闹羊花与野菊花红外光谱的分析与鉴定

采用傅里叶变换红外光谱对杜鹃花科植物闹羊花与菊科植物野菊花两种花类中药材的主成分进行表征,其中闹羊花出现在1 648和1 543cm-1出现明显的酰胺Ⅰ带和酰胺Ⅱ带吸收峰,证明其中含有蛋白质,可能与其具有的免疫作用相关;野菊花出现在1 734和1 515cm-1等CO伸缩振动吸收峰,证明其中含有挥发油等酯类成分。由于二者的红外光谱具有较高的相似性且难以区分,通过二级鉴别比较闹羊花与野菊花的二阶导数红外光谱可看出,在1 656和1 515cm-1附近的吸收峰,表明二者均含有黄酮类成分;野菊花的二阶导数谱图中出现在1 163,1 077,1 026,986和869cm-1的吸收峰与菊糖的特征吸收峰一致,因此可以看出野菊花中含有菊糖。选取不同波数范围的闹羊花与野菊花的二维相关红外光谱进行对比,发现在1 700~1 400cm-1黄酮类成分区域闹羊花有3个明显的自动峰,野菊花有10个明显的自动峰;在1 250~900cm-1糖苷类成分区域闹羊花有10个明显的自动峰,野菊花有9个明显的自动峰。红外光谱的"三级鉴定法"为中药材的鉴别提供更快速、准确、方便的手段。     

Toughening Effect of Ethylene Propylene DieneTerpolymer-Graft-Styrene-Acrylonitrile Copolymer (EPDM-g-SAN) on SAN Resin

The reaction product EPDM-g-SAN, synthesized by suspension graft copolymerization of styrene (St) and acrylonitrile (AN) in the presence of ethylene-propylene-diene terpolymer (EPDM), was blended with a commercial styrene-acrylonitrile copolymer (SAN resin) to prepare AES blends with high impact strength. The effects of AN mass percentage in the St-AN comonomer mixture (f _AN), EPDM mass percentage in the feed of EPDM and St-AN (f _EPDM) and reaction time on monomer conversion ratio (CR), grafting ratio (GR), and AES notched Izod impact strength were characterized. The notched Izod impact strength of AES containing 15 wt% EPDM reached its maximum with f _AN of 40 wt% and f _EPDM of 45 wt%; this was attributed to the polarity of the SAN copolymer obtained being appropriate with that of the SAN resin matrix. The dependences of GR and the notched Izod impact strength of AES containing 25 wt% EPDM on the reaction time were in rough agreement. The effect of EPDM content on the AES notched Izod impact strength indicated that the brittle-ductile transition of AES occurred for an EPDM content from 12.5 to 15 wt%. TEM and SEM analysis showed that the phase structure of AES exhibited a “salami” like structure, and the toughening mechanism of AES was shear yielding of the SAN resin matrix, which endowed AES with excellent toughness.     

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.     

Modification of structural,optical, thermal and mechanical properties of KDP crystals on the addition of Ni

Nonlinear optical materials are acquiring a new significance day by day with the advent of a large number of devices utilizing solid state laser sources. Owing to this technological application KDP having superior nonlinear optical property has been exploited for various applications. KDP crystals were grown from aqueous solutions added with Ni²⁺. SHG studies confirm that the title exhibits NLO property. The influence of doping Ni²⁺ on the structural, optical, thermal, NLO and mechanical properties has been studied in this present investigation. It is observed that addition of Ni²⁺ improves the optical, thermal and mechanical properties of the crystal.     

Growth and characterization of a new organic nonlinear optical crystal: Vanillylideneaniline

Vanillylideneaniline with chemical formula C₁₄H₁₃NO₂ (VAN), a second order nonlinear optical (SONLO) organic single crystal was synthesized and grown for the first time from dimethyl formamide (DMF) employing slow solvent evaporation technique. Single crystal X-ray diffraction data reveals that the crystal belongs to noncentrosymmetric orthorhombic space group C222₁. The high-resolution diffraction curve containing single peak with full width at half maximum (FWHM) of 62 arc s ascertains VAN was perfectly crystallized and free from structural grain boundaries. The formation of the material was confirmed quantitatively by FTIR, ₁H¹ and ¹³C NMR spectral analyses. The UV–vis–NIR spectrum reveals the percentage of the transmission of VAN crystal in the entire region. The variations of dielectric constant (?_r) and dielectric loss (D) with frequency at different temperatures were investigated. The SHG of VAN crystal is confirmed by Kurtz Powder technique. The mechanical strength of the crystal was estimated by Vickers hardness test. VAN has yield strength of 8.70 MPa. Thus the grown organic VAN single crystal can be recommended as a promising candidate for SONLO application and device fabrication technology.     

