Analysis of aromatic amines by high-performance liquid chromatography with pre-column derivatization by 2-(9-carbazole)-ethyl-chloroformate

2-(9-Carbazole)-ethyl-chloroformate (CEOC), a novel pre-column fluorescence derivatization reagent, has been developed for the analysis of aromatic amines. Taking five monocyclic aromatic amines (o-toluidine, aniline, 3,4-dimethylaniline, N-ethyl-p-toluidine, and p-phenylenediamine) as testing compounds, derivatization conditions such as pH of borate buffer, reaction time and fluorescent tagging reagent concentration have been investigated. By a one-step procedure, CEOC reacts readily with the aromatic amines to form stable derivatives with excitation and emission wavelengths, respectively, at 293 and 360 nm. This derivatization reaction could be finished within 20 min even at room temperature. The peak shapes of the derivatized aromatic amines can be improved greatly without any addition of competition amines into the mobile phase. Furthermore, this method can offer excellent quantitative precision with high tolerance of the matrix of samples. (C) 2003 Elsevier B.V. All rights reserved.

Characterization of structure and diffusion behaviour of Ca-alginate beads prepared with external or internal calcium sources

Ca-alginate beads were prepared with either external or internal calcium sources. The structures of both beads were investigated with the aid of scanning electron microscopy (SEM) and confocal microscopy. It was shown that the beads with internal calcium source had a looser structure and bigger pore size than those with external calcium source. The attempts to interpret the difference were carried out by determining the Ca content within the beads at various times, which indicated that it was the different gelation mechanisms that caused the difference of structures of both beads. Furthermore, it was also found that the diffusion rate of haemoglobin (Hb) within the beads with an internal calcium source was faster than that of the beads with an external one, which was consistent with the observation of their structures.

Ordered FePt Nanoparticle Arrays Prepared by a Micellar Method

City Univ Hong Kong

Hollow fibers of yttria-stabilized zirconia (8YSZ) prepared by calcination of electrospun composite fibers

8YSZ fibers were synthesized by calcination of PVP/zirconium oxychloride/yttrium nitrate composite fibers (PVP-Precursor) obtained by electrospinning. Scanning electron microscopy (SEM) indicated that the 8YSZ fibers are hollow and the gas released during organic binder decomposition resulted in the formation of hollow center in fibers

Upconversion luminescence of Y2O3 : Er3+, Yb3+ nanoparticles prepared by a homogeneous precipitation method

Y2O3: Er3+, Yb3+ nanoparticles were synthesized by a homogeneous precipitation method without and with different concentrations of EDTA 2Na. Upconversion luminescence spectra of the samples were studied under 980 nm laser excitation. The results of XRD showed that the obtained Y2O3:Er3+,Yb3+ nanoparticles were of a cubic structure. The average crystallite sizes calculated were in the range of 28-40 nm. Green and red upconversion emission were observed, and attributed to H-2(11/2), S-4(3/2) -> I-4(15/2) and F-4(9/2) -> I-4(15/2) transitions of the Er3+ ion, respectively.

Grafting acrylic acid onto polypropylene by reactive extrusion with pre-irradiated PP as initiator

In this paper, the modification of polypropylene (PP) with acrylic acid (AA) by reactive extrusion using pre-irradiated PP (rPP) as initiator was investigated. It was found the relatively high graft degree (Gd) and slight degradation of modified PP was obtained when 20 wt% rPP was used. This result can be explained in terms of effective concentration of free radicals.

Quality analysis of herbal medicine products prepared from Herba sarcandrae by capillary electrophoresis with electrochemical detection

A capillary electrophoresis with electrochemical detection(CE-ED) method was developed for the quality analysis of herbal medicine products prepared from the same herb of Herba Sarcandrae: Fufang Caoshanhu tablets, Qingrexiaoyanning capsules, and Xuekang oral liquids. Under the optimal analysis conditions, the low detection limit[1.0x10(-7) mol/L(S/N=3)] and the wide linear range(1.0x10(-7)-1.0x10(-4) mol/L) were obtained for quality standard compound of isofraxidin. The precisions of the peak current and the migration time(as RSDs) for the real sample analysis were 2.0%-2.6%, and 1.2%-1.8% for isofraxidin, respectively.

Polyamide thin film composite membranes prepared from isomeric biphenyl tetraacyl chloride and m-phenylenediamine

Three novel of isomeric tetra-functional biphenyl acid chloride: 3,3',5,5'-biphenyl tetraacyl chloride (mm-BTEC), 2,2',4,4'-biphenyl tetraacyl chloride (om-BTEC), and 2,2',5,5'-biphenyl tetraacyl chloride (op-BTEC) were synthesized, and used as new monomers for the preparation of the thin film composite (TFC) reverse osmosis (RO) membranes through interfacial polymerization with m-phenylenediamine (MPDA). The results of membrane performance test showed that membranes prepared from om-BTEC and op-BTEC had higher flux at the expanse of rejection compared with membranes prepared from mm-BTEC.

Fabrication, thermal stability and mechanical properties of novel (W0.5Al0.5)C-0.8-Co composite prepared by mechanical alloying and hot-pressing sintering

A novel cemented carbides (W0.5Al0.5)C-0.8-Co with different cobalt contents were prepared by mechanical alloying and hot-pressing technique. Hot-pressing technique as a common technique was performed to fabricate the bulk bodies of the hard alloys. The novel cemented carbides have superior mechanical properties compared to WC-Co. The density, operating cost of the novel material were much lower than WC-Co. There is almost no eta-phase in the (W0.5Al0.5)C-0.8-Co cemented carbides system although the carbon deficient get the value of 20%, and successfully got the nanostructured rounded (W0.5Al0.5)C-0.8 particles.

A novel (W-Al)-C-Co composite cemented carbide prepared by mechanical alloying and hot-pressing sintering

Novel cemented carbides (W0.4Al0.6)C-0.5-Co With different cobalt contents were prepared by mechanical alloying and hot-pressing technique. Hot-pressing technique as a common technique was performed to fabricate the bulk bodies of the hard alloys. The novel cemented carbides have good mechanical properties compared with WC-Co. The density and operation cost of the novel material were much lower than the WC-Co system. It was easy to process submicroscale sintering with the novel materials and obtain the rounded particles in the bulk materials. There is almost no eta-phase in the (W0.4Al0.6)C-0.5-CO cemented carbides system although the carbon deficient obtains the astonishing value of 50%.

Bulk ultrafine binderless (W0.4Al0.6)C prepared by high pressure sintering

Pure (W0.4Al0.6)C powder of about 1 mu m in diameter was sintered by the high pressure sintering (HPS) process without the addition of any binder phase. The microstructure, Vickers micro hardness and density versus the sintering time and temperature are well described. The most suitable sintering condition under pressure of 4.5 GPa is 1873 K for 8 min. Under this sintering condition, the hardness can reach 2295 kg mm(-2) and the relative density can reach 98.6%.

Bluish-white emission from radical carbonyl impurities in amorphous Al2O3 prepared via the Pechini-type sol-gel process

Many efforts have been devoted to exploring novel luminescent materials that do not contain expensive or toxic elements, or do not need mercury vapor plasma as the excitation source. In this paper, amorphous Al2O3 powder samples were prepared via the Pechini-type sol-gel process. The resulting samples were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, field emission scanning electron microscopy (FESEM), photoluminescence (PL) excitation and emission spectra, kinetic decay, and electron paramagnetic resonance (EPR).