• Title/Summary/Keyword: removal of residual solvents

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Removal of Residual Solvents in Paclitaxel by Supercritical Carbon Dioxide (초임계 이산화탄소를 이용한 Paclitaxel의 잔류용매 제거)

  • 김진현;박흥복;기은숙;강인선;최형균;홍승서
    • KSBB Journal
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    • v.16 no.3
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    • pp.233-236
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    • 2001
  • Because of casehardenign effect of amorphous paclitaxel, residual solvents, methylene chloride and emthanol could not be reduced to the maximum value allowed, 600 ppm and 3,000 ppm, in accord with the guidelines issued by the International Conference on Harmonization (ICH, 1997), using rotary evaporation and successive drying in a vacuum oven. However, methylene chloride and methanol were reduced to 486 ppm and 403 ppm, respectively using supercritical $CO_2$ on purified paclitaxel. The optimum pressure and operating time were 80 bar and 30 min at fixed operating temperature ($40^{circ}C$). This approach serves as a novel application of supercritical fluid extraction to remove residual solvents from active pharmaceutical ingredients.

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Ethanol-pretreated Drying of (+)-dihydromyricetin for Removal of Residual Solvents (잔류 용매 제거를 위한 (+)-dihydromyricetin의 에탄올 전처리 건조)

  • Lee, Hee-Gun;Kim, Jin-Hyun
    • Korean Chemical Engineering Research
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    • v.60 no.2
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    • pp.237-242
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    • 2022
  • In this study, a drying method that can effectively remove residual solvent from (+)-dihydromyricetin was developed. Residual acetone concentration was efficiently removed below ICH-specified value (5,000 ppm) by simple rotary evaporation with ethanol pretreatment. In addition, the residual ethanol met the ICH-specified value (5,000 ppm) by simple rotary evaporation through the addition of water, and the residual moisture also met the specified value (<4%) for active pharmaceutical ingredients. At all the drying temperature (35, 45, and 55 ℃), a large amount of the residual solvent was initially removed during the drying, and the drying efficiency increased when increasing the drying temperature. Removal of residual solvent by ethanol pretreatment was shown to be related to high vapor pressure of acetone-ethanol mixture and hydrogen bonding between acetone and ethanol.

Effects of Residual PMMA on Graphene Field-Effect Transistor

  • Jung, J.H.;Kim, D.J.;Sohn, I.Y.;Lee, N.E.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2012.02a
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    • pp.561-561
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    • 2012
  • Graphene, two dimensional single layer of carbon atoms, has tremendous attention due to its superior property such as fast electron mobility, high thermal conductivity and optical transparency, and also found many applications such as field-effect transistors (FET), energy storage and conversion, optoelectronic device, electromechanical resonators and chemical sensors. Several techniques have been developed to form the graphene. Especially chemical vapor deposition (CVD) is a promising process for the large area graphene. For the electrically isolated devices, the graphene should be transfer to insulated substrate from Cu or Ni. However, transferred graphene has serious drawback due to remaining polymeric residue during transfer process which induces the poor device characteristics by impurity scattering and it interrupts the surface functionalization for the sensor application. In this study, we demonstrate the characteristics of solution-gated FET depending on the removal of polymeric residues. The solution-gated FET is operated by the modulation of the channel conductance by applying a gate potential from a reference electrode via the electrolyte, and it can be used as a chemical sensor. The removal process was achieved by several solvents during the transfer of CVD graphene from a copper foil to a substrate and additional annealing process with H2/Ar environments was carried out. We compare the properties of graphene by Raman spectroscopy, atomic force microscopy(AFM), and X-ray Photoelectron Spectroscopy (XPS) measurements. Effects of residual polymeric materials on the device performance of graphene FET will be discussed in detail.

