ASSIGNMENT

Course Title: BTEC HND in Applied Sciences

Unit No. & Title Learning Outcomes

Unit 1 – Fundamentals of Laboratory
LOC 2
Techniques
Student Information

Student Name: Sankalpa D.M.K.S.

Reg.No:As/002/003 Pearson No: MD75258 Semester No: 01 Batch No: 02

Assignment Title Assignment 3 – Individual Assignment

Assessor Name Ms. Ann Deluxy David

Date Issued Deadline Submitted On
08/10/2020 29/10/2020 29/10/2020

Assessor Feedback Criteria Achievement

Final Grade Distinction
Awarded (Y / N)
AchievedVerification
Internal D2. Well done
Signature Date P3
IV Name Y
Action Plan
Signature Date
Assessor Name
D.R. Ann Deluxy 01/11/2020
P4
I understand the feedback given to me and agree to carry out the actions in future
Y works
Student as required and indicated.
Verification
Student Feedback M2
Y

D2
Y

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 ASSESSMENT DECLARATION FORM

Student Name

Pearson Reg No. Student Reg No.

PLEASE TICK TO INDICATE THAT YOU HAVE SATISFIED THESE REQUIREMENTS

This assignment is my own work, I have not participated in collusion, nor have I previously
submitted this or a version of it for assessment in any other Unit of Study.

I have taken proper and reasonable care to prevent this work from being copied by another
student.

I confirm that I have clearly indicated, by in text and end Referencing, where I have used
someone else’s graphics or data, concepts, words, irrespective of whether I have quoted or I
have paraphrased in my own words.

I have carefully read the assessment criteria that will be used to evaluate my work as given
below.

ASSESSMENT CRITERIA
I certify that the statements I have attested to above have been made in good faith and are true and
participated in collusion.

……………………………………. …29/10/2020……

Student Signature Date

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 Grading Matrix – Pass Criteria
Page Achieve
Learning Tas
Pass criteria numb d
outcome k
er Y/N
Grading Matrix – Distinction Criteria
Learning Distinction criteria Task Page Achie
outcome Undertake a procedure to synthesize and purify numb Yve d
LOC 2 an organic liquid 1.1 06e Y/N
r
LOC 2 1.3 06
Carry out 2.3
Carry out
synthetic Y
synthetic Evaluate the success of the syntheses
chemistry Y
chemistry n
techniques Undertake a procedure to synthesize and 2.1 06
techniques purify a

Grading Matrix – Merit Criteria

Learning Page Achieved
outcome Merit criteria Task number Y/N

Y
LOC 2
Carry out
Explain the reasons for carrying out the steps 1.2
synthetic 06
in the syntheses 2.2
chemistry
techniques

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 Possible
Learning Outcome Tasks
Evidence

P3 Undertake a procedure to synthesize and

1.1
purify an organic liquid

P4 Undertake a procedure to synthesize and

2.1
purify an organic solid

Assignment 3

M2 Explain the reasons for carrying out the steps 1.2

in the syntheses 2.2

D2 Evaluate the success of the syntheses 1.3

2.3

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 Acknowledgement

I like to thank the Asian institute of business and science for providing laboratory
facilities for student to study about laboratory techniques. It is important to
mention institute provide all necessary laboratory equipment to every student.
Also I like to thank again to module lecturer Ms. Ann Deluxy David for
providing guidelines and knowledge for us.

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Table of content

1. Synthesis of Ethyl acetate…………………………………………..

2. Synthesis of paracetamol……………………………………………

3. References………………………………………………………….

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 Synthesis of Ethyl acetate

Introduction

Ethyl ethanoate also name as Ethyl acetate is an organic compound that has a characteristic smell
and it is used in glues, nail polish and decaffeination process of tea and coffee. This is ester
obtain from reaction between ethanol and acetic acid. This is a condensation reaction.

CH3COOH (aq) + CH3CH2OH (aq) CH3COOCH2CH3 (aq) + H2O (liquid)

This is reversible reaction that creates equilibrium between product and reactant. We can
improve yield of ethyl ethanoate by removing water from the system using drying agent. Also
H2SO4 add to reactant mixture as catalyst. This reaction identified as esterification reaction
however the water molecule removes as result of combining the both ethanol and acetic acid.
Hence this reaction can consider as condensation reaction. After production of ethyl acetate
mixture we use distillation technique to isolate the ethyl acetate from by-product water (hobby
chemistr, 2014).

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Procedure use to prepare ethyl acetate and purify the ethyl acetate

We can produce ethyl acetate from reaction between ethanol and glacial acetic acid. We use
below mention procedure to synthesis.

