• Title/Summary/Keyword: gamma-ray spectrometry

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Simultaneous Determination of Titanium, Zirconium and Niobium by Reactor Neutron Activation (원자로 중성자에 의한 티탄, 지르코늄 및 니오브의 동시 정량)

  • Chul Lee;Yung Chang Yim;Koo Soon Chung
    • Journal of the Korean Chemical Society
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    • v.18 no.1
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    • pp.40-46
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    • 1974
  • The fission neutron reactions of $^{47}Ti(n.p)^{47}Sc$ and $^{93}Nb(n,{\alpha})^{90m}Y$, along with epicadmium neutron reaction of $^{96}Zr(n,{\gamma})^{97}Zr$ were used for the simultaneous determination of Ti, Nb and Zr in synthetic mixture. Prior to neutron irradiation, Ti, Zr and Nb in the mixture were separated together in one group through the cation exchange column of Dowex $50{\times}8$ resin using 0.5 M ${\alpha}$-hydroxy-iso-butyric acid as the eluent. After irradiation of the eluate the product nuclides, $^{97}Zr$, ^{47}Sc$ and ^{90m}Y$, were eluted sequentially through the same column with 0.5 M ${\alpha}$-HIBA, 0.5 M ${\alpha}$-HIBA-1 N HNO_3 and 0.5 M ${\alpha}$-HIBA-2 N HNO_3$ solution, respectively. The gamma-ray spectrometry was used for the measurement of the gamma-ray activities of the eluted nuclides. The detection limits of Nb, Ti and Zr were found to be 0.2 %, 0.01 % and 0.002 %, respectively.

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Dry reforming of Propane to Syngas over Ni-CeO2/γ-Al2O3 Catalysts in a Packed-bed Plasma Reactor (충전층 플라즈마 반응기에서 Ni-CeO2/γ-Al2O3 촉매를 이용한 프로페인-합성 가스 건식 개질)

  • Sultana, Lamia;Rahman, Md. Shahinur;Sudhakaran, M.S.P.;Hossain, Md. Mokter;Mok, Young Sun
    • Clean Technology
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    • v.25 no.1
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    • pp.81-90
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    • 2019
  • A dielectric barrier discharge (DBD) plasma reactor packed with $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst was used for the dry ($CO_2$) reforming of propane (DRP) to improve the production of syngas (a mixture of $H_2$ and CO) and the catalyst stability. The plasma-catalytic DRP was carried out with either thermally or plasma-reduced $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst at a $C_3H_8/CO_2$ ratio of 1/3 and a total feed gas flow rate of $300mL\;min^{-1}$. The catalytic activities associated with the DRP were evaluated in the range of $500{\sim}600^{\circ}C$. Following the calcination in ambient air, the ${\gamma}-Al_2O_3$ impregnated with the precursor solution ($Ni(NO_3)_2$ and $Ce(NO_3)_2$) was subjected to reduction in an $H_2/Ar$ atmosphere to prepare $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst. The characteristics of the catalysts were examined using X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectrometry (EDS), temperature programmed reduction ($H_2-TPR$), temperature programmed desorption ($H_2-TPD$, $CO_2-TPD$), temperature programmed oxidation (TPO), and Raman spectroscopy. The investigation revealed that the plasma-reduced $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst exhibited superior catalytic activity for the production of syngas, compared to the thermally reduced catalyst. Besides, the plasma-reduced $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst was found to show long-term catalytic stability with respect to coke resistance that is main concern regarding the DRP process.

Di- and Triorganotin(IV) Complexes of Sulfur-containing Ylidenemalonates

  • Jung, Ok-Sang;Lee, Young-A;Hong, Jong-Ki;Jeong, Jong-Hwa;Sohn, Youn-Soo
    • Bulletin of the Korean Chemical Society
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    • v.14 no.6
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    • pp.722-726
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    • 1993
  • Organotin(IV) complexes of ylidenemalonates $(R_xSn)_{x-1}(O_2C)_2C=C(SR')_2\;(R=n-C_4H_9,\;C_6H_5,\;cyclo-C_6H_{11},\;CH_3OOCCH_2CH_2;\;x=2,3;\;R'=CH_3,\;R_2'=-CHCH-,\;-CH_2CH_{2^-})$ have been synthesized and characterized by means of various spectroscopic methods. The X-ray crystal structure of $(Ph_3Sn)_2(O_2C)_2C=C(SCH_3)_2$ has been determined (Pi; a= 9.704(2) ${\AA}$, b= 14.412(1) ${\AA}$, c= 14.760(3) ${\AA}$, ${alpha}$=74.26(1)$^{\circ}$, ${beta}$=99.38(l)$^{\circ}$, ${\gamma}$=79.09(1)$^{\circ}$, $V= 1950.7(7){\AA}^3$) and refined to R= 0.045. The crystal structure discloses a discrete molecule with bidentate-like carboxylate ligand. For diorganotin analogues, the structures are discussed in terms of IR, $^1H-NMR,\;^{13}C-NMR$, and FAB mass spectrometry. The mass spectrum indicates that the diorganotin complexes of ylidenemalonates are dimeric.

