BROKENSHIRE COLLEGE PA

Madapo Hills, Davao City

Name: Maturan,Zaire Grace Rating:

Course & Year: Date:

Learning Activity No. 11

PURIFICATION OF SOLIDS BY SUBLIMATION

Specific Learning Objectives:

At the end of the experiment the learners shall be able to:
a. purify organic solids through sublimation
b. determine the weight of the obtained sublimate.
c. calculate the percentage of the pure crystals recovered from the sample.

Time Allotment: 2 hours

Learning Resources:
Reagents:
Acetanilide Benzoic acid Napthalen
e

Apparatus
2-Filter paper 3-Watch glass (10 cm and 12 Microspatula
cm)
Funnel Crucible tong Wire gauze
Air bath Bunsen burner Iron stand
Wooden test tube holder Calibrated medicine dropper 50 mL Beaker
Hot Plate Hot Hand Test Tube
brush

Learning Strategies:

When an impure organic solid is heated, the vapor pressures of all the components are increased. If
the vapor pressure of the major component rises more rapidly than that of the impurity so that this
vapor pressure equals one atmosphere before the melting point of this component is reached, the
solid will pass into vapor without intermediate passage through the liquid state. By cooling, the
vapor is converted to crystals which have high degree of purity. This process is known as
sublimation.
Only a few compounds with relatively high vapor pressure can be purified by sublimation under
normal pressure. These include naphthalene, anthracene, benzoic acid, salicylic acid, alpha and beta
naphthol, camphor, iodoform and acetanilide. The process yields products of high purity, but
considerable loss of products may occur.

Procedures:
1. Weigh about 0.5g of impure sample. Record the weight to the nearest 0.01 g. PA
2. Spread the sample on the 12 cm watch glass leaving a margin at the edge.
3. Cover with an inverted 10 cm watch glass which has been previously weighed to the
nearest 0.01g.
4. Heat the watch glass with the sample over an air bath(water bath without water)using hot
plate.
5. cool the center top of the inverted watch glass with a 25 mm filter paper or a folded tissue
paper disc kept moist with drops of water.
6. When a film is formed on the condensing surface, adjust the heat so that condensation
proceeds very slowly over a period of 30 min. The set-up is inspected occasionally until
most of the sample has vaporized.
7. When no more crystals appear to sublime, cool the set-up. Very carefully remove the
inverted watch glass taking care not to disturb the sublimate.
8. Observe the crystalline structure of the sublimate. Compare with the original.
9. Determine the weight of the sublimate and calculate the percentage of the pure crystals
recovered from the impure sample, using the formula.
10. Keep the crystals in a small vial for future use. Label properly.

Weight of recovered crystals (sublimate)

% Recovery = ------------------------------------------- x 100
Weight of original crystal
 Name: _______Maturan, Zaire Grace __________________________________ Date: _________________________
Instructor’s Signature: _____________________ Score: ________________________
PA
Learning Activity No. 11
PURIFICATION OF SOLIDS BY SUBLIMATION

Data and Results

Acetanilide Benzoic acid Naphthalene

Weight of empty watch 46.97g 23.50g 46.97g

glass, g

Weight of crystals, g 0.5g 0.5g 0.5g

Weight of empty watch 47.16g 47.14g 47.18g

glass + sublimate, in grams

Weight of sublimate, g 0.19g 0.33g 0.21g

% Recovery 38% 31% 42%

Compare the physical 135 degree 121-125 degree 128 degree celsius
properties of the celsius celsius
original sample and
sublimate.

Guide Questions:

1. How to determine the purity of the sublimate?

Purification of solids by sublimation is a widely used technique in chemistry to separate and purify compounds based
on their differing sublimation temperatures and volatility. The process involves heating a solid substance to its
sublimation temperature, where it transitions directly from a solid to a vapor without passing through the liquid phase.
The determination of the purity of a sublimate involves a combination of analytical techniques to identify and quantify
any impurities. It's important to carefully control the sublimation conditions to maximize the separation of the
compound of interest from impurities. This process not only ensures the purity of the substance but also plays a crucial
role in various industries, including pharmaceuticals, where pure compounds are essential for drug development and
manufacturing.

2. Define the following:

 a. Sublimation
PA
Sublimation is a crucial process in the purification of solids, particularly in chemistry and
material science. It is a phase transition phenomenon in which a substance changes directly
from a solid to a vapor without passing through the liquid phase. This process occurs when the
vapor pressure of the solid exceeds its external pressure and temperature conditions allow for
such a transition. Sublimation is a highly useful technique for separating and purifying solids,
especially when dealing with substances that are sensitive to heat or can undergo
decomposition in the liquid state.

b. Deposition

Deposition is the reverse process of sublimation. It involves the transformation of a substance

from a vapor directly into a solid state. In the context of purification by sublimation, deposition
plays a vital role in the collection of the purified substance. The vaporized material, produced
during sublimation, is collected on a cold surface or within a suitable container where it reverts
to its solid form. This collected solid is the purified product of the sublimation process.

c. Sublimate
The substance that undergoes sublimation and forms the vapor is often referred to as the sublimate. The
sublimate is the purified product that results from the sublimation process. It is typically the material of
interest in purification, and its characteristics can be significantly improved by this technique. The sublimate
can be isolated and collected, and it is free from impurities that may have been present in the original solid
material.

Conclusion
The process of purification of solids by sublimation is an essential technique in the field of chemistry and materials
science. This method is particularly useful for separating and purifying substances that sublime, or transition directly
from a solid to a gaseous state, without passing through the liquid phase. The key principle behind sublimation is the
selective vaporization of impurities, leaving behind a purified solid product. This purification technique offers several
advantages, including the ability to obtain highly pure substances, often with minimal loss of the desired compound.

One of the primary advantages of sublimation is its ability to separate volatile impurities from the desired solid. When
heat is applied to the mixture, the impurities are converted into gasses and removed, while the main compound
remains in the solid state. This results in a higher level of purity and quality in the final product. Additionally,
sublimation is a relatively mild process that minimizes the risk of chemical degradation or decomposition of the
substance, making it suitable for a wide range of compounds.
In conclusion, sublimation is a powerful and versatile purification method in the realm of chemistry. Its ability to
separate and purify solids through the selective vaporization of impurities makes it a valuable tool for researchers and
industrial applications. By harnessing the principles of sublimation, scientists can obtain highly pure substances
PA with
precision and efficiency, contributing to advancements in various fields, from pharmaceuticals to materials science.
This technique exemplifies the importance of understanding physical properties and phase transitions in chemistry,
showcasing how the careful manipulation of these factors can lead to the isolation of pure and high-quality materials.