On-line introduction of high-pressure gas-liquid sample for capillary gas chromatographic analysis

An on-line sample introduction technique in capillary gas chromatograph (CGC) for the analysis of high-pressure gas-liquid mixtures has been designed and evaluated. A sample loop of 0.05 muL and a washing solvent loop of 0.5 muL are mounted on a 10-port switching valve, which serves as the injection valve. A capillary resistor was connected to the vent of sample loop in order to maintain the pressure of the sample. Both the sample and the washing solvent are transferred into the split-injection port through a narrow bore fused silica capillary inserted into the injection liner through a septum. The volume of the liner is used both as the pressure-release damper and evaporation chamber of the sample. On-line analysis of both reactants and resultants in ethylene olimer reaction mixture at 5 MPa was carried out, which demonstrated the applicability of the technique. (C) 2004 Elsevier B.V. All rights reserved.

Reduction of NO by CH4 with microwave heating

The reduction of NO by CH4 in the presence of excess O-2 over Co/HZSM-5, Ni/HZSM-5 and Mn/HZSM-5 catalysts with microwave heating was studied. By comparing the activities of the catalysts in the microwave heating mode with that in the conventional reaction mode, it was demonstrated that microwave heating could greatly reduce the reaction temperature, and could clearly expand the temperature window of the catalysts. Especially for the Co/HZSM-5 catalyst, the maximum conversion of NO to N-2 in the conventional reaction mode was consistent with that in the microwave heating mode. However, the temperature window for the maximum conversion in the microwave heating mode was from 260 to 360degreesC instead of a temperature of 420degreesC in the conventional reaction mode. The results suggest that microwave heating has a novel effect in the reduction of NO.

The shape parameter of Liposomes and DNA-lipid complexes determined by viscometry utilizing small sample volumes

A minicapillary viscometer utilizing <0.5 ml of sample at a volume fraction of <0.1% is described. The calculated a/b of DPPC/DPPG multilamellar liposome was 1.14 as prolate ellipsoids and a/b of dioleoylpropyltrimethyl ammonium methylsulfate-DNA complex at a charge ratio of 4: 1 (+/-) was 3.7 as prolate ellipsoids or 4.9 as oblate ellipsoids. The deviation of shape from perfect sphere is thus expressed quantitatively in more than two significant figures. In these measurement, the necessary amount of DNA is <0.5 mg.

Quantitative sample injection for capillary electrophoresis

An apparatus including a rotary-type injector was designed for quantitative sample injection in capillary electrophoresis (CE), in which both pressurized flow and electroosmotic flow were used to drive the background electrolyte solution. A relative standard deviation of peak area of lower than 1% was achieved by using this apparatus. The effects of back-pressure regulator, restrictor, and applied voltage on separation efficiency and resolution were investigated. The utility of this apparatus in both micro-HPLC and pressurized capillary electrochromatography (pCEC) was also demonstrated.

Direct decomposition of NO by microwave heating over Fe/NaZSM-5

Catalytic decomposition of NO was studied over Fe/NaZSM-5 catalyst. Novel results were observed with the microwave heating mode. The conversion of NO to N-2 increased remarkably with the increasing of Fe loading. The effects of a series of reaction parameters, including reaction temperature, O-2 concentration, NO concentration, gas flow rate and H2O addition, on the productivity of N-2 have been investigated. It is shown that the catalyst exhibited good endurance to excess O-2 in the microwave heating mode. Under all reaction conditions, NO converted predominantly to N-2. The highest conversion of NO to N-2 was up to 70%. (C) 2002 Elsevier Science B.V. All rights reserved.

Morphological transition of dry vesicles into onion-like multilamellar micelles induced through heating at high temperature

In this Letter, we report the morphological transition of dry block copolymer vesicles into onion-like multilamellar micelles induced through heating. When the temperature is higher than the glass transition temperature of block copolymer, the vesicles can collapse, and finally form onion-like multilamellarmicelles via micro phase separation. This phenomenon is observed in both A-B and A-B-A block copolymer vesicles, indicating that the technique used in this study can be an alternative method to synthesize multilamellar micelles.

