UNIVERSITI KUALA LUMPUR

MALAYSIAN INSTITUTE OF CHEMICAL

& BIOENGINEERING TECHNOLOGY

LABORATORY REPORT COVER PAGE

Title of experiment: Pulsed Column Liquid-Liquid Extraction Unit

Group number: 1 Section: LO1-P3

Date of experiment: Date of submission:

Name & ID No.: 1. Muhammad Adib Haziq bin Amran 55218119173

2. Noor Hasniza binti Abd Hasani 55218119188
3. Izzira Azreen binti Ismail 55218119164
4. Wan Ahmad Thaqif bin Ahmad Kamal 55218119177
5. Nur Aisyahton Wan Sabri 55218119163
*Penalty:
 For any late of submission, the mark will be reduced by 5% per day to a maximum of 3 days, after which it will NOT BE
ACCEPTED.
 Plagiarism will not be tolerated and will be given ZERO.
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Criteria
(1) (2) (3) (4) (5)
Report format (5%)
1.Organization of the report.
Summary (10%)
1.Brief review on the objectives of the experiment, major
findings and significant conclusions
Objectives (5%)
1.State the objectives of the experiment in point form
Introduction & Theory (10%)
1. State the background to the experiment conducted.
2. Summary of theories including formulations related to
the experimental work.
Data & Results (10%)
1. Data are presented as deemed suitable with
complete labels and units.
Analysis & Discussion (40%)
1. Explanations of the referred table and figure are
presented after the table and figure
2. Discuss on the findings and relations to the theory
and objective of experiment
Conclusion & Recommendation (10%)
1.Summary of the results to relate the findings or results
with the theory applicable to the experimental
2.Suggest improvements in apparatus or measurement
procedure, or experimental procedures for future
References (5%)
1. Cite references in the text.
2. References taken from books, journals and articles.
References from website are not recommended.
Appendices (5%)
1. Put raw data and sample calculation.

TOTAL (100%)

Date of Submitted:
Student Name & ID:
Subject & Code:
Experiment title:
Lecture Name: Stamp
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Summary

The purpose of this experiment are to operate a Liquid-Liquid Extraction Experiment using
a Pulsed Column Liquid-Liquid Extraction Unit, to determine the height equivalent theoretical
plates (HETP) for column by using equilateral triangular diagram and to investigate the effect
of the pulsation stroke on the HETP. This experiment was carried out by using extraction
process. Extraction is a unit operation used to separate the components based on their Chemical
Differences instead of differences in Physical Properties. Liquid-liquid extraction is used to
separate the components of a mixture of liquids by means of a solvent in which the component
of the components that are to be extracted have marked solubility in respects to the others. The
chemicals that are required in this experiment are acetone (solute), deionized water (diluent)
and toluene (solvent). The sample was taken every 5 minutes in V10 and V12 to check the
refractive index (RI). The number of stage value is only valid if there is tie line located in the
operating area. The more the number of theoretical stages, the more the composition extraction
achieve in the process. To achieve highest number of extractions, it needs a lot of time in doing
the liquid-liquid extraction process. Theoretically, when the pulsation applied to the extractor
increase, it will produce a better dispersion of the phases and creates more interfacial area of for
mass transfer. The rate of extraction will improve as turbulence within the column is increased.

Objectives

1. To operate a Liquid-Liquid Extraction Experiment using a Pulsed Column Liquid-Liquid

Extraction Unit.

