• Title/Summary/Keyword: 저온 합성

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INTRINSIC NMR ISOTOPE SHIFTS OF CYCLOOCTANONE AT LOW TEMPERATURE (저온에서의 싸이클로옥타논에 대한 고유동위원소 효과)

  • Jung, Miewon
    • Analytical Science and Technology
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    • v.7 no.2
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    • pp.213-224
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    • 1994
  • Several isotopomers of cyclooctanone were prepared by selective deuterium substitution. Intrinsic isotope effects on $^{13}C$ NMR chemical shifts of these isotopomers were investigated systematically at low temperature. These istope effects were discussed in relation to the preferred boat-chair conformation of cyclooctanone. Deuterium isotope effects on NMR chemical shifts have been known for a long time. Especially in a conformationally mobile molecule, isotope perturbation could affect NMR signals through a combination of isotope effects on equilibria and intrinsic effects. The distinction between intrinsic and nonintrinsic effects is quite difficult at ambient temperature due to involvement of both equilibrium and intrinsic isotope effects. However if equilibria between possible conformers of cyclooctanone are slowed down enough on the NMR time scale by lowering temperature, it should be possible to measure intrinsic isotope shifts from the separated signals at low temperature. $^{13}C$ NMR has been successfully utilized in the study on molecular conformation in solution when one deals with stable conformers or molecules were rapid interconversion occurs at ambient temperature. The study of dynamic processes in general requires analysis of spectra at several temperature. Anet et al. did $^1H$ NMR study of cyclooctanone at low temperature to freeze out a stable conformation, but were not able initially to deduce which conformation was stable because of the complexity of alkyl region in the $^1H$ NMR spectrum. They also reported the $^1H$ and $^{13}C$ NMR spectra of the $C_9-C_{16}$ cycloalkanones with changing temperature from $-80^{\circ}C$ to $-170^{\circ}C$, but they did not report a variable temperature $^{13}C$ NMR study of cyclooctanone. For the analysis of the intrinsic isotope effect with relation to cylooctanone conformation, $^{13}C$ NMR spectra are obtained in the present work at low temperatures (up to $-150^{\circ}C$) in order to find the chemical shifts at the temperature at which the dynamic process can be "frozen-out" on the NMR time scale and cyclooctanone can be observed as a stable conformation. Both the ring inversion and pseudorotational processes must be "frozen-out" in order to see separate resonances for all eight carbons in cyclooctanone. In contrast to $^1H$ spectra, slowing down just the ring inversion process has no apparent effects on the $^{13}C$ spectra because exchange of environments within the pairs of methylene carbons can still occur by the pseudorotational process. Several isotopomers of cyclooctanone were prepared by selective deuterium substitution (fig. 1) : complete deuterium labeling at C-2 and C-8 positions gave cyclooctanone-2, 2, 8, $8-D_4$ : complete labeling at C-2 and C-7 positions afforded the 2, 2, 7, $7-D_4$ isotopomer : di-deuteration at C-3 gave the 3, $3-D_2$ isotopomer : mono-deuteration provided cyclooctanone-2-D, 4-D and 5-D isotopomers : and partial deuteration on the C-2 and C-8 position, with a chiral and difunctional case catalyst, gave the trans-2, $8-D_2$ isotopomer. These isotopomer were investigated systematically in relation with cyclooctanone conformation and intrinsic isotope effects on $^{13}C$ NMR chemical shifts at low temperature. The determination of the intrinsic effects could help in the analysis of the more complex effects at higher temperature. For quantitative analysis of intrinsic isotope effects, the $^{13}C$ NMR spectrum has been obtained for a mixture of the labeled and unlabeled compounds because the signal separations are very small.

