• Title/Summary/Keyword: Fluorination

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Characterization of $YBa_2Cu_3O_{7-x}F_y$ Superconducting Materials Made by a Sol-Gel Process (졸-겔법으로 제조한 $YBa_2Cu_3O_{7-x}F_y$ 초전도물질의 특성분석)

  • 김봉흡;강형부;김현택
    • The Transactions of the Korean Institute of Electrical Engineers
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    • v.41 no.5
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    • pp.525-532
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    • 1992
  • Fluorine-doped YBaS12TCuS13TOS17-xTFS1yT superconducting materials with y varing two orders of magnitude form 0.02 to 2.0 have been prepared by a sol-gel process by using metal nitrate salts, sodium hydroxide and sodium fluoride. Fluorine contents have been measured using an ion-selective electrode. All fluorine doped as reactant were found to be present in the resulted samples. From the observation of XRD it has been concluded that the samples with y 0.2 formed simply the single phase of perovskite structure, whereas those with y 0.5 yielded together some compounds such as BaFS12T, YFS13T and CuO in the resulted samples. The observation of solid state S019TF NMR has been carried out in order to check whether fluorine was actually incorporated into the lattice sites, and the experimental results revealed that the mole ratio of fluorine incorporated into the lattice sites of YBaS12TCuS13TOS17-xT was approximately 0.2 per mole of the compound. Also electrical resistivity measurement indicated that onset transition temperature has the tendency to increase slightly with increasing y in the dilute region as y 0.2.

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A Study on Surface Etching of Metallic Co and Mo in R.F. Plasma (RF 플라즈마를 이용한 금속 코발트와 몰리브데늄의 표면 식각 연구)

  • 서용대;김용수;정종헌;오원진
    • Journal of the Korean institute of surface engineering
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    • v.34 no.1
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    • pp.10-16
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    • 2001
  • Recently plasma etching research has been focused on the metal surfaces in the nuclear industry. In this study, surface etching reaction of metallic Co and Mo, principal contaminants in the spent nuclear components, in CF$_4$/O$_2$, gas plasma has been experimentally investigated to look into the applicability and the effectiveness of the technique for the surface decontamination. Experimental variables are $CF_4$/$O_2$ ratio and substrate temperature between 29$0^{\circ}C$ and 38$0^{\circ}C$. Experimental results Show that the optimum gas composition is 80%CF$_4$-20%$O_2$ and the metallic Co and Mo are etched out well enough in the temperatures range. Cobalt starts to be etched above $350^{\circ}C$ and the etching rate increases with increasing substrate temperature. Maximum rate achieved at 38$0^{\circ}C$ under 220 W r.f. plasma power is 0.06 $\mu\textrm{m}$/min. On the other hand, the metallic Mo is etched easily even at low temperature and the reaction rate drastically increases as the substrate temperature goes up. Highest rate obtained under the same conditions is $1.9\mu\textrm{m}$/min. OES (Optical Emission Spectroscopy) analysis reveals that the intensities of F atom and CO molecule reach maximum at the optimum gas composition, which demonstrates that the principal reaction mechanism is fluorination and/or carbonyl reaction. It is confirmed, therefore, that dry processing technique using reactive plasma is quite feasible and applicable for the decontamination of surface-contaminated parts or equipments.

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Synthesis of a Dopamine Transporter Imaging Agent, N-(3-[$^{18}F$]fluoropropyl)-$2{\beta}$-carbomethoxy-$3{\beta}$-(4-iodophenyl)nortropane (도파민운반체 방사성추적자 N-(3-[$^{18}F$Fluoropropyl)-$2{\beta}$-carbomethoxy-$3{\beta}$-(4-iodophenyl)nortropane의 합성)

