FACULTY OF CHEMICAL ENGINEERING

UiTM Cawangan Terengganu,

Kampus Bukit Besi
23200 Bukit Besi, Terengganu

TECHNICAL/EXECUTIVE REPORT : CHEMICAL ENGINEERING

Lab No. : 3 Module :

Topic : LIQUID-LIQUID EXTRACTION Mark :

Date : 1 JULY 2021

Participant Course : 249 Semester : 4 Group: 6
No. Name Matrix No. Signature
1 MOHAMMAD HAFIZUDDIN BIN ALIAS 2019205858
2 MUHAMMAD NAZMI ZUHAILI BIN IBRAHIM 2019666564
3 WAN AHMAD IRFAN BIN WAN ISMAIL 2019421488
4 MUHAMMAD AFIQ AIMAN BIN JAMALUDDIN 2019402404
Instructor 1. MADAM ZARINA BINTI OMAR

Objective :
1. To operate a liquid-liquid extraction experiment using a rotating disc column.
2. To determine the height equivalent theoretical plates or HETP for the column.
3. To identify the effect of the solvent toward the feed flow ratios and rotating disc based on HETP.

Introduction :

The experiment is conducted by utilizing Toluene (light stage) as the solvent and acetone water
combination (heavy stage) as the feed in the feed streams, while in the outlet streams, the extract is Toluene
rich stage while the raffinate is the water rich stage all together for the height equivalent theoretical plates
(HETP) for the segment to be resolved. This test is additionally directed to investigate the effect of the
solvent to feed flow rate ratios and rotating disc speed on the HETP.

Liquid–liquid extraction (LLE), also known as solvent extraction and partitioning, is a method to
separate compounds or metal complexes, based on their relative solubilities in two different immiscible
liquids, usually water (polar) and an organic solvent (non-polar). There is a net transfer of one or more
species from one liquid into another liquid phase, generally from aqueous to organic. The transfer is driven
by chemical potential, which is, once the transfer is complete, the overall system of chemical components
 that make up the solutes and the solvents are in a more stable configuration (lower free energy). The solvent
that is enriched in solute(s) is called extract. The feed solution that is depleted in solute(s) is called the
raffinate. LLE is a basic technique in chemical laboratories, where it is performed using a variety of
apparatus, from separatory funnels to countercurrent distribution equipment called as mixer settlers. This
type of process is commonly performed after a chemical reaction as part of the work-up, often including an
acidic work-up.

Material and Procedure:

Material

1. 50 L graduated cylindrical feed vessels, B1 and B3.

2. 10mm stainless steel saddles pack column, K1.
3. 42 L/h piston pump, P1 and P2.
4. 50 L graduated cylindrical receiving vessels, B3 and B4.
5. Pulsation dampers, B5 and B6.
6. Rotating stirrer.
7. Acetone
8. Water
9. Toluene

General start-up procedure.

1. All valves are ensured to be initially closed.

2. The feed vessel B1 is ensured to be filled up with pure toluene which is the solvent and the feed vessel
B2 is filled up with the acetone water solution.
3. Main switch at the control panel is turned on.
4. The ventilation line valves which are HV18, HV19, HV20, HV21, HV11, HV13 and the outlet vessel
valve HV02, HV24, HV07 and HV22 are opened.
5. Pump P2 is switched on. The acetone water solution which is heavy phase is allowed to enter the column
and filled to the level of about 100cm above the solvent inlet. Then the pump P2 is stopped.
6. Pump P1 is switched on. The interface level which forms between the light and heavy phases is carefully
washed as the pure toluene which is light phase or solvent enters the column.
7. The interface level is maintained at 100cm above the solvent inlet but the height of the overflow u-tube
above is getting adjusted.
8. Pump P1 is stopped when the liquid starts to overflow at the top of the column.
9. The stirrer at the control panel is switched on.
10. The equipment is ready for the experiment.

General Shut-Down Procedure

1. Pump P1 and P2 are switched off.

2. The stirrer at the control panel is switched off.
3. Valve HV12, HV14 and HV16 are opened. All liquid from the equipment is drained to the waste tank.
4. Pump P2 is switched on. The column is washed until it is clean.
 5. Valve HV16 is opened. So all liquid from the column is drained to the waste tank.
6. Valve HV02, HV07, HV12, HV14, HV18, HV19, HV22 and HV24 are closed.
7. The main switch at the control panel is turned off.

