• Journal of the Korean Chemical Society
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• v.36 no.2
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• pp.255-260
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• 1992

A procedure for spectrophotometric determination of traces of phosphorus(P) in high-purity trichlorosilane(TCS) is proposed using an adsorptive separation. $PCl_3$, which is a dominant P impurity within TCS, is first oxidized by oxygen to a stable form as $POCl_3$. $AlCl_3$ is selected as an adsorbent which forms a thermally stable complex with $POCl_3$ in TCS and can be well dissolved in aqueous ethanol solution. The proposed adsorptive separation method is free from the formation of silica gel and gas bubbles during the colorimetric analysis of TCS. The method reveals that the P concentration in a semiconductor-grade TCS is 5.32 ${\mi}g/l$ within the standard deviation of ${\pm}$ 17%. On the other hand, the P concentration of the purified TCS which is separated from the $AlCl_3$${\cdot}$$POCl_3$ complex is reduced to be less than 0.15 ${\mi}g/l$, showing the efficient applicability of $AlCl_3$ to the wet chemical analysis. The proposed method is also tested to verify the effectiveness of other well-known adsorbents.

• Membrane Journal
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• v.21 no.1
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• pp.62-71
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• 2011

Highly enriched oxygen is used in energy-efficient combustion due to decreased non-flammable nitrogen, while high purity nitrogen is used for explosion proof in the LNG ships and keeping the freshness of green stuffs. Membrane technology can be used in these $O_2$ and $N_2$ generation with low energy consumption. In this study, PES was used as a membrane material and 1-methyl-2-pyrollidone (NMP) and acetone were employed as a good solvent and nonsolvent addictive (swelling agent to PES), respectively. Dope solutions were prepared by changing the content of acetone (0, 6.5, 15, 25, 31.5 wt%) in 37 wt% PES solutions. Hollow fiber spinning was performed at 0~10 cm of air-gap distances for each dope solution. $O_2/N_2$ selectivity and permeability were investigated by comparing of hollow fibers coated or not by silicons. $O_2/N_2$ selectivity increased and permeance of $O_2$ and $N_2$ decreased with increasing air-gap height independently of acetone addictions. Optimized PES hollow fibers were obtained with 37/6.5/56.5 wt% PES/acetone/NMP dope solution and 10 cm air-gap, which showed 7.3 of $O_2/N_2$ selectivity and 4.3 GPU of $O_2$ permeability after silicon coating.

• Journal of Hydrogen and New Energy
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• v.7 no.1
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• pp.81-92
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• 1996

The Ar/Ar-$H_2$ plasma method was applied to reduce oxides and refine metals of V, Ta and B. In addition, the high temperature chemical reaction in Ar plasma and of the refining reaction in the Ar-(20%)$H_2$ plasma were analyzed. The crude V of 96wt% purity was obtained at the ratio of $C/V_{2}O_{5}=4.50$ by the Ar plasma reduction grade and the maximum reduction was obtained at $C/V_{2}O_{5}=4.50$ due to the $O_{2}$ loss from the thermal decomposition of vanadium oxide. In the Ar-(20%)$H_2$ plasma refining, the metallic V of 99.2wt% was produced at the ratio of $C/V_{2}O_{5}=4.40$. It was considered that a main refining reaction resulted from the chemical reaction between the residual carbon and residual oxygen. The metallic Ta of 99.8wt% was obtained at the ratio of $C/Ta_{2}O_{5}=5.10$ in a Ar plasma reduction and the Oz loss from the thermal decomposition of tantalum pentoxide did not take place. The deoxidation reaction was more significant than the decarburization reaction in the Ar-(20%)$H_2$ plasma refining and the metallic Ta of 99.9wt% was produced within the range of $C/Ta_{2}O_{5}$ ratio of 4.50 to 5.10. The Vickers hardness of Ta in the above mentioned range was about 220Hv due to the decrease in a residual oxygen by the deoxidation reaction. On the other hand, C is no suitable agent for the reduction of $B_{2}O_{3}$ by the Ar and Ar-$H_2$ plasma. But Fe-B-Si alloy was produced with the reduction of $B_{2}O_{3}$ in the melt when Fe, C, $B_{2}O_{3}$, and ferroboron mixtures were melted by the high frequency induction melting.

• Analytical Science and Technology
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• v.22 no.4
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• pp.285-292
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• 2009

It has been observed that, after long term storage, some ammunitions are misfired by tamping (combustionstopping) due to aging of the chemicals loaded in the ammunitions. Used in ammunitions are percussion powder which provides the initial energy, igniter which ignites the percussion powder, and a delay system that delays the combustion for a period of time. The percussion powder is loaded first, followed by the igniter and then the delay system, and the ammunitions explode by the energy being transferred in the same order. Tamping occurs by combustion-stopping of the igniter or insufficient energy transfer from the igniter to the delay system or the combustion-stopping of the delay system, which are suspected to be caused by low purity of the components, inappropriate mixing ratio, size distribution of particulate components, type of the binder, blending method, hydrolysis by the humidity penetrated during the long term storage, and chemical changes of the components by high temperature. Goal of this study is to find the causes of the combustion-stopping of the igniter and the delay system of the ammunitions after long term storage. In this study, a method was developed for testing of the combustion-stopping, and the size distributions of the particulate components were analyzed with field-flow fractionation (FFF), and then the mechanism of chemical change during long term storage was investigated by thermal analysis (differential scanning calorimetry), XRD (X-ray diffractometry), and XPS (X-ray photoelectron spectroscopy). For the ignition system, M (metal)-O (oxygen) and M-OH peaks were observed at the oxygen's 1s position in the XPS spectrum. It was also found by XRD that $Fe_3O_4$ was produced. Thus it can be concluded that the combustion-stopping is caused by reduction in energy due to oxidation of the igniter.

