Synthesis of Titania Pillared Saponite in Aqueous Solution of Acetic Acid

The preparation of TiO₂-pillared saponite was carried out in a CH₃COOH aqueous solution. Titanium ion species to intercalate into the interlayer of saponite were obtained by an addition of Ti(C₃H₇O)₄ to an aqueous solution of CH₃COOH and by subsequent aging of the solution for a prescribed time. Ti⁴⁺-intercalated saponite including organic materials was obtained by ion exchange. After the sample was calcined at 500°C in air, TiO₂-pillared saponite was obtained. The resulting TiO₂-pillared saponite (Ti-Sapo) possessed surface areas in the range 300–400 m²/g and a sharp pore size distribution with the pore radius of 1.2 nm. The basal spacing of the product heated at temperature >250°C was about 2.45 nm. The pillar height of TiO₂ in the Ti-Sapo was estimated to be 1.5 nm.     

Influence of In3＋ ions concentration on spectroscopic properties of Ho：LiNbO3 crystals

In:Ho:LiNbO3 crystals doped with various concentrations of In3+(0, 1 mol.%, 3 mol.%, 5 mol.%), fixed concentrations of Ho3+ (1 mol.%) were grown by Czochralski method. The X-ray powder diffraction, infrared and UV-visible absorption spectra were measured and modified. Judd-Ofelt approach was employed to study the effect of In doping on spectroscopic properties of Ho:LiNbO3 crystals. In concentrations in crystals were analyzed by an inductively coupled plasma optical emission spectrometry (ICP-OE/MS). For In (3 mol.%):Ho (1 mol.%):LiNbO3 crystal, the obtained intensity parameters were: Ω2=9.6563, Ω4=4.2195, Ω6=14.1526. The results showed that the Ω2 and Ω6 parameters increased with the increase of In3+ concentration. When the In doping concentration was up to 5 mol.%, Ω2 and Ω6 suddenly decreased. In2O3 incorporation had a strong effect on the radiative lifetime, but had less influence on fluorescence branching ratios. The effective distribution coefficient of In3+ in In:Ho:LiNbO3 crystals was less than 1 and increased with increasing concentration of In3+ in the melt.     

A spectrophotometric method for quantitative determination of xylose in fermentation medium

Monitoring the consumption of sugars during fermentation is a key to optimizing product formation and maintaining a healthy environment for microorganisms. Difficulty arises in the availability of a rapid, inexpensive and sensitive method for the detection of sugars because fermentation media are a complex mix of nutrients, cell debris, waste and target products. A method involving reaction-based UV-Vis spectrophotometry for the quantitative determination of xylose as the target sugar was developed. Factors affecting xylose concentration measurements such as hydrochloric acid concentration, heating time and the amount of Fe³⁺ catalyst were investigated. A continuous scan revealed the working wavelength to be 671 nm. The effect of other components in the fermentation broth was found to be negligible. Absorbance shows a linear relationship with xylose concentration within a range of 0.1-0.5 g/L. Xylose concentrations from fermentation samples obtained at specific time intervals (0-168 h) were determined with the method and compared with YSI 2700, an enzyme electrode, HPLC-ELSD method, currently a common technique for measuring xylose and GC aldononitrile sugar derivatization method. Dilution is necessary for comparable xylose concentrations with YSI 2700 and HPLC-ELSD. Xylose concentration measurements obtained with the UV-Vis spectrophotometric method although quantitatively comparable to HPLC-ELSD xylose measurements were easily and conveniently obtained compared to YSI 2700, HPLC-ELSD and GC derivatization methods.     

工业氨肟化工艺失活HTS分子筛的结构特征和Ti物种状态

采用XRD及其Rietveld全谱拟合、低温N₂吸附-脱附、XPS、TEM（包括EFTEM和HRTEM）、UV-Vis等手段对失活HTS分子筛的晶胞参数、骨架结构、颗粒形貌和Ti物种的位置与状态进行分析。结果表明, HTS分子筛失活后,其拓扑结构保存完整,且晶胞参数未发生明显变化,但部分微孔结构发生溶解,介孔体积增大,比表面积略有下降。HTS分子筛失活后,部分骨架Ti物种转变为非骨架Ti物种,富集且高度分散于分子筛颗粒形成小碎片,可以初步判定该碎片为高度分散的无定型TiO₂或TiO₂-SiO₂氧化物。     

