Liezl Mae A.

Sermense BS Biology I

Experiment 3: Recrystallization and Melting Point Determination

Post-Laboratory Report

Post-lab Questions:
1. Explain the principles behind recrystallization. How does it remove impurities from
a solid?
2. What criteria should be considered in choosing a solvent for recrystallization?
3. How does the rate of cooling (after addition of hot solvent) affect crystal growth?
4. Enumerate techniques that can help prevent premature recrystallization. Explain
each one. What is the consequence of premature recrystallization?
5. A difficulty often encountered is the failure of the solute to recrystallize. Explain why
this might happen. What steps can be done to induce crystallization if this
happens?
6. Why should you never use a beaker for recrystallization?
7. Why is it important not to add too much solvent during filtration?
8. Why is it not advisable to dry samples in an oven?
9. What is the effect of impurities on the melting point of a sample?
10. Explain why the following steps are done:
a. Adding boiling chips to the oil bath
b. Addition of charcoal during recrystallization
c. Using fluted filter paper
d. Pre-heating or using a stemless/short-stemmed funnel
e. Placing a small piece of wire between the funnel and the flask during filtration
f. Pulverizing the sample for melting-point determination
g. Stirring the oil bath in melting-point determination

11. A mixture containing 2.0 g of A and 8.0 g of B is to be separated and the

components purified by a single crystallization using 100 mL of solvent. Their
solubilities (g/ 100 mL) are given in the table below:

A B
SOLVENT Cold Hot Cold Hot
Ethanol 0.5 10.0 5.0 20.0
Acetone 5.0 20.0 0.1 8.0
Water 0.6 15.0 0.5 10.0

a. What solvent would you choose?

 b. Given your answer in (a), what would be the % purity of A and B after one
crystallization?
12. A mixture of three compounds A, B, and C is to be separated and purified by
crystallization. Their solubilities in g/100 mL ethanol are given below:
SOLVENT A B C
Cold 1.05 5.6 4.2
Hot 20.5 2.3 3.5

a. If a mixture containing 4.0 g each of A, B, and C is recrystallized from 100 mL

ethanol, which compound would be obtained pure?
b. If the filtrate from (a) is evaporated to 50 mL, which of the compound(s) will
separate upon cooling? What is its purity?

Answers to Post-lab Questions:

1. Also termed as fractional crystallization, recrystallization is a process for an

impure compound’s purification in a solvent. It is said to be the primary method for
purifying solid, nonvolatile organic compounds. Its method is based on the principle
that the amount of solute that can be dissolved by a solvent is greatly reliant on
temperature. A direct proportionality is observed within the relationship of solubility
and temperature such that the solubility of most solids increases with increased
temperature.

In fact, in recrystallization, a solution is created by dissolving a solute in a solvent at

or near its boiling point. This would entail that, with the increased solubility of the solid,
lesser quantity of the hot solvent is needed than when the solvent is in room
temperature. Employing a filtration, insoluble impurities are taken out, and the solid
evaporated to produce the solid compound. For colored impurities, the addition of
activated charcoal is done. Both types of impurities remain in the filter paper after
filtration.

However, impurities can also be soluble, in which case, a solubility test is done from
which a suitable solvent is chosen. A series of steps similar to that taken in the
experiment (right after the initial filtration) is done. The solution is heated near its
boiling point, stirring vigorously, and then allowing it to cool. To further promote the
formation of crystals, the solution is dunked in an ice bath, after which, it is filtered
once more and the crystals rinsed. Impurities ought to be washed away from the
crystals at this point and only the pure solid will remain in the paper.

2. in choosing the most suitable solvent with which to dissolve the impure compound,
a solubility test must be conducted. Generally, the criteria for choosing the perfect
solvent should include: high temperature coefficient, ability to dissolve impurities
readily or not at all, decreased reactivity with solute, nonflammable yet volatile.
High temperature coefficient ensures that the solvent wouldn’t dissolve the compound
at low temperature, while still being able to dissolve it at high temperatures.

Secondly, if the solvent dissolves the impurities readily, the impurities will remain
dissolved in the solvent. In contrast, if the opposite were true and the impurities remain
undissolved, gravity filtration can be more easily conducted.

It is also important that the solvent would not react with the solute as recrystallization
should not and does not chemically alter a molecule.

Solvents with low boiling points can be easily evaporated from the resultant crystals.

3. in crystal formation, the rate of cooling can also affect the outcome. With the gradual
cooling of solution, it becomes saturated with the desired compound as its solubility
decreases. The slow cooling with minimal interruption grants the solution time to be
saturated on its pure compound. Allowing the solution to sit in a cold bath promotes
the formation of crystals that are free from impurities. The slower the formation of the
crystals, the purer it is bound to come out.

Of course, doing the same steps but in a faster rate would not warrant the same
results.

4. premature recrystallization may be prevented by following 2 techniques: the filtration

set-up must be kept warm, and the hot solution should be poured incrementally.

