Separatory funnel

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Separating funnel in use. The organic phase (yellow, upper phase) has a lower density than the aqueous phase (lower phase). The aqueous phase is being drained into the beaker. Scheidetrichter zwei Phasen brauner Hintergrund.png
Separating funnel in use. The organic phase (yellow, upper phase) has a lower density than the aqueous phase (lower phase). The aqueous phase is being drained into the beaker.

A separatory funnel, also known as a separation funnel, separating funnel, or colloquially sep funnel, is a piece of laboratory glassware used in liquid-liquid extractions to separate (partition) the components of a mixture into two immiscible solvent phases of different densities. [1] Typically, one of the phases will be aqueous, and the other a lipophilic organic solvent such as ether, MTBE, dichloromethane, chloroform, or ethyl acetate. All of these solvents form a clear delineation between the two liquids. [2] The more dense liquid, typically the aqueous phase unless the organic phase is halogenated, sinks to the bottom of the funnel and can be drained out through a valve away from the less dense liquid, which remains in the separatory funnel. [3]

Contents

Description

Two funnels: A - Cone, or Pear-shaped, B - cylindrical. Separatory funnel-diagrams.svg
Two funnels: A - Cone, or Pear-shaped, B - cylindrical.

A separating funnel takes the shape of a cone with a hemispherical end. It has a stopper at the top and stopcock (tap), at the bottom. Separating funnels used in laboratories are typically made from borosilicate glass and their taps are made from glass or PTFE. Typical sizes are between 30 mL and 3 L. In industrial chemistry they can be much larger and for much larger volumes centrifuges are used. The sloping sides are designed to facilitate the identification of the layers. The tap-controlled outlet is designed to drain the liquid out of the funnel. On top of the funnel there is a standard taper joint which fits with a ground glass or Teflon stopper. [4]

To use a separating funnel, the two phases and the mixture to be separated in solution are added through the top with the stopcock at the bottom closed. The funnel is then closed and shaken gently by inverting the funnel multiple times; if the two solutions are mixed together too vigorously emulsions will form. The funnel is then inverted and the stopcock carefully opened to release excess vapor pressure. The separating funnel is set aside to allow for the complete separation of the phases. The top and the bottom stopcock are then opened and the lower phase is released by gravitation. The top must be opened while releasing the lower phase to allow pressure equalization between the inside of the funnel and the atmosphere. When the bottom layer has been removed, the stopcock is closed and the upper layer is poured out through the top into another container.

Theory

The separating funnel relies on the concept of "like dissolves like", which describes the ability of polar solvents to dissolve polar solutes and non-polar solvents to dissolve non-polar solutes. When the separating funnel is agitated, each solute migrates to the solvent (also referred to as "phase") in which it is more soluble.

The solvents normally do not form a unified solution together because they are immiscible. When the funnel is kept stationary after agitation, the liquids form distinct physical layers - lower density liquids will stay above higher density liquids. A mixture of solutes is thus separated into two physically separate solutions, each enriched in different solutes.

The stopcock may be opened after the two phases separate to allow the bottom layer to escape the separator funnel. The top layer may be retained in the separating funnel for further extractions with additional batches of solvent or drained out into a separate vessel for other uses. If it is desired to retain the bottom layer in the separating funnel for further extractions, both layers are taken out separately, and then the former bottom layer is returned to the separating funnel.

Each independent solution can then be extracted again with additional batches of solvent, used for other physical or chemical processes. If the goal was to separate a soluble material from mixture, the solution containing that desired product can sometimes simply be evaporated to leave behind the purified solute. For this reason, it is a practical benefit to use volatile solvents for extracting the desired material from the mixture. [5]

Emulsions

One of the drawbacks of using a separating funnel is emulsions can form easily, and can take a long time to separate once formed. They are often formed while liquids are being mixed in the separating funnel. This can occur when small droplets are suspended in an aqueous solution. If an emulsion is formed, one technique used to separate the liquids is to slowly swirl the solution in the separating funnel. If the emulsion is not separated by this process, a small amount of saturated saline solution is added ("salting out"). [6]

Research is being done on alternative, more efficient techniques, mostly utilizing stir bars (stirrer bars) to decrease or even eliminate the chance of emulsification, thus decreasing the amount of waiting time. [7]

Safety concerns

The largest risk when using a separating funnel is that of pressure build-up. Pressure accumulates during mixing if a gas evolving reaction or physical change occurs. This problem can be easily handled by simply opening the stopper at the top of the funnel routinely while mixing. More standard procedure is to invert the separating funnel upside down, and open the stopcock to release the pressure, a step done repeatedly known as 'venting'. This should be done with the tip of the funnel pointed away from the body. [8]

See also

Related Research Articles

In chemical analysis, chromatography is a laboratory technique for the separation of a mixture into its components. The mixture is dissolved in a fluid solvent called the mobile phase, which carries it through a system on which a material called the stationary phase is fixed. Because the different constituents of the mixture tend to have different affinities for the stationary phase and are retained for different lengths of time depending on their interactions with its surface sites, the constituents travel at different apparent velocities in the mobile fluid, causing them to separate. The separation is based on the differential partitioning between the mobile and the stationary phases. Subtle differences in a compound's partition coefficient result in differential retention on the stationary phase and thus affect the separation.

