EDUC 705L (ORGANIC CHEMISTRY- Laboratory)
Experiment #1 : Crystallization
Introduction:
One of the techniques of purification of organic compounds is crystallization,
which involves three stages: removal of impurities, nucleus formation and
encouragement of crystal growth.
Objectives:
1. Purify an organic compound through crystallization.
2. Differentiate the crystals formed in rapid cooling and in slow cooling process..
Test Mixture:
Mixture of benzoic acid, sodium chloride and congo red
Reagents:
Animal charcoal, 5% nitric acid solution, 1% silver nitrate solution, distilled water,
ice
Apparatus and materials:
Beaker, graduated cylinder,, glass rod, Hot plate,
Procedure:
1. Place one spatulaful of the test mixture in a 250-ml beaker,
2. Add 50 ml distilled water, and heat, with stirring.
3. When practically all white solid particles has dissolved, add 0.5 gram of animal
charcoal and continue heating with vigorous stirring.
4. Bring the solution to boil for one minute, and then immediately filter while still hot.
[Use a fluted filter paper].
5. Collect equal amounts of the hot filtrate in two separate test tubes. One test tube
labelled “slow cooling” (just set aside on a safe place on top of your working
table) and another “rapid cooling” (using ice bath in a big evaporating dish).
6. Record observations of the following for both processes: color of filtrate; and
color, size and shape of crystals.
7. Combine the contents of the two test tubes and pour into a clean beaker. Filter th
crystals and wash 2-3 times with cold distilled water.
8. Spread the crystals on a clean and dry filter paper, cover with another filter paper
and allow to dry.
9. Test for the completeness of the separation:
a. Dissolve a pinch amount of the purified crystals using 1.0 ml of hot distilled
water in a test tube
b. Acidify with one drop of 5% nitric acid and add 2 drops of 1% silver nitrate
solution. Observe and record the result.
WORKSHEET #1 : Crystallization
Group No. ______
Surnames only (Alphabetical): Date:________
I. Results and Observations: (10 points)
Color of the filtrate for Slow Cooling: _____________________
Color of the filtrate for Rapid Cooling: _____________________
Table 1 Comparison of the CRYSTALS formed by Rapid and Slow Cooling
Color Size Shape
Crystals formed on
SLOW Cooling
Crystals formed
using RAPID
Cooling
Observation/s for the completeness of separation:
II. Questions:
1. Determine the function/purpose of the following: (15 points)
A. Adding animal charcoal to the hot solution:
B. Filtering the solution while still hot:
C. Adding silver nitrate solution to the purified crystals:
2. Compare very briefly the two methods of producing crystal formation from
solutions? (4 points)
References:
CONTRIBUTION/S of Each Member:
