Ion Exchanger Lab Report

EKC 396 Open-ended Laboratory.
Semester II, Session 2022/2023)
UNIVERSITI SAINS MALAYSIA

SCHOOL OF CHEMICAL ENGINEERING
SEMESTER 2, ACADEMIC SESSION 2022/2023
EKC396: CHEMICAL ENGINEERING LABORATORY III
UO07: ION EXCHANGER
GROUP 8
LOH LI YAN 152840

MAH HIN MAN 148703
NUR AMYRA BINTI SAHRIR 150204
MUHAMMAD ROSLAN FIKRI BIN ROSLEE 153899
LECTURER : PROFESSOR DR. LIM JIT KANG

EKC 396 Open-ended Laboratory. Semester II, Session 2022/2023)
Problem Statement
In general, drinking water quality wouldn’t be influenced too much by its hardness, however, it
poses a serious threat in industrial settings. Water hardness needs to be controlled and monitored in
order to avoid the complete breakdown of certain operational units, most notably, cooling towers,
boilers etc. Under this scenario, water softening is the only option to reduce the water hardness and
ion exchange resin has been used quite pervasively as one of the effective materials to serve this
purpose. Recently your company has installed an ion exchange column and your team is putting a
task to study it effective usages. You and your colleagues are putting on a task to first determine the
loading capacity of the column. Taking a simple binary exchange reaction between ion a (charge za)
and ion b (charge zb) as:
𝒛𝑩 𝑨𝒁𝑨 + 𝒁𝑨 𝑩¯𝒁𝑩 ↔ 𝒛𝑨 𝑩𝒁𝑩 + 𝒛𝑩 𝑨¯𝒁𝑨
Where superscript bars refer to the ions in a solid ion exchanger. Determine the selectivity
coefficient of your system. At equilibrium, determine the distribution coefficient of your model
system and verify whether this distribution coefficient changes with respect to the concentration of
your targeted ion.
Table of Content
Abstract ................................................................................................................................................ 1
1.0 Introduction ............................................................................................................................... 1
2.0 Objectives.................................................................................................................................. 3
3.0 Methodology ............................................................................................................................. 3
3.1 Experimental Setup .................................................................................................................... 3
3.2 Calibration Curve ....................................................................................................................... 3
3.3 Regeneration .............................................................................................................................. 3
3.4 Rinsing ....................................................................................................................................... 4
3.5 Experiment A: Effect of Ion Valency ........................................................................................ 4
3.6 Experiment B: Effect of Concentrations .................................................................................... 5
3.7 Result Calculation and Analysis ................................................................................................ 5
4.0 Results ....................................................................................................................................... 6
4.1 Calibration Curve ....................................................................................................................... 6
4.2 Experiment A: Effect of Ion Valency ........................................................................................ 7
4.3 Experiment B: Effect of Concentration ..................................................................................... 8
4.4 Graphical Illustration of Loading Capacity, Selectivity Coefficient and Distribution
Coefficient at Varied Conditions ..................................................................................................... 9
5.0 Discussion ............................................................................................................................... 11
5.1 Calibration Curve ..................................................................................................................... 11
5.2 Experiment A: Effect of Ion Valency ...................................................................................... 11
5.3 Experiment B: Effect of Concentration ................................................................................... 12
5.4 Error Analysis .......................................................................................................................... 13
5.5 Recommendations on Further Improvements .......................................................................... 13
6.0 Conclusion .............................................................................................................................. 14
7.0 References ............................................................................................................................... 15
Appendices ............................................................................................................................................ i
Appendix A.1: Experimental Setup .................................................................................................. i
Appendix A.2: Raw Data .................................................................................................................ii
Appendix A.3: Sample Calculation ................................................................................................ xi
Abstract
This study assesses the effect of ion valency and test water concentration on loading capacity,
selectivity coefficient of the system and the distribution coefficient of targeted ions at equilibrium.
In this experiment, the ion exchanger unit, made up of a cation and anion exchanger column,
however only the cation exchange column was used. Two solutions of different valency i.e.,
magnesium chloride (+2) and aluminium chloride (+3) were used to study the effect of ion valency
on the loading capacity and the selectivity coefficient of the system. The results proved that the
loading capacity is the same while the system is more selective towards the ions of higher valency.
Then, aluminium chloride solution is used in the second part of the experiment since the system is
more selective towards Al3+ ions than it does Mg 2+
ions. Our findings suggested that the loading
capacity of the system is still the same; the selectivity coefficient of the system increases at
increasing concentration; however, at exceedingly high test water concentrations, the distribution
coefficient of Al3+ ions decrease as the test water concentration increases.
1.0 Introduction
Water hardness is a long-standing issue that has plagued a great number of Earth population,
causing them to lose access to healthy drinkable water. Hard water is typically defined as water that
contains a high concentration of calcium and magnesium ions; however, hardness can be caused by
several dissolved metals that form multivalent ions (Sengupta, 2013). Various separation processes
have been introduced in water treatment to soften hard water for safe consumption, namely reverse
osmosis, adsorption, ion exchange and so on.
According to (Kubisch & Korff, 2013), ion exchange reaction is a chemical reaction in which the
unwanted ions are “exchanged” for more favorable ions. In many cases, it is desirable to replace the
targeted ions with safer ions such as Na+. In an ion exchanger, the hard water is conducted through
a column filled with resins, which bind the targeted ions and release the more tolerable ions. In this
process, the targeted ions become “fixed” ions as they attached onto the resin bed. These fixed ions
displace the desirable ions (Na+), referred to as counterions, from the column. The resins are said to
have “exchanged” ions with the test water. This process is illustrated in Figure 1.1 below.
1
Figure 1.1: Illustration of Ion Exchange (Kubisch & Korff, 2013)

