• Journal of the Society of Cosmetic Scientists of Korea
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• v.25 no.3
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• pp.23-46
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• 1999

LC/MS는 HPLC의 분리능과 질량분석기의 화합물의 확인 능력을 결합시킨 기기이다. 여기서 사용되는 이온화 방법은 GCJMS에서 사용되어지는 전자이온화법(electron ionization, EI)이나, 화학이온화법(chemical ionization, CI)은 부적당하기 때문에 최근 개발되어진 연성 이온화법의 대표적인 고속원자폭격식(Fast atom bombardment, FAB)이나 전기분무이온화식 (electrospray ionization, ESI) 등이 사용되고 있다. 이중 전기분무이온화법은 고속원자폭격법에서 사용되는 매트릭스를 사용하지 않기 때문에 매트릭스 이온의 부재로 인한 낮은 바탕 신호, 오래 지속되면서 안정된 초기 이온 전류, 샘플링의 용이성, HPLC와의 더 좋은 호환성 등의 장점을 제공한다. 이러한 전기분무이온화 방법은 극성이 매우 크거나 휘발성이 낮은 물질로 보통의 EI나 CI 이온화 방법으로 분석이 어려운 물질들을 분석할 수 있다. 또한 열에 불안정하거나 분자의 분자량이 다른 단백질 등의 분석도 가능하다. 이러한 LC/ESI/MS 방법을 이용하여 열에 불안정하고 극성이면서 분자량이 커서 GC/MS 펄의 분석이 어려운 기능성 화장품 원료로 주목받고 있고 생체에 존재하는 지질 성분으로 알려진 레시틴과 세라마이드의 분석이 가능함을 소개하고 분리와 동시에 그 분자량과 구조에 대한 정보를 빠르게 얻을 수 있음을 소개하였다.

• Journal of the Korean Applied Science and Technology
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• v.30 no.4
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• pp.586-591
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• 2013

This paper describes the characteristics of thermo-field emission in a freestanding silicon nanomembrane under ion bombardment with various thermal and field conditions. The thermal effect and field effect in thermo-field emission in silicon nanomembrane are investigated by varying kinetic energy of ions and electric field applied to the silicon nanomembrane surface, respectively. We found that thermo-field emission increases linearly as the electric field increases, when the electric field intensity is lower than the threshold. The thermo-field emission (schottky effect) increases proportionally to the power of temperature, which agree well with the predictions of a thermo-field emission model.

• The Journal of the Petrological Society of Korea
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• v.10 no.3
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• pp.190-201
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• 2001

Isotope Dilution Mass Spectrometry(IDMS) is one of the analytical method which uses enriched isotope spikes and analyzes the abundance of element by comparison of the spectrum between spiked mass and non-spike mass. Especially, the Thermal Ion Mass Spectrometry with isotope dilution technique (in general ID-TIMS) is the most accurate method of the chemical analysis, which enables us to obtain the data better than 1% in accuracy and precision. In IDMS, enriched isotope spike is one of the most important factor in order to obtain the best data. For rare earth elements, in general, a mixture of /sup 138/La, /sup 142/Ce, /sup 145/Nd, /sup 149/Sm, /sup 151/Sm, /sup 151/Eu, /sup 157/Gd, /sup 163/Dy, /sup 167/Er, /sup 171/Yb, and /sup 176/Lu is used as composite spike. IDMS is very useful in geochronology and REE geochemistry. Especially, it is very effective in studying the “tetrad effect” of rare earth elements in natural samples.

• Analytical Science and Technology
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• v.18 no.1
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• pp.27-34
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• 2005

$Li_2B_4O_7$ and $Na_2B_4O_7$ were synthesized with boron isotopic standard material for the measurement of boron isotopes of positive ions (PTIMS) such as $Li_2BO_2{^+}$ (mass 56, 57) and $Na_2BO_2{^+}$ (mass 88, 89) instead of boron mass 10 and 11. The negative ions (NTIMS) such as $^{10}BO_2{^-}$ and $^{11}BO_2{^-}$(mass 42와 43) were also measured with the same boron isotopic standard material. The precision and accuracy were compared between each method, and prescan of isobaric effect was studied. Good result was obtained from NTIMS method which provided the stable and enough peak intensities with good precision and accuracy. The measurement of boron isotopes were performed in ground water sample with about 8 ng-B ($5{\mu}L$ sample solution) obtained from IAEA for international inter-comparison analysis. The standard deviation was found to be 0.03%. Boron content of this ground water was measured using the NTIMS-IDMS. The result was $1.65{\pm}0.003ug-B/mL$ which was better precision compared to the ICP-AES result.

• Analytical Science and Technology
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• v.23 no.5
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• pp.498-504
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• 2010

It is very difficult to get stable ion peak intensity of ruthenium by thermal ionization mass spectrometry because of its high ionization potential and high volatility of its oxides which causes to lose much of ruthenium ions, so the intensity of the signal decrease quickly. Accordingly, a study was performed in oder to increase the ionization efficiency and to prevent sample losses due to volatilization and to check with isobaric effect by impurities in filament for the measurement of ruthenium isotopes. Both single filament and double filament were tested. The former was proved to be more efficient for the stable and strong intensity of signal and revealed less isobaric effect from the molybdenum (Mo) as a filament impurity. Also, when the temperature of filament increased too high, the isobaric effect from Mo greatly appeared. That is, Mo impurity from filament gave a serious effect for measuring the ruthenium isotopes. It was proved to be of importance that filament current should be slowly increased with time interval. Finally, ruthenium isotopes were accurately measured by correction with measuring $^{94}Mo/^{99}Ru$.

