• Title/Summary/Keyword: Residual solvent

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Effect of Thermal Imidization and Curing on Fluorescence Behavior of a Phenylethynyl-Terminated Poly(amic acid)

  • Cho, Donghwan;Yang, Gyeongmo;Drzal, Lawrence T.
    • Macromolecular Research
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    • v.11 no.5
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    • pp.297-302
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    • 2003
  • The imidization and cure reaction of a thermosetting phenylethynyl-terminated amic acid (LaRC PETI-5) in film form have been monitored as a function of temperature by means of a steady-state fluorescence technique using a front-face illumination method. The variation of the fluorescence emission spectra of LaRC PETI-5 can be divided into four temperature regions; Region I: below 15$0^{\circ}C$, Region II: 150-25$0^{\circ}C$, Region III: 250-35$0^{\circ}C$, and Region IV: above 35$0^{\circ}C$. The fluorescence spectra in Region I are largely influenced by residual N-methyl-2pyrrolidinone in the polymer and also slightly by partial imidization of the polymer. There is a combined effect of imidization and solvent removal on the fluorescence behavior in Region II. The spectra in Regions III and IV are due significantly to the cure reaction of LaRC PETI-5 and to a post-cure effect of the polyimide, respectively. This spectroscopic evidence indicating the transformation of the amic acid imide oligomer into the corresponding polyimide via imidization and cure, agrees well with thermal analysis results obtained previously. The intermediate stage of cure in the range of 250-30$0^{\circ}C$ predominantly influences the change of the fluorescence intensity. The later stage above 30$0^{\circ}C$ significantly influences the position of the spectrum. This fluorescence study also supports the mechanism proposed in earlier work that the crosslinking reaction takes place at the reaction sites in the conjugated polyene and the phenylethynyl end group in the polyimide chain.

Preliminary screening to assess the antimicrobial activities of extracts of evergreen woody species from South Korea against Staphylococcus aureus

  • Jang, Bo Kook;Chi, Lai Won;Cho, Ju Sung;Lee, Cheol Hee
    • Journal of Plant Biotechnology
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    • v.47 no.1
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    • pp.90-99
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    • 2020
  • This study aimed to screen for plants with antimicrobial potential among the evergreen woody species of South Korea that are used for horticulture and landscaping and to provide basic information about plants with proven antimicrobial activity to underpin future research. The plant materials were extracted under various conditions, and the antimicrobial activities of the extracts were evaluated by agar diffusion assay. The screening tests demonstrated that the crude extracts of 43 species had inhibitory effects against S. aureus. The inhibitory activities of four species (Elaeocarpus sylvestris, Camellia japonica, Cleyera japonica, and Quercus salicina) were relatively higher than that of the synthetic antimicrobial agents methylparaben and phenoxyethanol. The highest inhibitory activity was observed with the leaf extracts (extracted with methanol for 30 minutes) of E. sylvestris, based on induction of the largest inhibition zone of 23.3 mm in size. In addition, solvent fractions of E. sylvestris were evaluated. The largest inhibitory zone of 23.1 mm was observed for the n-butanol fraction, which is likely to contain effective compounds that exhibit inhibitory activity against S. aureus. In contrast, n-hexane and residual aqueous fractions showed no antimicrobial activity. Overall, our findings confirm that evergreen woody plants native to South Korea have potential antimicrobial activity.

Studies on the Characteristic of Removal Type Pressure-Sensitive Acrylic Adhesives (4원 공중합체 박리형 아크릴 점착제의 특성에 관한 연구)

  • Seo, Young-Ok;Seul, Soo-Duk
    • Journal of Adhesion and Interface
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    • v.1 no.1
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    • pp.15-22
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    • 2000
  • To prepare acrylic type pressure-sensitive adhesive, quarter polymers were synthesized from butylacrylate (BA), 2-ethylhexylacrylate (2-EHA), methyl methacrylate (MMA), 2-hydroxyethylmethacrylate (2-HEMA). The quarter polymer was identified by FT-IR. Molecular weight was measured by Gel Pearmeation Chromatograhy. Also, viscosity, solid content and peel strength were investigated. The peel strength was $160g_f/25mm$ when the volume ratio of feed monomer to solvent was 1.3:1 and the ratio was relevant to commercial usage. The pot life of adhesive was 30 s at the 50 m/min of heat treatment rate, and it indicated that the minimum drying time was 30 s. Not only weathering resistance keep up peel strength $160{\sim}180g_f/25mm$ after 1000 h, but also no residual remains.

