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Enrichment Factor (enrichment + factor)
Selected AbstractsIntegrated Microanalytical System Coupling Permeation Liquid Membrane and Voltammetry for Trace Metal Speciation.ELECTROANALYSIS, Issue 10 2004Optimization, Technical Description Abstract A new minicell coupling the liquid-liquid extraction technique called permeation liquid membrane (PLM) with an integrated Ir-based Hg-plated microelectrode array for voltammetric detection has been developed for the speciation of heavy metals in natural waters. Lead and cadmium have been used as model compounds. The PLM consists of a carrier (0.1,M 22DD+0.1,M lauric acid) dissolved in 1,:,1 mixture of toluene/phenylhexane held in the small pores (30,nm) of a hydrophobic polypropylene membrane (Celgard 2500). One side of this membrane is in contact with a flowing source solution, containing the metal ions of interest. An acceptor or strip solution (pyrophosphate) is placed on the other side of the PLM with the microelectrode array placed at 480,,m of the PLM. The analyte is transported by the carrier from the source solution to the strip solution. The originality of the new minicell is that accumulation in the strip solution is voltammetrically followed by the integrated microelectrode array in real time, and at low concentration level, using square-wave anodic stripping voltammetry (SWASV). In order to protect the Hg microelectrodes from the adsorption of the hydrophobic carrier, the microelectrodes are embedded in a thin gel layer (280,,m) of 1.5% LGL agarose gel containing 10% of hydrophobic silica particles C18. The choice of optimum conditions is discussed in details in this article. Due to the very small effective strip volume of the new cell (less than 1,,L), high enrichment factor can be obtained (e.g., 330 for Pb) after 2,hours of accumulation. No deaeration of the solutions is required for SWASV measurements. Detection limits under these conditions are 2,pM and 75,pM for Pb and Cd, respectively, using a voltammetric deposition time of 5,min. In addition, no fouling effects were observed with natural water samples. [source] Cloud point preconcentration prior to capillary zone electrophoresis: Simultaneous determination of platinum and palladium at trace levelsELECTROPHORESIS, Issue 18 2005Soledad Cerutti Professor Abstract The incorporation of a cloud point extraction (CPE) step prior to capillary electrophoresis (CE) for simultaneously determining platinum and palladium at sub-,g/L levels is presented and evaluated. The analytes were extracted as 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol complexes, at pH,2.0, mediated by micelles of the nonionic surfactant polyethyleneglycolmono- p -nonylphenyl ether (PONPE 7.5). The separation,determination step was developed from 150,,L of the extracted surfactant-rich phase diluted with 50,,L of acetonitrile (ACN). An exhaustive study of the variables affecting the cloud point extraction with PONPE 7.5 and the CZE step was done. The type and composition of the background electrolytes (BGEs) were investigated with respect to separation selectivity, reproducibility, and stability. A BGE of 50,mM monobasic sodium phosphate containing 30% ACN, pH 4.53 was found to be optimal for the separation of metal chelates. Detection was performed at 576,nm. An enrichment factor of 250 was obtained for the preconcentration of 50,mL of sample solution. The detection limits for the preconcentration of 50,mL of sample were 0.04,,g/L for Pt and 0.08,,g/L for Pd. As an analytical demonstration, ultratrace concentrations of platinum and palladium were conveniently quantitated in spiked water and urine samples. [source] On-line preconcentration for capillary electrophoresis-atomic fluorescence spectrometric determination of arsenic compoundsELECTROPHORESIS, Issue 12 2004Xue-Bo Yin Abstract An on-line preconcentration method was developed for capillary electrophoresis (CE) with hydride generation-atomic fluorescence spectrometric (HG-AFS) detection of arsenite, arsenate, dimethylarsenic acid, and monomethylarsenic acid. These arsenic species were negatively charged in the sample solution with high pH. When the potential was applied to the electrophoretic capillary, the negatively charged analyte ions moved faster and stacked at the boundary of sample and CE buffer with low pH. So, high sample pH in combination with low buffer pH allowed the injection of large sample volumes (, 1100 nL). Comparison of the preconcentration of analyte solution, prepared with doubly deionized water and that prepared with lake or river water, indicated that preconcentration was independent on the original matrix. With injection of ,1100 nL sample, an enrichment factor of 37,50-fold was achieved for the four species. Detection limits for the four arsenic species ranged from 5.0 to 9.3 ,g·L,1. Precisions (RSDs, n = 5) were in the range of 4.9,6.7% for migration time, 4.7,11% for peak area, and 4.3,7.1% for peak height, respectively. The recoveries of the four species in locally collected water solution spiked with 0.1 ,g·mL,1 (as As) ranged from 83 