Aparna Matur

Date: 9/15/2020
Protocol- Recrystallization and Melting point.
Hirsch funnel (Simple Isolation)
Table of Pertinent information:
Substance Purpose
Benzoic Acid (MW 122.12) (Meting point- Crystallization substance
122.3C)
Deionozed water Solvent for recrystallization
Percent Recovery Calculation (Amount To observe the purity of the recrystallized
recovered/amount started with x 100) substance.
Observation of the melting point range To determine the purity of the recrystallized
product

1. Obtain the 150mgs of crystallized Benzoic Acid (MW 122.12).

2. Set up approx. 25ml of water to boil to use as a solvent for this experiment. In the sand
bath, with a stirrer inside. Sand should be approx. 1cm high on the hot plate. (Do not
increase the hot plate temperature above 4 or sand bath will crack)
3. Once boiled/heated, dissolve the benzoic acid.
4. (May/may not apply) If the solution has visible impurities, gravity filter the solution to
remove insoluble impurities.
5. Place the obtained sample in a small Erlenmeyer flask on the sand bath as well.
6. Once the water has reached boiling, through the use of a Pasteur pipette, transfer the
boiling water into the Erlenmeyer Flask until the sample is JUST dissolved. (Record
volume used)
7. Gravity-Filter this solution to remove insoluble impurities, making sure to use the right-
sized filter paper. Place a second Erlenmeyer flask on the sand bath to warm up and
prevent fast recrystallization with a short-necked funnel.
8. Filter the solution into the empty funnel into the Erlenmeyer Flask to remove the
insoluble impurities. If there are any crystals remaining on the filter paper, rinse with
boiling water to dissolve.
9. Once this is complete, take the sample solution out of the sand-bath and allow it to cool
on the bench.
10. Then place this in the ice-bath to further cool it.
11. Then vacuum filter the remaining through the use of a Hirsch funnel to obtain a dry
recrystallized solid.
12. Making sure the sample is dry, record the mass and determine a melting range. And
calculate the
Craig-Tube Isolation
1. From the small sample given, measure out between 20-25mgs of Benzoic acid and
place them in a Craig tube.
2. Create a hot supersaturated solution within the Craig tube by adding boiling water
until the sample just dissolves and in the heated sand bath.
3. Remove this from the heat and clamp it to allow for slow cooling.
4. Induce further crystals by placing the solution in an ice-bath.
5. Centrifuge the sample to isolate it.
6. Once dry, find the percent recovery, melting range and weight of the recrystallized
sample.