Anagha Narayanan Organic and Biochemistry Mr.

Franz April 16 2012

Saponification

Purpose: In this lab, we prepared soap by hydrolizing a fat by reacting it with a strong base to create the salt of the fatty acid (which is soap).

Materials: 800 mL beaker Boiling chips 150 mL beaker 15 mL of oil 20% NaOH

10 mL of ethanol heating plate ethanol-deionized water (1:1) Side Arm Flask Rubber tubing Distilled water Ice 50 mL saturated NaCl Buchner Funnel

Anagha Narayanan Organic and Biochemistry Mr. Franz April 16 2012 filter paper glass stirring rod

Procedure: Begin by assembling a hot water bath. Fill an 800 mL beaker with water, and heat on the heating plate. Add boiling chips to the water to prevent it from boiling over. While you wait, prepare the reaction mixture. In the 150 mL beaker, add 15 mL of oil, 20 mL of 20% NaOH, 10mL of ethanol and boiling chips. Note the initial volume of the mixture, and the separation of layers. After the bath has reached a slow boil, gently lower the smaller beaker into the 800 mL beaker, making sure that no water spills into the reaction beaker. After you have established that the small beaker sits comfortably, let it boil for 25 minutes. Stir frequently with a glass stirring rod. Maintain the initial volume of the reaction mixture by adding 1:1 ethanol-deionized water as needed. At the end of the 25 minutes, the layers should no longer be visible. Test the mixture by placing a few drops of it into a test tube, and then adding 10 mL of cold distilled water. If you see fat drops form, add 5 mL of 20% NaOH and 5 mL ethanol to the reaction mixture and heat for 10 more minutes. Continue until no fat droplets form. To isolate the soap, turn the heating plate off, add 25 mL of distilled water to the beaker, and then let the beaker cool for 5 minutes. Then place the beaker into an ice bath for approx. 10 minutes Measure out 50 mL of cold NaCl solution. Decant any liquid from the soap mixture, then add the 50 mL of NaCl. This process separates the soap from the glycerol. Collect the solid using a buchner funnel (attach tube to side arm flask and sink to create a vacuum). Continue to wash the soap with

Anagha Narayanan Organic and Biochemistry Mr. Franz April 16 2012 distilled water. Collect final product. Obvservations: When the reaction mixture was initially formed, there were two distinct layers. After the boiling, the mixture was a darkish yellow, single layer. Upon our first test with cold water, small yellow globs of fat formed in the test tube, and we had to add ethanol and NaOH and boil again. After adding the NaCl, we had to stop the experiment for a week. When we came back, the soap mixture had crusted in the beaker, leaving an easily decant-able liquid all around Our final product was crumbly for whatever reason, and had a texture much more like gravel than like soap.

Conclusions: Our experiment DID yield soap or a fatty acid salt. The problem is that the texture of the soap was off. While the expected soap was meant to be smooth and lumpy, our group's soap came out gravelly like many small rocks. The problem might have been during the final steps, because we left our soap to sit with NaCl for over a week, or the problem might have been during collection.

Anagha Narayanan Organic and Biochemistry Mr. Franz April 16 2012