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PHRM 309 Presentation Topic: Liquid-liquid extraction

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Group members:
Shahriar Rahman (ID: 2006-1-70-008) Thamina Hossain Pinky (ID: 2006-1-70-007) Farzana Khan (ID: 2005-3-70-030) Nazrana Parvin (ID: 2005-2-70-096) Samiha Raisa Karim (ID:)

What is liquid-liquid extraction?

Liquid-liquid extraction is a versatile and dependable separation technique wherein an aqueous solution is usually brought into contact with another organic solvent exclusively immiscible with the former so as to affect legitimate and actual transfer of either one or more solutes into the latter.

The Nernst Distribution Law


The Nernst Distribution Law or the Partition Law states that a neutral species will distribute between two immiscible solvent with a constant ratio of concentration. Kp=Co/Caq Kp is the distribution constant or the partition coefficient or partition ratio (solvent-to-feed ratio) Co is the concentration of the analyte in the organic phase (Solvent) Caq is the concentration of the analyte in the aqueous phase (Feed)

Limitations of Partition Law


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is solely applicable to very dilute solutions. does not hold good when the distributing substances encounter association or distribution in either phases.

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In liquid-liquid extractions the following two aspects are very crucial and important:
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Error due to the volume change: There are a number of


procedure have been adopted to avoid error due to the volume change incurred thereby:

Measure the volume of the phase employed for the analysis and incorporate this volume in the calculations. Separate the phase quantitatively and subsequently dilute to a known volume, Separate the phase quantitatively and make use of the entire volume in the remaining steps of the ongoing analysis, and Carry a marker substance through the extraction to automatically compensate for volume changes.

In liquid-liquid extractions the following two aspects are very crucial and important:
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Effectiveness of an extraction: Based on the appropriate partition coefficient of an immiscible solvent pair it is possible to calculate the effectiveness of an extraction. Let us assume that x moles of solute present initially in a volume V2 of Solvent b. Now, this particular sample undergoes extraction with a volume V1 of Solvent a and subsequently y moles of compound are left in V2 at equilibrium. Substituting these values in partition coefficient equation :

Continuation
The fraction extracted is absolutely independent of the initial solute concentration. So, the fraction left unextracted after n extraction may be given by the following expression,

Solvent selection criteria


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Miscibility: The two solvents should be immiscible with each other. We cannot use solvents that are miscible with water e.g. acetone, acetonitrile, pyridine etc. Density: Large density differences between two solvents is favoured for good extraction process. More dense solvent will form the lower layer and less dense solvents will form the upper layer with water when mixed with water e.g. ethyl ether has a density of 0.7133 g/mL at 20 and would constitute the upper phase when combined with water which has a density of 0.9982 g/mL. Solubility: Although immiscible solvents may form two visibly distinct phases when mixed together, they are often somewhat soluble in each other and become mutually saturated when mixed together e.g. 1.6% of the dichloromethane is soluble in water . Conversely , water is 0.24% soluble in dichloromethane .

Factors influencing solvent extraction


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A number of factors exert a positive influence on solvent extraction: Effect of temperature Effect of pH on extraction Effect of ion-pair formation Effect of synergistic extraction

Emulsion problem
Emulsion may be defined as a dispersed system containing at least two immiscible liquid phases. Emulsion formation is a serious problem encountered during the extraction of drugs from biological as well as pharmaceutical formulations. Emulsion formation makes the separation of the two phases difficult.

Factors responsible for slowcoalescence of an emulsion


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Finely divided powders, albumin, gelatin and natural gums have a tendency to coat the droplets formed in an emulsion which ultimately prevent them from coalescing. Surfactants decrease the interfacial tension between the two immiscible liquids which help in stabilizing an emulsion. Ionic species may get absorbed at the interface of two immiscible layers resulting in the formation of a net charge on the droplets. As the droplets attain a similar charge they repel each other preventing coalescence.

Substances which stabilize emulsions

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Some natural and synthetic substances are used in the formulation of drugs which are found to stabilize emulsions by: Coating the tablets e.g. starch, acacia. silica, gelatin, finely divided talc. Minimizing the interfacial tension e.g. mono& di-glycerides, stearates, sorbitan monoleate.

Ways to prevent emulsion formation


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Cautious & gentle agitation besides employing a sufficiently large liquid-liquid interface to obtain a good extraction. Removal of any finely divided insoluble material in a liquid phase must be done by filtration before performing extraction. Using solvent pairs having a large density difference & a high interfacial tension. When performing extraction from water always ensure not to work at pH extremes particularly at high/basic pH to avoid emulsification. Anion exchangers, alumina or silica gel are used in case of acute emulsion problems.

Breaking of an emulsion (coalescence)


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Mechanical means Centrifugation Addition of monovalent & divalent ions Ethanol or higher alcohol Sudden cooling of emulsion (thermal shock) Altering the ratio of solvents Silicone defoaming agent Thin-bed of an adsorbent

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