[UNIT 4C]
[MAKING ASPIRIN]
07/03/2023
LEVEL 3 APPLIED SCIENCE
CHEMISTRY
P.5
RISK ASSESMENT
Acetylsalicylic Acid: Risk: - Inhalation of dust
can cause irritation to the upper respiratory
tract and lungs. - Skin contact can cause
irritation and redness. - Eye contact can cause
severe irritation and burning. - Ingestion can
cause gastrointestinal irritation, nausea, and
,vomiting. Controls: - Wear protective clothing,
gloves, and protective eyewear when handling
the powder. - Wear a dust mask when handling
the powder. - Wash hands thoroughly after
handling. - Store in a cool, dry place away from
heat and flame.
Acetic Acid: Risk: - Inhalation of vapor can
cause respiratory irritation and breathing
difficulty. - Skin contact can cause irritation
and burns. - Eye contact can cause irritation
and burns. - Ingestion can cause irritation and
burns to the mouth, throat, and stomach.
Controls: - Wear protective clothing, gloves,
and protective eyewear when handling the
acid. - Wear a dust mask when handling the
acid. - Wash hands thoroughly after handling.
- Store in a cool, dry place away from heat and
flame.
Acetic Anhydride: Risk: - Inhalation of fumes
can cause irritation to the upper respiratory
tract and lungs. - Skin contact can cause
irritation and redness. - Eye contact can cause
severe irritation and burns. - Ingestion can
cause severe irritation and burns to the mouth,
throat, and stomach. Controls: - Wear
protective clothing, gloves, and protective
eyewear when handling the anhydride. - Wear
a dust mask when handling the anhydride. -
Wash hands thoroughly after handling. - Store
in a cool, dry place away from heat and flame.
Salicylic Acid: Risk: - Inhalation of dust can
cause irritation to the upper respiratory tract
and lungs. - Skin contact can cause irritation
and redness. - Eye contact can cause irritation
and burning. - Ingestion can cause
gastrointestinal irritation, nausea, and
vomiting. Controls: - Wear protective clothing,
gloves, and protective eyewear when handling
the powder. - Wear a dust mask when handling
the powder. - Wash hands thoroughly after
handling. - Store in a cool, dry place away from
heat and flame.
Sulfuric Acid: Risk: - Inhalation of vapor can
cause irritation to the upper respiratory tract
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,and lungs. - Skin contact can cause irritation
and burns. - Eye contact can cause severe
irritation and burns. - Ingestion can cause
severe irritation and burns to the mouth,
throat, and stomach. Controls: - Wear
protective clothing, gloves, and protective
eyewear when handling the acid. - Wear a dust
mask when handling the acid. - Wash hands
thoroughly after handling. - Store in a cool, dry
place away from heat and flame.
Phosphoric Acid: Risk: - Inhalation of vapor
can cause irritation to the upper respiratory
tract and lungs. - Skin contact can cause
irritation and burns. - Eye contact can cause
irritation and burns. - Ingestion can cause
irritation and burns to the mouth, throat, and
stomach. Controls: - Wear protective clothing,
gloves, and protective eyewear when handling
the acid. - Wear a dust mask when handling
the acid. - Wash hands thoroughly after
handling. - Store in a cool, dry place away from
heat and flame.
Benzene: Risk: - Inhalation of vapor can cause
irritation to the upper respiratory tract and
lungs. - Skin contact can cause irritation and
burns. - Eye contact can cause irritation and
burns. - Ingestion can cause irritation and
burns to the mouth, throat, and stomach.
Controls: - Wear protective clothing, gloves,
and protective eyewear when handling the
liquid. - Wear a dust mask when handling the
liquid. - Wash hands thoroughly after
handling. - Store in a cool, dry place away from
heat and flame.
Toluene: Risk: - Inhalation of vapor can cause
irritation to the upper respiratory tract and
lungs. - Skin contact can cause irritation and
burns. - Eye contact can cause irritation and
burns. - Ingestion can cause irritation and
burns to the mouth, throat, and stomach.
Controls: - Wear protective clothing, gloves,
and protective eyewear when handling the
liquid. - Wear a dust mask when handling the
liquid. - Wash hands thoroughly after
handling. - Store in a cool, dry place away from
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,heat and flame.
Ethanoic Acid: Risk: - Inhalation of vapor can
cause irritation to the upper respiratory tract
and lungs. - Skin contact can cause irritation
and burns. - Eye contact can cause irritation
and burns. - Ingestion can cause irritation and
burns to the mouth, throat, and stomach.
Controls: - Wear protective clothing, gloves,
and protective eyewear when handling the
acid. - Wear a dust mask when handling the
acid. - Wash hands thoroughly after handling.
- Store in a cool, dry place away from heat and
flame.
INTRODUCTION
Aspirin is a synthetic compound derived from salicylic acid, and the industrial production of aspirin
involves several steps, including synthesis, purification, and packaging. This paper will discuss the
various processes involved in the industrial production of aspirin, as well as the various safety steps
taken to ensure quality control. The paper will also discuss the environmental implications of aspirin
production and how the industry is working to reduce its impact on the environment. Finally, the
paper will discuss the various regulations in place to ensure the safety of consumers.
