N-[(2,2–propinyldiferrocenyl)methinyl]benzoyl hydrazone and its bivalent transition metal complexes

Transition Metal Chemistry -     

Synthesis of monodisperse poly(chloromethylstyrene-co-divinylbenzene) beads and their application in separation of biopolymers

The monodisperse, porous poly(chloromethylstyrene-co-divinylbenzene) beads of 7.9 microm were prepared by a single-step swelling and polymerization method. The seed particles prepared by dispersion polymerization exhibited good absorption of the monomer phase. Based on this media, a weak cation-exchange (WCX) stationary phase for HPLC was synthesized by a new chemically modified method. The prepared resin has advantages of biopolymer separation, high column efficiency, low column backpressure, high protein mass recovery, and good resolution for proteins. The dynamic protein-loading capacity of the synthesized WCX packings was 18.2 mg/g. Five proteins were separated in 3.0 min using the synthesized WCX stationary phase. The experimental results show that the obtained WCX resin has very weak hydrophobicity. The WCX resin was also used for the rapid separation and purification of lysozyme from egg white in 5.0 min with only one step. The purity and specific bioactivity of the purified lysozyme were found to be more than 93% and 70 245 U/mg, respectively.     

Synthesis of Polyacrylaminothiourea Chelating Fiber and Properties of Concentration and Separation of Trace Noble Metal Ions from Samples

A novel polyacrylaminothiourea chelating fiber was synthesized simply and rapidly from nitrilon (an acrylonitrile-based synthetic fiber), which was applied to preconcentrate and separate of trace amount of Au(Ⅲ）,Pt(Ⅳ）,Pd(Ⅳ） and Ir (Ⅳ） ions from solution of samples.The analyzed ions can be quantitatively concentrated by the fiber up to a flow rate of 20.0mL/min at pH2, and can also be desorbed with 15 mL of 4mol/L HCl 3% thiourea from the fiber column with recoveries of 96.5%-100%.The chelating fiber can be reused for ten times,the recoveries of these ions are still over 92%,and hundred to thousand times of excess of Fe(Ⅲ）,Al（Ⅲ）,Ca(Ⅱ），Mg（Ⅱ）,Ni(Ⅱ）,Mn（Ⅱ),Cu(Ⅱ），Zn(Ⅱ），and Cd(Ⅱ） cause no interference on the determination of the analyzed ions by inductively-coupled plasma atomic emission spectrometry (ICP-AES).The static saturation adsorption capacities of the fiber for the analytes are in the range of 1.15-2.80mmol/g.The relative standard deviations for the determination of 20.0ng/mL each of Au(Ⅲ）,Pt(Ⅳ）,Pd(Ⅳ）and Ir(Ⅳ） are in the range of 0.7%-3.0%.The recoveries for test from standard additions to real solution samples are between 96% and 100%.The concentration of each ion in powder sample detected by the method is in good agreement with the certified value.     

A High-Order Finite Difference Scheme for 3D Unsteady Convection Diffusion Reaction Equations北大核心CSCD

针对三维非稳态对流扩散反应方程,构造了一种高精度紧致有限差分格式,对空间的离散采用四阶紧致差分方法,对时间的离散采用Taylor级数展开和余项修正技术,所提格式在时间上的精度为二阶、在空间上的精度为四阶。利用Fourier稳定性分析法证明了该格式是无条件稳定的。最后给出数值算例验证了理论结果。     

探究苯与酸性高锰酸钾溶液的褪色反应

人教版高中教材《化学2》明确指出苯不能使酸性高锰酸钾溶液褪色。但在实验中多次发现苯与酸性高锰酸钾溶液混合后放置一段时间能够褪色。为探讨这一问题，设计了以光照或黑暗、加酸或不加酸为条件，利用紫外-可见分光光度计对放置不同时间后的混合液体进行测试，并对反应后生成的沉淀物进行XRD表征的实验方案。通过对实验数据的综合分析提出了苯与酸性高锰酸钾溶液褪色反应的可能反应机理。     

