1. Dissolve 1.5 g of the analgesic mixture (acetylsalicylic acid, acetaminophen, caffeine, binder) in 20 mL...

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1. Dissolve 1.5 g of the analgesic mixture (acetylsalicylic acid, acetaminophen, caffeine, binder) in 20 mL of diethyl ether. Filter the solution by gravity filtration into a separatory funnel to separate the soluble and insoluble components. (Caution: stopcock must be in the closed position!!!) Transfer the insoluble components to a 50 mL Erlenmeyer flask for later extraction. Label this Erlenmeyer flask as "Insoluble Components". Add 10 mL of 1 M aqueous KaHPOs to the separatory funnel and mix the layers as instructed by the laboratory instructor. (Caution: Vent the separatory funnel!) 2. 3. Drain the aqueous layer to a 25 mL Erlenmeyer flask and set aside for further extraction. Label this layer as "Extraction 1". Set aside for further extraction. Leave the organic layer in the separatory funnel. 4. To the separatory funnel containing the organic layer, add 10 mL of a saturated NaCl solution to wash the ether. Separate the layers and dry the ether layer over 1 to 1.5 g of anhydrous sodium sulfate into a 50 mL Erlenmeyer flask for 10 minutes. If the anhydrous sodium sulfate clumps, add more of the salt to dry the organic layer. Let stand for an additional 10 minutes 5. Decant the ether layer to a clean pre-weighed 50 mL Erlenmeyer flask and evaporate the solvent using the steam. The caffeine should crystallize as a solid material. Transfer the solid to a beaker labelled "Extraction 2" and air dry for a week. Obtain the dry mass of the product and measure its melting point. 6. To the flask labelled "Extraction 1", add 6 M HCl until the solution becomes acidic to litmus paper. Place in an ice-water bath to promote precipitation of the analgesic component. Vacuum filter the product and place in a beaker to air dry for a week. Obtain the dry mass of the product and measure its melting point. . Dissolve the "Insoluble Components" in 5 mL of acetone by gently shaking the 50 mL Erlenmeyer flask. Vacuum filter the solution. Rinse the Erlenmeyer flask with a small volume of acetone and vacuum filter. Discard the insoluble impurities. Transfer the filtrate to a 25 mL Erlenmeyer flask and label "Extraction 3". Evaporate the solvent on a steam bath to crystallize the product. 8 Perform a hot water recrystallization on "Extraction 3" to purify the third analgesic component. Vacuum filter the product and place in a beaker to air dry for a week. Obtain the dry mass of the product and measure its melting point. 1. Dissolve 1.5 g of the analgesic mixture (acetylsalicylic acid, acetaminophen, caffeine, binder) in 20 mL of diethyl ether. Filter the solution by gravity filtration into a separatory funnel to separate the soluble and insoluble components. (Caution: stopcock must be in the closed position!!!) Transfer the insoluble components to a 50 mL Erlenmeyer flask for later extraction. Label this Erlenmeyer flask as "Insoluble Components". Add 10 mL of 1 M aqueous KaHPOs to the separatory funnel and mix the layers as instructed by the laboratory instructor. (Caution: Vent the separatory funnel!) 2. 3. Drain the aqueous layer to a 25 mL Erlenmeyer flask and set aside for further extraction. Label this layer as "Extraction 1". Set aside for further extraction. Leave the organic layer in the separatory funnel. 4. To the separatory funnel containing the organic layer, add 10 mL of a saturated NaCl solution to wash the ether. Separate the layers and dry the ether layer over 1 to 1.5 g of anhydrous sodium sulfate into a 50 mL Erlenmeyer flask for 10 minutes. If the anhydrous sodium sulfate clumps, add more of the salt to dry the organic layer. Let stand for an additional 10 minutes 5. Decant the ether layer to a clean pre-weighed 50 mL Erlenmeyer flask and evaporate the solvent using the steam. The caffeine should crystallize as a solid material. Transfer the solid to a beaker labelled "Extraction 2" and air dry for a week. Obtain the dry mass of the product and measure its melting point. 6. To the flask labelled "Extraction 1", add 6 M HCl until the solution becomes acidic to litmus paper. Place in an ice-water bath to promote precipitation of the analgesic component. Vacuum filter the product and place in a beaker to air dry for a week. Obtain the dry mass of the product and measure its melting point. . Dissolve the "Insoluble Components" in 5 mL of acetone by gently shaking the 50 mL Erlenmeyer flask. Vacuum filter the solution. Rinse the Erlenmeyer flask with a small volume of acetone and vacuum filter. Discard the insoluble impurities. Transfer the filtrate to a 25 mL Erlenmeyer flask and label "Extraction 3". Evaporate the solvent on a steam bath to crystallize the product. 8 Perform a hot water recrystallization on "Extraction 3" to purify the third analgesic component. Vacuum filter the product and place in a beaker to air dry for a week. Obtain the dry mass of the product and measure its melting point.

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