用光谱诊断技术测定高能单元推进剂的温度分布

采用光谱诊断技术中的相对强度法测定了单元推进剂六硝基六氮杂异伍兹烷(HNIW)在3 MPa和5 MPa两种压力下的燃烧火焰温度分布。结果表明,相对强度法能准确地测出单元推进剂HNIW在整个燃烧过程的温度分布曲线,测得的最高燃烧火焰温度低于相应压力下的理论计算温度;测量压力升高,最高燃烧火焰温度更接近于理论计算温度。此实验结果说明：在较高压力条件下,用相对强度法能够准确地测定高能高燃速推进剂的燃烧火焰温度分布。     

模拟深海极端环境下烷类气体的拉曼光谱实验研究

利用高温高压深海模拟实验系统,进行了深海热液环境下烷类气体水溶液的拉曼光谱探测,分析了烷类分子的拉曼特征峰随温度和压力的变化规律,建立了温度与光谱之间的数学模型.结果表明:由于水的氢键作用,导致溶于其中的烷类分子的拉曼特征峰频移量较其气态时减小;常温下,在≤40 MPa 压力范围内,烷类分子的拉曼特征峰均未见明显变化;...     

单次冲击压缩下液态硝基甲烷的拉曼光谱

在单次冲击压缩实验中,运用高敏度瞬态拉曼光谱技术观测了液态硝基甲烷分子的拉曼光谱. 将该拉曼测量技术与二级轻气炮的实验平台结合起来,获得硝基甲烷分子振动模式的高压动态行为. 硝基甲烷被12 GPa压力冲击时的拉曼光谱可清晰探测,其拉曼振动峰仅仅发生了峰位蓝移和峰宽展宽的变化,未显示出化学变化产生的迹象.     

双苯氟嗪盐酸盐和苯甲酸的共晶制备和谱学分析

药物共晶是改善药物活性成分(API)的物理化学特性的新技术和新思维,具有很大的应用潜力。本实验采用研磨法制备了双苯氟嗪盐酸盐(DF-HCl)和苯甲酸的共晶,应用红外光谱(IR)、拉曼光谱(Raman)、差示扫描量热分析(DSC)、X射线衍射(XRD)和太赫兹光谱(THz)对共晶进行了表征。结果表明:双苯氟嗪盐酸盐与苯甲酸之间形成共晶分子,太赫兹谱的研究进一步表明两种分子之间有氢键形成。     

六硝基六氮杂三环十四烷对二呋咱（HHTTD）的合成

杂环硝胺是重要的含能化合物，研究表明：用羰基取代环胺中的次甲基，可以提高炸药的结晶密度，进而提高爆速，比如硝基甘脲及我国20世纪70年代就已合成的六硝基六氮杂三环十二烷二酮。如果将呋咱基引入到氮杂稠环类化合物分子结构中，以取代结构中的羰基，则又有可能创造一类密度及能量都非常高的炸药。基于该思想，文中利用两种化合物DAF和1，4-甲酰基-2，3，5，6-四羟基哌嗪（DFTHP），合成了目标炸药分子：六硝基六氮杂三环十四烷对二呋咱（HHTTD）及前体化合物六氮杂三环十四烷对二呋咱（HTTD）。文中给出了HTTD的合成方法及HTTD的硝化反应，提出了一种新化合物HHTTD的合成方法并对羟胺缩合反应进行了较详细的研究，HTTD及HHTTD的结构见图1。     

纳米级金刚石超微细粉的性能参数分析

本文对用爆炸法合成的两批纳米级金刚石超细粉进行了初步研究,ＸＲＤ表明样品Ⅰ和样品Ⅱ是立方相金刚石晶体结构,粒径平均为～４０;ＦＴＩＲ光谱显示样品Ⅰ中含有较多的石英杂质;测量了纳米级金刚石超细粉的拉曼光谱,对其不同于大块金刚石拉曼峰的现象,用量子限制效应模型作出解释。     

