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Abstract: The different modes of extraction; single stage, cross current and
countercurrent were done in this experiment using the beaker scale extraction
operation. This experiment uses mainly of the sand, NaCl and water mixture
together with the series of laboratory beakers. The extractions were carried out at
different values of solvents for each case. The solutions are withdrawn off after
extraction process for the determination of density using westphal balance. The
density-concentration plot aids in the calculation of the amount of solute in the final
extract and raffinat for different cases.
The efficiencies were computed using the formula for extraction
efficiency. The obtained efficiencies showed that a large amount of solute was
removed from the solution. The cross current operation also showed a decreasing
pattern for the values of the efficiencies.
1
solute through the porous structure of the secondly because the solution will generally
residual solids is the controlling factor, the become more viscous.
material should be of small size so that the Temperature. In most cases, the solubility of
distance the solute has to travel is small. On the material which is being extracted will
the other hand, if diffusion of the solute from increase with temperature to give a higher
the surface of the particles to the bulk of the rate of extraction. Further, the diffusion
solution is the controlling factor, a high coefficient will be expected to increase with
degree of agitation of the fluid is required. rise in temperature and this will also improve
the rate of extraction. In some cases, the
There are four important factors to be upper limit of temperature is determined by
considered: secondary considerations, such as, for
example, the necessity to avoid enzyme
Particle size. Particle size influences the action during the extraction of sugar.
extraction rate in a number of ways. The Agitation of the fluid. Agitation of the
smaller the size, the greater is the interfacial solvent is important because this increases
area between the solid and liquid, and the eddy diffusion and therefore the transfer
therefore the higher is the rate of transfer of of material from the surface of the particles
material and the smaller is the distance the to the bulk of the solution, as discussed in the
solute must diffuse within the solid as already following section. Further, agitation of
indicated. On the other hand, the surface may suspensions of fine particles prevents
not be so effectively used with a very fine sedimentation and more effective use is made
material if circulation of the liquid is of the interfacial surface.
impeded, and separation of the particles from
the liquid and drainage of the solid residue Processes Involved in Leaching
are made more difficult. It is generally
desirable that the range of particle size should Three distinct processes are usually involved
be small so that each particle requires in leaching operations:
approximately the same time for extraction (a) Dissolving the soluble constituent.
and, in particular, the production of a large (b) Separating the solution, so formed, from
amount of fine material should be avoided as the insoluble solid residue.
this may wedge in the interstices of the larger (c) Washing the solid residue in order to free
particles and impede the flow of the solvent. it of unwanted soluble matter or to obtain as
Solvent. The liquid chosen should be a good much of the soluble material as possible as
selective solvent and its viscosity should be the product.
sufficiently low for it to circulate freely.
Generally, a relatively pure solvent will be Leaching has in the past been carried out
used initially, although as the extraction mainly as a batch process although many
proceeds the concentration of solute will continuous plants have also been developed.
increase and the rate of extraction will The type of equipment employed depends on
progressively decrease, first because the the nature of the solid —whether it is granular
concentration gradient will be reduced, and or cellular and whether it is coarse or fine.
2
The normal distinction between coarse and (B) Preparation of the Fresh Feed
fine solids is that the former have sufficiently 1. Weight 12 dry 1L beakers and label
large settling velocities for them to be readily as follows: I, II, III, IV, V, VI, VII,
separable from the liquid, whereas the latter VIII, IX, X, XI, XII.
can be maintained in suspension with the aid 2. Place into each beaker the sand-salt
of only a small amount of agitation. mixture pack. The pack contains 150g
sand; the amount salt is unknown.
The objectives of the experiment are to 3. Pour 150 mL of water into each
compare single-stage, crosscurrent and beaker and mix thoroughly.
countercurrent beaker-scale extraction 4. Measure the liquor density of beaker
operation and to calculate single-stage, XII. This is the fresh feed liquor
crosscurrent and countercurrent extraction density.
efficiencies. 5. Determine the weight percent
composition of the fresh feed.