In first step 30ml of ethanol, 30ml of glacial acetic acid and 6ml of 98% sulfuric acid was
measured out and ethanol and acetic acid mixed in round-bottom flask under ice bath. Then
sulfuric acid was added to mixture drop wise to avoid heat the mixture. After that flask was
connected to reflux condenser and solution was boiled gently for 30 minutes. Then simple
distillation method was applied until 2/3 of mixture was distilled off. Then distillate was
collected into beaker and it was introduce to separatory funnel. Then 3g of anhydrous Na2CO3
dissolve in 15ml distilled water was added to separatory funnel and mix the solvents in funnel.
Then funnel was kept in suitable time until layer separation happen. Then aqueous layer was
removed. Again 3g of anhydrous calcium chloride dissolve in 15ml of water was added to
separatory funnel and mix the solutions. Then funnel was kept for layer separation happen and

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after separation take place the aqueous layer was removed from funnel. In next step ethyl acetate
was drained into Erlenmeyer flask and the 1.5g anhydrous magnesium sulphate was added to
flask as drying agent. If we want we can use excess alcohol for this drying purpose. Then
solution was stirred for 20minutes using magnetic stirrer. Again ethyl acetate was decanted into
boiling flask and flask was set up for simple distillation. Distillation was done at 74-79 Celsius
degree. Then product was transferred into dark colour bottle and store in cool, dry place.

The reasons for carrying out the steps in the syntheses

We mixed ethanol and acetic acid in ice bath because this reaction is exothermic reaction. To
avoid heat the flask we use ice bath. Also concentrated sulfuric acid add drop wise to reduce risk
of heating the flask. Also this is done using ice bath. It also helps to avoid unnecessary heating of
the flask. Then using reflux condenser we boil the mixture for 30 minutes. Many reactions
including esterification reaction between covalent compounds are very slow processes. Hence to
obtain acceptable amount of product we use reflux technique in synthesis. The reactants are
dissolving in suitable solvent and the solution boil up to boiling point for generate vapour. Then
vapour condense and condensate allow returning into original solution. This process gives
enough thermal energy to complete the relevant reaction to produce high yield of products. The
reaction carried out under reflux can be for minutes, hours or even few days to promote the
completion of reaction. In our experiment we carried out reaction in 30 minutes. This reflux
helps to produce high yield of ethyl acetate. Then we apply simple distillation method.
Distillation can use to separate component in a liquid mixture based on their boiling point. The
liquid mixture boils to generate vapour. Then condensing the vapour and collect that condensate
in distillation process. We use this simple distillation to isolate ethyl acetate from reaction
mixture base on boiling point of the ethyl acetate. The esterification reaction is reversible
reaction. Hence there are reactant and product in mixture. Due to this reason we need to isolate
our product from reaction mixture containing by-product water and reactant ethanol and acetic
acid. Then we treated our solution mixture with anhydrous sodium carbonate to remove acetic
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acid in our mixture. The unreacted acetic acid in organic layer containing ethyl acetate product
easily move to aqueous layer containing sodium carbonate because acid react with sodium
carbonate to facilitate acid in organic layer rapidly distribute to aqueous layer. This is actually
done for isolate the ethyl acetate by removing other chemicals in mixture. Then we use
anhydrous calcium chloride to remove remaining unreacted ethanol from the mixture. This is
also done for isolate the product. However the by-product water still remains in our solution
containing ethyl acetate. Then we use drying agent to remove this water molecules to completely
isolate our product ethyl acetate. We use magnesium sulphate as drying agent. That is the reason
we add magnesium sulphate for solution. Again we use simple distillation technique to
completely isolate our product ethyl acetate. This is high flammable chemical. Also it evaporate
very easily and it is become toxic when inhaled happen. If it contact with eyes or skin it may lead
to irritation. Hence we store this ethyl acetate in glass bottle and seal it.

Evaluation of success of the syntheses

Results

In experiment using 30ml 0f ethanol and 30ml acetic acid we obtain 24.57ml of ethyl acetate.
(22.04g)

Analysis

Density of acetic acid = 1.0492g/ml

Number of moles of acetic acid = mass of acetic acid/ molar mass of acetic

acid Density of acid (d) = mass of acid (m)/ volume of acid (v)

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Hence,

Mass of acetic acid = dv

= (1.0492g/ml) × 30ml

= 31.476g

Number of moles of acetic acid = m/M

= 31.476g/ 60.05gmol-

= 0.524mol

In this experiment we want to know limiting reagent for determine theoretical yield of ethyl
acetate.