An ion exchange process can either be a cation exchange or an anion exchange. Water softening
process typically involves only the cation exchange column. Therefore, our study merely focuses on
the cation exchange process. A typically representation of a cation exchange reaction is shown
below:
𝐴𝑛+ + 𝑛𝐵 + 𝑅 ↔ 𝐴𝑛+ 𝑅𝑛 + 𝑛𝐵 + (1)
Whereas A is the targeted ions; B is the ions embedded onto the resin; R is the resin; and n is the
valency of targeted ions.
The ion exchange reaction is reversible and does not cause any permanent changes to the solid ion-
exchanger. Thence, it can be used repeatedly unless fouling occurs due to the attachment of organic
compounds in the liquid feed onto the ion exchange sites (Seader, J. D., & Henley, E. J., 2005).
Figure 1.2 below shows the water softening and recharge process of an ion exchanger:
Figure 1.2: Schematics of Water Softening and Recharging of an Ion Exchanger (Taiyuan Lanlang
Technology Industrial Corp., n.d.)
2
2.0 Objectives
1. To determine the loading capacity of the ion exchange column at different valency of ions,
and different concentration of ions.
2. To determine the selectivity coefficient of the system at different valency of ions.
3. To study the effect of concentration of ions on the distribution coefficient of the system at
equilibrium.
3.0 Methodology
3.1 Experimental Setup
The ion exchanger unit, made up of a cation and anion exchanger column, was used in this
experiment. Throughout our experiment, we merely utilized the cation exchanger column. The
chemicals used in the whole experiment were sodium chloride ( 𝑁𝑎𝐶𝑙 ), magnesium chloride
hexahydrate (𝑀𝑔𝐶𝑙2 ⋅ 6𝐻2 𝑂), aluminium chloride hexahydrate (𝐴𝑙𝐶𝑙3 ⋅ 6𝐻2 𝑂) and cation exchange
resin (RESINEX K-8). Magnesium chloride hexahydrate and aluminium chloride hexahydrate
solutions were used to study the effect of ion valency on selectivity coefficient of the system.
Magnesium and aluminium salts are used since they are in the same period of periodic table,
therefore they have similar size: effect of ionic sizes will not be significant in this study. Measuring
tools such as a flowmeter and conductivity meter were used to control the flow rate (in cm 3/min)
and measure the conductivity of the solution (in milliSiemens per centimeter, mS/cm), respectively.
3.2 Calibration Curve
Six standard solutions of 100mL magnesium chloride hexahydrate with different concentrations (0
M, 0.2 M, 0.4 M, 0.6 M, 0.8 M, and 1.0 M) were prepared by accurately measuring the requirement
amount of the salt and dissolving it in deionized water to achieve the required volume. The
conductivity of each solution was taken to be the average of three conductivity readings of each
solution measured using a conductivity meter. The measured conductivities for each solution were
then tabulated for their corresponding concentrations and a calibration curve of conductivity against
concentration was plotted. Similar steps were repeated for aluminium chloride hexahydrate.
3.3 Regeneration
To regenerate the resins in the ion exchange column after each run of, a 5L solution of 10% sodium
chloride solution was prepared by dissolving 500g of NaCl in 5L of deionized water. The initial
conductivity of the sodium chloride solution was measured and recorded using a conductivity meter.
3
The sodium chloride solution is flowed in an upward flow pattern by opening valves V3, V5, and
V9 with the bypass valve V4 partially opened to relieve pressure buildup. The selector tube was
placed inside the tank containing the sodium chloride solution. The pump was switched on to pump
the sodium chloride solution into the column at a flowrate of 50 cm3/min for a minimum of 30
minutes contact time. The conductivity meter reading was observed until it approached its initial
conductivity reading. Finally, valves V4 and V8 are opened to drain all the residual solution from
the column. The regeneration of the resins in the column was completed.
3.4 Rinsing
Before we started each run of the experiment, the column was flushed with deionized water to
remove any residue within the column from previous operations. 5L of deionized water is prepared,
and the initial conductivity of deionized water is measured using the conductivity meter . The
deionized water was then poured into the tank. Similar to in regeneration, the cationic resin was
then rinsed in an upward flow pattern by opening valves V3, V5, and V9. The bypass valve V4 was
partially opened. The selector tube was placed into the tank containing the deionized water. Then,
the pump was started to pump the deionized water into the column at a flow rate of 50cm3/min. The
conductivity meter reading was observed until it approached the conductivity reading of the
deionized water, which can take up to two hours. Valves V4 and V8 were opened to flush out the
deionized water in the column until all the residue in the column was removed. The rinsing of the
column was completed.
3.5 Experiment A: Effect of Ion Valency
A solution of 0.5 M magnesium chloride solution was prepared and poured into the tank. Prior to
the start of the experiment, the initial conductivity of the magnesium chloride solution was
measured and recorded. For this experiment, the solution was pumped into the column in a
downward flow pattern. Therefore, valves V2, V5, and V12 were opened. The pump was then
switched on and pumped the solution into the system at a flow rate of 30 cm3/min. The conductivity
reading was recorded at a 5-second interval as soon as the effluent started to flow out. The
recording continued until the conductivity reading reached a steady state. The breakthrough curve
was obtained by plotting a graph of C/C0 based on the calibration curve earlier for further analysis.
Lastly, the system was regenerated with 10% sodium chloride solution and rinsed with deionized
water. Identical steps were then repeated using a 0.5 M solution of aluminium chloride hexahydrate.
4
3.6 Experiment B: Effect of Concentrations
A solution of 0.5 M aluminium chloride hexahydrate was prepared and poured into the tank. Before
we started the experiment, the initial conductivity of the aluminium chloride solution was measured
and recorded. For this experiment, the solution was pumped into the column in a downward flow
pattern. Therefore, valves V2, V5, and V12 were opened. The pump was then switched on and
pumped the solution into the system at a flow rate of 30 cm3/min. The conductivity reading was
recorded at a 5-second interval as soon as the effluent started to flow out. The recording was
continued until the conductivity reding reached a steady state. The breakthrough curve is obtained
by plotting a graph of C/C0 based on the calibration curve earlier for further analysis. Finally, the
system was regenerated with sodium chloride solution and rinsed with deionized water. The same
steps were then repeated using solutions of aluminium chloride hexahydrate at 1.0M.
3.7 Result Calculation and Analysis
Breakthrough curves of concentration ratio (C/C0) against time were plotted for the two different
solutions . From the plots, the break-point time tb and the saturation time ts are determined. Further
analyses were done to obtain the loading capacity of the column, the selectivity coefficient as well
as the distribution coefficient at various operating conditions. Equations involved are shown below
(Geankoplis et al., 2018) (de Dardel, n.d.) (Ben Sik Ali et al., 2004):
1. Time equivalent up to any point:

𝑡
𝐶
𝑡 =∫ 1− 𝑑𝑡 (2)
0 𝐶0
2. Loading Capacity:
𝑒𝑞𝑢𝑖𝑣𝑎𝑙𝑒𝑛𝑐𝑒 𝑜𝑓 𝐴 𝑖𝑛 𝑟𝑒𝑠𝑖𝑛 𝑝ℎ𝑎𝑠𝑒
𝐿𝑜𝑎𝑑𝑖𝑛𝑔 𝑐𝑎𝑝𝑎𝑐𝑖𝑡𝑦 = (3)
𝑟𝑒𝑠𝑖𝑛 𝑣𝑜𝑙𝑢𝑚𝑒
3. Selectivity Coefficient:
[𝐴𝑛+ 𝑅𝑛 ][𝐵 + ]𝑛
𝐾𝐴𝐵 = 𝑛+ + 𝑛 (4)
[𝐴 ][𝐵 𝑅]
4. Distribution Coefficient:
[𝐴𝑛+ 𝑅𝑛 ]
𝐷𝐴𝐵 = (5)
[𝐴𝑛+ ]
5
4.0 Results
In all parts of experiment, all the results are subjected to a 10% percent of errors. In Figures 4.1.1
and 4.1.2, the conductivity of both magnesium chloride solution and aluminium chloride solution
increase linearly with concentration. It is also noted that the conductivity of aluminium chloride is
always higher than that of magnesium chloride within the concentration range observed.
Based on Figure 4.2, it is seen that aluminium chloride solution gives a shorter breakthrough time
than magnesium chloride does. This indicates that ions of higher valency will gives a faster
breakthrough time than that of lower valency. Also, based on the data shown in Table 4.2, the
selectivity coefficient when aluminium chloride solution is treated is higher than that of magnesium
chloride solution. These will be further discussed in Section 5.2.
In Figure 4.3, it is observed that 1.0M aluminium chloride solution gives a faster breakthrough time
than 0.5M aluminium chloride solution does. Our result suggests that ions at higher concentration
will gives a faster breakthrough time than that at lower concentration. In addition to that, based on
the data tabulated in Table 4.3, the selectivity coefficient is greater at higher concentration, yet the
distribution coefficient is lower at higher concentration. These will be further discussed in Section
5.3.

50
45
y = 38.113x + 2.9097
40
R² = 0.9845
Conductivity [mS/cm]
35
30
25
20
15
10
5
0
0 0.2 0.4 0.6 0.8 1 1.2
Concentration [mol/L]
Figure 4.1.1: Calibration Curve of Magnesium Chloride Solution
6
70
60 y = 53.643x + 3.4175
R² = 0.9819
Conductivity [mS/cm]
50
40
30
20
10
0
0 0.2 0.4 0.6 0.8 1 1.2
Concentration [mol/L]
Figure 4.1.2: Calibration Curve of Aluminium Chloride Solution
Graph of CA/CA0 vs t
1.2
0.8
0.6
CA/CA0
0.4
0.2
0
0 100 200 300 400 500 600 700 800
-0.2
time [s]
MgCl2 AlCl3
Figure 4.2: Breakthrough Curves for Solutions of Divalent and Trivalent Ions
Table 4.2: Loading Capacities, Selectivity Coefficients and Distribution Coefficients at Different
Ion Valences
Parameter MgCl2 AlCl3
Resin volume 1.4792 dm3
Breakthrough time, tb 525 s 403 s
Volume of test solution at tb 0.2625 dm3 0.2015 dm3
7
Saturation time, ts 590 s 455 s
[𝐴𝑛+ 𝑅𝑛 ] 0.0942 M 0.0716 M
[𝑁𝑎 + ] 1.5467 M 1.4292 M
[𝐴𝑛+ ] 0.0275 M 0.0236 M
[𝑁𝑎 + 𝑅] 0.9449 M 1.5202 M
Loading Capacity 0.1884 eq/dm3-resin 0.2149 eq/dm3-resin
Selectivity Coefficient 1.2767 2.5237
4.3 Experiment B: Effect of Concentration
1.2000
1.0000
0.8000
0.6000
CA/CA0
0.4000
0.2000
0.0000
0 100 200 300 400 500 600 700 800
-0.2000
time [s]
0.5 mol/L 1 mol/L
Figure 4.3: Breakthrough Curves for 0.5M and 1.0M Aluminium Chloride Solutions
Table 4.3: Loading Capacities, Selectivity Coefficients and Distribution Coefficients at Different
Concentrations
Parameter 0.5M AlCl3 1.0M AlCl3
Resin volume 1.4792 dm3
Breakthrough time, tb 403 s 220 s
Saturation time, ts 455 s 250 s
8
[𝐴𝑛+ 𝑅𝑛 ] 0.0716 M 0.0794 M
[𝑁𝑎 + ] 1.4292 M 2.8200 M
[𝐴𝑛+ ] 0.0236 M 0.0600 M
[𝑁𝑎 + 𝑅] 1.5202 M 1.4969 M
Loading Capacity 0.2149 eq/dm3-resin 0.2383 eq/dm3-resin
Selectivity Coefficient 2.5237 8.8521
Distribution Coefficient 3.0369 1.3239
4.4 Graphical Illustration of Loading Capacity, Selectivity Coefficient and Distribution