to 109%. [source] Liquid,liquid,liquid microextraction followed by HPLC with UV detection for quantitation of ephedrine in urineJOURNAL OF SEPARATION SCIENCE, JSS, Issue 18 2008Habib Bagheri Abstract Liquid,liquid,liquid microextraction (LLLME) in combination with HPLC and UV detection has been used as a sensitive method for the determination of ephedrine in urine samples. Extraction process was performed in a homemade total glass vial without using a Teflon ring, usually employed. Ephedrine was first extracted from 3.5 mL of urine sample (pH 12) into a microfilm of toluene/benzene (50:50). The analyte was subsequently back extracted into an acidic microdrop solution (pH 2) suspended in the organic phase. The extract was then injected into the HPLC system directly. An enrichment factor of 137 along with a good sample clean-up was obtained under the optimized conditions. The calibration curve showed linearity in the range of 0.01,50 mg/L with regression coefficient corresponding to 0.998. The LODs and LOQs, based on a S/N of 3 and 10, were 5 and 10 ,g/L, respectively. The method was eventually applied for the determination of ephedrine in urine sample after oral administration of 5 mg single dose of drug. [source] Ion imprinted polymer particles for separation of yttrium from selected lanthanidesJOURNAL OF SEPARATION SCIENCE, JSS, Issue 9 2006Ramakrishnan Kala Abstract Lanthanide(III) (Dy, Gd, Tb and Y) ion imprinted polymer (IIP) materials were synthesized via single pot reaction by mixing lanthanide imprint ion with 5,7-dichloroquinoline-8-ol, 4-vinylpyridine, styrene, divinylbenzene and 2,2,-azobisisobutyronitrile in 2-methoxyethanol porogen. The imprint ion was removed by stirring the above materials (after powdering) with 6 mol/L HCl to obtain the respective lanthanide IIP particles. Y-Dy, Y-Gd and Dy-Gd polymer particles were obtained by physically mixing equal amounts of the respective leached individual lanthanide(III) particles. Control polymer (CP) particles were similarly prepared without imprint ion. Application of the above synthesized polymer particles was tested for separation of Y from Dy, Gd and Tb employing batch and column SPE methods using inductively coupled plasma atomic emission spectrometry for the determination. Optimization studies show that Y present in 500 mL can be preconcentrated using Dy-Gd IIP particles and eluted with 20 mL of 1.0 mol/L of HCl, providing an enrichment factor of , 25. Dy-Gd IIP particles offer higher selectivity coefficients for Y over other lanthanides compared to other IIP particles and commercial liquid,liquid extractants. Selectivity studies for Y over other coexisting inorganic species (other than lanthanides) were also conducted and the results obtained show a quantitative separation of Y from other inorganics other than Cu(II) and Fe(III). Furthermore, both batch and column studies indicate the purification of yttrium concentrate from 55.0 ± 0.2 to 65.2 ± 0.2% in a single stage of operation. [source] Ion-pair mediated transport of angiotensin, neurotensin, and their metabolites in liquid phase microextraction under acidic conditionsJOURNAL OF SEPARATION SCIENCE, JSS, Issue 11 2005J. Léon E. Reubsaet Abstract This paper discusses the behaviour of angiotensin 1 and neurotensin together with their metabolites in a three-phase liquid phase microextraction under acidic conditions. Variations in donor phase, organic phase, and acceptor phase are studied with extraction recovery as response variable. It is proved that for all peptides the transport across the organic phase is mediated by heptane-1-sulphonic acid. n -Octanol gave overall best results as organic phase. A donor phase volume of 1.0 mL was chosen as a compromise between optimal recovery and robustness of the LPME device. The optimal pH of the donor phase (using acceptor phase of pH 2) was found to be different for the peptides, which opens opportunities for selective sample preparation. Decreasing the acceptor phase pH to 1.0 resulted in increased extraction recoveries. On using 1.0 mL of donor phase containing 50 mM heptane-1-sulphonic acid pH 3, n -octanol as organic phase immobilized in the pores of the fibre, and 20 ,L of acceptor phase containing 0.1 mol/L HCl, extraction recoveries up to 82% (enrichment factor = 41) were achieved. To our knowledge this is the first report on liquid phase microextraction of angiotensins and neurotensins. [source] Extraction of Proteins from Biological Fluids by Use of an Ionic Liquid/Aqueous Two-Phase SystemCHEMISTRY - A EUROPEAN JOURNAL, Issue 7 2007Zhuo Du Abstract An ionic liquid/aqueous two-phase system based on the hydrophilic ionic liquid 1-butyl-3-methylimidazolium chloride (BmimCl) and K2HPO4 has been employed for direct extraction of proteins from human body fluids for the first time. Proteins present at low levels were quantitatively extracted into the BmimCl-rich upper phase with a distribution ratio of about 10 between the upper and lower phase and an enrichment factor of 5. Addition of an appropriate amount of K2HPO4 to the separated upper phase results in a further phase separation, giving rise