三溴偶氮胂催化光度法测定痕量铁

本文研究了硫酸介质中痕量 Fe(Ⅲ)催化加速抗坏血酸、溴酸钾和三溴偶氮胂之间的褪色反应及动力学条件,建立了动力学光度法测定痕量Fe(Ⅲ)的新方法.方法灵敏度为1.82×10~(-12)g·ml~(-1).测定范围为Fe(Ⅲ)0～30ng/25ml.已用于人发和食品中痕量铁的测定.结果满意.     

EFFECT OF MOLECULAR WEIGHT OF PDMS ON MORPHOLOGY AND MECHANICAL PROPERTIES OF PP/PDMS BLENDS

 A series of polydimethylsiloxane (PDMS) with varied molecular weights (Mw = 3  106, 1  106 and 0.5  106) were melt blended with PP to investigate the effect of PDMS molecular weight (MW) on the morphology and mechanical properties of PP/PDMS blends. Scanning electron microscopic (SEM) examination showed that the size of PDMS domains was dependent on the MW of PDMS. It was found that the lower the value of PDMS MW, the better dispersion of the PDMS domains in the PP matrix. Tensile and Izod impact tests revealed that the addition of PDMS with lower MW would lead to a more significant increase in impact strength of the blends compared with the blends with higher MW ones, while the influence of the molecular weight on tensile strengths of the blends was relatively small in the MW range studied. Differential scanning calorimetry (DSC) results also showed that the crystallization temperature of PP was increased with decreasing PDMS MW, indicating a better nucleation capability of lower MW of PDMS. Melting flow rate (MFR) measurements indicated that the processibility of PP could be enhanced by adding PDMS, and again the lower MW PDMS resulted in better data. Our work demonstrates that not only the processibility but also the mechanical properties of PP could be enhanced to a more significant degree by using low MW PDMS than the higher ones.     

Vibrational energy relaxation dynamics of Si---H stretching modes on stepped H/Si(111) 1×1 surfaces

The vibrational energy relaxation rates of excited Si---H stretching modes on the monohydride steps of miscut H/Si(111) 1×1 surfaces are calculated using Bloch-Redfield theory combined with classical molecular dynamics (MD) simulation. The structure and vibrational frequencies of the surface are first investigated using the Car-Parrinello ab initio MD method. The calculated Si---Si---H bending frequencies and relaxed structures are then used to refine the empirical potential for the classical MD simulations. The lifetime of the excited Si---H stretching mode at the step is found to be shorter than the modes on the terrace. Both the magnitude and the trend of the calculated results agree well with the experimental measurement on the 9° monohydride stepped surface. The vibrational relaxation rate of the Si---H stretching modes on the 15° monohydride stepped surface are also calculated and predicted to have a slightly shorter lifetime than for the 9° surface.     

水热合成CdS纳米晶体的形貌控制研究

研究了水热合成CdS纳米晶体形貌的化学控制，选择不同的络合试剂为模板,研究其对水热合成CdS纳米晶体形貌的影响.实验发现若以络合试剂乙二胺、甲胺为模板时，产品CdS晶体的形貌分别为（20～30） nm×（200～600） nm和（40～50） nm×（200～600） nm尺寸的纳米棒;而以络合试剂吡啶、 氨为模板时，产品CdS晶体的形貌分别为平均尺寸约30 nm和20 nm的纳米颗粒.用XRD、TEM、XPS、PL和Raman光谱等技术对所得CdS纳米棒进行了表征.同时对水热合成CdS纳米晶体形貌的模板控制机制进行了探讨，提出了一种水热合成CdS纳米棒的络合物结构诱导生长机理.     

茂基稀土胺化物与异氰酸正己酯的反应-{(MeC5H4)2Yb[OC(NPh2)N(n-hexyl)]}2的合成及表征

茂基稀土胺化物(MeCp)2YbNPh2(THF)与异氰酸正己酯(n-HexylNCO)按11摩尔比反应, 分离出产物{(MeC5H4)2Yb[OC(NPh2)N(n-hexyl)]}2. 产物经元素分析和核磁共振表征, 并测定了其晶体结构. 配合物属三斜晶系, R-3空间群, 晶胞参数为a=2.9533(11) nm, b=2.9533(11) nm, c=1.5873(6) nm, V=11.9896(80) nm3, Z=9, Dc=1.562 mg·m-3, μ=3.536 mm-1 (Mo Kα), F(000)=5670, R=0.034, Rw=0.064. 该化合物具有二个对称氧桥的双分子结构, 并存在着由氮原子向中心金属镱分子内配位而形成的三环骨架, 中心金属镱的配位数是九, 整个分子呈中心对称.     

