SPECTROPHOTOMETRIC DETERMINATION OF LANTHANUM AND SUM OF OTHER LIGHT RARE-EARTHS BY FLEXIBLE TOLERANCE SIMPLEX-METHOD

The absorptivities of color elements in a mixture can be obtained by using Gauas' elimination with selection of principal element in matrix to the standards. These values can be applied to flexible tolerance simplex method to give the composition of samples. In the exprimental design and data treatment, an effort was made to minimize the errors of results according the principal of optimization. When the difference of absorptivities of color material is significant to the exprimental error, the pr...

Improvement of different source function expressions in SWAN model for the Bohai Sea

The simulating wave nearshore (SWAN) wave model has been widely used in coastal areas, lakes and estuaries. However, we found a poor agreement between modeling results and measurements in analyzing the chosen four typical cases when we used the default parameters of the source function formulas of the SWAN to make wave simulation for the Bohai Sea. Also, it was found that at the same wind process the simulated results of two wind generation expressions (Komen, Janssen) demonstrated a large difference. Further study showed that the proportionality coefficient alpha in linear growth term of wave growth source function plays an unperceived role in the process of wave development. Based on experiments and analysis, we thought that the coefficient alpha should change rather than be a constant. Therefore, the coefficient alpha changing with the variation of friction velocity U (*) was introduced into the linear growth term of wave growth source function. Four weather processes were adopted to validate the improvement in the linear growth term. The results from the improved coefficient alpha agree much better with the measurements than those from the default constant coefficient alpha. Furthermore, the large differences of results between Komen wind generation expression and Janssen wind generation expression were eliminated. We also experimented with the four weather processes to test the new white-capping mechanisms based on the cumulative steepness method. It was found that the parameters of the new white-capping mechanisms are not suitable for the Bohai Sea, but Alkyon's white-capping mechanisms can be applicable to the Bohai Sea after amendments, demonstrating that this improvement of parameter alpha can improve the simulated results of the Bohai Sea.

Fast analysis of capillary electrochromatography with non-porous ODS as the stationary phase

High-speed capillary electrochromatography was developed on both short and long packed columns with 2 mu m non-porous ODS as the stationary phase. Factors that affect the analysis time of samples, such as voltage, electrolyte concentration, pH and organic modifier concentration in the mobile phase, were studied systematically. Fast analysis of aromatic compounds within 13 seconds was realized with column efficiency of 573,000 plates/m and a R.S.D.% of the retention times of all components in 8 consecutive injections below 1.0%. which demonstrated the high efficiency and high reproducibility of such a technique. In addition, DNPH derived aldehydes and ketones in both standards and environmental samples were separated with high speed.

Separation of neutral compounds by high speed capillary electrochromatography

With using short capillary column packed with porous and non-porous ODS stationary phases, high speed separation of 6 neutral aromatic compounds within 36 s by capillary electrochromatography (CEC) has been performed. Good reproducibility of the migration times for those solutes in high speed CEC was observed with RSD less than 1%. Both the linear velocity of EOF and the current linearly increases with the applied voltage, which means that the thermal effect by Joule heating was small. However, the capacity factor of solutes was found to decrease with the increase of the applied voltage, which was caused by the fact that about several seconds needed for the increase of voltage from 0 to applied value on a commercial CE instrument made larger contributions to the migration times of the early eluted compounds than those of lately eluted ones during high speed CEC, and voltage effect would increase with the higher applied voltage used. The linear relationship between the logarithm of capacity factor and the number of carbon for homologous compounds was observed, and positive value of slope means that the hydrophobicity of solutes is one of the main contribution factors to retention in high speed CEC packed with ODS stationary phases.

Column switching-back flushing technique for the analysis of aromatic compounds in gasoline

A simple method, based on the technique of capillary column switching-back flushing, has been developed for the detailed analysis of aromatic compounds in gasoline. The sample was first separated on a 30-m long OV-2330 polar precolumn and then backflushed onto a nonpolar analytical column. The early eluting components from the precolumn and the components of interest (aromatic compounds plus heavier compounds) eluting from the analytical column are all directed to the same flame ionization detection system through a T piece, which permits the quantitative analysis of aromatic hydrocarbons in gasoline by a normalization method using correcting factors. The switching time window of the method is +/-5 s, resulting in easier operation and higher reliability. The reproducibility of the quantitative analysis was less than or equal to3% RSD for real gasoline samples. (C) 2002 Elsevier Science B.V. All rights reserved.

On-line concentration of peptides and proteins with the hyphenation of polymer monolithic immobilized metal affinity chromatography and capillary electrophoresis

An iminodiacetic acid (IDA)-type adsorbent is prepared at the one end of a capillary by covalently bonding IDA to the monolithic rods of macroporous poly(glycidyl methacrylate-co-ethylene dimethacrylate). Cu(II) is later introduced to the support via the interaction with IDA. By this means, polymer monolithic immobilized metal affinity chromatography (IMAC) materials are prepared. With such a column, IMAC for on-line concentration and capillary electrophoresis (CE) for the subsequent analysis are hyphenated for the analysis of peptides and proteins. The reproducibility of such a column has been proved good with relative standard deviations (RSDs) of dead time of less than 5% for injection-to-injection and 12% for column-to-column (n = 3). Through application on the analysis of standard peptides and real protein samples, such a technique has shown promising in proteome study.

Using oxidized carbon nanotubes as matrix for analysis of small molecules by MALDI-TOF MS

Oxidized carbon nanotubes are tested as a matrix for analysis of small molecules by matrix assisted laser desorption/ionization time of flight mass spectrometry (MALDI-TOF-MS). Compared with nonoxidized carbon nanotubes, oxidized carbon nanotubes facilitate sample preparation because of their higher solubility in water. The matrix layer of oxidized carbon nanotubes is much more homogeneous and compact than that of nonoxidized carbon nanotubes. The efficiency of desorption/ionization for analytes and the reproducibility of peak intensities within and between sample spots are greatly enhanced on the surface of oxidized carbon nanotubes. The advantage of the oxidized carbon nanotubes in comparison with alpha-cyano-4-hydroxycinnamic acid (CCA) and carbon nanotubes is demonstrated by MALDI-TOF-MS analysis of an amino acid mixture. The matrix is successfully used for analysis of synthetic hydroxypropyl P-cyclodextrin, suggesting a great potential for monitoring reactions and for product quality control. Reliable quantitative analysis of jatrorrhizine and palmatine with a wide linear range (1-100 ng/mL) and good reproducibility of relative peak areas (RSD less than 10 %) is achieved using this matrix. Concentrations of jatrorrhizine (8.65 mg/mL) and palmatine (10.4 mg/mL) in an extract of Coptis chinensis Franch are determined simultaneously using the matrix and a standard addition method. (c) 2005 American Society for Mass Spectrometry.