Solvent extraction reflux

Dual solvent fractional extraction (Fig. 7b) makes use of the selectivity of two solvents (A and B) with respect to consolute components C and D, as defined in equation 7. The two solvents enter the extractor at opposite ends of the cascade and the two consolute components enter at some point within the cascade. Solvent recovery is usually an important feature of dual solvent fractional extraction and provision may also be made for reflux of part of the product streams containing C or D. Simplified graphical and analytical procedures for calculation of stages for dual solvent extraction are available (5) for the cases where is constant and the two solvents A and B are not significantly miscible. In general, the accurate calculation of stages is time-consuming (28) but a computer technique has been developed (56). 

NaBH4 has also been crystd from isopropylamine by dissolving it in the solvent at reflux, cooling, filtering and allowing the solution to stand in a filter flask connected to a Dry-ice/acetone trap. After most of the solvent was passed over into the cold trap, crystals were removed with forceps, washed with dry diethyl ether and dried under vacuum. [Kim and Itoh J Phys Chem 91 126 1987.] Somewhat less pure crystals were obtained more rapidly by using Soxhlet extraction with only a small amount of solvent and extracting for about 8h. The... 

The first step for the determination of PAHs is removal from the matrix by solvent extraction, which preferably is performed with boiling toluene or benzene (hot solvent extraction by refluxing see Jacob and Grimmer 1994), although other solvents (e.g. tol-uene/acetone, acetone, and dichloromethane) and other extraction procedures (ultrasonic treatment, Soxhlet extraction, and accelerated solvent extraction) can also be applied. 

Figure 8.9 is an example of the use of solvent extraction to isolate polychlorinated biphenyls from a fat sample [6]. In this example the matrix is chemically modified to improve the selectivity of the extraction. The fat is first hydrolyzed by refluxing in 1 N ethanolic potassium hydroi prior to the... 

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... 

Principles and Characteristics In boiling under reflux procedures a small amount of ground polymer (typically 3g) is placed in a headspace jar (typically 100 mL) and solvent (typically 30 mL) is added. After sealing, the jar is placed in an oven at a temperature where the solvent slowly refluxes. The solvent is, therefore, at the highest temperature possible without applying an external pressure. Consequently, reflux extractions tend to be much faster than Soxhlet extractions. Examples are Soxtec , Soxtherm , FEXTRA and intermittent extraction. Whilst, in theory, partitioning of the analyte between the polymer and solvent prevents complete extraction, this hardly ever constitutes a problem in practice. As the quantity of solvent is much larger than that of the polymer, and the partition coefficients usually favour the solvent, very low additive levels in the polymer result at equilibrium. Any solvent or solvent mixture can be used. 

Additionally, advanced tools for special applications are offered, including provisions for parallel reflux, solvent extraction, and hydrolysis, as well as electrodeless discharge lamps for photochemistry (Fig. 3.10). A detailed description of these accessories can be found on the Milestone website [11],... 

Sample refluxed with F[C104, solvent extracted, Spectrophotometry... 

Otera has reported that fluorous distannoxanes such as 23, which dissociate to give Lewis acidic species, catalyze transesterifications in or-ganic/fluorous solvent mixtures [8,9]. Although 23 was insoluble in toluene at room temperature, it dissolved at reflux and efficiently promoted the transformation in reaction D of Scheme 4, as well as others. The catalyst precipitated upon cooling, but a fluorous solvent extraction was utilized for recovery (100%). Another thermomorphic fluorous Lewis acid catalyst was developed by Mikami [11]. He found that the ytterbium tris(sulfonamide) 24 could be used for Friedel-Crafts acylations imder homogeneous conditions in CICH2CH2CI at 80 °C, and precipitated upon cooHng to -20 °C (reaction E, Scheme 4). 

The advantages that may justify the additional costs of reflux at the bottom of a solvent extraction tower are illustrated in Figure 6. Minimum reflux is represented by the tie line from / to fe. Maximum reflux would be represented by the line / to the extract layer which would exist for infinite solvent to feed ratio. Practical operation of the equipment will fall between the limits of minimum and maximum reflux, as represented by fy. The operating point for the enriching section of the extraction column is located by an intersection between the lines erE and fy, and the reflux ratio is the ratio of the distances k e /k e (22). 

