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THE EFFECT OF THERMOCYCLING ON THE DURABILITY OF DENTIN ADHESIVE SYSTEMS (열순환이 상아질 접착제의 결합 내구성에 미치는 영향)

  • Moon, Young-Hoon;Kim, Jong-Ryul;Choi, Kyung-Kyu;Park, Sang-Jin
    • Restorative Dentistry and Endodontics
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    • v.32 no.3
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    • pp.222-235
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    • 2007
  • The objectives of this study was to evaluate the effect of thermocycling on the ${\mu}TBS$ (microtensile bond strength) to dentin with four different adhesive systems to examine the bonding durability. Freshly extracted $3^{rd}$ molar teeth were exposed occlusal dentin surfaces, and randomly distributed into 8 adhesive groups 3-steps total-etching (Scotchbond Multi-Purpose Plus; SM, All Bond-2; AB), 2-steps total-etching (Single Bond; SB, One Step plus; OS), 2-steps self-etching (Clearfil SE Bond; SE, AdheSE AD) and single-step self-etching systems (Promp L-Pop; PL, Xeno III; XE) Each adhesive system in 8 adhesives groups was applied on prepared dentin surface as an instruction and resin composite (Z250) was placed incrementally and light-cured. The bonded specimens were sectioned with low-speed diamond saw to obtain $1\times1mm$ sticks after 24 hours of storage at $37^{\circ}C$ distilled water and proceeded thermocycling at the pre-determined cycles of 0, 1,000 and 2,000. The ${\mu}TBS$ test was carried out with EZ-tester at 1mm/min. The results of bond strength test were statistically analyzed using one-way ANOVA/ Duncan's test at the a < 0.05 confidence level. Also, the fracture mode of debonded surface and the interface were examined under SEM. The results of this study were as follows ; 1. 3-step total etching adhesives showed stable, but bond strength of 2-step adhesives were decreased as thermocycling stress. 2. SE showed the highest bond strength, but single step adhesives (PL, XE) had the lowest value both before and after thermocycling. 3 Most of adhesives showed adhesive failure. The total-etching systems were prone to adhesive failure and the single-step systems were mixed failure after thermocycling. Within limited results of this study, the bond strength of adhesive system was material specific and the bonding durability was affected by the bonding step/ procedure of adhesive Simplified bonding procedures do not necessarily imply improved bonding performance.

Study of Polysulfone Membrane for Membrane-covered Oxygen Probe System (산소 전극 시스템에 사용되는 polysulfone막에 대한 연구)

  • Hong, Suk In;Kim, Hyun Joon;Park, Hee Young;Kim, Tae Jin;Jeong, Yong Seob
    • Applied Chemistry for Engineering
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    • v.7 no.5
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    • pp.877-887
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    • 1996
  • The ideal membranes for membrane-covered oxygen probes system should be selectively permeable for oxygen and chemically inert, and have good mechanical strength. Polysulfone(PSf) was selected to develop the membrane for membrane-covered oxygen electrodes system. PSf membranes have properties such as good reproducibility, good mechanical strength, chemical inertness, and high heat resistance. PSf membranes were cast from polymer solution on the glass plate at constant temperature, and casting solvents used were tetrahydrofuran(THF), methylene chloride, and N-methyl-2-pyrrolidone(NMP). Tricresyl phosphate(TCP) as plasicizer was added to PSf to increase the softness of membrane. The permeation characteristics were observed for pure oxygen and nitrogen through pure PSf membranes by variable volume method and membrane-covered electrode system. The permeability coefficients of oxygen and nitrogen measured by variable volume method were slightly decreased with increasing of upstream pressure. The permeation properties of PSf membrane using methylene choride as casting solvent were not affected by the PSf amount of polymer solution. The permeability coefficients of oxygen and nitrogen for PSf membrane containing TCP were very slightly lower than those for pure PSf membrane, but ideal separation factors were slightly higher. The flexibility of PSf membrane containing 2wt% TCP was better than that of pure PSf membrane. It was expected that this increase in flexibility would solve the difficulty of fixing the membrane to the cathode. The membrane-covered oxygen probes system was composed of anode, cathode and electrolyte. The type of the anode was Ag/AgCl half-cell, that of cathode was Ag, and the electrolyte was 4N KCl solution. The result of sampled current voltametry for PSf membrane showed the plateu region at -0.3V~-1.0V. The correlation coefficient of oxygen partial pressure versus current for PSf membrane was relatively high, 0.99949. It was concluded that PSf membrane was the good candidate for the membrane-covered oxygen probes system.