to an improved enrichment factor of 20. FTIR and UV spectroscopy demonstrated that no chemical (bonding) interactions between the ionic liquid and the protein functional groups were identifiable, while no alterations of the natural properties of the proteins were observed. The partitioning of proteins in the two-phase system was assumed to have been facilitated by the electrostatic potential difference between the coexisting phases, as well as by salting out effects. The system could be applied successfully for the quantification of proteins in human urine after on-line phase separation in a flow system. The use of an ionic liquid, as a green solvent, offers clear advantages over traditional liquid,liquid extractions, in which the use of toxic organic solvents is unavoidable. [source] Direct chiral analysis of primary amine drugs in human urine by single drop microextraction in-line coupled to CEELECTROPHORESIS, Issue 16 2009Kihwan Choi Abstract Three-phase single drop microextraction (SDME) was in-line coupled to chiral CE of weakly basic amine compounds including amphetamine. SDME was used for the matrix isolation and sample preconcentration in order to directly analyze urine samples with the minimal pretreatment of adding NaOH. A small drop of an acidic aqueous acceptor phase covered with a thin layer of octanol was formed at the tip of a capillary by simple manipulation of the liquid handling functions of a commercial CE instrument. While the saline matrix of the urine sample was blocked by the octanol layer, the basic analytes in a basic aqueous donor phase were concentrated into the acidic acceptor drop through the octanol layer by the driving force of the pH difference between the two aqueous phases. The enantiomers of the enriched amines were resolved by using (+)-(18-crown-6)-tetracarboxylic acid as a chiral selector for the subsequent CE separation. From 10,min SDME with the agitation of the donor phase by a small stirrer retrofit to the CE instrument, enrichment factors were about a 1000-fold, yielding the LOD of 0.5,ng/mL for amphetamine. This low LOD value as well as the convenience of in-line coupled SDME make the proposed scheme well suited for the demanding chiral analysis of amphetamine-type stimulants. [source] Emission of trace toxic metals during pulverized fuel combustion of Czech coalsINTERNATIONAL JOURNAL OF ENERGY RESEARCH, Issue 13 2003P. Danihelka Abstract A study of the trace elements emission (As, Se, Cd, Co, Cr, Cu, Zn, Hg, Tl, Pb, Ni, Sn, Sb, V, Mn and Fe) from pulverized coal combustion has been made at six heating and power stations situated in the Czech Republic. The amount of chlorine in coal has considerable influence on volatilization of some elements such as Zn, Cu, Pb, Hg and Tl, which is explained by the formation of thermodynamically stable compounds of these elements with chlorine. Generally, the affinities for Cl follows the order Tl > Cu > Zn > Pb > Co > Mn > Sn > Hg. The experimental data indicates enrichment of some of the trace toxic elements in the emissions (Cu, Zn, As, Se, Cd, Sn, Sb, Hg and Pb) and good agreement was obtained by thermodynamic equilibrium calculations with a few exceptions. In the case of Fe, Mn, Co, Cr and Sn calculated values are overestimated in the bottom ash and there are zero predicted amounts of these elements in the fly ash. In comparison, the results from experiments show up to 80% of these elements retained in fly ash. This implies that there exist additional steps leading to the enrichment by Fe, Mn, Co, Cr and Sn of small particles. Such mechanisms could include the ejection during devolatilization of small inorganic particles from the coal of bottom ash particles, or disintegration of the char containing these metals to small particles of fly ash. On the other hand, there are slightly overestimated or similar values of relative enrichment factors for As, V, Cu, Cd, Sb, Tl and Pb in the fly ashes and zero predicted values for bottom ashes. Our experimental results show about 5% or less of these elements are retained in bottom ashes, so they probably remain in the bottom ash inside unburned parts of coal. Copyright © 2003 John Wiley & Sons, Ltd. [source] Ultrasound-assisted dispersive liquid,liquid microextraction coupled with capillary gas chromatography for simultaneous analysis of nine pyrethroids in domestic wastewatersJOURNAL OF SEPARATION SCIENCE, JSS, Issue 12 2010Hongyuan Yan Abstract A simple and rapid ultrasound-assisted dispersive liquid,liquid microextraction method coupled with GC-flame ionization detection was developed for simultaneous determination of nine pyrethroids in domestic wastewater samples. An ultrasound-assisted process was applied to accelerate the formation of the fine cloudy solution using small volume of disperser solvent, which markedly increased the extraction efficiency and reduced the equilibrium time. Various parameters affecting the extraction efficiency were investigated, including the type and volume of extraction solvent and disperser solvent, extraction and ultrasonic time. Good linearity was obtained for all analytes in the range of 