Continuous Spectroscopy Characterization of Emulsions

In emulsion polymerization, the formation of particles has an important effect on the rate of reaction and on the final properties of the latex. To investigate particle nucleation mechanisms in emulsion polymerization it is necessary to establish the initial conditions of the emulsified system before the reaction takes place. This research reports on a technique to continuously monitor the droplet size distribution of liquid-liquid emulsions using spectroscopy. The on-line particle characterization methodology is based on an integrated sampling and dilution strategy combined with spectroscopy methods. It is shown that the sampling system integrated with a multiwavelength turbidity detector provides reliable estimates of droplet populations as function of the dispersed phase concentration in emulsions of saturated hydrocarbons. The results provide not only the groundwork necessary for the elucidation of particle nucleation during emulsion polymerization process but also suggests the potential of this combined technology to further our understanding of liquid-liquid emulsions.     

Contact Angle Measurement for Dispersed Microspheres Using Scanning Confocal Microscopy

Abstract

Scanning confocal microscopy was used for contact angle measurement of individual microspheres. The measurements were carried out by using different laser‐scanned layers of the particle floating on the air–water interface. The ratio of the diameter for the cross‐section of the protruded area of the particle at the air–water interface to the actual diameter of the particle is used for contact angle measurements. Two systems, i.e., glass and polystyrene microspheres with diameters of 3–10 and 6 µm, respectively, with water were used for this investigation (this size range of particles are most relevant to inhalation applications). Using the developed methodology, contact angles of 27° and 41° were measured (with water) for glass and polystyrene particles, respectively. The theoretical error in contact angle measurement for the developed methodology is determined to be generally about 1° with a maximum of 3° for contact angle of particles ranging from 2 to 24 µm in size; the experimental error was 4–6°. The contact angles of glass and polystyrene particles were compared to those obtained from pendant drop method and confirmed.     

微流控技术制备微胶囊负载钯催化剂

采用微流控技术结合悬浮聚合方法实现了百微米级含膦配体聚苯乙烯微胶囊的可控制备, 微胶囊尺寸在320~420 μm范围内可调, 且单分散性好. 扫描电子显微镜、能量散射光谱和电感耦合等离子发射光谱结果证实了其形貌和组成的均匀性及钯负载的可控性和有效性. 以溴代芳烃与苯硼酸的Suzuki偶联反应为模型反应评价了负载Pd(PPh₃)₄的百微米级微胶囊的催化性能, 发现其性能与文献报道的7~8 μm的同类催化剂微胶囊接近, 且均优于均相催化剂; 该催化剂经简单过滤后, 可实现多次循环使用, 未发现活性物种的流失. 该法实现了连续制备, 因而有助于提高制备的效率和可控性. 另外, 所制百微米级催化剂微胶囊在固定床反应器内具有较高催化剂浓度和机械性能, 且优于浆态床中使用的微米级催化剂微胶囊.     

浅海波导界面对点源振速方向的影响

采用“虚源法”分析计算了浅海波导环境中接收点处点源总振速方向与水平面夹角,侧重讨论确定性界面反射对总振速方向的影响。研究结果表明：总振速方向和接收点与声源的水平距离、两者深度,海底、海面特性以及声速剖面等有关。在等声速均匀浅海波导中,由于确定性界面反射的影响,当直达声掠射角为1°～50°时,合成总振速方向偏离直达声方向达1.5°～10.5°,声速剖面呈负梯度时,偏离程度更甚.     

光静态散射测试系统的研究与实现

随着科学技术的发展,对粒子的大小、浓度及其他特性的探测已经发展成为一个专门的研究领域和现代测量学中的一个重要分支,而光散射法已经成为一种常用的粒子测量方法。为了满足应用需求,文中提出了一种基于C8051F500单片机的光静态散射测试系统方案,详细介绍了该测试系统的设计理论原理、硬件电路的设计依据、固件程序的设计思想和测试系统的具体实现。选取一定浓度的样品溶液,运用该系统进行光散射的角度依赖性测试,实际测量值与理论依据基本相符;在不同激光功率下,对同一角度的散射光强进行测试,将测量得到的数据分析,线性度良好,满足设计要求。     

Destructive Effect of an α‐Particle on TEX

By computational studies it was found that interaction of an α‐particle with TEX (an explosive molecule having a cage structure) disturbs the molecular skeleton dramatically. As the α‐particle exerts its positive electrostatic field, the C–C bond between the dioxalane rings present in TEX breaks down forming the dication of TEX. The calculation were done within the constraints of the density functional theory at the level of B3LYP using various bases sets, mainly 6‐31++G(d,p).     