Density of ethanol = 0.7893g/ml

Volume of ethanol = 30ml

Mass of ethanol use in experiment = dv

= (0.7893g/ml) × 30ml

= 23.679g

Number of moles of ethanol = m/M

= 23.679g/ 46.07gmol-

Number of moles of ethanol = 0.514mol

From reaction

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CH3COOH (aq) + CH3CH2OH (aq) CH3COOCH2CH3 (aq) + H2O (liquid)

0.524mol 0.514mol

Ethanol is a limiting reagent. Hence it can control the reaction because amount of limiting
reagent directly affected to the final yield. According to reaction stoichiometric ratio,

Number of moles of ethyl acetate = 0.0514mol

Theoretical mass of ethyl acetate produce from reaction = Mn

= 88.11gmol- × 0.514mol

= 45.29g

Density of ethyl acetate = 0.9003g/ml

Theoretical volume that can produce from ethyl acetate = m/d

= 45.29g/ (0.9003g/ml)

= 50.3ml

Percentage yield of ethyl acetate = (practical yield /theoretical yield) × 100

= (24.57ml/ 50.3ml) × 100

= 48.8%

When we think about success of any synthesis, we can say if practical yield is equal to
theoretical yield it is 100% successful synthesis. However it is impossible due to experimental
errors and experimental condition not suitable to get 100% yield. Sometime some reactant
become a limiting reagent to cause reduce yield. However if our percentage yield is very high we
can consider our synthesis is successful. In this ethyl acetate synthesis we able to get 48.8%

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percentage yield. This yield is lower than the 50%. Hence we cannot say this is very successful
synthesis.

Conclusion

The ethyl acetate synthesis is not very successful synthesis. We unable to produces more yield of
product. It is less than the 50%. However we follow all necessary safety guidelines and wear
personnel protective equipment when we doing the synthesis. But we unable to performed very
successful synthesis.

Achieved P3, M2, D2

Synthesis of paracetamol
Introduction

Paracetamol also called as Acetaminophen is a drug use as mild to moderate pain killer. This is
prepared from reaction between p-aminophenol and acetic anhydride Presence of few drop of
concentrated H2SO4 acid as catalyst. This is nucleophillic acyl substitution in which the nitrogen
atom in p-aminophenol act as nucleophile by attacking a carbonyl group present in acetic
anhydride forms an intermediate which undergo the further elimination reaction of the acetate
anion. After produce acetaminophen, recrystallization method used to purifying the product
followed by hot gravity and vacuum filtration. The acetic acid form as side product from reaction
use to produce paracetamol. Actually acetaminophen is amide derivative.

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Procedure use to prepare paracetamol and purify the paracetamol

 As I previously mention paracetamol production can consider as preparation of amide

derivative. It can produce according to below procedure. Mainly 4-aminophenol react
with acetic anhydride under 120 Celsius degree temperatures to form acetaminophen. The
acetic acid formed as by-product. Then we isolate resultant precipitate of acetaminophen
using vacuum filtration for purification. The recrystallization method is applying for
purification.

As first step 4-aminophenol sample was weighted into watch glass (10.75g). Then it was added
to conical flask. Then 30ml of distilled water was measured using 50ml measuring cylinder and
it was add to conical flask. Actually we must take suitable amount of distilled water according to
amount of 4-aminophenol we take to produce paracetamol. Then 4-aminophenol was dissolved
in distilled water by stirred mixture using magnetic follower. Then the portion of 3ml acetic
anhydride was measured and it was added to conical flask. After that reactant mixture was heated
up to 120 Celsius degrees with continuous stirring of solution using stirrer bar. The solution was

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kept heating near one hour. The water bath was used to heat solution. After that one hour time
period stirrer bar was removed and wash with hot water. Then flask was kept in ice bath to form
solid particles. Then vacuum filtration was applied to isolate paracetamol particles from solution.
In this filtration process we use few drop of cold water to wash paracetamol solid particles. Then
recrystallization method was applied for purification. The little amount (50ml) of 50:50 MeOH
and distilled water solution was added to solid paracetamol in beaker. Then beaker was heated
until all the precipitate dissolved in solvent. The resultant mixture was filtered using hot gravity
filtration method with what-man filter paper. Then filtrate was cold in ice bath. Again vacuum
filtration was applied to filter paracetamol particle. The precipitate was washed with cold water
several times. Finally resultant paracetamol was dried under vacuum with P2O5 (Denney, 2012).

