Unit 4: Laboratory Techniques and their Application
Learning aim C : Explore manufacturing techniques and testing
methods for an organic solid
EVERYTHING YOU RESEARCH NEEDS TO BE REFERENCED.
For pass standard, learners will correctly and competently follow given techniques and procedures to prepare and test their
organic solid. Learners will use the techniques of vacuum filtration, filtration through filter paper, solvent extraction and
recrystallisation. They will measure the melting point of the organic solid prepared from reaction and extraction, and carry out a
mixed-melting point measurement on the two samples, using a pure sample as a comparison. It is expected that at pass
standard learners will be given support to assemble the equipment associated with these techniques safely. Learners will draw
simple conclusions about the purity of the samples based on the tests carried out. Learners will research the industrial
production and testing of the solid and describe the scale, equipment, testing and the raw materials used to produce the solid.
The information should be in learners’ own words and all reference sources should be acknowledged.
PASS
Introduction:
An introduction to the assignment, what you will be looking at in your report (use assignment brief context).
I am a lab technician working in the research and development department of a pharmaceutical company. One of the
products made by the company is aspirin. I am going to be investigating how to produce and test the purity of aspirin so that
the company can make it efficiently. I will produce a sample of aspirin and test its purity. I will then compare my laboratory
technique with the industrial process used by the pharmaceutical company to manufacture aspirin on a large scale.
What is aspirin, what is it used for?
Acetylsalicylic acid is a generic name for aspirin, which is a commonly used medicine that has anti-inflammatory, fever-reducing
and pain-relieving properties. Aspirin was first made from willow bark and has long been an essential in the medical community.
Aspirin is a member of the nonsteroidal anti-inflammatory drug class, and it works by preventing the activity of cyclooxygenases,
which are enzymes involved in the synthesis of prostaglandins, which are chemicals linked to fever, inflammation, and pain.
Aspirin is frequently used to treat mild to moderate pain, lower temperature, and reduce inflammation because of its many
uses. It is also well known for having an blood-thinning effect, which helps to prevent blood clots and lower the risk of
cardiovascular events including strokes and heart attacks. Aspirin is commonly prescribed as an over-the-counter drug due to its
wide range of applications. It comes in different forms such as tablets, chewable tablets, and pill form. As aspirin can have
negative effects and mix with other medications, it is important that it is used sensibly and under a healthcare professional's
supervision.
Synthesis of Aspirin
Risk Assessment for synthesis of aspirin.
Risk Hazard Precaution
Salicylic acid Irritation to eyes and skin Avoid contact with eyes and skin.
Ethanoic anhydride Flammable and dangerous if swallowed. Avoid contact with fire and do not ingest
Concentrated Sulfuric acid Can irritate and cause burns to the skin and eyes Wear PPE such as eye goggles to protect
in worst cases can cause blindness yourself during the experiment
Glassware Can shatter and you can cut yourself. Keeping glass in Centre of desk.
Method for Synthesis of Aspirin
Equipment
2-hydroxybenzoic acid (Salicylic acid)
Ethanoic anhydride
Conical flask
Measuring cylinder
Pipette
, Stopwatch
Distilled water
Mixing rod
Buchner funnel
Vacuum pump
Filter paper
Watch glass
Spatula
Method
1. Record the mass of the empty Conical flask.
2. Then weight 6g of 2-hydroxybenzoic acid (Salicylic acid) into the conical flask and record the exact mass used.
3. Then inside a fume cupboard measure 10cm3 of ethanoic anhydride into a measuring cylinder and pour it into the conical
flask slowly whilst swirling the contents.
4. Then inside the fume cupboard use a pipette to add 5 drops of CH 2SO4 and then swirl the mixture and wait 2 minutes.
5. On a stopwatch for twenty minutes and place the conical flask in a water bath set at 60°C, during these twenty minutes
make sure to continuously swirl the conical flask.
6. Then allow the flask to cool and measure 75cm3 of distilled water into a measuring cylinder and pour it into the conical
flask, then using a mixing rod gently stir well in order to precipitate the solid 2-ethanoyloxybenzoic acid (aspirin).
7. Then attach the Buchner funnel to the vacuum pump and turn it on, then place a sheet of filter paper onto the Buchner
funnel and pour the mixture inside the conical flask into the funnel. Once you have poured the mixture if there is still some
undissolved aspirin inside the conical flask use distilled water to re-rinse the conical flak to increase the yield of aspirin.
8. Continue vacuuming the aspirin until no water is no longer coming out then off the vacuum pump.
9. Next weigh an empty watch glass and record the mass then transfer the solid from the Buchner funnel ono the watch glass
using a spatula.
