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Optimum Kinetic Parameters of Mefenamic Acid Crystallization by PBM PBM结晶甲氨酰胺的最佳动力学参数
Pub Date : 2012-07-26 DOI: 10.4236/JCPT.2012.23011
C. Serap, Yaylaci Cihan
Mefenamic acid (MA) is a high-dose, anti-inflammatory, analgesic agent that is widely prescribed for pain related to menstrual disorders. It has some negative properties, such as a high hydrophobicity with a propensity to stick to surfaces, and possess great problems during granulation and tableting. Crystallization kinetics was investigated for mefenamic acid. Availability of data on the kinetics of crystal growth is very important for the development and operation of industrial crystallisation processes. The experiments for the measurement of crystal growth kinetics were carried out using the desupersaturation curve technique based on the measurement of the solution concentration versus time in a seeded isothermal batch experiment. To predict the optimum parameters (b, kb, g, kg) for the nucleation and growth kinetics from the desupersaturation curve obtained, the Population Balance Modelling was used and solved by the method of moments. The initial values for the optimisation problem were estimated by using the approach developed by Garside et al. (1982) [1].
甲氧胺酸(MA)是一种大剂量、抗炎、止痛剂,广泛用于与月经紊乱有关的疼痛。它有一些负面的性质,如高疏水性和粘在表面的倾向,在造粒和压片过程中存在很大的问题。研究了甲氧胺酸的结晶动力学。晶体生长动力学数据的可用性对于工业结晶过程的开发和操作是非常重要的。在种子等温间歇实验的基础上,采用脱饱和曲线技术测量了溶液浓度随时间的变化,实现了晶体生长动力学的测量。为了从脱饱和曲线中预测成核和生长动力学的最佳参数(b, kb, g, kg),采用了种群平衡模型,并用矩量法求解。优化问题的初始值是使用Garside等人(1982)开发的方法来估计的。
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引用次数: 5
Design and Calculation for Test Tube with the Aim of Regulation Simultaneous Crystallization Tests 规范同步结晶试验用试管的设计与计算
Pub Date : 2012-07-26 DOI: 10.4236/JCPT.2012.23016
A. Janićijević, N. Danilović, B. Čabrić
A design for an air-cooled test tube, with a series of modular and movable rings (cylindrical “crystallization comb”), installed in a laboratory crucible furnace is presented. The setup allows easy regulation simultaneous crystallization tests of a series of different crystallization rates in several columns (matrix) of test tubes, enabling fast studies of obtaining crystals. This low-budget, portable device (i.e. adjustable airstream with more simple control options), can also be applied in tube and chamber furnaces. The relations between the crystallization rate and parameters of air-cooled test tube are given and numerically analyzed.
介绍了一种安装在实验室坩埚炉中的风冷试管的设计,该试管具有一系列模块化和可移动的环(圆柱形“结晶梳”)。该设置允许在试管的几个柱(矩阵)中轻松调节一系列不同结晶速率的同时结晶测试,从而实现对获得晶体的快速研究。这种低预算,便携式设备(即可调气流与更简单的控制选项),也可以应用于管炉和室炉。给出了结晶速率与风冷试管参数之间的关系,并进行了数值分析。
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引用次数: 0
Optical and Dielectric Studies on L-Valinium Picrate Single Crystal 苦克酸盐L-Valinium单晶的光学和介电研究
Pub Date : 2012-07-26 DOI: 10.4236/JCPT.2012.23015
P. Koteeswari, P. Mani, S. Suresh
Single crystals of L-Valinium picrate were grown from aqueous solution by slow evaporation technique. Single crystal X-ray diffraction analysis reveals that the crystal belongs to monoclinic system. The optical transmission study reveals the transparency of the crystal in the entire visible region and the cut off wave length has been found to be 470 nm. The optical band gap is found to be 2.55 eV. The transmittance of L-Valinium picrate crystal has been used to calculate the refractive index (n), the extinction coefficient (K) and both the real (er) and imaginary (ei) components of the dielectric constant as functions of wavelength. Low dielectric loss at high frequency region is indicative of enhanced optical quality with lesser defects. Photoconductivity measurements carried out on the grown crystal reveal the negative photoconducting nature.