2. To determine the height equivalent theoretical plates (HETP) for column by using triangular
diagram.

3. To investigate the effect of the pulsation stroke on the HETP.

Introduction
Extraction is a process where a liquid immiscible solvent, one or more components are isolated
selectively from a liquid or solid mixture by the feed. Liquid liquid extraction separation can be
described as the selective removal of one or more of the components, either from a homogeneous
liquid mixture or from a solution, by means of a second liquid or a solvent, partly or entirely
immiscible from the first. The component transfer from the feed to the solvent is regulated in the
corresponding step by the solubility behaviour of each component. Two phases from the extraction
step one is enriched (EXTRACT Phase) and the other depleted (RAFFINATE Phase) in the
components to be separated, respectively. Liquid liquid extraction are most commonly used and
will be taken in this laboratory. In fact, toluene is used to remove solute, acetone, from water as a
solvent. The toluene rich form is called extract and the raffinate is called the water rich form. Gas
liquid extraction which is also called absorption is another application.

A widely used terminology describes the system in terms of :

 F : feed
 S : solvent
 R : raffinate
 E : extract

The equilateral-triangle diagram developed by Hunter and Nash is commonly used for
multistage extraction calculations involving ternary systems. In practice, toluene is used as solvent
to remove the solute, acetone, from water; the toluene-rich phase is called the extract, and the
water-rich phase the raffinate.
The following diagram indicates the Flow of Streams and Components in a Liquid-Liquid
Extraction System.

Components of Pulsed Column Liquid-Liquid Extraction Unit are as follows:

 Feed Vessels (B1/B2) – Graduated Cylindrical Vessels with 25 L capacity.
 Column (K1) – a DN 80 Packed Column with 10 mm Ceramic Saddles. Effective Height of
column is 2.5m.
 Dosing Pumps (P1/P2) – 0.25 kW Piston Pumps with up to 42 L/h capacity.
 Pulsator (P3) – 0.25 kW Pulsator Pump with a 20 mm stroke and 50 Hz frequency.
 Receiving Vessels (B3/B4) = Graduated Cylindrical Vessels with 25 L capacity
 Pulsation Dampers (B5/B6)
Theory
Liquid-liquid extraction is the classical method used for herbicide isolation, especially from
water and biological fluid samples. Ethyl acetate and their mixtures are among the preferred
extraction solvents triazoles, amides, carbamates, benzimidazoles and chlorotriazines. The
extraction efficiency is modified by adjustment of pH and ionic strength in the aqueous phase. In
derivatization of the target analytes is also used as an effective for example chlorophenoxy
acidic herbicides are derivatized with dimethyl sulfate prior to their extraction by n-hexane. The
classical way of performing liquid-liquid extraction is the separation funnel extraction.
Liquid-liquid extraction, also known as solvent extraction and partitioning is derived from
the Luke method but not used in multiresidue methods. Traditionally this method is used for clean-
up of the sample. This method is used to separate compounds based on their relative solubilities in
two different immiscible liquids, usually water and an organic solvent. In this method after
extraction of sample with acetone, solvent mixture containing dichloromethane alone or combined
with petroleum ether is used. Liquid-liquid extraction is applicable for grapes and by-products. The
main disadvantage of liquid-liquid extraction method is that this method is time consuming,
tedious, laborious and requires large amounts of toxic solvents that pose a potential threat to human
health, environment, problem of emulsion formation, and if there exist lots of target compounds
with significant difference in polarity in samples, it would be difficult to obtain good sample
separation using a single liquid-liquid extraction procedure.
 Data & Results

Raffinate Extract
(water rich phase) (Toluene rich phase)
Feed Solvent Solvent Pulsation T
flowrate flowrate to Feed stroke ime Refractive Solute Refractive Solute

(L/hr ) (L/hr ratio (mm) (min) Index (Acetone) Index (Acetone)

