Orgo5 - Organic Chemistry Lab Experiment title: Separation...

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Organic Chemistry Lab Experiment title: Separation and Purification of the Components of an Analgesic Powder Introduction/Purpose of experiment: The main purpose of this experiment was to separate the three components of an analgesic powder containing acetaminophen, aspirin, and caffeine. Several lab techniques were required for this separation, such as filtration, extraction, and recrystallization. There were also inactive ingredients present in the powder that needed to be extracted in order to purify the substances. The melting points and Thin Layer Chromatography (TLC) were performed to verify and check the success of both the separation and purification of the components of the powder. Main reaction/equation: Components-From Goody’s extra strength Headache Powder: (a) Acetaminophen : Insoluble upon the addition of warm methylene chloride, precipitates out as a solid that also includes inactive ingredients (b) Inactive ingredients : insoluble upon addition of warm ethanol, acetaminophen left after evaporation (c) Caffeine : Soluble upon addition of warm ethanol. Due to the neutrality of caffeine, addition of base will not cause it to dissolve (d) Aspirin : soluble upon addition of warm ethanol. However, the acidity of aspirin will allow it to dissolve upon addition of base to remain as anion. Solution must be neutralized and the solid precipitates out Data: Goody’s Extra strength Headache Powder: 1.003 g Components Formula Weight Melting Point Amount in Powder Aspirin 180.159 g/mol 135˚C 520 mg Acetaminophen 151.165 g/mol 169-170.5˚C 260 mg Caffeine 194.194 g/mol 235˚C 32.5 mg Procedure Preliminary Separation: 1. Massed original sample of Goody’s Extra Strength Powder and saved a 5mg
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sample for TLC analysis 2. Warmed 6 mL of methylene chloride in 40˚C water bath by constant swirling and mixed with the powder in a small Erlenmeyer flask (50 mL flask) 3. After mixing the powder and methylene chloride, filtered the mixture by suction filtration with a large funnel and filtering flask 4. After filtration was completed, used an additional 2 mL of warm methylene chloride to rinse the flask and the solid in the funnel Isolation and purification of Acetaminophen 1. Transferred the insoluble powder in the funnel to the original small Erlenmeyer flask 2. Added 2 mL of ethanol and heated to boiling in a hot (75-80˚C) water bath, using a 150 mL beaker 3. Collected the insoluble material by suction filtration on a clean Hirsch funnel, using 1 mL of hot ethanol to aid the transfer and rinse the solid 4. Transferred the filtrate with the aid of a disposable pipette to a small (50 mL) labeled beaker and allowed the ethanol to evaporate on a steam cone 5. After weighing, discarded inactive ingredients
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This note was uploaded on 02/16/2010 for the course CHEMISTRY V25.0246 taught by Professor Callahan during the Spring '08 term at NYU.

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Orgo5 - Organic Chemistry Lab Experiment title: Separation...

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