诺氟沙星与DNA的拉曼光谱研究

报道了诺氟沙星(NFX)及诺氟沙星胶囊内容物的FT-Raman光谱和在银胶基底上的表面增强拉曼光谱(SERS),归属了各个振动;研究了诺氟沙星与DNA的相互作用的SERS,结果表明:胶囊内容物的拉曼光谱图与对照品的拉曼光谱图的特征振动峰:C-F键的伸缩振动,C=C伸缩振动,O-C-O的对称伸缩振动峰值未发生变化,发生变化主要是分子骨架振动峰,诺氟沙星胶囊的辅料对拉曼光谱无实质影响,可建立拉曼光谱法检测诺氟沙星药物的分析方法;诺氟沙星可以在没有金属离子的存在下与DNA直接作用,与DNA相互作用的主要键合模式是插入作用,NFX分子中的平面结构插入DNA的双螺旋碱基平面,为深入了解喹诺酮类抗生素的抗菌机理提供可靠依据.     

N-(4-硝基苯基)马来酰亚胺分子结构、光谱和热力学性质的理论研究

N-(4-硝基苯基)马来酰亚胺是一种新合成的NPMI类化合物，在B3LYP/6-311++G**水平对N-(4-硝基苯基)马来酰亚胺分子进行几何结构优化和频率、热力学性质计算，得到它的红外光谱、拉曼光谱和不同温度下的热力学性质。结果显示，该分子中两个C=O与五元环在同一个平面内，苯环上硝基中的N-O与六元环也在同一个平面内，五元环与六元环呈129.6的二面角，整个分子不具有对称性；热容、熵、焓等热力学性质与温度之间存在很好的函数关系式。     

饱和一元醇类分子拉曼光谱振动峰的归属研究

选用B3LYP/6-31G(d)优化并计算了31种饱和一元醇类分子的拉曼光谱,以甲醇为例,考察了理论计算结果的准确性,分析了碳原子数小于7的直链饱和一元醇拉曼光谱振动峰的归属。研究结果显示,B3LYP/6-31G(d)用于饱和一元醇类分子拉曼光谱振动的模拟计算较为准确,通过饱和一元醇拉曼光谱振动峰归属分析,确认C—O伸缩振动引起的振动峰可作为饱和一元醇类分子拉曼光谱的特征峰;进一步研究还发现,饱和一元醇类分子拉曼光谱的特征峰与其极化率、热力学、能量等主要参数具有显著的相关性(sig.为0.015),为同系物的拉曼光谱研究提供了一定的参考价值。     

KTN晶体及其熔体结构的高温拉曼光谱研究

测量并研究了不同温度(室温—1573 K)范围内KTN晶体的拉曼光谱及其熔体的高温拉曼光谱,分析了KTN晶体结构随温度变化的规律及其熔体的结构特征.随着温度的升高,KTN晶体的拉曼光谱谱峰都不同程度地向低波数方向移动,同时存在不同程度的展宽,并伴随强度的减弱.观察并解释了温度353 K附近KTN晶体样品的四方—立方转相现象.研究了KTN晶体拉曼光谱中538cm^-1,585cm^-1,835cm^-1和877cm^-1谱峰及其 关键词： 高温拉曼光谱 熔体 KTN晶体     

西佛碱型液晶化合物相变过程中分子排列方式变化的拉曼光谱研究

用变温拉曼光谱对相变过程的研究表明,液晶化合物的初始晶态与熔融后缓慢降温得到的晶态并不吻合,两个状态下分子尾链的构象及刚性核部分的构象不同导致分子的聚集状态不同。西佛碱型液晶化合物VO10相变过程中,在晶态到液晶态相转变过程中,烷氧基尾链链内构象发生突变,同时有序性降低,刚性核部分两个苯环之间的二面角在相变点时发生明显变化,二面角加大。     

Vibrational spectra and structural studies of nonlinear optical crystal ammonium D,L‐tartrate: a density functional theoretical approach

Single crystals of ammonium D , L ‐tartrate, a potential nonlinear optical (NLO) material of interest, were grown by the slow evaporation technique. The crystal structure was determined by single‐crystal X‐ray diffraction. Fourier transform infrared and Raman spectra of the crystallized molecule were recorded and analyzed. The geometry, intermolecular hydrogen bonding, first hyperpolarizability and harmonic vibrational wavenumbers were calculated with the help of B3LYP density functional theory method. The red shift of hydroxyl and NH₄⁺ stretching wavenumbers indicate the formation of inter‐ and intramolecular hydrogen bonding. Simultaneous activation of CH stretching wavenumbers shows the presence of intramolecular charge transfer in the molecule. Natural bond orbital analysis was carried out to demonstrate the various inter‐ and intramolecular interactions that are responsible for the stabilization of this molecule, leading to high NLO activity. Copyright © 2010 John Wiley & Sons, Ltd.     