<span class="mw-page-title-main">Phase (matter)</span> Region of uniform physical properties

In the physical sciences, a phase is a region of material that is chemically uniform, physically distinct, and (often) mechanically separable. In a system consisting of ice and water in a glass jar, the ice cubes are one phase, the water is a second phase, and the humid air is a third phase over the ice and water. The glass of the jar is another separate phase.

<span class="mw-page-title-main">Solution (chemistry)</span> Homogeneous mixture of a solute and a solvent

In chemistry, a solution is a special type of homogeneous mixture composed of two or more substances. In such a mixture, a solute is a substance dissolved in another substance, known as a solvent. If the attractive forces between the solvent and solute particles are greater than the attractive forces holding the solute particles together, the solvent particles pull the solute particles apart and surround them. These surrounded solute particles then move away from the solid solute and out into the solution. The mixing process of a solution happens at a scale where the effects of chemical polarity are involved, resulting in interactions that are specific to solvation. The solution usually has the state of the solvent when the solvent is the larger fraction of the mixture, as is commonly the case. One important parameter of a solution is the concentration, which is a measure of the amount of solute in a given amount of solution or solvent. The term "aqueous solution" is used when one of the solvents is water.

<span class="mw-page-title-main">Solvent</span> Substance dissolving a solute resulting in a solution

A solvent is a substance that dissolves a solute, resulting in a solution. A solvent is usually a liquid but can also be a solid, a gas, or a supercritical fluid. Water is a solvent for polar molecules, and the most common solvent used by living things; all the ions and proteins in a cell are dissolved in water within the cell.

<span class="mw-page-title-main">Solubility</span> Capacity of a substance to dissolve in a solvent in a homogeneous way

In chemistry, solubility is the ability of a substance, the solute, to form a solution with another substance, the solvent. Insolubility is the opposite property, the inability of the solute to form such a solution.

<span class="mw-page-title-main">High-performance liquid chromatography</span> Technique in analytical chemistry

High-performance liquid chromatography (HPLC), formerly referred to as high-pressure liquid chromatography, is a technique in analytical chemistry used to separate, identify, and quantify specific components in mixtures. The mixtures can originate from food, chemicals, pharmaceuticals, biological, environmental and agriculture, etc, which have been dissolved into liquid solutions.

<span class="mw-page-title-main">Paper chromatography</span> Separation of coloured chemicals on paper

Paper chromatography is an analytical method used to separate coloured chemicals or substances. It is now primarily used as a teaching tool, having been replaced in the laboratory by other chromatography methods such as thin-layer chromatography (TLC).

<span class="mw-page-title-main">Column chromatography</span> Method to isolate a compound in a mixture

Column chromatography in chemistry is a chromatography method used to isolate a single chemical compound from a mixture. Chromatography is able to separate substances based on differential adsorption of compounds to the adsorbent; compounds move through the column at different rates, allowing them to be separated into fractions. The technique is widely applicable, as many different adsorbents can be used with a wide range of solvents. The technique can be used on scales from micrograms up to kilograms. The main advantage of column chromatography is the relatively low cost and disposability of the stationary phase used in the process. The latter prevents cross-contamination and stationary phase degradation due to recycling. Column chromatography can be done using gravity to move the solvent, or using compressed gas to push the solvent through the column.

<span class="mw-page-title-main">Liquid–liquid extraction</span> Method to separate compounds or metal complexes

Liquid–liquid extraction, also known as solvent extraction and partitioning, is a method to separate compounds or metal complexes, based on their relative solubilities in two different immiscible liquids, usually water (polar) and an organic solvent (non-polar). There is a net transfer of one or more species from one liquid into another liquid phase, generally from aqueous to organic. The transfer is driven by chemical potential, i.e. once the transfer is complete, the overall system of chemical components that make up the solutes and the solvents are in a more stable configuration. The solvent that is enriched in solute(s) is called extract. The feed solution that is depleted in solute(s) is called the raffinate. Liquid-liquid extraction is a basic technique in chemical laboratories, where it is performed using a variety of apparatus, from separatory funnels to countercurrent distribution equipment called as mixer settlers. This type of process is commonly performed after a chemical reaction as part of the work-up, often including an acidic work-up.

<span class="mw-page-title-main">Solid-phase extraction</span> Process to separate compounds by properties

Solid-phase extraction (SPE) is a solid-liquid extractive technique, by which compounds that are dissolved or suspended in a liquid mixture are separated, isolated or purified, from other compounds in this mixture, according to their physical and chemical properties. Analytical laboratories use solid phase extraction to concentrate and purify samples for analysis. Solid phase extraction can be used to isolate analytes of interest from a wide variety of matrices, including urine, blood, water, beverages, soil, and animal tissue.