Coefficient at Varied Conditions
Experiment A: Effect of Ion Valency
0.25
loading capacity [eq/dm3-resin]
0.2
0.15
0.1
0.05
0
1.5 2 2.5 3 3.5
valency
Figure 4.4.1: Effect of Ion Valency on Loading Capacity
3
selectivity coefficient
2.5
1.5
1
1.5 2 2.5 3 3.5
valency
Figure 4.4.2: Effect of Ion Valency on Selectivity Coefficient
9
Experiment B: Effect of Concentration
0.3
loading capacity [eq/dm3-resin]

0.25
0.2
0.15
0.1
0.05
0
0.4 0.6 0.8 1 1.2
concentration [M]
Figure 4.4.3: Effect of Test Water Concentration on Loading Capacity
12
10
selectivity coefficient
0
0.4 0.6 0.8 1 1.2
concentration [M]
Figure 4.4.4: Effect of Test Water Concentration on Selectivity Coefficient
4
3.5
distribution coefficient
3
2.5
2
1.5
1
0.5
0
0.4 0.6 0.8 1 1.2
concentration [M]
Figure 4.4.5: Effect of Test Water Concentration on Distribution Coefficient
10
5.0 Discussion
Based on the calibration curves depicted in Figures 4.1.1 and 4.1.2, the conductivity of both
magnesium chloride solution and aluminium chloride solution increases linearly with concentration.
The R2 values for are 0.9845 and 0.9815 for magnesium chloride solution and aluminium chloride
solution respectively. These high R2 values close to unity indicates that the calibration curve should
be accurate enough to be utilized in further analysis.
Also, it is observed that the conductivity of the solution increases with the concentration for both
magnesium chloride solution and aluminium chloride solution. This is indeed true as there are more
ions present in the solution at higher concentrations. More ions present in the solution means that
the solution can conduct electricity better, thereby bringing about a higher conductivity. Also, the
conductivity of aluminium chloride solution is always higher than that of magnesium chloride
solution. This can be attributed to the fact that ions of higher valency should provide higher
conductivity than ions of lower valency.
In Experiment A, in order to study the effect of ion valency on loading capacity as well as
selectivity coefficient, the ion exchanger was used to treat magnesium chloride solution (valency:
+2) and aluminium chloride solution (+3) as these ions displaced the Na+ ions in the cation
exchange resin.
Based on Table 4.2 and Figure 4.4.1 , it is seen that the loading capacity is 0.1884 eq/dm3-resin
and 0.2149 eq/dm3-resin for MgCl2 solution and AlCl3 solution respectively. These loading
capacities are almost similar, around 0.2 eq/dm3-resin. According to (de Dardel, n.d.), the loading
capacity, also known as the operating capacity or useful capacity, is the number of ion exchange
sites where exchange has really happened during the loading, which is basically the actual quantity
of ions loaded in the resin between regeneration. The loading capacity, therefore, should be the
same theoretically. Since our findings suggested that the loading capacity of the resin is about 0.2
eq/dm3-resin under 10% allowed percent of error, our results are valid.
In addition to that, as seen from Table 4.2 and Figure 4.4.2, the selectivity coefficient of the system
increases as the ion valency increases. This means that the system is more selective to Al3+ ions
11
compared to Mg2+ ions. This can be explained by the following: according to the work by (Valiskó
et al., 2007), the trivalent Al3+ ions are attracted onto the surface of resin with the electrostatic
interaction between the Al3+ ions and the resin 1.5x of that between the Mg2+ ions and resin surface.
This stronger electrostatic attraction between the trivalent ions and the resin caused the system to
exhibit higher affinity towards the trivalent Al3+ ions. With a stronger affinity, the rate of ion
exchange between Al3+ from the solution and Na+ on the resin bed becomes higher, the resin is said
to have a higher selectivity towards Al3+ ions. This can also be indicated by the shorter
breakthrough time when AlCl3 solution is used compared to MgCl2 as shown in Figure 4.2.
5.3 Experiment B: Effect of Concentration
In Experiment A, our results proved that the cation exchange resin is more selective towards Al3+
ions. Therefore, we have chosen to vary the concentration of AlCl3 solution to study the effect of
concentration towards loading capacity, selectivity coefficient and most importantly, distribution
coefficient at equilibrium.
From the data shown in Table 4.3 and Figure 4.4.3, the loading capacity is 0.2149 eq/dm3-resin
and 0.2383 eq/dm3-resin for 0.5M AlCl3 solution and 1.0M AlCl3 solution respectively. Again,
these loading capacities are almost similar, around 0.2 eq/dm3-resin. Although the loading capacity
when 1.0M AlCl3+ solution is used slightly deviated even though the result is subjected to 10%
allowed error, nevertheless it is still very close to the value of 0.2 eq/dm 3-resin calculated
previously.
Next, we discuss the effect of test water concentration towards the selectivity coefficient of the
system. As seen from Table 4.3 and Figure 4.4.4, the selectivity coefficient of the system increases
from 2.5237 at 0.5M to 8.8521 at 1.0M. This can be explained by the following: at higher test water
concentration, there is a higher concentration of Al3+ ions. The greater the Al3+ ions concentration,
the less the interference from the Na+ ions embedded onto the resin bed (Horiba Advanced Techno,
Co., Ltd., n.d.).
Lastly, we evaluate the effect of test water concentration on the distribution coefficient of the
system. Based on Table 4.3 and Figure 4.4.5, the distribution coefficient decreases from 3.0369 at
0.5M to 1.3239 at 1.0M. The distribution coefficient can be defined as how much the targeted ions
like the resin phase as compared to the aqueous phase. The study by (Singare et al., 2009) suggested
12
that at sufficiently low concentrations (0.005M – 0.020M), the distribution coefficient of the ions in
the ion exchanger should increase. However, our results disagree with the findings by Singare et al.
This can be attributed to the fact that we run our experiment at a much higher concentration range
(0.5M – 1.0M). At such high concentrations, at equilibrium, after the resins have exhausted, there
would still be a great number of Al3+ ions in the aqueous phase. Therefore, it would seem like the
Al3+ ions prefer the aqueous phase, when in fact the Na+ ions on the resin have all been displaced by
Al3+ ions from the test water.
5.4 Error Analysis
As seen from Figures 4.2 and 4.3, the breakthrough curves do not start at C/C0 = 0 and do not end
at C/C0 = 1 after breakthrough and steady state has been attained. The calculations may not have
been sufficiently accurate since the region of C/C0 < 0 and C/C0 > 1 are omitted. The reason why
these regions present in the breakthrough curves can be attributed to the fact that the calibration
curve may not be accurate due to potential impurities and residues in the standard solutions, and the
fluctuation of the conductivity readings shown by the highly sensitive conductivity meter.
Besides, there was one occurrence in which the test water could not pass into the ion exchange
column while we were doing the experiment. As we were debugging, we noticed that a little test
water had been oozing out the pressure-relief valve V4. This indicates that there might be pressure
buildup at the top part of the column, and the test water could not pass into the cation exchange
column. The fact that a little test water was seen oozing out V4 indicates that there might be some
backward flow of the test water through valve V5, and the test water might have been passed to the
sample port prior to any ion-exchange treatment. As a result, the breakthroughs occur at a small
interval (a minimum of 30s for 1.0M AlCl3 solution to a maximum of 65s for 0.5M MgCl2 solution).
This may have caused inaccuracies in the breakthrough curves obtained, consequently the accuracy
of the results obtained may be jeopardized.
5.5 Recommendations on Further Improvements
In the experiment, our findings suggested that at exceedingly high test water concentration, the
distribution coefficient of Al3+ ions decreases at increasing test water concentration. From Section
5.3, we know that this is because at equilibrium, after the resins have exhausted, there would still be
a great number of Al3+ ions in the aqueous phase. Therefore, it would seem like the Al3+ ions prefer
the aqueous phase; thus, the distribution coefficient of Al3+ ions decreases. This finding contradicts
13
the work of other researchers that suggests at low test water concentration, the distribution
coefficient of the targeted ions should increase with increasing concentration. Therefore, we suggest
that in future experiment involving the ion exchanger used, low test water concentrations should be
used to obtain more accurate results regarding the relationship between the test water concentration
and the distribution coefficient of the system.
Apart from that, as seen from Tables 4.2 and 4.3, the volumes of test water treated are much less
than the total volume of resins. This indicates that few targeted ions had been “exchanged” onto the
resins upon breakthrough, that the resins have low sorption capacity after repeated use. Thus, we
suggest that the resins within the ion exchanger should be replaced with new resins, so that the ion
exchanger can soften more hard water in each use.
6.0 Conclusion
In short, the three objectives for this experiment have been achieved. First, it is obtained that the
loading capacity of the cation exchange column used is 0.2 eq/dm3-resin. Second, it is found that
the system is more selective towards ions of higher valency (Al3+) than that of lower valency (Mg2+).
This is due to the stronger electrostatic interaction between the resin bed and ions of higher valency,
resulting in shorter breakthrough time and saturation time. Third, our results suggest that at high test
water concentration, the distribution coefficient of Al3+ decreases at increasing concentration. This
is because at equilibrium, after the resins have exhausted, there would still be a great number of
Al3+ ions in the aqueous phase. Therefore, it would seem like the Al3+ ions prefer the aqueous phase,
nonetheless all the Na+ ions on the resin have been displaced by Al3+ ions from the test water.
14
7.0 References
Ben Sik Ali, M., Hamrouni, B., Bouguecha, S., & Dhahbi, M. (2004). Silica removal using ion-
exchange resins. Desalination, 167, 273–279. https://doi.org/10.1016/j.desal.2004.06.136
de Dardel, F. (n.d.). Ion exchange capacity. Ion Exchange Capacity. Retrieved 26 May 2023, from
http://dardel.info/IX/capacity.html
Geankoplis, C. J., Hersel, A. A., & Lepek, D. H. (2018). Transport Processes and Separation
Process Principles. USA: Pearson Education.
Horiba Advanced Techno, Co., Ltd. (n.d.). Selectivity coefficient. Retrieved 18 June 2023, from
https://www.horiba.com/int/water-quality/support/electrochemistry/the-basis-of-
ion/selectivity-coefficient/
Kubisch, A., & Korff, C. (2013, October 2). Hard Water. Chemistry LibreTexts.
https://chem.libretexts.org/Bookshelves/Inorganic_Chemistry/Supplemental_Modules_and_
Websites_(Inorganic_Chemistry)/Descriptive_Chemistry/Main_Group_Reactions/Hard_Wa
ter
Lenntech. (n.d.). Resinex K-8 Ion Exchange Resin. https://www.lenntech.com/Data-sheets/Resinex-
K8-L.pdf
Pushnov, A. S. (2006). Calculation of average bed porosity. Chemical and Petroleum Engineering,
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39833933.html
15
Appendices
Appendix A.1: Experimental Setup
1
2
7
8
3 4
5 6
Figure A.1: Experimental Setup
Whereas: -
1: pump
2: flowmeter
3: sump tank
4: water/ chemical tank
5: drain
6: conductivity meter
7: conductivity meter holder
8: cation exchange column
i
Appendix A.2: Raw Data
Table A.2.1: Raw Data for 0.5M Magnesium Chloride at 30cm3/min
Time [s] Conductivity (mS/cm) CA [M] CA/CA0

