Quantification of flupirtine maleate polymorphs using X-ray powder diffraction

Flupirtine maleate,a pharmaceutical compound for treating psychotic disease in clinics,has seven polymorphs.Form A,with better crystal stability and bioavailability,has been widely used as the pharmaceutical crystal form.Unfortunately,it is usually found in a polymorphic mixture with form B.In this study,pure crystal forms of A and B were prepared and characterized by X-ray powder diffraction (XRPD),Fourier transform infrared spectroscopy (FT-IR) and thermal analysis.An XRPD-based method for the quantitative determination of the amount of the flupirtine maleate polymorphs form A and form B was also established through a systematic optimization of instrumental parameters.The results of the analytical methodology validation showed that the XPRD method had a broad quantitative range of 0-100%(w/w),good linear relationship,with R²=0.999,excellent repeatability and precision and low limits of detection (LoD) of 0.15%(w/w) and quantification (LoQ) of 0.5%(w/w).The results also showed that the single-peak method was not as good as the whole pattern in reducing the influence of the preferred orientation,but this can be compensated for by a systematic optimization of instrumental parameters and validating the analytical methodology to reduce errors and obtain a good,repeatable,sensitive,and accurate method.This XRPD method can be used to analyze mixtures of flupirtine maleate polymorphs (forms A and B) quantitatively and control the quality of the bulk drug.     

Raman polarization analysis of highly crystalline polyethylene fiber

The complex orientation dependence in space of Raman active vibrations in the orthorhombic structure of polyethylene (PE) is discussed in terms of Raman tensor elements as intrinsic physical parameters of the lattice. Building upon the symmetry assignment of these vibrational modes, we systematically studied, from both theoretical and experimental viewpoints, the changes of polarized intensity for the A_g and the B_2g + B_3g vibrational modes with respect to PE molecular orientation. After explicitly expanding the Raman selection rules associated with the A_g and the B_2g + B_3g modes, introducing them into general expressions of the orientation distribution function, and validating them by means of a least‐square fitting procedure on experimental data, we compare here two mesostructural models for a highly crystallized and self‐aligned PE fiber structure. Stereological arguments are shown concerning the arrangement of orthorhombic fibrils in such a sample that unfold the correct values of five independent Raman tensor elements for orthorhombic PE. Copyright © 2010 John Wiley & Sons, Ltd.     

Wetting, Bonding and Interfacial Energy of Nanocrystalline Metal Particles on Crystalline DCH Polymer and Amorphous Carbon Substrates

Experimental results concerning the interaction between a variety of nanocrystalline metals (gold, silver, nickel and chromium) and both crystalline polymer [poly-DCH (1,6-di (N-carbazolyl)-2,4-hexadiene)] and amorphous carbon substrates, are presented and analyzed. Attention is focused on aspects of the interaction that concern interfacial bonding, its correlation with the cohesive energies of the various metals and the energy of the interfaces. Experimental contributions include qualitative estimates of the magnitude of interfacial energies for the crystalline polymer/metal and amorphous carbon/metal interfaces and a direct measurement of the interfacial energies for gold and silver nanocrystals deposited on the amorphous carbon substrate. The sequence of interfacial energy values for the polymer/metal and amorphous carbon/metal systems is also determined. The interfacial energies for both the poly-DCH and amorphous carbon substrates decreases in the order silver, gold, nickel, and chromium, as expected from cohesive energy, melting point and surface energy data for these elements. The crystalline polymer/metal interfaces were examined for the presence of orientation relationships using selected area diffraction and optical diffractometry of high-resolution TEM images. No orientation relationships were found for any of the polymer/metal combinations spanning a large range of metal reactivities. Lack of atomic matching or some as yet unknown surface condition on the polymer may be responsible for this effect.     

Effect of initial orientation on twinning in commercially pure titanium

Abstract

The effect of initial orientation on twinning micro-mechanisms during tensile deformation of commercially pure titanium has been studied using micro focus X-ray diffraction and electron back scatter diffraction (EBSD) in a scanning electron microscope. Three orientations A, B and C obtained from a rolled and annealed block of commercially pure titanium were deformed in uniaxial tension till failure and the tested specimens were characterised with regard to bulk texture, microstructure and crystal orientation mapping using EBSD. Orientation B along the transverse direction in ND-TD plane exhibits higher strength and lower strain hardening compared to orientations A and C along the rolling direction in TD-RD and ND-RD plane, respectively. This is attributed to different texture of sample B compared to samples A and C leading to dissimilar twinning micro-mechanisms and characteristic variation in nature of twinning. It is observed that limited twin nucleation and prominent lateral growth plays a dominant role in orientation B while multiple twin nucleation with significant non-Schmid behaviour is dominant for the other two orientations. It is proposed from this study that conventional factors associated with twin formation like Schmid factor play a main role in twin nucleation and propagation, however, growth or lateral thickening of the twins is explained by elastic stiffness variation across twins and their parent grains.     

