Exercise 4

Separation and Purification of Organic Compounds

Sublimation

The direct conversion of a substance from solid to gas without passing through the liquid state is
sublimation. As a process of separation, it can be applied when the components of a solid mixture differ
appreciably in their vapor pressures. It involves gentle heating of the mixture in a confined container until
particles of the solid escape into the vapor phase. When the vapors are condensed on a solid surface,
crystals of the component with high vapor pressure can be collected, with the component of lower vapor
pressure left in the container.

As a process of purification, it also depends on differences in volatility – that is, in cases when
the impurities can be volatilized. Less volatile or non-volatile impurities will remain as residue while the
sublimate is being formed.

Although sublimation is convenient to apply and requires less time, its applicability is limited. It
cannot be used for separation of compounds having similar vapor pressures.

Test Compounds: Apparatus/Materials:

Salicylic acid Evaporating dish
Sodium sulfate watch glass
Wire gauze
Reagents: tripod
5% BaCl2 solution Bunsen burner or hot plate
Distilled water test tubes
Filter paper
PROCEDURE

1. Place a mixture of 0.5gram salicylic acid and a pinch of sodium sulfate in a clean, dry
evaporating dish. Cover the evaporating dish with a watch glass.
 2. Set up under the fumehood the evaporating dish with its contents on a tripod with wire gauze over
a Bunsen burner.
3. Heat gently with a low flame. Observe what happens inside the evaporating dish.
4. Cool the set-up completely and describe the substance formed on the watch glass and the one left
on the evaporating dish.
5. Collect the substance formed on the watch glass by scraping off carefully into a clean piece of
paper. Get a pinch for use in step 6 and submit the rest to your instructor.
6. Dissolve the substance in 1mL hot distilled water in a test tube. Add 2 drops of 5% BaCl 2
solution. Observe and record the result.
7. Get a small amount of the substance left in the evaporating dish and dissolve in 1mL hot distilled
water in a test tube. Add 2 drops of 5% BaCl2 solution. Observe and record the result.

Questions

1. What properties do substances which undergo sublimation possess?

2. Which compound in the mixture is the sublimate? Which did not sublimate?
3. How do you interpret the results obtained in steps 4 and 5?
4. Write the chemical reaction/s involved/
DATA AND ANSWER SHEET

Name _________________________________________________ Date__________________

Class Schedule _________________________________________ Rating _________________
Group No. _____________________________________________

Exercise 4
Separation and Purification of Compounds
Sublimation

I. Results and Observations

1. Description of mixture:

a. Before heating ____________________________________________________

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b. While heating ____________________________________________________
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c. Upon cooling:
Sublimate ____________________________________________________
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Residue ____________________________________________________
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2. a. Sublimate crystals + H2O + BaCl2: ____________________________________________

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b. Residue+ H2O +BaCl2: ______________________________________________________
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II. Answers to Questions
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