采用慢蒸发法制备苦味酸l -缬氨酸单晶。单晶x射线衍射分析表明该晶体属于单斜晶系。光透射研究表明,该晶体在整个可见光区域都是透明的,截止波长为470nm。光学带隙为2.55 eV。利用l -苦克酸钡晶体的透射率计算了晶体的折射率(n)、消光系数(K)以及介电常数的实、虚分量(ei)随波长的变化。高频区的低介电损耗表明光学质量提高,缺陷减少。在生长晶体上进行的光导测量揭示了负光导性质。
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引用次数: 7
Resistivity Stability of Ga Doped ZnO Thin Films with Heat Treatment in Air and Oxygen Atmospheres Ga掺杂ZnO薄膜在空气和氧气环境中热处理的电阻率稳定性
Pub Date : 2012-04-24 DOI: 10.4236/JCPT.2012.22010
T. Rao, M. Kumar
The effect of annealing in air and oxygen on structural, electrical and optical properties of gallium doped ZnO thin films was investigated. The X-ray diffraction patterns showed that the films were highly preferentially oriented along (002) plane. After the heat treatment in air and oxygen environments, the intensity of (002) peak was apparently improved. It was found that heat treatment in air atmospheres lead to increase in surface roughness of the film. The GZO films annealed in oxygen at 673 K exhibited low resistivity of 4.21 × 10–3 Ω.cm, while the resistivity of film annealed in air showed a slightly higher value of 7.14 × 10–3 Ω.cm. In addition to this, all films have good optical transmittance about 80% in the visible region. It is found from the photoluminescence studies that the broad visible emissions in GZO films originated from the intrinsic shallow traps (VZn) and deep level vacancies (ZZi, OZn and Vo)
研究了在空气和氧气中退火对掺镓ZnO薄膜结构、电学和光学性能的影响。x射线衍射图表明,薄膜沿(002)平面高度优先取向。在空气和氧气环境下热处理后,(002)峰强度明显提高。结果表明,在空气中热处理可使膜的表面粗糙度增大。在673 K氧中退火的GZO薄膜的电阻率为4.21 × 10-3 Ω。而在空气中退火的薄膜的电阻率略高,为7.14 × 10-3 Ω.cm。除此之外,所有薄膜在可见光区都有良好的透光率,约为80%。从光致发光研究中发现,GZO薄膜的宽可见发射源于本征浅阱(VZn)和深能级空位(ZZi, OZn和Vo)。
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引用次数: 59
Energy Efficiency Improvement of an Industrial Crystallization Process Using Linearizing Control 利用线性化控制提高工业结晶过程的能源效率
Pub Date : 2012-04-24 DOI: 10.4236/JCPT.2012.22007
C. Damour, M. Benne, L. Boillereaux, B. Grondin-Perez, J. Chabriat
This paper illustrates the benefits of a multivariable linearizing control approach applied to an industrial crystallization process. This relevant approach is declined according to two different strategies: first, a setpoint tracking is proposed for the couple crystal mass/concentration, whereas a second way consists in tracking of crystal content and concentration. The controlled variables, unavailable online, are issued from an observer developed in previous works. The performance of these strategies, which application to cane sugar crystallization constitutes a real novelty, are compared with experimental data issued from a PID-controlled industrial plant. The results reveal a significant improvement of energy efficiency, leading to an economy of more than 10% of energy.
本文说明了多变量线性化控制方法应用于工业结晶过程的好处。根据两种不同的策略,提出了一种针对晶体质量/浓度耦合的设定值跟踪方法,而第二种方法包括跟踪晶体含量和浓度。控制变量,在线上不可用,是由以前的作品中开发的一个观察者发出的。应用于蔗糖结晶的这些策略的性能是真正的新颖,并与pid控制的工业装置的实验数据进行了比较。结果显示能源效率显著提高,节约能源10%以上。
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引用次数: 3
Kinetics Estimation and Polymorphic Transformation Modeling of Buspirone Hydrochloride 盐酸丁螺环酮的动力学评价及多态转化模型
Pub Date : 2012-04-24 DOI: 10.4236/JCPT.2012.22006
Trifkovic Milana, Rohani Sohrab, Sheikhzadeh Mehdi
In this work, solvent-mediated polymorphic transformation of metastable Form II to stable Form I of Buspirone Hy-drochloride (BUS-HCl) was studied. The polymorphic transformation was monitored using in-situ Raman spectroscopy. The solvent-mediated transformation process is governed by the dissolution of Form II and the nucleation and subsequent growth of Form I. The model parameters for each of these sub-processes were determined with the aid of experimental data including polymorphic fraction in solid phase, solute concentration, and the crystal size distribution. In order to estimate the kinetic parameters, independent seeded batch sets of experiments were conducted, first to estimate the growth rate of Form I, and consequently to estimate the secondary nucleation of Form I and dissolution rate of Form II. The experimental data showed that the secondary nucleation of Form I occurred slightly after the dissolution of Form II was initiated. The estimated parameters for growth, nucleation and dissolution rates were successfully implemented in the population model and validated with the experiments.
