Upon spectrophotometric testing of trace zinc(Ⅱ) using a new color reagent——meso-tetrakis(3-trifluoromethyl-phenyl) porphyrin(T(3-TFMP) P) the impact of microwave catalyzed reaction and the microwave operating conditions on the color reaction was studied.Experiments showed that in a mixture containing a buffer solution with a pH value of 10.8,Tween-80,and hydroxylamine hydrochloride,the color reactions were realized when the mixture was heated for 50 minutes via microwave catalysis.The linear range of the amount of zinc(Ⅱ) thus determined was 0～4.0 μg/25 mL,while the molar absorptivity e429 was 5.13×105 L·mol-1·cm-1.When CyDTA was added along with a mixed screening agent during the discoloring spectrophotometric tests,the interference from most coexisting ions could be avoided.This method can be applied to the testing of trace zinc(Ⅱ) in triethylene glycol and health products.

Nanometer copper ferrite was synthesized by auto-combustion method using cupric nitrate, ferric nitrate and malic acid as raw materials. The precursor and as-burnt sample were characterized by X-ray Diffraction (XRD) and Transmission Electron Microscopy (TEM). Average particle size of sample is 26nm. The catalytic performance of nanometer CuFe2O4 on the thermal decomposition of ammonium perchlorate (AP) was investigated by DTA. The results show that the nanometer CuFe2O4 has high a catalytic activity. and the thermal decomposition temperature of AP shift 105 degrees C downward with the effect of nanometer copper ferrite. When the content of CuFe2O4 Comes to 5%, the catalytic performance is the best. (C) 2008 Published by Elsevier B.V.

3-aminoanisole was diazotized with conc.HCl and NaNO_2 below 5 ℃ and treated with fluoroboric acid 4%(Schiemann reaction)to give 3-fluoroanisole in 36.6% yield.Then,the mixture of 65%～68% nitric acid,glacial acetic acid and acetic anhydride was dropped slowly to 3-fluoroanisole at 60℃ for 1h(3-fluoroanisole and nitric acid molar ratio 0.0624∶0.0721,glacial acetic acid and acetic anhydride volume ratio 10.6∶7.6) on water bath to produce 3-fluoro-4-nitroanisole in 48.7% yield(bp 151.2 ℃).3-Fluoro-4-nitroanisole was reduced by ZnCl_2 and HCl for 12h to form 3-fluoro-4-aminoanisole in 84.1% yield(mp 240～241 ℃).Finally,3-fluoro-4-iodoanisole was obtainde in 72.0% yield(mp 123～123.5 ℃)by diazotization of 3-fluoro-4-aminoanisole at 5 ℃ in NaNO_2 and H_2SO_4 and addition of KI(Sandmeyer reaction).The product was characterized by boiling point,melting point,melting point IR,()~1H NMR,MS and elemental analysis.

It is very important to determine the protonation constants of tetraphenylporphyrin derivatives for studying their colorful performance.The over-all protonation constants of two tetraphenylporphyrin derivatives were determined by spectrophotometric methods.The influence of electron effect and steric hindrance of substituting group on overall protonation constants was discussed.With chromophore introduced,it is expected to enhance the selectivity of tetraphenylporphyrin derivatives reagents.

Nano-sized MgO were prepared by a solid-state method at lower temperature using MgCl2·6H2O and H2C2O4·2H2O as raw materials and soluble starch and PEG1000 as dispersing agents.The particle size and morphology of nano-sized MgO were investigated by IR,TG-DTA,XRD and TEM.The results indicate that the species and using level of dispersing agent were important factors to the particle size and distribution of the nano powder.

NiO nanoparticles have been successfully prepared by calcining malate gel, using basic nickel carbonate (BNC) and malic acid as the raw materials and H2O as the solvent. The reaction was studied by TG-DTA, XRD and FT-IR. The particle size and morphology of NiO nanoparticles was characterized by TEM. The results show that nickel malate could be formed by the reaction of BNC and malic acid; the gel was composed of nickel malate and residual malic acid; the precursor can translate into NiO nanoparticles completely at 400 degrees C under the air, and the as-prepared sample has a cubic crystal structure with about 14 nm of average diameter by the Schemer formula. The NiO calcined at 400 degrees C for 1 h was of narrow particle size distribution, weak agglomeration and small particle size. The particle size of NiO increased with the increase in temperature. Compared with other methods, the developed method is simple and the raw materials were inexpensive, so that it has the potential for further scale-up application in the industry. Furthermore, the reason for the metallic nickel formation in the course of the preparation was explained. (c) 2006 Elsevier B.V. All rights reserved.

Cubic crystals of nanosized magnesium oxide were prepared by the lower-temperature hydrothermal method,using magnesium dichloride and sodium oxalate as rawmaterials in the exist of the surfactant and MgO nanocrystallites can be easily obtained by calcining the precursors.Effect to the size of the crystals of thermal treatment temperature,hydrothermal reaction time and concentration of rawmaterials had been studied by XRD.The as-prepared sample were characterized by TG-DTA,FTIR,TEM,SAEM and XRD.The results showed that the crystals are uniform and unabridged and the size of the crystals is about 5nm.

Novel acetylpyrazine thiocarbohydrazone (1), 1-acetylpyrazine-5-[5- bromosalicylaldehyde]-dithiocarbohydrazone (2a), 1-acetylpyrazine-5-[5- chlorosalicylaldehyde]-dithiocarbohydrazone (2b), and 1-acetylpyrazine-5-[5- nitrosalicylaldehyde]- dithiocarbohydrazone (2c) have been synthesized and characterized by IR, 1H NMR, MS spectra and element analysis. The crystal structure of compound 1 was determined by X-ray single crystal diffraction analysis. Crystal structure of compound 1 belongs to monoclinic system with space C2/c. The unit cell parameters are a = 2.3057(14)nm, b = 0.7297 (4) nm, c = 1.1940(7) nm, V = 1.909(2) nm3, Z = 8, D c = 1.463g/cm3, μ = 0.309mm-1, F(000) = 880, R1 = 0.0866, wR2 = 0.2072.

分析了由于化学学科本身的特点、化学学科发展的现状以及中学化学课程改革而产生的化学知识更新问题,认为中学化学教师必须重视化学专业知识的再学习.提出至少应包括以下几个方面的学习:化学史;化学发展的新理论、新知识:社会发展涉及的化学知识;与化学有关的自然科学综合知识;化学研究中的科学方法.

N,N'-bis(L-phenylalanyl)ethane-1,2-diamine was prepared by using L-phenylalanine and ethanediamine. The synthetic process was improved. The ligand reacted with copper dichloride to form the chiral coordination compound. The single crystal was obtained in methanol solution. It is shown by X-ray structural studies that the crystal belongs to the tetragonal system and the space group is I4. The lattice parameters are as follows: a = 2.5044(4) nm, b = 2.5044(4) nm, c = 0.8707(3) nm, V=5. 461(2) nm(3), D-c = 1.365 g/ cm(3), Z = 8. In the structure of the complex, the Cu(II) cation is coordinated by two nitrogen atoms, two oxygen atoms and one chlorine atom.

OBJECTIVE METHODS 2-[(3,4-dimethoxy-benzylidene)amino]-ethanol,was synthesized and its composition and structure was characterized by elemental analysis,IR,MS,and ~(1)H-NMR.This compound was a new Schiff base.Its antibacterial activities were tested.RESULTS CONCLUSION The results showed that this new Schiff base is resistant to five different bacteria.

2,3-Diaminoanisole was diazotized with conc.HCl and NaNO_2 below 5 ℃ and treated with fluoroboric acids(w(HBF_4)=40%)(Schiemann reaction) to give 2,3-difluoro-4-iodoanisole(Ⅰ) in 40.7% yield.Then,the mixture of w(HNO_3)=65%～68% nitric acid,glacial acetic acid and acetic anhydride was dropped slowly to Ⅰ at 50～60 ℃ on water bath to produce 2,3-difluoro-4-nitroanisole(Ⅱ) in 51.9% yield,m.p.124 ℃.Ⅱ was reduced by SnCl_2 and HCl for 12 h to form 2,3-difluoro-4-aminoanisole(Ⅲ) in 84.6% yield,m.p.81～82 ℃.Finally,2,3-difluoro-4-iodoanisole were obtained in 75.5% yield(m.p.63～64 ℃) by diazotization of Ⅲ at 5 ℃ in NaNO_2 and H_2SO_4 and addition of KI(Sandmeyer reaction).The product was characterized by melting point,IR,~1HNMR,MS and elementary analysis.

