Lab#1

Re-crystallization or Purification of a Crystalline Compound

Purpose
In this experiment a sample of impure acetanilide will be re-crystallized from
water, a single solvent. This will be done by weighing a crude sample of each
and the pure product and to figure out the melting point before and after the
re-crystallization.
Procedure
Weigh out 2.0g of the Acetanilide mixture, then place in a small rounded
flask, use a powder funnel and add 35ml of distilled water. Then connect the
flask to a reflux condenser and start a slow stream of water through the
jacket of the condenser. Heat until no more solid appears to dissolve
meanwhile heat a glass Erlenmeyer flask and glass funnel in the oven. Boil
20ml of water to wet the filter paper. Take a malting point of the crude
sample of Acetanilide. Once the reflex is complete HOT filter the solution by
gravity. using the Erlenmeyer flask and funnel from the oven. Cool the filtrate
until crystals begin to form and then place in an ice bath. Set up the vacuum
filtration apparatus. set a piece of weighed filter paper into the funnel. Then
connect the flask to the aspirator and collect the crystals by vacuum
filtration. Then transfer the crystals to a pre-weighed watch glass and let sit
for 24 hours. Lastly weight the dried product and determine the melting
point.
Reagent/ Safety Information
Acetanilide:
Melting point: 114.3 C
Formula: C6H5NH(COCH3)
Boiling point: 304 C
Density: 4.65
Solubility: slightly soluble in water
Appearance: White glistening crystals
Safe handling: Wash thoroughly after handling and make sure to have lot of
ventalization. Minimize dust generation and accumulation. Avoid contact
with eyes, skin, and clothing and avoid ingestion and inhalation.
Storage: Keep away from heat and flame and keep in a tight container. Store
in a cool, dry, well ventilated area away from incompatible substances.
Disposal: Dispose container according to federal requirements.
Clean up: vacuum or sweep up material and place into a suitable container
for latter disposal.
Sources: MSDS:
http://ccinfoweb2.ccohs.ca.dproxy.library.dcuoit.ca/msds/records/6248473.pd
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Equipment

- Weigh scale
- Small round bottom flask
- powder funnel
- Reflux condenser
- Rubber tubing
-Erlenmeyer flask
- Glass funnel
- Beaker
- Melting point tube
-Filter paper
- Vacuum filtration apparatus
- Watch glass
- Melting point machine
(Vacuum Filtration Apparatus)

( Reflux Condenser)

Observations
The crude sample of Acetanilide was black and when the water was added it
turned the water black as well. The water boiled/bubbled on the heater.
When the reflux condenser process is done the white crystals started to
form. Once placed in the ice bath and cooled they turned partially
solid/liquid. When the crystals were dry before letting them sit for 24 hours
they looked white and crystallized. After they sat for 24 hours they looked
white and they also looked very shinny.
Data
Melting point of crude sample- 120.7C
Melting point of purified sample- 118.1C
Weight of crude Acetanilide- 2.0g
Weight of filter paper- 0.2185g
Weight of container- 10.45g
Weight of dry crystals with container- 12.40g
and molecular
weight of dry crystals - weight of filter paper - weight ofStructure
container
formula for acetanilide.
=12.40g - 0.2185g- 10.45 = 1.73g
Weight of crystals after re-crystallization/purification = 1.73g
Percentage recovered= weight of purified product
x 100
weight of crude sample
= 1.73g
x 100
2.0g
Percent recovered= 86.5%
Discussion
The crude sample of Acetanilide that was weighed out was 2.0g, so this
mean after re-crystallizing the weight should be very close to 2.0g, this
would mean that you did not lose very much product during the purification
process. The amount of purified acetanilide recovered was 1.73g. This means
that there could of been a few things done to get closer to the 2.0g mark.

Some things that could have prevent this from happening would be losing
crystals while transferring them to different containers and also from not
vacuuming the crystals enough or not letting them dry long enough before
weighing them.
Post Lab Questions
1. Water is a good solvent for the re-crystallization of acetanilide because at
high temperatures, acetanilide dissolves in water very well, but at low
temperatures it is not very soluble.
2 The charcoal is caught by the filtration paper, and the sugar remains
dissolved in the solution when the acetanilide precipitates out
3. Vacuum filtration is often faster than gravity filtration and is most useful if
the solid must be kept or if a filtration must be done rapidly.
4 a) It is important to pack the sample tightly in the melting point tube in
order to get a accurate reading of the melting point.
b) Heating the sample slowly when it is approaching its melting point is
important because the melting point approaches quickly and in order to get
an accurate reading if its going slowing you are more likely to get that
reading.
5. If you use a sample too large to determine the melting point then your
melting point will be off because your sample is bigger than needed. So it will
take longer for it to melt and will give you an inaccurate result.
Conclusion
In the process of doing a re-crystallization there is a lot of things that can be
done wrong to achieve the wrong melting point and the wrong purified
weight. As discussed in the discussion there are some ways to help get the
purification from 1.73g to closer to the original 2.0g.

Lab#1 - Re-crystallization or Purification of a Crystalline

Compound
January 7, 2014
Submitted to: Kevin
Submitted by: Taylor Sanderson
Lab Partner: Chloe Van Der Cruysen