The reasons for carrying out the steps in the syntheses

As a first step we weigh the 4-aminophenol sample. It is necessary to calculate theoretical yield
of the paracetamol. Then 30ml of distilled water was added to conical flask to completely
dissolve 4-aminophenol because then all the molecules of 4-aminophenol in our sample can react
with acetic anhydride very easily. Every chemical reaction in this universe take place when
reactant overcome activation energy barrier. We can give needed energy to reactant molecules
for overcome activation energy barrier by heating the solution. Hence we heat reactant mixture
up to 120 Celsius degrees. Also reaction rate of the reaction increase with increasing temperature
help to produce more yield of paracetamol. The kinetic energy of reactant is increase by
absorbing energy giving by heating the solution. Due to this reason number of collision between
reactant molecules increase and then reaction rate goes up. It helps to produce more paracetamol.
Another reason for increasing reaction rate is due to heat absorbance number of reactant
molecules contains energy than activation energy goes up. We use water bath to heat solution
because water bath helps to heat entire solution equally. This will reduce risk of break down
(blast) the conical flask due to ununiformed thermal expansion of the flask. The solution is
stirring to get

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homogeneous mixture while heating the solution. It will cause to produce homogeneous
precipitate. Then to increase cooling rate of heated solution we use ice bath for cooling the
solution. To remove by-product, acetic acid, impurities and unreacted reactant molecules from
paracetamol precipitate we use vacuum filtration technique. This help to rapidly filter solution
compare to gravity filtration. Also vacuum filtration helps to remove considerable amount of
liquid particle from paracetamol. The recrystallization method applies to purify the paracetamol.
In this method first we dissolve paracetamol in little amount of 50:50 MeOH and water mixture
by heating the mixture. It helps to remove impurities trap inside the precipitate because
impurities dissolve in solution. Then hot gravity filtration method applies to remove insoluble
impurities. Then filtrate allows cooling down to get paracetamol as precipitate and applies
vacuum filtration to remove solution contact with precipitate. The soluble impurities remove
with filtrate. In vacuum filtration we wash precipitate with cold water to remove solution trap
with surface of precipitate. Also it is important to use cold water because solubility of
paracetamol in cold water is very small value. That allows obtaining maximum yield of
paracetamol. Then moisture trap inside the precipitate remove from it dried under vacuum with
P2O5. The P2O5 absorb moisture contain inside the precipitate. When remove stirrer bar from
reaction mixture it is wash with distilled water and that water added to the flask for avoiding
loose product.

Evaluation of success of the syntheses

In experiment we able to obtain 13.1g of paracetamol using 10.75g of 4-aminophenol.

Number of moles of 4-aminophenol = m/M

= 10.75g/109gmol-

= 0.0986mol

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From reaction

C6H4OHNH2(aq) + CH3CO2COCH3(aq) C6H4OHNHOCH3(aq) + CH3COOH(aq)

(4-aminophenol) (Acetic anhydride) (Paracetamol) (Acetic acid)

4-aminophenol: Paracetamol = 1:1 hence,

Number of moles of paracetamol = 0.0986mol

Theoretical mass of paracetamol = nM

= 0.0986mol × 151gmol-

= 14.9g

Percentage yield = (practical yield / theoretical yield) × 100

= (13.1g/14.9g) × 100

= 87.9%

When we think about success of any synthesis, we can say if practical yield is equal to
theoretical yield it is 100% successful synthesis. However it is impossible due to experimental
errors and experimental condition not suitable to get 100% yield. Sometime some reactant
become a limiting reagent to cause reduce yield. However if our percentage yield is very high we
can consider our synthesis is successful. In this paracetamol synthesis we produce paracetamol in
87.9% percentage yield. This value is very close to 100%. Hence we can say our paracetamol
synthesis is very success.

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Conclusion

Paracetamol is a drug that use as pain killer. This also name as N-acetyle-para-aminophenol or
acetaminophen. This is belonging to the analgesics and antipyretics drug classes. Metabolism of
the drug happens predominantly in the liver. In this synthesis we can conclude it is very
successful synthesis because we obtain 87.9% yield.

Achieved P4, M2, D2

References

Denney R.C., Mendham J., Barnes J.D., Thomas M.,(2012). Vogel’s textbook of quantitative
chemical analysis. pearson.

Hobby chemistry. (2014). Synthesis of ethyl acetate. Hobby chemistry.[online]. Available at

https://www.google.com/amp/s/hobbychemistry.wordpress.com/2015/04/17/synthesis-of-
ethyl-acetate/amp/. Accessed on 27th of October 2020, 2:00am.

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