ABSTRACT

This experiment was conducted to perform a single stage extraction to separate acetic acid from
its pollution and to determine the acid contents in the raffinate and extract phase. Liquid-liquid
extraction is a process in which a compound is extracted when solvents A and B are not soluble
or partially soluble.

In this experiment,firstly,we prepared the binary acetic acid-chloroform solution by adding the 4
mL acetic acid to 5 mL chloroform in separating funnel.After that,we will turn it into a
homogenous binary solution which act as the feed solution.To extract the acid from the binary
solution,we measured about 10 mL of distilled water and poured it into the tunnel which
generate a vapor.Then,we continually shaking and venting the funnel for about 5 minutes.After
this step,the funnel was put into the o-ring wait about 10 minutes to let the content settle into
each phases reach their equilibrium.The mass of two empty conical flask was weighed and
recorded and each phases from the funnel was transferred into each flask.Lastly,two drops of
phenolphthalein was put into each flask and was titrated using 2.0 M of NaOH.This is to
observed the end point of each phases which happened when it turns into color.

Based on this experiment,we observed and recorded the mass of raffinate and extract and the
volume of of NaOH used.The average mass of solution by both of the raffinate and extract are
5.19 g and 15.2 g.Meanwhile,the average volume of NaOH used for the raffinate and extract are
3.45 mL and 36.1 mL

As in this experiment,we used a corrosive chemical likes acetic acid and chloroform,we need to
be more careful to make sure that any unexpected incident will not happened.It is because
chloroform is believed to be one of the agent that caused cancer.So,we need to obey the rules
when do this experiment to ensure our safety.
INTRODUCTION

Extraction between two solvents that are either immiscible or only partially miscible is known as
liquid-liquid extraction. Liquid-liquid extraction is also frequently used to wash an organic phase,
such as to get rid of inorganic compounds or to protonate or deprotonate bases or acids so they
can dissolve in water. An extremely typical extraction flow diagram shows how a reaction
mixture is quenched with water, extracted (many times), washed with brine, dried, filtered, and
lastly evaporated to obtain a crude product or a pure product.

By taking use of a substance's varying solubilities in several solvents, the liquid-liquid extraction
process is used to remove impurities. The sample can be either solid or liquid, which
distinguishes it from crystallisation. First, the impure sample dissolves in solvent 1. After that, a
second solvent 2 is introduced such that the sample migrates from the first solvent to the
second without picking up any contaminants. This, of course, calls for the immiscibility of the two
solvents 1 and 2, as well as the ideality of the sample being more soluble in solvent 2 than in
solvent 1.

Liquid-liquid extraction is frequently carried out with one aqueous phase (either pure water, or
an aqueous solution), and one organic phase. From this point forward, we will simply refer to
this process as extraction. It's crucial to remember that the desired compound, which is typically
an organic molecule, might theoretically be in either phase. It depends on both the composition
of the substance and the composition of the aqueous phase. Before talking about technological
considerations, we will first look at some typical extraction cases.

One frequent issue with extractions is one that doesn't result from poor method but rather from
the unpleasant behaviour of some compounds, which is that they create emulsions. These
frequently occur between the two lays and are chemically made up of the two solvents and
other substances present in the initial solution. The emulsion can clear up on its own after a
short while or it can be very persistent. In the latter situation, draining the emulsion in the
product-free phase and repeating the extraction process numerous times can occasionally be a
wise move.

Any given extraction operation produces two product streams: the extracted feed solution, which
is more commonly referred to as the raffinate phase, and the solvent containing the extracted
solute, which is referred to as the extract phase. The terminology used from now on is exclusive
to liquid-liquid extraction procedures.

In addition to becoming familiar with the liquid-liquid extraction method and what can be
achieved with it, the experiment's objective is to recover the two components as nearly
quantitatively as feasible. The actual extraction can be done quantitatively with caution. Sample
loss occurs frequently during filtering, recrystallization, and other processes, however this can
be reduced with proper methodology. More frequently, samples are lost due to labelling errors or
throwing out the inappropriate phase. Make sure you identify the watery layer by testing to
determine which layer can dissolve a few extra drops of water or by comparing the relative
densities of the solvents.