  • Choe, Yearn-Seong;Oh, Seung-Jun;Chi, Dae-Yoon;Kim, Sang-Eun;Choi, Yong;Lee, Kyung-Han;Kim, Byung-Tae
    • The Korean Journal of Nuclear Medicine
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    • v.33 no.3
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    • pp.298-305
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    • 1999
  • Purpose: N-(3-[$^{18}F$]Fluoropropyl)-$2{\beta}$-carbomethoxy-$3{\beta}$-(4-iodophenyl)nortropane [$^{18}F$]FP-CIT) has been shown to be very useful for imaging the dopamine transporter. However, synthesis of this radiotracer is somewhat troublesome. In this study, we used a new method for the preparation of [$^{18}F$]FP-CIT to increase radiochemical yield and effective specific activity. Materials and Methods: [$^{18}F$]FP-CIT was prepared by N-alkylation of nor-${\beta}$-CIT (2 mg) with 3-bromo-1-[$^{18}F$]fluoropropane in the presence of $Et_3N$ (5-6 drops of $DMF/CH_3CN$, $140^{\circ}C$, 20 min). 3-Bromo-1-[$^{18}F$]fluoropropane was synthesized from $5{\mu}L$ of 3-bromo-1-trifluoromethanesulfonyloxypropane (3-bromopropyl-1-triflate) and $nBu_4N^{18}F$ at $80^{\circ}C$. The final compound was purified by reverse phase HPLC and formulated in 13% ethanol in saline. Results: 3-Bromo-1-[$^{18}F$]fluoropropane was obtained from 3-bromopropyl-1-triflate and $nBu_4N^{18}F$ in 77-80% yield. N-Alkylation of nor-${\beta}$-CIT with 3-bromo-1-[$^{18}F$]fluoropropane was carried out at $140^{\circ}C$ using acetonitrile containing a small volume of DMF as the solvents. The overall yield of [$^{18}F$]FP-CIT was 5-10% (decay-corrected) with a radiochemical purity higher than 99% and effective specific activity higher than the one reported in the literature based on their HPLC data. The final [$^{18}F$]FP-CIT solution had the optimal pH (7.0) and it was pyrogen-free. Conclusion: In this study, 3-bromopropyl-1-triflate was used as the precursor for the [$^{18}F$]fluorination reaction and new conditions were developed for purification of [$^{18}F$]FP-CIT by HPLC. We established this new method for the preparation of [$^{18}F$]FP-CIT, which gave high effective specific activity and relatively good yield.

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Effect of Fluorination of Carbon Nanotubes on Physico-chemical and EMI Shielding Properties of Polymer Composites (고분자 복합재의 물리화학적 및 전자파차폐 특성에 미치는 탄소나노튜브의 불소화 영향)

  • Lee, Si-Eun;Kim, Doyoung;Lee, Man Young;Lee, Min-Kyung;Jeong, Euigyung;Lee, Young-Seak
    • Polymer(Korea)
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    • v.39 no.1
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    • pp.114-121
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    • 2015
  • Mutli-walled carbon nanotubes (MWCNTs) were surface-modified by a hydrofluoric acid solution to remove impurities and improve interfacial bonding and dispersion of nanotubes in an epoxy matrix. The crystallinity on the surface of treated MWCNTs was investigated by X-ray photoelectron spectroscopy and Raman spectroscopy. The mechanical properties were characterized by tensile test, and the enhancement of mechanical properties of the modified MWCNTs/epoxy composites was indicated by a 33% increase in tensile strength. The electromagnetic interference shielding effectiveness (EMI-SE) of modified MWCNTs/epoxy composites was improved with an increase in concentration of hydrofluoric solution, and EMI-SE showed the maximum increase with 25% HF. However, mechanical and EMI-SE properties didn't show further increase with over 50% HF concentration because the properties of MWCNTs were influenced by degradation of crystallinity and intrinsic properties of MWCNTs. The mechanical and electrical property enhancements of the polymer composites are attributed to the modification of MWCNTs which improve crystallinity of MWCNTs and dispersion in the epoxy resin.

