4PY011: The Physicochemical Nature of Drugs - Management Assignment Help

Assignment Task:

Task:

Experimental procedure
Part 1. Preparing the aspirin
• Allow up to 1 hour for this
• Lab coats and eye protection MUST be worn throughout
• Conduct the experiment in a fume hood
Conical flask Magnetic stirrer & flea Plastic disposable pipette

Weigh 2.4 g (to the nearest 0.1g using a 2 figure top-pan balance) of sodium salicylate directly into a 100 cm3 conical flask and add 30cm3 of 2M NaOH. Using the magnetic stirrer & flea provided, stir the mixture until everything has dissolved (no heating is required). Turn off the stirrer and add crushed ice to your flask until the total volume reads approximately 50 cm3 ± 5 cm3
. With
continued stirring, add 5.0 cm3 of ethanoic anhydride (commonly called acetic anhydride) and stir gently for 15 minutes. You can use a 3 ml plastic disposable pipette, with graduations, for measuring out the anhydride (but add it quickly to the flask without delay)**.

Part 2. Analysis of your product
a) Determine the melting point using the conventional heated block apparatus. If you are unsure about this see determining a melting point. We provide tubes that are pre-sealed at one end and you can take your sample directly from the beaker. Only do this part when the sample is fully dry. (Allow at least 20 mins for this).
The melting point technique will be demonstrated to you on request.

b) Analyse your product for purity by titration with standard NaOH using a phenolphthalein indicator. See below for details. (Allow up to 50 mins for this).

1. Weigh approximately (0.2-0.3) g of your dry product into a small sample tube without a lid. Accurately weigh the tube and product on a four-figure balance (to 3d.p.). Now carefully tip the product into a 250 cm3 conical flask, making sure as much as possible has gone into theflask. Weigh the sample tube with any residual powder remaining. The4difference between the two weights gives an accurate estimate of the sample actually transferred to the conical flask. This technique is called weighing by difference. Record your weights in the table provided.

2. Dissolve the sample in about 25 cm3 of ethanol, using the calibration on the flask itself as a rough guide. Be careful not to ‘slop’ any solution out of the flask.

3. Add a few drops of phenolphthalein indicator, and titrate with the 0.10 M sodium hydroxide provided until a permanent pale pink colour remains.
4. Record your titre in the table provided.

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