Extraction schemes

Two main schemes exist for the separation and purification of tantalum and niobium using liquid-liquid extraction. The first is based on the collective extraction of tantalum and niobium from an initial solution into an organic phase so as to separate them from impurities that remain in the aqueous media, the raffinate. The separation of tantalum and niobium is subsequently performed by fractional stripping into two different aqueous solutions. In this case, stripping of niobium is performed using relatively weak acids prior to the stripping of tantalum. Fig. 125 presents a flow chart of the process. 

The second method is based on selective extraction that consists of extraction into two different organic solutions. In the first step, tantalum is extracted into an organic phase. In the second step of the procedure, niobium is extracted into a separate portion of the extractant. Fig. 126 presents a flow chart of the process based on the selective extraction scheme. 

In both cases, the extraction process includes washing (scrubbing) of the extract, a stage that is not shown separately. The organic phase that results from the stripping process is returned to the beginning of the extraction process for reuse as an extractant. 

The second process of selective extraction is more effective and leads to better separation of tantalum and niobium and to more effective purification. Its performance, however, requires the initial solution to be of relatively low acidity. 

Tantalum and niobium processing - liquid - liquid extraction 

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Extraction of hemiceUulose is a complex process that alters or degrades hemiceUulose in some manner (11,138). Alkaline reagents that break hydrogen bonds are the most effective solvents but they de-estetify and initiate -elimination reactions. Polar solvents such as DMSO and dimethylformamide are more specific and are used to extract partiaUy acetylated polymers from milled wood or holoceUulose (11,139). Solvent mixtures of increasing solvent power are employed in a sequential manner (138) and advantage is taken of the different behavior of various alkaUes and alkaline complexes under different experimental conditions of extraction, concentration, and temperature (4,140). Some sequences for these elaborate extraction schemes have been summarized (138,139) and an experimenter should optimize them for the material involved and the desired end product (102). 

Another solvent extraction scheme uses the mixed anhydrous chlorides from a chlorination process as the feed (28). The chlorides, which are mostly of niobium, tantalum, and iron, are dissolved in an organic phase and are extracted with 12 Ai hydrochloric acid. The best separation occurs from a mixture of MIBK and diisobutyl ketone (DIBK). The tantalum transfers to the hydrochloric acid leaving the niobium and iron, the DIBK enhancing the separation factor in the organic phase. Niobium and iron are stripped with hot 14—20 wt % H2SO4 which is boiled to precipitate niobic acid, leaving the iron in solution. 

Product recovery possibly requiring an exotic, expensive distillation (or extraction) scheme... 

Despite the recent efforts for settling operational conditions for metal and metalloid fractionation, conventional batch sequential extraction schemes lack automation and are rather time consuming and laborious. Two additional main problems are the phase overlapping and possible re-adsorption of released elements. 

In the present work it has been shown that on-line coupling of flowthrough fractionation in RCC with ICP-EAS detection enables not only the fast and efficient fractionation of trace elements (TE) in environmental solids to be achieved but allows real-time studies on the leaching process be made. A novel five-step sequential extraction scheme was tested in on-line mode. The optimal conditions for the fractionation were chosen. Investigating elution curves provides important information on the efficiency of the reagents used, the leaching time needed for the separation of each fraction, and the potential mobility of HM forms. 

Microwave and fluorous technologies have been combined in the solution phase parallel synthesis of 3-aminoimidazo[l,2-a]pyridines and -pyrazines [63]. The three-component condensation of a perfluorooctane-sulfonyl (Rfs = CgFiy) substituted benzaldehyde by microwave irradiation in a single-mode instrument at 150 °C for 10 min in CH2CI2 - MeOH in the presence of Sc(OTf)3 gave the imidazo-annulated heterocycles that could be purified by fluorous solid phase extraction (Scheme 9). Subsequent Pd-catalyzed cross-coupling reactions of the fluorous sulfonates with arylboronic acids or thiols gave biaryls or aryl sulfides, respectively, albeit it in relatively low yields. 

The theory and development of a solvent-extraction scheme for polynuclear aromatic hydrocarbons (PAHs) is described. The use of y-cyclodextrin (CDx) as an aqueous phase modifier makes this scheme unique since it allows for the extraction of PAHs from ether to the aqueous phase. Generally, the extraction of PAHS into water is not feasible due to the low solubility of these compounds in aqueous media. Water-soluble cyclodextrins, which act as hosts in the formation of inclusion complexes, promote this type of extraction by partitioning PAHs into the aqueous phase through the formation of complexes. The stereoselective nature of CDx inclusion-complex formation enhances the separation of different sized PAH molecules present in a mixture. For example, perylene is extracted into the aqueous phase from an organic phase anthracene-perylene mixture in the presence of CDx modifier. Extraction results for a variety of PAHs are presented, and the potential of this method for separation of more complex mixtures is discussed. 

Another equally important consideration before development of a determinative or confirmatory method is an understanding of the chemical properties of the analyte. Such an understanding becomes the cornerstone of a successful method since the unique chemical properties of each analyte provide the basis for isolation and detection schemes. Table 1 lists some of the important chemical properties that could be considered. For example, knowing the or p/fb of an analyte could influence the choice of a liquid-liquid extraction scheme, solid-phase extraction (SPE) cartridge, mobile phase pH, or mass spectrometric ionization. Knowing the overall polarity of the analyte can be very helpful in the evaluation of an extraction or separation. Currently, computational methods are available to obtain an estimate of the logP... 