OBJECTIVES
1. To perform a single stage extraction to separate acetic acid from its solution
2. To determine the acid contents in the raffinate and extract phase

APPARATUS AND CHEMICAL

● Conical flasks
● stopper
● retort stand
● dropper
● O-ring
● separating funnel
● distilled water
● chloroform
● acetic acid
● 2.0M NaOH solution
● beaker
● phenolphthalein
● hand glove
PROCEDURE

1. A binary acetic acid-chloroform was prepared by adding 4mL acetic acid solution to 5mL
chloroform in separating funnel.

2. With the funnel mouth still opened, the mixture was swirled to mix them well into a
homogenous binary solution.

3. Then, the acid from the binary solution was extracted using equal mass of an extraction
solvent which was water. 10mL of distilled water was measured and poured into a
funnel.

4. Hand glove was put on. The funnel was shaken with a stopper on and then the stopcock
was opened to release any pressure build up. It was then shaked and vented for about 5
minutes.

5. The funnel was put on the O- ring support to let them settle into phases. Then, wait for
about 5- 10 minutes to allow them to reach their equilibrium.

6. Two clean empty conical flasks were weighed and transferred each phase into each
flask. The beaker was reweighted.

7. Two drops of phenolphthalein were put into each flask and titrated them using 2.0 M
NaOH. The end point was reached when the solution turns colour.
RESULTS AND DATA

A. mass of raffinate and extract

SET 1

Phases Raffinate Extract

Mass of empty conical 106.55 110.12

flask (g)

Mass of empty conical 111.63 125.42

flask + solution (g)

Mass of solution (g) 5.08 15.30

SET 2

Phases Raffinate Extract

Mass of empty conical 106.55 110.12

flask (g)

Mass of empty conical 111.85 125.22

flask + solution (g)

Mass of solution (g) 5.30 15.10

Average = 5.19 raffinate

= 15.20 extract
 B. Titration of raffinate and extract

Set 1

Phases Raffinate Extract

Initial volume (mL) 0 0

Final volume(mL) 3.5 36.2

Volume of NaOH used 3.5 36.2

(mL)

SET 2

Phases Raffinate Extract

Initial volume (mL) 0 0

Final volume(mL) 3.4 36.0

Volume of NaOH used 3.4 36.0

(mL)

average = 3.45 - raffinate

=36.1 - extract
Calculation :

Feed solution Extracting solvent

Component A (Acetic acid) B (Chloroform) Distilled water

Volume used(mL) 4.00 5.00 10.00

Density(g/mL) 1.049 1.4832 1.00

Mass (g) 4.196 7.416 10.00

Total mass (g) 11.612 10.00

DISCUSSION

Liquid - liquid extraction is a chemical process of extraction of solute from a mixture by using a
solvent. In this experiment, we are extracting acetic acid from chloroform by using water as
solvent. After the experiment has been done, samples from feed, raffinate and extract were
taken to determine the concentration of acetic acid present. This experiment was carried out to
perform a single stage extraction to separate acetic acid from its solution.

This procedure results in the formation of two layers which are a heavy phase and a light phase.
The feed solution is the combined solid, the heavy phase, and the solvent, the light phase. The
light phase is visible at the top of the separatory funnel, and the heavy phase is visible at the
bottom. This is so because the heavy phase has a higher density than the light phase. Although
acetic acid, chloroform, and water are all used in this experiment, only the extract and raffinate
phases can be seen. This is so that acetic acid and water only interact with one another and not
with chloroform.

It is possible to see the flow of water through the chloroform by looking for bubbles in the
separatory funnel, which for a short period of time produces an intermediate phase. Between
the chloroform and the water solvent, there is a substantial surface area provided by the
resultant bubbles. After that, equilibrium is reached when the intermediate sinks to the raffinate's
liquid phase and extracts the liquid phase.