The precursor for nano-sized magnesia was prepared by using Mg(NO3)(2) center dot 6H(2)O as raw material, the hydrolysis product of hexamethylene tetramine as precipitating reagent and water as reaction media, and with the polymer (PEG) and DMF as protection reagents for particles. Nano-sized magnesia was prepared by calcining the precursor at 873 K after being dehydrated by freeze centrifugation and vacuum drying at a constant temperature. The formation process and structure of MgO nanocrystallites were investigated by means of TG-DTA, FTIR, TEM, XRD and BET. The results showed that the crystal belonged to cubic system and the average size was 3.1 mn and the specific surface area was 229 m(2) center dot g(-1).

The magnesium oxide nanocrystallites were prepared by means of a sol-gel method with malic acid and magnesium nitrate as raw materials.Under different preparing conditions,the particle size can vary from(7 nm) to 20 nm.The intermediate gel and final product were characterized by FI-IR,TG-DTA,XRD and TEM.The effects of the ratio of the raw materials,calcined temperature and time,the initial pH value and the amount of ethanol on the particle size and morphology of the sample were analyzed.The results show that the conditions of the molar ratio of Mg~(2+) to malic acid being 1∶1.5,calcined temperature 500～700 ℃,calcined time 3 h,the initial pH value 3~7 and the volume ratio 1∶4 are favorable for the formation of nanosized(magnesium) oxide.The UV-Vis Spectra show that the UV-shielding capacity of the nanosized magnesium oxide is better than that of normal magnesium oxide.

N, N'-bis(L-phenylalanyl) ethane-1, 2-diamine was prepared by using L-phenylalanine and ethanediamine. The synthetic process was improved. The ligand reacted with copper dichloride to form the chiral coordination compound. The single crystal was obtained in methanol solution. It is shown by X-ray structural studies that the crystal belongs to the tetragonal system and the space group is I4. The lattice parameters are as follows: a=2.5044(4) nm, b=2.5044(4) nm, c=0.8707(3) nm, V=5.461(2) nm^3, D(subscript c)=1.365g/cm^3, Z=8. In the structure of the complex, the Cu(Ⅱ) cation is coordinated by two nitrogen atoms, two oxygen atoms and one chlorine atom.

Meso-tetrakis [3,5-bis (trifluoromethyl) phenyl] porphyrin [T(3,5-DTFMP)P] for the spectrophotometric determination of trace cadmium has been studied. The experimental results showed that the reaction was completed by heating at 100 ℃ for 7 min in an alkaline solution of pH 10.60. It was a sensitive and selective chromometric reagent for the direct determination of cadmium in the presence of Tween-80 and o-phenanthroline. Its apparent molar absorptivity e_(442) is 2.19×10~5 L·mol~(-1)·cm~(-1). Beer′s law is obeyed in the range of 0～3 μg of per 25 mL. This method has been successfully applied to the determination of cadmium in tobacco.

介绍Photoshop图像处理软件的功能与特点及其在化学作图中的应用

结合硕士研究生高等无机化学实验教学的实践与体会,提出了充分利用实验课加强对研究生创新能力培养的几点建议。

Combining the practice and experience of master degree candidates' high inorganic chemistry experiment teaching,this article put forward some suqgestion how to fully utilize the experimental lesson to strengthen training graduate students' innovation abilities.

Three new asymmetric bis-Schiff bases containing thiocarbohydrazide were synthesized by the reaction of thiocarbohydrazide with ketone and different aldehydes step by step. Compositions of these compounds were determined by IR, MS and elemental analysis.