Growth structural,spectral, optical and mechanical studies of gamma bis glycinium oxalate (GBGOx) new NLO single crystal by SEST method

Gamma bis glycinium oxalate (GBGOx) crystal was synthesized and grown by slow evaporation solution technique. The structure of pure GBGOx crystal has been examined by single crystal X-ray diffraction analysis. The confirmation with single crystal XRD reveals that the crystal belongs to monoclinic system with space group C₂. The FTIR spectrum was recorded to identify the expected functional groups. UV–vis-spectrum shows the lower cut off wavelength and 80% of transmittance in the UV–vis region. The photoluminescence measurement shows that the material is suitable for photonic devices. Preliminary measurement of green light emission using Kurtz powder technique indicates that their second harmonic generation (SHG) efficiency. The microhardness analysis revealed that the grown crystal belongs to soft material category. The encouraging results show that the GBGOx crystals have great potential applications in optical devices.     

Structural and permeability sensitivity of cells to low intensity ultrasound: Infrared and fluorescence evidence in vitro

This work is focused on the in vitro study of the effects induced by medical ultrasound (US) in murine fibroblast cells (NIH-3T3) at a low-intensity of exposure (spatial peak temporal average intensity I_ta < 0.1 W cm⁻²). Conventional 1 MHz and 3 MHz US devices of therapeutic relevance were employed with varying intensity and exposure time parameters. In this framework, upon cells exposure to US, structural changes at the molecular level were evaluated by infrared spectroscopy; alterations in plasma membrane permeability were monitored in terms of uptake efficiency of small cell-impermeable model drug molecules, as measured by fluorescence microscopy and flow cytometry. The results were related to the cell viability and combined with the statistical PCA analysis, confirming that NIH-3T3 cells are sensitive to therapeutic US, mainly at 1 MHz, with time-dependent increases in both efficiency of uptake, recovery of wild-type membrane permeability, and the size of molecules entering 3T3. On the contrary, the exposures from US equipment at 3 MHz show uptakes comparable with untreated samples.     

Estimation of carbonate concentration and characterization of marine sediments by Fourier Transform Infrared Spectroscopy

Fourier Transform Infrared Spectroscopy (FTIR) is a well established method for the characterization of mineralogical and geochemical properties of marine sediments. Understanding the biogeochemical changes in marine ecosystems is challenging task since it requires adequate analytical techniques and efforts. Biogeochemical characteristics of twenty one marine sediment samples collected off Chennai coast, Bay of Bengal, India were analyzed using FTIR spectroscopy. The FTIR peaks at 1460 cm⁻¹ (stretching vibration) and 880 cm⁻¹ (bending vibration) were used for carbonate determination. To verify the FTIR results, the obtained carbonate data were compared with carbonate values obtained by chemical analyses. The ranges of carbonate in sediments using FTIR and chemical analyses were 4.5–9.6% and 4.8–10%, respectively. The significant positive relationship was obtained between the carbonate results of FTIR and chemical analyses. This study demonstrates that instead of expensive and time consuming chemical methods, FTIR spectroscopic technique is found as a suitable, rapid and effective method for the quantification of carbonate in marine sediments.     

Synthesis Characterization and Crystal Structure of 2-(3,4,5-trimethoxyphenyl)-1-(4-fluorophenyl)-4,5-diphenyl-1H-imidazole

The title compound, C₃₀H₂₅FN₂O₃, was prepared from the four-component one-pot condensation reaction and the product crystallized using dimethylformamide. The structure of the compound was established by elemental analysis, Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), UV-Visible, and single-crystal X-ray diffraction. The compound crystallizes in the triclinic crystal system with the space group Pī, with unit cell parameters a = 10.286(2) Å, b = 11.795(2) Å, c = 21.331(4) Å, α = 100.270(3)°, β = 90.093(3)°, γ = 90.062(3)°, and Z = 4. The crystal and molecular structure of the title molecule is stabilized by intra-molecular interactions of types C–H···N and C–H···O.