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Maturation, Sex Ratio and Sex-reversal of Red Spotted Grouper, Epinephelus akaara (붉바리의 성숙과 성비 및 성전환)

  • Lee, Chang-Kyu;Hur, Sung-Bum;Ko, Tae-seung;Park, Seung
    • Journal of Aquaculture
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    • v.11 no.4
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    • pp.573-580
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    • 1998
  • Red spotted grouper, Epinephelus akaara is distributed in the south and west coasts of Korea. The natural stocks of the fish are decreasing sharply year by uear because of reckless overfishing. This research was carried out to understand general informations on maturation, sex composition and sex-reversals of the fish. Annual fishing uields of red spotted grouper in the castal area of Byonsan Peninsular of Kora decreased over 10% from 1992 to 1994. The main fishing season was from May to July with fishing gear of Hand-lines. Gonadosomatic index (GSI) and condition factor were highest on early and late July, respectively, thus main spawning reriod was assumed from late July to early August. The relationship between total length (X) and body weight (Y) for wild adults was represented as a regression, Y=$0.0169X^{2.9705}$, ($r^2$=0.96). Frequency of sex of wild red spotted gouper showed that the number of female below 38cm in total length was more than that of male, and hermaphrodite mainly occurred from 28cm to 32cm in total length the frequency of male and female were almost same. Also hermaphrodite occurred mainly between 25~29cm. Sex reversal ration of the adults reared in a tank for a year with different sexual compositions revealted that the frequency of female reversed from male was more than that of male reversed from female at 1:1 and 1:2 stocking densities of female and male, respectively. Also, about 20% of female was reversed to male when all females were reared. And the size of the fish reversed to male was larger than that of non-reversed female.

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Microstructural property and catalytic activity of nano-sized MnOx-CeO2/TiO2 for NH3-SCR (선택적 촉매 환원법 재료로서 나노 사이즈 MnOx-CeO2/TiO2 촉매에 대한 미세 구조적 특성과 촉매활성 평가)

  • Hwang, Sungchul;Jo, Seung-hyeon;Shin, Min-Chul;Cha, Jinseon;Lee, Inwon;Park, Hyun;Lee, Heesoo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.26 no.3
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    • pp.115-120
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    • 2016
  • $CeO_2$ is used as a co-catalyst with $TiO_2$ to improve the catalytic activity of $MnO_x$ and characterization of nano-sized powder is identified with de-NOx efficiency. A comparison between $MnO_x-CeO_2/TiO_2$ and single $CeO_2$ was conducted in terms of microstructural analysis to observe the behavior of $CeO_2$ in the ternary catalyst. The $MnO_x-CeO_2/TiO_2$ catalyst was synthesized by sol-gel method and the average particle size of the single $CeO_2$ is about $285{\mu}m$ due to the low thermal stability, whereas the particle size $MnO_x-CeO_2/TiO_2$ is about 130 nm. The strong interaction between Ce and Ti was identified through the EDS mapping by transmission electron microscopy (TEM). The improvement about 20 % of $de-NO_x$ efficiency is observed in the low-temperature ($150^{\circ}C{\sim}250^{\circ}C$) and vigorous oxygen exchange by well-dispersed $CeO_2$ is the reason of catalytic activity improvement.

Determination of Shelf-life of Black Mini Tomato Based on Maturity and Storage Temperature (흑색 방울토마토의 숙기 및 저장온도에 따른 상품성 유지기간 구명)

  • Park, Mehea;Seo, Jeongmin;Won, Heeyeon;Seo, Jongbun;Moon, Doogyung;Kim, Wooil;Shim, Sangyoun
    • Horticultural Science & Technology
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    • v.33 no.5
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    • pp.687-696
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    • 2015
  • Black mini tomato 'Hei-G' fruits were harvested at different stages of maturity (immature-mature green and mature-black red) and stored at different temperatures (8, 12, and $20^{\circ}C$) to investigate the quality and lycopene content during storage. Weight loss increased dramatically at higher temperature for both harvesting stages without significant differences. Firmness of immature fruits decreased below the initial level of mature fruit (8.1N) after 5, 8, and 19 days storage, when they were stored at 20, 12, and $8^{\circ}C$, respectively. Soluble solid contents of mature fruit increased at initial storage, and were higher as compared to immature fruits before deterioration at each storage temperature. Decrease in titratable acid of mature fruits depended on storage time and temperature. However, titratable acid of immature fruits showed little change during storage, and so it did not affect flavor. Hunter a value changed greatly in immature fruit stored at high temperature. Unlike ripe tomatoes, there was no significant difference in black tomato Hunter b values of immature and mature fruit at initial and 12 days storage. However, immature fruits stored at $8^{\circ}C$ did not reach full maturity and color development and ripening. High storage temperature increased lycopene production while low storage temperature blocked lycopene development. Shelf life of the immature fruits, which was evaluated by elapsed days to conventional mature stage, was 12 and 15 days when they were stored at 20 and $12^{\circ}C$, respectively. The optimum storage temperature to maintain the quality and lycopene content of mature fruits was $12^{\circ}C$. Moreover, the shelf life of mature fruits stored at $20^{\circ}C$ could reach up to 5 days.

