• Analytical Science and Technology
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• v.36 no.1
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• pp.32-43
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• 2023

This study reports for the first time about a stability indicating RP-HPLC method for qualitative and quantitative determination of acalabrutinib in bulk and dosage form and in presence its impurities 1, 2 and 3. The chromatographic separation was carried on Zorbax XDB-C18 (250×4.6 mm; 5 µ id) as stationary phase, Phosphate buffer pH 6.4 and methanol 80:20 (v/v) as mobile phase at a flow rate of 1.0 mL/min, UV detection was carried at wavelength of 238 nm and the analysis was completed with a run time of 15 min. In these conditions the retention time of acalabrutinib and its impurities 1, 2 and 3 was observed to be 3.50, 4.83, 8.40 and 9.93 min respectively. The method was validated for system suitability, range of analysis, precision, specificity, stability and robustness. Spiked recovery at 50 %, 100 % and 150 % was carried for both standard and impurities and the acceptable % recovery of 98-102 was observed for acalabrutinib and both impurities studied and the % RSD in each spiked level was found to be less than 2. Stability tests were done through exposure of the analyte solution to five different stress conditions i.e expose to 1N hydrochloric acid, 1 N sodium hydroxide, 3 % peroxide, 80 ℃ temperature and UV radiation at 254 nm. In all the degradation condition, standard drug acalabrutinib was detected along with both the impurities studied and the degradation products were successfully separated. In the formulation analysis there is no other chromatographic detection of other impurities and formulation excipients. Hence the developed method was found to be suitable for the quantification of acalabrutinib and can separate and analyse impurities 1 and 2.

• Nuclear Engineering and Technology
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• v.56 no.7
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• pp.2711-2717
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• 2024

The current work aims to fabricate metal oxide-doped (PbO, Fe₂O₃, MgO, and Al₂O₃, each of which boasts a purity of 99%) zinc barium borate glasses through the melt quenching technique at the 1000 ℃ melting temperature. The results showed that adding 5 mol.% of metal oxides PbO, Fe₂O₃, Al₂O₃, and MgO increases the density of the zinc barium borate glasses. Additionally, the fabricated glasses' mechanical properties were determined based on the Makishima-Mackenzie model, which proved that the highest mechanical properties were achieved for glasses doped with Al₂O₃ compounds. The mechanical moduli for the glasses doped with Al₂O₃ reach 80.95 GPa (Young), 59.90 GPa (bulk), 31.75 GPa (shear), and 102.23 GPa (longitudinal). Additionally, the Al₂O₃-doped glasses' microhardness reaches 4.77 GPa. Moreover, estimation of the fabricated glasses' gamma-ray shielding capacity utilized Monte Carlo simulation. The highest linear attenuation coefficients are 29.132, 19.906, 19.243, and 18.923 cm^-1 obtained at 0.033 MeV for glasses dopped by PbO, Fe₂O₃, MgO, and Al₂O₃, respectively. Therefore, glasses doped with 5 mol.% of PbO have high gamma-ray shielding capacities followed by glasses doped by Fe₂O₃.

• Proceedings of the Korean Vacuum Society Conference
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• 2012.08a
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• pp.154-155
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• 2012

