Concentration step

Stripping voltammetry involves the pre-concentration of the analyte species at the electrode surface prior to the voltannnetric scan. The pre-concentration step is carried out under fixed potential control for a predetennined time, where the species of interest is accumulated at the surface of the working electrode at a rate dependent on the applied potential. The detemiination step leads to a current peak, the height and area of which is proportional to the concentration of the accumulated species and hence to the concentration in the bulk solution. The stripping step can involve a variety of potential wavefomis, from linear-potential scan to differential pulse or square-wave scan. Different types of stripping voltaimnetries exist, all of which coimnonly use mercury electrodes (dropping mercury electrodes (DMEs) or mercury film electrodes) [7, 17]. 

Improved sensitivities can be attained by the use of longer collection times, more efficient mass transport or pulsed wavefomis to eliminate charging currents from the small faradic currents. Major problems with these methods are the toxicity of mercury, which makes the analysis less attractive from an eiivironmental point of view, and surface fouling, which coimnonly occurs during the analysis of a complex solution matrix. Several methods have been reported for the improvement of the pre-concentration step [17,18]. The latter is, in fact. 

Assuming a lineal equiUbiium lelationship (over the range of the small concentration step, q = ifc), this becomes... 

In some cases, a mixture of natural petroleum feedstock is preblended with synthetic alkylated aromatics, such as detergent aromatic alkylate bottoms or with first-intent synthetic mono- or dialkylated aromatics, selected to provide a suitable molecular weight for cosulfonation and subsequent processing. The use of blended feedstocks may eliminate the need for conducting an oil extraction—concentrating step, particularly for a typical 40% Ca or Mg petroleum sulfonated product. 

Sequential batch diafiltration is a series of dilution—concentration steps. The concentration of membrane-permeable species is... 

Chemical Precipitation. The product of the extraction processes, whether derived from acid or carbonate leach, is a purified uranium solution that may or may not have been upgraded by ion exchange or solvent extraction. The uranium ia such a solution is concentrated by precipitation and must be dried before shipment. Solutions resulting from carbonate leaching are usually precipitated directly from clarified leach Hquors with caustic soda without a concentration step, as shown ia equation 9. 

A numerical solution of this equation for a constant surface concentration (infinite fluid volume) is given by Garg and Ruthven [Chem. Eng. ScL, 27, 417 (1972)]. The solution depends on the value of A. = n i — n )/ n — n ). Because of the effect of adsorbate concentration on the effective diffusivity, for large concentration steps adsorption is faster than desorption, while for small concentration steps, when D, can be taken to he essentially constant, adsorption and desorption curves are mirror images of each other as predicted by Eq. (16-96) see Ruthven, gen. refs., p. 175. 

Conventional elution chromatography has the serious disadvantage of dilution, and usually a concentration step must follow. The technique of displacement chromatography circumvents dilution and may even result in an eluant more concentrated than the feed. A displacer compound breaks the desired product from the chromatographic material sharply, and a column heavily loaded with several biochemicals will release them one at a time depending on their adsorption equilibria. However, the displacers tena to be expensive and can be troublesome to remove from the product. 

The concentration mode is used when the extract from the SEE module is not concentrated enough to be directly analyzed by the CE instrument, and thus requires a concentration step, which is carried out in the concentrator device. In this mode, during the concentration step the extract from the SEE cell enters the first valve (positioned in the concentration mode (Eigure 6.11(a)), and is then directed to and adsorbed into the sample concentrator which contains an SPE cartridge. While the... 

The direct mode is used when the concentration of the SEE extract is enough for direct analysis in the CE instrument without the need for a pre-concentration step. In this case, the sample concentrator is by-passed and the SEE extract goes directly to the CE instrument. The extract is collected in a CE vial containing an appropriate solvent and is thus ready for the CE analysis (Eigure 6.12). 

Figure 6.11 Schematic diagrams of the valve configurations for the SFE-CEST coupling in the concentration mode, shown for (a) the concentration step and (b) the elution step, (from ref. 58)...

Voltaic cells 64. 504 Voltammetry 7, 591 anodic stripping, 621 concentration step, 621 mercury drop electrode, 623 mercury film electrode, 623 peak breadth, 622 peak current, 622 peak potential, 622 purity of reagents, 624 voltammogram, 622 D. of lead in tap water, 625 Volume distribution coefficient 196 Volume of 1 g of water at various temperatures, (T) 87... 

Accurate quantitation in GC/MS requires the addition of a known quantity of an internal standard to an accurately weighed aliquot of the mixture (matrix) being analyzed. The internal standard corrects for losses during subsequent separation and concentration steps and provides a known amount of material to measure against the compound of interest. The best internal standard is one that is chemically similar to the compound to be measured, but that elutes in an empty space in the chromatogram. With MS, it is possible to work with isotopically labeled standards that co-elute with the component of interest, but are distinguished by the mass spectrometer. 