Experimental procedure

1. The General Startup procedure is performed. Both pump P1 and P2 are switched on to allow the liquid
into the collection vessel B3 which is raffinate and B4 which is the extract respectively.
2. The interface level is monitored and maintained at about 10cm above the solvent inlet but the height of
the overflow u-tube is adjusted. The sample is collected once both collection vessels B3 and B4 are filled
with sample products.
3. Valve HV17 is opened to collect the sample of raffinate and valve HV15 is opened to collect the sample
of the extract.
4. The stopwatch is started. Product samples are continued to be collected at 2 minutes, 4 minutes or 6
minutes until the refractive index (RI) values are constant.
5. The refractive index values are recorded into the data table which is appendix A and then both pumps P1
and P2 are stopped.
6. The experiment is repeated, the rotating stirrer is switched on and the stirrer speed is set at 250
revolutions per minute.
7. The general shutdown procedure is performed when the experiment is done.

Data/Results/Calculation:

Ru Feed Solven Solven Rotatin Tim Raffinate Extract HETP Separatio

n flow t flow t to g disc e Refractiv Solute Refractiv Solute (mm) n
No rate rate feed speed (min e index compositio e index compositio efficiency
. (L/min (L/min ratio (RPM) ) n (%) n (%) (%)
) )
1 0.12 0.24 1.2 0 10 1.3385 17.8078 1.4698 10.4280 417.12
20 1.3415 17.8477 1.4120 10.0179 400.716
30 1.4165 18.7951 1.3423 9.5234 380.936
40 1.4211 18.8561 1.3413 9.5163 531. 380.652
50 1.4641 19.4867 1.3402 9.5085 3 380.34
60 1.4650 19.498 1.3401 9.5078 380.312
70 1.4651 19.5 1.3390 9.5 380

2 0.12 0.12 1.1 200 0 1.3372 7.0 1.4335 32.3120 646.24

10 1.3375 7.0 1.4447 32.5645 797 651.29
20 1.3375 7.0 1.4445 32.56 651.2
30 1.3372 7.0 1.4463 32.6 652
SAMPLE CALCULATION SOLUTE COMPOSITION

Calculate for raffinate composition:

Refractive index Solute composition

1.4650 X
1.4651 19.5

𝑥 19.5
=
1.4650 1.4651

𝑥 = 19.498

Calculate for extract composition

Refractive index Solute composition

1.3401 X
1.3390 9.5

𝑥 9.5
=
1.3401 1.3390

𝑥 = 9.51

calculation for all the values are same as the above

Calculation for Height Equivalent Theoretical Plates (HETP)

𝑬𝒇𝒇𝒆𝒄𝒕𝒊𝒗𝒆 𝒄𝒐𝒍𝒖𝒎𝒏 𝒉𝒆𝒊𝒈𝒉𝒕

𝑯𝑬𝑻𝑷 =
𝑵𝒐. 𝒐𝒇 𝒕𝒉𝒆𝒐𝒓𝒆𝒕𝒊𝒄𝒂𝒍 𝒑𝒍𝒂𝒕𝒆𝒔
𝒙
𝟕𝟗𝟕 =
𝟐

𝒙 = 𝟏𝟓𝟗𝟒 (RUN 2)

𝟏𝟓𝟗𝟒
𝑯𝑬𝑻𝑷 =
𝟑

𝑯𝑬𝑻𝑷 = 𝟓𝟑𝟏. 𝟑 (RUN 1)

*calculation for all the values are same as the above

Calculation for Separation Efficiency

𝐴𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑒𝑥𝑡𝑟𝑎𝑐𝑡𝑒𝑑 𝑠𝑜𝑙𝑢𝑡𝑒

𝑬𝒇𝒇𝒆𝒄𝒊𝒆𝒏𝒄𝒚 =
𝐴𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑓𝑒𝑒𝑑

𝐸𝑥𝑡𝑟𝑎𝑐𝑡 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 × 𝐸𝑥𝑡𝑟𝑎𝑐𝑡 𝑐𝑜𝑚𝑝𝑜𝑠𝑖𝑡𝑖𝑜𝑛

