Courtney Courter Organic I (night class) September 21, 2010

Lab Experiment # 1
Recrystallization: Purification of a solid substance

Purpose of the Experiment: Purify aspirin tablets to obtain pure acetylsalicylic acid
solid

Material: Ten 5-grain aspirin tablets, 10 mL of 95% ethanol

Equipment: Two 125 mL Erlenmeyer flasks, Hot plate, gravity filter equipment, Ice
bath, funnel, melting point reader.

Procedure: Weigh the ten 5-grain aspirin tablets in a 125 mL Erlenmeyer flask. Add 10
mL of 95% ethanol. Heat on a hot plate until material dissolves. Use stirring rod. Gravity
filter the warm solution into a warm Erlenmeyer flask to remove undissolved material.
Pour 50 mL of cool water into this flask and allow crystallization to occur for 10 minutes
at room temp and than for 5 minutes in the ice bath. Collect the product my suction
filtration and wash it in the funnel with a small amount of cold water. Weigh the dry
product. We also calculated the melting point.

Table of Physical Constants:

Ethanol Aspirin (Acetylsalicylic Acid)

Formula Weight 46.07 g/mol 180.2 g/mol
Density 0.789g/mL 1.4 g/mL
Boiling Point 78.4 C 140
Melting Point -114.3 C 135

Structure
Courtney Courter Organic I (night class) September 21, 2010

Observations: We observed that the material dissolved when we heated it and crystals
formed when we cooled it. When we took the melting point we saw that it was fairly
close to the real melting point of Acetylsalicylic Acid.

Data Collected
Original weight of aspirin 3.636 g
End weight of Aspirin 1.444 g
When cooling Start time: 7:24 End time: 7:34
When cooling with Ice Start time: 7:34 End time: 7:39
Our melting point (happened between) 120 C - 130 C

Evaluation: Recrystallization is a technique used to purify solids based on their

solubilities. The technique is as follows: a small amount of solvent is added to a flask
containing an impure compound. The contents of the flask are heated until the solid
dissolves. Than, the solution is cooled. A more pure solid precipitates, leaving impurities
dissolved in the solvent. Vacuum filtration is used to isolate the crystals. The waste
solution is thrown out. After we obtained our crystal we checked its melting point and
found that it was very close to that of pure aspirin, therefore, recrystallization is a good
way to purify.

Questions:

Pre Lab
1 grain = 0.0648 g

So a 5 grain aspirin = 0.0648 x 5 = 3.24 g

If we had ten of them than altogether they should = 32.4 g

If the student isolated 3.05 g of the acetylsalicyclic acid than her percent yield is….

Percent yield=[(actual yield)/(theoretical yield)] x 100

(3.05)/(3.24) x 100 = 94.1 % yield

 Courtney Courter Organic I (night class) September 21, 2010

Calculations

Percent yield for all ten tablets Percent yield for separate tablets

Theoretical = 3.24 g If 1.444 g = total of all ten tablets - than -> 1.444 g / ten =
Actual 1.444 g 0.1444 single tablet

Percent yield=[(actual yield)/(theoretical yield)] x 100 Percent yield=[(actual yield)/(theoretical yield)] x 100

(1.444)/(3.24) = 0.4456 (0.1444)/(0.324) = 0.4456

x 100 = 44.56 % x 100 = 44.56 %

2. Appearance of the sample before and after purification.

Before purification the sample was very white and chalky. After, you could observe the
small crystals.

3. How much starch is in each tablet?

Started with 3.636 g and ended with 1.444 g. So 3.636 – 1.444 = 2.192 g of starch

4. Describe the events you saw in the flask as crystals formed. What shape are the
crystals?

The material started to gather together into small crystals. The shape was small and
round.

References:

http://scifun.chem.wisc.edu/chemweek/pdf/ethanol.pdf

http://chemistry.about.com/od/chemistryhowtoguide/ss/recrystallize.htm