0 0.3 -0.0685 -0.14
5 0.3001 -0.0685 -0.14
10 0.3008 -0.0685 -0.14
15 0.3009 -0.0684 -0.14
20 0.3009 -0.0684 -0.14
25 0.3011 -0.0684 -0.14
30 0.3012 -0.0684 -0.14
35 0.3013 -0.0684 -0.14
40 0.3014 -0.0684 -0.14
45 0.3015 -0.0684 -0.14
50 0.3016 -0.0684 -0.14
55 0.302 -0.0684 -0.14
60 0.3021 -0.0684 -0.14
65 0.3021 -0.0684 -0.14
70 0.3031 -0.0684 -0.14
75 0.3071 -0.0683 -0.14
80 0.3071 -0.0683 -0.14
85 0.3071 -0.0683 -0.14
90 0.3071 -0.0683 -0.14
95 0.3071 -0.0683 -0.14
100 0.3071 -0.0683 -0.14
105 0.31 -0.0682 -0.14
110 0.31 -0.0682 -0.14
115 0.31 -0.0682 -0.14
120 0.31 -0.0682 -0.14
125 0.31 -0.0682 -0.14
130 0.31 -0.0682 -0.14
135 0.31 -0.0682 -0.14
140 0.31 -0.0682 -0.14
145 0.31 -0.0682 -0.14
150 0.31 -0.0682 -0.14
155 0.31 -0.0682 -0.14
160 0.315 -0.0681 -0.14
165 0.315 -0.0681 -0.14
170 0.315 -0.0681 -0.14
175 0.318 -0.068 -0.14
180 0.318 -0.068 -0.14
185 0.318 -0.068 -0.14
190 0.318 -0.068 -0.14
195 0.318 -0.068 -0.14
200 0.318 -0.068 -0.14
205 0.321 -0.0679 -0.14
210 0.321 -0.0679 -0.14
ii
215 0.321 -0.0679 -0.14

220 0.325 -0.0678 -0.14
225 0.32 -0.0679 -0.14
230 0.321 -0.0679 -0.14
235 0.319 -0.068 -0.14
240 0.319 -0.068 -0.14
245 0.318 -0.068 -0.14
250 0.318 -0.068 -0.14
255 0.318 -0.068 -0.14
260 0.318 -0.068 -0.14
265 0.325 -0.0678 -0.14
270 0.326 -0.0678 -0.14
275 0.326 -0.0678 -0.14
280 0.326 -0.0678 -0.14
285 0.327 -0.0678 -0.14
290 0.328 -0.0677 -0.14
295 0.328 -0.0677 -0.14
300 0.328 -0.0677 -0.14
305 0.33 -0.0677 -0.14
310 0.33 -0.0677 -0.14
315 0.33 -0.0677 -0.14
320 0.33 -0.0677 -0.14
325 0.334 -0.0676 -0.14
330 0.332 -0.0676 -0.14
335 0.334 -0.0676 -0.14
340 0.334 -0.0676 -0.14
345 0.335 -0.0676 -0.14
350 0.335 -0.0676 -0.14
355 0.335 -0.0676 -0.14
360 0.335 -0.0676 -0.14
365 0.335 -0.0676 -0.14
370 0.337 -0.0675 -0.14
375 0.338 -0.0675 -0.13
380 0.335 -0.0676 -0.14
385 0.335 -0.0676 -0.14
390 0.335 -0.0676 -0.14
395 0.335 -0.0676 -0.14
400 0.335 -0.0676 -0.14
405 0.338 -0.0675 -0.13
410 0.337 -0.0675 -0.14
415 0.337 -0.0675 -0.14
420 0.336 -0.0675 -0.14
425 0.338 -0.0675 -0.13
430 0.336 -0.0675 -0.14
435 0.336 -0.0675 -0.14
440 0.335 -0.0676 -0.14
445 0.336 -0.0675 -0.14
450 0.335 -0.0676 -0.14
iii
455 0.331 -0.0677 -0.14