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Immobilization of GH78 α-L-Rhamnosidase from Thermotoga petrophilea with High-Temperature-Resistant Magnetic Particles Fe3O4-SiO2-NH2-Cellu-ZIF8 and Its Application in the Production of Prunin Form Naringin

  • Xu, Jin;Shi, Xuejia;Zhang, Xiaomeng;Wang, Zhenzhong;Xiao, Wei;Zhao, Linguo
    • Journal of Microbiology and Biotechnology
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    • v.31 no.3
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    • pp.419-428
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    • 2021
  • To efficiently recycle GH78 thermostable rhamnosidase (TpeRha) and easily separate it from the reaction mixture and furtherly improve the enzyme properties, the magnetic particle Fe3O4-SiO2-NH2-Cellu-ZIF8 (FSNcZ8) was prepared by modifying Fe3O4-NH2 with tetraethyl silicate (TEOS), microcrystalline cellulose and zinc nitrate hexahydrate. FSNcZ8 displayed better magnetic stability and higher-temperature stability than unmodified Fe3O4-NH2 (FN), and it was used to adsorb and immobilize TpeRha from Thermotoga petrophilea 13995. As for properties, FSNcZ8-TpeRha showed optimal reaction temperature and pH of 90℃ and 5.0, while its highest activity approached 714 U/g. In addition, FSNcZ8-TpeRha had better higher-temperature stability than FN. After incubation at 80℃ for 3 h, the residual enzyme activities of FSNcZ8-TpeRha, FN-TpeRha and free enzyme were 93.5%, 63.32%, and 62.77%, respectively. The organic solvent tolerance and the monosaccharides tolerance of FSNcZ8-TpeRha, compared with free TpeRha, were greatly improved. Using naringin (1 mmol/l) as the substrate, the optimal conversion conditions were as follows: FSNcZ8-TpeRha concentration was 6 U/ml; induction temperature was 80℃; the pH was 5.5; induction time was 30 min, and the yield of products was the same as free enzyme. After repeating the reaction 10 times, the conversion of naringin remained above 80%, showing great improvement of the catalytic efficiency and repeated utilization of the immobilized α-L-rhamnosidase.

Synthesis of Carbon Materials from PFO, Byproducts of Naphtha Cracking Process (나프타 분해공정 부산물인 PFO로부터 탄소구조체 합성)

  • Lee, Jiyon;Park, Seung-Kyu
    • Applied Chemistry for Engineering
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    • v.22 no.5
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    • pp.495-500
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    • 2011
  • Separation of naphthalene from pyrolyzed fuel oil, by product of Naphta cracking process (NCC) process, has been accomplished by the solvent extraction, distillation and purification process. The residual pyrolyzed fuel oil (PFO), called precursor of carbon materials, has been calcined at $300{\sim}800^{\circ}C$ in nitrogen gas to raw pitch. After the treatment of PFO by hexane and methanol, either a flake phased carbon at $350^{\circ}C$ or a carbon sphere at above $400^{\circ}C$ forms. As the calcination temperature increases, the shape of raw pitch changes from the flake phase to the sphere one, and the size of them decreases to several ${\mu}m$. Based on the BET and XRD spectrum, the carbon sphere is classified to a mesophase amorphous carbon with a cubic phase.

β-Galactosidase-catalyzed Synthesis of 1, 2-Hexanediol Galactoside and its Purification using Ethyl Acetate Extraction followed by Silica Gel Chromatography (대장균 β-Galactosidse를 이용한 1, 2-Hexanediol galactoside의 합성과 Ethyl Acetate 추출 및 Silica Gel Chromatography를이용한 정제)

  • Kim, Yi-Ok;Jung, Kyung-Hwan
    • Journal of the Korean Applied Science and Technology
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    • v.33 no.3
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    • pp.498-506
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    • 2016
  • 1, 2-Hexanediol galactoside (HD-gal) has been previously synthesized from 1, 2-hexanediol (HD), in which recombinant ${\beta}$-galactosidase (${\beta}$-gal) of Escherichia coli (E. coli) was used for transgalactosylation reaction. In this study, a method for HD-gal purification from the reaction mixture was particularly investigated. Using ${\beta}$-gal-containing E. coli, HD-gal was synthesized from 75 mM HD for 48 hr under 300 g/l lactose concentration. Then, HD-gal synthesis from HD was confirmed by TLC analysis, and the existence of E. coli ${\beta}$-gal during 48 hr-reaction was also confirmed by Western blotting, in which the conversion yield of HD to HD-gal reached about 94% during 48 hr. To establish an efficient method for HD-gal purification, we carried out the solvent extraction of the reaction mixture, followed by silica gel chromatography, particularly in order to remove the residual HD. Two water-immiscible solvents, such as methylene chloride and ethyl acetate, were investigated comparatively to find out appropriate solvent. Then, it was found that residual HD was almost removed when ethyl acetate extraction of water phase of reaction mixture was carried out four times. Subsequently, silica gel chromatography was carried out, and purified HD-gal could be finally obtained. The production yield for HD-gal from 75 mM HD was $8.9{\pm}0.6%$ (n=3) (mole basis) or $21.1{\pm}1.4%$ (n=3) (weight basis). For further study, using purified HD-gal, we will investigate the minimum inhibitory concentrations (MICs) of HD-gal against bacteria. In addition, cytotoxicity to human skin cells of HD-gal will be examined.

