1. PUT ON YOUR CHEMICAL SPLASH-PROOF SAFETY GOGGLES!

Caution: Oil will be hot, and may splatter or catch fire. Wear goggles at all times.

Assembling the hot water bath

2. Assemble a hot water bath by filling an 800 mL beaker approximately 3/4 full
with water and begin heating the water with a bunsen burner.

3. Add three or four boiling chips to the water in the hot water bath to prevent the
water from boiling over.

Preparing the reaction mixture

4. In a 150 mL beaker add the following ingredients.

A. 15 mL of oil (or 10 g of solid shortening)

 B. 20 mL of 20% NaOH

C. 10 mL of ethanol

D. 3 boiling chips (These will help prevent the mixture from boiling over
while it is being heating.)

5. Note the total volume (level) in the 150 mL beaker and how many layers the
ingredients initially form.

Heating the reaction mixture

6. Begin heating the reaction mixture by clamping the beaker and contents in the
hot water bath. Heat the mixture for about 25 minutes after the water comes to a
slow boil. The 150 mL beaker should be clamped so that the reaction mixture is
below the level of the water in the water bath. Maintain the water level in the
water bath by adding water as needed.

7. Using a stirring rod, stir the reaction mixture frequently so that it does not boil
over.

8. Maintain the total volume of the reaction mixture by adding small quantities of
1:1 (volume/volume) ethanol-deionized water.

9. After the initial 25 minute heating there should be no separation of layers in

the beaker.

Testing the reaction mixture

10. Test the reaction mixture to determine if the saponification process is
complete by carefully placing a few drops of the reaction mixture in a 6-inch test
tube. Add 10 mL of cold water. If fat droplets form, add 5 mL of the 20% NaOH
and 5 mL of ethanol to the beaker and continue to heat for an additional 10
minutes, or until no fat droplets form upon testing.

Isolating the soap CAUTION: Remember that the beaker and clamp are hot!
11. When the saponification process is complete, turn the bunsen burner off, add
25 mL of deionized water to the beaker and place the beaker on the bench top to
cool for about 5-6 minutes. Then place the soap reaction beaker into an ice bath
and cool for about 10 minutes.
12. At this point, measure out about 50 mL of saturated NaCl solution and cool it
also for about 5-6 minutes in the ice bath.

13. After the cooling time is complete for the soap reaction mixture, decant any
liquid from the beaker. (Be careful not to pour off the soap.)

14. Next add, add the 50 mL cold, saturated NaCl solution to the soap beaker and
stir thoroughly with a glass rod. This process separates the soap from the glycerol
and excess base and is called "salting out."

15. Collect the solid soap, using a Buchner funnel. [Note: Decant as much liquid
off before adding the solid soap to the Buchner funnel.]

16. While the air is being drawn over the soap in the funnel, wash the soap with
two 20 mL volumes of ice cold deionized water. Continue to draw air over the
soap for another 3 minutes.

Analyzing the soap

17. Fill four, 6-inch test tubes one-third full with deionized water. Place a small
amount of the soap in each test tube and mix the soap and water well.

A. Test the pH of the first tube by dipping a clean stirring rod into the solution
and touching the solution to both red and blue litmus paper. Record your
observations on the Data Sheet.

B. In the second test tube add several drops of calcium chloride solution.
Record your observations.

C. In the third test tube add several drops of iron(III) chloride solution. Record
your observations.

D. In the fourth test tube add a single drop of kerosene and shake the solution.
Record your observations.

18. Pour the contents of the four test tubes into the designated waste container.

Soap disposal
19. Place the soap in the designated container.

20. Thoroughly rinse all of the glassware with water before storing.