460 0.332 -0.0676 -0.14
465 0.331 -0.0677 -0.14
470 0.3 -0.0685 -0.14
475 0.325 -0.0678 -0.14
480 0.335 -0.0676 -0.14
485 0.502 -0.0632 -0.13
490 0.472 -0.064 -0.13
495 0.461 -0.0642 -0.13
500 0.46 -0.0643 -0.13
505 0.465 -0.0641 -0.13
510 1.501 -0.037 -0.07
515 1.826 -0.0284 -0.06
520 2.315 -0.0156 -0.03
525 3.647 0.0193 0.039
530 5.67 0.0724 0.145
535 7 0.1073 0.215
540 8.15 0.1375 0.275
545 8.76 0.1535 0.307
550 8.95 0.1585 0.317
555 10.31 0.1942 0.388
560 12.55 0.2529 0.506
565 13.67 0.2823 0.565
570 15.67 0.3348 0.67
575 17 0.3697 0.739
580 17.81 0.391 0.782
585 19.07 0.424 0.848
590 21.2 0.4799 0.96
595 20.86 0.471 0.942
600 21.66 0.492 0.984
605 21.05 0.476 0.952
610 21.15 0.4786 0.957
615 21.05 0.476 0.952
620 21.15 0.4786 0.957
625 21.07 0.4765 0.953
630 21.06 0.4762 0.952
635 21.1 0.4773 0.955
640 21 0.4747 0.949
645 21.5 0.4878 0.976
650 21.5 0.4878 0.976
655 21.5 0.4878 0.976
660 22 0.5009 1.002
665 22 0.5009 1.002
670 22.05 0.5022 1.004
675 22.05 0.5022 1.004
680 22.07 0.5027 1.005
685 22.08 0.503 1.006
690 21.5 0.4878 0.976
iv
695 21.3 0.4825 0.965

700 21.7 0.493 0.986
Table A.2.2: Raw Data for 0.5M Aluminium Chloride at 30cm3/min

0 0.192 -0.06 -0.1203
5 0.31 -0.058 -0.1159
10 0.34 -0.057 -0.1147
15 0.345 -0.057 -0.1146
20 0.346 -0.057 -0.1145
25 0.34 -0.057 -0.1147
30 0.393 -0.056 -0.1128
35 0.42 -0.056 -0.1118
40 0.4 -0.056 -0.1125
45 0.4 -0.056 -0.1125
50 0.42 -0.056 -0.1118
55 0.395 -0.056 -0.1127
60 0.42 -0.056 -0.1118
65 0.425 -0.056 -0.1116
70 0.43 -0.056 -0.1114
75 0.434 -0.056 -0.1112
80 0.425 -0.056 -0.1116
85 0.425 -0.056 -0.1116
90 0.436 -0.056 -0.1112
95 0.426 -0.056 -0.1115
100 0.435 -0.056 -0.1112
105 0.426 -0.056 -0.1115
110 0.429 -0.056 -0.1114
115 0.426 -0.056 -0.1115
120 0.426 -0.056 -0.1115
125 0.433 -0.056 -0.1113
130 0.424 -0.056 -0.1116
135 0.335 -0.057 -0.1149
140 0.442 -0.055 -0.1109
145 0.452 -0.055 -0.1106
150 0.446 -0.055 -0.1108
155 0.433 -0.056 -0.1113
160 0.41 -0.056 -0.1121
165 0.437 -0.056 -0.1111
170 0.438 -0.056 -0.1111
175 0.453 -0.055 -0.1105
180 0.46 -0.055 -0.1103
185 0.44 -0.056 -0.111
190 0.4377 -0.056 -0.1111
195 0.438 -0.056 -0.1111
200 0.438 -0.056 -0.1111
205 0.439 -0.056 -0.111
v
210 0.444 -0.055 -0.1109

215 0.436 -0.056 -0.1112
220 0.439 -0.056 -0.111
225 0.444 -0.055 -0.1109
230 0.442 -0.055 -0.1109
235 0.44 -0.056 -0.111
240 0.441 -0.055 -0.111
245 0.451 -0.055 -0.1106
250 0.441 -0.055 -0.111
255 0.442 -0.055 -0.1109
260 0.441 -0.055 -0.111
265 0.442 -0.055 -0.1109
270 0.442 -0.055 -0.1109
275 0.442 -0.055 -0.1109
280 0.442 -0.055 -0.1109
285 0.442 -0.055 -0.1109
290 0.443 -0.055 -0.1109
295 0.444 -0.055 -0.1109
300 0.444 -0.055 -0.1109
305 0.445 -0.055 -0.1108
310 0.444 -0.055 -0.1109
315 0.446 -0.055 -0.1108
320 0.446 -0.055 -0.1108
325 0.447 -0.055 -0.1107
330 0.45 -0.055 -0.1106
335 0.452 -0.055 -0.1106
340 0.453 -0.055 -0.1105
345 0.457 -0.055 -0.1104
350 0.458 -0.055 -0.1103
355 0.471 -0.055 -0.1099
360 0.51 -0.054 -0.1084
365 1.35 -0.039 -0.0771
370 1.4 -0.038 -0.0752
375 1.35 -0.039 -0.0771
380 1.33 -0.039 -0.0778
385 1.325 -0.039 -0.078
390 1.315 -0.039 -0.0784
395 1.4 -0.038 -0.0752
400 3.65 0.004 0.0087
405 6.5 0.057 0.1149
410 12.7 0.173 0.3461
415 12.45 0.168 0.3368
420 13.2 0.182 0.3647
425 14.9 0.214 0.4281
430 16.25 0.239 0.4784
435 24.7 0.397 0.7935
440 25.85 0.418 0.8364
445 25.23 0.407 0.8133
vi
450 25.6 0.414 0.827

455 25.79 0.417 0.8341
460 26.15 0.424 0.8476
465 29.16 0.48 0.9598
470 29.18 0.48 0.9605
475 29.15 0.48 0.9594
480 29.11 0.479 0.9579
485 29.15 0.48 0.9594
490 29.22 0.481 0.962
495 29.23 0.481 0.9624
500 29.22 0.481 0.962
505 29 0.477 0.9538
510 28.95 0.476 0.9519
515 28.8 0.473 0.9464
520 28.7 0.471 0.9426
525 28.9 0.475 0.9501
530 29.01 0.477 0.9542
535 29.03 0.477 0.9549
540 28.75 0.472 0.9445
545 28.75 0.472 0.9445
550 28.51 0.468 0.9355
555 28.51 0.468 0.9355
560 28.58 0.469 0.9382
565 28.59 0.469 0.9385
570 29.7 0.49 0.9799
575 29.89 0.493 0.987
580 29.3 0.482 0.965
585 29.4 0.484 0.9687
590 29.51 0.486 0.9728
595 29.4 0.484 0.9687
600 29.35 0.483 0.9669
605 29.35 0.483 0.9669
610 29.85 0.493 0.9855
615 29.64 0.489 0.9777
620 29.58 0.488 0.9754
625 29.98 0.495 0.9903
630 30.41 0.503 1.0064
635 30.45 0.504 1.0079
640 30.51 0.505 1.0101
645 30.55 0.506 1.0116
650 30.57 0.506 1.0123
655 30.8 0.51 1.0209
660 31 0.514 1.0284
665 31.12 0.516 1.0329
670 30.12 0.498 0.9956
675 30 0.496 0.9911
680 29.47 0.486 0.9713
685 29.48 0.486 0.9717
vii
690 29.48 0.486 0.9717

695 29.45 0.485 0.9706
700 29.42 0.485 0.9695
Table A.2.3: Raw Data for 1.0M Aluminium Chloride at 30cm3/min