=
𝐹𝑒𝑒𝑑 𝐹𝑙𝑜𝑤𝑟𝑎𝑡𝑒 × 𝐹𝑒𝑒𝑑 𝑐𝑜𝑚𝑝𝑜𝑠𝑖𝑡𝑖𝑜𝑛

𝟎. 𝟏𝟐 × 𝟑𝟐. 𝟔
𝟔𝟓𝟐 =
𝟎. 𝟏𝟐 × 𝑭𝒆𝒆𝒅 𝒄𝒐𝒎𝒑𝒐𝒔𝒊𝒕𝒊𝒐𝒏

𝑭𝑪 = 𝟎. 𝟎𝟓
*calculation for all the values are same as the above
Determine of The Binodal / Solubility Curve

Refractive index for pure acetone = 1.3581

Refractive index for pure water = 1.3332
Refractive index for pure toluene = 1.4954

Toluene Rich Phase

No. Amount in mixture (mL) Water added (mL) Composition (wt%) Refractive Index
Acetone Toluene Acetone Toluene Water
1 12.7 104.1 2.5 9.79 2.42 87.78 1.4753
2 25.2 91.8 3.0 19.48 2.92 77.60 1.4649
3 54.0 64.8 4.1 41.61 3.97 54.42 1.4304
4 67.4 50.0 5.4 52.30 5.27 42.43 1.4147
5 77.4 37.5 7.3 60.67 7.20 32.14 1.4006
6 81.6 16.3 23.0 63.58 22.54 13.89 1.3687

Amount in mixture (mL) Water added (mL) Mass (g) Mass Fraction
Acetone Toluene Acetone Toluene Water Acetone Toluene Water
12.7 104.1 2.5 10.1 90.2 2.5 0.0978 0.8778 0.0243
25.2 91.8 3.0 19.9 79.50 3.0 0.1946 0.7761 0.0293
54.0 64.8 4.1 42.7 55.9 4.1 0.4157 0.5444 0.0399
67.4 50.0 5.4 53.3 43.3 50.0 0.3636 0.2953 0.3410
77.4 37.5 7.3 61.3 32.5 37.5 0.4668 0.2475 0.2858
81.6 16.3 23.0 64.6 14.11 16.3 0.6798 0.1486 0.1717

Water Rich Phase

No. Amount in mixture (mL) Water added (mL) Composition (wt%) Refractive Index
Acetone Toluene Acetone Toluene Water
1 81.6 22.0 16.8 63.93 21.68 14.39 1.3681
2 80.1 25.1 13.9 63.14 24.88 11.98 1.3692
3 74.7 34.6 8.0 58.84 34.27 6.89 1.3661
4 65.0 46.1 3.6 51.22 45.68 3.90 1.3618
5 50.4 59.6 1.6 39.65 58.97 1.38 1.3556
6 25.5 80.2 1.4 19.94 78.86 1.20 1.3449

Amount in mixture (mL) Toluene added (mL) Mass (g) Mass Fraction
Acetone Toluene Acetone Toluene Water Acetone Toluene Water
81.6 22.0 16.8 64.5 22.0 14.6 0.6392 0.2178 0.1439
80.1 25.1 13.9 63.4 25.1 12.04 0.6304 0.2498 0.1198
74.7 34.6 8.0 59.1 34.6 6.93 0.5872 0.3439 0.0689
65.0 46.1 3.6 51.4 46.1 3.12 0.5109 0.4581 0.0310
50.4 59.6 1.6 39.9 59.6 1.4 0.3856 0.5913 0.0138
25.5 80.2 1.4 20.2 20.2 1.21 0.1986 0.7895 0.0119
Calculation for Table Toluene Rich Phase & Water Rich Phase
Density of acetone: 0.791 (g/mL)
Density of toluene: 0.866 (g/mL)
Density of water: 1.000 (g/mL)

𝑀𝑎𝑠𝑠 𝑜𝑓 𝑋
MASS FRACTION = 𝑇𝑜𝑡𝑎𝑙 𝑚𝑎𝑠𝑠

Mass of A = amount of mixture x density of mixture

Acetone
Mass of Acetone =12.7mL x 0.791 (g/mL)
= 10.05 (g)
Toluene
Mass of Toluene = 104.1mL x 0.866 (g/mL)
=90.15 (g)