A Study on Plasma Etching Reaction of Cobalt for Metallic Surface Decontamination (금속 표면 제염을 위한 코발트의 플라즈마 식각 반응 연구)

  • Jeon, Sang-Hwan;Kim, Yong-Soo
    • Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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    • v.6 no.1
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    • pp.17-23
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    • 2008
  • In this study, plasma processing of metal surface is experimentally investigated to enhance the surface decontamination efficiency and to find out the reaction mechanism. Cobalt, the major contaminant in the nuclear facilities, and three fluorine-containing gases, $CF_4/O_2$, $SF_6/O_2$, and $NF_3$ are chosen for the investigation. Thin metallic disk specimens are prepared and their surface etching reactions with the three plasma gases are examined. Results show that the maximum etching rate of $17.2\;{\mu}m/min.$ is obtained with NF3 gas at $420^{\circ}C$, while with $CF_4/O_2$, $SF_6/O_2$ gas plasmas those of $2.56\;{\mu}m/min.$ and $1.14\;{\mu}m/min.$ are obtained, respectively. Along with etching experiments, constituent elements of the reaction products are identified to be cobalt, oxygen, and fluorine by AES (Auger Electron Spectroscopy) analysis. It turns out that the oxygen atoms are physically adsorbed ones to the surface from the ambient not participation ones during the analysis after reaction, which supports that the surface reaction of cobalt is mainly to be a fluorination reaction.

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Fluorination of Polymethylmethacrylate (PMMA) Film and Its Surface Characterization (폴리메틸메타아크릴레이트(PMMA) 필름의 불소화 및 그 표면특성)

  • Jung, Min-Jung;Lim, Jae-Won;Park, In-Jun;Lee, Young-Seak
    • Applied Chemistry for Engineering
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    • v.21 no.3
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    • pp.317-322
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    • 2010
  • In this study, poly(methyl methacrylate) (PMMA) was treated with changing mixing ratios of $F_2$ and $O_2$ using oxyfluorination method for hydrophilic modification of PMMA film. For the characterizations of oxyfluorinated PMMA surface, contact angle, surface free energy, X-ray photoelectron spectroscopy (XPS) and optical transmittance (UV-vis) were carried out. After the oxyfluorination, PMMA surface became more hydrophilic showing the decrease of water contact angle from $69^{\circ}$ to $44^{\circ}$. So, surface free energy of oxyfluorinated PMMA film was increased from 46 to $58\;mN\;m^{-1}$. These results are attributed to hydrophilic functional groups such as hydroxyl group formed oxyfluorination method on the PMMA surface. From XPS results, it was confirmed that O/C concentration ratio on the surface of PMMA was increased, the amount of C-OH bonding which shows hydrophilicity was also largely increased from 6.7 to 24.8% with increasing fluorine partial-pressure via the oxyfluorination, The oxyfluorination conditions, room temperature, 1 bar with one mixture ratio of $F_2$ to $O_2$ had little influence on optical transmittance properties of PMMA film but enhanced its surface hydrophilicity. This result suggests that oxyfluorination method could be useful to change hydrophobic PMMA surface to hydrophilic.

A Study on the Automation and Optimization of 9-(4-[$^{18}F$] Fluoro-3-hydroxymethylbutyl) Guanine Synthesis (9-(4-[$^{18}F$] Fluoro-3-hydroxymethylbutyl) guanine 합성의 자동화와 최적화에 관한 연구)