本研究研究了丁螺环酮氢氯化物(BUS-HCl)亚稳型II型在溶剂介导下向稳定型I型的多晶转化。利用原位拉曼光谱监测了其多晶转变。溶剂介导的转变过程是由形式II的溶解和形式i的成核和随后的生长控制的。每个子过程的模型参数是借助实验数据确定的,包括固相中的多晶分数、溶质浓度和晶体尺寸分布。为了估计动力学参数,我们进行了独立的种子批实验,首先估计了形式I的生长速度,然后估计了形式I的二次成核和形式II的溶解速度。实验数据表明,在形式II的溶解开始后,形式I的二次形核发生了轻微的变化。估计的生长速率、成核速率和溶解速率参数成功地应用于种群模型,并通过实验进行了验证。
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引用次数: 9
The Synthesis, Characterization and Application of Ciprofloxacin Complexes and Its Coordination with Copper, Manganese and Zirconium Ions 环丙沙星配合物的合成、表征与应用及其与铜、锰、锆离子的配位
Pub Date : 2012-04-24 DOI: 10.4236/JCPT.2012.22008
Z. Tan, Feng-Jiao Tan, Li Zhao, Jun-Yong Li
In our work, ciprofloxacin was extracted from the raw material ciprofloxacin hydrochloride and coordinated with the metal ions of copper, manganese and zirconium. The procedures include the comparison of the autoclave method with the solvothermal method, synthesizing the corresponding complexes and conducting antibacterial test on nearly 20 kinds of bacteria. It is shown that under the condition of PH1 and 110℃ - 116℃, the autoclave method and solvothermal method can be utilized to obtain the ciprofloxacin complexes with Cu2+, Mn2+ and Zr2+ as the metal ligands after reacting for 8 hours. The raw material, ligands and monocrystals were characterized by IR, DSC, UV and fluorescence spectrum. Meanwhile a great number of antibacterial tests were carried out, revealing favorable bacteriocidal properties of the resulting complexes.
在我们的工作中,从原料盐酸环丙沙星中提取环丙沙星,并与铜、锰、锆金属离子配合。程序包括热压灭菌法与溶剂热法的比较,合成相应的配合物,并对近20种细菌进行抑菌试验。结果表明,在ph为1,110℃~ 116℃的条件下,用热压罐法和溶剂热法反应8 h后,可以得到以Cu2+、Mn2+和Zr2+为金属配体的环丙沙星配合物。通过IR、DSC、UV和荧光光谱对原料、配体和单晶进行了表征。同时进行了大量的抗菌试验,结果表明所得到的配合物具有良好的杀菌性能。
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引用次数: 15
Thermal Characterization of Se80-xTe20Inx Glasses Using Iso-Conversional Methods 用等转换方法表征Se80-xTe20Inx玻璃的热特性
Pub Date : 2012-04-24 DOI: 10.4236/JCPT.2012.22009
Renu Shukla, Pragya Agarwal, Ashok Kumar
Alloys of Se80-xTe20Inx glassy system are obtained by quenching technique and crystallization kinetics has been studied using Differential Scanning Calorimetric [DSC] technique. Well defined endothermic and exothermic peaks are ob- served at glass transition temperature (Tg) and crystallization temperature (Tc). From DSC scans, Tc is obtained at dif- ferent heating rates (5, 10, 15, 20, 25 K/min). It is observed that Tc increases with increasing heating rate for a particular glassy alloy. Activation energy of crystallization (Ec) has been calculated by different Non-isothermal Iso-conversional methods, i.e., Kissinger-Akahira-Sunose [KAS], Friedman, Flynn-wall-Ozawa [FWO], Friedman-Ozawa [FO] and Sta-rink methods. It is observed that Ec is dependent on extent of crystallization (α). Activation energy is also found to vary with atomic percentage of In in ternary Se80-xTe20Inx glassy system. The compositional dependence of Ec shows a re-versal in the trend at x = 15 in Se80-xTe20Inx, which is explained in terms of mechanically stabilized structure at this composition.
