• 제목/요약/키워드: Isotope

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Accurate mass 및 isotope ratio 측정을 위한 GC-TOF 질량분석기에서의 화학적 이온화방법 (Development of chemical ionization method in a GC-TOF mass spectrometer for accurate mass and isotope ratio measurement)

  • 정주희;나윤철;황금숙;신정화;안윤경
    • 분석과학
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    • 제24권1호
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    • pp.15-23
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    • 2011
  • 본 연구에서는 미지 대사물질 동정을 위해 GC-TOF/MS의 양이온 화학적 이온화 방법(positive chemical ionization, $CI^+$)을 이용, 정확한 질량 값(accurate mass)과 동위원소 비(isotope ratio) 측정을 위한최적 조건을 확립하였다. 분자이온 $[M+H]^+$ 세기를 증가시킬 수 있는 high mass tune 방법이 사용되었으며, 화합물들의 분리 및 감도에 따른 검출조건이 고려되어 졌다. 24종의 trimethylsilyl (TMS)기로 유도체화 된 표준 대사물질들을 분석한 결과 $[M+H]^+$의 경우 이론 값 과의 절대평균오차는 6.8 ppm이였으며, 동위원소 비(M+1/M, M+2/M)의 경우는 각각 1.5%와 1.7%였다. 얻어진 질량 값과 동위원소 비를 원소조성 알고리즘에 적용한 결과 21개의 화합물의 구조식이 2순위 내에서 일치하였다.

Deuterium Isotope Effects on the $^{13}C$ Chemical Shifts of Cyclooctanone-2-D

  • 정미원
    • Bulletin of the Korean Chemical Society
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    • 제19권8호
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    • pp.836-840
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    • 1998
  • The intrinsic and equilibrium isotope effects on the 13C NMR chemical shift of the cyclooctanone-2-D were investigated. Equilibrium constants and changes in the free energies, enthalpy, entropy, which are derived from the temperature dependence of the isotope shifts, are reported for this isotopomer.

삼기층(三紀層)에 배태(胚胎)된 벤토나이트의 산소(酸素) 및 수소동위원소(水素同位元素) 연구(硏究) (Hydrogen and Oxygen Isotopic Compositions of Tertiary Montmorillonites in Southern Korea)

  • 문희수
    • 자원환경지질
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    • 제19권spc호
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    • pp.131-138
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    • 1986
  • Hydrogen and oxygen isotope ratios of thirteen of the under 2 micron size fraction of the montmorillonites were measured. The oxygen isotopic compositions of these samples range from + 17.0 to +25.1 permil and the hydrogen isotope compositions range from -47.5 to -65.8 permil with an average standard deviation of 0.7 and 2.7 permil, respectively. The oxygen isotope compositions show a positive relationship with stratigraphy whereas the hydrogen isotope compositions do not. It suggest that the montmorillonite attained isotopic equilibrium at the maximum burial depth and ratained their oxygen isotope composition on subsequent uplift. Possibilities of montmorillonite formation by weathering or hydrothermal alteration of volcanic material are eliminated by the ${\delta}D$ and ${\delta}^{18}O$ values of these samples. Calculated formation temperature lie between 29 to $80^{\circ}C$.

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Oxidation of Benzyl Alcohols with Extraordinarily High Kinetic Isotope Effects

  • Jo, Myeong-Ran;Seok, Won-K.
    • Bulletin of the Korean Chemical Society
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    • 제32권spc8호
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    • pp.3003-3008
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    • 2011
  • Reactions of benzyl alcohol and its derivatives by [Ru$^{IV}$(tpy)(dcbpy)(O)]$^{2+}$ (tpy = 2,2':6',2"-terpyridine; dcbpy = 4,4'-dicarboxy-2,2'-bipyridine) leading to the corresponding benzaldehydes in acetonitrile and water have been studied. Kinetic studies show that the reaction is first-order in both alcohol and oxidant, with k = 1.65 (${\pm}$ 0.1) $M^{-1}s^{-1}$ at $20^{\circ}C$, ${\Delta}H^{\ddag}$ = 4.3 (${\pm}$ 0.1) kcal/mol, ${\Delta}S^{\ddag}$ = -22 (${\pm}$ 1) eu, and $E_a$ = 4.9 (${\pm}$ 0.1) kcal/mol. High ${\alpha}$ C-H kinetic isotope effects are observed, but O-H solvent isotope effects are negligible. Spectral evidences with the isotope effects suggest that oxidation of benzyl alcohols occurs by a two-electron, hydride transfer. The catalytic cycles of aerobic benzyl alcohol oxidation are employed.

Analysis of the Irradiated Nuclear Fuel Using the Heavy Atom and Neodynium Isotope Correlations with Burnup

  • Kim, Jung-Suk
    • Nuclear Engineering and Technology
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    • 제29권4호
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    • pp.327-335
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    • 1997
  • The correlation of isotope composition of uranium, plutonium and neodymium with the burnup in M uranium dioxide fuel has been investigated experimentally. The total and fractional($^{235}$ U) burnup were determined by Nd-148 and, U and Pu mass spectrometric method respectively. The isotope compositions of these elements, after their separation from the fuel samples were measured by mass spectrometric. The content of the elements in the irradiated fuel ore determined by isotope dilution mass spectrometric method using $^{233}$ U, $^{242}$ Pu and $^{150}$ Nd as spikes. The content of plutonium in the irradiated fuel was expressed by the correlation with uranium isotopes. The correlations between isotope compositions themselves and the total and fractional burnup ore compared with those calculated from ORIGEN2 code.

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Low Temperature Test of HWR Cryomodule

  • Kim, Heetae;Kim, Youngkwon;Lee, Min Ki;Park, Gunn-Tae;Kim, Wookang
    • Applied Science and Convergence Technology
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    • 제25권3호
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    • pp.47-50
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    • 2016
  • Low temperature test for half-wave resonator (HWR) cryomodule is performed at the superfluid helium temperature of 2 K. The effective temperature is defined for non-uniform temperature distribution. Helium leak detection techniques are introduced for cryogenic system. Experimental set up is shown to make the low temperature test for the HWR cryomodule. The cooldown procedure of the HWR cryomodule is shown from room temperature to 2 K. The cryomodules is precooled with liquid nitrogen and then liquid helium is supplied to the helium reservoirs and cavities. The pressure of cavity and chamber are monitored as a function of time. The vacuum pressure of the cryomodule is not increased at 2 K, which shows leak-tight in the superfluid helium environment. Static heat load is also measured for the cryomodule at 2.5 K.

Attenuation of Background Molecular Ions and Determination of Isotope Ratios by Inductively Coupled Plasma Mass Spectrometry at Cool Plasma Condition

  • 박창준
    • Bulletin of the Korean Chemical Society
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    • 제18권7호
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    • pp.706-710
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    • 1997
  • Isotope ratios of K, Ca, Cr and Fe are measured at cool plasma condition generated using high carrier flow rate and relatively low RF power of 900 W. Background molecular ions are suppressed to below 100 counts which give isobaric interference to the analytes. The background ions show different attenuation characteristics at increased carrier flow rate and hence for each element different carrier flow rate should be used to measure isotope ratios without isobaric interference. Isotope ratios are measured at both scan and peak-hopping modes and compared with certified or accepted ratios. The measured isotope ratios show some mass discrimination against low mass due to low ion energy induced from a copper shield to eliminate capacitive coupling of plasma with load coil.