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College of Engineering
Department of Chemical Engineering
Experiment 1:
Extraction of CuSO4 from sand/CuSO4
mixture using solvent (water)
Name
Mohammad Abdulla Rustom
Fawaz Hussain Alhamry
Khaled Mohammed Saif
Hani Saad Al-qashar
I.D
20123943
2011747
20120276
20123940
Experiment#1:
Name
Part Assigned
Percenta
ge %
Fawaz Husain
Alhamry
25%
Khaled
Mohammed
Saif
Mohammed
Abdulla
Rostum
25%
25%
25%
Signatu
re
Abstract
Leaching is a process where solid-liquid separation occurs. So this
experiment aims to extract Copper Sulfate from sand/ Copper
Sulfate mixture by using water as a solvent. The experiment
objective is achieved by first mixing the solute (Copper Sulfate
CuSO 4 ) with the sand and introducing them to the single step
extractor, Then the liquid solvent will be introduced to the extractor
for the separation to take place. The single stem extractor is a
vessel that has a membrane where the mixture is placed on. This
vessel is connected to a heater and condenser in order to remove
the impurities from the solvent (water) before processing it. Then,
samples are going to be taken every 20 minutes and fit them to the
standard cure (Beer's law) in order to measure their concentrations.
Moreover, the standard cure will be obtained using the UV
spectroscopy, where the absorbances of known samples are going
to be measured and related to their concentrations. The known
samples were prepared by the students and they are 20, 15, 10, 5,
2.5, 1.25 g/L. worth mentioning, the standard curve has coefficient
determination (R) of 0.9865, which indicates a linear relationship
between the absorbance and the concentration. The observed
results were expected, the mass of extracted solute
(CuSO 4)
was
Table of contents
1. Introduction and background.......................................................................1
2. Theory.......................................................................................................... 3
2.1. Definitions of the extraction processes..................................................3
2.2. Types of extractors................................................................................. 3
2.3. Solid liquid extraction (Leaching process)...........................................3
2.4. Special aspects for the extractors..........................................................4
2.5. Selection of the solvent..........................................................................4
2.6. Solid liquid extraction (Leaching) Principles...........................................4
3. Industrial applications..................................................................................7
3.1. Gold carbon in leach process.................................................................7
3.2. Extraction of caffeine from tea leaves...................................................7
3.3. Extraction process of sugar beets..........................................................8
4. Apparatus and procedure.............................................................................9
4.1. Apparatus.............................................................................................. 9
4.2. Procedure............................................................................................. 10
5. Safety and environment.............................................................................11
6. Results....................................................................................................... 14
7. Discussion.................................................................................................. 17
8. Conclusions................................................................................................ 18
9. Recommendations...................................................................................... 19
9.1. Improvement of the lab........................................................................19
9.2. Correction of errors.............................................................................. 19
10. References............................................................................................... 20
11. Appendices............................................................................................... 21
2
List of figu
Figure 1: golden ore ............................................................................... 1
Figure 2: Example for Beer's law .....................................................................5
Figure 3: The spectroscopy device ...............................................................5
Figure 4: The molecules transformation .................................................5
Figure 5: Extraction of caffeine from tea leaves ...........................................8
Figure 6: sugar beets ................................................................................... 8
Figure 7: Extraction apparatus.........................................................................9
Figure 8: Single step extractor.........................................................................9
Figure 9: Single extractor location....................................................................9
Figure 10: The mixture................................................................................... 10
Figure 11: UV spectroscopy............................................................................10
Figure 12: copper sulfate solution..................................................................10
Figure 13: Safety guidelines...........................................................................11
Figure 14: Fire Extinguisher............................................................................11
Figure 15: Fire blanket and first Aid kit...........................................................11
Figure 16: Eye wash fountain.........................................................................12
Figure 17: Emergency shower........................................................................12
Figure 18: Fume hood..................................................................................... 12
Figure 19: Fire exit door..................................................................................12
Figure 20: sewage.......................................................................................... 12
Figure 21: Chemical waste container..............................................................13
Figure 22: Gas cylinder................................................................................... 13
Figure 23: Standard curve (Beer's law), prepared using the data from the
spectrometer.................................................................................................. 14
Figure 24: Extraction rate of
CuSO 4
List of tables
Table 1: observed absorbances for the prepared samples to perform the STD
curve.............................................................................................................. 14
Table 2: obtained absorbances for the known samples, and the calculated
concentrations using the STD curve...............................................................15
Table 3: presents useful quantities to analyze leaching.................................15
`
Extraction process is the process of extracting a substance (solute)
from a mixture of substances by using proper solvent based on the
solubility criteria. There are different types of extraction process such
as liquid-liquid extraction, solid-liquid extraction, liquid-gas extraction
and high pressure extraction. Liquid liquid extraction is the
extraction of a substance from one liquid to another liquid phase
1
the
experiment.
Moreover,
recommendations
were
2. Theory
In this part of the report, the theoretical aspects of the experiment will
be illustrated. Firstly, the extraction process could be defined as the
process that is used to separate one substance from another
substance. Moreover, there are different types of extraction processes
such as solid liquid extraction (leaching process), liquid liquid
extraction, gas liquid extraction (absorption) and high pressure
extraction [4].