Fabrication of Gd2O2S:Tb fine scintillator film and evaluation of image quality for resolution improvement of X-ray imaging based on CMOS (CMOS 기반 X선 영상의 해상력 향상을 위한 Gd2O2S:Tb 미세형광체 필름 제작 및 영상 질 평가)

  • Kang, Sang-Sik;Choi, Young-Zoon;Jung, Bong-Jae;No, Si-Cheul;Cho, Chan-Hoon;Yoon, In-Chan;Park, Ji-Koon
    • Journal of the Korean Society of Radiology
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    • v.5 no.5
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    • pp.283-287
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    • 2011
  • In this study, fine $Gd_2O_2S$:Tb powder was synthesized by using a low temperature solution-combustion method for a high-resolution digital x-ray imaging detector. From the fabricated phosphor power, the fine scintillator films was fabricated by particle sedimentation method and was investigated the luminescent property. From the experimental results of relative light output as a function of terbium concentration, the highest luminescent efficiency has at 5 wt% Tb concentration, and luminescent intensity decreased rapidly according to quenching effect about higher Tb concentration. Also, the relative light output of $270{\mu}m$-$Gd_2O_2S$:Tb film has 2945 pC/$cm^2$/mR. And light intensity was saturated at higher film thickness. Finally, to evaluate an image acquisition performance of fabricated phosphor, images were obtained by using commercial CMOS sensor and measured the MTF, NPS, and DQE. DQE(0 lp/mm) of fine phosphor film has 37%. But, DQE improvement of fine phosphor film is possible by resolving problem of film fabrication process and has a significant potential in the application of digital radiation imaging system later.

Morphological change of Pt/MoO3/SiO2 for the Synthesis of i-Butylene from n-Butene (N-Butene으로부터 i-Butylene 합성을 위한 Pt/MoO3/SiO2 촉매의 표면 구조 변화)

  • Kim, Jin Gul
    • Applied Chemistry for Engineering
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    • v.7 no.5
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    • pp.861-868
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    • 1996
  • Skeletal isomerization reaction known as exothermic reaction shows possible maximum yield of i-butene from n-butene at $110^{\circ}C$ over $Pt/MoO_3/SiO_2$. Compared with conventional catalyst such as silica, zeolite, alumina etc., $Pt/MoO_3/SiO_2$ demonstrates higher yield while by-products except 2-butene do not form. Faster H spillover rate over $Pt/MoO_3/SiO_2$ is demonstrated via isothermal reduction experiment at $110^{\circ}C$ compared to the rate over $Pt/MoO_3/Al_2O_3$. Overall isomerization rates are proportional to higher spillover rates from Pt onto $MoO_3$ surface. The skeletal isomerization reaction is composed of two elementary steps. First, carbonium ion formation over Pt crystallites by H spillover. Second, carbenium ion formation over $MoO_3$ followed by formation of i-butene. Moreover, it is suggested that H spillover step from Pt surface onto $MoO_3$ is assumed to be the rate determining step and control the overall isomerization rate.