Equipment list:
Laboratory:
1. Beakers
2. Test tubes
3. Funnels
4. Glass rods
5. Hot plates
6. Erlenmeyer flasks
7. Thermometers
8. Pipettes
9. Glassware
10. Graduated cylinders
11.Evaporating dish
12.Small conical flask
13.Sample vial
14.2 pipette fillers
15.2 pipettes
16. Plugged pipette
17.Buchner funnel, flask & vacuum pump (recrystallisation apparatus)
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,Industry:
1. Reactors
2. Filters
3. Grinders
4. Evaporators
5. Centrifuges
6. Separators
7. Dryers
8. Blenders
9. Distillation columns
10. Analytical instrument
P.6
[MANUFACTURE AND TESTING]
Industrial aspirin manufacture begins with salicylic acid extraction from the bark of
the willow tree. The salicylic acid is then reacted with acetic anhydride to form
aspirin. The aspirin is then purified through filtration and recrystallization.
Testing of aspirin typically involves measuring the purity of the aspirin, testing for
the presence of impurities, and testing for stability. Purity is typically measured
using high performance liquid chromatography (HPLC). Impurities are tested by
examining by-products such as salicylic acid, acetic acid, and other compounds.
Stability is tested by measuring the temperature at which the aspirin melts and the
degree to which the aspirin degrades over time.
The laboratory manufacture and testing of aspirin is typically done on a small scale
in a lab setting, using reagents and special laboratory equipment. The process
typically involves synthesizing the aspirin and then testing it for purity and
strength. Industrial manufacture and testing of aspirin is done on a much larger
scale and involves using large-scale chemical processes, such as reaction vessels and
distillation columns, to produce the aspirin. The aspirin is then tested for purity and
strength using automated systems and quality control systems. In addition, the
industrial process often involves added steps such as drying and packaging the
aspirin before it is shipped.
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,[INDUSTRY AND LABORATORY]
Laboratory manufacture and testing of
an organic solid typically involves the
synthesis of small batches of the
compound using manually ran
laboratory equipment and analytical
methods. This includes various
purification techniques to obtain a pure
sample, followed by characterization
using a variety of analytical techniques
such as spectroscopy, chromatography,
and thermal analysis.
Industrial manufacture and testing of
an organic solid involves the large-
scale production of the compound in a
chemical plant. This typically requires
large-scale equipment such as reactors,
distillation columns, and centrifuges.
Quality control is also important and
requires automated analytical
instruments such as HPLC (High
performance liquid Chromatography),
GC (Gas Chromatography), and other
specialized analytical methods.
Furthermore, industrial manufacture
also involves the use of a variety of
safety protocols and procedures to
ensure the quality and safety of the
final product.
Laboratory manufacture of aspirin
involves the careful mixing of precise
amounts of ingredients in a controlled
environment to produce a small
number of aspirin. The ingredients are
usually carefully weighed and
combined using a variety of techniques,
such as distillation or titration. The
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,Solvents and catalysts are necessary components of aspirin production, both in the
laboratory and industrial setting. In the laboratory, solvents such as ethanol and
acetic acid are commonly used to dissolve the starting materials and ease the
reaction. Catalysts, such as sulfuric acid and acetic anhydride, are then used to speed
up the reaction and improve the yield.
In industrial settings, solvents such as benzene and toluene are often used to improve
the reaction rate and increase the yield. Catalysts such as sulfuric/phosphoric acid
are used to speed up the reaction and improve the efficiency of the process. These
catalysts are more effective than laboratory catalysts due to their greater solubility
and reactivity.
The relevance of solvents and catalysts to industrial aspirin production lies in their
ability to speed up the reaction and improve the yield. By using more efficient
catalysts and solvents, manufacturers can reduce the time and cost associated with
production, resulting in better quality products at a lower cost.
The yield and purity of an organic solid in the laboratory are affected by a variety of
factors. These include the type of reaction used, the reactants used, the solvent used,
the temperature, the pressure, the duration of the reaction, the equipment used, and
the purification steps taken.
The type of reaction used affects the yield and purity of the product because different
reactions can produce assorted products with varying yields and purities. For
example, a nucleophilic substitution reaction may produce a product with a higher
yield and better purity than an elimination reaction.
The reactants used also affect the yield and purity of the product. Different reactants
may produce assorted products with different yields and purities depending on the
reaction conditions. For example, the use of different catalysts or solvents may
produce assorted products with different yields and purities.
The solvent used affects the yield and purity of the product because different solvents
can affect the rate of reaction, the product formed, and the amount of product formed.
For example, a polar solvent may speed up a reaction and produce a higher yield of
product than a non-polar solvent. The temperature of the reaction also affects the
yield and purity of the product.
