amounts to below acceptable levels. The purpose of this study was to develop and evaluate an analytical method for the screening of residual solvents in health functional foods. Furthermore, the aim of this study was to constitute a reasonable management system based on the current state of the market and case studies of foreign countries. Eleven volatile solvents such as MeOH, EtOH, trichloroethylene and hexane were separated depending on their column properties, temp. and time using Gas Chromatography (GC). After determining the GC conditions, a sample preparation method using HSS (Head Space Sampling) was developed. From the results, a method for analyzing residual solvents in health functional foods was developed considering matrix effect and interference from the sample obtained from the solution of solvents-free health functional foods spiked with 11 standards solutions. Validation test using the developed GC/HSS/MS (Mass Spectrometry) method was followed by tests for precision, accuracy, recovery, linearity and adequate sensitivity. Finally, examination of 104 samples grouped in suits was performed by the developed HSS/GC/MS for screening the solvents. The 11 solvents were isolated from health functional foods based on vapor pressure difference, and followed by separation within 15 minutes in a single run. The limt of detection (LOD), limit of quantification (LOQ), recovery and coefficient of variation (C.V.) of these compounds determined by the HSS/GC/MS were found to be 0.1 pg/mL, 0.1-125 pg/g, 51.0-104.6%, and less than 15%, respectively. Using the developed HSS/GC/MS method, residual solvent from 16 out of 104 health functional products were detected as a EtOH. This method therefore seems t o be a valuable extension ofanalytical method for the identification of residual solvents in health functional food.
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