The extraction efficiencies using a blender and a shaker were compared and both methods gave similar results. A corn sample treated with radiolabeled carfentrazone-ethyl and collected from a metabolism study was used for comparison. Multiple samples can be extracted simultaneously if extraction is performed by shaking. In addition, since the extraction procedures in the residue study closely followed the extraction scheme in the metabolism study, the resulting extraction efficiencies from both studies were almost identical. 

From these results, one can understand that the liquid-liquid interface can assist effectively in the interfacial reaction through the adsorption of extractants like a solid catalyst. The whole extraction scheme of the chelate extraction system is represented in Scheme 1. 

Hall G.E.M., Gauthier G., Pelchat J.C., Pelchate P., Vaive J.E. Application of a sequential extraction scheme to ten geological certified reference materials for the determination of 20 elements. J Anal At Spectrom 1996 11 787-796. 

Extraction scheme for a single solute by Craig counter-current distribution. (Figures represent the proportions in each phase for D= 1 and equal volumes. Only the first four extractions are shown). 

Adapted from Nemati K, Baker NKA, Abas MRB, Sobhanzadeh E, Low KH. Comparison of unmodified and modified BCR sequential extraction schemes for the fractionation of heavy metals in shrimp aquaculture sludge from Selangor, Malaysia. Environ. Mont. Assess. 2011 176 313-320. 

The sequential extraction scheme developed by Foerstner [4] was chosen for these investigations except for one modification. In the last step a digestion with aqua regia (German Regulations DIN 38414, part 7) was used. 

The most important step in any aqueous extraction scheme is facilitation of the transfer of mineral particles from the bituminous matrix to the aqueous phase (Fig. 1). This process appears to be more favorable in the Athabasca tar sands than in other tar sands due to a postulated, but unobserved, film of absorbed water present on the mineral particles. The transfer process may be visualized in 2 stages 1) the transition from complete immersion in the bulk bituminous phase to partial contact with both phases, and 2) the transition from partial contact with both phases to complete immersion in the aqueous phase (Fig. la,b). 

The paddle mill was used to study the effect of surfactant type on a solvent-aqueous-surfactant extraction scheme for the recovery of bitumen from Athabasca tar sand. n the experiments of Figures 4,5 and 6, bitumen recovered from the surface phases was measured as a function of the mole fraction of ethylene oxide in the surfactant and as a function of the extraction step in which the surfactant was added. The results are reported as the % of the total bitumen present in the surface fraction. The amount of surfactant used was that required to give a final aqueous concentration of 0.02% (w/v), but in different sets of experiments the surfactant was added at various stages in the process. 

The form of nickel in particles from different industries varies. The mineralogical composition, chemical content, and form of dusts from nine industries in Cracow, Poland, were examined (Rybicka 1989). The chemical form of a particle-associated heavy metal that was assessed by a five-step extraction scheme classified the metal as exchangeable, easily reducible (manganese oxides, partly amorphous iron oxyhydrates and carbonates), moderately reducible (amorphous and poorly crystallized iron oxyhydrates), organically bound or sulfidic, and residual. Dusts from power plants had a silicate characteristic with quartz and mullite predominant. Approximately 90% of the nickel from these... 

While hundreds of materials probably could fulfill the broad requirements of a solvent for the extraction of pollutants, in this example we will start our investigation with work done at the University of Alabama on a process called biphasic extraction. Homopolymers and copolymers (referred to in this book as polyols) use components made from ethylene oxide (EO) and blends of ethylene oxide and propylene oxide (PO), respectively. Since they are soluble in water, they are not useful in solvent extraction schemes. 

The concentrated extract is then split. To one portion, 1.0 mL of DMSO is added, and the dichloromethane is removed under a stream of nitrogen. The resulting DMSO solution is used for the direct assay of the extract. If fractionation of the remaining extract is required, the investigator is given the option of using the acid/base-neutral extraction scheme described in step 3 of the nonaqueous liquid protocol or the HPLC technique described in the sample fractionation methods section. 

Analytical separation of several organics from water by PVC polymer is feasible. A solvent extraction model describes the separation dynamics and pH dependence. Selectivity via pH control of the extraction step and preconcentration of analyte can be accomplished. These results suggest that other polymer solvent extraction schemes can be developed by using this approach. The flow-through amperometric technique provides a well-suited detector component for the technique. 

The PGase extraction scheme outlined below (see Support Protocol) is based on the properties of the enzyme from tomato (Pressey, 1986). Enzymes from other sources will probably require different extraction conditions. A more detailed discussion of common approaches to enzyme extraction is included (see Background Information, discussion of samples for pectic enzyme assays). 

Optimal conditions for the extraction of polygalacturonase (PGase) depend on the sample matrix (type of food product) and the source of the enzyme (plant versus microbial origin). The extraction scheme presented below is that developed for the PGase of tomato (Pressey, 1986). 

The nozzle consists of an expansion chamber and tube (common stainless steel fittings), a shock absorber (spring) and splash prevention cover (a small inverted polyethylene delivery funnel). In a 12 vessel extraction scheme, two nozzles are used for each pair of vessels. 

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