Synthesis, Crystal Structure, UV-vis and EPR Studies of（ NH3CH2CH2NH2 ） 2.5 [ Mo0.5^（V）W0.5^（VI）O2 （ OC6H4O ） 2]

Cis-dioxo-metal complex ( NH3CH2CH2NH2 ) 2.5 [ Mo0.5^(V)W0.5^(VI)O2 ( OC6H4O ) 2] 1 was obtained by the reaction of tetra-butyl ammonium hexamolybdotungstate with 1, 2-dihydroxybenzene in the mixed solvent of CH3OH, CH3CN and ethylenediamine,and characterized by X-ray diffraction, UV-vis and EPR analysis. Compared with its analogous complexes (NH3CH2CH2NH2)3[Mo^(V)O2(OC6H40)2] 2 and (NH3CH2CH2NH2)2[W^(VI)O2(OC6H4O)2] 3, the results show that tungsten(VI) is less active in redox than molybdenum (VI) and that the change of the valence induced by substitution of W(VI) for Mo(V) in EMO2(OC6H40)2]n- does not influence the coordination geometry of the complex anion in which the metal center exhibits distorted octahedral coordination with cis-dioxo catechol. The responses to EPR of complexes 1 and 2 are active but complex 3 is silent,and the UV-vis spectra exhibited by the three complexes are obvious different because of the different electronic configuration between the central Mo(V) and W(VI) ions in the complexes.It is noteworthy that complexes 1 and 2 have the similar EPR signal to flavoenzyme, suggesting that the three complexes have the same coordination geometry feature with the co-factor of flavoenzyme.     

A Flexible Approach to the γ－Amino－β－hydroxy Acid Moiety of Hapalosin

A flexible approach to ethyl (3R,4S)-N-Boc-4-amino-3-hydroxy-5-phenylpentanoate (N-Boc-AHPPA-OEt), the γ-amino-β-hydroxy acid moiety of hapalosin is described. The synthetic method features a ring-opening ethanolysis of an activated N-Boc-lactam, which is obtained via a diastereoselective reductive-alkylation of (R)-malimide derivative. The flexibility of the method resides in the introduction of the alkyl side chain by Grignard reagent addition.     

Synthesis, Crystal Structure and Biological Activity of Novel Dichloroacetyl Oxazolidine Herbicide Safeners

A series of novel N-dichloroacetyl oxazolidine herbicide safeners was synthesized and characterized by IR, 1H NMR, 13C NMR, elemental analysis and X-ray diffraction. The preliminary biological test shows that the compounds could protect maize against injury caused by chlorsulfuron to a certain extent.     

金衢盆地加积型红土地球化学特征

金衢盆地广泛分布着不同类型的第四纪红土。通过X射线荧光光谱法（XRF）对金衢盆地的85个样品进行了测试。结果表明：（1）主量元素组成以SiO2、Fe2O3、Al2O3为主,K、Na、Ca、Mg等易溶组分的含量很低,TiO2含量的平均值高于UCC值;（2）MnO含量在网纹红土和均质红土的交界处明显聚集,推测与不同沉积物交界处理化性质突变有关;（3）在剖面上,SiO2、Fe2O3、AkO3等化学成分和硅铝率沿剖面变化的趋势,以及基岩和上覆沉积层的元素组成、化学风化指标和Ti／Zr的区别,均表明所研究的金衢盆地红土剖面具有较好的相似性,与典型的岩石风化壳存在明显差别。     

Electromagnetic Properties of YIG Polycrystalline Ceramics Fabricated by Tape-casting Method

Pure phase Y_3Fe_5O_(12) (YIG) ceramic was successfully produced by tape-casting forming process and one-step solid-state sintering method.The activation energy for densification was calculated to be 183.81 kJ/mol.Pure YIG ceramic with a relative density as high as 99.8%was fabricated.The existence of O vacancy and Fe~(2+)ions was determined by XPS and EPR spectra.The RT saturation magnetization was measured to be 28.2 emu/g,and the hysteresis loss was calculated to be smaller than 10 mJ/kg in the temperature range of 230～360 K and be as high as238.8 mJ/kg at 30 K.The dielectric loss tangent tan was nearly zero at 6～7 GHz and 11～12 GHz.For complex permeability in the frequency range of 5～18 GHz,the magnetic loss tangent tan fluctuated at around zero.Therefore,the low values of tan and tan indicate that it is a low loss ceramic material.     

