复式螺旋测微器螺距误差补偿与示值误差综合

本文简要介绍了复式螺旋测微器的设计原理,在复式螺旋运动误差分析的基础上,提出了一种螺距误差自动补偿方法。通过样机的螺距误差实测曲线和测微器示值误差检定结果,验证了它的可行性和示值误差综合的正确性。     

CoC60(OH)的合成及氧化还原性能

富勒烯独特的电子及空间结构 ,使富勒烯及其衍生物具有特殊的物理化学性能[1 ,2 ] 。在富勒烯金属化合物方面 ,如碱金属原子可以与C60 键合成类“离子型”化合物而表现出十分良好的超导特性[3] 。过渡金属也能与富勒烯形成稳定的过渡金属富勒烯化合物[4] ,此类化合物可能具有与碱金属富勒烯化合物不同的性能 ,如Pd和C60 形成C60 Pdn后具有良好的催化性能[5] 。最近Chi等[6] 合成出稀土富勒烯化合物Sm3C70 ,并且认为Sm与C70 是以共价键的形式结合。研究的主要目的是通过研究富勒烯衍生物结构与性能之间的内在联系规律 ,以期在开发应用方…     

A Novel Mixed-valence and Capped-keggin Structural Polyoxometal Complex： {[Co（dien）]4- [（PO4）MoVs（WVI0.56 noVI0.44）4033（OH）3]}.nH2O （n ≈ 1）

A novel inorganic-organic hybrid compound, {[Co（dien）]4[0aO4）MoV8（wV10.56MoV10.44）4- O33（OH）3]}＇nH20 （1, n = 1, dien = diethylenetriamine）, has been synthesized hydrothermally and characterized by single-crystal X-ray diffraction. Compound 1 crystallizes in the triclinic system with a = 11.927（2）, b = 13.328（3）, c = 19.306（4）A, a = 93.76（3）, β = 94.14（3）, γ = 109.99（3）°, V= 2863.2（12） A3, space group P1 and Z = 2 at 173 K. The final full-matrix least-squares refinement converged to R = 0.049 for 9621 observed reflections with 1 〉 2σ（I） and wR = 0.139 for all data （9871） and S = 1.073. Crystal structure analysis shows that 1 contains a kind of the first reported mixed-valence and molybdenum-tungsten mixed-distributed e-Keggin structural polyanion capped by four Co（dien） fragments with the main group element P occupying the center site. These results were further confirmed by energy-dispersive X-ray spectroscopy （EDS）, X-ray powder diffraction （XRD）, Fourier transform infrared spectroscopy （FTIR）, Raman spectroscopy, Thermogravimetry （TG） and X-ray photoelectron spectroscopy （XPS） analyses.     

Stabilization of zeylenone in rat plasma by the presence of esterase inhibitors and its LC‐MS/MS assay for pharmacokinetic study

Six esterase inhibitors, namely EDTA·2Na⁺, NaF, phenylmethanesulfonyl fluoride, dichlorvos, bis‐nitrophenyl phosphate (BNPP) and thenoyltrifluoroacetone, and the mixture of NaF and BNPP, were evaluated for the stabilization of labile benzoate containing zeylenone in rat plasma. The mixture appeared to exhibit the most effectively stabilizing effect with the degraded content of zeylenone decreasing from >60% (in the absence of inhibitors) to <6%. Following the stabilization by the addition of NaF (5 mm ) and BNPP (5 mm ), the analytes in rat plasma were acidified by formic acid and extracted into ethyl acetate at 0°C. After chromatographic separation, the detection of zeylenone was performed on a 3200 Q‐Trap with positive ion electrospray mode, monitoring the ion transition m/z 383.2 → 105.0. The method was validated over the range from 2.68 to 1340 ng/mL with inter‐ and intra‐run precision for the quality control samples being less than 6.8%. The assay accuracy was within 100 ± 7.0%. The validated method was successfully applied to a pharmacokinetic study in rats after the intratracheal administration of zeylenone in free drug or polymeric micellar solutions. The results showed that the pulmonary absorption of zeylenone loaded in micelles was significantly retarded compared with that of free drug solutions. Copyright © 2012 John Wiley & Sons, Ltd.     