0 0.321 -0.0577 -0.0577
5 0.274 -0.0586 -0.0586
10 0.262 -0.0588 -0.0588
15 0.311 -0.0579 -0.0579
20 0.295 -0.0582 -0.0582
25 0.296 -0.0582 -0.0582
30 0.316 -0.0578 -0.0578
35 0.327 -0.0576 -0.0576
40 0.285 -0.0584 -0.0584
45 0.316 -0.0578 -0.0578
50 0.292 -0.0583 -0.0583
55 0.334 -0.0575 -0.0575
60 0.333 -0.0575 -0.0575
65 0.266 -0.0587 -0.0587
70 0.326 -0.0576 -0.0576
75 0.337 -0.0574 -0.0574
80 0.285 -0.0584 -0.0584
85 0.319 -0.0578 -0.0578
90 0.279 -0.0585 -0.0585
95 0.303 -0.0581 -0.0581
100 0.333 -0.0575 -0.0575
105 0.310 -0.0579 -0.0579
110 0.284 -0.0584 -0.0584
115 0.280 -0.0585 -0.0585
120 0.295 -0.0582 -0.0582
125 0.292 -0.0583 -0.0583
130 0.286 -0.0584 -0.0584
135 0.306 -0.0580 -0.0580
140 0.324 -0.0577 -0.0577
145 0.29 -0.0583 -0.0583
150 0.29 -0.0582 -0.0582
155 0.26 -0.0588 -0.0588
160 0.25 -0.0590 -0.0590
165 0.28 -0.0585 -0.0585
170 0.28 -0.0585 -0.0585
175 0.315 -0.0578 -0.0578
180 0.346 -0.0573 -0.0573
185 0.344 -0.0573 -0.0573
190 0.296 -0.0582 -0.0582
195 0.274 -0.0586 -0.0586
200 0.326 -0.0576 -0.0576
viii
205 0.326 -0.0576 -0.0576

210 0.324 -0.0577 -0.0577
215 0.324 -0.0577 -0.0577
220 4.520 0.0206 0.0206
225 14.74 0.2111 0.2111
230 16.84 0.2502 0.2502
235 30.51 0.5051 0.5051
240 48.74 0.8449 0.8449
245 52.67 0.9182 0.9182
250 57.30 1.0045 1.0045
255 56.89 0.9968 0.9968
260 57.77 1.0133 1.0133
265 56.16 0.9832 0.9832
270 57.44 1.0071 1.0071
275 57.42 1.0068 1.0068
280 57.07 1.0002 1.0002
285 56.32 0.9862 0.9862
290 57.14 1.0016 1.0016
295 56.55 0.9905 0.9905
300 56.22 0.9843 0.9843
305 56.38 0.9872 0.9872
310 57.74 1.0127 1.0127
315 56.09 0.9820 0.9820
320 56.43 0.9883 0.9883
325 56.06 0.9813 0.9813
330 56.83 0.9958 0.9958
335 55.98 0.9798 0.9798
340 57.74 1.0128 1.0128
345 56.34 0.9866 0.9866
350 56.14 0.9828 0.9828
355 56.56 0.9908 0.9908
360 56.86 0.9963 0.9963
365 56.15 0.9831 0.9831
370 57.94 1.0164 1.0164
375 56.61 0.9917 0.9917
380 56.54 0.9904 0.9904
385 56.07 0.9816 0.9816
390 56.55 0.9904 0.9904
395 56.04 0.9810 0.9810
400 56.96 0.9981 0.9981
405 57.47 1.0077 1.0077
410 57.21 1.0028 1.0028
415 56.13 0.9827 0.9827
420 56.11 0.9823 0.9823
425 57.50 1.0083 1.0083
430 57.76 1.0130 1.0130
435 57.02 0.9992 0.9992
440 56.17 0.9834 0.9834
ix
445 57.60 1.0101 1.0101

450 56.63 0.9919 0.9919
455 56.54 0.9903 0.9903
460 57.44 1.0071 1.0071
465 55.97 0.9797 0.9797
470 56.05 0.9811 0.9811
475 57.29 1.0042 1.0042
480 57.16 1.0018 1.0018
485 57.00 0.9989 0.9989
490 57.41 1.0065 1.0065
495 57.36 1.0057 1.0057
500 57.51 1.0084 1.0084
505 56.53 0.9900 0.9900
510 57.34 1.0051 1.0051
515 57.06 1.0001 1.0001
520 56.74 0.9941 0.9941
525 56.07 0.9816 0.9816
530 57.51 1.0084 1.0084
535 56.63 0.9919 0.9919
540 57.17 1.0020 1.0020
545 57.43 1.0069 1.0069
550 56.16 0.9832 0.9832
555 56.21 0.9841 0.9841
560 57.05 0.9998 0.9998
565 56.92 0.9974 0.9974
570 57.73 1.0125 1.0125
575 57.55 1.0091 1.0091
580 57.42 1.0067 1.0067
585 56.05 0.9812 0.9812
590 56.10 0.9820 0.9820
595 56.13 0.9826 0.9826
600 57.55 1.0091 1.0091
605 57.84 1.0145 1.0145
610 57.32 1.0048 1.0048
615 56.21 0.9842 0.9842
620 57.40 1.0062 1.0062
625 56.17 0.9834 0.9834
630 56.18 0.9837 0.9837
635 58.23 1.0218 1.0218
640 58.61 1.0289 1.0289
645 57.26 1.0037 1.0037
650 56.45 0.9886 0.9886
655 56.12 0.9825 0.9825
660 56.43 0.9882 0.9882
665 56.42 0.9881 0.9881
670 56.42 0.9881 0.9881
675 56.89 0.9968 0.9968
680 56.68 0.9929 0.9929
x
685 56.12 0.9825 0.9825

690 56.68 0.9930 0.9930
695 56.69 0.9931 0.9931
700 56.32 0.9862 0.9862
Appendix A.3: Sample Calculation
A.3.1: Preparation of Test Waters
To prepare 5L of 0.5M magnesium chloride solution, magnesium chloride hexahydrate salt is used.
First, we determine the number of moles of hydrated salts:
𝑚𝑜𝑙 𝑀𝑔𝐶𝑙2 1 𝑚𝑜𝑙 𝑀𝑔𝐶𝑙2 ⋅ 6𝐻2 𝑂

𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑀𝑔𝐶𝑙2 ⋅ 6𝐻2 𝑂 = 0.5 × 5𝐿 ×
𝐿 1 𝑚𝑜𝑙 𝑀𝑔𝐶𝑙2
𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑀𝑔𝐶𝑙2 ⋅ 6𝐻2 𝑂 = 2.5 𝑚𝑜𝑙 𝑀𝑔𝐶𝑙2 ⋅ 6𝐻2 𝑂
Then, we calculate the mass of hydrated salt required:
203.31𝑔 𝑀𝑔𝐶𝑙2 ⋅ 6𝐻2 𝑂

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑀𝑔𝐶𝑙2 ⋅ 6𝐻2 𝑂 = 2.5 𝑚𝑜𝑙 𝑀𝑔𝐶𝑙2 ⋅ 6𝐻2 𝑂 ×
1 𝑚𝑜𝑙 𝑀𝑔𝐶𝑙2 ⋅ 6𝐻2 𝑂
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑀𝑔𝐶𝑙2 ⋅ 6𝐻2 𝑂 = 508.2750 𝑔 𝑀𝑔𝐶𝑙2 ⋅ 6𝐻2 𝑂
Next, we determine the number of moles of water to be reduced for the solution:
𝑚𝑜𝑙 𝑀𝑔𝐶𝑙2 6 𝑚𝑜𝑙 𝐻2 𝑂

𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝐻2 𝑂 𝑟𝑒𝑑𝑢𝑐𝑒𝑑 = 0.5 × 5𝐿 ×
𝐿 1 𝑚𝑜𝑙 𝑀𝑔𝐶𝑙2
𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝐻2 𝑂 𝑟𝑒𝑑𝑢𝑐𝑒𝑑 = 15 𝑚𝑜𝑙 𝐻2 𝑂
After that, we determine the volume of water to be reduced for the solution:
18.015 𝑔 𝐻2 𝑂 1 𝑚𝐿 𝐻2 𝑂
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐻2 𝑂 𝑟𝑒𝑑𝑢𝑐𝑒𝑑 = 15 𝑚𝑜𝑙 𝐻2 𝑂 × ×
1 𝑚𝑜𝑙 𝐻2 𝑂 1 𝑔 𝐻2 𝑂
xi
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐻2 𝑂 𝑟𝑒𝑑𝑢𝑐𝑒𝑑 = 270 𝑚𝐿 𝐻2 𝑂
Finally, we determine the actual volume of deionized water required for the 5L solution:
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐻2 𝑂 𝑟𝑒𝑞𝑢𝑖𝑟𝑒𝑑 = 5000 𝑚𝐿 − 270 𝑚𝐿 = 4730 𝑚𝐿
The same steps are repeated to obtain the volume of water required for 0.5M aluminium chloride
solution and 1.0M aluminium chloride solution. The relevant parameters are tabulated below.
Table A.3.1: Parameters to Obtain Various 5L Solutions of Varied Concentrations
Parameter 0.5M Magnesium 0.5M Aluminium 1.0M Aluminium