10. Leave the aspirin to dry once it has dried, re weight the mass of the watch glass and solid.
11. Finally calculate the percentage and theoretical yield of aspirin and transfer your sample into a clean labelled sample tube
ready for recrystallisation.
Explain why each step was taken, what happened at each stage?
I first weighed 6g of salicylic acid out carefully into a conical flask in order to determine the starting amount of salicylic acid so
that this could be used later on to calculate the theoretical yield as this was the limiting reactant in the reaction. I then added
ethanoic anhydride to my conical flask inside the fume cupboard and swirled it around in order to speed up the reaction. Next, I
added five drops of sulfuric acid into my conical flask whilst swirling, this was added as a catalyst in order to speed up the rate of
reaction without being used up itself this was done inside of a fume cupboard for my safety due to the corrosiveness of sulfuric
acid. I then placed my conical flask into a water bath for 20 minutes whilst continuously swirling in order to heat the reaction
mixture thoroughly and speed up the reaction by increasing the collisions between molecules. I then added cold distilled water
into the conical flask and used a mixing rod to precipitate the solid aspirin, as the aspirin had a lower solubility in cold water. I
used reduced pressure filtration in order to separate the solid aspirin from the liquid mixture. The solid aspirin was then
transferred to an empty watch glass for further drying in order to remove any remaining water from the solid. Once the aspirin
had completely dried, I measured the mass so that I could calculate the actual yield of aspirin produced.
What steps did you do in your method and testing that were skillful?
When carrying out the method for the synthesis of aspirin, I carried out several skillful steps which required me to ensure
attention to detail and precision. Firstly, I took great detail when measuring my limiting reactant in this case salicylic acid, as this
was crucial for obtaining a good yield. I then added ethanoic anhydride to my conical flask inside the fume cupboard as my
reagent was dangerous and volatile, which showed that I understood the hazards of my experiment and how to keep myself
safe, showcasing my responsible lab practice skills. In order to maintain the temperature to a specified range when heating my
mixture, I used a water bath set at 60°C during my experiment, whilst making sure to continuously swirl my conical flask to
control and monitor the temperature and obtain an optimal yield and high product quality. After this I used reduced filter
filtration in order to dry my product faster and prevent my product from decomposing. I then carefully transferred my product
into an empty watch glass using a spatula making sure not to drop any product as this would have affected my overall product
yield, which highlighted my proficiency in the laboratory. Finally, I used my mass at the start and end to find the theoretical and
percentage yield of my results.
Learning aim C : Explore manufacturing techniques and testing
methods for an organic solid
EVERYTHING YOU RESEARCH NEEDS TO BE REFERENCED.
For pass standard, learners will correctly and competently follow given techniques and procedures to prepare and test their
organic solid. Learners will use the techniques of vacuum filtration, filtration through filter paper, solvent extraction and
recrystallisation. They will measure the melting point of the organic solid prepared from reaction and extraction, and carry out a
mixed-melting point measurement on the two samples, using a pure sample as a comparison. It is expected that at pass
standard learners will be given support to assemble the equipment associated with these techniques safely. Learners will draw
simple conclusions about the purity of the samples based on the tests carried out. Learners will research the industrial
production and testing of the solid and describe the scale, equipment, testing and the raw materials used to produce the solid.
The information should be in learners’ own words and all reference sources should be acknowledged.
PASS
Introduction:
An introduction to the assignment, what you will be looking at in your report (use assignment brief context).
I am a lab technician working in the research and development department of a pharmaceutical company. One of the
products made by the company is aspirin. I am going to be investigating how to produce and test the purity of aspirin so that
the company can make it efficiently. I will produce a sample of aspirin and test its purity. I will then compare my laboratory
technique with the industrial process used by the pharmaceutical company to manufacture aspirin on a large scale.
What is aspirin, what is it used for?
Acetylsalicylic acid is a generic name for aspirin, which is a commonly used medicine that has anti-inflammatory, fever-reducing
and pain-relieving properties. Aspirin was first made from willow bark and has long been an essential in the medical community.
Aspirin is a member of the nonsteroidal anti-inflammatory drug class, and it works by preventing the activity of cyclooxygenases,
which are enzymes involved in the synthesis of prostaglandins, which are chemicals linked to fever, inflammation, and pain.
Aspirin is frequently used to treat mild to moderate pain, lower temperature, and reduce inflammation because of its many
uses. It is also well known for having an blood-thinning effect, which helps to prevent blood clots and lower the risk of
cardiovascular events including strokes and heart attacks. Aspirin is commonly prescribed as an over-the-counter drug due to its
wide range of applications. It comes in different forms such as tablets, chewable tablets, and pill form. As aspirin can have
negative effects and mix with other medications, it is important that it is used sensibly and under a healthcare professional's
supervision.