Single-walled carbon nanohorn as new solid-phase extraction adsorbent for determination of 4-nitrophenol in water sample

Single-walled carbon nanohorn (SWCNH) was developed as new adsorbent for solid-phase extraction using 4-nitrophenol as representative. The unique exoteric structures and high surface area of SWCNH allow extracting a large amount of 4-nitrophenol over a short time. Highly sensitive determination of 4-nitrophenol was achieved by linear sweep voltammetry after only 120 s extraction. The calibration plot for 4-nitrophenol determination is linear in the range of 5.0 x 10(-8) M-1.0 x 10(-5) M under optimum conditions. The detection limit is 1.1 x 10(-8) M. The proposed method was successfully employed to determine 4-nitrophenol in lake water samples, and the recoveries of the spiked 4-nitrophenol were excellent (92-106%).

Effect of the gamma-form crystal on the thermal fractionation of poly(propylene-co-ethylene)

The effect of the gamma-form crystal on the thermal fractionation of a commercial poly(propylene-co-ethylene) (PPE) has been studied by differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD) techniques. Two thermal fractionation techniques, stepwise isothermal crystallization (SIC) and successive self-nucleation and annealing (SSA), have been used to characterize the molecular heterogeneity of the PPE. The results indicate that the SSA technique possesses a stronger fractionation ability than that of the SIC technique. The heating scan of the SSA fractionated sample exhibits 12 endothermic peaks, whereas the scan of the SIC fractionated sample only shows eight melting peaks. The WAXD observations of the fractionated PPE samples prove that the content of the gamma-form crystals formed during the thermal treatment of the SIC technique is much higher than that of the SSA treatment. The former is 57.4%, whereas the later is 12.6%. The effect of they-form crystals on thermal fractionation ability is discussed.

One-step preparation and characterization of poly(propyleneimine) dendrimer-protected silver nanoclusters

Highly stable silver nanoclusters with narrow size distribution have been prepared by heating a third-generation poly(propyleneimine) dendrimer/AgNO3 aqueous solution without the additional step of introducing other reducing agents and protect agents. UV-vis absorption, transmission electron microscopy (TEM), X-ray photoelectron spectra (XPS), and X-ray diffraction (XRD) have been used to characterize the resulting products. The as-obtained sample was in coexistence of Ag and Ag2O. It also suggested that increasing temperature resulted in both the decrease in number of small particles and the increase in size of large particles.

Field-amplified sample stacking capillary electrophoresis with electrochemiluminescence applied to the determination of illicit drugs on banknotes

Capillary electrophoresis (CE) with Ru(bpy)(3)(2+) electrochemiluminescence. (ECL) detection system was established to the determination of contamination of banknotes with controlled drugs and a high efficiency on-column field-amplified sample stacking (FASS) technique was also optimized to increase the ECL intensity. The method was illustrated using heroin and cocaine, which are two typical and popular illicit drugs. Highest sample stacking was obtained when 0.01 mM acetic acid was chosen for sample dissolution with electrokinetical injection for 6 s at 17 kV. Under the optimized conditions: ECL detection at 1.2 V, separation voltage 10.0 kV, 20 mM phosphate-acetate (pH 7.2) as running buffer, 5 mM Ru(bpy)(3)(2+) with 50 mM phosphate-acetate (pH 7.2) in the detection cell, the standard curves were linear in the range of 7.50 x 10(-8) to 1.00 x 10(-5) M for heroin and 2.50 x 10(-7) to 1.00 x 10(-4) M for cocaine and detection limits of 50 nM for heroin and 60 nM for cocaine were achieved (S/N = 3), respectively. Relative standard derivations of the ECL intensity and the migration time were 3.50 and 0.51% for heroin and 4.44 and 0.12% for cocaine, respectively.The developed method was successfully applied to the determination of heroin and cocaine on illicit drug contaminated banknotes without any damage of the paper currency.