This experiment has been done by titrating sodium hydroxide into the samples collected from
liquid - liquid extraction equipment. The samples which are collected from feed, extract and
raffinate were titrated by using 2.0 M NaOH. Before the titration, two drops of phenolphthalein
were added into the sample in order to detect the alkaline ions from sodium hydroxide solution.
As a sodium hydroxide solution added into the conical flask containing the sample, it will change
the sample colour from colourless to pink colour. The volume of 2.0 M sodium hydroxide
solution needed to turn the solution from colourless to pink for feed, extract and raffinate for set
1 was 36.2 mL and 3.5 mL meanwhile for set 2 was 36.0 mL and 3.4 mL respectively. From the
data collected on the titration, the concentration of acetic acid is determined at each phase. The
resultant solution is heated after titrating each phase with sodium hydroxide solution (base).
This is because exothermic, or the release of energy, occurs. As a result, an acetic acid and
chloroform solution is formed by breaking the C-H and C-Cl bonds.

Although the experiment was proven a success, there are several recommendations that we
apply to increase the quality of experiment conducted. We ensure that our eyes are
perpendicular to the meniscus while using the measuring cylinder to avoid parallax error. We
also ensure that the titration is done carefully and slowly since the end point of the titration
process can cine abruptly. Besides that, we also wear proper PPE ( personal protective
equipment ) such as gloves while conducting this experiment to avoid the chemical used from
making contact with the skins. We also properly familiarize ourselves with the equipment and
the apparatus used for the experiment to ensure the experiment is done in a correct manner so
that accurate data is obtained. Last but not least, we conduct this experiment at least twice to
ensure accuracy of the data obtained.
QUESTIONS

Using the ternary phase equilibrium curve provided in Appendix 1, determine the theoretical
mass fractions of acid in the raffinate and extract phases and compare to those obtained by this
experiment.
Explain if have any problems encounter during experiment in your discussion. The following
questions can be used as your guideline in writing discussion.

1. Briefly explain what you do to your data in order to obtain your results?
To achieve the result, we, first of all, need to obtain the mass of the raffinate phase and extract
phase. The mass of the solution and the conical flask will be subtracted from the mass of the
empty conical flask. Then, we calculate the average volume of 2.0 M NaOH used to titrate the
raffinate and extract phase solution. The objective is to calculate the mass fraction of acetic acid
in extract and raffinate solution. For theory value, we use the total materials mass balance
equation and tertiary diagram to achieve the mass of the extract and raffinate phase with the
mass of acetic acid in both phases. Meanwhile, the experiment value was obtained using the
ratio of mols which is 1 mol of CH3COOH is equal to 1 mol of NaOH. The mass fraction is
calculated using the formula that is the mass of acetic acid divided by the total mass of each
phase.

2. Discuss your experimental result by comparing to your theoretical result. If they differ,
how much?
Mass fraction of acetic acid in raffinate phase solution from the experiment which is 0.07985 g is
higher than the theoretical value which is 0.06499 g. There is 0.01486 g difference from the
theoretical value. Meanwhile, mass fraction of acetic acid in extract phase solution from the
experiment which is 0.2853 g is higher than the theoretical value which is 0.265 g.

3. Why do you think they differ? Include all contributing errors and how these errors
effect your result.
There’s a small difference that occurred because of some errors that were made while
conducting the experiment such as the eyes not parallel with the meniscus of the burette when
doing the neutralization. Besides, in liquid-liquid separation, the gas pressure not be removed
properly when venting the mixtures and the valve is not closed before the solution is poured into
the separation funnel.

4. Explain when liquid-liquid extraction method is suitable to apply compare with

distillation method.
Extraction can cover a wide range of the mixtures phase like solid and liquid. It is a separation
based on their relative solubilities in two immiscible liquids. Meanwhile, distillation is based on
boiling point differences.
Thus, the liquid-liquid extraction method is suitable to apply compared with the distillation
method when removing a component present in small concentrations like hormones in animal
oil. Next, it is also suitable when recovering a high-boiling component present in small quantities
in a waste stream such as acetic acid from cellulose acetate. Lastly, when recovering
heat-sensitive materials, where low to moderate processing temperatures are needed.

CONCLUSION
In conclusion, we have performed a single stage extraction that is to separate acetic acid from
its solution in chloroform. In this experiment, we use water as the extraction solvent. Next, the
actual value of mass fraction of acid acetic in extract phase is 0.2853 g while the theory value is
0.265 g. Then, the actual value of mass fraction of acid acetic in raffinate phase is 0.07985 g
while the theory value is 0.06499 g.
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