膨胀石墨 3 mm波消光数值计算

为探讨膨胀石墨作为3 mm波干扰材料的消光、散射特性及其影响因素, 基于有限长度、有限电导率圆柱状导体的电磁散射, 利用矩量法建立了膨胀石墨的消光、散射、吸收及后向散射截面(雷达散射截面RCS)的计算式. 运用Mathematica编程计算并分析了膨胀石墨长度、半径、电导率、磁导率等因素与膨胀石墨消光、散射、吸收截面及RCS的关系. 结果表明: 当膨胀石墨的长度为1.5 mm、半径为0.05 mm时, 具有较好的消光、散射效果; 适当增大膨胀石墨的电导率、磁导率, 有利于提高其消光、散射能力. 本研究为探索增强膨胀石墨干扰3 mm波效果的技术途径提供了有价值的参考.关键词：膨胀石墨石墨层间化合物消光截面矩量法     

Ion Exchange Separation of Eu3+ from Different Salt Solutions

Two samples of potassium zinc hexacyanoferrate were prepared using two different ratios of the initial materials. The distribution coefficient of Eu³⁺ on the two samples was determined. The effect of the cation concentration in the aqueous phase on the adsorption of Eu³⁺ was also studied. The mechanism of the exchange process was described on the light of the data obtained, and the equilibrium constant of the exchange reaction was also calculated.     

一步法合成的FeOOH/黑磷纳米复合材料协同实现体系优异的析氧性能

通过水热法,在黑磷(BP)纳米片表面生长FeOOH纳米材料,制备出FeOOH/BP纳米复合材料。作为电化学析氧反应(OER)催化剂,该复合材料在20 mA·cm^-2时的过电位仅为191 mV,Tafel斜率为49.9 mV dec^-1;在循环1 000圈后,过电位仅仅增加了3 mV,且循环过程中元素价态不变,表现出优秀的稳定性。纳米FeOOH负载于BP表面,客观上能隔断氧气对BP的氧化,保护BP的载流子传导性能。同时,生长的FeOOH颗粒尺度小,结晶性弱,这有利于丰富其活性位点,增大活性面积。     

A μ3-OH- bridged two-dimensional zinc(Ⅱ) coordination polymer based on an anthryl ligand：Synthesis, characterization and luminescent properties

A two-dimensional (2D) 3,3,3,4,5,5,6-connected ZnⅡ coordination compound [Zn5(L)2(OH)6]∞ (L=9,10-dioxo-9,10-dihydroanthracene-1,8-dicarboxylate) has been synthesized and characterized by IR, elemental analysis, X-ray powder diffraction and single crystal X-ray diffraction analysis. Moreover, the luminescent properties of the ligand and corresponding compound have been briefly investigated.     

Phen-铜(II)-氨基酸配合物的合成、表征及其SOD活性

合成了3个新的SOD模拟配合物：[Cu(Phen)(L-Gln)(H₂O)]Cl·2H₂O (1)、[Cu(Phen)(L-Ala)(H₂O)]Cl·4H₂O (2)、[Cu(Phen)(L-Thr)(H₂O)]Cl·2H₂O (3) [Phen(1，10-邻菲咯啉)、L-Gln(谷氨酰胺)、L-Ala(丙氨酸)、L-Thr(苏氨酸)]。用元素分析、摩尔电导、红外光谱、紫外-可见光谱对配合物进行了表征。用X-射线衍射对配合物[Cu(Phen)(L-Gln)(H₂O)]Cl·2H₂O的晶体结构进行了测定。用氯化硝基四氮唑蓝(NBT)光还原法对这3个配合物催化歧化超氧阴离子自由基(O₂^{- ·})的能力进行了测定。结果表明：这些配合物具有较高的SOD活性， 催化速率常数K_Q分别为1.58 × 10⁷ mol^-1·L·s^-1、5.65 × 10⁷ mol^-1·L·s^-1、0.83 × 10⁷ mol^-1·L·s^-1。     

希土脯氨酸配合物的合成和性质研究

通过希土氯化物与L-脯氨酸反应,制得了四种新的希土脯氨酸固体配合物。其通式为:Ln(prol)Cl₃·nH₂O(Ln=Y、La、Sm和Er).用化学分析、电导测定、热重分析、差热分析、红外光谱和核磁共振氢谱,确定了产物的组成,讨论了金属-配体的化学键性质。