2.1. Definitions of the extraction processes
Here are the definitions of these processes shortly. Liquid liquid
extraction is the extraction of a substance from one liquid to another
liquid phase based on their relative solubility [5]. Gas liquid
extraction is the extraction or absorbing of a gas by using liquid
solvent [4]. High pressure extraction is an extraction process occurred
at relatively high pressure condition, also it usually uses densified gas
as a solvent [6]. Solid-liquid extraction is the extraction of a solid by
using liquid solvent and it`s called leaching process [4].
as
Single
step
mixer,
mixer
settler
cascade,
centrifugal
taking
the
corresponding
concentration
of
the
measured
mcuso 4 (extract)
m cuso 4 (initial)m cuso4 (extract )
(3)
mcuso 4 (extract)
(4 )
mcuso 4 (initial)
m cuso 4(extract )
m cuso 4(initial )
100(5)
3. Industrial applications
Solid-liquid extraction is widely used in many applications such as
laboratory applications (sample preparation), industrial applications
(extraction
from
vegetable
matrices)
and
practical
applications
from one end to the other and the water is moved in the opposite
direction and that called counter-current flow and as the water goes it
becomes a stronger sugar solution mostly called juice [14].
First of all, a single step extractor where placed in the extraction unit
as elaborated in figure 9. Then, the control panel as shown in figure 7
is turned on to start heating the distilled water inside the round flask
which is placed in the heater as shown in figure 7. The water will
evaporate inside the round vessel and heated by boiler and pass
through the distillation column to reach the condenser as shown in
figure 7. Water vapor will condense after touching the running water
tubes through the condenser as shown in figure 7, then the saturated
vapor is going to be a saturated liquid. Finally, the saturated liquid will
fall down to the single step extraction vessel in form of drops because
of gravity as shown in figure 8. Distilled water will mix with the sand
and copper sulfate mixture inside the extractor vessel location. The
distilled water penetrates loaded with copper sulfate throw the filter in
order to extract the CuSO4 from sand.
10
Condenser
Condenser
Distillation column
Distillation column
Control panel
Control panel
Thermometer
Thermometer
Figure Boiler
7: Extraction
Round vessel
apparatus.
Boiler
4.2. Procedure
Round vessel
First of all, 10 g of
copper sulfate are mixed with amount of sand, then placing them
inside a vessel extractor as elaborated in figure 10 which is going to be
placed in the extraction unit below the condenser. Then saturated
water will fall down inside the vessel to diffuse into the mixture of
copper sulfate and sand in order to be mixed with the solute which is
copper sulfate. After that, Solvent will go down through the filter
loaded with copper sulfate.
Every 20 minutes, a sample of solution was taken for four times to
observe and test the concentration change of the samples with the
time. Finally, analytically the copper sulfate solution is to be tested to
relate the concentration with absorbance using UV spectroscopy as
shown in figure 11. Six different concentrations (20, 15, 10, 5, 2.5,
11
Figure 11: UV
spectroscopy
5. Safety and
environment
Other important point that is found in the laboratory is eye wash which
is a necessary tool while dealing with chemicals, it was fixed in a
proper place as shown in figure 16 and it is working properly. Also,
emergency shower was located side by side with the eye wash as
illustrated in figure 17.
Moreover, figure 18 shows the fume hood which was provided in the
laboratory which is a very important thing to be exist in any chemical
laboratory in order to remove the toxic gases of chemicals
Fire exit door was located in a visible place and noticed to be a wide
enough but it does not open properly as shown in figure 19. Other
negative point that is noticed in the laboratory is the sewage area, it
was found that the electricity wires are so close to the water that is
kept running to the sewage as shown in figure 20.
13
14
6. Results
The results for this experiment are divided into two parts, first
performing the standard curve, then the extraction process. The curve
was performed by having 6 samples of
CuSO 4
dissolved in water
Molar concentration
(mol/L)
0.125
0.0940
0.0627
0.0313
0.0157
0.00783
15
Absorbance
1.318
0.81
0.472
0.25
0.135
0.05
Table 1: observed absorbances for the prepared samples to perform the STD
curve.
0.12
0.1
0.08
0.06
0.04
0.02
0
0
0.2
0.4
0.6
0.8
1.2
1.4
Figure 23: Standard curve (Beer's law), prepared using the data from the
spectrometer.
CuSO 4
Volume
(mL)
Absorbanc
e
Molarity
(mol/L)
20
40
60
80
205
365
395
490
0.234
0.076
0.01
0.009
0.028
0.0094
0.00895
0.0087
Mass
concentration
(g/L)
5
1.5
1.42
1.39
Table 2: obtained absorbances for the known samples, and the calculated
concentrations using the STD curve.