Effects of ball-to-powder diameter ratio and powder particle shape on EDEM simulation in a planetary ball mill

The effects of the ball-to-powder diameter ratio (BPDR) and the shape of the powder particles on EDEM simulation results and time in the planetary ball mill was investigated. BPDR was varied from 1 to 40/3 by changing the powder particle diameter from 8 to 0.6 ?mm. The size and shape of the powder particles do not give a significant change in both the ball motion pattern and simulation results when BPDR is over 20/3. It can be assumed that the kinetic energy of the ball has nothing to do with the size and shape of the powder particle. The simulation time and data size increase exponentially as BPDR increases. The effect of change of the powder particle shape on the calculated data size is not significant, but the more complicated its shape, the longer the simulation time, which is linearly related to the number of spheres composing a particle.     

A review on key aspects of wet granulation process for continuous pharmaceutical manufacturing of solid dosage oral formulations

Wet granulation process is a major unit operation in production of pharmaceuticals as solid dosage oral formulation. Indeed, granulation is used to improve the formulation properties such as flowability, compressibility, and so on for pharmaceutical manufacturing. Different types of granulations can be used in pharmaceutical manufacturing in which the selection of proper process depends on the operational conditions as well as formulation properties. In current decades, twin-screw wet granulation has been of paramount interest owing to its superior properties. Pharmaceutical manufacturing industry are trying to move towards continuous mode by which the efficiency can be improved compared to the batch mode. Therefore, development of continuous granulation process is of great importance. In this review article, various processing units applicable for wet granulation of pharmaceutical formulations for solid dosage forms are reviewed and discussed. The advantages and disadvantages of the processes are discussed and listed along with modeling approaches for simulation of process. The governing models and numerical schemes applicable for design of wet granulation are also critically discussed. The main focus is on wet granulation as this method has attracted much attention in pharmaceutical processing.     

Exciplex Formation in Lipid-bound Escherichia coli Flavohemoglobin

Flavohemoglobins have the particular capability of binding unsaturated and cyclopropanated fatty acids as free acids or phospholipids. Fatty acid binding to the ferric heme results in a weak but direct bonding interaction. Ferrous and ferric protein, in presence or absence of a bound lipid molecule, have been characterized by transient absorption spectroscopy. Measurements have been also carried out both on the ferrous deoxygenated and on the CO bound protein to investigate possible long-range interaction between the lipid acyl chain moiety and the ferrous heme. After excitation of the deoxygenated derivatives the relaxation process reveals a slow dynamics (350 ps) in lipid-bound protein but is not observed in the lipid-free protein. The latter feature and the presence of an extra contribution in the absorption spectrum, indicates that the interaction of iron heme with the acyl chain moiety occurs only in the excited electronic state and not in the ground electronic state. Data analysis highlights the formation of a charge-transfer complex in which the iron ion of the lipid-bound protein in the expanded electronic excited state, possibly represented by a high spin Fe III intermediate, is able to bind to the sixth coordination ligand placed at a distance of at 3.5 Å from the iron. A very small nanosecond geminate rebinding is observed for CO adduct in lipid-free but not in the lipid-bound protein. The presence of the lipid thus appears to inhibit the mobility of CO in the heme pocket.     

Structure-based virtual screening of dipeptidyl peptidase 4 inhibitors and their in vitro analysis

Type 2 diabetes mellitus (T2DM) is one of the most widely prevalent metabolic disorders with no cure to date thus remains the most challenging task in the current drug discovery. Therefore, the only strategy to control diabetes prevalence is to develop novel efficacious therapeutics. Dipeptidyl Peptidase 4 (DPP-4) inhibitors are currently used as anti-diabetic drugs for the inhibition of incretins. This study aims to construct the chemical feature based on pharmacophore models for dipeptidyl peptidase IV. The structure-based pharmacophore modeling has been employed to evaluate new inhibitors of DPP-4. A four-featured pharmacophore model was developed from crystal structure of DPP-4 enzyme with 4-(2-aminoethyl) benzenesulfonyl fluoride in its active site via pharmacophore constructing tool of Molecular Operating Environment (MOE) consisting F1 Hyd (hydrophobic region), F2 Hyd|Cat|Don (hydrophobic cationic and donor region), F3 Acc (acceptor region) and F4 Hyd (hydrophobic region). The generated pharmacophore model was used for virtual screening of in-house compound library (the available compounds which were used for initial screening to get the few compounds for the current studies). The resultant selected compounds, after virtual screening were further validated using in vitro assay. Furthermore, structure-activity relationship was carried out for the compounds possessing significant inhibition potential after docking studies. The binding free energy of analogs was evaluated via molecular mechanics generalized Born surface area (MM-GBSA) and Poisson-Boltzmann surface area (MM-PBSA) methods using AMBER 16 as a molecular dynamics (MD) simulation package. Based on potential findings, we report that selected candidates are more likely to be used as DPP-4 inhibitors or as starting leads for the development of novel and potent DPP-4 inhibitors.