Discrete salt crystallization at the surface of a porous medium

Efflorescence refers to crystallized salt structures that form at the surface of a porous medium. The challenge is to understand why these structures do not form everywhere at the surface of the porous medium but at some specific locations and why there exists an exclusion distance around an efflorescence where no new efflorescence forms. These are explained from a visualization experiment, pore-network simulations and a simple efflorescence growth model.     

On a weak sum theorem in dimension theory

A metric spaceX = U _i-0 ^x X is constructed such thatX _o={x _o} consists of a single pointx _o , X _i , i=0, 1, 2, … are disjoint and closed,X _i , i=1, 2, … are open, indX _i =0 fori=0, 1, … and indX=1. The above space (proved to be, in some sense, most simple) shows also that the dimension ind of a metric space can be raised by adjoining of a single point, a fact proved recently by E.K. Van Douwen and by T. Przymusiński. Some maximality property of the family {X; IndX=0} is proved and conditions implyingP-ind=P-Ind are given. This is part of a research thesis at the Technion, Israel Institute of Technology, towards an M.Sc. degree, directed by Professor M. Reichaw.     

Solid-phase microextraction coupled to liquid chromatography for the analysis of phenolic compounds in water

Solid-phase microextraction (SPME) coupled to high-performance liquid chromatography (HPLC) has been applied to the analysis of priority pollutant phenolic compounds in water samples. Two types of polar fibers [50 microm Carbowax-templated resin (CW-TPR) and 60 microm polydimethylsiloxane-divinylbenzene (PDMS-DVB)] were evaluated. The effects of equilibration time and ionic strength of samples on the adsorption step were studied. The parameters affecting the desorption process, such as desorption mode, solvent composition and desorption time, were optimized. The developed method was used to determine the phenols in spiked river water samples collected in the Douro River, Portugal. Detection limits of 1-10 microg l(-1) were achieved under the optimized conditions.     

Determination of quinolones in water samples by solid-phase extraction and liquid chromatography with fluorimetric detection

A method is reported for the determination, in water samples, of 10 quinolones which are used as veterinary drugs. Analytes are isolated from samples by solid-phase extraction (SPE) and analysed by reversed-phase high-performance liquid chromatography using fluorimetric detection. A solid-phase extraction procedure based on retention on HBL OASIS cartridges and elution with a mixture of acetonitrile-water in basic medium is suitable for pre-concentration of the analytes. Pre-concentration factors up to 250 can be obtained. The quinolones are separated with an octyl silica-based column and mobile phases consisting of aqueous oxalic acid solutions and acetonitrile mixtures. The attained detection limits of the whole process are in the ng l(-1) level when 250 ml of water sample is processed. Recovery rates, from natural water samples spiked at 2060 ng l(-1) level, range from 70 to 100% and common standard deviation are about 6-12%.     

Solvent extraction equilibria of the nickel-3-(2-furyl)-2-mercaptopropenoic acid complex as an ion-pair with the diphenylguanidinium ion

The extraction of nickel from aqueous media (0.1M NaClO₄) with 3-(2-furyl)-2-mercaptopropenoic acid (FMPA) in dichloroethane at 25° has been studied. The extraction is efficient only if a suitable counter-ion is present to form an ion-associate with the Ni—FMPA complex. The diphenylguanidinium ion has been found suitable as the counter-ion.     

Study on partition equilibria of metal complexes in non-ionic micellar solutions from spectrophotometric data

The complexation equilibria for Zn(II)-8-quinolinol and Zn(II)-5,7-dichloro-2-methyl-8-quinolinol systems were studied spectrophotometrically in aqueous micellar solutions of the non-ionic surfactant Brij-35 in NaCl 0.1 M medium at 25 degrees C. The partition model, in which the different species involved in the equilibria can distribute themselves between aqueous and micellar pseudophases, was applied. Calculations were performed by means of the spdis program, developed specifically to handle multiwavelength spectrophotometric data in micellar systems. A factor analysis was applied to the spectrophotometric data in order to determine the number of species in equilibrium. A quantitative relationship was found between fluorescence intensity and the micellar solubilization of metal chelates.     

Ultrashort partial-filling technique in capillary electrophoresis for infinite resolution of tramadol enantiomers and its metabolites with highly sulfated cyclodextrins

The possibility to enhance resolution to infinite value in chiral capillary electrophoresis is attained as soon as the apparent mobility of one enantiomer becomes opposite to the other. This could be achieved on the basis of the carrier ability of multiple charged chiral selectors such as highly sulfated cyclodextrin (HS-CD). With tramadol and its phase I metabolites selected as model compounds, the HS-gamma-CD was found to be the most appropriate chiral selector. The CD concentration was determined where one enantiomer still migrated as a cation while the other migrated in the opposite side. Besides the chiral selector concentration, secondary parameters such as buffer concentration appeared to be critical to reach infinite resolution. The latter was achieved with partial filling technique using ultrashort separation zones (a few mm). In order to better understand the interaction mechanism between the selected CD and the analytes, the classical affinity capillary electrophoresis method, although not fully satisfactory because of ionic strength variations within a series of mobility shift measurements, was applied to estimate complexation constants and complex mobilities. The results obtained point to the prevailing role of complex mobility differences in the enantioselectivity mechanism.     

Residue analysis of macrolides in poultry muscle by liquid chromatography-electrospray mass spectrometry

A liquid chromatography-mass spectrometry method is proposed for the determination of seven macrolides authorised in the EU as veterinary drugs for food-producing animals. Sample treatment involves extraction of the analytes with a water-methanol mixture containing metaphosphoric acid and clean-up by SPE with a cation-exchange cartridge. Separation was carried out in an end-capped silica-based C18 column and mobile phases consisting of water/acetonitrile mixtures containing trifluoroacetic acid. A gradient elution, from 28 to 40% acetonitrile was used. Detection was performed by mass spectrometry with electrospray ionisation in the positive mode. Several parameters affecting the mass spectra were studied. The protonated molecular ion was selected for quantitation purposes under selected ion monitoring mode. Detection limits were in the range 1-20 microg l(-1). Recoveries ranged between 56 and 93% with RSD lower than 12%. The method has been successfully applied for multiresidue determination of seven macrolides below the MRLs established by the European Union.     

Analysis of quinolone residues in edible animal products

A comprehensive review on the analysis of quinolone antibacterials is presented. The review covers most of the methods described for the determination of quinolone residues in edible animal products. Sample handling, chromatographic conditions and detection methods have been discussed. A summary of the most relevant information about the analytical procedures has been included.     

Optimisation of mobile phase pH in liquid chromatography. Application to fluorimetric detection of series of quinolones

Summary The dissociation constants of several quinolones in a 7% acetonitrile-water mixture are determined. A model describing the effect of pH on the retention of quinolones by an octadecylsilica stationary phase with a 7% acetonitrile-water mobile phase is proposed. The model uses pH values in the mobile phase instead of pH values in water and takes into account the effect of activity coefficients. Fluorescence of quinolones in the mobile phase is studied, and a chromatographic separation with fluorimetric detection is established. Detection limits for the proposed method range from 3 to 12 μg·L⁻¹.