Chem Pre-task - Recrystallisation

Equations for yield and atom economy:

-Atom economy is (mass of all products/mass of desired products) x 100

-Yield is (possible mass of product/actual mass of product) x 100
-Yield will never be 100% because impurities cause side reactions to take place, reversible
reactions take place and the desired product may continue to a secondary reaction.

How impurities can be created in products and ways to purify products:

-Impurities are created from side reactions, secondary reactions and impurities already present
on the equipment if it hasnt been cleaned properly.
- These impurities can be removed and various number of methods but the one discussed
below, recrystallisation, will be the focus of attention.

Procedures for recrystallisation

1. Weigh 5 grams of salicylic acid in a weigh boat on a scale and place into a conical flask.
2. Measure 7 ml of acetic anhydride in a measuring cylinder and add to the conical flask.
Ensure goggles are worn during this procedure to avoid the vapour going into the eyes.
Avoid contact with skin.
3. Add 8 drops of sulphuric acid to the conical flask.
4. Heat the flask in a water bath. When the water begins to boil, heat the flask for a further
15 minutes.
5. Cool the flask for 3 minutes after heating and 15 ml of room temperature water to
decompose the excess acetic anhydride. Swirl the flask to mix the contents.
6. Place the flask in an ice bath and allow Aspirin crystals to form. Crystal growth can be
induced by scratching the crystallisation vessel with a glass stirring rod.
7. Filter solid crystals using a Buchner funnel into a filter flask. Rinse the conical flask 2
times with 3 ml of deionised water to ensure all crystals have been retrieved.
8. Discard the filtrate in the filter flask.
9. Transfer the solid to a 250 ml beaker and add 10 ml of 95% ethanol or as much as it
takes to dissolve the crystals.
10. Add 10 ml of deionised water, cover the beaker and allow to cool for 10 minutes then
place in an ice bath.
11. Use the suction filter process to separate the Aspirin from the filtrate once the crystals
have form and leave to dry for 15 minutes.
12. Discard the filtrate and rinse the filter flask, then discard the wash water.
13. Place the Aspirin on a double piece of paper towel to dry, meanwhile rinse the funnel
with water.
14. Calculate the percentage yield of the aspirin using the theoretical yield for your weighed
amount of starting reactant.
 15. Place a few crystals into a melting point capillary tube. Starting at 120C allow the
temperature to increase by 1C each minute and record melting point range ( the point at
which the Aspirin starts to melt to the point where no crystals remain).
16. Compare this to the theoretical melting point to determine the purity of the product.

(Aspirin Synthesis, n.d.)