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Effects of Residual Solvents in the Phase Transition, Transition Enthalpy, and Transition Temperature of Phospholipid Membranes (잔류 유기 용매가 모델 세포 지질막의 상전이, 상전이 엔탈피 및 상전이 온도에 미치는 영향)

  • An, Eun Seol;Choi, Jae Sun;Lee, Dong Kuk
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.40 no.2
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    • pp.163-170
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    • 2014
  • Lipid membranes composed of phosphatidylcholine (PC) are used in biophysical study to mimic cellular membranes and interactions between the membrane and chemicals, where organics solvents are used in dissolving lipids or chemicals. Later, solvents are removed from the solution under nitrogen gas at room temperature, followed by the further removal of the solvent at vacuum condition for several hours. In this process, some solvents are easily removed under described conditions above and others are required more severe conditions. In this study, $^{31}P$ solid-state nuclear magnetic resonance (SSNMR) techniques and differential scanning calorimetry (DSC) were used to see any changes in the line shapes of $^{31}P$ NMR spectra of multilamellar vesicles (MLVs) samples of POPC and in the phase change temperature of multilamellar vesicles (MLVs) of DPPC in DSC thermogram with or without any residual solvents. The thermodynamic parameters associated with the solvents did exhibit noticeable changes depending on solvent types. Thus, it is concluded that solvents should be carefully chosen and removed completely and experimental results should also be interpreted with caution particularly for the experiments investigating lipid phase changes and related topics.

Sorption behavior of slightly reduced, three-dimensionally macroporous graphene oxides for physical loading of oils and organic solvents

  • Park, Ho Seok;Kang, Sung Oong
    • Carbon letters
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    • v.18
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    • pp.24-29
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    • 2016
  • High pollutant-loading capacities (up to 319 times its own weight) are achieved by three-dimensional (3D) macroporous, slightly reduced graphene oxide (srGO) sorbents, which are prepared through ice-templating and consecutive thermal reduction. The reduction of the srGO is readily controlled by heating time under a mild condition (at 1 10−2 Torr and 200℃). The saturated sorption capacity of the hydrophilic srGO sorbent (thermally reduced for 1 h) could not be improved further even though the samples were reduced for 10 h to achieve the hydrophobic surface. The large meso- and macroporosity of the srGO sorbent, which is achieved by removing the residual water and the hydroxyl groups, is crucial for achieving the enhanced capacity. In particular, a systematic study on absorption parameters indicates that the open porosity of the 3D srGO sorbents significantly contributes to the physical loading of oils and organic solvents on the hydrophilic surface. Therefore, this study provides insight into the absorption behavior of highly macroporous graphene-based macrostructures and hence paves the way to development of promising next-generation sorbents for removal of oils and organic solvent pollutants.

A Study on the Extraction of Monasil PCA using Liquid CO2 (액체 이산화탄소 이용한 Monasil PCA 추출에 대한 연구)

  • Cho, Dong Woo;Oh, Kyoung Shil;Bae, Won;Kim, Hwayong;Lee, Kab-Soo
    • Korean Chemical Engineering Research
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    • v.50 no.4
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    • pp.684-689
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    • 2012
  • 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.

Investigation of Nonylphenols Contamination in Solvents and Solid-phase Extraction Cartridge, and its Removal Protocols (정밀분석용 용매 및 SPE의 Nonylphenols 오염평가 및 제거)

  • Park, Jong-Min;Choi, Geun-Hyonng;Kim, Jung-Im;Hong, Su-Myeong;Kwon, Oh-Kyung;Im, Geon-Jae;Kim, Jin-Hyo
    • The Korean Journal of Pesticide Science
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    • v.15 no.1
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    • pp.22-27
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    • 2011
  • Nonylphenols are toxic compounds classified as endocrine disruptors. We investigated the nonylphenols clean-up procedures for the contamination control in the quantitative analysis. In this research we analyzed the residual nonylphenols in the solvent and the SPE cartridges. First, at the analysis of HPLC grade solvents (n-hexane, diethyl ether, ethyl acetate and its mixture), diethyl ether was confirmed the residue as 0.963 ${\mu}g/mL$, and we eliminated the contaminant through the distillation with $CaH_2$, Second, at the analysis of SPE cartridges (silica gel and Florisil), all products were showed the residue at 0.046~13.0 ${\mu}g/mL$, but unfortunately the residue in the cartridge were not easily removed with referenced methods in all tested SPE cartridges except in silica gel SPE cartridge with glass ware.

