• Title/Summary/Keyword: Spectrometric data

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Synthesis of Long-Chain Unsaturated Acetates (장직쇄상(長直鎖狀) 불포화(不飽和) 초산화합물(醋酸化合物)의 합성(合成)에 관(關)한 연구(硏究))

  • Oh, Sung-Ki
    • Applied Biological Chemistry
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    • v.19 no.1
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    • pp.1-23
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    • 1976
  • The female moths of Lepidoptera comprising over 1,000,000 described species possess long-chain unsaturated alcohols or esters as the typical structure of potential sex attractants. In this experiment, various stereoisomers of $C_{16}-unsaturated$ acetates were synthesized for potential sex attractants; e.g., $CH_3(CH_2)_mCH=CH(CH_2)_nOR$ (m=0-12, n=1-13, R=H and $-COCH_3$). Seventeen acetates were spectrometrically examined so that the data would provide a ready catalog of gas chromatography and mass spectrometric data for comparison with natural insect sex attractants. Exclusively cis and trans isomers were obtained by the catalytic and chemical reduction methods, respectively. Commercially available $CH_3(CH_2)_mBr,\;CH_3(CH_2)_mC{\equiv}CH,\;HC{\equiv}C(CH_2)_nOH\;and\;HO(CH_2)_n\;OH$ were used for the synthetic starting material. 1-Alkynes, $CH_3(CH_2)_m\;C{\equiv}CH$ exceeding nine methylene groups did not condense with alkyl dihalides. The yield of coupling products was gradually decreased with increasing the molecular weight of diols. In the coupling reaction of $BrCH_2CH_2$ OTHP with acetylene gas, the tetrahydropyranyl ether of bromohydrin produced undesirable elimination product. In this experiment, it seems that p-toluenesulfonic acid is greatly favoured hydrolyzing agent over dilute sulfuric acid in the hydrolysis of the tetrahydropyranyl ether of long-chain alkynols.

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Evaluation of soybean oil rancidity by pentanal and hexanal determination (Pentanal과 hexanal 측정에 의한 대두유의 산패도 측정)

  • Chun, Ho-Nam;Kim, Ze-Uook
    • Applied Biological Chemistry
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    • v.34 no.2
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    • pp.149-153
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    • 1991
  • Several commercial soybean oils were stored at $20^{\circ}C,\;40^{\circ}C$ and $60^{\circ}C$ with daily exposure of fluorescent light for 12 hours and evaluated their rancidity by headspace gas chromatographic analysis of pentanal and hexanal. The data of gas chromatographic analysis was compared with organoleptic flavor evaluation. For headspace gas chromatographic analysis, the volatile compounds were recovered by porous polymer trap and flushed into a fused silica capillary column at $250^{\circ}C$, The pentanal and hexanal separated were identified by gas chromatography and gas chromatography-mass spectrometric method. The results showed that the contents of pentanal and hexanal were linearly increased during storage for 100 days. A very simple linear relationship was found between organoleptic flavor scores and amounts of two volatile compounds with very high correlation coefficient. A similar linear relationship was also obtained for acid and peroxide value with sensory data. This results suggested the possible implication of pentanal and hexanal as an quality index for rancidity evaluation of soybean oil.

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Identification of Water Soluble Metabolites of Pentachlorophenol(PCP) in the Suspension Cultures of Soybean and Rice Cells;3. Identification of PCP Glucose conjugates (콩과 벼 현탁배양(懸濁培養) 중 PCP 수용성대사물(水溶性代謝物)의 동정(同定);3. PCP glucose conjugates의 동정(同定))

  • Kim, Pil-Je;Park, Chang-Kyu
    • Korean Journal of Environmental Agriculture
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    • v.15 no.2
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    • pp.167-178
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    • 1996
  • In order to identify PCP glucose conjugates transformed from PCP in soybean and rice cell suspension cultures, the purified metabolites were acetylated, purified twice by HPLC using a normal and a reversed phase column, and then subjected to fast atom bombardment(FAB) mass spectrometric analysis. As were the conjugates, their acetylated derivatives of the glucose conjugates formed at the early stage(48 hr) of metabolism were separated by HPLC into three fractions. FABMS analysis of each fraction revealed that, at least in two fractions, the locations of the spectral peaks were practically coincident with those deducible from the structures of pentachlorophenyl and tetrachlorophenyl ${\beta}-D-glucopyranosides$. Based on information obtained from mass spectral and chromatographic analysis of not only the water-soluble metabolites but also aglycones and glycone, it is concluded that PCP is primarily metabolized to glucose conjugates, which account for more than 50% recovery of the PCP-conveyed radioactivity from the water soluble metabolites : The conjugates are mainly made up of pentachlorophenyl ${\beta}-D-glucopyranoside$, tetrachlorophenyl ${\beta}-D-glucopyranosides$( probably 2 or more isomers), and 2-hydroxy-3,4,5,6-tetrachlorophenyl ${\beta}-D-glucopyranoside$.

