Synthesis and Characterization of Aspirin Product Identity and Purity After synthesizing a

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Synthesis and Characterization of Aspirin
Product Identity and Purity
After synthesizing a chemical, especially a drug, it is important to confirm the identity and purity of the product. You will perform three tests to examine the identity and purity of the aspirin that you synthesized. One test will detect the presence of leftover salicylic acid in the synthesized aspirin and allow you to determine its concentration. Government regulations stipulate that commercial aspirin must not contain residual salicylic acid since it is irritating to the mouth, throat, and stomach. Iron salts react with phenols to form a complex ion that has a purple color, therefore iron (III) chloride can be used to determine if your aspirin sample contains
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Procedure

Actual Mass of Product. If you have not already done so, weigh your dry recrystallized product. If your product isn’t dry place your vial in the oven in the room for 10-15 minutes.

Melting Point Determination
You will determine the melting point of pure acetylsalicylic acid and your synthesized acetyl salicylic acid (aspirin).

1. Obtain two melting point capillary tubes. Note that these are sealed at one end. Also note that a solid must be dry before it can be “pushed” into the tube.
2. Place a small amount of the your synthesized aspirin crystals on a clean watch glass.
3. Hold the melting point tube open side down and carefully pick up/push crystals into the tube. Turn the tube and tap the closed end gently on the bench to “knock” the crystals to the bottom of the tube. The bottom of the tube should be about 2 mm full.
4. Follow the same procedure to fill the second mp tube with crystals of pure acetylsalicylic acid.
5. Place the sealed end of the two tubes into the melting point apparatus as follows: your product on the left and pure acetylsalicylic acid on the right. You may need to share a melting point apparatus with another two lab partners. In this case, since there are only three sample slots in the apparatus, put the pure acetylsalicylic acid in the middle and
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