Aqueous biphasic systems (ABS) or aqueous two-phase systems (ATPS) are clean alternatives for traditional organic-water solvent extraction systems.

A multiphasic liquid is a mixture consisting of more than two immiscible liquid phases. Biphasic mixtures consisting of two immiscible phases are very common and usually consist of an organic solvent and an aqueous phase.

Countercurrent distribution is an analytical chemistry technique which was developed by Lyman C. Craig in the 1940s. Countercurrent distribution is a separation process that is founded on the principles of liquid–liquid extraction where a chemical compound is distributed (partitioned) between two immiscible liquid phases according to its relative solubility in the two phases. The simplest form of liquid-liquid extraction is the partitioning of a mixture of compounds between two immiscible liquid phases in a separatory funnel. This occurs in five steps: 1) preparation of the separatory funnel with the two phase solvent system, 2) introduction of the compound mixture into the separatory funnel, 3) vigorous shaking of the separatory funnel to mix the two layers and allow for mass transfer of compounds in and out of the phases, 4) The contents of the separatory funnel are allowed to settle back into two distinct phases and 5) the two phases are separated from each other by draining out the bottom phase. If a compound is insoluble in the lower phase it will distribute into the upper phase and stay in the separatory funnel. If a compound is insoluble in the upper phase it will distribute into the lower phase and be removed from the separatory funnel. If the mixture contains one or more compounds that are soluble in the upper phase and one or more compounds that are soluble in the lower phase, then an extraction has occurred. Often, an individual compound is soluble to a certain extent in both phases and the extraction is, therefore, incomplete. The relative solubility of a compound in two phases is known as the partition coefficient.

<span class="mw-page-title-main">Mixer-settler</span>

Mixer settlers are a class of mineral process equipment used in the solvent extraction process. A mixer settler consists of a first stage that mixes the phases together followed by a quiescent settling stage that allows the phases to separate by gravity.

Acid–base extraction is a subclass of liquid–liquid extractions and involves the separation of chemical species from other acidic or basic compounds. It is typically performed during the work-up step following a chemical synthesis to purify crude compounds and results in the product being largely free of acidic or basic impurities. A separatory funnel is commonly used to perform an acid-base extraction.

In chemistry, work-up refers to the series of manipulations required to isolate and purify the product(s) of a chemical reaction. The term is used colloquially to refer to these manipulations, which may include:

Partition chromatography theory and practice was introduced through the work and publications of Archer Martin and Richard Laurence Millington Synge during the 1940s. They would later receive the 1952 Nobel Prize in Chemistry "for their invention of partition chromatography".

<span class="mw-page-title-main">Extraction (chemistry)</span> Separation of a desired substance from other substances in the sample

Extraction in chemistry is a separation process consisting of the separation of a substance from a matrix. The distribution of a solute between two phases is an equilibrium condition described by partition theory. This is based on exactly how the analyte moves from the initial solvent into the extracting solvent. The term washing may also be used to refer to an extraction in which impurities are extracted from the solvent containing the desired compound.

<span class="mw-page-title-main">Centrifugal extractor</span>

A centrifugal extractor—also known as a centrifugal contactor or annular centrifugal contactor—uses the rotation of the rotor inside a centrifuge to mix two immiscible liquids outside the rotor and to separate the liquids in the field of gravity inside the rotor. This way, a centrifugal extractor generates a continuous extraction from one liquid phase into another liquid phase.

Solvent impregnated resins (SIRs) are commercially available (macro)porous resins impregnated with a solvent/an extractant. In this approach, a liquid extractant is contained within the pores of (adsorption) particles. Usually, the extractant is an organic liquid. Its purpose is to extract one or more dissolved components from a surrounding aqueous environment. The basic principle combines adsorption, chromatography and liquid-liquid extraction.

References

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  2. "Archived copy" (PDF). Archived from the original (PDF) on 2012-04-25. Retrieved 2011-11-17.{{cite web}}: CS1 maint: archived copy as title (link)
  3. Padìas, Anne B. (2011). Making the Connections2: A How-To Guide for Organic Chemistry Lab Techniques.Plymouth, Michigan: Hayden-McNeil Publishing, p. 129.
  4. "Chemistry and Biochemistry". 2018-09-06.
  5. "Recrystallization Technique - [www.rhodium.ws]".
  6. "Separatory Funnel module". Archived from the original on 2012-03-14. Retrieved 2016-12-12.
  7. Bye, Ragnar; Agasöster, Tone; Åsheim, Arne (1993). "A novel and fast extraction technique as an alternative to conventional separatory funnels". Fresenius' Journal of Analytical Chemistry. 345 (6): 411–414. doi:10.1007/BF00325616. S2CID   97042736.
  8. Fessenden, J., Joan S. Fessenden, Patty Feist. Organic Laboratory Techniques, 3rd Edition, 2001. Pacific Grove, California: Brooks Cole Publishing, p. 59.