Synthesis of Aspirin
Risk Assessment for synthesis of aspirin.
Risk Hazard Precaution
Salicylic acid Irritation to eyes and skin Avoid contact with eyes and skin.
Ethanoic anhydride Flammable and dangerous if swallowed. Avoid contact with fire and do not ingest
Concentrated Sulfuric acid Can irritate and cause burns to the skin and eyes Wear PPE such as eye goggles to protect
in worst cases can cause blindness yourself during the experiment
Glassware Can shatter and you can cut yourself. Keeping glass in Centre of desk.
Method for Synthesis of Aspirin
Equipment
2-hydroxybenzoic acid (Salicylic acid)
Ethanoic anhydride
Conical flask
Measuring cylinder
Pipette
, Stopwatch
Distilled water
Mixing rod
Buchner funnel
Vacuum pump
Filter paper
Watch glass
Spatula
Method
1. Record the mass of the empty Conical flask.
2. Then weight 6g of 2-hydroxybenzoic acid (Salicylic acid) into the conical flask and record the exact mass used.
3. Then inside a fume cupboard measure 10cm3 of ethanoic anhydride into a measuring cylinder and pour it into the conical
flask slowly whilst swirling the contents.
4. Then inside the fume cupboard use a pipette to add 5 drops of CH 2SO4 and then swirl the mixture and wait 2 minutes.
5. On a stopwatch for twenty minutes and place the conical flask in a water bath set at 60°C, during these twenty minutes
make sure to continuously swirl the conical flask.
6. Then allow the flask to cool and measure 75cm3 of distilled water into a measuring cylinder and pour it into the conical
flask, then using a mixing rod gently stir well in order to precipitate the solid 2-ethanoyloxybenzoic acid (aspirin).
7. Then attach the Buchner funnel to the vacuum pump and turn it on, then place a sheet of filter paper onto the Buchner
funnel and pour the mixture inside the conical flask into the funnel. Once you have poured the mixture if there is still some
undissolved aspirin inside the conical flask use distilled water to re-rinse the conical flak to increase the yield of aspirin.
8. Continue vacuuming the aspirin until no water is no longer coming out then off the vacuum pump.
9. Next weigh an empty watch glass and record the mass then transfer the solid from the Buchner funnel ono the watch glass
using a spatula.
10. Leave the aspirin to dry once it has dried, re weight the mass of the watch glass and solid.
11. Finally calculate the percentage and theoretical yield of aspirin and transfer your sample into a clean labelled sample tube
ready for recrystallisation.
Explain why each step was taken, what happened at each stage?
I first weighed 6g of salicylic acid out carefully into a conical flask in order to determine the starting amount of salicylic acid so
that this could be used later on to calculate the theoretical yield as this was the limiting reactant in the reaction. I then added
ethanoic anhydride to my conical flask inside the fume cupboard and swirled it around in order to speed up the reaction. Next, I
added five drops of sulfuric acid into my conical flask whilst swirling, this was added as a catalyst in order to speed up the rate of
reaction without being used up itself this was done inside of a fume cupboard for my safety due to the corrosiveness of sulfuric
acid. I then placed my conical flask into a water bath for 20 minutes whilst continuously swirling in order to heat the reaction
mixture thoroughly and speed up the reaction by increasing the collisions between molecules. I then added cold distilled water
into the conical flask and used a mixing rod to precipitate the solid aspirin, as the aspirin had a lower solubility in cold water. I
used reduced pressure filtration in order to separate the solid aspirin from the liquid mixture. The solid aspirin was then
transferred to an empty watch glass for further drying in order to remove any remaining water from the solid. Once the aspirin
had completely dried, I measured the mass so that I could calculate the actual yield of aspirin produced.
What steps did you do in your method and testing that were skillful?
When carrying out the method for the synthesis of aspirin, I carried out several skillful steps which required me to ensure
attention to detail and precision. Firstly, I took great detail when measuring my limiting reactant in this case salicylic acid, as this
was crucial for obtaining a good yield. I then added ethanoic anhydride to my conical flask inside the fume cupboard as my
reagent was dangerous and volatile, which showed that I understood the hazards of my experiment and how to keep myself
safe, showcasing my responsible lab practice skills. In order to maintain the temperature to a specified range when heating my
mixture, I used a water bath set at 60°C during my experiment, whilst making sure to continuously swirl my conical flask to
control and monitor the temperature and obtain an optimal yield and high product quality. After this I used reduced filter
filtration in order to dry my product faster and prevent my product from decomposing. I then carefully transferred my product
into an empty watch glass using a spatula making sure not to drop any product as this would have affected my overall product
yield, which highlighted my proficiency in the laboratory. Finally, I used my mass at the start and end to find the theoretical and
percentage yield of my results.