3
beaker V, and in four 150mL portions 7. Add Decant IX into beaker X, mix
to beaker VI (e.g. Pour 300mL of well, and then decant 600mL of
water into beaker IV, stir well and solution. Label this solution Decant
allow to settle; then, draw off 300mL XI again.
of the clear liquor into a separate 8. Add 600mL of water into Beaker X,
container. Add the next portion of mix well, and then decant 600mL of
water. Mix well, and then draw off solution. The measuring mixture is
300mL into another container.) the raffinate.
2. Determine the density and percent
weight of NaCl of the clear liquors. 9. Measure the density of the raffinate
solution and determine the wt%
composition.
(E) Steady-state Multistage
10. Add Decant X into beaker XI, mix
Countercurrent Extraction
well, and then decant 600mL of
Operation
solution. This solution is called the
1. Add 600mL of water into beaker VII, extract.
mix well, and then decant 600mL of 11. Measure the density of the extract and
solution. Label this solution Decant determine the weight percent
VII. composition.
2. Add 600 mL of water into beaker VII, 12. Calculate the salt extraction
mix well, and then decant 600mL of efficiency using two different
solution. Label this solution Decant formulas.
VIII.
3. Add Decant VII into beaker VIII, mix Results and Discussion
well, and then decant 600mL of
Density Weight % NaCl
solution. Label this solution Decant
VII again. 0.10 mg/L 0%
4. Add 600mL of water into beaker VIII,
mix well, and then decant 600mL of 0.25 mg/L 4%
solution. Label this solution Decant-
XI. 0.35 mg/L 8%
5. Add Decant VIII into beaker IX, mix 0.39 mg/L 12%
well, and then decant 600mL of
solution. Label this solution Decant 0.3925 mg/L 16%
VIII again.
6. Add 600mL of water into beaker IX, 0.435 mg/L 20%
mix well, and then decant 600mL of 0.65 mg/L 25%
solution. Label this solution Decant
X.
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A. Construction of Density-
Concentration Plot for NaCl
Solution
0.6
0.5
0.4
DENSITY
0.3
0.2
0.1
0
0% 5% 10% 15% 20% 25% 30%
WEIGHT % COMPOSITION
5
B. Preparation of the Fresh Feed C. Single-Stage Extraction Operation
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝐹𝑒𝑒𝑑
(8)(5𝑔) + 5(50𝑚𝑔) + 6(500𝑚𝑔) V2 V1
=
150 Beaker I
𝑔 L1 L2
= 0.2833
𝑚𝐿
(8)(5𝑔) + 2(6)(500𝑚𝑔)
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝑉2 =
150 𝑚𝐿
𝐴𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑁𝑎𝐶𝑙 𝑖𝑛 𝐹𝑒𝑒𝑑 = 0.054 𝑔
= 0.3067
𝑥 𝑔 𝑁𝑎𝐶𝑙 𝑚𝐿
=
150 𝑔 𝑠𝑎𝑛𝑑 + 150 𝑔 𝐻2 𝑂 + 𝑔 𝑁𝑎𝐶𝑙
𝑥 = 17.12 𝑔 𝑁𝑎𝐶𝑙
Baed on Density-Concentration plot,
concentration of NaCl in V2 is 0.062
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(8)(5𝑔) + (7)(5𝑔) 𝐴𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑁𝑎𝐶𝑙 𝑖𝑛 𝑉2 = 0.02
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝑉2 = 𝑥
300𝑚𝐿 =
𝑔 600 + 𝑥
= 0.25
𝑚𝐿 𝑥 = 12.24 𝑔
12.24
𝐸𝑥𝑡𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝐸𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦 = 𝑥 100
17.12
Based on Density-Concentration plot,
= 71.50%
concentration of NaCl in V2 is 0.04
𝑒𝑥𝑡𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑒𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦
Based on Density-Concentration plot, 𝑎𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑠𝑎𝑙𝑡 𝑖𝑛 𝑡ℎ𝑒 𝑒𝑥𝑡𝑟𝑎𝑐𝑡
concentration of NaCl in V2 is 0.02 = 𝑥 100%
𝑎𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑠𝑎𝑙𝑡 𝑖𝑛 𝑡ℎ𝑒 𝑓𝑒𝑒𝑑
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The extraction efficiencies obtained were
57.89%, 73.015% and 71.50% for beaker I, II
