Separation of a Mixture by Extraction: Crystallization

Objectives

Separation of a mixture containing acidic and a neutral compounds extraction. Purification of the solid component crystallization. Identify those components from its spectrum and its melting point.

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IR

Terms

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Separation Extraction Crystallization

 To separate a components from other species that would interfere in the analysis .Separation Why we need to separate mixture??  To isolate or concentrate components from a mixture.

Methods of Separation     Extraction Crystallization Distillation Chromatography .

Extraction  Extraction: Transfer of a solute from one phase to another. .

supercritical fluid).Useful for the isolation and purification of naturally occurring sources.Types of Extraction   Can use most any combination of phases (solid. . Solid – Liquid . gas. liquid.

.Extraction  Making coffee is an example for extraction.

Like dissolves like So ideally. .Depend on solubility properties of components. the extracting solvent should be similar to the solute.Extraction  Liquid – Liquid .More common method .

Typically aqueous / organic solvent combos . .Extraction  We will use two immiscible liquids.

Toluene.Dichloromethane. Hexane Organic solvents more dense than water. .Extraction   Organic solvents less dense than water. .Diethyl ether. . Chloroform and Carbon tetrachloride.

It should readily dissolve the compound to be extracted. Easily separated from the compound. It should dissolve little or none of the unwanted compounds / impurities. Should not undergo any reaction with the compounds. .Qualities of the Solvent      Immiscible with other solvent.

Extraction .

Extraction  Equilibrium constant for this partitioning is K (partition coefficient or distribution coefficient) [S]2 K= [S]1 .

Extraction   Chemically Inert Extraction. Chemically Active Extraction. .

.Chemically Active Extraction   A reagent that reacts chemically with the substance to be extracted. Solubility property changes after the reaction.

Chemically Active Extraction COOH 10 % NaOH Soluble in Diethyl ether & Insoluble in Water 10 % NaOH COONa No Reaction & Stay in ether layer Soluble in Water & Stay in aqueous layer .

Chemically Active Extraction CH2NH2 NO2 10 % HCl Soluble in Diethyl ether & Insoluble in Water 10 % HCl CH2NH3+ No Reaction & Stay in ether layer Soluble in Water & Stay in aqueous layer .

Procedure for Today’s Lab     Get your unknown mixture. Add 15 mL more of diethyl ether and rinse the beaker. stir slowly to dissolve the mixture. . Add 30 mL of diethyl ether. Transfer all your unknown into a 100 mL beaker and find the mass of your unknown.

Repeat these steps two times using fresh 5 % sodium bicarbonate solution. Separate the two layers. Pool all the aqueous layers i.Procedure for Today’s Lab      Add 15 mL of 5 % sodium bicarbonate to the ether solution. sodium bicarbonate solution .e. Swirl the separatory funnel first and shake gently.

If it is not acidic enough.Recovery of Acidic Compound     Cool all the aqueous extracts for about 5 minutes in an ice – water bath. . add 1 mL of acid more. Add 3 mL of concentrated hydrochloric acid. Test the acidity of this solution with blue litmus paper (TURN RED).

of anhydrous sodium sulfate over the cotton plug and transfer all the ether layer carefully through the neck. Keep a fresh and dry Erlenmeyer Flask under the funnel.Recovery of Neutral Compound    Place a small piece of cotton in a dry glass funnel. Add 5g. .

Cork the flask tightly once all the ether has gone. .Recovery of Neutral Compound    Rinse the separatory funnel with 5 mL of ether pour into drying agent. Add few boiling chips and keep on a steam bath.

1.Recrystallization  It’s a technique to purify the solid organic compounds. Liquid diffusion 4. Slow evaporation 2. Use of seed crystal . Slow cooling 3.

  Easily removed after crystallization. Should not react with substance being purified. Insoluble in hot solvent or high soluble in cold solvent. Low in cold solvent  Impurities: 1. .Recrystallization  Compound to be purified: 1. Moderate or high solubility in hot solvent 2.

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Slowly cool the solution to room temperature. Filter the solution when it is hot. wash it with minimum amount of cold solvent.Procedure for Recrystallization      Dissolve all the acidic compound in minimum amount of hot solvent. Filter the crystals. then keep on ice bath. Allow to dry on its own. .

Find the amount of neutral compound you recovered from the mixture.Characterization   Neutral Compound 1. Obtain its IR spectrum. Acidic Compound 1. Find its melting point. Calculate the % of recovery. 2. . 2.

.Changes  Use Blue Litmus instead of Congo Red.

Notes   Do not forget to add the boiling chips when you evaporate diethyl ether. Vent the separatory funnel very often to relieve the developed pressure. .

Caution NO FLAMES IN LAB TODAY .

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