OBJECTIVE

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

SUMMARY
A Liquid-Liquid Extraction (LLE) method of separation usually done when separation of
components of a liquid mixture cannot be done by using distillation process. Therefore this LLE
method will be use to separate the liquid mixture. In this experiment, the study will involves with
the operations of LLE by using a pulsed column LLE unit in order to determine the height
equivalent theoretical plates (HETP) for column by using the equilateral triangular diagram and
at the same time to investigate the effect pulsation stroke on the HETP. The experiment was done
by having a feed flows containing of solvent (Toluene in light phase) and Feed (Acetone-Water
mixture in heavy phase). The outlet flows will contain two different outlet which will be an
extract containing the toluene in rich phase and the raffinate containing with water also in rich
phase. The product obtained which the extract is as for in this experiment, the toluene will be
analyzed by reading its RI in order to confirm if it has the correct RI for toluene. The separation
of the liquid generally was based on their selectivity (separation factor), distribution coefficient,
solvent insolubility, density and more. The experiment can be concluded as a success if the
theoretical stages calculated in the triangular plot is between 4 to 5 stages. In this experiment, the
plotted triangular shows a theoretical stages to achieve the final raffinate and extract
compositions has 4 stages, therefore the experiment was a success.As the pulsation stroke kept
constant the LLE experiment performance were at its optimum performance. Theoretically it was
said that when the pulsation intensity or stroke increase the performance of column will also
increase.
INTRODUCTION & THEORY

Firstly, must prepare 20 litres of 50wt % mixture of Acetone in Water by mixing

appropriate quantities of the Acetone in distilled water. Then, Prepare 20 litres of Solvent that
Pure Toluene. Next, The bottom product contains the Water Rich Phase (Raffinate ) while the top
product contains the Toluene Rich Phase ( Extract ) were collected to make samples in 10 ml of
Raffinate and 10 ml sample of Extract .After, Record the Refractive Index of both samples by
using refractive index measurement.

Extraction is the pulling out of something from something else and separation by liquid-
liquid extraction can be defined as the selective removal of one or more components either from
a homogeneous liquid mixture or from a solution, using a second liquid or solvent, which is
partially or wholly immiscible with the first (Thornton). In liquid-liquid extraction, two phases
must be brought into contact to permit transfer of material and then be separated. Extraction
equipment may be operated continuous and the extract is the layer of solvent plus extracted
solute also the raffinate is the layer from which solute has been removed. The extract may be
lighter or heavier than the raffinate, and so the extract may be shown coming from top of the
equipment in some cases and from the bottom in others (Gavin,2007).

Whereas distillation affects a separation by utilizing the differing volatilities of the

components of a mixture, liquid-liquid extraction makes use of the different extent to which the
components can partition into a second immiscible solvent. This property is frequently
characteristic of the chemical type so that entire classes of compounds may be extracted if
desired. In general, extraction is applied when the materials to be extracted are heat-sensitive or
nonvolatile and when distillation would be inappropriate because components are close-boiling,
have poor relative volatilities or form azeotropes (Heity,2013).
The simplest extraction operation is single-contact batch extraction in which the initial
feed solution is agitated with a suitable solvent, allowed to separate into two phases after which
the solvent containing the extracted solute is decanted. Final settling or phase separation is
achieved under gravity at one end of the column by allowing an adequate settling volume for
complete phase disengagement. Any one extraction operation gives rise to two product streams:
the extracted feed solution, more usually termed the raffinate phase, and the solvent containing
extracted solute termed the extract phase (Perry,1984).

Figure 1.1 Pulsed column liquid-liquid

extraction.
For this experiment, the extraction process using

tertiary system (acetone-water-toluene). For Feed Vessel B1, filled with AcetoneWater solution
while in the Feed Vessel B2 with Pure Toluene Solvent. Then Acetone-Water solution which is
Heavy Phase will combine with solvent (Light Phase). The form of layer between the light and
the heavy phases is the Interface Layer. The bottom product will contain the Water Rich Phase
(Raffinate) while the top product contain the Toluene Rich Phase (Extract).
 Figure 1.2 equilateral triangular diagram.
Equilateral triangular coordinates are often used to present the equilibrium data for a
three-component system, since there are three axes. Each of the three corners represents a pure
component A, B, C. The point 1 represent a mixture of A, B, C. the perpendicular distance from
the point 1 to the base AB represent the mass fraction of XC of C mixture at point 1, the distance
to the base CB the mass fraction of XA of A, and the distance to base AC the mass fraction XB of
B.
A theoretical plate in many separation processes is a hypothetical zone or stage in which two phases,
such as the liquid and vapor phases of a substance, establish an equilibrium with each other. The
performance of many separation processes depends on having a series of equilibrium stages and is
enhanced by providing more such stages. Any physical device that provides good contact between
the vapor and liquid phases. Physical plate is rarely a 100% efficient equilibrium stage, the number of
actual plates is more than the required theoretical plates (Kister,1992).
RESULTS