采用淬火技术制备了Se80-xTe20Inx玻璃系合金,并用差示扫描量热技术研究了合金的结晶动力学。在玻璃化转变温度(Tg)和结晶温度(Tc)下观察到明确的吸热和放热峰。从DSC扫描中,获得了不同加热速率(5、10、15、20、25 K/min)下的Tc。观察到,对于特定的玻璃态合金,Tc随升温速率的增加而增加。结晶活化能(Ec)的计算采用了不同的非等温等转换方法,即Kissinger-Akahira-Sunose [KAS]、Friedman、Flynn-wall-Ozawa [two]、Friedman- ozawa [FO]和Sta-rink方法。观察到Ec与结晶程度(α)有关。在Se80-xTe20Inx三元玻璃体系中,活化能随In的原子百分数而变化。在Se80-xTe20Inx中,Ec的组分依赖性在x = 15处呈现出相反的趋势,这可以用该组分的机械稳定结构来解释。
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引用次数: 3
Determination of A.C. Conductivity of Nano-Composite Perovskite Ba(1- x - y)Sr(x)TiFe(y)O3 Prepared by the Sol-Gel Technique 溶胶-凝胶法制备纳米复合钙钛矿Ba(1- x - y)Sr(x) fe (y)O3的交流电导率测定
Pub Date : 2012-01-13 DOI: 10.4236/JCPT.2012.21001
M. Willander, O. Nur, M. Israr, A. Hamad, F. G. E. Desouky, M. A. Salem, I. Battisha
Nano-composite, perovskite Ba(1- x - y)Sr(x)TiFe(y)O3, denoted as (BSTFe) in powder form was derived via sol-gel (SG) method followed by sintering at fixed temperature 750℃ for one hour. The chemical composition, morphology and structure of the powder samples were investigated by using X-ray diffraction (XRD), transmission electron microscope (TEM) and scanning electron microscope (SEM). The XRD characterization indicates formation of a cubic crystalline phase in the pure BST. A well defined perovskite phase with nano-crystallite sizes equal to about 34 nm was achieved from XRD for B10ST3F sample, while TEM study confirmed the obtained XRD results giving the following crystallite size value about 33.75 nm for the same sample. The dielectric A.C. conductivity was evaluated as a function of temperature and frequency ranging from 42 Hz up to 1 MHz.
采用溶胶-凝胶(SG)法制备了Ba(1- x - y)Sr(x) fe (y)O3纳米复合材料(BSTFe),并在750℃固定温度下烧结1h。采用x射线衍射(XRD)、透射电子显微镜(TEM)和扫描电子显微镜(SEM)对粉末样品的化学成分、形貌和结构进行了研究。XRD表征表明,在纯BST中形成立方晶相。对B10ST3F样品进行XRD分析,得到了一个清晰的钙钛矿相,其纳米晶尺寸约为34 nm, TEM研究证实了所得XRD结果,得出了相同样品的晶尺寸约为33.75 nm。电介质交流电导率被评估为温度和频率范围从42 Hz到1 MHz的函数。
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引用次数: 20
Qualititative Analysis of Interface Behavior under First Phase Transition 第一相变条件下界面行为的定性分析
Pub Date : 2012-01-13 DOI: 10.4236/JCPT.2012.21005
A. Guskov
At present there is no explanation of the nature of interface instability upon first order phase transitions. The well-known theory of concentration overcooling under directed crystallization of solutions and Mullins-Sekerka instability cannot account for the diversified liquid component redistribution during solid state transition. In [1-3], within the framework of the nonequilibrium mass transfer problem, it has been shown that there are regimes of the interface instability, which differ from the known ones [4-6]. Moreover, the instability theory of works [1-3] demonstrates a complete experimental agreement of the dependence of eutectic pattern period on interface velocity. However, it is difficult to explain interface instability within the framework of a general setting of the mass-transfer problem. This paper is de-voted to qualitative analysis of the phenomena that are responsible for interface instability. The phenomena are connected by a single equation. Qualitative analysis revealed a variety of different conditions responsible for instability of flat interface stationary movement upon phase transition. The type of instability depends on system parameters. It is important that interface instability in the asymptotic case of quasi-equilibrium problem setting is qualitatively different from interface instability in the case of nonequilibrium problem setting.
目前还没有解释一阶相变时界面不稳定性的性质。众所周知的溶液定向结晶下的浓度过冷理论和Mullins-Sekerka不稳定性不能解释固态转变过程中多样化的液体组分再分配。在[1-3]中,在非平衡传质问题的框架内,已经表明存在与已知的[4-6]不同的界面不稳定状态。此外,作品的不稳定性理论[1-3]证明了共晶图案周期与界面速度的依赖关系的完全实验一致性。然而,很难在传质问题的一般设定框架内解释界面不稳定性。本文旨在定性分析导致界面失稳的现象。这些现象由一个方程联系起来。定性分析揭示了多种不同的条件导致平面界面在相变时的静止运动不稳定。不稳定性的类型取决于系统参数。重要的是,准平衡问题设置的渐近情况下的界面不稳定性与非平衡问题设置的界面不稳定性有质的区别。
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引用次数: 0
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