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.

2-(2-Phenyl-1H-phenanthro-[9,10-d]imidazole-1-yl)-acetic acid (PPIA) and its application for determination of amines by high performance liquid chromatography with fluorescence detection and identification with mass spectroscopy/atmospheric pressure chemical ionization

A simple, sensitive, and mild method for the determination of amino compounds based on a condensation reaction with 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (EDC-HCI) as the dehydrant with fluorescence detection has been developed. Amines were derivatized to their acidamides with labeling reagent 2-(2-phenyl-1H-phenanthro-[9,10-d]imidazole-1-yl)-acetic acid (PPIA). Studies on derivatization conditions indicated that the coupling reaction proceeded rapidly and smoothly in the presence of a base catalyst in acetonitrile to give the corresponding sensitively fluorescent derivatives with an excitation maximum at lambda(ex) 260nm and an emission maximum at lambda(em) 380nm. The labeled derivatives exhibited high stability and were enough to be efficiently analyzed by high-performance liquid chromatography. Identification of derivatives was carried out by online post-column mass spectrometry (LC/APCI-MS/MS) and showed an intense protonated molecular ion corresponding m/z [MH](+) under APCI in positive-ion mode. At the same time, the fluorescence properties of derivatives in various solvents or at different temperature were investigated. The method, in conjunction with a gradient elution, offered a baseline resolution of the common amine derivatives on a reversed-phase Eclipse XDB-C-8 column. LC separation for the derivatized amines showed good reproducibility with acetonitrile-water as mobile phase. Detection limits calculated from 0.78 pmol injection, at a signal-to-noise ratio of 3, were 3.1-18.2 fmol. The mean intra- and inter-assay precision for all amine levels were < 3.85% and 2.11%, respectively. Excellent linear responses were observed with coefficients of > 0.9996. The established method for the determination of aliphatic amines from real wastewater and biological samples was satisfactory. (c) 2006 Elsevier B.V. All rights reserved.

Flow Characteristics of Liquids in Microtubes Driven by a High Pressure

The flow characteristics of liquids in microtubes driven by a high pressure ranging from 1 MPa to 30 MPa are studied in this paper. The diameter of the microtube is from 3 μm to 10 μm and liquids composed of simple small molecules are chosen as the working fluids. The Reynolds number ranges from 0. 1 to 24. The behavior of isopropanol and carbon tetrachloride under high pressure is found different from the prediction from conventional Hagen-Poiseuille (HP) equation. The normalized friction coefficient C* increases significantly with the pressure. From an analysis of the microtube deformation, liquid compressibility, viscous heating and wall slip, it may be seen that the viscosity at high pressure plays an important role here. An exponential function of viscosity vs pressure is introduced into the HP equation to counteract the difference between experimental and theoretical values. However, this difference is not so marked for di-water.

Preliminary study on the photoproduction of hydroxyl radicals in aqueous solution with Aldrich humic acid, algae and Fe(III) under high-pressure mercury lamp irradiation

Under a high-pressure mercury lamp (HPML) and using an exposure time of 4 h, the photoproduction of hydroxyl radicals ((OH)-O-.) could be induced in an aqueous solution containing humic acid (HA). Hydroxyl radicals were determined by high-performance liquid chromatography using benzene as a probe. The results showed that (OH)-O-. photoproduction increased from 1.80 to 2.74 muM by increasing the HA concentration from 10 to 40 mg L-1 at an exposure time of 4 h (pH 6.5). Hydroxyl radical photoproduction in aqueous solutions of HA containing algae was greater than that in the aqueous solutions of HA without algae. The photoproduction of (OH)-O-. in the HA solution with Fe(111) was greater than that of the solution without Fe(III) at pH ranging from 4.0 to 8.0. The photoproduction of (OH)-O-. in HA solution with algae with or without Fe(111) under a 250 W HPML was greater than that under a 125 W HPML. The photoproduction of (OH)-O-. in irradiated samples was influenced by the pH. The results showed that HPML exposure for 4 h in the 4-8 pH range led to the highest (OH)-O-. photoproduction at pH 4.0.

Influence of processing temperature on microstructure and microhardness of copper subjected to high-pressure torsion

Cu samples were subjected to high-pressure torsion (HPT) with up to 6 turns at room temperature (RT) and liquid nitrogen temperature (LNT), respectively. The effects of temperature on grain refinement and microhardness variation were investigated. For the samples after HPT processing at RT, the grain size reduced from 43 mu m to 265 nm, and the Vickers microhardness increased from HV52 to HV140. However, for the samples after HPT processing at LNT, the value of microhardness reached its maximum of HV150 near the center of the sample and it decreased to HV80 at the periphery region. Microstructure observations revealed that HPT straining at LNT induced lamellar structures with thickness less than 100 nm appearing near the central region of the sample, but further deformation induced an inhomogeneous distribution of grain sizes, with submicrometer-sized grains embedded inside micrometer-sized grains. The submicrometer-sized grains with high dislocation density indicated their nonequilibrium nature. On the contrary, the micrometer-sized grains were nearly free of dislocation, without obvious deformation trace remaining in them. These images demonstrated that the appearance of micrometer-sized grains is the result of abnormal grain growth of the deformed fine grains.