Theoretical and experimental vibrational property of 1,3,4,6-tetramethylpiperazine-2,5-dione

1,3,4,6-tetramethylpiperazine-2,5-dione was synthesized, and the crystal structure was characterized by single-crystal X-ray diffraction method, vibrational spectral measurements were obtained by Fourier transform infrared spectroscopy and Fourier transform Raman spectroscopy. The measurements agree well with the calculated geometrical structure and harmonic vibrational wavenumbers (usingab initio and density functional theory Becke’s three parameters hybrid method with the Lee, Yang, and Parr non-local functions methods with 6-311G and 6-311G** basis sets).     

吡拉西坦和3-羟基苯甲酸药物共晶体及其形成过程的光谱特性分析

药物共晶可以改善药物活性成分的物理化学性质,这一特性使其在改善药物性质特征方面具有很大的应用潜力。本文采用固体研磨的方法制备由吡拉西坦(Piracetam)和3-羟基苯甲酸(3-Hydroxybenzoic acid, 3HBA)作为原料药的药物共晶体,应用傅里叶变换红外(FTIR)、拉曼(Raman)和太赫兹(THz)光谱方法对研磨获得的共晶样品进行表征,并对两原料药和共晶体的分子振动模式进行归属。FTIR,Raman和THz光谱均表明共晶体的振动模式与原料药有着显著的区别。另外,使用Raman和THz光谱技术深入分析共晶体形成的动态过程,实验结果表明在研磨的最初几分钟反应迅速,之后共晶体形成的反应速率变得缓慢,在研磨35 min之后,共晶体的形成过程结束。这一结果为药学领域中有关药物共晶形成的实时监控及其定量分析提供了理论依据和一种有效的技术方法。     

Growth and characterization of organic nonlinear optical crystal: l-Valinium salicylate (LVS)

The new organic NLO crystal l-valinium salicylate (LVS) was grown by slow evaporation method using the mixed solvent of methanol and water in equal ratio. The crystal structure parameters were observed by powder and single crystal X-ray diffraction (XRD). The various functional groups present in the grown crystal were confirmed by Fourier transform infrared spectroscopy (FTIR) technique. ¹H and ¹³C Fourier transform nuclear magnetic resonance (FT-NMR) spectra were recorded to elucidate the molecular structure. The optical absorption study confirmed the good transmission window of the title crystal suitable for optical applications. The second harmonic generation (SHG) efficiency of LVS was confirmed by Kurtz Perry technique.     

Synthesis,structural characterization,spectroscopic, thermal,dielectric and Hirshfeld surface analysis of 1-(2-methoxyphenyl)piperazinium chloranilate

The new compound 1-(2-methoxyphenyl)piperazinium chloranilate (MPP.CA) was synthesized and studied by the single crystal X-ray diffraction method. Its structure was confirmed by infrared spectroscopy. The crystal structure consists of ribbons of chloranilate anions and 1-(2-methoxyphenyl)piperazinium cations linked together by NH…O hydrogen bonds. Two protons are transferred from a chloranilic acid molecule to the nitrogen of the piperazine in this structure. Measurements of AC conductivity as a function of frequency at different temperatures indicated the hopping conduction mechanism; in addition, the variation of dielectric constant as a function of T confirmed the transition phase indicated by the differential scanning calorimetry (DSC). The physico-chemical properties, UV-Vis, DSC and dielectric properties are described. Hirshfeld surface analyzes all the intermolecular interactions involved within the structure, which are important to stabilize the structure.     