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Structural Behavior of Mixed $LiMn_2O_4-LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ Cathode in Li-ion Cells during Electrochemical Cycling

  • Yun, Won-Seop;Lee, Sang-U
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.05a
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    • pp.5-5
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    • 2011
  • The research and development of hybrid electric vehicle (HEV), plug-in hybrid electric vehicle (PHEV) and electric vehicle (EV) are intensified due to the energy crisis and environmental concerns. In order to meet the challenging requirements of powering HEV, PHEV and EV, the current lithium battery technology needs to be significantly improved in terms of the cost, safety, power and energy density, as well as the calendar and cycle life. One new technology being developed is the utilization of composite cathode by mixing two different types of insertion compounds [e.g., spinel $LiMn_2O_4$ and layered $LiMO_2$ (M=Ni, Co, and Mn)]. Recently, some studies on mixing two different types of cathode materials to make a composite cathode have been reported, which were aimed at reducing cost and improving self-discharge. Numata et al. reported that when stored in a sealed can together with electrolyte at $80^{\circ}C$ for 10 days, the concentrations of both HF and $Mn^{2+}$ were lower in the can containing $LiMn_2O_4$ blended with $LiNi_{0.8}Co_{0.2}O_2$ than that containing $LiMn_2O_4$ only. That reports clearly showed that this blending technique can prevent the decline in capacity caused by cycling or storage at elevated temperatures. However, not much work has been reported on the charge-discharge characteristics and related structural phase transitions for these composite cathodes. In this presentation, we will report our in situ x-ray diffraction studies on this mixed composite cathode material during charge-discharge cycling. The mixed cathodes were incorporated into in situ XRD cells with a Li foil anode, a Celgard separator, and a 1M $LiPF_6$ electrolyte in a 1 : 1 EC : DMC solvent (LP 30 from EM Industries, Inc.). For in situ XRD cell, Mylar windows were used as has been described in detail elsewhere. All of these in situ XRD spectra were collected on beam line X18A at National Synchrotron Light Source (NSLS) at Brookhaven National Laboratory using two different detectors. One is a conventional scintillation detector with data collection at 0.02 degree in two theta angle for each step. The other is a wide angle position sensitive detector (PSD). The wavelengths used were 1.1950 ${\AA}$ for the scintillation detector and 0.9999 A for the PSD. The newly installed PSD at beam line X18A of NSLS can collect XRD patterns as short as a few minutes covering $90^{\circ}$ of two theta angles simultaneously with good signal to noise ratio. It significantly reduced the data collection time for each scan, giving us a great advantage in studying the phase transition in real time. The two theta angles of all the XRD spectra presented in this paper have been recalculated and converted to corresponding angles for ${\lambda}=1.54\;{\AA}$, which is the wavelength of conventional x-ray tube source with Cu-$k{\alpha}$ radiation, for easy comparison with data in other literatures. The structural changes of the composite cathode made by mixing spinel $LiMn_2O_4$ and layered $Li-Ni_{1/3}Co_{1/3}Mn_{1/3}O_2$ in 1 : 1 wt% in both Li-half and Li-ion cells during charge/discharge are studied by in situ XRD. During the first charge up to ~5.2 V vs. $Li/Li^+$, the in situ XRD spectra for the composite cathode in the Li-half cell track the structural changes of each component. At the early stage of charge, the lithium extraction takes place in the $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ component only. When the cell voltage reaches at ~4.0 V vs. $Li/Li^+$, lithium extraction from the spinel $LiMn_2O_4$ component starts and becomes the major contributor for the cell capacity due to the higher rate capability of $LiMn_2O_4$. When the voltage passed 4.3 V, the major structural changes are from the $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ component, while the $LiMn_2O_4$ component is almost unchanged. In the Li-ion cell using a MCMB anode and a composite cathode cycled between 2.5 V and 4.2 V, the structural changes are dominated by the spinel $LiMn_2O_4$ component, with much less changes in the layered $LiNi_{1/3}Co_{1/3}Mn_{1/3}O_2$ component, comparing with the Li-half cell results. These results give us valuable information about the structural changes relating to the contributions of each individual component to the cell capacity at certain charge/discharge state, which are helpful in designing and optimizing the composite cathode using spinel- and layered-type materials for Li-ion battery research. More detailed discussion will be presented at the meeting.

