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THE AFFECT OF TEMPERATURE ON THE PURITY OF ASPIRIN Chemical purity: the amount of a specified compound or element within an impure

sample Salicylic acid the active ingredient within aspirin PROCEDURE In this individual investigation I will be carrying out and analysing different methods and procedures to discover the purity of samples of aspirin these samples will be synthesized by myself within the lab; the different samples will also be synthesized at varying temperatures, subsequently allowing me to look at the affect of temperature on the chemical purity of aspirin. Synthesis of the aspirin will be done in two major steps: 1) Preparing 2-hydroxybenzoic acid (salicylic acid) this is the active ingredient within aspirin. 2) Using ethanoic anhydride to convert the salicylic acid into aspirin this step will be carried out at different temperatures in different test tubes, so that the affect of temperature on the purity of aspirin may be seen empirically and then calculated qualitatively. In botany, Wintergreen plants are known to contain substantial amounts of wintergreen oil (also known as oil of wintergreen); oil of wintergreen is comprised of many substances, but its main composition is methyl salicylate (approximately 98%) more commonly known as methyl 2-hydroxybenzoate. To obtain 2hydroxybenzoic acid, the oil of wintergreen is hydrolysed; sodium hydroxide (aqueous) is reacted with it under boiling heat and the product formed is sodium 2-hydroxybenzoate. The sodium 2hydroxybenzoate is then reacted with hydrochloric acid to get the desired 2-hydroxybenzoic acid. Chemical equation for preparing salicylic acid:

Salicylic acid

NOTE: in this step you will be diluting 4 mol dm-3 sodium hydroxide to 2 mol dm 3 sodium hydroxide. Step 1 will be done as follows:

Figure 1

a) Set out an apparatus as shown in figure 1. One slight change that needs to be made is that the flask should be placed in a water bath, instead of being heated by a Bunsen burner. Also, remember to add anti bumping granules (boiling chips) in the flask. b) Place 8g of wintergreen oil into the flask, together with 100cm3 of 2 mol dm3 sodium hydroxide (aqueous). c) Heat using the water bath for at least 30 minutes. d) Pour mixture into a beaker and cool (with water or ice). Add methyl orange indicator to the mixture; now add hydrochloric acid to the mixture (concentrated) stir solution whilst adding acid. When solution turns reddish stop adding hydrochloric acid. e) The product should be filtered using a Buchner funnel and suction apparatus. f) The product should be washed with a bit of cool water and placed in a small beaker; the product should now be left to dry overnight this is the salicylic acid. Chemical equation for preparation of aspirin:

Step 2 is as follows: a) Set up an apparatus as shown in figure 2 b) Measure out some of the Figure 2 salicylic acid that you have prepared this should be no more than 1g. place the salicylic acid in a reflux flask c) Add 4cm3 of ethanoic anhydride with no more than 8 drops of phosphoric acid (concentrated) this is the catalyst. d) Place the apparatus in a water bath in a fume cupboard. e) Warm mixture for 10 minutes f) Add some cool glacial ethanoic acid to the solution (about 4 cm3). g) Swirl the flask for 10 minutes h) The product should be filtered using a Buchner funnel and suction apparatus. i) The product should be washed with a bit of cool water and placed in a small beaker. j) Now repeat this step, with varying temperatures in the water bath. Label the flasks with the corresponding temperature; the products should be left overnight this is the aspirin. To find the purity of each aspirin sample, I will be carrying out aspirin assays; the procedure is as follows: a) Set up a titration apparatus as shown in figure 3. Burette b) Crush the sample of aspirin with a mortar and pestle. c) Weigh a specimen tube and note Stand down this weight d) Transfer the crushed aspirin from the mortar to the specimen tube; weigh the aspirin and specimen tube and note this down in a table.

Figure 3 Sodium hydroxid e solution

Clamp

Flask

ethanol

e) Measure out 10cm3 of ethanol (95%) in a beaker and place into a flask; add a few drops of phenolphthalein to view end point f) Place all the aspirin from the specimen tube to the flask; swirl until aspirin has all dissolved. g) Place 0.1 mol dm-3 sodium hydroxide solution in the burette (you will dilute 0.2 mol dm-3 sodium hydroxide to 0.1 mol dm3 sodium hydroxide); record the volume that you have placed in the burette (in a table) h) Titrate the solution in the flask; when a light pale pink colour comes into view, stop the titration and record volume of sodium hydroxide that was needed for this change to occur note this down in a table. i) Repeat the titration for each sample of aspirin j) Calculate the purity of aspirin using the following equations: Moles = concentration * volume 1000 And Moles = Mass Mr

EQUIPMENTS: Anti-bumping granules small irregular shaped materials that help a solution to boil more smoothly. Flask used to hold solutions/liquids or used for chemical reactions and/or processes. Condenser used as to cool hot gases/liquids in chemical processes such as distillation and reflux system; this equipment works by allowing cool water to move in and out through the water in and water out passages. Beaker used for the measurement of liquids/solutions or for their containment. They are usually marked as 100, 150, 200 or 250 ml (with markings between intervals); this is helpful whilst measuring out a fixed volume. Water Bath used for heating up reactions; very convenient when looking to carry out a reaction in a specific and controlled temperature. Buchner Funnel and suction used in the filtration of mixtures, so that desired substances can be separated from other compounds in the mixture.

Fume cupboard used to limit exposure of chemist to harmful gases. Burette long cylindrical glassware used in the laboratory to hold liquid reagents; common in titration experiments, such as neutralisation reactions. Extremely suitable to this investigation as it is very precise (tolerance of 0.05 cm3). Clamp used in laboratory experiments, usually to hold a burette in fixed vertical position. Clamp stand used to hold the clamp itself in a fixed position. Funnel for use when pouring liquid reagent into the burette. Pipette may be needed to transfer small volumes of a substance, such as the phenolphthalein indicator.