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Recrystallization

Introduction
Products from an organic reaction are seldom

obtained in pure state directly from the reaction mixture. Most organic compounds are more soluble in hot solvents. Impurities present will have different solubilities from those of the desired compounds. Solvent must be properly selected.

1. Steps in recrystallization of organic compounds


Dissolve the impure material in a minimum amount of

solvent Filter the hot solution Allow the substance to cool and deposit the crystals of the compound Filter the compounds from the solution Wash the crystals with a little cold solvent Dry the crystals

2. Properties of a solvent to be well suited for recrystallizing


Dissolve a moderate quantity of the substance to be

purified at elevated temperature Not react with the substance to be purified Dissolve impurities readily at low temperature or not dissolve them at all Be readily removable from the purified product Inexpensive

3. Solubility of acetanilide in hot and cold water. Why is water a good solvent for recrystallization of acetanilide?

HOT WATER
5.5g/ 100 mL @ 100 degrees

COLD WATER
0.53g/ 100 mL @ 0 degrees

Water is a good solvent for recrystallization of acetanilide because at high temps, acetinalide dissolves in water readily but is not very soluble at low temps.

4.Why is fluted paper used in the filtration process?


A fluted filter paper is used to increase the surface area

of the filter paper and make the filtration more efficient.

The fluting creates gaps between the filter paper and the funnel in which it is resting. These gaps provide channels for the solvent to flow through after it passes through the filter paper, thus greatly increasing the speed of solvent flow through the paper.

Objectives
To be able to purify the crude sample through

recrystallization

Procedure:
Weigh about 1.0g sample in a 100mL beaker and pour 25mL

of water. Then heat the contents with stirring.

When residue has gone into solution, remove the flame

and add about 0.5g of charcoal.

Continue heating with vigorous stirring and bring the

solution to a boil.

Then filter through a hot stemless funnel fitted with a

fluted filter paper without delay.

Divide the filtrate to two equal amounts in separate 50mL

beaker. Cover one beaker with watch glass and set it aside to cool slowly.

Place other beaker in an ice water mixture and stir rapidly while cooling.

Data
Weight of container 52.03g Weight of filter paper Weight of filter paper + crystallized sample Weight of crystallized sample 0.75g 1.15g

Weight of 53.03g container + sample

Weight of sample

1g

0.40

Percentage yield of purified crystals:

%yield = weight of pure product x 100 weight of crude sample = 0.4g x 100 1g = 40%

Observations
Pinkish color diminished as charcoal was added
Smaller crystals are formed in rapid recrystallization

process than slow recrystallization process Faster crystallization in low temperature.

1.) Why must the hot solution be filtered without delay?


Hot solution must be filtered without delay because if

there is delay, the temperature would drop. This will allow crystallization of the organic content in the hot solution. Crystals would then be filtered with the impurities present.

2.) If charcoal and sugar were the main impurities present in the crude sample, would recrystallization from water be a good method of purification? Why?
If charcoal and sugar were the main impurities

present, water would be a good method of purification. Charcoal can be filtered easily since it is not soluble with water. Thus, it is now separated from sugar and the organic content. When the pure sample crystallizes, sugar would still be left dissolved in water.

3. Why can water-ethanol but not water-hexane be used as a solvent?


Water-ethanol can be used as a solvent because water

and ethanol are both polar substances water-hexane one is polar and the other is nonpolar.

4. How do you account for the formation of crystals different sizes in slow and rapid crystallizing process?
In rapid crystallizing process- the crystals are smaller

and finer. It is because of the stirring, the particles are not compact. The time it took for the crystals to crystallize was short because of the temperature.
In slow crystallizing process- the crystals are greater in

terms of size because they are undisturbed.

5. List the chief reasons why a process of crystallization would not give a yield of 100%?
There is always some dissolved chemical left in the solution, even in small amounts
Transferring of crystals on different containers

may lessen the amount Some may evaporate

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