and III respectively. 𝐴𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑁𝑎𝐶𝑙 (𝑦)𝑖𝑛 𝐸2 = 0.018
𝑦
=
300 + 𝑦
𝑦 = 5.50 𝑔
D. Multistage Crosscurrent Extraction
Operation 𝐸𝑥𝑡𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝐸𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦
9.28 + 5.50
Beaker IV = 𝑥 100
17.12
300 g H2O 300 g H2O = 86.33%
150 g sand
17.12g NaCl
150 g H2O
E1 Beaker V
x g NaCl E2
y g NaCl
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝐸1
(8)(5𝑔) + (5)(5𝑔) + (3)(500𝑚𝑔) + (7)(500𝑚𝑔) 200 g H2O 200 g H2O 200 g H2O
=
300 𝑚𝐿
𝑔
= 0.2393 150 g sand
𝑚𝐿
17.12g NaCl
150 g H2O
E1 E2 E3
Based on Density-Concentration plot, x g NaCl y g NaCl z g NaCl
concentration of NaCl in E1 is 0.03
(8)(5𝑔) + (2)(500𝑚𝑔)
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝐸1 =
𝐴𝑚𝑜𝑢𝑛𝑡 𝑖𝑓 𝑁𝑎𝐶𝑙 (𝑥) 𝑖𝑛 𝐸1 = 0.03 200 𝑚𝐿
𝑔
𝑥 = 0.205
= 𝑚𝐿
300 + 𝑥
𝑥 = 9.28𝑔 Based on Density-Concentration plot,
concentration of NaCl in E1 is 0.018
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝐸2
(7)(5𝑔) + (5)(5𝑔) + (2)(500𝑚𝑔) + (7)(500𝑚𝑔)
=
300 𝑚𝐿
𝑔 𝐴𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑁𝑎𝐶𝑙 (𝑥)𝑖𝑛 𝐸2
= 0.215
𝑚𝐿 𝑥
0.018 =
200 + 𝑥
𝑥 = 3.67𝑔
Based on Density-Concentration plot,
concentration of NaCl in E2 is 0.018
8
(8)(5𝑔) + (1)(500𝑚𝑔) Beaker VI
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝐸2 =
200 𝑚𝐿
𝑔
= 0.2025 150mL 150 mL 150 mL 150mL
𝑚𝐿
150 g sand
17.12g NaCl
150 g H2O
Based on Density-Concentration plot,
concentration of NaCl in E2 is 0.045
E1 E2 E3 E4
w x y z
(9)(5𝑔) + (1)(5𝑔)
𝐴𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑁𝑎𝐶𝑙 (𝑦)𝑖𝑛 𝐸2 𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝐸1 =
𝑦 150 𝑚𝐿
0.045 = 𝑔
200 + 𝑦 = 0.333
𝑚𝐿
𝑦 = 9.42
(7)(5𝑔) + (7)(500𝑚𝑔)
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝐸3 = Based on Density-Concentration plot,
200𝑚𝐿
𝑔 concentration of NaCl (w) in E2 is 0.071
= 0.1925
𝑚𝐿
(5)(5𝑔) + (1)(5𝑔)
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝐸2 =
150 𝑚𝐿
𝑔
𝐴𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑁𝑎𝐶𝑙 (𝑧)𝑖𝑛 𝐸3 0.20
𝑧 𝑚𝐿
0.008 =
200 + 𝑧
𝑧 = 1.61 𝑔
Based in Density-Concentration plot,
𝐸𝑥𝑡𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝐸𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦 concentration of NaCl in E2 is 0.008
3.67 + 9.42 + 1.61
= 𝑥 100
17.12
= 85.89%
𝐴𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑁𝑎𝐶𝑙 (𝑥)𝑖𝑛 𝐸2
𝑥
0.008 =
150 + 𝑥
𝑥 = 1.21𝑔
(5)(5𝑔) + 9(500)
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝐸3 =
150 𝑚𝐿
9
𝑔 from the solution. The densities were then
= 0.1967
𝑚𝐿 measured using the westphal balance. The
corresponding amount of NaCl in the extract
Based on Density-Concentration plot, were calculated using the readings from the
concentration of NaCl in E3 is 0.004 density-concentration plot. As you can see in
the data, the values of efficiencies were
86.33%, 85.88% and 80.61%. These values
showed a decreasing pattern, and it means
𝐴𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑁𝑎𝐶𝑙 (𝑦)𝑖𝑛 𝐸3
𝑦 that the solute extracted for the first two
0.004 = stages has a higher value than that in the last
150 + 𝑦
stage. This is simply because, as extraction
𝑦 = 0.60 𝑔
proceeds, the solute being extracted
(5)(5𝑔) + (8)(500𝑚𝑔) decreases. The computation also showed that
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝐸4 = extraction of the solute is highest at the 2nd
150 𝑚𝐿
= 0.1933 stage. This must be due to human and
instrumental error, because usually, the first
extract has the greatest value.
