• Title/Summary/Keyword: bulk temperature

검색결과 1,307건 처리시간 0.033초

Novel stability indicating high-performance liquid chromatography method for the separation and simultaneous quantification of acalabrutinib and its impurities in pharmaceutical formulation

  • Venu Gopal Kamani;Sujatha M;Guna Bhushana Daddala
    • 분석과학
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    • 제36권1호
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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.

Influence of various metal oxides (PbO, Fe2O3, MgO, and Al2O3) on the mechanical properties and γ-ray attenuation performance of zinc barium borate glasses

  • Aljawhara H. Almuqrin;K.A. Mahmoud;U. Rilwan;M.I. Sayyed
    • Nuclear Engineering and Technology
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    • 제56권7호
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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.

Highly Doped Nano-crystal Embedded Polymorphous Silicon Thin Film Deposited by Using Neutral Beam Assisted CVD at Room Temperature

  • 장진녕;이동혁;소현욱;홍문표
    • 한국진공학회:학술대회논문집
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    • 한국진공학회 2012년도 제43회 하계 정기 학술대회 초록집
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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.

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$^{17}O$ NMR 기법을 이용한 상자성 자기공명조영제의 물분자 교환에 관한 연구 ($^{17}O$ NMR Study On Water Excharge Rate of Paramagnetic Contrast Agents)

  • Yongmin Chang;Sung Wook Hong;Moon Jung Hwang;Il Soo Rhee;Duk-Sik Kang
    • Investigative Magnetic Resonance Imaging
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    • 제5권1호
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    • pp.33-37
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    • 2001
  • 목적 : 자성 자기공명조명제의 효율을 결정하는데는 상자성물질의 물분자 결합위치에 구속되어 있는 물분자와 자유 물분자사이의 물분자 교환율이 매우 중요한 역할을 담당한다. 따라서 본 연구에서는 $^{17}O-NMR$기법을 사용하여 현재 상용화 되어 있는 Gd 자기공명조영제 및 최근 간특이성 자기공명조영제로 제안되고 있는 Gd-EOB-DTPA의 물분자 교율을 측정하고자 하였다. 대상 및 방법 본 연구에 사용된 조영제는 Gd-DTPA, Gd-DTPA-BMA, Gd-DOTA, Gd-EOB-DTPA 이며 여기에 Isotech 사의 5% $^{17}O$로 치환된 증류수를 혼합하여 사용하였다. 결과적인 시료의 pH는 buffer용액을 사용하여 pH=7로 고정하였으며 다양한 온도에서 Bruker-600 (14.1 T, 81.3 MHz)모델의 NMR장비를 사용하여 측정하였다. 에코열 24개의 Carr-Purcell-Meiboom-Gill (CPMG) 펄스 시권스를 사용하여 $^{17}O$의 스핀-스핀 이완시간(T2)을 측정하고 이렇게 얻어진 T2 데이터는 최소자승법을 이용하여 Solomon-Bloembergen방정식에 fitting시켜서 최종적으로 각 조명제의 물분자 교환율을 계산하였다. 결과 : 측정된 각 조영제의 물분자 교환시간은 300k의 온도에서는 Gd-DTPA의 경우 0.427, Gd-DTPA-BMA의 경우 $1.99{\;}{\mu}s$, Gd-DOTA의 경우 $0.27{\;}{\mu}s$, Gd-EOB-DTPA의 경우 $0.11{\;}{\mu}s$로 나타났으며 이러한 물분자 교환시간은 온도에 따라 변화함을 알았다. 물분자 교환시간의 온도 의존성은 모든 조영제에서 지수함수의 형태로 나타났으나 조영제에 따라 온도가 올라감에 따라 물분자 교환시간이 감소하는 감소율에서는 차이를 나타내었다. 결론 : 상자성 조영제의 relaxation enhancement 기전을 이해하는데는 물분자 교환율에 대한 정보가 매우 중요하며 이러한 물분자 교환율을 정확히 측정하는데는 $^{17}O-NMR$기법이 매우 유용함을 알 수 있었다.

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오일팜 바이오매스의 자원화 연구 V - 오일팜 바이오매스 펠릿의 반탄화 연구 - (Study of Oil Palm Biomass Resources (Part 5) - Torrefaction of Pellets Made from Oil Palm Biomass -)

  • 이지영;김철환;성용주;남혜경;박형훈;권솔;박동훈;주수연;임현택;이민석;김세빈
    • 펄프종이기술
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    • 제48권2호
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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.

Sb/Bi비에 따른 5원계 바리스터의 소결거동 및 전기적 특성(II) : ZnO-Bi2O3-Sb2O3-Co3O4-Cr2O3 (Sintering and Electrical Properties According to Sb/Bi Ratio(II) : ZnO-Bi2O3-Sb2O3-Co3O4-Cr2O3 Varistor)

  • 홍연우;이영진;김세기;김진호
    • 한국재료학회지
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    • 제22권12호
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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.

황금 GAP 지침 설정을 위한 건조방법, 저장조건 및 포장재료에 따른 품질변화 (Changes in Quality by Drying Methods, Different Storage Conditions and Package Mediums for Established GAP Guide Book in Scutellaria baicalensis Georgi)

  • 김명석;김길자;최진경;권오도;박흥규;김현우;김성일;김영국;차선우;심재한
    • 한국약용작물학회지
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    • 제25권2호
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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.