A Study on Development of Alternative Non-aqueous Cleaning Agents to Ozone Depletion Substances and its Field Application (오존파괴물질 대체 비수계세정제 개발 및 현장 적용 연구)

  • Park, Yong-Bae;Bae, Jae-Heum;Lee, Min-Jae;Lee, Jong-Gi;Lee, Ho-Yeoul;Bae, Soo-Jung;Lee, Dong-Kee
    • Clean Technology
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    • v.17 no.4
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    • pp.306-313
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    • 2011
  • Flux or solder is used in soldering process for manufacturing electronic parts such as printed circuit boards (PCB). After soldering process, residual flux and solder paste on the parts should be removed since their residuals could cause performance degradation or failure of parts due to their corrosion and electric leakage. Ozone depletion substances such as 1,1,1- trichloroethane (TCE) and HCFC-141b have widely been using for removal of residual flux and solder paste after soldering process In manufacturing of electronic parts until now. In this study, non-aqueous cleaning agents without flash point were developed and applied to industrial field for replacement of cleaning agents with ozone depletion. In order to develop non-aqueous cleaning agents without ethers, esters, fluoride- type solvents. And their physical properties and cleaning abilities were evaluated, and they were applied to industrial fields for cleaning of flux and solder on the PCB. And vacuum distillation apparatus were operated to determine their operating conditions and recycling yields for recycling of used cleaning agents formulated in this study. As a result of physical properties measurement of our formulated cleaning agents, they were expected to have good wetting and penetrating power since their surface tensions were relatively low as 18.0~20.4 dyne/$cm^2$ and their wetting indices are relatively large. And some cleaning agents holding fluoride-type solvents as their components did not have any flash point and they seemed to be safe in their handling and storage. The cleaning experimental results showed that some cleaning agents were better in their cleaning of flux and solder paste than 1,1,1-TCE and HCFC-141b. And industrial application results of the formulated cleaning agents for cleaning PCB indicated that they can be applicable to industry due to their good cleaning capability in comparison with HCFC-141b. The recycling experiments of the used formulated cleaning agents through a vacuum distillation apparatus also showed that their 91.9~97.5% could be recycled with its proper operating conditions.

Variation of Pesticide Residues in Strawberries by Washing and Boiling Processes (딸기의 세척 및 가공 과정에 따른 농약 잔류량 변화)

  • Kwak, Se-Yeon;Lee, Sang-Hyeob;Jeong, Hye-Rin;Nam, Ae-Ji;Sarker, Aniruddha;Kim, Hyo-Young;Lim, Chae-Uk;Cho, Hyun-Jeong;Kim, Jang-Eok
    • Korean Journal of Environmental Agriculture
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    • v.38 no.4
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    • pp.281-290
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    • 2019
  • BACKGROUND: As the demand for strawberries increases, people are paying attention to food safety in strawberry, especially pesticide residues. To remove the pesticides from strawberry, various washing and processing technique in households are additionally required. METHODS AND RESULTS: Strawberries were washed with water, detergent, alcohol, and ultrasonication and processed to strawberry jam. The mean reduction efficiency according to the washing solvent and method was found to be higher in the order of detergent (42.5%) > alcohol (41.7%) > water (41.3%) > ultrasoniation with alcohol (40.2%) > ultrasoniation with water (38.6%) > ultrasoniation with detergent (36.9%), but there was no significant difference among the treatments. The residue levels of pesticides during processing to jam decreased by 11.9-94.4% for etoxazole, fluopyram, procymidone, spiromesifen, and prochloraz, while the other pesticides were concentrated by boiling, or rather increased by 11.8-40.2%. However, when the residue levels were converted to residual amounts in consideration of the change in weight after processing, the residual amounts of the tested pesticides were reduced by 59.8-98.4% during processing. The processing factor (PF) were different for each pesticide, but PFs were < 1 for all washing solvents and methods, and 0.06-1.40 when processed into jam. CONCLUSION: To ensure the consumption of pesticide-free strawberry, the most efficient washing method is to immerse the strawberry in fresh water for few minutes, followed by rinsing them under running water.