光电成像探测中目标方位测量方法

为了在光电成像探测目标的同时给出目标相对探测器的方位信息,探讨了一种基于单目视觉的运动目标方位测量方法。根据投射成像原理,推算出二维目标像点坐标与目标的空间三维位置之间的映射关系,建立了单目视觉测量目标方位的数学模型。结合帧间差分法和KLT方法检测静止背景下和变化背景下的运动目标,并对目标特征点进行亚像素定位。试验和仿真结果分析表明,该方法能够有效提取目标的特征点,可对目标较为准确地定位,并通过单目视觉测量出目标方位信息,误差控制在8%的范围内。     

基于XRD和FTIR的香樟木质部提取物处理材褐腐的光谱学分析

植物源防腐剂因其环保、广谱、高效等特点越来越受到木材防腐行业的重视,从微观层面探索香樟提取物影响木材腐朽的机理是发展利用植物源防腐剂的重要基础。试验采用香樟木质部的四种溶剂提取物、ACQ及樟脑配制成防腐剂进行防腐试验,结果表明:10%浓度的香樟木质部甲醇提取物以及4%浓度的ACQ处理试件均达到I级强耐腐水平,4%樟脑、10%香樟乙酸乙酯和10%丙酮提取物处理的试件达到Ⅱ级耐腐水平。通过XRD对比发现结晶区2θ衍射强度由大到小的顺序为:10%蒸馏水提取物处理材、马尾松素样、10%丙酮提取物处理材、10%甲醇提取物处理材、10%乙酸乙酯提取物处理材,四种香樟木质部提取物的防腐效果与相对结晶度大小呈正相关。通过FTIR研究发现表征纤维素和半纤维素的特征峰值越低,则被降解的量也越大,相对应的防腐剂防腐效果越差。处理试件中表征木质素的一系列特征峰峰高与未处理材相比有所升高。香樟甲醇提取物以及ACQ处理试件的I1 510/I1 738,I1 510/I1 374,I1 510/I1 160的比值最小,证明褐腐菌对其综纤维素的降解能力最弱,防腐效果最好。     

Oriented noncrystalline structure in PET fibers prepared with threadline modification process

The development of an oriented noncrystalline phase in a semicrystalline polymer filament has been studied via X-ray scattering. These unique PET fibers contain a relatively high noncrystalline content and also have high tenacity, high modulus, and low breaking elongation. Fiber properties were found to be very responsive to the oriented amorphous phase content. This phase was utilized for interpreting noncrystalline orientation in PET fibers produced by a new extrusion technique. Here, the oriented noncrystalline regions in a series of PET fibers varies from 6% to 63%, depending strongly on the production conditions. In particular, samples produced with a newly developed threadline modification process possess a high content of oriented noncrystalline polymer. Measurements such as dynamic and static mechanical properties have been performed on various samples, and these properties are related to the oriented noncrystalline phase. The results provide direct evidence for the existence of highly oriented noncrystalline material in these unique PET fibers spun with a threadline modification process. © 1996 John Wiley & Sons, Inc.     

Dielectric and tunable properties of highly (110)-oriented (Ba<Subscript>0.65</Subscript>Sr<Subscript>0.35</Subscript>)TiO<Subscript>3</Subscript> thin films deposited on Pt/LaNiO<Subscript>3</Subscript>/SiO<Subscript>2</Subscript>/Si substrates

Highly (110)-oriented Ba_0.65Sr_0.35TiO₃ films were deposited on Pt/LaNiO₃/SiO₂/Si substrates by a sol–gel method. It was found that the (110)-preferred Pt film was very effective for growing (110)-oriented ferroelectric films with perovskite structure. The as-grown Ba_0.65Sr_0.35TiO₃ films showed good dielectric properties with dielectric constant and loss tangent tan δ = 0.026. Excellent dielectric tunability was also achieved in the (110)-oriented films. With applying an electric field of 230 kV/cm at 100 kHz, the dielectric tunability and the figure of merit can reach up to 63.4% and 16, respectively. These results indicate that the highly (110)-oriented Ba_0.65Sr_0.35TiO₃ film is a promising candidate for the applications in microwave tunable devices.