The drying/concentration step of the Dryex process has been conceived to upgrade the processed surfactants depending on product type, this upgrading may consist of an increase of active matter in the product (obtainable by H20 removal) or require the reduction or elimination of undesirable byproducts (i.e., 1,4-dioxane in FAES). 

Step 3 In the third row write the equilibrium concentrations by adding the change in concentration (step 2) to the initial concentration for each substance (step 1). 

Step 1 Initial concentration Step 2 Change in concentration Step 3 Equilibrium concentration... 

Ethyl chloroformate obtained from Aldrich Chemical Company, Inc., was distilled, b.p. 93°. The progress of the reaction may be followed by proton magnetic resonance spectroscopy. Aliquots are partitioned between dichloromethane and water, the organic layer is concentrated, and the spectrum is recorded. A quartet from the ethoxy group of the mixed anhydride appears at 8 4.2. Ethyl chloroformate, which exhibits a quartet at 6 4.3, is removed in the concentration step. 

The first four steps of the seven-step strategy are identical to the ones in Example. In this example, addition of a strong acid or base modifies the concentrations that go into the buffer equation. We need to determine the new concentrations (Step 5) and then apply the buffer equation (Step 6). In dealing with changes in amounts of acid and base, it is often convenient to work with moles rather than molarities. The units cancel in the concentration term of the buffer equation, so the ratio of concentrations can be... 

Depending on the means of extraction, decreasing the ratio of extraction solvent to plant material may avoid the need for a concentration step. However, quantitative extractions usually require an adequate rate of solvent to material and two or more re-extractions until a clear or faintly colored solution is obtained. ... 

The filtrate supplied with a 2 liter culture, was treated with increasing amounts of ammonium sulfate. At each concentration step, the precipitate was checked for the polygalacturonase activity. SA specific activity TA total activity. 

The organic solvent used to elute the compound must be adequately strong (polar for the adsorbent silica gel) and a good solvent for the component. Absolute methanol should be avoided as a siugle solvent because silica gel itself and some of its common impurities (Fe, Na, SO4) are soluble iu this solvent and will contaminate the isolated material. Solvent containing less than 30% methanol is recommended, or ethanol, acetone, chloroform, dichloromethane, or the mobile phase originally used for PLC are other frequently nsed choices for solnte recovery. Water is not recommended because it is so difficult to remove by evaporation during the concentration step (removal by lyophilization is necessary). A formula that has been used to calculate the volume of solvent needed when the PLC mobile phase is chosen for elution is ... 

Exudate collection in trap solutions usually requires subsequent concentration steps (vacuum evaporation, lyophilization) due to the low concentration of exudate compounds. Depending on the composition of the trap solution, the reduction of sample volume can lead to high salt concentrations, which may interfere with subsequent analysis or may even cause irreversible precipitation of certain exudate compounds (e.g., Ca-citrate, Ca-oxalate, proteins). Therefore, if possible, removal of interfering salts by use of ion exchange resins prior to sample concentration is recommended. Alternatively, solid-phase extraction techniques may be employed for enrichment of exudate compounds from the diluted trap solution (11,22). High-molecular-weight compounds may be concentrated by precipitation with organic solvents [methanol, ethanol, acetone 80% (v/v) for polysaccharides and proteins] or acidification [trichloroacetic acid 10% (w/v), per-... 

Volatile analytes. As residue analysis is also trace analysis in the lower ppm (mg kg ) to ppb ( ug kg ) range, concentration steps usually involve evaporation of solvents (sometimes with traces of water present) to near dryness. The volatility of analytes can be deduced from their elution temperatures in GC, and thus whenever an analyte elutes from a nonpolar GC phase of film thickness <0.25 qm below approximately 150 °C, losses due to co-evaporation during concentration by the rotary evaporator or by a stream of nitrogen need to be avoided. 

Environmental monitoring of chloroacetanilides requires methods that have the capability to distinguish between complex arrays of related residues. The two example methods detailed here for water monitoring meet this requirement, but the method for metabolites requires sophisticated mass spectral equipment for the detection of directly injected water samples. In the near term, some laboratories may need to modify this method by incorporation of an extraction/concentration step, such as SPE, that would allow for concentration of the sample, so that a less sensitive and, correspondingly, less expensive, mass spectral detector can be used. However, laboratories may want to consider purchasing a sensitive instrument rather than spending time on additional wet chemistry procedures. In the future, sensitive instrumentation may be less expensive and available to all laboratories. Work is under way to expand the existing multi-residue methods to include determination of additional chloroacetanilides and their metabolites in both water and soil samples. 

If the detectability of an analyte in a final eluate volume of 10 mL is not sufficient for the GC determination, then pipet an aliquot (Vi) of the eluate Vce into a 25-mL pear-shaped flask and concentrate the aliquot to ca 0.5 mL in a rotary evaporator (water-bath temperature 30 0 °C). By rinsing the flask, transfer the concentrated solution quantitatively into a graduated test-tube and dilute the sample to a suitable volume ( 2). Without this concentration step, volumes V and V2 need not be considered for the equation given below. 

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