• The Journal of the Petrological Society of Korea
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• v.10 no.3
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• pp.157-171
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• 2001

This study investigated the effects of Pb/Tl ratio, Pb concentration and concomitant matrix elements on the measurement of Pb isotope ratios using multi-collector ICP/MS (AXIOM MC model). Accuracy and reproducibility of Pb isotope ratios in NBS 981 solution were estimated for 42 data measured from March to August 2001. Pb isotopes measured in rocks, bronzes and sediments were compared to data measured by TIMS. Reproducibilities for $^{206}Pb/^{204}Pb,\; ^{207}Pb/^{204}Pb,\;and\;^{208}Pb/^{204}Pb$ ratio were about 500 ppm (2sd) and for $^{207}Pb/^{206}Pb$\;and\;^{208}Pb/^{206}Pb$ were 100~200 ppm for 200 ng of Pb in NBS 981 solution. The optimum conditions for the analysis of Pb isotope ratios with AXIOM MC for best accuracy and reproducibility were defined as follows; 1) Pb/Tl ratio is about 10 2) Pb concentration is about 100 ng/ml 3) correction for mass discrimination is performed by exponential law using 2.3887 of $^{205}Tl/^{203}Tl$ and Pb mass fractionation factor empirically obtained from $ln(^{208}Pb/^{206}Pb)-ln(^{205}Tl/^{203}Tl)$ relationship. The sample data measured with MC/ICP/MS for acid-digested and chemically separated rock samples, and acid-digested bronze samples and sediment samples coincide with those of TIMS within analytical errors. Therefore, MC/ICP/MS is a rapid analytical technique for Pb isotope ratios with the similar precision compared with TIMS.

• Analytical Science and Technology
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• v.22 no.5
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• pp.415-421
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• 2009

A study was performed to investigate the isobaric effects of impurities in isotope measurement of gadolinium by TIMS. Especially, the ratio of $^{155}Gd/^{158}Gd$ showed the higher value than that of natural gadolinium and also decreased as the measuring time increased. This phenomenon is considered to be due to the oxide form of La ($LaO^+$, m/z=155) causing to create a serious bias on the measurement of $^{155}Gd$ abundance by La as an impurity, and due to $LaO^+$ produced more than the $Gd^+$ in the early time which disappears as the time goes on because of lower melting point and ionization potential of La than Gd. Although isobaric effects from Ba($BaO^+$), Ce($CeO^+$), Sm($SmO^+$), La($LaO^+$), and $K_4{^+}$(m/z=156)-cluster were detected even when blank rhenium filaments were used, these could be avoided by preconditioning(baking out) the filament. And we found that the measurement of $GdO^+$ instead of $Gd^+$ is more suitable in avoiding the isobaric effect from impurities such as La, Ce and Ba in the measurement of Gd isotope only in case of absence or extremely low level of Yb, Sm, Dy, Er, Lu.

• Korean Journal of Materials Research
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• v.2 no.1
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• pp.35-42
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• 1992

Thermal behavior of residue and damaged layer formed by reactive ion etching (RIE) in $CHF_3/C_2F_6$ were investigated using X-ray photoelectron spectroscopy(XPS) and secondary ion mass spec-trometry(SIMS) techniques. Decomposition of polymer residue film begins at $200^{\circ}C$ and above $400^{\circ}C$ carbon compound as graphite mainly forms by in-situ resistive heating. It reveals that thermal decomposition of residue can be completed by rapid thermal anneal treatment above $800^{\circ}C$ under nitrogen atmosphere and out-diffusion of carbon and fluorine of damaged layer is observed.

• The Journal of the Petrological Society of Korea
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• v.10 no.3
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• pp.133-147
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• 2001

Recently developing method of age determination using stepwise dissolution technique to expand the applicability of absolute age determination significantly is evaluated whether it is applicable to the Korean samples. The materials selected for the study are uranium-bearing black slates from Changni Formation of Ogcheon metamorphic belt, tourmaline separated from Naedeongni granite of Yeongnam massif, garnet and ilmenite separated from ilmenite-bearing anorthositic rock of Yeongnam massif, scheelites from Ogbang mine, and magnetite separated from Gyemyeongsan Formation of Ogcheon metamorphic belt. For the stepwise dissolution, various acid steps with different normalities and different durations were applied to leach the samples. The leachate from each step was analyzed to determine the Pb isotopic composition and concentrations of Pb and U using thermal ionization mass spectrometer. The black slates from the Changni Formation and the tourmaline from the Naedeongni granite reveal significant variation of Pb isotopic composition, which reveals the potential of such stepwise dissolution technique as a dating method. The behaviors of uranium and lead during the each stage of step leaching are different, which seem to reflect the differences in positions within the crystal lattices depending upon mineral species.

• Polymer(Korea)
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• v.39 no.2
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• pp.346-352
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• 2015

Polyalphaolefin (PAO) is a synthetic lubricant that is superior to mineral-based lubricants in the terms of physical and chemical characteristics such as low pour point, high viscosity index (VI), and thermal and oxidation stability. Several kinds of PAOs have been synthesized by using 1-pentene, 1-hexene, 1-octene, or 1-dodecene as monomer with three kinds of aluminum-based Lewis acid catalysts via cationic polymerization. The control of the catalytic performance and physical properties of PAO such like molecular weight, kinematic viscosity, pour point, and viscosity index was done by changing polymerization parameters. The alkyl aluminum halide-based catalysts show better catalytic activity than that of the conventional $AlCl_3$ catalyst. The microstructure of PAO was investigated by means of TOF-MS (time of flightmass spectroscopy) analysis in order to elucidate the correlation between the performances of the lubricant (VI, pour point) and the molecular structure of PAO. The VI of PAO increases with increases in the carbon number of ${\alpha}$-olefin. In other words, the performances of PAO as a lubricant strongly depended on the branch length of PAO.