The promise of nano-crystalites (nc) as a technological material, for applications including display backplane, and solar cells, may ultimately depend on tailoring their behavior through doping and crystallinity. Impurities can strongly modify electronic and optical properties of bulk and nc semiconductors. Highly doped dopant also effect structural properties (both grain size, crystal fraction) of nc-Si thin film. As discussed in several literatures, P atoms or radicals have the tendency to reside on the surface of nc. The P-radical segregation on the nano-grain surfaces that called self-purification may reduce the possibility of new nucleation because of the five-coordination of P. In addition, the P doping levels of ${\sim}2{\times}10^{21}\;at/cm^3$ is the solubility limitation of P in Si; the solubility of nc thin film should be smaller. Therefore, the non-activated P tends to segregate on the grain boundaries and the surface of nc. These mechanisms could prevent new nucleation on the existing grain surface. Therefore, most researches shown that highly doped nc-thin film by using conventional PECVD deposition system tended to have low crystallinity, where the formation energy of nucleation should be higher than the nc surface in the intrinsic materials. If the deposition technology that can make highly doped and simultaneously highly crystallized nc at low temperature, it can lead processes of next generation flexible devices. Recently, we are developing a novel CVD technology with a neutral particle beam (NPB) source, named as neutral beam assisted CVD (NBaCVD), which controls the energy of incident neutral particles in the range of 1~300eV in order to enhance the atomic activation and crystalline of thin films at low temperatures. During the formation of the nc-/pm-Si thin films by the NBaCVD with various process conditions, NPB energy directly controlled by the reflector bias and effectively increased crystal fraction (~80%) by uniformly distributed nc grains with 3~10 nm size. In the case of phosphorous doped Si thin films, the doping efficiency also increased as increasing the reflector bias (i.e. increasing NPB energy). At 330V of reflector bias, activation energy of the doped nc-Si thin film reduced as low as 0.001 eV. This means dopants are fully occupied as substitutional site, even though the Si thin film has nano-sized grain structure. And activated dopant concentration is recorded as high as up to 1020 #/$cm^3$ at very low process temperature (＜ $80^{\circ}C$) process without any post annealing. Theoretical solubility for the higher dopant concentration in Si thin film for order of 1020 #/$cm^3$ can be done only high temperature process or post annealing over $650^{\circ}C$. In general, as decreasing the grain size, the dopant binding energy increases as ratio of 1 of diameter of grain and the dopant hardly be activated. The highly doped nc-Si thin film by low-temperature NBaCVD process had smaller average grain size under 10 nm (measured by GIWAXS, GISAXS and TEM analysis), but achieved very higher activation of phosphorous dopant; NB energy sufficiently transports its energy to doping and crystallization even though without supplying additional thermal energy. TEM image shows that incubation layer does not formed between nc-Si film and SiO2 under later and highly crystallized nc-Si film is constructed with uniformly distributed nano-grains in polymorphous tissues. The nucleation should be start at the first layer on the SiO2 later, but it hardly growth to be cone-shaped micro-size grains. The nc-grain evenly embedded pm-Si thin film can be formatted by competition of the nucleation and the crystal growing, which depend on the NPB energies. In the evaluation of the light soaking degradation of photoconductivity, while conventional intrinsic and n-type doped a-Si thin films appeared typical degradation of photoconductivity, all of the nc-Si thin films processed by the NBaCVD show only a few % of degradation of it. From FTIR and RAMAN spectra, the energetic hydrogen NB atoms passivate nano-grain boundaries during the NBaCVD process because of the high diffusivity and chemical potential of hydrogen atoms.

• Investigative Magnetic Resonance Imaging
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• v.5 no.1
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• pp.33-37
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• 2001

Purpose : The water exchange rate between bulk water and bound water is an important parameter in deciding the efficiency of paramagnetic contrast agents. In this study, we evaluated the water exchange rates of various Gd-chelates using oxygen-17 NMR technique. Material and Methods : The samples (Gd-DTPA, Gd-DTPA-BMA, Gd-DOTA, Gd-EOB-DTPA) were prepared by mixing 5% $^{17}O-enriched$ water (Isotech, USA). The pH of the samples was adjusted to physiological value [pH=7.0] by buffer solution. The variable temperature $^{17}O-NMR$ measurements were performed using Bruker-600 (14.1 T, 81.3 MHz) spectrometer. Bruker VT-1000 temperature control units were used to stabilize the temperature. The $^{17}O$ spin-spin relaxation times (T2) were measured using Carr-Purcell-Meiboom-Gill (CPMG)I pulse sequence with 24 echo trains. The variable temperature T2 relaxation data were then fitted into Solomon-Bloembergen equations using least square fit algorithm to estimate the water exchange times. Results : From the measured $^{17}O-NMR$ relaxation rates, the determined water exchange rates at 300K are $0.42{\;}{\mu}s$ for Gd-DTPA, $1.99{\;}{\mu}s$ for Gd-DTPA-BMA, $0.27{\;}{\mu}s$ for Gd-DOTA, and $0.11{\;}{\mu}s$ for Gd-EOB-DTPA. The Gd-DTPA-BMA showed slowest exchange whereas Gd-EOB-DTPA had fastest water exchange rate. In addition, it was found that the water exchange rates (${\tau}_m$) of all samples had exponential temperature dependence with different decay constant. Conclusion : $^{17}O-NMR$ relaxation rate measurements, when combined with variable temperature technique, provide a solid tool for studying water exchange rate, which is very important in investigating the detailed mechanism of relaxation enhancement effect of the paramagnetic contrast agents.

