BTEC Level 3 National Foundation Diploma in Applied
Qualification
Science
Unit number and title Unit 4: Laboratory Techniques and their Application
C: Explore manufacturing techniques and testing methods
Learning aim
for an organic solid
Assignment title Manufacturing Aspirin
P5 Correctly prepare and test the purity of an organic solid and draw conclusions
M4 Demonstrate skilful application of techniques in preparing and testing the purity
of an organic solid and draw detailed conclusions.
Method
1. Firstly set up the apparatus, making
sure the glassware is set up
correctly, to heat up the mixture. To
create the mixture, add about 2.0g of
salicylic acid and record the mass
used, with 4cm3 of ethanoic
anhydride and 5 drops of 85%
phosphoric acid to a 50cm3 pear
shaped flask, ensuring that the
ethanoic anhydride and the
phosphoric acid is kept in the fume
cupboard for health and safety, for example, the fumes
produced can cause lung and eye damage. Then swirl the mixture.The phosphoric
acid is used to help speed up a reaction, where it transfers protons, as it gives
hydrogen protons to the other atoms, therefore, if we didn't add phosphoric acid, the
reaction would be slower. Also, if we didn’t accurately measure out the ethanoic
anhydride carefully, the results would’ve been inaccurate.
2. Next, heat up the mixture for 5 minutes, to do this, use a heating mantle, not a
bunsen burner because the reactions may be highly flammable and fit the pear
shaped flask with a reflux condenser, this condenser will stop any vapour from
escaping. When the reflux has finished heating, turn off the heating mantle.
Moreover, it is important to not heat up the mixture for too long, this is because it
can burn and give out fumes, this causes the eyes to water and hurt.
3. Add 2cm3 of water down the condenser, while the mixture is still hot, this is so that
the excess ethanoic anhydride can hydrolyse, however, whilst doing this step, be
careful because the equipment will be hot. Also, if we didn't add enough water, the
contents in the flask wouldn’t boil and the excess ethanoic anhydride won’t
hydrolyze correctly.
4. Let the mixture cool down a little before pouring the mixture into a small beaker,
therefore it won’t burn the hands. Add 40cm3 of cold water to a 100cm3 beaker and
add the mixture to it. Then stir the sides using a stirring rod. If too less or too little
cold water is added, this may affect the crystallization process.
5. Let the mixture stand in an ice bath for crystallization to occur. If it isn’t left to
crystalise long enough, it might cause error and make the results inaccurate.
6. Using a buchner funnel and a suction apparatus, filter the product but make sure all
the product is there to be filtered, therefore the results don’t get affected, also
ensure that plenty of time is given for the liquid to be sucked into the funnel. In
, addition, this product needs to be dry, otherwise this affects the purity of the
product. This is the sample of the impure aspirin. Using the vacuum filtration
method with a buchner funnel increases the speed of the filtration, therefore it
removes the impure solid from the liquid faster, and reduces the pressure.
7. From this step is the recrystallization process, which is the method to purify the
product, where all the impure product is dissolved in warmed and cooled water.
8. Add the impure aspirin to a 100cm3 conical flask, and then a hot water bath, with
minimum quantity hot water, this is to keep the conical flask hot.
9. Next, filter the insoluble impurities, this is done by using gravity filtration, which is a
simple filtration with the use of fluted filter paper in a filter funnel, the use of the fold
will remove impure solid from the liquid quicker because the centre surface is
larger, in the water bath to prevent the soluble product from crystallizing out of the
solution. Ensure that there is minimum insoluble impurities so that the results are
accurate.
10. Then cool the solution so it is at room temperature, and add it to an ice bath so the
aspirin will crystallize out of the solution, which leaves the impurities in the solvent.
11. The formed crystals then need to be filtered using the suction filtration, and the
glass container has to be washed out with distilled water, so that all, or most of the
aspirin is transferred.
12. Wash the aspirin crystals with cold water, this must be done while the aspirin is dry
by sucking air over them.
13. Remove the filter paper and add it to a sample bottle, and leave the sample to dry
14. The next day, find the mass of the sample bottles, do this by removing the lid. Then
find the mass of pure aspirin made by taking the mass of the filter paper and the
mass of the sample bottle away from the total mass, this meant that for my results it
was the following:
Mass of Aspirin, with the sample bottle and filter paper: 20.87g
Mass of filter paper: 0.31g
Mass of sample bottle: 20.22g
Mass of filter paper and sample bottle: 20.53g
Mass of Pure aspirin: 0.34g
15. I then needed to determine the melting point of the aspirin, which should be around
135 degrees. The melting point of my aspirin was 101 degrees, this therefore tells
me that I have made a pure substance, with a difference of 34 degrees below.
There are some risks of this experiment, such as some of the measurements may be
inaccurate, therefore the aspirin wouldn’t work correctly and something may happen to
someone who takes this. Also, the wrong filter may be used, therefore some of the
mixtures that should’ve gone are still in therefore this product might not be correct. Also,
the water baths should’ve all been set at the same temperature so that at all the steps that
have needed a water bath that it is always the same. In addition to this, if my melting point
was to be far from the value 135 degrees, this wouldn’t have been pure aspirin.