含噻吩环1,2,4-噁二唑类衍生物的合成及光电性能

以硫代二甘酸和取代苯甲腈为原料,经酯化、环化、酸化等反应合成了2,5-双[3-苯基-1,2,4-噁二唑-5-基]-3,4-二丁氧基噻吩衍生物,通过1HNMR、FTIR和元素分析进行了结构表征,并考察了该系列化合物的紫外-可见吸收光谱、荧光发射光谱及电化学性质。该系列化合物紫外吸收出现在240～250nm和320～350nm两个波段;荧光发射峰位于395～401.5nm,且随苯环上取代基供电子性的增强而规律性红移;循环伏安测定结果表明,该系列化合物中ⅧA、ⅧB、ⅧC和ⅧF具有高于常用电子传输材料2-(4-联苯基)-5-对叔丁基苯基-1,3,4-噁二唑(PBD)的电子亲和势,因而该类化合物的研究,对设计小分子类电致发光材料有重要意义。     

Speciation of Molybdenum (VI) In Aqueous and Organic Phases of Selected Extraction Systems

Abstract

The extraction study of molybdenum (VI) by 30% tri-n-butyl phosphate in n-dodecane and 0.2 M octyl (phenyl)-N,N-di-isobutylcarbamoylmethylphosphine oxide in 30% tri-n-butyl phosphate extraction systems was performed from aqueous solution containing HCl, HNO₃ and acetohydroxamic acid. Depending on extraction conditions, acetohydroxamic acid can significantly affect the speciation of molybdenum and can increase or decrease its distribution ratio. Our investigation confirmed the strong ability of the acetohydroxamic acid to form complexes with Mo even in highly acidic solutions. UV absorption spectra confirmed that a fraction of the Mo(VI)-AHA species can be present in the organic phase after extraction.     

含偶氮基团的不对称弯曲型液晶分子的合成及其光谱特性

合成了6个含偶氮基团的具有不同苯环个数的不对称弯曲型液晶分子,用1 H NMR、HRMS表征其结构,采用差示扫描量热法(DSC)和偏光显微镜(POM)研究其液晶性能。考察结果表明:所有化合物均出现了液晶相,特别是含有3个苯环的分子在较低温度下出现了向列相;偶氮基团的吸收光谱在330～360nm出现了较强的由π-π*电子跃迁引起的吸收,在430～450nm出现了较弱的由n-π*电子跃迁引起的吸收,其吸收波长的变化表明分子的弯曲形状和电子分布使分子吸收波长有较大的变化。     

Use of a Reflectance Spectroscopy Accessory for Optical Characterization of ZnO-Bi(2)O(3)-TiO(2) Ceramics

The optical band-gap energy (E(g)) is an important feature of semiconductors which determines their applications in optoelectronics. Therefore, it is necessary to investigate the electronic states of ceramic ZnO and the effect of doped impurities under different processing conditions. E(g) of the ceramic ZnO + xBi(2)O(3) + xTiO(2), where x = 0.5 mol%, was determined using a UV-Vis spectrophotometer attached to a Reflectance Spectroscopy Accessory for powdered samples. The samples was prepared using the solid-state route and sintered at temperatures from 1140 to 1260 °C for 45 and 90 minutes. E(g) was observed to decrease with an increase of sintering temperature. XRD analysis indicated hexagonal ZnO and few small peaks of intergranular layers of secondary phases. The relative density of the sintered ceramics decreased and the average grain size increased with the increase of sintering temperature.     

Investigating the impact of Cloisite® 15A nanoclays on the diffusivity of Irganox 1035 antioxidant in high-density polyethylene nanocomposite

Knowing the diffusion coefficients of antioxidants in packaging materials is essential to assess their effectiveness in protecting materials against oxidation, but also to prevent their eventual migration to food. In this work, the diffusion of a commercial phenolic antioxidant (Irganox 1035) was measured experimentally in pristine high-density polyethylene (HDPE) and in HDPE nanocomposite filled with 3 wt% of nanoclays (Cloisite® 15A). Diffusion experiments were performed using the Roe's method between 60 and 100°C. The local concentration of Irganox1035 in each film was measured by UV–Vis spectroscopy from the UV absorbance at 282 nm. The adjustment of the experimental data by Fick's second law allowed us to deduce the values of the diffusion coefficient of Irganox1035 at each temperature and to show that the temperature dependence of this coefficient obeys an Arrhenius' law. It is shown that the incorporation of 3 wt% of Cloisite®15A into HDPE significantly hinders the diffusion of Irganox 1035 and increases its activation energy. Several mechanistic assumptions could explain this result, first the increase in the tortuosity of diffusion paths, but also the possible establishment of strong intermolecular interactions between the antioxidant and some chemical groups on the nanofiller surface, or even the formation of an interphase with reduced molecular mobility around the nanofillers.