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Synthesis and Characterization of Li-Graphite intercalation Compounds (리튬-흑연 층간 화합물의 합성 및 특성)

  • Oh, Won-Chun;Kim, Myung-Kun;Ko, Young-Shin
    • Analytical Science and Technology
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    • v.7 no.3
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    • pp.315-320
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    • 1994
  • Li-GICs as a high performance energy storager were synthesized as a function of the Li content by the admixture and add-pressure method. The characteristics of these prepared compounds have been determined from the studies by X-ray diffraction, UV-VIS spectrometry and CHN analysis. It follows from the results of X-ray diffraction that the lower-stage intercalation compounds are formed as the Li contents increase, however the mixed stages in these compounds are also observed. In the case of the $Li_{40wt%}$, the compound with the structure of stage 1 has been predominently, but the structure of only stage 1 is not obtained. The $d_{001}$ value of stage 1 was determined to be ca. $3.70{\AA}$. An analysis of spectrometric data shows that each of the compounds gives distingushible energy state spectra. It is seen from the spectra that the positions of $R_{min}$ values, with increase in the Li contents, are shifted in the region of higher energy state. Such a result can be attributed to the formation of stable stages. The results of CHN analysis allow us to find the mixing state related to chemical compositions of the intercalated compounds and the superiority to admixture and add-pressure method. From the results determined, it reveals that $Li_{10wt%}$-GIC and $Li_{20wt%}$-GIC can be utilized for an anode of rechargable battery.

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Gas Chromatographic and Mass Spectrometric Determination of Alcohol Homologues in the Korean Folk Sojues (Distilled Liquor) (기체크로마토그래피 및 질량분석법에 의한 민속 소주중의 알코올 동족체 분석)

  • Lee, Dong Seon;Park, Hye Seong;Kim, Geon;Lee, Taek Su;No, Bong Su
    • Journal of the Korean Chemical Society
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    • v.38 no.9
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    • pp.640-652
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    • 1994
  • This work is undertaken to determine alcohol homologues so-called fusel oil that may be present in the Korean folk sojues (distilled liquor) made from grains and to describe sample preparation and analytical method by GC-FID-MS. Solid phase extraction method for sample preparation by using porous styrene divinyl benzene polymer (Porapak Q) was compared with steam distillation and solvent extraction method. Retention behaviors of homologous series of alcohols were also studied. Log values of retention time, molecular weight, boiling point, and capacity factor of alcohols showed linear correlations to the carbon number of an alcohol, to the oven temperature, and to the dielectric constant. Components such as methyl alcohol, n-propyl alcohol, isobutyl alcohol, isopentyl alcohol, and phenethyl alcohol have been identified. The more amount of isopentyl alcohol than other alcohols are contained in the Korean folk sojues, while that of n-propyl alcohol are contained in Chinese kaoliangchiew. Degree of similarity or dissimilarity and classification of the individual samples were discussed using multivariate statistical analysis(principal components analysis) based on GC data.

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Uncertainty evaluation of the analysis of 11-nor-9-carboxy-Δ9-tetrahydrocannabinol in hair by GC-NCI-MS/MS (GC-NCI-MS/MS를 이용한 모발 중 대마 대사체 분석의 측정불확도 평가)

  • Kim, Jin-Young;Lee, Jae-Il;Cheong, Jae-Chul;Suh, Yong-Jun;In, Moon-Kyo
    • Analytical Science and Technology
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    • v.24 no.1
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    • pp.1-9
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    • 2011
  • We described an estimation of measurement uncertainty in quantitative analysis of 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THC-COOH), the metabolite of ${\Delta}^9$-tetrahydrocannabinol, in hair samples by using the bead-assisted liquid-liquid extraction and gas chromatography-tandem mass spectrometric (GC-NCI-MS/MS) detection. Traceability of measurement was established through the use of reference materials, calibrated volumetric tubes, volume measuring devices, and measuring instruments. The analytical results were compared and the different contributions to the uncertainty were evaluated. Inter-day variation was performed by using statistical analysis of several indicative factors. Measurement uncertainty associated with the analyte in real forensic hair samples were estimated using QC data. The major factor of contribution to combined standard uncertainty was inter-day repeatability, while those associated with preparation of analytical standard and also sample of weight were insignificant considering the degree of contribution. Relative uncertainty of relative extended standard uncertainty divided into the measured concentration of the analyte was 17% in a hair sample. The uncertainty of result evaluation will be invaluable to improve quality of the analysis.