Composition Composition
(wt %) (wt %)
12 12 1 5 0 1.339 29.4 1.423 44.29

12 12 1 5 5 1.339 29.4 1.428 41.35

12 12 1 5 10 1.339 29.4 1.434 37.82

12 12 1 5 15 1.351 33.4 1.435 37.26

12 12 1 5 20 1.352 35.4 1.445 31.35

12 12 1 5 25 1.350 31.4 1.455 25.47

12 12 1 5 30 1.352 35.4 1.469 17.24

Table 1: Table of The Result of Raffinate and Extract

Figure 1: Calibration curve for Water Rich Phase

 Figure 2: Calibration curve for Toluene Rich Phase

9.0 APPENDICES
Calculations
1) Equation for calibration curve for toluene rich phase
y = -0.0017x +1.4983
Data 1
RI = 1.423
1.423 = -0.0017x + 1.4983
x = 44.29
Data 2
RI = 1. 434
1.434 = -0.0017x + 1.4983
x = 41.35
Data 3
RI = 1.435
1.435 = -0.0017x + 1.4983
x = 37.26
Data 4
RI = 1.445
1.445 = -0.0017x + 1.4983
x = 31.35
Data 5
RI = 1.455
1.436 = -0.0017x + 1.4983
x = 25.47
Data 6
RI = 1.469
1.469 = -0.0017x + 1.4983
X = 17.24

2) Equation for calibration curve for water rich phase

y = 0.0005x + 1.3343
Data 1
RI = 1.339
1.339 = 0.0005x + 1.3343
x = 29.4
Data 2
RI = 1.339
1.339 = 0.0005x + 1.3343
x = 29.4
Data 3
RI = 1.339
1.339 = 0.0005x + 1.3343
x = 29.4
Data 4
RI = 1.351
1.351 = 0.0005x + 1.3343
x = 33.4
Data 5
RI = 1.352
1.352 = 0.0005x + 1.3343
x = 35.4

Data 6
RI = 1.350
1.350 = 0.0005x + 1.3343
x = 35.4
Discussion

The purpose of this experiment is to operate a liquid-liquid extraction experiment using a