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Fate of the herbicide bensulfuron-methyl in a soil/rice plant microecosystem (벼 재배 microecosystem 내에서 제초제 bensulfuron-methyl의 행적)

  • Lee, Jae-Koo;Fuhr, F.;Kwon, Jeong-Wook;Ahn, Ki-Chang;Park, Ju-Hyoung;Lee, Yong-Pil
    • The Korean Journal of Pesticide Science
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    • v.8 no.4
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    • pp.299-308
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    • 2004
  • In order to elucidate the behavior of bensulfuron-methyl, a sulfonylurea herbicide, in a soil/plant microecosystem, rice plants (Oryza sativa L.) were grown for 12 weeks in the specially made stainless steel pots (17cm I.D. $\times$ 10cm H.) containing two different paddy soils treated with fresh and 13-week-aged residues of [phenyl-$^{14}C$]bensulfuron-methyl, respectively. During the aging period, the mineralization to $^{14}CO_2$ from soil A (OM, 3.59%; CEC, 7.65 $cmol^+\;kg^{-1}$; texture, sandy clay loam) and B (OM, 1.62%; CEC, 4.51 $cmol^+\;kg^{-1}$; texture, sandy loam) amounted to 6.79 and 10.15% of the originally applied $[^{14}C]$bensulfuron-methyl, respectively. The amounts of $^{14}CO_2$ evolved from the soils with fresh residues were higher than those from the soils with aged residues. At harvest after 12-week growing, $^{14}C$-radioactivity absorbed and translocated into rice plants from soils A and B containing fresh residues of bensulfuron-methyl was 1.53 and 4.40%, while 4.04 and 6.37% in the two soils containing aged residues, respectively. Irrespective of aging and soil type, the $^{14}C$-radioactivity remaining in soil ranged from 80.41 to 98.87% of the originally applied $[^{14}C]$bensulfuron-methyl. The solvent extractability of tile soils was $39.25\sim70.39%$, showing the big differences among the treatments. Most of the nonextractable soil-bound residues of $[^{14}C]$bensulfuron-methyl were incorporated into the fulvic acid fraction$(61.32\sim76.45%)$. Comparing the microbial activity of the soils with rice plants grown with that of the soils without them, the former was $1.6\sim3.0$ times higher than the latter. However, it did not correlate with the $^{14}CO_2$ evolution.

Effect of 2-D DBP/PLGA Hybrid Films on Attachment and Proliferation of Intervertebral Disc Cells (2차원적 DBP/PLGA 하이브리드 필름이 디스크 세포의 부착과 증식에 미치는 영향)

  • Ko, Youn-Kyung;Jeong, Jae-Soo;Kim, Soon-Hee;Lim, Ji-Ye;Rhee, John-M.;Kim, Moon-Suk;Lee, Hai-Bang;Khang, Gil-Son
    • Polymer(Korea)
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    • v.32 no.2
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    • pp.109-115
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    • 2008
  • Because demineralized bone particle (DBP) contains various bioactive molecules such as cytokines, it is widely used biomaterials in the field of tissue engineering. In this study, we investigated the effect of 2-dimensional DBP/PLGA hybrid films on adhesion, proliferation and phenotype maintenance of intervertebral disc cells. PLGA films incorporated with different amount (0, 10, 20, 40 and 80 wt%) of DBP were prepared by the solvent evaporation method and characterized by scanning election microscopy (SEM). PLGA film has a flat and smooth surface. According to the increase of content of DBP, the surface of DBP/PLGA film exhibited few agglomerates and increased the roughness of the surface. Annulus fibrosus (AF) and nucleus pulposus (NP) cells were cultured on PLGA and DBP/PLGA film surface, and then examined the cell adhesion and proliferation by the cell count and SEM observation. The result of cell count and SEM observation revealed that 10 and 20% DBP in DBP/PLGA films were superior to adhesion and proliferation of both AF and NP cells. We confirmed that specific gene expression of disc cells on DBP/PLGA film based on the cell count result. Disc cells seeded on 20% DBP/PLGA film expressed the gene of type I and II collagen continuously. Therefore, pertinent content of biomaterials could provide more appropriate condition on adhesion and proliferation of cell. And this results may be used as a basic data for the intervertebral disc regeneration using tissue engineering.