Keeping the filtration set-up constantly warm would prevent the hot solution from
immediately cooling down as it runs through the filter, enabling crystallization to occur.
Warming the funnel and filter paper helps prevent crystallization from occurring as no
sudden drop pf temperature would then be expected when pouring the solution. This
also explains why the receiving flask is heated beforehand (with the addition of hot
water). Produced vapors keeps the flask and funnel warm.

Pouring the hot solution in small amounts also prevents premature recrystallization
since it lessens the time by which the solution sits in filter, preventing it to cool and
crystallize. If there are already crystals, adding hot water/solution immediately
dissolves this.

5. Too much solvent is perhaps one of the most common reasons for failure to extract
enough crystals by the end of the process. Adding too much solvent would result in a
diluted solution that would make it harder for the crystals to form. A simple preventative
measure for this is to only add the recommended amount of solvent or to only add
small amounts of water when rinsing. For solute to recrystallize, evaporation of the
solvent until enough liquid is left can be done.

The addition of ‘crystal seeds’ is also recommended to induce nucleation. A stirring

rod could also be used to scratch the inner surface of the flask from where the solution
is being poured. This provides a small speck of glass upon which nucleation might
occur. Placing the flask containing the solution in an ice bath also drastically decreases
the temperature, allowing for saturation to occur.
6. Beakers, unlike Erlenmeyer flasks, have a larger surface area that allows for more
efficient heat travel and escape. This is proven to be counterproductive when aiming
to induce crystal formation. An uneven recrystallization process may also be expected
of this, even leaving crystal deposits in rings around the beaker.

7. The principle of crystal formation can be greatly likened to the formation of

precipitates, and to favor precipitate formation, liquid should be added in least amount
possible. Failure to do so would only dissolve the forming clump. Likewise, it is of
essence to only add a minimal amount of solvent during filtration since adding too
much would certainly affect and even hinder the recrystallization process. A diluted
solution is not favorable for crystal growth.

8. Oven drying isn’t advisable when drying the crystals as it might lead to unforeseen
reactions the crystal might have with the presence of heat, or simply as it might result
in melting. Drying in the oven can only be more confidently done with the complete
knowledge that the compound is pure. The temperature in the oven might go beyond
the ideal for drying and, instead, melt the compound.

9. Impurities might induce a ‘melting point depression’ in the compound – meaning it

can melt over a wide range of temperatures. A substance present with impurities
usually melts at lower temperature than the pure compound. Generally, the smaller
the range of melting temperature, the purer is the compound.

10. a. Adding boiling chips to an oil bath reduces the occurrence of bumping by
creating steam. This helps prevent the apparatus from shaking too much and from
creating undesired booming noise.

b. Adding charcoal during the recrystallization process is done to remove the color
from the impurities present in the substance. Charcoal absorbs color impurities.

c. Fluted paper makes filtration faster by maximizing the surface area in which the
paper and solution could be in direct contact. This increases the liquid flow into it.

d. Pre-heating or using a short-stemmed funnel prevents the premature formation

of crystals. Pre-heating would warm up the apparatus, while a short-stemmed
funnel allows for a lesser distance to be traveled by the solution. All of this favors
crystal formation.

e. Placing a small piece of wire between the paper and the funnel relieves any
pressure increase brought about by the hot filtrate. This prevents the formation of
solvent seal that would block the air flow.

f. Determining the melting point of a compound calls for the use of thin capillary
tubes. Pulverizing the crystals only allows for it to fit and be contained in the narrow
body of the tube.

g. Constant stirring of the oil bath evenly distributes heat across the oil that allows
for faster response to external thermal inputs and outputs.
11. a. For both compounds, water fits the role of solvent best due to its high solubility
in high temperature and low solubility in low temperature. Earlier, it was established
how such a characteristic is included in the criteria for the best solvents to use.

𝑎𝑐𝑡𝑢𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
b. Solution for purity: % 𝑝𝑢𝑟𝑖𝑡𝑦 = 𝑔𝑖𝑣𝑒𝑛 𝑠𝑎𝑚𝑝𝑙𝑒 × 100%

2.0𝑔−0.6𝑔 1.4𝑔
Compound A: % 𝑝𝑢𝑟𝑖𝑡𝑦 = × 100% = 2.0𝑔 × 100% = 70%
2.0𝑔

8.0𝑔−0.5𝑔 7.5𝑔
Compound B: % 𝑝𝑢𝑟𝑖𝑡𝑦 = × 100% = × 100% = 93.75%
8.0𝑔 8.0𝑔

12. a. Among the three, compound A is most likely to be obtained pure as it

possesses a solubility on 1.05 g/mL in cold ethanol, smaller than either that of
compound B or C. it also has a solubility of 20.5 g/mL in hot ethanol, much greater
than the rest.

b. Having the least solubility value, compound C is most likely to separate upon
cooling.
4.2𝑔
4.0𝑔− 1.9𝑔
2
Compound C: % 𝑝𝑢𝑟𝑖𝑡𝑦 = × 100% = × 100% = 47.5%
4.0𝑔 4.0𝑔
 References:

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solids-melt-lower-temperatures/

Libretexts. (2019, June 5). Recrystallization. Retrieved from

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