Water
Mass of Water = 2.5 mL x 1.000 (g/mL)
=2.5 (g)
Total Mass
Mass of Acetone + Mass of Toluene + Mass of Water
10.05(g) + 90.15(g) + 2.5(g)
= 102.7 (g)

Mass Fraction of Acetone

10.05 𝑔
= 0.0978
102.7 𝑔
Mass Fraction of Toluene
90.15 𝑔
= 0.8778
102.7 𝑔
Mass Fraction of Water
2.5 𝑔
= 0.0243
102.7 𝑔

*calculation for all the values are same as the above

For table toluene rich phase & water rich phase
Density of acetone: 0.791 g/mL
Density of toluene: 0.866 g/mL
Density of water: 1.000 g/mL
Mass of A
MASS FRACTION, XA = Total mass

Mass of A = amount of mixture (mL) x density of mixture (g/mL)

Acetone
Mass of Acetone =12.7mL x 0.791 g/mL
= 10.05 g
Toluene
Mass of Toluene = 104.1mL x 0.866 g/mL
=90.15 g
Water
Mass of Water = 2.5 mL x 1.000 g/mL
=2.5 g

Total Mass
Mass of Acetone + Mass of Toluene + Mass of Water
10.05g + 90.15g + 2.5g
= 102.7 g

Mass Fraction of Acetone

10.05 g
= 0.0978
102.7 g
Mass Fraction of Toluene
90.15 g
= 0.8778
102.7 g
Mass Fraction of Water
2.5 g
= 0.0243
102.7 g

*Calculation for other values are the same as above

Determine of Equilibrium Solute Distribution (Tie Lines)

No. Amount of mixture (mL) Water rich phase Toluene rich phase
Aceton Water Toluen Refractive Acetone Refractive Acetone
e e index composition index composition
(%) (wt%)
1 76.5 20.0 23.2 1.3621 51.7 1.3735 69.8
2 68.8 20.0 30.2 1.3574 40.8 1.3979 55.5
3 63.7 20.0 34.8 1.3544 32.7 1.3943 50.4
4 56.1 20.0 41.7 1.3531 30.1 1.4213 42.2
5 45.9 20.0 51.0 1.3494 21.4 1.4084 39.4
6 30.6 20.0 64.9 1.3443 9.6 1.4183 32.5

Amount in mixture (mL) Mass (g) Mass Fraction

Acetone Water Toluene Acetone Water Toluene Acetone Water Toluene
76.5 20.0 23.2 60.51 20.0 20.10 0.6015 0.1988 0.1997
68.8 20.0 30.2 54.42 20.0 26.15 0.5411 0.1987 0.2600
63.7 20.0 34.8 50.40 20.0 30.13 0.5013 0.1990 0.2997
56.1 20.0 41.7 44.40 20.0 36.11 0.4416 0.1990 0.3593
45.9 20.0 51.0 36.30 20.0 44.16 0.3613 0.1991 0.4396
30.6 20.0 64.9 24.20 20.0 56.20 0.2410 0.1992 0.5598
Discussion:

1. Determine the required theoretical extraction stage from the liquid-liquid extraction experiment results.
Conclusion:

Solvent extraction is the most versatile of all analytical techniques, with an extremely broad range of
applications that employ most of the physical and chemical principles used in analytical chemistry. Solvent
extraction, also known as liquid-liquid extraction, is based on the principle that a solute can distribute itself in a
specific ratio between two immiscible solvents, one of which is typically water and the other an organic solvent.

So, this experiment can be concluded that from the graph above we get 2 theoretical stages. Based on
the result obtained, the value of Height Equivalent Theoretical Plates (HETP) is higher when the number of
theoretical plates is lower which means the relationship between HETP and the number of theoretical plates is
inversely proportional.

From the overall experiment, it can be concluded that this experiment was successful because all the
objective achieved.

For the recommendation, the experiment should be repeated with three different speeds of the stirrer so
that we can determine the best speed that can get higher value efficiency.

References:
1. Liquid-Liquid Extraction, retrieve from
https://en.wikipedia.org/wiki/Liquid%E2%80%93liquid_extraction
2. Chemical engineering separation, retrieve from
https://iastate.pressbooks.pub/chemicalengineeringseparations/chapter/liquid-liquid-extraction-2/
3. Science Direct, 2007, retrieve from
https://www.sciencedirect.com/topics/immunology-and-microbiology/liquid-liquid-extraction