Feed RI 1.0
Feed Composition 0.5
TABLE 1: Data Tabulation

Raffinate Extract
Feed Solvent Solvent Pulsation (water rich phase ) (Toluene rich phase)

flowrate flowrate to Feed stroke Time Refractive Solute Refractive Solute

(min) Index (Acetone) Index (Acetone)
(L/hr ) (L/hr ratio (mm)
Composition Composition
(wt %) (wt %)

7.77 7.77 1 5 5 1.453 0.29 1.342 0.64

7.77 7.77 1 5 10 1.345 0.64 1.463 0.23
7.77 7.77 1 5 15 1.346 0.64 1.443 0.35
7.77 7.77 1 5 20 1.345 0.64 1.346 0.64
APPENDIX

Appendix B

TABLE 2: Calibration Curve Data for Toluene Rich Phase

Average % Weight (Acetone) Refractive Index (Average)
0.10 1.4753
0.198 1.4649
0.424 1.4304
0.529 1.4147
0.607 1.4006
0.640 1.3687

FIGURE 1: Toluene Rich Phase Calibration Curve

 Appendix C

TABLE 3: Equilibrium data Binodial/ Solubility Data for Acetone-Toluene-Water System

Toluene Rich Phase Water Rich Phase
Acetone Toluene Acetone Toluene
0.0979 0.8778 0.6393 0.1439
0.1948 0.7760 0.6314 0.1198
0.4161 0.5442 0.5884 0.0659
0.5230 0.4243 0.5112 0.0310
0.6067 0.3214 0.3965 0.0138
0.6358 0.1389 0.1994 0.0120

TABLE 4: Data for Solute Distribution (Tie lines)

Heavy Phase (Water Rich) Light Phase (Toluene Rich)
Acetone Weight Composition
0.517 0.698
0.408 0.555
0.327 0.504
0.301 0.422
0.214 0.394
0.096 0.325
ANALYSIS AND DISCUSSION

As mention in the objective of the experiment, the main purpose of running this experiment
was to operate a Liquid-Liquid Extraction (LLE) by using Pulsed Column LLE unit. The
experiment was done also to determine the height equivalent theoretical pates (HETP) for the
column by using equilateral triangular diagram. Furthermore, the experiment also run to
investigate the effect of the pulsation stroke on the HETP. This separation method of solvent
extraction or usually known as the LLE involves with the separation of compounds based on
their relative solubility between two distinct immiscible liquids or almost immiscible.

In this experiment where it involves with the operation of LLE by using the pulsed column,
the separation involves with feed flows divided into two which was solvent and feed. The solvent
will be the toluene (Light Phase) and the feed will be a mixture of water and acetone (Heavy
Phase). The outlet flows also divide into two which contain of extract and raffinate where the
extract will the toluene in rich phase and the raffinate will be the water in rich phase.

The refractive index (RI) of the outlet flows was determined by using a digital refract meter
and tabulated in table 1 by taking sample every 5 minutes until it reach 20 minutes. In order to
determine the solute acetone composition (SAC) in both outlet flows, a calibration curve need to
be plotted as shown in figure 1 by using the information in table 2 with RI verses Average weight
5 of acetone. Using the RI of outlet flows, refer the RI in the calibration curve to determine the
SAC. In table 1, the SAC for raffinate shows that as the refractive index decrease the SAC will
increase and at some time it will reach a constant value while for the extract, the RI should be
increasing and the SAC will decrease.

The two outlet flows RI reading where in raffinate which was a water rich phase it should have a
RI reading of water of 1.34, the first sample at 5 min, the samples rather shows a higher RI
reading of 1.453 which was nearer to toluene RI of 1.49 but starting from sample two at 10 min
to 20 min the RI reading shows a correct reading that shows it was a water rich phase. The
Extract which will be a toluene rich phase shows a reading RI reading of water in the first 5
minutes and it recorded a toluene RI for samples 10 min and 15 min but the RI reading turn back
into water RI. The RI reading of toluene rich phase should be showing more of toluene RI
reading as the times increase.