Analysis of Zirconium and Nickel Based Alloys and Zirconium Oxides by Relative and Internal Monostandard Neutron Activation Analysis Methods

  • Shinde, Amol D.;Acharya, Raghunath;Reddy, Annareddy V.R.
    • Nuclear Engineering and Technology
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    • v.49 no.3
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    • pp.562-568
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    • 2017
  • Background: The chemical characterization of metallic alloys and oxides is conventionally carried out by wet chemical analytical methods and/or instrumental methods. Instrumental neutron activation analysis (INAA) is capable of analyzing samples nondestructively. As a part of a chemical quality control exercise, Zircaloys 2 and 4, nimonic alloy, and zirconium oxide samples were analyzed by two INAA methods. The samples of alloys and oxides were also analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES) and direct current Arc OES methods, respectively, for quality assurance purposes. The samples are important in various fields including nuclear technology. Methods: Samples were neutron irradiated using nuclear reactors, and the radioactive assay was carried out using high-resolution gamma-ray spectrometry. Major to trace mass fractions were determined using both relative and internal monostandard (IM) NAA methods as well as OES methods. Results: In the case of alloys, compositional analyses as well as concentrations of some trace elements were determined, whereas in the case of zirconium oxides, six trace elements were determined. For method validation, British Chemical Standard (BCS)-certified reference material 310/1 (a nimonic alloy) was analyzed using both relative INAA and IM-NAA methods. Conclusion: The results showed that IM-NAA and relative INAA methods can be used for nondestructive chemical quality control of alloys and oxide samples.

Synthesis of TiO2-Fe2O3 Nanocomposite Powders for Magnetic Photocatalyst (자성광촉매용 TiO2-Fe2O3 나노복합분말의 합성)

  • Lee Chang-Woo;Kim Soon-Gil;Yun Sung-Hee;Lee Jai-Sung;Choa Yong-Ho
    • Korean Journal of Materials Research
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    • v.15 no.8
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    • pp.508-513
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    • 2005
  • [ $TiO_2-Fe_2O_3$ ] nanocomposite powders for magnetic photocatalyst were synthesized by sol-gel process, in which $TiO_2$ photocatalytic layer was formed on the surface of $\gamma-Fe_2O_3$ magnetic core. Transmission electron microscopy (TEM) observation and X-ray diffractometry (XRD) analysis revealed that$\gamma-Fe_2O_3$ nanoparticles, $10\~20nm$ in diameter, were coated by $TiO_2$ shell of 5nm in thickness and $TiO_2$ was anatase phase. Also hydroxyl group (-OH) used to decompose organic compounds was detected by Fourier transformation infrared spectrometry(FT-IR) analysis. UV-Visible spectrophotometry results showed that light absorption occurred in the wavelength range of $400\~700 nm$, and the band gap energy $(E_g)$ of powder was 1.8 eV. Finally it was found that the coercivity $(H({ci})$ and saturation magnetization $(M_s)$ of the powder were 79 Oe and 14.8 emu/g, respectively as experimental vibrating sample magnetometer (VSM) measurements.

