Liquid-solid extraction shake flask

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... 

Conventional liquid-solid extraction, in the form of shake-flask extraction, is carried out by placing a soil sample into a suitable glass container, adding a suitable organic solvent, and then agitating or shaking. 

Mineral Oil Hydraulic Fluids. Methods are available for analysis of the hydrocarbon components of mineral oil hydraulic fluids (predominantly straight and branched chain alkanes) in environmental samples. Some of these methods are summarized in Table 6-3. In general, water and sediment samples are extracted with a suitable solvent in a Soxhlet extractor (for solid samples) or in separatory funnel or shake flask (for liquid samples) (Bates et al. 1984 Peterman et al. 1980). The extract is cleaned up on silica gel or Florisil columns using a nonpolar solvent to elute the nonpolar alkanes. Analysis is usually performed by GC/MS (Bates et al. 1984 Kawamura and Kaplan 1983 Peterman et al. 1980). Method performance has not been reported, although 82% recovery of aliphatic hydrocarbons was reported for rainwater (Kawamura and Kaplan 1983). 

The synthesis of 6-hydroxy fluvastatin with M. rammaniana DSM 62752 gave high conversion (>95 %) in shake flask culture on 400 mL scale with 0.1 g L of fluvastatin as well as on 22 L scale in a Wave bioreactor-fed batch process at a final substrate concentration of 0.4 g L Instead of the partial purification by a second solid-phase extraction described above, 6-hydroxy fluvastatin can be obtained in high purity ( 95 %) by, for example, preparative medium-pressure liquid chromatography (MPLC) on RP18 silica gel. ... 

To 50g of soil (as sampled, recoveries of Oxamyl are constant for moisture contents of up to at least 30%) contained in a 450g wide-necked jar fitted with a ground-glass stopper, add 50g of anhydrous sodium sulphate and 200ml of acetone-dichloromethane solvent. Shake orbitally for 4h, ensuring that all the solids are kept in suspension. Allow to settle, and remove a 100ml aliquot of the supernatant liquid by pipette. Evaporate this extract just to dryness in a 250ml round-bottomed flask fitted to a rotary evaporator. 

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. 

Add 30 mL of alcohol if the sample is liquid, or 23 mL of alcohol and 7 mL of glycerin if the sample is solid, followed by 3 mL of a 9 10 potassium hydroxide solution. Reflux under an all-glass condenser for 30 min. Cool the solution, add 30 mL of water, and transfer into a separator. Add 2 g of finely powdered sodium sulfate. Extract by shaking for 2 min with one 150-mL portion of ether and if an emulsion forms, with three additional 25-mL portions of ether. Combine the ether extracts, if necessary, and wash by swirling gently with 50 mL of water. Wash more vigorously with three additional 50-mL portions of water. Transfer the washed ether extract into a 250-mL volumetric flask, and add ether to volume. 

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