  • An, Jae-Seok;Hong, Sung-Tack;Kang, Se-Hun;Won, Woo-Jae
    • The Korean Journal of Nuclear Medicine Technology
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    • v.15 no.2
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    • pp.72-75
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    • 2011
  • Purpose: The HSV1-tk reporter gene system is the most widely used system because of its advantage is that it is possible to monitor directly without the introduction of a separate reporter gene in case of HSV1-tk suicide gene therapy. This study was performed to automate 9-(4-[$^{18}F$] Fluoro-3-hydroxymethylbutyl) guanine ([$^{18}F$] FHBG) that are widely used as substrate for the HSV1-tk reporter gene in living organisms with positron emission tomography (PET) and find the optimized conditions of synthesis. Materials and Methods: Fully automated synthesis of [$^{18}F$] FHBG was performed using Explora-RN (CTI, USA) module. We have changed of reaction time (3, 5, 10 min) and temperature (110, 120, $130^{\circ}C$) for the optimized conditions of synthesis. Also we experimented to find the optimal concentration of precursor (5, 7, 10 mg). Results: [$^{18}F$] FHBG was purified by HPLC system and collected at around 10-12 min. Synthesis using Explora-RN module showed a $32.0{\pm}1.2%$ yield of radiochemical (decay corrected), the purity was greater than 98%. And the entire synthesis time was less than 48 min. Temperature of the highest synthesis yield was $130^{\circ}C$, reaction time was 5 minutes and concentration of precursor was 10 mg (recommended volume in manual) (n=36). In contrast to radiochemical yield of precursor 10 mg ($32{\pm}1.2%$), yield of 5 and 7 mg precursor was unstable. Conclusion: Automation of [$^{18}F$] FHBG synthesis at Explora-RN module has been completed. In addition, we were able to obtain optimized reaction time, temperature and concentration of precursor. Therefore this study would be provided more rapid synthesis and higher radiochemical yield.

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Development of Radiosynthetic Methods of 18F-THK5351 for tau PET Imaging (타우 PET영상을 위한 18F-THK5351의 표지방법 개발)

  • Park, Jun-Young;Son, Jeong-Min;Chun, Joong-Hyun
    • The Korean Journal of Nuclear Medicine Technology
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    • v.22 no.1
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    • pp.51-54
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    • 2018
  • Purpose $^{18}F-THK5351$ is the newly developed PET probe for tau imaging in alzheimer's disease. The purpose of study was to establish the automated production of $^{18}F-THK5351$ on a commercial module. Materials and Methods Two different approaches were evaluated for the synthesis of $^{18}F-THK5351$. The first approach (method I) included the nucleophilic $^{18}F$-fluorination of the tosylate precursor, subsequently followed by pre-HPLC purification of crude reaction mixture with SPE cartridge. In the second approach (method II), the crude reaction mixture was directly introduced to a semi-preparative HPLC without SPE purification. The radiosynthesis of $^{18}F-THK5351$ was performed on a commercial GE $TRACERlab^{TM}$ $FX-_{FN}$ module. Quality control of $^{18}F-THK5351$ was carried out to meet the criteria guidelined in USP for PET radiopharmaceuticals. Results The overall radiochemical yield of method I was $23.8{\pm}1.9%$ (n=4) as the decay-corrected yield (end of synthesis, EOS) and the total synthesis time was $75{\pm}3min$. The radiochemical yield of method II was $31.9{\pm}6.7%$ (decay-corrected, n=10) and the total preparation time was $70{\pm}2min$. The radiochemical purity was>98%. Conclusion This study shows that method II provides higher radiochemical yield and shorter production time compared to the pre-SPE purification described in method I. The $^{18}F-THK5351$ synthesis by method II will be ideal for routine clinical application, considering short physical half-life of fluorine-18 ($t_{1/2}=110min$).

Synthesis of Cyclen-Based Copper Complexes as a Potential Estrogen Receptor Ligand (에스트로젠 수용체 리간드로서 사이클렌을 기본 구조로 한 구리 착물의 합성)