Evaluation of Denitrification Reactivity by the Supported Nanoscale Zero-Valent Iron Prepared in Ethanol-Water Solution (이중용매에서 제조된 나노영가철을 이용한 질산성질소의 환원반응성 평가)

  • Park, Heesu;Park, Yong-Min;Oh, Soo-Kyeong;Lee, Seong-Jae;Choi, Yong-Su;Lee, Sang-Hyup
    • Korean Chemical Engineering Research
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    • v.46 no.5
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    • pp.1008-1012
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    • 2008
  • Nanoscale zero-valent iron(nZVI) is famous for its high reactivity originated from its high surface area and it has received considerable attentions as one of the latest innovative technologies for treating contaminated groundwater. Due to its fine powdery form, nZVI has limited filed applications. The efforts to overcome this shortcoming by immobilizing nZVI on a supporting material have been made. This study investigated the differences of resin-supported nZVI's characteristics by changing the preparation methods and evaluated its reactivity. The borohydride reduction of an iron salt was proceeded in ethanol/water solvent containing a dispersant and the synthesis was conducted in the presence of ion-exchange resin. The resulting material was compared to that prepared in a conventional way of using de-ionized water by measuring the phyrical and chemical characteristics. BET surface area and Fe content of nZVI-attached resin was increased from $31.63m^2/g$ and 18.19 mg Fe/g to $38.10m^2/g$ and 22.44 mg Fe/g, respectively, by switching the solution medium from water to ethanol/water with a dispersant. The reactivity of each material was tested using nitrate solution without pH control. The pseudo first-order constant of $0.462h^{-1}$ suggested the reactivity of resin-supported nZVI prepared in ethanol/water was increased 61 % compared to that of the conventional type of supported nZVI. The specific reaction rate constant based on surface area was also increased. The results suggest that this new supported nZVI can be used successfully in on-site remediation for contaminated groundwater.

Experiments on Flow Characteristics of Asphalt Seal Composite Waterproofing Method for Underground Concrete Structure Exterior Wall Waterproofing (지하 콘크리트 구조물 외벽 방수용 아스팔트 씰재 복합방수 공법의 흘러내림 특성에 관한 실험)

  • Ko, Sang-Ung;Kim, Kyoung-Hoon;Kim, Young-Sam;Shin, Hong-Chul;Kim, Jin-Man
    • Journal of the Korean Recycled Construction Resources Institute
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    • v.6 no.4
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    • pp.297-303
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    • 2018
  • With the changing trend of the building construction to high rising and large scaling, the underground structure has been increased, and its usage also increased and variety. Hence, to protect the underground structure against underground water, various water proofing methods has been developed. Among the many water proofing methods, the combined water proofing method using both asphalt seal and sheet has been widely used to secure the sufficient performance and decrease the construction failure. However, during the summer period of extremely high temperature conditions, the asphalt sealing materials were separated and leaked into the structure. Therefore, the aim of the research is to provide the quality standard of asphalt sealing material based on the various temperature changes depending on seasons. According to the experimental results, the temperature of the sealing materials applied on the slab was increased up to $54^{\circ}C$ which was $3^{\circ}C$ higher than the structure temperature of $51^{\circ}C$. Based on the melting test for asphalt sealing materials applied on the outside wall of the structure, in the case of water-dispersing typed materials showed significant melting down due to its slow evaporation and low viscosity. Furthermore, from the accelerated test conducted indoor conditions, a solvent-type and water-dispersing typed materials showed significant melting down due to their low viscosity and melting point in ambient conditions. Based on these results, viscosity and melting point are found as the important factors on asphalt sealing materials' quality, and it is necessary to designate the quantitative level of the viscosity and melting point for quality control.

tans-Resveratrol Content of Varieties and Growth Period in Peanut (땅콩 품종 및 생육기별 trans-Resveratrol 함량)

  • Lee, Mi-Ja;Cheong, Young-Keun;Kim, Hyung-Soon;Park, Ki-Hun;Doo, Hong-Soo;Suh, Duck-Yong
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.48 no.6
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    • pp.429-433
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    • 2003
  • trans-Resveratrol(3,5,4'-trihydroxystilbene) is phenolic compound present in grapes, wines, and peanuts, has been reported to have health benefits including anticarcinogenic effects, protection against cardiovascular diseases and reduced cancer risk. A simple method for the quantitative extraction of trans-resveratrol from peanut has been developed. Optimal conditions for extraction were investigated. Type of solvent, time, and temperature assayed influenced trans-resveratrol yield. Adequate extraction condition was decided to ethanol/water (80:20v/v) maintained at $25^{\circ}C$ for 45 min. After extraction, the protocol consists of sample preparation using a $\textrm{C}_{18}$ solid-phase extraction (SPE) cartridge after concentrate with rotary evaporator and quantified by reversed phase HPLC using a $\textrm{C}_{18}$ column at 308 nm. Analytical methods for measuring trans-resveratrol in peanut were adapted to isolate, identify, and quantify trans-resveratrol in 11 peanut varieties by HPLC (high-performance liquid chromatography) with UV detector, The 11 peanut varieties content ranged from 0.018 to 1.125 $\mu\textrm{g}/\textrm{g}$ with an average of 0.289 $\mu\textrm{g}/\textrm{g}$. The contents were higher in the seeds with than without testa, regardless of varieties. The trans-resveratrol content was Higher in 110, 130 days after sowing than that of other period.

