Feed RI 1.

0
Feed 0.5Solvent
Feed Composition Raffinate Extract
flowrate flowrate (water rich phase) (Toluene Rich Phase)
(L/hr) (L/hr) Solvent Pulsation
Time Solute Solute
to Feed stroke
Table 1: (min) Refractive (Acetone) Refractive (Acetone)
ratio (mm)
Index Composition Index Composition
(wt%) (wt%)
7.7 7.7 1 5 5 1.3560 43.4 1.3789 63.5
7.7 7.7 1 5 10 1.3571 45.6 1.3850 62.5
7.7 7.7 1 5 15 1.3472 25.8 1.3998 60.5
7.7 7.7 1 5 20 1.3410 13.4 1.4154 53.0
Refractive Index and Solute Composition
Raffinate : 0.3205
Extract : 0.598

Avg % Weight Refractive Index

10.0 1.4753

19.8 1.4649

42.4 1.4304

52.9 1.4147

60.7 1.4006

64.0 1.3687
 Figure 1: Refractive Index vs Acetone Weight % (Toluene Rich Phase)

Avg % Weight Refractive Index

10.0 1.3681

19.8 1.3682

42.4 1.3661

52.9 1.3618

60.7 1.3556
 20.0 1.3449

Figure 2: Refractive Index vs Acetone Weight %

(Water Rich Phase)

For Mass Balance:

Extraction
Solvent (Toluene)
(Toluene Rich-Phase)

Feed (Acetone + Water) Raffinate (Water + Toluene)

From the Calculation, Rn = 0.3205
 E1 = 0.598
Overall Mass Balance:
S + F = E + R
20kg + 20kg = E + R Acetone Mass Balance:
40kg = E + R
S(Xs) + F(Xf) = E(Xe) + R(Xr)
20(0) + 20(0.5) = E(0.598) + R(0.3205)
10 = 0.5985E + 0.3205R

Acetone Mass Balance for Raffinate:

S(Xs) + F(Xf) = E(Xe) + R(Xr)

20(0) + 20(0.5) = E(0.598) + R(0.3205)
10 = (40 - R)(0.598) + 0.3205R
-13.92 = -0.598R
R = 23.28 kg

Acetone Mass Balance for Extract:

S + F = E + R
20 + 40 = E + 23.28
60 = E + 23.28
60 (23.28) = E
E = 36.72 kg
ANALYSIS & DISCUSSION

In this part, the main purpose of this experiment was to operate a Liquid-Liquid Extraction (LLE) by using Pulsed Column LLE unit. The
experiment was done 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.
Liquid-liquid extraction (LLE) was known as solvent extraction is a method to separate compounds based on the relative solubility in two
different immiscible liquids, usually water and an organic solvent. This is an extraction of a substance from one liquid phase into another liquid
phase. LLE is a basic technique in chemical laboratories to perform. This type of process is commonly performed after a chemical reaction as
part of the workup.
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.
Based on the result obtained 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 which is Refractive Index vs Acetone Weight % (Toluene Rich Phase). 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 unstable the SAC also decrease while, for the extract, the RI should be also unstable and the SAC decrease respectively.
 However, the value for raffinate is 0.3205 and the value of extract is 0.598. The value of feed is 0.5 and the value of solvent is 1.0. The
feed and solvent mixture, M was plotted by the intersection of extract and raffinate with solvent and feed (E-R intersect with F-S). The feed and
solvent mixture, M was 38% of acetone, 38% of water and 24% of toluene). After getting the feed and solvent mixture point, the operating line
R was plotted by drawing a straight line between the point of feed and extract and another straight line between the point of toluene and water.
The operating line obtained was placed at the outside of the graph which is on the right side. Then, tie line was plotted (refer appendix C) from
point E to its equilibrium point on the bimodal plot. The operating line was connected from equilibrium end of the tie line to the R. The number
of tie lines contained inside the EFRS quadrilateral was the number of required theoretical stage to achieve final raffinate and extract
compositions and the number of theoretical stage obtained was 4 stages which is 3 theoretical plates. The pulsation stroke effect the result on the
height equivalent theoretical plates (HETP).
Based on the experiment, when the pulsation stroke increases, the flow rate of the liquid inside the column increases. The rate of transfer
of solute to solvent increases due to the increasing flow rate and the vapor and liquid reach equilibrium faster. Thus, the number of height
equivalent theoretical plates (HETP) decreases. There are various factors that can help to increase the rate of transfer of solute to solvent phase.
Firstly, increase in pulsation frequency resulted in decreasing of time to achieve steady state of solute in the extract phase. Secondly, when the
stroke length increases, the rate of transfer of solute to solvent phase increases. This is because the stroke length works as additional force that
increases the turbulence. Then, when the amplitude and frequency of the pulsation increases, the rate of transfer of solute to solvent also
increases. Pulsation frequency increases the rate of transfer in pulsed column. This is because the column was pulsed by blowing air at a certain
amplitude and frequency. When the pulsation frequency was increased, it creates a huge turbulence towards the solvent inside the column and
this increases the rate of transfer of solute to solvent.