• The Korean Journal of Nuclear Medicine
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• v.36 no.3
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• pp.195-202
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• 2002

Purpose: For clinical application of beta-emitter labeled antibody, high specific activity is imporiant. Carrier-free $^{188}Re$ from $^{188}W/^{188}Re$ generator is an ideal radionuclide for this purpose. However, low stability of $^{188}Re$ labeled antibody, especially in high specific activity, due to radiolytic decomposition by high energy (2.1 MeV) beta ray was problem. We studied the stability of $^{188}Re$ labeled antibody, and stabilizing effect of several stabilizers. Materials and Methods: Pre-reduced monoclonal antibody (CEA79.4) was labeled with $^{188}Re$ by incubating with generator-eluted $^{188}Re-perrhenate$ in the presence of stannous tartrate for 2 hr at room temperature. Radiochemical purity of each preparation was determined by chromatography. Human serum albumin was added to the labeled antibodies (2%). Stability of $^{188}Re-CEA79.4$ was investigated in the presence of ascorbic acid, ethanol, of Tween 80 as stabilizing agents. Results: Labeling efficiencies were $88{\pm}4%\;(n=12)$. Specific activities of $1.25{\sim}4.77MBq/{\mu}g$ were obtained. If stored after purging with $N_2$, all the preparations were stable for 10 hr. However, stability decreased in the presence of air. Perrhenate and $^{188}Re-tartrate$ was major impurity in declined preparation. colloid-formation was not a significant problem in all cases. Addition of ascorbic acid stabilized the labeled antibodies either under $N_2$ or under air by reducing the formation of perrhenate. Conclusion: High specific activity $^{188}Re$ labeled antibody is unstable, especially, in the presence of oxygen. Addition of ascorbic acid increased the stability.

• Applied Biological Chemistry
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• v.13 no.1
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• pp.1-27
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• 1970

The process of the forced aging of flue-cured tobacco leaves were studied extensively from various scientific points of view. The Flue-cured tobacco leaves were inoculated and fermented with nicotine resistant Hansenula yeast, or the leaves were subjected under simple forced aging. The above two processes of forced aging were studied from the summarized points of microbiology, physics, chemistry, and biochemistry, and the resulted products ware compared in their physical, chemical and biochemical quality determining factors with that of raw material tobacco leaves (dried-tobacco leaves) and 2 years aged high quality tobacco leaves. The summary results were as follows. 1) The Korean flue-cured tobacco leaves, were forcedly aged under the basic optimum aging condition, temperature $40^{\circ}C$, moisture contents 18%, relative humidity 74%. It was found that this aging condition was the best in bringing the quality of forcedly aged tobacco leaves to the utmost state. 2) Under this optimum temperature and moisture condition of forced aging in about 20 days the forcedly aged tobacco leaves both with yeast inoculation and without yeast inoculation showed the equivalent tobacco qualities comparable with that of more than 2 years aged tobacco leaves. 3) The forcedly aged tobacco leaves both with and without yeast inoculation under $40^{\circ}C$ temperature and $74^{\circ}C$ relative humidity achieved the necessary quality determining physical and chemical changes in about 20 days. 4) The microbial changes during the forced aging were as follows. The population of yeasts and bacteria increased until to 15 days of aging, then decreased thereafter. Whereas the molds grew continously until the end of fermentation. 5) The tobacco quality determing physico-chemico-properties of yeast inoculated aged and simple forcedly aged tobacco leaves, progressed as the follows in time. As the forced aging progresses, swelling and combustibility properties were improved. The pH, total reducing materials, total sugars, alkaloids contents decreased. The contents of organic and ether extractable materials increased. The total nitrogen, protein, crude fiber, ash contents showed no changes. The color properties, excitation purity, luminance, main wave length, showed equivalent changes comparable with that of 2 years aged tobacco leaves. 6) The changes in chemical components in yeast treated and simple forcedly aged tobacco leaves during $15{\sim}20{\;}days$ of forced aging were as follows. The following chemical components decreased as the aging. Sugars-sucrose. rhamnose, glucose. Pigments-chlorophyll, carotenes, xanthophyll and violax anthine. Polyphenols-rutin, chlorogenic and, coffeic acid. Organic acids-iso-butylic, crotonic, caprylic, galacturonic, tartaric, succinic, citric acid. Alkaloids-nicotine, nornicotine. The following components increased as the forced aging progressed. Sugars-frutose, maltose, raffinose. Amino acids-proline, cystine. Organic acids-formic, acetic, propionic, n-butyric, iso-valeric, n-valeric, malic, oxalic, malonic, ${\alpha}-ketoglutaric$, fumaric, glutaric acid. 7) During the forced aging of tobacco Leaves the oxygen-uptake decreased gradually. The enzyme activities of polyphenol oxidase, ${\beta}-amylase$ ${\alpha}-amylase$ decreased gradually. The activities of the enzymes, catalase, and invertase increased once then decreased at the later stage.