Solution Phase Photolyses of Substituted Diphenyl Ether Herbicides under Simulated Environmental Conditions (모조(模造) 환경조건하(環境條件下)에서의 치환(置換) Diphenyl Ether 제초제(除草劑)의 광분해(光分解)에 관(關)한 연구(硏究))

  • Lee, Jae-Koo
    • Applied Biological Chemistry
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    • v.17 no.3
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    • pp.149-176
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    • 1974
  • Eight substituted diphenyl ether herbicides and some of their photoproducts were studied in terms of solution phase photolysis under simulated environmental conditions by using a Rayonet photochemical reactor. The test compounds absorbed sufficient light energy at the wavelength of 300 nm to undergo various photoreactions. All the photoproducts were confirmed by means of tlc, glc, ir, ms, and/or nmr spectrometry. The results obtained are summarized as follows: Solution phase photolysis of C-6989: An exceedingly large amount of p-nitrophenol formed strongly indicates the readiness of the ether linkage cleavage of this compound as the main reaction in all solvents used. Photoreduction of nitro to amino group(s) and photooxidation of trifluoromethyl to carboxyl group were recognized as minor reactions. Aqueous photolysis of p-nitrophenol: Quinone(0.28%), hydroquinone (0.66%), and p-aminophenol (0.42%) were confirmed as photoproducts, in addition to a relatively small amount of an unknown compound. The mechanisms of formation of these products were proposed to be the nitro-nitrite rearrangement via $n{\rightarrow}{\pi}^*$ excitation and the photoreduction through hydrogen abstractions by radicals, respectively. Solution phase photolysis of Nitrofen: Photochemical reduction leading to the p-amino derivative was the main reaction in n-hexane. In aqueous solution, the photoreduction of nitro to amino group and hydroxylation predominated over the ether linkage cleavage. Nucleophilic displacement of the nitro group by hydroxide ion and replacement of chlorine substituents by hydroxyl group or, to a lesser extent, hydrogen were also observed as minor reactoins. Solution phase photolysis of MO-338: Photoreduction of the nitro to amino group was marked in the n-hexane solution photolysis. In the aqueous solution, photoreduction of the nitro substituent and hydroxylation were the main reactions with replacement of chlorine substituents by the hydroxyl group and hydrogen, and cleavage of the ether linkage as minor reactions. Photolyses of MC-4379, MC-3761, MC-5127, MC-6063, and MC-7181 in n-hexane and cyclohexane: Photoreduction of the nitro group leading to the corresponding amino derivative and replacement of one of the halogen substituents by hydrogen from the solvent used were the key reactions in each compound. Aqueous photolysis of MC-4379: Cleavage of the ether linkage, replacement of the carboxymethyl by hydroxyl group, hydroxylation, and replacement of the nitro by hydroxy group were prominent with photoreduction and dechlorination as minor reactions. Aqueous photolysis of MC-3761: Cleavage of the ether linkage, replacement of the carboxymethyl by hydroxyl group, and photoreduction followed by hydroxylation were the main reactions. Aqueous photolysis of MC-5127: Replacement of carboxyethyl by hydrogen was predominant with ether linkage cleavage, photoreduction, and dechlorination as minor reactions. It was obvious that the decarboxyethylation proceeded more readily than decarboxymethylation occurring in the other compounds. Aqueous photolysis of MC-6063: Cleavage of the ether linkage and photodechlorination were the main reactions. Aqueous photolysis of MC-7181: Replacement of the carboxymethyl group by hydrogen and monodechlorination were the remarkable reactions. Cleavage of the ether linkage and hydroxylation were thought to be the minor reactions. Aqueous photolysis of 3-carboxymethyl-4-nitrophenol: The photo-induced Fries rearrangement common to aromatic esters did not appear to occur in the carboxymethyl group of this type of compound. Conversion of nitro to nitroso group was the main reaction.

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