In toluene rich phase, the error pointed which was the last RI reading, instead of giving a
toluene RI reading, the digital refract meter read a water RI which cannot be happening since it
supposed to be in toluene extract. The error maybe due to the mixture of water and toluene
overflowing at the same place. Where the overflows for toluene contain some water or it can be a
leaked. Other reason for this error maybe affected while taking the RI reading of samples where
the experimenter did not rinsed off the refract meter before taking other samples RI. Furthermore,
the error might also contributed by confusion where the experimenter take the same samples to
examined the RI reading where instead of reading the toluene RI, the experimenter takes the
water RI, this confusion maybe contributed by the transparency of the samples as water and
toluene has the same transparency.

The theoretical stages to achieve final raffinate and extract compositions was determined by
plotting the Feed (F), Solvent (S), Raffinate (R), Extract (E) and Feed and solvent mixture (M) as
shown in figure 2 the triangular plot. The plotting was done by referring to the appendix given.
After the plotting has been done, the R located where all the operating lines meet. According to
figure 2, the theoretical stages was calculated by counting the lines insides the E-F-R-S
quadrilateral where only the lines that has the two dotted lines inside of the quadrilateral are
counted as the theoretical stages. As shown in figure 2, the theoretical stages to achieve the final
raffinate and extract compositions shows that it needs 4 stages only.

The transfer rate of solute to solvent phase can be affected by a high distribution ratio of the
solute of interest between the two liquid phases. The attainment of selectivity in an extraction
also important, where other factors that contribute to the transfer rate of solute depends on the
solvent choice, selectivity (separation factor), distribution coefficient, solvent insolubility,
density and more.
 Theoretically, the effect of pulsation intensity on the overall transfer rate for toluene-water-
acetone decreases as the pulsation intensity increase, but in this experiment, the pulsation
frequency or stroke was set to be constant at 5 mm, and it shows that the column performance
increased or it was at its optimum performance.[M. Torab, J. Safdari and A.
Ghaemi, 2010].
CONCLUSION

As a conclusion, this experiment was a success, where it meet the requirements of the
experiment which was the objectives of the experiment. The operation of the Liquid-Liquid
Extraction (LLE) experiment was a success where the HETP and also the effect of pulsation
stroke on the HETP can be determined. While running the experiment, the RI reading for the
outlet flows for raffinate was a success where it is in a water rich phase but for the outlet flows
for extract that supposed to reach toluene rich phase shows an error RI reading for the last
samples as it shows a water RI reading. This error maybe due to the instrument failure which
there may be some leaked or the water follows the toluene overflows. Other reason may be due
to the experimenter confusion by taking the water RI reading for toluene in confusion of the
outlet flows color transparency. Theoretically it is mention that the theoretical stages to achieve
final raffinate and extract compositions are in between 4 to 5 stages. In this experiment, the
theoretical stages obtain was 4 so it can be concluded that this experiment was a success.

RECOMMENDATIONS

In this experiment, some error was obtain while running the experiment. In order to avoid
this error to be happening in the future, the reading of samples refractive index (RI) should be
done by two person to be more accurate. Where one person will take the raffinate RI and the
other person take the extract RI. In the future, the LLE experiment should be using a various
kind of solvent and solute in other to compare which solvent and solute are more efficient. The
RI reading instrument also can be varies and differentiate, where other RI instrument can be used
to determine the RI which is the refractometer.
REFERENCE

M. Torab-Mostaedi, J. Safdari and A. Ghaemi, (June 2010). Mass Transfer Coefficients in Pulsed
perforated-plate extraction columns. [Online]. [Accessed 3-04-2016]. Available from World
Wide Web:
http://www.scielo.br/scielo.php?script=sci_arttext&pid=S0104-66322010000200003

Gavin Towler and R K Sinnott (2007). Chemical Engineering Design: Principles, Practice
and Economics of Plant and Process Design. Butterworth-Heinemann.

Heity. (2013.Design Principles for Liquid-Liquid Extraction. [Online]. [Accesses 3/4/2016].

Available from worldwide web:
http://www.aiche.org/resources/publications/cep/2015/november/design-principles-liquid-
liquid-extraction
Kister, H.Z. (1992). Distillation Design (1st ed.). McGraw-Hill.
Perry, Robert H. and Green, Don W. (1984). Perry's Chemical Engineers' Handbook (6th ed.).
McGraw-Hill.
Thornton, J.D. (2016). Extraction liquid-liquid. [Online]. [Accesses 3/4/2016]. Available from
worldwide web: http://www.thermopedia.com/content/752/