Extraction from a solid

FeOOH0.4H2O. Such a representation more closely resembles the actual condition of cations in soil, particularly if the discussion is about cations in the soil solution. This introduces a troublesome situation. When a cation is removed (extracted) from a solid matrix into an extracting solution, a species change most likely occurs. In the solid matrix, the cation may not be associated with water molecules, while in solution it most certainly will be. For hydrated species, the amount of associated water and the activity will also change. This raises the question of what form of the species actually exists in the solid matrix. When analyzing for a specific cation in soil, it is important to keep this issue in mind. 

There are instances in which the analyte needs to be extracted from a solid material sample rather than a liquid (see also Section 2.5.3). As in the above discussion for liquid samples, such an experiment is performed either because it is not possible or necessary to dissolve the entire sample or because it is undesirable to do so because of interferences that may also be present. In these cases, the weighed solid sample, preferably finely divided, is brought into contact with the extracting liquid in an appropriate container (not a separatory funnel) and usually shaken or stirred for a period of time, sometimes at an elevated temperature, such that the analyte species is removed from the sample and dissolved in the liquid. The time required for this shaking is determined by the rate of the dissolving. A separatory funnel is not used since two liquid phases are not present, but rather a liquid and a solid phase. A simple beaker, flask, or test tube usually suffices. See Workplace Scene 11.4 for a unique alternative. 

Most of the industrial SFE is for the extraction from a solid matrix. Because of the challenge in the pumping of the solids to high-pressure extractor, the process is usually carried out in a semibatch mode. A number of high-pressure extractors are used in parallel the solid mixture is tilled, extracted, and emptied in a sequential fashion, allowing almost a continuous stream of the extract product. 

Figure 4 depicts the main fractions that can be extracted from a solid-free petroleum fluid. The term "solid" here refers to mineral fines, clays, etc. Asphaltenes extracted from bitumen are very likely to contain solids. In this case, solids can be removed by centrifugation of a 5 wt% solution in toluene at 30,000 g for 3 h (Goual et al, 2006) or by filtration using 0.02 im... 

In the simple case of batch extraction from a solid in a contact stage, a mass balance on the solute gives the equation ... 

Extractables (cleaning) Materials that can be extracted from a solid by solvents that it may come into contact with. Example Extracting phthalates from vinyl gloves by alcohol. 

Phase Separation. Microporous polymer systems consisting of essentially spherical, intercoimected voids, with a narrow range of pore and ceU-size distribution have been produced from a variety of thermoplastic resins by the phase-separation technique (127). If a polyolefin or polystyrene is insoluble in a solvent at low temperature but soluble at high temperatures, the solvent can be used to prepare a microporous polymer. When the solutions, containing 10—70% polymer, are cooled to ambient temperatures, the polymer separates as a second phase. The remaining nonsolvent can then be extracted from the solid material with common organic solvents. These microporous polymers may be useful in microfiltrations or as controlled-release carriers for a variety of chemicals. 

Liquid-liquid extraction is a process for separating components in solution by their distribution between two immiscible liquid phases. Such a process can also be simply referred to as liquid extraction or solvent extraction however, the latter term may be confusing because it also applies to the leaching of a soluble substance from a solid. 

Albertsson (Paiiition of Cell Paiiicle.s and Macromolecules, 3d ed., Wiley, New York, 1986) has extensively used particle distribution to fractionate mixtures of biological products. In order to demonstrate the versatility of particle distribution, he has cited the example shown in Table 22-14. The feed mixture consisted of polystyrene particles, red blood cells, starch, and cellulose. Liquid-liquid particle distribution has also been studied by using mineral-matter particles (average diameter = 5.5 Im) extracted from a coal liquid as the solid in a xylene-water system [Prudich and Heniy, Am. Inst. Chem. Eng. J., 24(5), 788 (1978)]. By using surface-active agents in order to enhance the water wettability of the solid particles, recoveries of better than 95 percent of the particles to the water phase were obsei ved. All particles remained in the xylene when no surfactant was added. 

These mixers are specified when one liquid must be dissolved in another, a solid and a liquid must be mixed, a high viscosity liquid must be reacted, a light liquid must be extracted from a mixture of heavy and light liquids, or when gas must be absorbed in a liquid. To select the proper mixer, certain fluid properties must be know n ... 