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Property of Optical Spectroscopy on the Lanthanum Tungstate doped Eu3+ Ion (Eu3+ 이온이 첨가된 란타넘텅스텐산화물의 분광학 특성)

  • Seo, Hyojin;Park, Cheolwoo
    • Journal of the Korean Society of Radiology
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    • v.9 no.1
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    • pp.39-45
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    • 2015
  • $La_2W_3O_{12}:Eu^{3+}$ phosphors were prepared by solid state reaction method. The crystal structure was characterized by XRD pattern and ICSD card (78180). Luminescence properties of $La_2W_3O_{12}:Eu^{3+}$ are investigated by optical and laser-excitation spectroscopy in which emission and excitation spectra and time-resolved spectra are measured. The 1 mol % $Eu^{3+}$-doped $La_2W_3O_{12}$ phosphor exhibits broad excitation band peaking at 286 nm due to the ligand-to-metal charge transfer transition. The excitation lines due to the $^7F_0{\rightarrow}{^5D_4},{^5D_4},{^5L_6},{^5G_4},{^5D_3},{^5D_2}$ transitions of $Eu^{3+}$ are observed in the wavelength region 350-500 nm. The strong line emission is observed at 618 nm corresponding to the due to the $^5D_0{\rightarrow}^7F_2$ transition. The lifetime of 618 nm emission decreases with increasing temperature as 7 K ($114{\mu}s$), 100 K ($94{\mu}s$), 200 K ($10{\mu}s$) and 300 K ($0.5{\mu}s$).

유산균 발효에서 항생물질 불활화에 관한 연구

  • 강국희;이수원;김영진;김영창
    • Proceedings of the Korean Society for Applied Microbiology Conference
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    • 1978.10a
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    • pp.204.2-205
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    • 1978
  • 발효유 원료유중에 항생물질이 함유되어있을 경우 이것이 발효유 제조에 미치는 영향을 검토하였다. 발효유의 원가유 살균과정, 배양기간, 보존기간중에 있어서 항생물질의 변화를 검토하기 위하여 Bacillus stearothermophilus var. calidolactis C 953을 사용한 cylinder plate법으로 penicillin의 역가를 측정하였다. 저온 장시간 $살균(60^{\circ}C,$ 30분) 조건에서는 조금도 불활성화되지 않았으나, 온도를 높이고, 시간을 길게함에 따라 점점 불활화률이 높아져 $고압멸균조건(121^{\circ}C,$ 15분)에서는 약 90% 이상이 불활화되었다. 또 현재 우리나라에서 발효유제조에 사용되고 있는 Lactobacillus casei, Hy3와 Lactoba-cillus bulgaricus Hy4A, Hy4B를 사용하여 $37^{\circ}C에서$ 배양할 경우 배양기간 중에 있어서 penicillin은 2일내에 95% 이상 불활화되었다. 그리고 $보존기간(5^{\circ}C)$ 중에는 phosphate buffer(pH 6.0)와 10% skim milk의 경우에 10일까지도 거의 불활화가 되지 않았으나, 발효유내에서는 5일만에 85% 이상이 불활화된다는 결과를 얻었다. 이와같은 발효유 배양기간과 보존기간 중의 penicillin 불활화의 원인을 규명하기 위하여 각종 유기산의 영향을 조사한 결과(조건 pH.3.30~3.45, 보존온도 $37^{\circ}C),$ 염산과 유산의 경우 24시간, 구연산의 경우 48시간, 초산의 경우 72시간내에 실험에 사용한 penicillin 농도의 99.99%가 불활화되었다. 이러한 결과로 볼 때 유산발효에서 penicillin이 불활화되는 주원인은 발효에 의하여 생성된 유기산에 의한 것으로 추정된다.방식이군이 중지방식이군과 고지방식이군에 비해 혈장내 LCAT 활성이 유의하게9p<0.001) 증가하였다. 3) 간의 콜레스테롤합성 능력은 정어리유군이 다른지방군보다(p<0.001), 무지방식이군이 식이지방첨가군보다(p<0.001), 동물성지방군의 식물성유지군보다 유의하게(p<0.001) 증가하였으나, 식이 지방의 수준에 의한 차이는 나타나지 않았다. 수용성 식이섬유소가 생리져 기능이 거의 비슷하고 무독성이 관찰됨으로써 신갈나무로부터 제조된 수용성 식이섬유소의 제조 방법이 우수하다고 볼 수 있다.있었다.세에 해당되는 중년 여성의 에너지, 단백질, 철분 섭취량을 권장량과 비교하여 보면, 각각 74.8$\pm$12.6%, 94.6$\pm$26.4% 및 64.5$\pm$14.1%로 당뇨군 (각각 112.8$\pm$28.5%, 157.8$\pm$68.2%, 92.8$\pm$21.7%)에 비해 유의하게 낮았고 정상군과는 유의한 차이를 보이지 않았다.상고나성이 있었다. 혈중 호모시스테인 농도는 질병의 위험요인으로서 뿐 아니라 대사적으로 밀접하게 연관된 비타민 영양상태의 biomarker로서도 그 영향력이 크다고 할 수 있다. 따라서 성별에 다른 다양한 연령집단에서 건강한 일반인과 심혈관계 질환자 등을 대상으로 호모시스테인과 비타민 영양상태에 대한 연구가 체계적으로 이루어 져야 할 것이다.태를 보다 효율적으로 증진시킬 수 있는 대안이 마련되어져야 한다고 사료된다.$\ulcorner$순응$\lrcorner$의 범위를 벗어나지 않는다. 그렇기 때문에도 $\ulcorner$순응$\lrcorner$$\ulcorner$표현$\lrcorner$의 성격과 형태를 외형상으로 더욱이 공간상에서는