• Journal of Korea Technical Association of The Pulp and Paper Industry
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• v.48 no.2
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• pp.34-45
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• 2016

Global warming and climate change have been caused by combustion of fossil fuels. The greenhouse gases contributed to the rise of temperature between $0.6^{\circ}C$ and $0.9^{\circ}C$ over the past century. Presently, fossil fuels account for about 88% of the commercial energy sources used. In developing countries, fossil fuels are a very attractive energy source because they are available and relatively inexpensive. The environmental problems with fossil fuels have been aggravating stress from already existing factors including acid deposition, urban air pollution, and climate change. In order to control greenhouse gas emissions, particularly CO2, fossil fuels must be replaced by eco-friendly fuels such as biomass. The use of renewable energy sources is becoming increasingly necessary. The biomass resources are the most common form of renewable energy. The conversion of biomass into energy can be achieved in a number of ways. The most common form of converted biomass is pellet fuels as biofuels made from compressed organic matter or biomass. Pellets from lignocellulosic biomass has compared to conventional fuels with a relatively low bulk and energy density and a low degree of homogeneity. Thermal pretreatment technology like torrefaction is applied to improve fuel efficiency of lignocellulosic biomass, i.e., less moisture and oxygen in the product, preferrable grinding properties, storage properties, etc.. During torrefacton, lignocelluosic biomass such as palm kernell shell (PKS) and empty fruit bunch (EFB) was roasted under an oxygen-depleted enviroment at temperature between 200 and $300^{\circ}C$. Low degree of thermal treatment led to the removal of moisture and low molecular volatile matters with low O/C and H/C elemental ratios. The mechanical characteristics of torrefied biomass have also been altered to a brittle and partly hydrophobic materials. Unfortunately, it was much harder to form pellets from torrefied PKS and EFB due to thermal degradation of lignin as a natural binder during torrefaction compared to non-torrefied ones. For easy pelletization of biomass with torrefaction, pellets from PKS and EFB were manufactured before torrefaction, and thereafter they were torrefied at different temperature. Even after torrefaction of pellets from PKS and EFB, their appearance was well preserved with better fuel efficiency than non-torrefied ones. The physical properties of the torrefied pellets largely depended on the torrefaction condition such as reaction time and reaction temperature. Temperature over $250^{\circ}C$ during torrefaction gave a significant impact on the fuel properties of the pellets. In particular, torrefied EFB pellets displayed much faster development of the fuel properties than did torrefied PKS pellets. During torrefaction, extensive carbonization with the increase of fixed carbons, the behavior of thermal degradation of torrefied biomass became significantly different according to the increase of torrefaction temperature. In conclusion, pelletization of PKS and EFB before torrefaction made it much easier to proceed with torrefaction of pellets from PKS and EFB, leading to excellent eco-friendly fuels.

• Korean Journal of Materials Research
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• v.22 no.12
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• pp.682-688
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• 2012

In this study we aimed to examine the co-doping effects of 1/6 mol% $Co_3O_4$ and 1/4 mol% $Cr_2O_3$ (Co:Cr = 1:1) on the reaction, microstructure, and electrical properties, such as the bulk defects and the grain boundary properties, of ZnO-$Bi_2O_3-Sb_2O_3$ (ZBS; Sb/Bi = 0.5, 1.0, and 2.0) varistors. The sintering and electrical properties of Co,Cr-doped ZBS, ZBS(CoCr) varistors were controlled using the Sb/Bi ratio. Pyrochlore ($Zn_2Bi_3Sb_3O_{14}$), ${\alpha}$-spinel ($Zn_7Sb_2O_{12}$), and ${\delta}-Bi_2O_3$ were formed in all systems. Pyrochlore was decomposed and promoted densification at lower temperature on heating in Sb/Bi = 1.0 by Cr rather than Co. A more homogeneous microstructure was obtained in all systems affected by ${\alpha}$-spinel. In ZBS(CoCr), the varistor characteristics were improved (non-linear coefficient, ${\alpha}$ = 20~63), and seemed to form ${Zn_i}^{{\cdot}{\cdot}}$(0.20 eV) and ${V_o}^{\cdot}$(0.33 eV) as dominant defects. From impedance and modulus spectroscopy, the grain boundaries were found to be composed of an electrically single barrier (0.94~1.1 eV) that is, however, somewhat sensitive to ambient oxygen with temperature. The phase development, densification, and microstructure were controlled by Cr rather than by Co but the electrical and grain boundary properties were controlled by Co rather than by Cr.

• Korean Journal of Medicinal Crop Science
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• v.25 no.2
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• pp.89-94
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• 2017