Evaluation of the Cumulative Formation of High-Speed Liquid Jets

This paper describes the generation of pulsed, high-speed liquid jets using the cumulation method. This work mainly includes (1) the design of the nozzle assembly, (2) the measurement of the jet velocity and (3) flow visualization of the injection sequences. The cumulation method can be briefly described as the liquid being accelerated first by the impact of a moving projectile and then further after it enters a converging section. The experimental results show that the cumulation method is useful in obtaining a liquid jet with high velocity. The flow visualization shows the roles of the Rayleigh-Taylor and Kelvin-Helmholtz instabilities in the breakup of the liquid depend on the jet diameter and the downstream distance. When the liquid jet front is far downstream from the nozzle exit, the jet is decelerated by air drag. Meanwhile, large coherent vortex structures are formed surrounding the jet. The liquid will break up totally by the action of these vortices. Experimental results showing the effect of the liquid volume on the jet velocity are also included in this paper. Finally, a method for measuring the jet velocity by cutting two carbon rods is examined.

Melting and Crystallization of Nd60Al10Fe20Co10 Bulk Metallic Glass under High Pressure

Crystallization, melting and structural evolution upon crystallization in Nd60Al10Fe20Co10 bulk metallic glass (BMG) are in situ investigated by x-ray diffraction with synchrotron radiation under high pressure. It is found that the crystallization is pressure promoted, while themelting is inhibited. The crystallization and melting process are also changed under high pressure. The features of the crystallization and melting under high pressure are discussed.

Performance of a small high-speed liquid jet apparatus

The performance of a small high-speed liquid jet apparatus is described. Water jets of 200m/s to 700m/s have been obtained by firing a deformable lead slug from an air rifle into a stainless steel nozzle containing water sealed with a rubber diaphragm. Nozzle devices of using the impact extrusion (IE) method and cumulation (CU) method are designed to generate jets. The injection sequences are visualized using schlieren photography. The difference between the IE and CU methods in the jet generation is found.

Microstructure and mechanical properties of copper subjected to high pressure torsion

Experiments were conducted on copper subjected to High Pressure Torsion to investigate the evolution of microstructure and microhardness with shear strain, gamma. Observations have been carried out in the longitudinal section for a proper demonstration of the structure morphology. An elongated dislocation cell/subgrain structure was observed at relatively low strain level. With increasing strain, the elongated subgrains transformed into elongated grains and finally into equiaxed grains with high angle grain boundaries. Measurements showed the hardness increases with increasing gamma then tends to saturations when gamma >5. The variation tendency of microhardness with gamma can be simulated by Voce-type equation.

Microscopic Model Of Nano-Scale Particles Removal In High Pressure Co2-Based Solvents

A physical model is presented to describe the kinds of static forces responsible for adhesion of nano-scale copper metal particles to silicon surface with a fluid layer. To demonstrate the extent of particle cleaning, Received in revised form equilibrium separation distance (ESD) and net adhesion force (NAF) of a regulated metal particle with different radii (10-300 nm) on the silicon surface in CO2-based cleaning systems under different pressures were simulated. Generally, increasing the pressure of the cleaning system decreased the net adhesion force between spherical copper particle and silicon surface entrapped with medium. For CO2 + isopropanol cleaning system, the equilibrium separation distance exhibited a maximum at temperature 313.15 K in the Equilibrium separation distance regions of pressure space (1.84-8.02 MPa). When the dimension of copper particle was given, for example, High pressure 50 nm radius particles, the net adhesion force decreased and equilibrium separation distance increased with increased pressure in the CO2 + H2O cleaning system at temperature 348.15 K under 2.50-12.67 MPa pressure range. However, the net adhesion force and equilibrium separation distance both decreased with an increase in surfactant concentration at given pressure (27.6 or 27.5 MPa) and temperature (318 or 298 K) for CO2 + H2O with surfactant PFPE COO-NH4+ or DiF(8)-PO4-Na+. (C) 2008 Elsevier B.V. All rights reserved.

Numerical Study On Transient Flow In The Deep Naturally Fractured Reservoir With High Pressure

According to the experimental results and the characteristics of the pressure-sensitive fractured formation, a transient flow model is developed for the deep naturally-fractured reservoirs with different outer boundary conditions. The finite element equations for the model are derived. After generating the unstructured grids in the solution regions, the finite element method is used to calculate the pressure type curves for the pressure-sensitive fractured reservoir with different outer boundaries, such as the infinite boundary, circle boundary and combined linear boundaries, and the characteristics of the type curves are comparatively analyzed. The effects on the pressure curves caused by pressure sensitivity module and the effective radius combined parameter are determined, and the method for calculating the pressure-sensitive reservoir parameters is introduced. By analyzing the real field case in the high temperature and pressure reservoir, the perfect results show that the transient flow model for the pressure-sensitive fractured reservoir in this paper is correct.