Gas chromatographic/mass spectrometric and microbiological analyses on irradiated chicken

Ionizing radiation is widely used as treatment technique for food preservation. It involves among others reduction of microbial contamination, disinfestations, sprout inhibition and extension of shelf life of food. However, the commercialization of irradiated food requires the availability of reliable methods to identify irradiated foodstuffs. In this paper, we present results on the application to irradiated chicken of this method, based on the detection, in muscle and skin samples, of the peaks of ions 98 Da and 112 Da, in a ratio approximately 4:1, typical of radiation induced 2-dodecylcyclobutanones (2-DCB). Aim of the work was also to study the time stability of the measured parameters in samples irradiated at 3 and 5 kGy, and to verify the efficacy of the treatment from a microbiological point of view. Our results show that, one month after irradiation at 3 kGy, the method is suitable using the skin but not the muscle, while the measured parameters are detectable in both samples irradiated at 5 kGy. The microbial population was substantially reduced even at 3 kGy.     

Diffusion and localization of o-Ps in D2O determined from positron annihilation in SDS micellar solutions

A microscopic diffusion model is presented for the determination of orthopositronium (o-Ps) lifetime in micellar solutions. Among other parameters, the lifetime density function depends on the o-Ps diffusion coefficient in the water phase. Orthopositronium diffusion coefficients are determined by fitting this lifetime density function to positron annihilation spectra obtained from 1 mol/dm³ solution of sodium dodecylsulphate (SDS) in D₂O at different temperatures. The activation energy of the o-Ps diffusion in D₂O obtained from an Arrhenius plot as E_a = 0.9₂₂ ± 0.1₀₃ eV indicates strong localization.     

Selective Conversion of Glycerol to Methanol over CaO-Modified HZSM-5 Zeolite

Biodiesel is generally produced from vegetable oils and methanol, which also generates glycerol as byproduct. To improve the overall economic performance of the process, the selective formation of methanol from glycerol is important in biodiesel production. In the present study, a CaO modified HZSM-5 zeolite was prepared by an impregnation method and used for the conversion of glycerol to methanol. We found that the 10%CaO/HZSM-5 with Si/Al ratio of 38 exhibited highest selectivity to methanol of 70%, with a glycerol conversion of 100% under 340 ℃ and atmospheric pressure. The characterization results showed that the introduction of a small amount of CaO into the HZSM-5 did not affect the structure of zeolite. The incorporation of HZSM-5 as an acidic catalyst and CaO as a basic catalyst in a synergistic catalysis system led to higher conversion of glycerol and selectivity of methanol.     

Thermogravimetric study of alcohol adsorption on active charcoal

Interest of using the Mac Bain thermogravimetric balance in order to characterize alcohol adsorption or desorption on various active charcoal is developed. Precautions and peculiarities of proposed method are indicated. They result from very good precision and reproducibility in the thermal range of 273.15 to 313.5 K, and in the pressure range of 666.6 Nm⁻² to 26664 Nm⁻².Some results are given to illustrate the statics, and kinetics of adsorption desorption process of alcohol on various active charcoals.These results are important to develop and optimize refrigerating machines, or heat pumps, or physico-chemical storage using these systems.     

Ru、Rh、Pd掺杂GaSb的电子结构和光学性质

运用第一性原理计算方法研究了过渡族金属TM(TM=Ru、Rh、Pd)掺杂GaSb的电子结构和光学性质,结果表明:TM掺杂GaSb主要以TM替代Ga(TM @Ga)缺陷存在,并可增强GaSb半导体材料对红外光区光子的响应,使体系光学吸收谱的吸收边红移;TM@Ga所引入的杂质能级分布于零点费米能级附近,这极大地增强了体系的介电性能,促进了电子-空穴对的产生和迁移,因而提升了掺杂体系的光电转换效率;Ru 掺杂对GaSb光学性质的改善最为明显,当掺杂浓度为6.25%(原子数分数)且均匀掺杂时,Ru掺杂GaSb体系对红外光区光子的吸收幅度最大,有效提升了GaSb光电转换效率和光催化活性。