Synthesis and Characterization of Two Different 1,3-Dithiole-2-thiones as the Precursors of TTF Donor Molecule (TTF 주게분자의 전구체로서 두 가지 다른 1,3-Dithiole-2-thione 화합물의 합성 및 특성화)

  • Kim, Young-Youn;Lee, Ha-Jin;Namgoong, Sung Keon;Hong, Jong-Ki;Noh, Dong-Youn
    • Journal of the Korean Chemical Society
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    • v.44 no.6
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    • pp.513-517
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    • 2000
  • As a precursor of tetrathiafulvalene (TTF) derivative, 5,6-dimethyl-1,3-dithiolo[4,5-b][1,4]dithiin-2-thione (compound 3) was synthesized by the unusual Lawesson's reaction. Depending upon the substituents such as dimethyl and diphenyl groups, two different products containing 1,4-dithiin and thiophene moieties, respectively, were obtained and characterized by $^{13}C$ NMR and high-resolution electron impact (HREI) mass spectroscopy. The formation of 3 was further characterized by X-ray structure analysis. Crystallographic data for 3: triclinic, space group P1, a=4.145(2)$\AA$, b=10.600(2)$\AA$, c=12.279(2)$\AA$, $\alpha$=71.440(10)$^{\circ}$, $\beta$=84.30(2)$^{\circ}$, $\gamma$=87.31(2)$^{\circ}$, Z=2 and R(wR$_2$)=0.0559(0.1416). The formation mechanism of two products was suggested and compared each other.

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Efficiency calibration of a coaxial HPGe detector-Marinelli beaker geometry using an 152Eu source prepared in epoxy matrix and its validation by efficiency transfer method

  • Yucel, Haluk;Zumrut, Senem;Nartturk, Recep Bora;Gedik, Gizem
    • Nuclear Engineering and Technology
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    • v.51 no.2
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    • pp.526-532
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    • 2019
  • In this study, an in-house $^{152}Eu$ calibration source was produced from a custom epoxy matrix with a density of ${\rho}=1.14g\;cm^{-3}$, which is chemically stable and durable form after its solidification. The homogeneity of $^{152}Eu$ in matrix was obtained better than 98%. For a Marinelli beaker geometry, an efficiency calibration procedure was applied to a n-type, coaxial, 78.5% relative efficient HPGe detector in the energy range of 121.7-1408.0 keV by using in-house $^{152}Eu$ calibration source. Then the measured efficiencies for Marinelli geometry were compared with the results calculated by MEFFTRAN and ANGLE softwares for the validation. Although MEFFTRAN and ANGLE have two different efficiency transfer algorithms to calculate the efficiencies, they usually need to use a reliable and accurate reference efficiency values as input data. Hence, reference efficiency values were obtained experimentally from a multinuclide standard source for the same detector-Marinelli geometry. In the present source characterization, the corrections required for self-absorption and true coincidence summing effects for $^{152}Eu$ gamma-rays were also obtained for a such close counting geometry condition. The experimental results confirmed the validity of efficiency calculations obtained by MEFFTRAN and ANGLE softwares that are calculation tools.

Effect of additives on the hydrothermal synthesis of manganese ferrite nanoparticles

  • Kurtinaitiene, Marija;Mazeika, Kestutis;Ramanavicius, Simonas;Pakstas, Vidas;Jagminas, Arunas
    • Advances in nano research
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    • v.4 no.1
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    • pp.1-14
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    • 2016
  • Superparamagnetic iron oxide nanoparticles (Nps), composed of magnetite, $Fe_3O_4$, or maghemite, ${\gamma}-Fe_2O_3$, core and biocompatible polymer shell, such as dextran or chitozan, have recently found wide applications in magnetic resonance imaging, contrast enhancement and hyperthermia therapy. For different diagnostic and therapeutic applications, current attempt is focusing on the synthesis and biomedical applications of various ferrite Nps, such as $CoFe_2O_4$ and $MnFe_2O_4$, differing from iron oxide Nps in charge, surface chemistry and magnetic properties. This study is focused on the synthesis of manganese ferrite, $MnFe_2O_4$, Nps by most commonly used chemical way pursuing better control of their size, purity and magnetic properties. Co-precipitation syntheses were performed using aqueous alkaline solutions of Mn(II) and Fe(III) salts and NaOH within a wide pH range using various hydrothermal treatment regimes. Different additives, such as citric acid, cysteine, glicine, polyetylene glycol, triethanolamine, chitosan, etc., were tested on purpose to obtain good yield of pure phase and monodispersed Nps with average size of ${\leq}20nm$. Transmission electron microscopy (TEM), X-ray diffraction, energy dispersive X-ray spectroscopy (EDX), $M\ddot{o}ssbauer$ spectroscopy down to cryogenic temperatures, magnetic measurements and inductively coupled plasma mass spectrometry were employed in this study.