초음파 열분해법를 이용한 ZnO 성장 (Growth of ZnO Film by an Ultrasonic Pyrolysis)

  • 김길영;정연식;변동진;최원국
    • 한국세라믹학회지
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    • 제42권4호
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    • pp.245-250
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    • 2005
  • 단결정 사파이어 (0001) 기판 위에 저가의 초산아연(Zinc Acetate Dehydrate; ZAH) 전구체를 이용하여 초음파 열분해법과 Ar 가스를 이용한 ZnO 박막을 성장시켰다. Thermogravimetry-Differential Scanning Calorimetry(TG-DSC) 초산아연의 열분해 과정을 조사하여 $380^{\circ}C$ 이상에서 ZnO로 분해되는 것을 확인하였다. $380-700^{\circ}C$에서 증착된 ZnO 박막은 모두 ZnO (002), (101) 결정면으로 부터의 회절피크를 보여주고 있었으며, $400^{\circ}C$ 박막의 경우 c-압축 스트레인 ${\Sigma}Z=0.2\%$, 압축 응력 $\sigma=-0.907\;GPa$이 작용하고 있음을 알 수 있었다. 전자 현미경을 이용한 미세 구조의 관찰을 통하여 $380-600^{\circ}C$에서는 초산아연과 ZnO 초미세 입자가 혼합된 aggregate 형태의 결정립을 형성하고 있었으며, nanoblade 형태의 미세구조를 보였다. 한편 $700^{\circ}C$에서 증착된 박막내의 결정립은 찌그러진 육방정계의 형태를 취하고 있으며, 10-25nm 정도의 부결정림 초미세 ZnO 입자로 이루어져 있음을 알 수 있었다. 초미세 입자의 형성을 임의 핵형성 기구(random nucleation mechanism)로 설명하였고, photoluminescence(PL) 측정을 통하여 광 특성을 조사하였다.

저온 산화공정에 의해 낮은 Dit를 갖는 실리콘 산화막의 제조 (Preparation of the SiO2 Films with Low-Dit by Low Temperature Oxidation Process)

  • 전법주;정일현
    • 공업화학
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    • 제9권7호
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    • pp.990-997
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    • 1998
  • ECR 산소플라즈마를 이용하여 저온 확산법에 의해 서로 다른 종류의 기판에 마이크로파 출력, 기판의 위치 등을 실험변수로 실리콘 산화막을 제조하고, 열처리 전 후 물리 화학적 특성을 분석하여 Si/O 의 조성비, 산화막 표면의 morphology와 전기적 특성과의 관계를 살펴보았다. 마이크로파 출력이 높은 영역에서, 산화속도는 증가하지만 식각으로 인하여 표면조도가 증가하였다. 따라서 막내에 결함이 증가하고 기판자체에 걸리는 DC bias의 증가로 기상에 존재하는 산소 양이온이 다량 함유되어 산화막의 질이 저하되었다. 기판의 종류에 따라 기상에 존재하는 산소 양이온의 함량은 Si(100) $Si/SiO_2$계면에 존재하는 결함들은 줄일 수 있으나, 고정전하와 계면포획전하 밀도는 열처리와 무관하고 단지 기상에 존재하는 반응성 산소이온의 양과 기판자체 DS bias에 의존하였다. 마이크로파 출력이 300, 400 W인 실험조건에서 표면조도가 낮고, 계면결함밀도가 ${\sim}9{\times}10^{10}cm^{-2}eV^{-1}$$Si/SiO_2$계면에서 결함이 적은 양질의 산화막이 얻어졌다.

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초음파 진동자에 의해 유도된 음향유동을 이용한 첨단 냉각법 (A Novel Cooling Method by Acoustic Streaming Induced by Ultrasonic Resonator)

  • 노병국;이동렬
    • 한국음향학회지
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    • 제22권3호
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    • pp.217-223
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    • 2003
  • 30 ㎑의 초음파 (ultrasonic wave)의 미세 진동에 의해서 유도된 음향유동 (acoustic streaming)에 의한 공기대류를 이용한 새로운 냉각방법을 소개한다. 초음파 진동은 압전소자 (piezoelectric device)에 의해서 얻어지며 50 m 정도의 진동진폭을 얻기 위해 기계적 진동 증폭자인 혼 (horn)을 추가하여 전체 진동 시스템이 공진하도록 구성된다. 음향유동에 의한 열전달 효과의 상승을 측정하기 위해 열원 (heat source) 및 열원 주위의 대기의 온도변화를 실시간으로 측정하였다. 초음파 진동 시작 후 시간지연 없이 음향유동이 유도되어 진동자 주위의 대량의 공기유동으로 인한 급격한 온도감소가 관찰되었다. 또한 열원과 진동자와의 거리가 방사 (radiation)되는 음파 (sound wave)의 반파장 (half wave length)의 정배수가 될 때 열원의 냉각효과가 극대화됨을 실험적으로 관찰하였다. 이는 음파의 공진현상에 기인한 것으로 이론적 고찰을 통한 검증 또한 수행되었다. 음향유동을 이용한 냉각법의 장점은 초음파 진동을 이용하기 때문에 무소음이며 이동 형태의 부품이 없기 때문에 반영구적으로 사용할 수 있다. 또한 기존의 전기모터를 이용한 냉각팬 (cooling fan)으로는 냉각이 어려운 초소형 기전시스템 (MEMS)의 냉각법으로 사용될 수 있는 첨단 냉각방법이다.