A flow diagram of an anhydrous phenol solvent extraction plant is shown in Figure 8. Raw distillate is passed through a tower in which it absorbs phenol from the recovery system vapor. The oil is then passed to the treating tower, generally a few sections above the bottom. Anhydrous phenol is introduced at the top of this tower. Phenolic water condensate from the solvent recovery system (about 9.5% phenol) is introduced at the bottom of the tower to effect reflux. A temperature gradient of 10° to 75° F. may be... 

The determination of the exact composition of feed and product streams is also receiving attention. By precision fractionation in the laboratory, often at 100 plus plates and reflux ratios of equal magnitude, narrow boiling fractions are obtained that are further resolved by separation procedures such as azeotropic distillation, extractive distillation, chromatography, solvent extraction, and crystallization. In addition, the instrumental methods of analysis are increasing our information on the composition of complex hydrocarbon fractions. 

Three novel mesostructured tungsten sulfides, designated as MTS-W, MTS-M and MTS-C, were prepared by the condensation reaction of (NH4)2WS4 in the presence of octadecyltrimethylammonium bromide (OTAB) under refluxing conditions in water, methanol and carbon tetrachloride at 373 K, 338 K and 350 K, respectively. The three as-synthesized metal sulfides all have a layered structure with the d-spacing of 31 A, 30 A or 37 A. Partial removal of the organic surfactants from the layer galleries can be achieved by solvent extraction. 

However, solvent extraction has proven to be more effective. When a sample of 1 g MTS-W was dispersed in 50 mL of ethanol and refluxed for 12 hours. Elemental analysis showed that ca. 50% of the organic templates could be removed without any apparent effect on the stability of the mesostrucutre. We have also found that the mesostructured compounds are stable in concentrated HC1 solution. For example, when MTS-W was stirred in a 12M HC1 solution at room temperature for 12 hours, ca. 30% of the organic templates could be removed without collapsing the mesostructure or decomposing the inorganic walls. 

The solvent extraction of rare-earth nitrates into solutions of TBP has been used commercially for the production of high-purity oxides of yttrium, lanthanum, praseodymium and neodymium from various mineral concentrates,39 as well as for the recovery of mixed rare-earth oxides as a byproduct in the manufacture of phosphoric acid from apatite ores.272 273 In both instances, extraction is carried out from concentrated nitrate solutions, and the loaded organic phases are stripped with water. The rare-earth metals are precipitated from the strip liquors in the form of hydroxides or oxalates, both of which can be calcined to the oxides. Since the distribution coefficients (D) for adjacent rare earths are closely similar, mixer—settler assemblies with 50 or more stages operated under conditions of total reflux are necessary to yield products of adequate purity.39... 

Notes. (1) Warming the suspended solid in the solvent may be necessary by removing the porridge to a suitable flask and heating under reflux. Care must be taken if such is the case to supervise this operation carefully as there may be considerable tendency towards bumping . It should also be borne in mind that this batch-extraction process uses open-type vessels and usually large volumes of solvents precautions must therefore be taken in relation to the possible fire and toxic hazards involved in the use of a particular solvent. (2) As a first step, this procedure would involve solvent extraction procedures to divide the multicomponent mixture into acidic, basic and neutral fractions (see above). Subsequently chromatography, fractional crystallisation, etc., would be employed as appropriate. 

Pressurized solvent extraction (PSE), also called pressurized fluid extraction (PEE), accelerated solvent extraction (ASE ), pressurized liquid extraction (PEE), or enhanced solvent extraction (ESE), is a solid-liquid extraction that has been developed as an alternative to conventional extractions such as Soxhlet, maceration, percolation, or reflux. It uses organic solvents at high pressure and temperature to increase the efficiency of the extraction process. Increased temperature decreases the viscosity of the liquid solvent, enhances its diffusivity, and accelerates the extraction kinetics. High pressure keeps the solvent in its liquid state and thus facilitates its penetration into the matrix, resulting in increase extraction speed [30]. 

Removal of extractables from an elastomer or plastic matrix can be accomplished by a variety of techniques, including solvent extraction (e.g., reflux and Soxhlet), supercritical fluid extraction, thermal evolution, etc. Jenke has thoroughly discussed and classified extraction strategies for container closure system components associated with a drug product leachables assessment. His discussion is based on two so-called directives paraphrased as follows ... 

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