Two salts and the salt cocrystal of ciprofloxacin with thiobarbituric and barbituric acids: The structure and properties

Ciprofloxacin (CfH, C₁₇H₁₈FN₃O₃) crystallizes with 2‐thiobarbituric (H₂tba) and barbituric acid (H₂ba) in the aqueous solution to yield salt CfH₂(Htba)·3H₂O ( 1 ), salt cocrystal CfH₂(Hba)(H₂ba)·3H₂O ( 2 ), and salt CfH₂(Hba)·H₂O ( 3 ). The compounds are structurally characterized by the X‐ray single‐crystal diffraction. The numerous intermolecular hydrogen bonds N–H?O and O–H?O formed by water molecules, Htba^?/Hba^? and CfH₂⁺ ions, and H₂ba molecules stabilize the crystal structures of 1 to 3 . Hydrogen bonds form a 2D plane network in the salts of 1 and 3 and a 3D network in the salt cocrystal of 2 . There are different π‐π interactions in 1 to 3 . The compounds have been characterized by powder X‐ray diffraction, thermogravimetry/differential scanning calorimetry, and Fourier transform infrared spectroscopy. The compounds dehydration ends at 130°C to 150°C, and their oxidative decomposition is observed in the range of 250°C to 275°C.     

Quantum chemical insight into molecular structure,density functional theory calculations,vibrational dynamics,natural population analysis,Hirshfeld analysis,and molecular docking approach to chalcone 1-4-bromophenyl-3-(2-methoxyphenyl)prop-2-en-1-one

The structure of the novel chalcone 1-4-bromophenyl-3-(2-methoxyphenyl)prop-2-en-1-one has been characterized by Fourier transform infrared and Fourier transform Raman. Density functional theory with Becke, 3-parameter, Lee-Yang-Parr functional was used for the optimization of geometry. The comprehensive assignments of the vibrational spectra have been performed with the aid of normal coordinate analysis. Stability of the molecule and intra/intermolecular charge transfer have been analyzed using natural bond orbital analysis. The existence of intermolecular C-H?O, blueshifted hydrogen bond was investigated by bond length variation. Hirshfeld and two-dimensional fingerprint plot analyses have been performed to study the nature of interactions present in the molecule. The docked complex gives a constancy of ?8.2?kcal/mol toward the androgen receptor.     

FTIR和Raman用于盐酸曲马多的结构分析

采用AVATAR 360型傅里叶变换红外光谱仪和RM-1000型激光共聚焦拉曼光谱仪测定盐酸曲马多的红外光谱和拉曼光谱。拉曼光谱和红外光谱中均显示出了盐酸曲马多的特征峰,都能够用于其结构鉴别。采用红外、拉曼光谱这两种方法互相印证,互相补充,可增强鉴定的准确性、可靠性。     

56Fe13+离子引起GaP晶体的微结构损伤

利用X射线衍射（XRD）技术、傅里叶变换红外光谱（FTIR）和Raman光谱对经不同剂量的56Fe13+离子辐照的GaP晶体的微结构进行了表征。结果表明:随着辐照离子剂量的增加,GaP晶体中产生了局部的无序与缺陷。随着56Fe13+离子剂量的增加,Raman光谱展示出振动峰强度逐渐减弱而且一些逐渐消失,但其峰位几乎没有发生变化;XRD显示出GaP晶体的衍射峰的强度逐渐减小;FTIR主要表现为宽化及其强度增加。这表明重离子56Fe13+的辐照使得GaP晶体中的缺陷与无序性增加,导致晶体产生了局部的非晶化。The Misconstructural damage of GaP irradiated with 56Fe13+ to fluences ranging from 1×107 ions/cm2~1×1010 ions/cm2 were analyzed by X-ray diffraction (XRD) techniques, Fourier transform infrared spectroscopy (FTIR) and Raman spectroscopy. The result shows that, with the increase of irradiation ion fluences, local disorder and defects were produced in GaP crystal. With the increase of ion fluence, Raman spectra reveal the intensity of scattering peaks gradually weakens and some scattering peaks gradually disappear, however no changes in the peak position were found. XRD measurement displays that the intensity of diffraction peaks gradually decreases with an increase in ions fluences. Result from FTIR spectra exhibits that the intensity of reflection peaks gradually increases and the FWHM of reflection peaks broadens. These phenomena indicate that, the irradiation of heavy-ion Fe produces defects and disorder in GaP crystal, leading to a local amorphization.