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,Different temperatures can affect the rate of reaction, the product formed, and the
amount of product formed. For example, a higher temperature may speed up a
reaction and produce a higher yield of product than a lower temperature. The
pressure of the reaction also affects the yield and purity of the product.
Different pressures can affect the rate of reaction, the product formed, and the
amount of product formed. For example, a higher pressure may speed up a reaction
and produce a higher yield of product than a lower pressure.
The duration of the reaction affects the yield and purity of the product because
different lengths of time for a reaction can affect the product formed and the amount
of product formed. For example, a longer reaction time may produce a higher yield of
product than a shorter reaction time. The equipment used also affects the yield and
purity of the product.
Diverse types of equipment can affect the rate of reaction, the product formed, and
the amount of product formed. For example, using a more efficient reactor may
produce a higher yield of product than using a less efficient reactor. The purification
steps taken also affect the yield and purity of the product.
Different purification methods can affect the purity of the product produced. For
example, using chromatography may produce a higher purity product than other
methods. These factors are relevant to industrial manufacture because they can affect
the yield and purity of the product produced. Different reaction conditions can
produce assorted products with different yields and purities. Therefore, it is
important for industrial manufacturers to consider these factors to perfect their
process and produce a high yield and pure product.
H 2SO4
C7H6O3 + (CH3CO)2O C9H804 + CH3COOH
Atom economy: Mr. of desired product/Mr. of all reactants x 100 180/240
x 100-->0.75(100) =75%
Atom economy is a tool used to measure the efficiency of a chemical reaction or a
synthesis. Calculating the atom economy of the synthesis of aspirin helps scientists to
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,understand how much of the starting materials are converted into the desired
product. This helps to find any possible waste and to develop more efficient and
environmentally friendly syntheses.
This means that 75% of the total mass of the reactants ends up as the desired product.
The remaining 25% may be lost as by-products, unreacted starting materials, or
other waste.
1. Sulfuric Acid
2. Salicylic acid
3. Acetic anhydride
4. Aspirin
5. Acetic Acid
Stage 1: Make the product under reflux
Take about 2 g of 2-hydroxybenzoic acid (salicylic acid). Weigh and record the
exact mass in a round bottom flask.
Add 4 cm³ of ethanoic anhydride, followed by 5 drops of phosphoric/ sulphuric
acid. This needs to be done in a fume cupboard.
Clamp your flask, attach the condenser and check the water flow. Make sure the
quick fit apparatus is watertight.
Warm and swirl the mixture in an Iso mantle/water bath over Bunsen until all
the solid has dissolved. Heat for a further 10 minutes.
Do not excessively boil the mixture. Keep the Iso mantle on low (below 60
degrees). The mixture should not change colour.
Stage 2: Separate the impurities using filtration
6 Allow the mixture to cool before dismantling the condenser.
7 Carefully add 5 cm³ of cold distilled water to your solution.
8 Leave in an ice bath until all the solid has formed. You may need to stir with a
glass rod.
9 Filter the product using a Buchner filter and wash with ice chilly water. Use
double filter paper and moisten it before filtering.
10 Recrystallize the product from the smallest possible amount of hot distilled
water.
11 The product can be left in an oven overnight to dry.
Stage 3: Decide the yield of aspirin
12 Weigh your product.
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, 13 Determine the theoretical yield based on the moles of 2-hydroxybenzoic acid
used.
14 Calculate your percentage yield.
Stage 4: Check the purity by TLC and melting point
15 Put a sample amount of the product in a sealed capillary tube and use the
melting point apparatus to decide the melting point.
16 Run a TLC plate of your sample against a sample of pure aspirin.
17 Write a lab report on your preparation of aspirin. Your report should
include:
any alterations to the method results (yield, melting point and R, values)
calculations (atom economy, percentage yield, R.)
discussion: what factors affected the purity and yield of your aspirin
conclusion: use your discussions and literature values of melting point and R, to
assess the quality of your product.
Recrystallisation:
1.Heat up solvent and reagent.
2.Add activated charcoal and filter out the solution.
3.Place the solution in an ice bath for further cooling.
4-Cool down the solution to room temperature.
5-Enjoy your newly formed crystals.
P.5
Techniques:
-Vacuum filtration: Vacuum filtration is a technique used to separate a solid from a
liquid. It is done by passing the mixture through a filter paper in a Buchner funnel,
under a vacuum. The solid is kept on the filter paper, while the liquid passes through
and is collected in a flask. The vacuum helps to speed up the filtration process.
-Filtration through filter paper: Filtration through filter paper is a technique used to
separate a solid from a liquid. It is done by passing the mixture through a filter paper,
which keeps the solid particles while allowing the liquid to pass through. The solid is
then collected by vacuum filtration. This is to remove any impurities.
-Testing purity by melting point: Testing purity by melting point is a technique used
to find a compound or to verify its purity. It is done by measuring the melting point of
a sample and comparing it to the known melting point of the compound. If the
melting points are similar, the sample is likely to be pure. A sample of the purified
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