甲胺化反应催化剂稀土改性丝光沸石的研究

研究了稀土改性丝光沸石催化剂对常压固定床上甲胺化反应的活性及选择性的影响，结果表明，以钇改性丝光沸石催化剂的活性及对二甲胺的选择性最佳。催化剂表征结果表明，稀土改性丝光沸石主要是引起丝光沸石中Ｂ酸中心发生变化，而对丝光沸石的晶体结构及表面硅铝原子比基本不产生影响。稀土改性能增强催化剂的热稳定性，延长催化剂的寿命。     

Microcalorimetric investigation of the growth of the <Emphasis Type="Italic">Escherichia coli</Emphasis> DH5α in different antibiotics

The effects of Amoxicillin Sodium and Cefuroxime Sodium on the growth of E. coli DH5α were investigated by microcalorimetry. The metabolic power-time curves of E. coli DH5α growth were determined by using a TAM air isothermal microcalorimeter at 37°C. By evaluation of the obtained parameters, such as growth rate constants (k), inhibitory ratio (I), the maximum heat power (P _m) and the time of the maximum heat power (t _m), one found that the inhibitory activity of Amoxicillin Sodium vs. E. coli DH5α is enhanced with the increasing of the Amoxicillin Sodium concentration, and the Cefuroxime Sodium has a stimulatory effect on the E. coli DH5α growth when the concentration is about 1 μg mL⁻¹. The IC₅₀ for the Amoxicillin Sodium and the Cefuroxime Sodium are 1.6 and 2.0 μg mL⁻¹, respectively, it implicates that the E. coli DH5α is more sensitive to Amoxicillin Sodium than Cefuroxime Sodium.     

Synthesis of alpha-MoTe2 nanorods via annealing Te-seeded amorphous MoTe2 particles

Semiconductor alpha-MoTe2 nanorods have been synthesized by annealing Te-seeded particles of an amorphous MoTe2 intermediate. This intermediate is prepared by a solution reaction between Mo(CO)6 and elemental Te in diphenylmethane. The as-synthesized products were characterized by structural, compositional, and morphological techniques of X-ray diffraction, selected area electron diffraction, selected area energy dispersive spectroscopy, energy dispersive X-ray analysis, X-ray photoelectron spectroscopy, transmission electron microscopy, and high-resolution transmission electron microscopy. The results of the annealing process are MoTe2 nanorods with diameters of 50-200 nm and lengths ranging from 0.1 to 3.0 microm. Here, the rodlike structure of MoTe2 is reported for the first time, and added to the list as one kind of new morphology of MoTe2 nanomaterials. A mechanism for the formation of the nanorods is proposed. The sandwich-layered structure of Te-Mo-Te and the similarity in the structure between hexagonal alpha-MoTe2 and hexagonal Te are responsible for the formation of nanorods of MoTe2.     

羧酸铜催化反应的研究——Ⅰ.羧酸铜催化醛肟转变为睛

本文报道了在多种羧酸铜催化下,醛肟在含有氰基的溶剂中(如CH_3CN、CH_3OCH_2CH_2CN等),均可脱水转变成相应的腈。反应条件温和,产率较高。具有不同空间和电性效应取代基的羧酸铜对反应的产率影响不大。实验中还发现溶剂乙腈参与了上述反应。     

Sesquiterpenoids from the Rhizome of Ligularia virgaurea

Two novel sesquiterpene dimers, compounds 1 and 2 , were isolated from the rhizome of Ligularia virgaurea, together with the six known sesquiterpenoids 3 – 8 . Their structures were established by physico‐chemical and spectroscopic methods, especially by means of 1D‐ and 2D‐NMR as well as HR‐MS analyses. A mechanism based on a classical Diels–Alder cyclization is proposed for the formation of the dimer 1 from the precursors 8 and the quinone form of 6 (Scheme).