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Evaluation of Transparent Amorphous $V_2O_5$ Thin Film Prepared by Thermal Evaporation (진공증착법으로 제조한 투명 비정질 $V_2O_5$박막의 특성평가)

  • Hwang, Kyu-Seog;Jeong, Seol-Hee;Jeong, Ju-Hyun
    • Journal of Korean Ophthalmic Optics Society
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    • v.13 no.1
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    • pp.27-30
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    • 2008
  • Purpose: This research is that $V_2O_5$ cathode's composition is possible in low temperature. Methods: Transparent in visible spectra range and crystallographically amorphous $V_2O_5$ thin films were prepared by simple vacuum thermal evaporation on soda-lime-silica slide glass substrate. After annealing at 100$^{\circ}C$, 150$^{\circ}C$ and 200$^{\circ}C$ for 10 minutes in air, the surface morphology and the fracture-cross section of the films were investigated by field emission - scanning electron microscope. Transmittance in visible spectra range and surface roughness of the films were analyzed by ultra violet - visible spectrophotometer and scanning probe microscope, respectively. Results: As the increase of annealing temperature from 100$^{\circ}C$ to 150$^{\circ}C$ and 200$^{\circ}C$, transmittance of the $V_2O_5$ films decreased. Optical properties will be fully discussed on the basis of the surface morphological results. Conclusions: Optical transmissivity was superior in case of 100$^{\circ}C$, and could make amorphous $V_2O_5$ thin film that surface quality of thin film did homogeneity.

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Preparation and Characteristics of $Y_2O_3-CeO_2-ZrO_2$ Structural Ceramics : II. Mechanical Properties and Thermal Stability of Sintered Body ($Y_2O_3-CeO_2-ZrO_2$ 구조세라믹스의 제조 및 특성 : II. 소결체의 기계적 성질 및 열적 안정성)

  • 오혁상;이윤복;김영우;오기동;박홍채
    • Journal of the Korean Ceramic Society
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    • v.34 no.1
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    • pp.102-108
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    • 1997
  • ZrO2 powders stabilized with Y2O3 and CeO2 of various compositions were prepared by the coprecipitation of water-soluble ZrOCl2.8H2O, YCl3.6H2O and Ce(NO3)3.6H2O, and their compacts were pressurelessly sintered at 1400 and 150$0^{\circ}C$ for 2hrs in air. 2mol% Y2O3-ZrO3 showed the most superior strength (1003MPa) and microhardness (12.6GPa), while 10 mol%CeO2-ZrO2 had the hightest toughness (13.3 MPa.m1/2) after sintering at 140$0^{\circ}C$. The addition of Y2O3 into Y2O3-ZrO3 decreased mean grain size and increased strength and hardness but decrease toughness. On the other hand, the addition of CeO2 into Y2O3-ZrO2 enhanced the stability of tetragonal phase during low-temperature aging for a long time under hydrothermal atmosphere.

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