The theoretical treatment which has been developed in Sections 10.2-10.4 relates to mass transfer within a single phase in which no discontinuities exist. In many important applications of mass transfer, however, material is transferred across a phase boundary. Thus, in distillation a vapour and liquid are brought into contact in the fractionating column and the more volatile material is transferred from the liquid to the vapour while the less volatile constituent is transferred in the opposite direction this is an example of equimolecular counterdiffusion. In gas absorption, the soluble gas diffuses to the surface, dissolves in the liquid, and then passes into the bulk of the liquid, and the carrier gas is not transferred. In both of these examples, one phase is a liquid and the other a gas. In liquid -liquid extraction however, a solute is transferred from one liquid solvent to another across a phase boundary, and in the dissolution of a crystal the solute is transferred from a solid to a liquid. 

J.9 You are asked to identify compound X, which was extracted from a plant seized by customs inspectors. You run a number of tests and collect the following data. Compound X is a white, crystalline solid. An aqueous solution of X turns litmus red and conducts electricity poorly, even when X is present at appreciable concentrations. When you add sodium hydroxide to the solution a reaction takes place. A solution of the products of the reaction conducts electricity well. An elemental analysis of X shows that the mass percentage composition of the compound is 26.68% C and 2.239% H, with the remainder being oxygen. A mass spectrum of X yields a molar mass of 90.0 g-moF. (a) Write the empirical formula of X. (b) Write... 

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. 

In most unit operations it is of considerable importance that material is transferred from one phase to another across a boundary. The transfer of material from a solid phase to a liquid phase (as typically in leaching), or the transfer of material between one liquid phase to another liquid phase (as typically in molten metal and molten slag phases), extraction or between liquid and vapor phases (as typically in distillation) are well-known examples encountered in practice. 

In liquid-solid extraction (LSE) the analyte is extracted from the solid by a liquid, which is separated by filtration. Numerous extraction processes, representing various types and levels of energy, have been described steam distillation, simultaneous steam distillation-solvent extraction (SDE), passive hot solvent extraction, forced-flow leaching, (automated) Soxh-let extraction, shake-flask method, mechanically agitated reflux extraction, ultrasound-assisted extraction, y -ray-assisted extraction, microwave-assisted extraction (MAE), microwave-enhanced extraction (Soxwave ), microwave-assisted process (MAP ), gas-phase MAE, enhanced fluidity extraction, hot (subcritical) water extraction, supercritical fluid extraction (SFE), supercritical assisted liquid extraction, pressurised hot water extraction, enhanced solvent extraction (ESE ), solu-tion/precipitation, etc. The most successful systems are described in Sections 3.3.3-3.4.6. Other, less frequently... 

In extraction from a polymer/additive solid matrix the rate-determining step in the extraction process is governed by the interaction of the solvent of sufficient dissolution power with the matrix and the removal of the analyte (cf. Section 3.4.1.3). There appears to exist a direct relationship between degree of swelling and efficiency of extraction. The amount of C02 absorbed depends on temperature, pressure and the polymer concerned. Crystalline polymers are-not surprisingly-plasticised less... 

Principles and Characteristics Solid-phase extraction (SPE) is a very popular sample preparation and clean-up technique. In SPE solutes are extracted from a liquid (or gaseous) phase into a solid phase. Substances that have been extracted by the solid particles can be removed by washing with an appropriate liquid eluent. Usually, the volume of solvent needed for complete elution of the analytes is much smaller (typically < 1 mL) than the original sample volume. A concentration of the analytes is thus achieved. 

Speciation involves a number of discrete analytical steps comprising the extraction (isolation) of the analytes from a solid sample, preconcentration (to gain sensitivity), and eventually derivatisation (e.g. for ionic compounds), separation and detection. Various problems can occur in any of these steps. The entire analytical procedure should be carefully controlled in such a way that decay of unstable species does not occur. For speciation analysis, there is the risk that the chemical species can convert so that a false distribution is determined. In general, the accuracy of the determinations and the trace-ability of the overall analytical process are insufficiently ensured [539]. 

SPME can be used to extract organic compounds from a solid matrix as long as target compounds can be released from the matrix into the headspace. For volatile compounds, the release of analytes into the headspace is relatively easy because analytes tend to vaporise once they are dissociated from their matrix. For semi-volatile compounds, the... 

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