Vortex Counter-Current Chromatography: Performance of a New Preparative Column

A new preparative column for the vortex counter-current chromatograph was fabricated by making many (966) cylindrical separation units to a high-density polyethylene disk and then threading them with 6–40 taps. The resulting column had a total capacity of 364 mL. The performance of this vortex column was examined with three different two-phase solvent systems each using a set of suitable test samples: hexane–ethyl acetate–methanol–0.1 M hydrochloric acid (1:1:1:1, v/v) for the separation of DNP-amino acids; 1-butanol–acetic acid–water (4:1:5, v/v) for the separation of dipeptides; and hexane–acetonitrile–water (20:15:2, v/v) for the separation of Sudan dyes. Most of the separations show high partition efficiency of over a thousand theoretical plates, as expected based on the results previously obtained in preliminary separations with a small column. Overall, the results of the present study suggest that further improvement of the partition efficiency can be obtained by the modifying column configuration.

     

Corrosion inhibition of ammonium molybdate for AA6061 alloy in NaCl solution and its synergistic effect with calcium gluconate

The corrosion inhibition of ammonium heltamolybdate (AH) and calcium gluconate (CG) for AA6061 alloy in 3% NaCl solution was investigated by the electrochemical measurements. It indicates that AH inhibits the corrosion of AA6061 alloy and acts as an anodic inhibitor. Maximum inhibition efficiency reaches 74.3% at the concentration of 1 × 10^?4 mol.l^?1 AH. The results of the electrochemical studies reveal AH is physically adsorbed on the AA6061 alloy surface and the adsorption follows Langmuir isotherm. The combination of AH and CG enhances the inhibition efficiency to 95.9%. The enhanced inhibition is attributed to the promotion of AH adsorption by CG. The mixture of AH and CG is a mixed‐type inhibitor and renders the corrosion potential to more positive values. Copyright © 2011 John Wiley & Sons, Ltd.     

Organophosphine/phosphite‐stabilized silver(I) complexes bearing N‐acetylbenzamide ligand: synthesis,characterization and potential application in metal organic chemical vapor deposition

New N‐silver(I) acetylbenzamide complexes of type L_n?AgNC₉H₈O₂ (L = PPh₃; n = 1, 2a; n = 2, 2b; n = 3, 2c; L = P(OEt)₃; n = 1, 2d; n = 2, 2e; n = 3, 2f) were prepared. These complexes were obtained in high yields and characterized by elemental analysis, ¹H NMR, ¹³C{H} NMR, ³¹P{H} NMR and IR spectroscopy, respectively. The molecular structure of 2b has been determined by X‐ray single‐crystal analysis in which the silver atom is in a distorted tetrahedral geometry and crystallizes as cis–trans. New N‐silver(I) acetylbenzamide complexes have a four‐membered ring, which could influence their chemical and physical properties and modulate volatility. Metal organic chemical vapor deposition experiments were carried out successfully at 400°C and 450°C using 2e as precursor for the deposition of silver films, respectively. The high‐purity silver film obtained at 400°C is dense and homogeneous. Copyright © 2012 John Wiley & Sons, Ltd.     

Nanoscale Broadband Viscoelastic Spectroscopy of Soft Materials Using Iterative Control

A novel approach to nanoscale broadband viscoelastic spectroscopy is presented. The proposed approach utilizes the recently developed modeling-free inversion-based iterative control (MIIC) technique to achieve accurate measurement of the material response to the applied excitation force over a broad frequency band. Scanning probe microscope (SPM) and nanoindenter have become enabling tools to quantitatively measure the mechanical properties of a wide variety of materials at nanoscale. Current nanomechanical measurement, however, is limited by the slow measurement speed: the nanomechanical measurement is slow and narrow-banded and thus not capable of measuring rate-dependent phenomena of materials. As a result, large measurement (temporal) errors are generated when material is undergoing dynamic evolution during the measurement. The low-speed operation of SPM is due to the inability of current approaches to (1) rapidly excite the broadband nanomechanical behavior of materials, and (2) compensate for the convolution of the hardware adverse effects with the material response during high-speed measurements. These adverse effects include the hysteresis of the piezo actuator (used to position the probe relative to the sample); the vibrational dynamics of the piezo actuator and the cantilever along with the related mechanical mounting; and the dynamics uncertainties caused by the probe variation and the operation condition. In the proposed approach, an input force signal with frequency characteristics of band-limited white-noise is utilized to rapidly excite the nanomechanical response of materials over a broad frequency range. The MIIC technique is used to compensate for the hardware adverse effects, thereby allowing the precise application of such an excitation force and measurement of the material response (to the applied force). The proposed approach is illustrated by implementing it to measure the frequency-dependent plane-strain modulus of poly(dimethylsiloxane) (PDMS) over a broad frequency range extending over 3 orders of magnitude (~1 Hz to 4.5 kHz).     

北京自由电子激光最近进展──实现饱和振荡

北京自由电子激光(BFEL)装置于1993年底在10.68μm处实现了饱和振荡.输出激光能量为3mJ,饱和平顶宽度2μs.对应饱和振荡平均功率为210kW(宏脉冲),峰值功率约为20MW,比自发辐射高8个量级,单程小讯号净增益为24%,转换效率为0.45%,与理论预期结果相符.光束质量接近衍射极限.目前装置可工作于9-11μm.     

利用不完全自锁模激光研究C60的反饱和吸收效应

本文报道首次采用色心晶体的不完全自锁模激光（１０６４ｎｍ）对Ｃ６０分子反饱和吸收效应的研究，实验结果与采用平均过程的研究方法是一致的，文中还讨论了Ｃ６０分子反饱和吸收效应产生的原因。     

石油醚在流体静高压下的超声声速、衰减、密度和绝热压缩系数

 专门设计了用脉冲-回波-重合法在不同静水压下测量液体声速的装置，并对石油醚在0.1~650 MPa流体静压力范围内测量了其超声声速和衰减系数。还通过测量体积压缩量和质量得到石油醚密度ρ随流体静压力的变化。最后，给出了石油醚的绝热压缩系数β与流体静压力的关系。