Residual Characteristics of Bistrifluron and Chlorantraniliprole in Strawberry (Fragaria ananassa Duch.) for Establishing Pre-Harvest Residue Limit (생산단계 잔류허용기준 설정을 위한 딸기 중 bistrifluron과 chlorantraniliprole의 잔류 특성 연구)

  • Lee, Jae Won;Kim, Ji Yoon;Kim, Hee gon;Hur, Kyung Jin;Kwon, Chan Hyeok;Hur, Jang Hyun
    • Korean Journal of Environmental Agriculture
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    • v.36 no.1
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    • pp.57-62
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    • 2017
  • BACKGROUND: Pesticide residue analysis is essentially required for safety evaluation of agricultural products. Bistrifluron and chlorantraniliprole have been currently considered as potentials to deeply evaluate their residues in agricultural products because they are frequently found in strawberry. This work was performed to investigate the residual patterns of bistrifluron and chlorantraniliprole in strawberry after harvest. METHODS AND RESULTS: Strawberry was treated with bistrifluron and chlorantraniliprole 0, 1, 2, 3, 5, 7 and 10 days before harvest under greenhouse conditions. The strawberry samples were subjected to solvent and solid phase extractions followed by LC-MS/MS analysis. There covery percentages of bistrifluron and chlorantraniliprole for tified in the control samples ranged from approximately 82 to 103% with the method limit of 0.005 mg/kg. The concentrations of bistrifluron and chlorantraniliprole in strawberry samples decreased significantly in 10 days after treatment, giving the safety levels of 0.04 to 0.06 mg/kg at 10 days after application, as considered maximum residue limit. The half-lives of bistrifluron and chlorantraniliprole based on first order kinetics were determined to 6.3 days and 6.4 days, respectively. CONCLUSION: Bistrifluron and chlorantraniliprole are suggested to use in strawberry 10 days before harvest to reach residual safety levels.

Preparation and Characterization of Ipriflavone-Loaded Poly(L-lactide-co-glycolide) Scaffold for Tissue Engineered Bone (조직공학적 골을 위한 애프리플라본을 함유한 다공성 지지체의 제조 및 그 특성)

  • Jang, Ji-Wook;Lee, Bong;Han, Chang-Whan;Lee, Il-Woo;Lee, Hai-Bang;Khang, Gil-Son
    • Polymer(Korea)
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    • v.27 no.3
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    • pp.226-234
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    • 2003
  • Ipriflavone (IP), a non-hormonal isoflavone derivative, has been shown to interfere with bone remodeling by inhibiting bone resorption and stimulating bone formation. IP consistently increased the amount of Ca incorporated into the cell layer by mesenchymal stem cells (MSCs). In this study, we developed the novel IP loaded poly(L-lactide-co-glycolide) (PLGA) scaffolds for the possibility of the application of the tissue engineered bone. IP/PLGA scaffo1ds were prepared by solvent casting/salt leaching method and were characterized by porosimeter, scanning electron microscopy, determination of residual salt amount, differential scanning calorimetry, and X-ray diffractometer, respectively. IP/PLGA scaffolds were implanted into the back of athymic nude mouse to observe the effect of IP on the osteoinduction compared with control PLGA scaffo1ds. Thin sections were cut from paraffin embedded tissues and histological sections were stained H&E, von Kossa, and immunohistochemical staining for Type I collagen and osteocalcin. It can be observed that the porosity was above 91.7% and the pore size was above 101 $\mu\textrm{m}$. Control scaffo1d and IP/PLGA scaffo1ds of 50% IP were implanted on the back of athymic nude mouse to observe the effect of IP on the induction of cells proliferation for 9 weeks. The evidence of calcification, osteoblast, and osteoid from the undifferentiated stem cells in the subcutaneous sites and other soft connective tissue sites having a preponderance of stem cells has been observed. From these results, it seems that IP plays an important role for bone induction in IP/PLCA scaffolds.

Review of root canal irrigant delivery techniques and devices (최신 근관 세척 방법과 기구에 대한 고찰)

  • Yoo, Yeon-Jee;Shin, Su-Jeong;Baek, Seung-Ho
    • Restorative Dentistry and Endodontics
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    • v.36 no.3
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    • pp.180-187
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    • 2011
  • Introduction: Eliminating the residual debris and bacteria in the root canal system is one of the main purposes of the endodontic treatment. However, the complexity on the anatomy of the root canal system makes it difficult to eliminate the bacterial biofilm existing along the root canal surface and necrotic pulp tissue by mechanical instrumentation and chemical irrigation. Recently, more effective irrigant delivery systems for root canal irrigation have been developed. The purpose of this review was to present an overview of root canal irrigant delivery techniques and devices available in endodontics. Review: The contents of this paper include as follows; - syringe-needle irrigation, manual dynamic irrigation, brushes - sonic and ultrasonic irrigation, passive ultrasonic irrigation, rotary brush, RinsEndo, EndoVac, Laser Conclusion: Though technological advances during the last decade have brought to fruition new agitation devices that rely on various mechanisms, there are few evidence based study to correlate the clinical efficacy of these devices with improved outcomes except syringe irrigation with needle and ultrasonic irrigation. The clinicians should try their best efforts to deliver antimicrobial and tissue solvent solutions in predictable volumes safely to working length.

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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