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.

     

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.     

Rejoinder for Gaining effciency via weighted estimators for multivariate failure time data

We thank all the discussants for their interesting and stimulating contributions. They have touched various aspects that have not been considered by the original articles.     

Highly selective synthesis of single-walled carbon nanotubes from methane in a coupled Downer-turbulent fluidized-bed reactor

For the synthesis of single-walled carbon nanotubes (SWCNTs) from CH₄ over a Fe/MgO catalyst, we proposed a coupled Downer-turbulent fluidized-bed (TFB) reactor to enhance the selectivity and yield (or production rate) of SWCNTs. By controlling a very short catalyst residence time (1–3 s) in the Downer, only part of Fe oxides can be reduced to form Fe nano particles (NPs) available for the growth of SWCNTs. The percentage of unreduced Fe oxides increased and the yield of SWCNTs decreased accordingly with the increase of catalyst feeding rate in Downer. SWCNTs were preferentially grown on the catalyst surface and inhibited the sintering of the Fe crystallites which would be formed thereafter in the downstream TFB, evidenced by TEM, Raman and TGA. The coupled Downer-turbulent fluidized-bed reactor technology allowed higher selectivity and higher production rate of SWCNTs as compared to TFB alone.     

Etching Characteristics and Mechanisms of Mo and Al2O3 Thin Films in O2/Cl2/Ar Inductively Coupled Plasmas: Effect of Gas Mixing Ratios

An investigation of etching behaviors for Mo and Al₂O₃ thin films in O₂/Cl₂/Ar inductively coupled plasmas at constant gas pressure (6 mTorr), input power (700 W) and bias power (200 W) was carried out. It was found that an increase in Ar mixing ratio for Cl₂/Ar plasma results in non-monotonic etching rates with the maximums of 160 nm/min at 60 % Ar for Mo and 27 nm/min at 20 % Ar for Al₂O₃. The addition of O₂ in the Cl₂/Ar plasma causes the non-monotonic Mo etching rate (max. 320 nm/min at 40–45 % O₂) while the Al₂O₃ etching rate decreases monotonically. The model-based analysis of etching kinetics allows one to relate the non-monotonic etching rates in Cl₂/Ar plasma to the change in the etching regime from the ion-flux-limited mode (at low Ar mixing ratios) to the neutral-flux-limited mode (for high Ar mixing ratios). In the Cl₂/O₂/Ar plasma, the non-monotonic Mo etching rate is probably due to the change in reaction probability.     

On the structure of split Leibniz triple systems

We study the structure of arbitrary split Leibniz triple systems with a coherent 0-root space. By developing techniques of connections of roots for this kind of triple systems, under certain conditions, in the case of T being of maximal length, the simplicity of the Leibniz triple systems is characterized.     

Rapid and efficient column separation of Re(VII) as a surrogate for Tc(VII) with benzimidazole-based cross-linked poly(ionic liquid)s

Journal of Radioanalytical and Nuclear Chemistry - In this study, the imidazole-based poly(ionic liquid)s (PILs) synthesized by one step method has been applied for the enrichment and recovery of...