0.8,100,,g/L with the correlation coefficient (r2),0.998. The recoveries at three spiking levels ranged from 75.3 to 101.2% with the RSD less than 8.7% (n=5). Under the optimum condition, the enrichment factors for the nine pyrethroids ranged from 728- to 1725-fold. This method offered a good alternative for routine analysis due to its simplicity and reliability. [source] Application of continual injection liquid-phase microextraction method coupled with liquid chromatography to the analysis of organophosphorus pesticidesJOURNAL OF SEPARATION SCIENCE, JSS, Issue 4 2009Yanuardi Raharjo Abstract A liquid-phase microextraction coupled with LC method has been developed for the determination of organophosphorus pesticides (methidation, quinalphos and profenofos) in drinking water samples. In this method, a small amount (3 ,L) of isooctane as the acceptor phase was introduced continually to fill-up the channel of a 1.5 cm polypropylene hollow fiber using a microsyringe while the hollow fiber was immersed in an aqueous donor solution. A portion of the acceptor phase (ca. 0.4 ,L) was first introduced into the hollow fiber and additional amounts (ca. 0.2 ,L) of the acceptor phase were introduced to replenish at intervals of 3 min until set end of extraction (40 min). After extraction, the acceptor phase was withdrawn and transferred into a 2 mL vial for a drying step prior to injection into a LC system. Parameters that affect the extraction efficiency were studied including the organic solvent, length of fiber, volume of acceptor and donor phase, stirring rate, extraction time, and effect of salting out. The proposed method provided good enrichment factors of up to 189.50, with RSD ranging from 0.10 to 0.29%, analyte recoveries of over 79.80% and good linearity ranging from 10.0 to 1.25 mg/L. The LOD ranged from 2.86 to 82.66 ,g/L. This method was applied successfully to the determination of organophosphorus pesticides in selected drinking water samples. [source] Online preconcentration using monoliths in electrochromatography capillary format and microchipsJOURNAL OF SEPARATION SCIENCE, JSS, Issue 17 2007Violaine Augustin Abstract Online preconcentration and separation of analytes using an in situ photopolymerized hexyl acrylate-based monolith stationary phase was evaluated using electrochromatography in capillary format and microchip. The band broadening occurring during the preconcentration process by frontal electrochromatography and during the desorption process by elution electrochromatography was studied. The hexyl acrylate-based monolith provides high retention for neutral analytes allowing the handling of large sample volumes and its structure allows rapid mass transfer, thus reducing the band broadening. For moderately polar analytes such as mono-chlorophenols that are slightly retained in water, it was shown that enrichment factors up to 3500 can be obtained by a hydrodynamic injection of several bed volumes for 120 min under 0.8 MPa with a decrease in efficiency of 50% and a decrease of 30% for the resolution between 2- and 3-chlorophenol. An 8 min preconcentration time allows enrichment factors above 100 for polyaromatic hydrocarbons. The interest of these monoliths when synthesized in microchip is also demonstrated. A 200-fold enrichment was easily obtained for PAHs with only 1 min as preconcentration time, without decrease in efficiency. [source] Differences in the stable isotope signatures of seabird egg membrane and albumen , implications for non-invasive studiesRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 23 2009Petra Quillfeldt In many bird species, egg membranes can be obtained non-invasively after the chicks have hatched, and stable isotope analysis of egg membranes can be used to study the diet and foraging distribution of these birds during egg formation. It has been suggested that the enrichment factors of albumen and egg membranes differ for 13C, but are similar for 15N. In this study, we compared carbon and nitrogen stable isotopes of the membranes and albumen of individual eggs of three wild seabird species, the Southern Rockhopper penguin Eudypteschrysocome, the Imperial shag Phalacrocoraxatricepsalbiventer, and the Thin-billed prion Pachyptilabelcheri. We also included chicken eggs for comparison. Egg membranes were generally enriched in 13C, compared with albumen. The difference varied between species, with 2.1, in Rockhopper penguins, 1.6, in Imperial shags, but only 0.5, in Thin-billed prions and 0.4, in chicken eggs. Egg membranes were slightly enriched in 15N in Imperial shags (0.9,) and chickens (0.5,), compared with albumen, while there was no difference for Thin-billed prions and Rockhopper penguins. The isotopic values of carbon and nitrogen were correlated between albumen and egg membranes of individual eggs, suggesting that egg membranes can be used reliably to investigate trophic differences between individuals, seasons or colonies. Species-specific mathematical corrections could be used to compare results across studies that use different egg components. Copyright © 2009 John Wiley & Sons, Ltd. [source] | ||||||||||