Based on Density-Concentration plot,
concentration of NaCl in E4 is 0.0035
E. Steady-state Multistage Counter-
current Extraction Operation
𝐴𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑁𝑎𝐶𝑙 (𝑥)𝑖𝑛 𝐸4
𝑧
0.0035 = Extract (E) 600 g H2O
150 + 𝑧 y g NaCl
𝑧 = 0.53 𝑔
150 g sand Raffinate (R)
𝐸𝑥𝑡𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝐸𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦 17.12g NaCl
11.46 + 1.21 + 0.60 + 0.53 x g NaCl
150 g H2O
= 𝑥 100
17.12
= 80.61%
Raffinate:
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝑅𝑎𝑓𝑓𝑖𝑛𝑎𝑡𝑒
In crosscurrent extraction operation, the feed
(6)(5𝑔) + (9)(500𝑚𝑔)
containing the solute is contacted with the =
solvent for each extraction stage. The extracts 150 𝑚𝐿
𝑔
are collected separately at each stage. In this = 0.23
𝑚𝐿
case, in each stage, the feed was contacted
with 150 mL of water.
With the aid of beaker IV, V and VI, the Based on Density-Concentration plot,
extracts from each stage were withdrawn concentration of NaCl in R is 0.024
10
counter-currently. The extract phase contains
the solute we desire to remove. In this case,
𝐴𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑁𝑎𝐶𝑙 (𝑥)𝑖𝑛 𝑅𝑎𝑓𝑓𝑖𝑛𝑎𝑡𝑒 series of decantation were performed to
𝑥
= 0.029 = finally get the extract and raffinate solutions.
150 + 𝑥
The raffinate solution contains less of the
𝑥 = 4.489
solute. The raffinate and extract solution’s
𝐸𝑥𝑡𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝐸𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦 𝑏𝑎𝑠𝑒𝑑 𝑜𝑛 density were measured using the westphal
𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑁𝑎𝐶𝑙 𝑖𝑛 𝑅𝑎𝑓𝑓𝑖𝑛𝑎𝑡𝑒 balance. The density-concentration plot in
(17.12 − 4.48) the letter A was read to get the corresponding
= 𝑥 100
17.12 concentration of NaCl in both extract and
= 73.83% raffinate phases. The amount of NaCl in
extract and raffinate was then calculated
using the concentration obtained.
Extract:
Using the formula for extraction efficiency,
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝐸𝑥𝑡𝑟𝑎𝑐𝑡 the extraction efficiency based on the extract
(2)(9)(5𝑔) + (2)(4)(5𝑔) + (1)(500𝑚𝑔) and raffinate was calculated. The extraction
= efficiencies are 73.83% and 67.87% for the
600 𝑚𝐿
𝑔 raffinate and extract respectively. These
= 0.2175
𝑚𝐿 values of efficiencies showed that the solute
was quite efficiently removed from the
solution. This experiment may be prone to
Based on Density-Concentration plot, human and instrumental errors but still, we
concentration of NaCl in E is 0.019 got good results by what the efficiencies
showed.
11
withdrawn off at the final stage. In this
experiment we employed the use of beaker
scale extraction operation. Series of beakers
are used to separate the desired solute from
the solution. One must utilize the use of
beakers because they are used to transfer the
solution, decant and withdraw the extract.
References
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