ACTIVITY #5: PURIFICATION BY RECRYSTALLIZATION

OBJECTIVE

 To be able to know the advantages and disadvantages of using Recrystallization in purification of
substances.

THEORETICAL BACKGROUND
Recrystallization, also known as fractional crystallization, is a procedure for purifying an impure
compound in a solvent. The method of purification is based on the principle that the solubility of most
solids increases with increased temperature. This means that as temperature increases, the amount of
solute that can be dissolved in a solvent increases. The slower the rate of cooling, the larger the crystals
are that form.

The disadvantage of recrystallization is that it takes a long time. Also, it is very important that the proper
solvent is used. This can only be determined by trial and error, based on predictions and observations. The
solution must be soluble at high temperatures and insoluble at low temperatures. The advantage or
recrystallization is that, when carried out correctly, it is a very effective way of obtaining a pure sample of
some product, or precipitate.

PROCEDURE
A gram of impure acetanilide was placed in an Erlenmeyer flask. 40 ml of water and a small amount of
decolorizing activated charcoal was added into the flask and was boiled for 2-3 minutes. After, a fluted
filter paper on a funnel was placed on another Erlenmeyer flask and 20 ml of heated water was poured
with the purpose of heating the funnel and filter paper. The solution was poured hot through the funnel
fitted with the fluted filter. Flask was set aside to cool slowly and placed in an ice bath. After
crystallization, the crystals were collected and left to dry and were weighed
 Conclusions and recommendations

Recrystallization is another method used to purify a solid substance. It is a procedure for purifying an
impure compound in a solvent. The method of purification is based on the principle that the solubility of
most solids increases with increased temperature. In this experiment, impure acetanilide was used and has
gone into solution. The crystals of the flask placed in the ice water are smaller compared to the other one.

Nonetheless, it is recommended to use the methods cautiously to avoid incorrect results. Recrystallization,
boiling the solution is important so the impure substance will dissolve faster and will not crystallize
immediately.

APPENDICES

DEFINITION OF TERMS

Acetanilide crystals- An odorless solid chemical of leaf or flake-like appearance.

Recrystallization- A technique used to purify chemicals. By dissolving both impurities and a compound
in an appropriate solvent, either the desired compound or impurities can be removed from the solution

Crystallization - Refers to the solid-liquid separation and purification technique in which mass transfer
occurs from the liquid solution to a pure solid crystalline phase.

COMPUTATIONS

𝑝𝑢𝑟𝑒 𝑎𝑐𝑒𝑡𝑎𝑛𝑖𝑙𝑖𝑑𝑒 𝑐𝑟𝑦𝑠𝑡𝑎𝑙𝑠

%𝑃𝑢𝑟𝑖𝑡𝑦 = × 100%
𝑤𝑡 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒, 𝑖𝑚𝑝𝑢𝑟𝑒 𝑎𝑐𝑒𝑡𝑎𝑛𝑖𝑙𝑖𝑑𝑒

Weight of Filter paper – 1.0 gram

Weight of pure acetanilide crystals: 1.1 grams – 1 gram = 0.1 grams

0.1
% 𝑃𝑢𝑟𝑖𝑡𝑦 = × 100%
1𝑔

= 10%
 ANSWERS TO QUESTIONS

1. List the chief reasons why a recrystallization process would not give a yield of 100%
The yield for a recrystallization can never be 100%. because while the chilled solvent is saturated and
should release some crystals, at least some of your desired material will remain dissolved in the cold
solvent and will be lost when the crystals and solvent are separated. The primary necessary source of
mass loss is to the solvent. Obviously additional mass will be lost to physical handling, and some of
the lost mass is simply the impurities that you wanted to lose. (But normally the mass of impurities is
only a few percent or less.)

2. How may Crystallization be induced?

These are a few ways of inducing crystallization:
 Put in a crystal of the solute. Sometimes any small particle, or even dust, will do the trick.
 Scratch the glass container (on the inside)
 A firm knock or shake

3. Why is it important to minimize evaporation during the filtration of a hot solution?

Minimizing evaporation during the filtration of the hot solution is needed in order to avoid loss of
some crystals. Evaporation may cause early recrystallization on the filter paper, and so the crystals
may be lost among the insoluble impurities on the filter paper.
4. What properties of activated charcoal make it a good absorbing agent?
Charcoal (also activated charcoal) is known to adsorb a huge variety of substances including a variety
of paints, dyes and many different kinds of ions. Moreover, the amount of adsorption at normal
pressure and temperature is high.

Charcoal is also known to be porous, it has a great influence on its adsorbtion properties. Thus, the
ability of charcoal to retain soil water is widely attributed to its porosity. This expanded surface is due
to the fact that charcoal particles have thousands of crevices, pits, grooves, and holes which, when
opened out, make quite a large surface area.

5. What are the characteristics of a solvent used for recrystallization?

Characteristics of a Good Recrystallization Solvent:
1. The recrystallization solvent should NOT dissolve the substance to be purified at
room temperature, but it should dissolve it well at the solvent’s boiling point
 2. The solvent should dissolve soluble impurities well at room temperature.
3. The solvent should not dissolve insoluble impurities even at the solvent’s boiling
point. These insoluble impurities can then be removed by gravity filtration.
4. The solvent must not react with the substance to be purified.

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