基于机器学习的直接电离质谱爆炸物检测方法

直接电离质谱系统在现场快速检测中的应用日益广泛,主要用于爆炸物、毒品、食品添加剂等的检测.然而,直接电离质谱系统中质谱信号波动大且同一浓度样品峰强呈现对数正态分布,严重影响了检出限附近低浓度样品的检测准确性.该研究将乙酰水杨酸(115个样品)作为爆炸物模拟物,利用介质阻挡放电离子源与质谱系统,研究了基于机器学习的直接电...     

Au负载SBA-15分子筛上葡萄糖氧化反应

探讨了金与铝改性的SBA-15分子筛催化剂(Au-Al/SBA-15)上活性中心与葡萄糖氧化制葡萄酸反应性能的关系.通过固体核磁共振波谱(ss NMR)、X射线光电子能谱(XPS)、紫外-可见光谱(UV-Vis)和透射电子显微镜(TEM)等手段对不同Au及Al含量的Au-Al/SBA-15催化剂进行了结构表征.发现Al改性能够在SBA-15载体上产生四配位Al物种,Au主要以单质的形式存在; SBA-15上的四配位Al物种具有稳定Au颗粒大小的作用.通过对比发现,催化剂上的Au和骨架四配位Al物种间的相互协作促进了对葡萄糖氧化的活性,而非骨架Al物种会导致副反应的发生,降低葡萄糖酸产物的选择性.通过固体13C NMR揭示了反应体系中的NaOH能够将强吸附的产物葡萄糖酸分子从催化剂表面解离,保持活性位不被覆盖进而促进反应持续进行.     

岱衢族大黄鱼不同组织的同工酶谱

于2006年11月,在象山港采集30尾网养岱衢族大黄鱼,采用聚丙烯酰胺凝胶垂直电泳方法,研究分析了岱衢族大黄鱼眼睛、肌肉、肝脏、肾脏、脾脏、心脏、胸鳍、鳃和脑9种组织中16种同工酶（LDH、ADH、MDH、ME、SOD、POD、EST、GAD、ALP、ATP、FDH、SCD、IDH、GDH、ACP、GcDH）的表达情况,发现除IDH、GDH、ACP、GcDH 4种酶只显示微弱且不稳定的区带外,其他酶类在各组织中都显示出清晰稳定的酶谱,且这些酶在表型、分布和活性上均表现出高度的组织特异性,与各组织的生理功能相一致.     

马赫杆加载下无氧铜的动态破碎

为了深入了解金属材料在复杂加载下的动态破碎行为,在有限元模拟的基础上,设计了两类马赫杆加载实验,用于研究无氧铜在复杂加载下的动态破碎行为。实验中,采用火炮加载马赫透镜和激光粒子速度干涉仪测量自由面速度,实现了峰值压力分别为95.75和32.38 GPa的动态加载。结果表明,实验中成功实现了稳定的马赫杆加载,并且观察到马赫杆加载下无氧铜的2种不同近表面破碎模式,即高压下产生微层裂、低压下产生三角波层裂,且层裂区呈凸形分布。

     

自呼吸式DMFC电堆构建与电池性能研究

本文报道了一种能驱动风扇工作的自呼吸式DMFC小型电堆,电堆主要南燃料储罐、膜电极(MEA)、集流体等组成.文中针对影响该电池性能的主要参数,如电堆的活化过程、甲醇浓度等因素进行了研究.同时,本文还对电堆的恒电流放电时的电流曲线特点以及阴极水的生成规律进行了初步考察和探讨.