Determination of Nb and Ta in Nb/Ta minerals by inductively coupled plasmas optical emission spectrometry using slurry sample introduction

The determination of Nb and Ta in Nb-Ta minerals was accomplished by slurry nebulization inductively coupled plasma optical emission spectrometry (ICP-OES), using a clog-free V-groove ceramic nebulizer. Samples were first wet-ground to appropriate particle sizes with narrow size distribution and 90% of the particles in the slurry were smaller than 2.32 mu m in diameter. Subsamples were then dispersed in pH 9 aqueous solutions, and agitated in an ultrasonic bath for 15 min prior to analysis. Due to the lack of slurry standards matching well with the samples, calibration was simply carried out using aqueous solution standards. Results were compared with those obtained from a conventional fusion decomposition procedure and acid digestion procedures and a good agreement between the measured and referred values was obtained. The technique provided a good alternative for the rapid determination of Nb and/or Ta in their corresponding minerals.

Multiple melting behavior of isotactic polypropylene and poly(propylene-co-ethylene) after stepwise isothermal crystallization

The multiple melting behavior of several commercial resins of isotactic polypropylene (iPP) and random copolymer, poly(propylene-co-ethylene) (PPE), after stepwise isothermal crystallization (SIC) were studied by differential scanning calorimeter and wide-angle X-ray diffraction (WAXD). For iPP samples, three typical melting endotherms appeared after SIC process when heating rate was lower than 10 degreesC/min. The WAXD experiments proved that only alpha-form crystal was formed during SIC process and no transition from alpha1- to alpha2-form occurred during heating process. Heating rate dependence for each endotherm was discussed and it was concluded that there were only,two major crystals with different thermal stability. For the PPE sample, more melting endotherms appeared after stepwise isothermal crystallization. The introduction of ethylene comonomer in isotactic propylene backbone further decreased the regularity of molecular chain, and the short isotactic propylene sequences could crystallize into gamma-form crystal having a low melting temperature whereas the long sequences crystallized into alpha-form crystal having high melting temperature.

Electrochemiluminescent microoptoprobe with mini-grid working electrode and self-contained sample container

A new electrochemiluminescence (ECL) microoptoprobe with simple structure. small sampling volume and high efficiency was developed. It was constructed by fixing the transparent gold mini-grid on the end surface of the optical fiber, and by surrounding the fiber with the counter- and reference electrodes to form a self-contained three-electrode system. The use of mini-grid electrode increased the surface area and collection efficiency. which resulted in higher ECL signal and better sensitivity. The counter electrode together with one end of the fiber formed a mini-vessel, which eliminated the need of additional container and allowed to perform ECL detection in a very small volume (about 10 mul). The microoptoprobe obtained was characterized with the Ru(bpy)(3)(2-)-tripropylamine system and was applied for the determination of oxalate and chlorpromazine (CPZ). Detection limits (S/N = 3) were 5 x 10(-7) and 1 x 10(-6) mol l(-1) for oxalate and CPZ. respectively. The linear range for oxalate and CPZ extended from 1 x 10(-6) to 1 x 10(-3) mol l(-1), and from 5 x 10(-6) to 5 x 10(-4) mol l(-1). respectively.

Crystal form transition during heating of solvent-induced crystalline syndiotactic polystyrene

The phase transition of two kinds of solvent-induced crystalline syndiotactic polystyrene (sPS). gamma-sPS and delta(c)-sPS, has been studied via WAXD and DSC. gamma-sPS transform to a-sPS at 195-225 degrees C before melt during heating, whereas delta(e)-sPS transform to first gamma-sPS and then a-sPS at 100-200 degrees C and 200-215 degrees C, respectively. The transition of delta(e)-gamma and gamma-a occurs for below melting point of sPS indicates they are all solid-solid transition.