  • Park, Jeong-Chan;Pandya, Darpan N.;Jeon, Hak-Rim;Lee, Sang-Woo;Ahn, Byeong-Cheol;Lee, Jae-Tae;Yoo, Jeong-Soo
    • Nuclear Medicine and Molecular Imaging
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    • v.41 no.4
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    • pp.326-334
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    • 2007
  • Purpose: The estrogen receptor (ER), which is over-expressed in ER-positive breast tumors, has been imaged by positron emission tomography (PET) using $[^{18}F]$ labeled estrogen ligands, especially $[^{18}F]FES$. However, $[^{18}F]$ has relatively short-lived half-life ($t_{1/2}$ =1.8 h) and the labeling yield of radio-fluorination is usually low compared with $^{64}Cu\;(t_{1/2}=12.7\;h)$. 1,4,7,10-tetraazacyclododecane (cyclen) is used to form stable metal complexes with copper, indium, gallium, and gadolinium. With these in mind, we prepared cyclen-based Cu complexes which mimic estradiol in aspect of two hydroxyl groups. Materials and Methods: 1.7-Protected cyclen, 1.7-bis (benzyloxycarbonyl)-cyclen was synthesized according to the reported procedure. After introducing two 4-benzyloxybenzyl groups at 4,10-positions, the benzyloxycarbonyl and benzyl groups were removed at the same time by hydrogenation on Pd/C to give 1,7-bis(4-hydroxybenzyl)-1,4,7,10-tetraazacyclododecane (1). Results: The prepared ligand 1 was fully characterized by $^1H,\;^{13}C$ NMR, and mass spectrometer. The synthesized ligand was reacted with copper chloride and copper perchlorate to give copper complexes $[Cu(1)]^{2+}2(CIO_4^-)\;and\;[Cu(1)Cl]^+Cl^-$ which were confirmed by high-resolution mass (FAB). Conclusion: We successfully synthesized a cyclen derivative of which two phenol groups are located on trans position of N-atoms. And, two Cu(ll) complexes of +2 and +1 overall charge, were prepared as a potential PET tracers for ER imaging.

Synthesis and Evaluation of $2-[^{18}F]Fluoro-A85380$, a Radioligand for ${\alpha}_4{\beta}_2$ Nicotinic Acetylcholine Receptor Imaging (${\alpha}_4{\beta}_2$ 니코틴성 아세틸콜린 수용체 영상 방사성리간드 $2-[^{18}F]fluoro-A85380$의 합성 및 평가)

  • Ryu, Eun-Kyoung;Choe, Yearn-Seong;Kim, Sang-Eun;Hwang, Sae-Hwan;Paik, Jin-Young;Choi, Yong;Lee, Kyung-Han;Kim, Byung-Tae
    • The Korean Journal of Nuclear Medicine
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    • v.36 no.4
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    • pp.261-270
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    • 2002
  • Purpose: Nicotinic acetylcholine receptors (nAChRs), which mediate excitatory neurotransmission, are known to participate in various neurophysiological functions. Severe losses of nAChRs have been noted in Alzheimer's and Parkinson's diseases. Therefore, noninvasive and quantitative imaging of nAChRs would offer a better understanding on the function of these receptors. In this study, $2-[^{18}F]fluoro-A85380\;([^{18}F]1)$, an ${\alpha}_4{\beta}_2$ nAChRs radioligand, was prepared using one HPLC purification and evaluated in mouse brain, and the results were compared with those in the literature. Materials and Methods: $[^{18}F]1$ was prepared by $[^{18}F]$fluorination of the iodo precursor followed by acidic deprotection and then purified by HPLC. Tissue distribution studies were performed in mouse brain at the indicated time points and the result was expressed as %ID/g. Inhibition studies were also carried out with pretreatment of various ligands. Results: One HPLC purification method gave the desired product in 15-20% radiochemical yield and with high specific activity ($38-55GBq/{\mu}mol$). Tissue distribution studies showed that $[^{18}F]1$ specifically labeled nAChRs in mouse brain with a high thalamus to cerebellum uptake ratio (13.8 at 90 min). Inhibition studios demonstrated selective binding of $[^{18}F]1$ to nAChRs, blocking the uptake of the $[^{18}F]1$ in nAChR-rich legions by selective ligands such as cytisine and nicotine which are well-known nAChRs agonists. Conclusion: This study demonstrated that the $[^{18}F]1$ produced by the method using one HPLC purification gave the results similar to those reported in the literature. Therefore, this synthetic method can be readily applied to the routine preparation of $[^{18}F]1$, a PET radioligand for ${\alpha}_4{\beta}_2$ nAChRs imaging.