pulsed column liquid-liquid extraction unit and to determine the height equivalent theoretical plates
(HETP) for column by using equilateral triangular diagram. Besides, to investigate the effect of the
pulsation stroke on the HETP. Liquid-liquid extraction (LLE) is chemical process that used a
solvent to extract solute from a mixture. Extraction depends on Chemical differences compare with
physical differences to separate the component. The process is to produce an extract and raffinate
from the extraction of solute from the feed by using solvent. The process extraction also is to
remove the solute from the feed when the solvent rich liquid is leaving the extractor as the solvent
does the extraction. The feed rich that leaves the extractor known as raffinate (R). The separation of
liquid-liquid extraction can be called as a process of removal of certain component that can be
homogeneous liquid mixture, from the solution that used a second liquid and solvent that can
partially or wholly immiscible with the first.
The terms that usually used in this process and it is widely used to classify the system are feed
(F), solvent (S), extract (E) and raffinate (R). Feed is the substance that need to be extract than can
dissolved also known as an inlet stream while the substance needs to transfer from the feed can
called as solvent. The extract is solvent material which solute has been transferred and this process
occurred at the exit stream. Raffinate is the exit stream from the process being substantially feed
material from which the solute has been transferred. The unit of liquid-liquid extraction consists
packed and plate column contractors, mechanically agitated column, sundry devices, and mixer
settler.
For this experiment, the chemical used as solute is acetone while for diluent is deionized water
and for solvent is toluene. The experiment began with preparing 20 litres of 50 wt% mixture of
acetone in water and 20 litres of solvent which is pure toluene. Next, the feed vessel B1 filled with
acetone-water solution while feed vessel B2 filled with the pure toluene solvent. As the experiment
attained a steady state, both liquid flow into the collection vessel B3 and B4 respectively. The
bottom product is raffinate that contains water rich phase while the top product contains extract
which is toluene rich phase. The flowrate for feed and solvent while operating this experiment is set
to 12/L hr and 5mm the value of Pulsation stroke. Every 5 minutes the sample need to be collected,
there were two sample need to be collected which are sample of raffinate and sample of extract.
Sample of 10 ml raffinate was collected from valve 10- and 10-ml sample of extract is from valve
12. The sample need to collect start from 0 min to 30 min of experiment and the value of the
refractive index was taken for all samples.
Based on data tabulated in table 1, two calibration curved graph were plotted which are water
rich phase and toluene rich phase. Figure 2 is the graph toluene rich was plotted based on refractive
index against acetone weight percent (wt%). The linear equation obtains after the graph plotted was
the value of y= -0.0017x + 1.4983 where the slope of the curve is -0.0017 while y-intercept is
1.4983. After obtained value of sloped from the calibration curve, the percentage of acetone weight
can be calculated when the value of refractive index is substitute into X. From the graph plotted, it
can be determining that the value weight percent is increase, the value of refractive index will
decrease. For water rich phase, a calibration curve graph where refractive index against acetone
weight percent also has plotted as shown in figure 1. The linear equation obtained was y = 0.003x +
1.2508 where slope of the curve is 0.003 while y- intercept is 1.2508. The percentage of acetone
weight can obtain by using the same method to find value for toluene rich phase. From the graph,
the value of refractive index increases as acetone weight percentage increase.
The work process of liquid-liquid extraction can be increase to make it more efficient is by
making the rate of transfer of solute to solvent phase is high, and to increase the successful of
separation is by choosing the right type of solvent. The characteristic of choosing the right solvent
is the solvent must have high selectivity. This will help to increase the ability of the solvent to
extract and will determine the number of extraction stages required. Next, the distribution or
partition coefficient where the ratio of the solubility of the solute in solvent compared to feed. This
will increase the selectivity and the specific amount of solvent phase required. Interfacial tension
also need to be considered to increase the efficiency of the process. The interfacial facial need to be
large in order to make coalesces of emulsion is more ready. When, coalesces of emulsion is more
ready the separation process can become much easier. Furthermore, the difference density of the
solvent and feed need to be greater to make phase separation process become easier. The next
factor is the viscosity, vapour pressure and the freezing point. It should be low for ease in handling
and storage. To inhibit the mass transfer and separation process a high viscosity is required for the
process. Volatility factors need to list to make sure the solvent can be separated from solute and
feed.
To produce a better dispersion of the phases a pulsation need to be apply; this also help to create
more interfacial area for mass transfer. Then it will improve the rate of extraction when the
turbulence within the column is increased. This shows that the increasing of pulsation frequency it
help to increase the transfer rate in pulsed column.
Conclusion & Recommendation

The objectives of this experiment are to operate a liquid-liquid extraction using a pulsed
column liquid-liquid extraction unit, to determine the height equivalent theoretical plates (HETP)
for column by using equilateral triangular diagram and to investigate the effect of the pulsation
stroke on HETP. All the objectives were successfully achieved as the students already performed
the experiment and the students managed to identify the theoretical plate by using the equilateral
diagram. There are some recommendations that can be done to improve the results of the
experiment. Firstly, the period to operate the apparatus should be longer so that the extraction
process is more efficient. Make sure that all the apparatus such as the flowrate meter can be used.
This helps the students to learn on how to use the apparatus by themselves. Next, students need to
prepare themselves well by understanding the operation of the experiment. This can be done by
studying the lab manual before starting the experiment. By doing these steps, any accidents also
can be avoided. Besides, the refractometer should be improved by changing the colour to
differentiate the two area. Previous refractometer used about the same orange colour and make the
students having hard time to use it. Hence, some of the collected data may not be accurate. Lastly,
make sure that students wear the gloves and masks throughout the experiment to avoid themselves
from contaminated.
References
1. Helmenstine, A. M. (2017). What Is Distillation (Vol. 23). 2017-02.
2. Robinson, E. R. (1969). The optimisation of batch distillation operations. Chemical
Engineering Science, 24(11), 1661-1668.
3. Bai, P., Hua, C., Li, X., & Yu, K. T. (2005). Cyclic total reflux batch distillation with two
reflux drums. Chemical engineering science, 60(21), 5845-5851.