Background: The purpose of improving the quality of oriental medicinal herbs is to contribute to the improvement of the income of farm. The present study investigated the effect of reasonable drying methods, different storage conditions and packageing materials on quality and stability of Scutellaria baicalensis Georgi and for developing GAP (good agricultural practice) guide book. Methods and Results: Three methods of drying Scutellaria baicalensis roots produced over two years were used to estimate loss rate owing to drying, storage, and packaging. The methods of drying were categorized into natural drying (36 - 60 h by sunshine), drying with heat dryer (2 - 10 h), or drying with gas bulk dryer (2 - 10 h). After cleaning, and initial drying for a few days under controlled temperature conditions, the second phase of drying was carried out at 35, 45 and $55^{\circ}C$. Changes in hunter color values and quality under the two studied storage treatments (at $20^{\circ}C$ indoors and at $4^{\circ}C$ in a refigerator) were evaluated. Storage period for 60, 120, and 180 days in three packaging materials, PE (polyethylene package), PP (polypropylene gunnysack), and WP (watertight packing paper) were studied. Conclusions: Initial cleaning, reasonable gas drying and hot air drying, and drying in an oven at 35 and $45^{\circ}C$ after cutting the roots resulted in the lowest loss rates in S. Baicalensis root. Hunter color valuse indicated that stroage of dry roots at room temperature was better than PP packaging, and that cold stroage was better than PE packaging for long-term stability.

• Journal of the Korean Ceramic Society
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• v.42 no.4
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• pp.245-250
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• 2005

ZnO was deposited on sapphire single crystal substrate by an ultrasonic pyrolysis of Zinc Acetate Dehydrate (ZAH) with carrying Ar gas. Through Thermogravimetry-Differential Scanning Calorimetry(TG-DSC), zinc acetate dihydrate was identified to be dissolved into ZnO above $380^{\circ}C$. ZnO deposited at $380-700^{\circ}C$ showed polycrystalline structures with ZnO (101) and ZnO (002) diffraction peaks like bulk ZnO in XRD, and from which c-axis strain ${\Sigma}Z=0.2\%$ and compressive biaxial stress$\sigma=-0.907\;GPa$ was obtained for the ZnO deposited $400^{\circ}C$. Scanning electron microscope revealed that microstructures of the ZnO were dependent on the deposition temperature. ZnO grown below temperature $600^{\circ}C$ were aggregate consisting of zinc acetate and ZnO particles shaped with nanoblades. On the other hand the grain of the ZnO deposited at $700^{\circ}C$ showed a distorted hexagonal shape and was composed of many ultrafine ZnO powers of 10-25 nm in size. The formation of these ulrafine nm scale ZnO powers was explained by the model of random nucleation mechanism. The optical property of the ZnO was analyzed by the photoluminescence (PL) measurement.

• Applied Chemistry for Engineering
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• v.9 no.7
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• pp.990-997
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• 1998

In this work, the $SiO_2$ films on the silicon substrate with different orientations were first prepared by the low temperature process using the ECR plasma diffusion as a function of microwave power and oxidation time. Before and after thermal treatment, the surface morphology, Si/O ratio from physicochemical properties, and the electrical properties of the oxide films were also investigated. The oxidation rate increased with microwave power, while surface morphology showed the nonuniform due to etching. The film quality, therefore, was lowered with increasing the defect by etching and the content of positive oxide ions in the oxide films from bulk by higher self-DC bias. The content of positive oxide ions in the oxide films with different Si orientations showed Si(100) < Si(111) < poly Si. The defects in $Si/SiO_2$ interface of $SiO_2$ film could be decreased by annealing, while $Q_{it}$ and $Q_f$ were independent of thermal treatment and the dependent on concentration of reactive oxide ions and self-DC bias of substrate. At microwave power of 300, and 400 W, the high quality $SiO_2$ film that had lower surface roughness and defect in $Si/SiO_2$ interface was obtained. The value of interface trap density, then, was ${\sim}9{\times}10^{10}cm^{-2}eV^{-1}$.

• The Journal of the Acoustical Society of Korea
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• v.22 no.3
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• pp.217-223
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• 2003

A novel cooling method induced by acoustic streaming generated by ultrasonic vibration at 30㎑ is presented. Ultrasonic vibration is obtained by piezoelectric devices and the maximum vibration amplitude of 50 m is achieved by including a horn, mechanical vibration amplifier in the system and making the complete system resonate. To investigate the enhancement of heat transfer capability of acoustic streaming, the temperature variations of heat source and air in the vicinity of heat source are measured in real-time. It is observed that acoustic streaming is instantly induced by ultrasonic vibration, resulting in the significant temperature drop due to the bulk air flow caused by acoustic streaming. In addition, it is observed that the cooling effect on the heat source is maximized when the gap between the ultrasonic vibrator and heat source coincides with the multiples of half-wavelength of the ultrasonic wave. This fact results from the resonance of the sound wave. The theoretical analysis of the dependence on the gap is also accomplished and verified by experiment. The advantage of the proposed cooling method by acoustic streaming is noise-free due to the ultrasonic vibration and maintenance-free because of the absence of moving parts. Moreover. This cooling method can be utilized to the nano and micro-electro mechanical systems, where the fan-based conventional cooling method can not be employed.