16
Extractio
n factor
Extractio
n fraction
20
40
60
80
0.114
0.187
0.271
0.392
0.103
0.157
0.213
0.281
Extractio
n rate
(g/min)
0.0513
0.0393
0.0356
0.0352
%
Recovery
10.3
15.7
21.3
28.1
CuSO 4
20
30
40
50
60
70
80
90
17
CuSO 4
20
30
40
50
60
70
80
90
7. Discussion
In this part of the report, the results and the calculations will be
discussed for further understanding the leaching process. Table 1
shows
the
concentrations
of
the
prepared
samples
and
the
were
tabulated
in
table
2.
The
observed
coefficient
the observed values fit for linear relation between the absorbance and
the concentration.
Table 3 represents the extraction factor, fraction, recovery and the
extraction rate. Both the extraction factor and fraction were increasing,
which obvious, since as the solvent amount is increasing, more
CuSO 4
CuSO 4
time passes, so the rate at the beginning was high because the extract
amount is high, while then the extract reduces which reduces the rate.
Finally, the recovery is increasing which expected because as the time
passes more
CuSO 4
is that the final recovery that was achieved is 28.1%, which is too low.
That is because the 80 minutes were not enough for having better
recovery of
CuSO 4 .
The extraction rate was calculated and plotted with time in figure 24,
which indicates that as the separation is processing, the extraction rate
is decreased. That is expected since the driving force is decreasing,
which is the concentration gradient. Moreover, figure 25 shows the
decrease in the concentration of the
CuSO 4
in the raffinate.
8. Conclusions
To conclude, the experiment objectives were achieved. Many relations
were found during analyzing and discussing the results. The extraction
of the solute (Copper sulfate) is inversely proportional to the time of
19
20
9. Recommendations
9.1. Improvement of the lab
Regarding the environment of the laboratory it is recommended to
recycle the running water that is used in the condenser for other
purposes such as irrigation instead of draining it to sewage. Moreover,
it is recommended to have better housekeeping including arranging
the electrical wires. Further, it is recommended to place the chemical
waste in a proper place. Also, the chemical waste was noticed without
a proper sealing, it was covered with only gloves. In addition, a gas
cylinder was kept in the laboratory without any information about it.
Hence, it is safer to keep the gas cylinder in the corresponding
apparatus or take it outside the laboratory.
21
10. References
[1] Extraction process, http://www.jove.com/scienceeducation/5538/solid-liquid-extraction , Date accessed 4th October
2016.
[2] Liquid-liquid extraction,
http://courses.chem.psu.edu/chem36/Experiments/PDF's_for_technique
s/Liquid_Liquid.pdf , Date accessed 4th October 2016.
[3] Extraction process types,
https://www.researchgate.net/post/What_is_the_application_of_High_Pr
essure_Processing_on_edible_oil_extraction_from_plants , Date
accessed 4th October 2016.
[4] Laboratory manual.
[5] J. D. Keane, C. T. Smith 'Journal of the American Oil Chemists
Society 1958
[6] High pressure extraction,
https://www.researchgate.net/post/What_is_the_application_of_High_Pr
essure_Processing_on_edible_oil_extraction_from_plants, Date
accessed 29th September, 2016.
[7] Types of extractors, file:///C:/Users/DELL/Downloads/02%20Script
%20Extraction%20(1).pdf, Date accessed 30th September, 2016.
[8] Leaching process, http://documents.mx/documents/liquid-solidextraction-exp-3.html, Date accessed 30th September, 2016.
[9] Selection of the solvent,
http://www.separationprocesses.com/Extraction/SE_Solvent.htm, Date
accessed 1st October, 2016.
[10] Beer`s law,
http://webs.anokaramsey.edu/chemistry/Chem1061/Labs/BeersLaw/Bee
rsLaw-07.htm, Date accessed 1st October, 2016.
[11]
UV
spectroscopy,
http://www.chemguide.co.uk/analysis/uvvisible/theory.html,
Date
th
accessed 3 October, 2016.
22
11. Appendices
Appendix (A): Raw data
23
m
MW
24
For example,
n=
20 g / L
=0.1253mol / L
159.609 g/mol
Moreover, the previous equation was also used for the unknown
concentrations of the
CuSO 4
mass concentration.
After recording the volume of the unknown samples and finding the
concentrations from the standard cure, we were able to find the
extracted mass of
CuSO 4
through:
g
X 0.205 L=1.025 g of CuSO 4
L
For example,
mExtracted=101.025=8.975 g of CuSO 4
Then the extraction factor and fraction, as well as the % recovery could
be calculated through:
Extraction factor =
mExtracted
mRaffinate
Extraction fraction=
mExtracted
initial amount
25
mraffinate=8.975 g
Therefore,
Extractionfactor =
1.025
=0.114
8.975
Extraction fraction=
1.025
=0.1025
10
%Recovery=Extraction fraction100=10.25
1.5725 g
=0.0393 g/min
40 min
26
Symbol
Unit
Definition
C cuso 4 (extract )
mol
L
Concentration of extracted
copper sulfate
V mixture
ml
mcuso 4 (initial )
mcuso 4 (extract )
mcuso 4 (raffinate )
Dimension
less
Extraction factor
27
28