Photochromic Properties of Cellulose Derivatives Having Spirobenzopyran Group (스피로벤조피란을 포함하는 셀룰로오스 유도체의 광변색 특성)

  • Xiangdan, Li;Kim, Eun-Kyoung;Lee, Myong-Hoon
    • Polymer(Korea)
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    • v.29 no.1
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    • pp.25-31
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    • 2005
  • Cellulose acetate derivatives containing 6-(p-hexyloxyphenyl)carbonyl spirobenzopyran (CA-COSP) were prepared from base-catalyzed etherification of cellulose acetate, and their physical and photochromic properties were characterized. The degree of substitution of COSP was calculated from the amount of residual hydroxyl groups in cellulose acetate measured by the $^1H$-NMR and UV spectrometric data. It was ranging from 0.87 to 45.5% depending on the reaction condition. UV/vis spectrometry of the resulting CA-COSP revealed that the polymer shows a reversible color change by changing its color from colorless to blue upon UV irradiation forming a merocyanine structure, and returning back again to colorless spiropyran structure by visible light or by heat. The rate of color change was faster in solution than in the film. In the more polar solvent, the more stable was the resulting merocyanine, and the slower was the rate of reverse reaction to spiropyran. Compared to COSP blended with cellulose acetate, in which a phase separation was observed for samples containing more than 0.9 wt% of COSP, up to 48 wt% of COSP could be blended in CA-COSP without phase separation.

Study on The Quantification of Cosmic-Ray Component Contributed to Natural Background Radiation Exposure (자연 방사선량 중 우주선 기여 성분 정량 연구)

  • Jun, Jae-Shik;Oh, Hi-Peel;Ha, Chung-Woo;Oh, Heon-Jin;Kang, In-Seon
    • Journal of Radiation Protection and Research
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    • v.13 no.2
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    • pp.9-20
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    • 1988
  • In order to quantify the contribution of cosmic-ray ionizing component to the dose given by natural background radiation, a series of measurement has been carried out using LiF TLDs for about one and a half years on quarterly basis. Three different types of LiF TLDs namely, chips and PTFE based disks of $^{7}LiF$, and the same disks of $^{6}LiF$ for identifying possible contribution of neutron component were used. Measurements were made by placing badge-incased TLDs in a lead castle of 10 to 15cm thick installed in a room on the third floor of a four-story building in CNU Daedeok campus for 5 cycles of 90 days. For comparison a series of spectrometric study was also performed for the energy region over 3MeV using a 3'${\phi}\;{\times}\;3$'NaI(Tl) scintillation detector in association with an MCA of 1024 channels, and it was found that the data obtained by the TLDs placed in the lead castle indicate 75% of the dose given by outdoor cosmic-ray component. The results obtained by the TLDs through correction for shielding loss show that the outdoor dose contribution of ionizing component of cosmic rays at this campus is $34.3{\pm}1.1nGy/h$ which satisfactorily agrees with that expected for our particular location of measurement.

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Concentration of Radioactive Materials for the Phanerozoic Plutonic Rocks in Korea and Its Implication (국내 현생 심성암류의 방사성 물질의 농도 및 의미)

  • Kim, Sung Won
    • Economic and Environmental Geology
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    • v.53 no.5
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    • pp.565-583
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    • 2020
  • In recent years, various social issues related to the natural radioactive elements detected in household goods and building materials are addressed, and should be solved promptly. In Korea, for more than 20 years, the Ministry of Environment has investigated the natural radioactive materials such as heavy metals, uranium, and radon in soil or groundwater. The origins of natural radioactive materials in them may have a close correlation with the geological factors including classification of rocks, petrogenetic origins, and deformation characteristics, but the exact geological correlations are not clarified because of the absence of the government policy preserved in the basement rocks, soils as well as groundwater in fault-related reservoirs. This study aims to perform a research on the correlation between the petrogeneses of the Phanerozoic plutonic rocks and natural radioactive concentrations in rocks (radon, uranium, thorium, potassium etc.) in Korea. Among the Phanerozoic plutonic rocks, alkaline plutonic rocks (syenite, monzonite and monzodiorite and alkali granite) show high U and Th concentrations by high solubilities of U, Th, Zr, REE, and Nb until the most extreme stages of magmatic fractionation (viz. crystal fractionation) due to high magma temperature and high alkalinity tendency. The highly fractionated high-K calalkaline and peraluminous granitic rocks (leucogranite, two-mica granite and leucocratic pegmatite are also U and Th concentrations compared with other less or medium fractionated granitic rocks (diorite, granodiorite and granite). The alkaline plutonic rocks are associated with intracontinental rifting and extensional environment after crustal thickening by collisional and subductional processes. In contrast, the dominant calc-alkaline granitic rocks in Korea are related to the arc environment of the subduction zone. In summary, the trends of the U, Th and K concentration from the Phanerozoic plutonic rocks in Korea are closely linked to the petrogenesis of the rocks in tectonic environment. The preliminary data for gamma-spectrometric mesurments of natural radionuclide contents (226Ra, 232Th and 40K) in the Phanerozoic plutonic rocks show high values in the alkaline and highly fractionated granitic rocks.