Preparation and characterization of long methacrylate monolithic column for capillary liquid chromatography

Long methacrylate monolithic columns (100 cm x 320 mum i.d.) were prepared from silanized fused-silica capillaries of 320 mum i.d. by in situ copolymerization of butyl methacrylate (BMA) with ethylene dimethacrylate (EDMA) in the presence of a suitable porogen. The separation performance and selectivity of the column were evaluated and compared with a 25 cm x 320 mum i.d. column prepared in the same way by capillary high-performance liquid chromatography (mu-HPLC) The results showed that the 1 m long monolithic column can generate 33 x 10(3) plate number and exhibited good permeability, higher sample loadability, and separation capability. (C) 2004 Elsevier B.V. All rights reserved.

Preparation of A-type zeolite membranes on nonporous metal supports by using electrophoretic technique

A-type zeolite membranes were prepared on the nonporous metal supports by using electrophoretic technique. The as-synthesized membranes were characterized by XRD and SEM. The effect of the applied potential on the formation of the A-type zeolite membrane was investigated, and the formation mechanism of zeolite membrane in the electric field was discussed. The results showed that the negative charged zeolite particles could migrate to the anode metal surface homogenously and rapidly under the action of the applied electric field, consequently formed uniform and dense membranes in short time. The applied potential had great effect on the membrane formation, and more uniform and denser zeolite membranes were prepared on the nonporous metal supports with 1 V potential.

Preparation of palladium membrane over porous stainless steel tube modified with zirconium oxide

A palladium membrane has been prepared by electroless plating on the surface of a porous stainless steel tube. Since the large surface pores of the tube are obstacle for preparation of a defect-free palladium film on the surface, zirconium oxide particles were deposited inside the pores. The mean thickness of the resulting Pd membrane on the modified tube was ca. 10 mum. It is suggested that the permeability of hydrogen is partly governed by gas diffusion in the pores. (C) 2004 Elsevier B.V. All rights reserved.

Preparation and characterization of monolithic columns for capillary electrochromatography with weak electroosmotic flow

Monolithic columns of capillary electrochromatography (CEC) with weak electroosmotic flow (EOF) have been prepared by in situ polymerization of butyl methacrylate and ethylene dimethacrylate, without any charged groups in the reaction mixture. The reproducibility of such columns has been proved good no matter whether they are prepared in the same batch or in different batches. In the case of BMA-EDMA monoliths, besides the traditional ternary mixture - 1-propanol, 1,4-butanediol, and water, binary porogenic solvents with only alcohols have also been adopted. Compared with ternary porogenic solvents, the design with binary ones allows for fine control of the pore diameter and the formation of the specific surface of the monolithic polymers. The composition of porogenic reagents has also been shown to have an effect on EOF in the column systems. In addition, the Joule heat effect in such columns has been studied by varying the inner diameter of columns. Through the separation of acidic compounds, monolithic columns with low EOF have shown potential in the analysis of charged samples.

Preparation of highly active Pt/C cathode electrocatalysts for DMFCs by an improved aqueous impregnation method

An improved aqueous impregnation method was used to prepare 40 wt% Pt/C electrocatalysts. TEM analysis of the samples showed that the Pt particles impregnated for a short time have a very narrow size distribution in the range of 1-4 nm with an average size of 2.6 nm. UV-vis spectroscopy measurements verified that the redox reaction between PtCl62- and formaldehyde took place with a slow rate at ambient temperature via a two-step reaction path, where PtCl42- serves as an intermediate. The use of the short-time-impregnated 40 wt% Pt/C as cathode electrocatalysts in direct methanol fuel cells yields better performance than that of commercial 40 wt% Pt/C electrocatalyst. Experimental evidence provides clues for the fundamental understanding of elementary steps of the redox reactions, which helps in guiding the design and preparation of highly dispersed Pt catalyst for fuel cells.

Preparation and characterization of multiwalled carbon nanotube-supported platinum for cathode catalysts of direct methanol fuel cells

Multiwalled carbon nanotube-supported Pt (Pt/MWNT) nanocomposites were prepared by both the aqueous solution reduction of a Pt salt (HCHO reduction) and the reduction of a Pt ion salt in ethylene glycol solution. For comparison, a Pt/XC-72 nanocomposite was also prepared by the EG method. The Pt/MWNT catalyst prepared by the EG method has a high and homogeneous dispersion of spherical Pt metal particles with a narrow particle-size distribution. TEM images show that the Pt particle size is in the range of 2-5 nm with a peak at 2.6 nm, which is consistent with 2.5 nm obtained from the XRD broadening calculation. Surface chemical modifications of MWNTs and water content in EG solvent are found to be the key factors in depositing Pt particles on MWNTs. In the case of the direct methanol fuel cell (DMFC) test, the Pt/MWNT catalyst prepared by EG reduction is slightly superior to the catalyst prepared by aqueous reduction and displays significantly higher performance than the Pt/XC-72 catalyst. These differences in catalytic performance between the MWNT-supported or the carbon black XC-72-supported catalysts are attributed to a greater dispersion of the supported Pt particles when the EG method is used, in contrast to aqueous HCHO reduction and to possible unique structural and higher electrical properties when contrasting MWNTs to carbon black XC-72 as a support.

Preparation of uniform calcium alginate gel beads by membrane emulsification coupled with internal gelation

With the objective of making calcium alginate gel beads with small and uniform size, membrane emulsification coupled with internal gelation was proposed. Spherical gel beads with mean size of about 50 mum, and even smaller ones in water, and with narrow size distribution were successfully obtained. Experimental studies focusing mainly on the effect of process parameters on bead properties were performed. The size of the beads was mainly dependent on the diameter of the membrane pores. High transmembrane pressure made for large gel beads with wide size distribution. Low sodium alginate concentration produced nonspherical beads, whereas a high concentration was unsuitable for the production of small beads with narrow distribution. Thus 1.5% w/v was enough. A high surfactant concentration favored the formation of small beads, but the adverse effect on mass transfer should be considered in this novel process. (C) 2002 Wiley Periodicals, Inc.