GC/MS analysis of hydrocarbons and 2-alkylcyclobutanones from γ-ray irradiated walnut (Juglans nigra) (호두(Juglans nigra)의 감마선 조사에 따른 hydrocarbon류와 2-alkylcyclobutanone류의 GC/MS 분석)

  • Nho, Eun Yeong;Choi, Ji Yeon;Kim, Kyong Su
    • Food Science and Preservation
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    • v.21 no.6
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    • pp.859-865
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    • 2014
  • This study was conducted to analyze the hydrocarbons and 2-alkylcyclobutanones as marker compounds in walnuts after the walnuts' exposure to ${\gamma}$ irradiation. The samples were irradiated with gamma rays at 0, 1, 3, 5, 7, and 10 kGy doses. The lipids were extracted via soxhlet extraction using hexane, and were separated by florisil column and identified via gas chromatography / mass spectrometry (GC/MS). The hydrocarbons that were detected were 8-heptadecene ($C_{17:1}$) and 1,7-hexadecadiene ($C_{16:2}$) from oleic acid and 8,11-heptadecadiene ($C_{17:2}$) and 1,7,10-hexadecatriene ($C_{16:3}$) from linoleic acid. The 2-alkylcyclobutanones that were detected were 2-dodecylcyclobutanone (DCB) from palmitic acid, 2-tetradecylcyclobutanone (TCB) from stearic acid, 2-(5'-tetradecenyl)cyclobutanone (TECB) from oleic acid, and 2-(5',8'-tetradecadienyl)cyclobutanone (5',8'-TCB) from linoleic acid. The correlation between the irradiation dose and the concentrations of the hydrocarbons and 2-alkylcyclobutanones in the walnuts was found to be linear. The radio-induced hydrocarbons and 2-alkylcyclobutanones were clearly detected in the irradiated walnuts at 1 kGy and above, but not in the non-irradiated ones. The major hydrocarbons obtained after irradiation were 8-heptadecene from oleic acid and 8,11-heptadecadiene and 1,7,10-hexadecatriene from linoleic acid, and the major 2-alkylcyclobutanones were TECB from oleic acid and 5',8'-TCB from linoleic acid. Therefore, these major compounds were concluded to be the marker compounds for determining the irradiated and non-irradiated samples.

Cooling Time Determination of Spent Nuclear Fuel by Detection of Activity Ratio $^{l44}Ce /^{l37}Cs$ (방사능비 $^{l44}Ce /^{l37}Cs$ 검출에 의한 사용후핵연료 냉각기간 결정)

  • Lee, Young-Gil;Eom, Sung-Ho;Ro, Seung-Gy
    • Nuclear Engineering and Technology
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    • v.25 no.2
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    • pp.237-247
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    • 1993
  • Activity ratio of two radioactive primary fission products which had sufficiently different half-lives was expressed as functions of cooling time and irradiation histories in which average burnup, irradiation time, cycle interval time and the dominant fissile material of the spent fuel were included. The gamma-ray spectra of 36 samples from 6 spent PWR fuel assemblies irradiated in Kori unit-1 reactor were obtained by a spectrometric system equipped with a high purity germanium gamma-ray detector. Activity ratio $^{l44}$Ce $^{l37}$Cs, analyzed from each spectrum, was used for the calculation of cooling time. The results show that the radioactive fission products $^{l44}$Ce and $^{l37}$Cs are considered as useful monitors for cooling time determination because the estimated cooling time by detection of activity ratio $^{l44}$Ce $^{l37}$Cs agreed well with the operator declared cooling time within relative difference of $\pm$5 % despite the low counting rate of the gamma-ray of $^{l44}$Ce (about 10$^{-3}$ count per second). For the samples with several different irradiation histories, the determined cooling time by modeled irradiation history showed good agreement with that by known irradiation history within time difference of $\pm$0.5 year. From this result, it would be expected to be possible to estimate reliably the cooling time of spent nuclear fuel without the exact information about irradiation history. The feasibility study on identification of and/or sorting out spent nuclear fuel by applying the technique for cooling time determination was also performed and the result shows that the detection of activity ratio $^{l44}$Ce $^{l37}$Cs by gamma-ray spectrometry would be usefully applicable to certify spent nuclear fuel for the purpose of safeguards and management in a facility in which the samples dismantled or cut from spent fuel assemblies are treated, such as the post irradiation examination facility.mination facility.

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