Results
Mass of Salicylic at the start (g) 2.00
2
BTEC Assignment Brief v1.0
BTEC Internal Assessment QDAM January 2015
Qualification
Science
Unit number and title Unit 4: Laboratory Techniques and their Application
C: Explore manufacturing techniques and testing methods
Learning aim
for an organic solid
Assignment title Manufacturing Aspirin
P5 Correctly prepare and test the purity of an organic solid and draw conclusions
M4 Demonstrate skilful application of techniques in preparing and testing the purity
of an organic solid and draw detailed conclusions.
Method
1. Firstly set up the apparatus, making
sure the glassware is set up
correctly, to heat up the mixture. To
create the mixture, add about 2.0g of
salicylic acid and record the mass
used, with 4cm3 of ethanoic
anhydride and 5 drops of 85%
phosphoric acid to a 50cm3 pear
shaped flask, ensuring that the
ethanoic anhydride and the
phosphoric acid is kept in the fume
cupboard for health and safety, for example, the fumes
produced can cause lung and eye damage. Then swirl the mixture.The phosphoric
acid is used to help speed up a reaction, where it transfers protons, as it gives
hydrogen protons to the other atoms, therefore, if we didn't add phosphoric acid, the
reaction would be slower. Also, if we didn’t accurately measure out the ethanoic
anhydride carefully, the results would’ve been inaccurate.
2. Next, heat up the mixture for 5 minutes, to do this, use a heating mantle, not a
bunsen burner because the reactions may be highly flammable and fit the pear
shaped flask with a reflux condenser, this condenser will stop any vapour from
escaping. When the reflux has finished heating, turn off the heating mantle.
Moreover, it is important to not heat up the mixture for too long, this is because it
can burn and give out fumes, this causes the eyes to water and hurt.
3. Add 2cm3 of water down the condenser, while the mixture is still hot, this is so that
the excess ethanoic anhydride can hydrolyse, however, whilst doing this step, be
careful because the equipment will be hot. Also, if we didn't add enough water, the
contents in the flask wouldn’t boil and the excess ethanoic anhydride won’t
hydrolyze correctly.
4. Let the mixture cool down a little before pouring the mixture into a small beaker,
therefore it won’t burn the hands. Add 40cm3 of cold water to a 100cm3 beaker and
add the mixture to it. Then stir the sides using a stirring rod. If too less or too little
cold water is added, this may affect the crystallization process.
5. Let the mixture stand in an ice bath for crystallization to occur. If it isn’t left to
crystalise long enough, it might cause error and make the results inaccurate.
6. Using a buchner funnel and a suction apparatus, filter the product but make sure all
the product is there to be filtered, therefore the results don’t get affected, also
ensure that plenty of time is given for the liquid to be sucked into the funnel. In
, addition, this product needs to be dry, otherwise this affects the purity of the
product. This is the sample of the impure aspirin. Using the vacuum filtration
method with a buchner funnel increases the speed of the filtration, therefore it
removes the impure solid from the liquid faster, and reduces the pressure.
7. From this step is the recrystallization process, which is the method to purify the
product, where all the impure product is dissolved in warmed and cooled water.
8. Add the impure aspirin to a 100cm3 conical flask, and then a hot water bath, with
minimum quantity hot water, this is to keep the conical flask hot.
9. Next, filter the insoluble impurities, this is done by using gravity filtration, which is a
simple filtration with the use of fluted filter paper in a filter funnel, the use of the fold
will remove impure solid from the liquid quicker because the centre surface is
larger, in the water bath to prevent the soluble product from crystallizing out of the
solution. Ensure that there is minimum insoluble impurities so that the results are
accurate.
10. Then cool the solution so it is at room temperature, and add it to an ice bath so the
aspirin will crystallize out of the solution, which leaves the impurities in the solvent.
11. The formed crystals then need to be filtered using the suction filtration, and the
glass container has to be washed out with distilled water, so that all, or most of the
aspirin is transferred.
12. Wash the aspirin crystals with cold water, this must be done while the aspirin is dry
by sucking air over them.
13. Remove the filter paper and add it to a sample bottle, and leave the sample to dry
14. The next day, find the mass of the sample bottles, do this by removing the lid. Then
find the mass of pure aspirin made by taking the mass of the filter paper and the
mass of the sample bottle away from the total mass, this meant that for my results it
was the following:
Mass of Aspirin, with the sample bottle and filter paper: 20.87g
Mass of filter paper: 0.31g
Mass of sample bottle: 20.22g
Mass of filter paper and sample bottle: 20.53g
Mass of Pure aspirin: 0.34g
15. I then needed to determine the melting point of the aspirin, which should be around
135 degrees. The melting point of my aspirin was 101 degrees, this therefore tells
me that I have made a pure substance, with a difference of 34 degrees below.
There are some risks of this experiment, such as some of the measurements may be
inaccurate, therefore the aspirin wouldn’t work correctly and something may happen to
someone who takes this. Also, the wrong filter may be used, therefore some of the
mixtures that should’ve gone are still in therefore this product might not be correct. Also,
the water baths should’ve all been set at the same temperature so that at all the steps that
have needed a water bath that it is always the same. In addition to this, if my melting point
was to be far from the value 135 degrees, this wouldn’t have been pure aspirin.
Results
Mass of Salicylic at the start (g) 2.00
2
BTEC Assignment Brief v1.0
BTEC Internal Assessment QDAM January 2015