Chloride Solution Chloride Solution Chloride Solution
Moles of Hydrated 2.5 2.5 5

Salt [mol]
Mass of Hydrated 508.2750 603.5750 1207.1500

Salt [g]
Moles of H2O 15 15 30
Reduced [mol]
Volume of H2O 270 270 540

Reduced [mL]
Volume of H2O 4730 4730 4460

Required [mL]
A.3.2: Calculation of Loading Capacity, Selectivity Coefficient and Distribution Coefficient
This sample calculation is based on 0.5M AlCl3 solution at 30 cm3/min. The time equivalent to
achieve steady-state is obtained from the equation below:
𝑡𝑠
𝐶
𝑡 =∫ 1− 𝑑𝑡
0 𝐶0
xii
The equation above can be rearranged:
𝑡𝑠 𝑡𝑠
𝐶
𝑡𝑡 = ∫ 1𝑑𝑡 − ∫ 𝑑𝑡
0 0 𝐶0
Whereas ts is the time when the time taken until C/C0 just reaches steady state.
1.2
0.8
0.6
CA/CA0
0.4
0.2
0
0 100 200 300 400 500 600 700 800
-0.2
time [s]
AlCl3
Figure A.3.1: Breakthrough Curve of 0.5M AlCl3 Solution
The region below 𝐶/𝐶0 = 0 is ignored in the calculation. From Figure A.3.1 above, we can see that
ts is approximately 445s while tb is about 403s. The time equivalents are:
𝑡
𝐶
𝑡 =∫ 1− 𝑑𝑡
0 𝐶0
𝑡𝑏 = 403 𝑠
𝑡𝑠 = 445 𝑠
At ts = 445s, the total volume of test water is:
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑒𝑠𝑡 𝑤𝑎𝑡𝑒𝑟 (𝑡𝑠 ) = 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 × 𝑡𝑠
𝑐𝑚3 1 𝑑𝑚3 1𝑚𝑖𝑛

𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑒𝑠𝑡 𝑤𝑎𝑡𝑒𝑟 (𝑡𝑠 ) = 30 × 3
× 445𝑠 ×
𝑚𝑖𝑛 1000𝑐𝑚 60𝑠
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑒𝑠𝑡 𝑤𝑎𝑡𝑒𝑟 (𝑡𝑠 ) = 0.2225𝑑𝑚3
xiii
The total number of moles of A up till this point is:
𝑚𝑜𝑙 𝐴𝑡𝑜𝑡 = 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑒𝑠𝑡 𝑤𝑎𝑡𝑒𝑟 (𝑡𝑠 ) × 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛
𝑚𝑜𝑙
𝑚𝑜𝑙 𝐴𝑡𝑜𝑡 = 0.5 × 0.2225𝑑𝑚3 = 0.1113𝑚𝑜𝑙
𝑑𝑚3
Before breakthrough, all Al3+ ions are adsorbed onto the resin. At tb=403 s, the volume of test water
until breakthrough is:
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑒𝑠𝑡 𝑤𝑎𝑡𝑒𝑟 (𝑡𝑏 ) = 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 × 𝑡𝑏
𝑐𝑚3 1 𝑑𝑚3 1𝑚𝑖𝑛

𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑒𝑠𝑡 𝑤𝑎𝑡𝑒𝑟(𝑡𝑏 ) = 30 × 3
× 400𝑠 ×
𝑚𝑖𝑛 1000𝑐𝑚 60𝑠
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑒𝑠𝑡 𝑤𝑎𝑡𝑒𝑟(𝑡𝑏 ) = 0.2015𝑑𝑚3
Till breakthrough, the number of moles of Al3+ adsorbed is:
𝑚𝑜𝑙 𝐴𝑎𝑑,𝑡𝑏 = 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑒𝑠𝑡 𝑤𝑎𝑡𝑒𝑟 (𝑡𝑏 ) × 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛
𝑚𝑜𝑙
𝑚𝑜𝑙 𝐴𝑎𝑑,𝑡𝑏 = 0.5 × 0.2015𝑑𝑚3 = 0.11125 𝑚𝑜𝑙
𝑑𝑚3
From the region of 𝐶/𝐶0 = 0 until tb = 403s and 𝐶/𝐶0 ≈ 1 at ts = 445s, some of the targeted ions
are still adsorbed onto the resin bed while the others remain in aqueous phase. The area under the
breakthrough curve is the number of moles of Al3+ not adsorbed but remain in the aqueous phase, as
approximated by the orange region in Figure A.3.1 above. On the other hand, the number of moles
of Al3+ adsorbed is represented by the blue colored region in Figure A.3.1 above. Both these two
regions can be approximated by the area of a triangle:
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑒𝑠𝑡 𝑤𝑎𝑡𝑒𝑟 (𝑡𝑏 − 𝑡𝑠 ) = (𝑡𝑏 − 𝑡𝑠 ) × 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒
𝑐𝑚3 1𝑑𝑚3
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑒𝑠𝑡 𝑤𝑎𝑡𝑒𝑟 (𝑡𝑏 − 𝑡𝑠 ) = (445 − 403) × 30 ×
𝑚𝑖𝑛 1000𝑐𝑚3
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑒𝑠𝑡 𝑤𝑎𝑡𝑒𝑟 (𝑡𝑏 − 𝑡𝑠 ) = 0.0210 𝑑𝑚3
𝑚𝑜𝑙 𝐴 (𝑡𝑏 − 𝑡𝑠 ) = 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑒𝑠𝑡 𝑤𝑎𝑡𝑒𝑟 (𝑡𝑏 − 𝑡𝑠 ) × 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛
xiv
𝑚𝑜𝑙
𝑚𝑜𝑙 𝐴 (𝑡𝑏 − 𝑡𝑠 ) = 0.0210 𝑑𝑚3 × 0.5 = 0.0105 𝑚𝑜𝑙
𝑑𝑚3
𝑚𝑜𝑙 𝐴𝑎𝑑 (𝑡𝑏 − 𝑡𝑠 ) = 0.5 × 1 × 0.0105 = 0.00525 𝑚𝑜𝑙
𝑚𝑜𝑙 𝐴𝑎𝑞 ≈ 𝑚𝑜𝑙 𝐴𝑎𝑑 (𝑡𝑏 − 𝑡𝑠 ) = 0.00525 𝑚𝑜𝑙
The total moles of Al3+ adsorbed in the column is given by:
𝑚𝑜𝑙 𝐴𝑎𝑑,𝑡𝑜𝑡𝑎𝑙 = 𝑚𝑜𝑙 𝐴𝑎𝑑,𝑡𝑏 + 𝑚𝑜𝑙 𝐴𝑎𝑑 (𝑡𝑏 − 𝑡𝑠 )
𝑚𝑜𝑙 𝐴𝑎𝑑,𝑡𝑜𝑡𝑎𝑙 = 0.11125 + 0.00525 = 0.1060 𝑚𝑜𝑙
The loading capacity is given by:

𝑙𝑜𝑎𝑑𝑖𝑛𝑔 𝑐𝑎𝑝𝑎𝑐𝑖𝑡𝑦 =
We first estimate the volume of resin as shown in the following (Pushnov, 2006) (Lenntech, n.d.):
𝜌𝑏
𝑟𝑒𝑠𝑖𝑛 𝑣𝑜𝑙𝑢𝑚𝑒 = (1 − 𝑓)𝑉𝑐𝑜𝑙𝑢𝑚𝑛 = (1 − (1 − )) 𝑉𝑐𝑜𝑙𝑢𝑚𝑛
𝜌𝑝
820 1000𝑑𝑚3
𝑟𝑒𝑠𝑖𝑛 𝑣𝑜𝑙𝑢𝑚𝑒 = (1 − (1 − )) × 𝜋(0.035𝑚)2 (0.6𝑚) ×
1280 1𝑚3
𝑟𝑒𝑠𝑖𝑛 𝑣𝑜𝑙𝑢𝑚𝑒 = 1.4792 𝑑𝑚3
Thus, the loading capacity is:

𝑙𝑜𝑎𝑑𝑖𝑛𝑔 𝑐𝑎𝑝𝑎𝑐𝑖𝑡𝑦 =
xv
𝑒𝑞
0.1060 𝑚𝑜𝑙 × 3
𝑙𝑜𝑎𝑑𝑖𝑛𝑔 𝑐𝑎𝑝𝑎𝑐𝑖𝑡𝑦 = 𝑚𝑜𝑙
1.4792 𝑑𝑚3
𝑒𝑞
𝑙𝑜𝑎𝑑𝑖𝑛𝑔 𝑐𝑎𝑝𝑎𝑐𝑖𝑡𝑦 = 0.2150
𝑑𝑚3
Consider the ion-exchange reaction below:
𝐴𝑛+ + 𝑛𝐵 + 𝑅 ↔ 𝐴𝑛+ 𝑅𝑛 + 𝑛𝐵 +
Then, to calculate the selectivity coefficient and distribution coefficient, we use:
[𝐴𝑛+ 𝑅𝑛 ][𝐵 + ]𝑛
𝐾𝐴𝐵 = 𝑛+ + 𝑛
[𝐴 ][𝐵 𝑅]
[𝐴𝑛+ 𝑅𝑛 ]
𝐷𝐴𝐵 =
[𝐴𝑛+ ]
To calculate the number of moles of B (in this case Na+) in resin phase, we first determine the initial
number of moles of B in 5L of solution used in the regeneration process:
1 𝑚𝑜𝑙 𝑁𝑎𝐶𝑙
𝑚𝑜𝑙 𝐵 𝑖𝑛 𝑟𝑒𝑔𝑒𝑛𝑒𝑟𝑎𝑡𝑖𝑜𝑛 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 = 500 𝑔 𝑁𝑎𝐶𝑙 × = 8.5558 𝑚𝑜𝑙 𝑁𝑎𝐶𝑙
58.44 𝑔 𝑁𝑎𝐶𝑙
The concentration of the 10% NaCl solution used in the regeneration of resin is given by:
8.5558 𝑚𝑜𝑙 𝑁𝑎𝐶𝑙 𝑚𝑜𝑙

𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑁𝑎𝐶𝑙 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 = 3
= 1.7112
5𝑑𝑚 𝑑𝑚3
Since the regeneration is done at 50 cm3/min for 30 minutes , therefore, the volume of NaCl
solution used to regenerate the column is:
𝑐𝑚3 1𝑑𝑚3
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑁𝑎𝐶𝑙 𝑢𝑠𝑒𝑑 = 50 × 30 𝑚𝑖𝑛𝑠 × = 1.5 𝑑𝑚3
𝑚𝑖𝑛 1000𝑐𝑚3
Now, we assume that for the 30 minutes, all the Na+ ions are regenerated onto the resins. Therefore,
the initial number of moles of Na+ in the resin phase can be obtained:
𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑚𝑜𝑙 𝐵𝑅 = 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑁𝑎𝐶𝑙 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 × 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑁𝑎𝐶𝑙 𝑢𝑠𝑒𝑑
xvi
𝑚𝑜𝑙
𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑚𝑜𝑙 𝐵𝑅 = 1.7112 × 1.5 𝑑𝑚3 = 2.5667 𝑚𝑜𝑙 𝐵
𝑑𝑚3
Then, we obtain the number of moles of B in aqueous phase at steady state via stoichiometry:
3 𝑚𝑜𝑙 𝐵 +
𝑚𝑜𝑙 𝐵𝑎𝑞 = 𝑚𝑜𝑙 𝐴𝑎𝑑,𝑡𝑜𝑡𝑎𝑙 ×
1 𝑚𝑜𝑙 𝐴3+
3 𝑚𝑜𝑙 𝐵 +
𝑚𝑜𝑙 𝐵𝑎𝑞 = 0.1060 𝑚𝑜𝑙 × = 0.3180 𝑚𝑜𝑙 𝐵
1 𝑚𝑜𝑙 𝐴3+
After that, we get each concentration term in the equations as followed:
𝑖𝑛𝑖𝑡𝑖𝑎𝑙 𝑚𝑜𝑙 𝐵𝑅 − 𝑚𝑜𝑙 𝐵𝑎𝑞

[𝐵 + 𝑅] =
2.5667 − 0.3180 𝑚𝑜𝑙

[𝐵 + 𝑅] = = 1.5202
1.4792 𝑑𝑚3
𝑚𝑜𝑙 𝐵𝑎𝑞
[𝐵 + ] =
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑒𝑠𝑡 𝑤𝑎𝑡𝑒𝑟 𝑎𝑡 𝑡𝑠
0.3180 𝑚𝑜𝑙
[𝐵 + ] = = 1.4292
0.2225 𝑑𝑚3
𝑚𝑜𝑙 𝐴𝑎𝑑,𝑡𝑜𝑡𝑎𝑙
[𝐴𝑛+ 𝑅𝑛 ] =
0.1060 𝑚𝑜𝑙
[𝐴𝑛+ 𝑅𝑛 ] = = 0.0717
1.4792 𝑑𝑚3
𝑚𝑜𝑙 𝐴𝑎𝑞
[𝐴𝑛+ ] =
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡𝑒𝑠𝑡 𝑤𝑎𝑡𝑒𝑟 𝑎𝑡 𝑡𝑠
0.00525 𝑚𝑜𝑙
[𝐴𝑛+ ] = = 0.0236
0.2225 𝑑𝑚3
xvii
Therefore, the selectivity coefficient and the distribution coefficient are found out to be:
(0.0717)(1.42923 )
𝐾𝐴𝐵 = = 2.5237
(0.0236)(1.52023 )
0.0717
𝐷𝐴𝐵 = = 3.0369
0.0236
All the previous steps are sone first for 0.5M magnesium chloride solution, then repeated for 0.5M
aluminium chloride solution, and lastly 1.0M aluminium chloride solution.
xviii

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EKC 396 Open-ended Laboratory.

Semester II, Session 2022/2023)

UNIVERSITI SAINS MALAYSIA

SEMESTER 2, ACADEMIC SESSION 2022/2023

EKC396: CHEMICAL ENGINEERING LABORATORY III

UO07: ION EXCHANGER

LOH LI YAN 152840

LECTURER : PROFESSOR DR. LIM JIT KANG

𝒛𝑩 𝑨𝒁𝑨 + 𝒁𝑨 𝑩¯𝒁𝑩 ↔ 𝒛𝑨 𝑩𝒁𝑩 + 𝒛𝑩 𝑨¯𝒁𝑨

Figure 1.1: Illustration of Ion Exchange (Kubisch & Korff, 2013)

3.2 Calibration Curve

3.5 Experiment A: Effect of Ion Valency

3.6 Experiment B: Effect of Concentrations

3.7 Result Calculation and Analysis

1. Time equivalent up to any point:

4.1 Calibration Curve

Figure 4.1.1: Calibration Curve of Magnesium Chloride Solution

Figure 4.1.2: Calibration Curve of Aluminium Chloride Solution

4.2 Experiment A: Effect of Ion Valency

Parameter MgCl2 AlCl3

Resin volume 1.4792 dm3

Breakthrough time, tb 525 s 403 s

Volume of test solution at tb 0.2625 dm3 0.2015 dm3

Saturation time, ts 590 s 455 s

Volume of test solution at tb 0.295 dm3 0.2225 dm3

[𝐴𝑛+ 𝑅𝑛 ] 0.0942 M 0.0716 M

[𝑁𝑎 + ] 1.5467 M 1.4292 M

[𝐴𝑛+ ] 0.0275 M 0.0236 M

[𝑁𝑎 + 𝑅] 0.9449 M 1.5202 M

Loading Capacity 0.1884 eq/dm3-resin 0.2149 eq/dm3-resin

Selectivity Coefficient 1.2767 2.5237

4.3 Experiment B: Effect of Concentration

0.5 mol/L 1 mol/L

Parameter 0.5M AlCl3 1.0M AlCl3

Resin volume 1.4792 dm3

Breakthrough time, tb 403 s 220 s

Volume of test solution at tb 0.2015 dm3 0.1100 dm3

Saturation time, ts 455 s 250 s

Volume of test solution at tb 0.2225 dm3 0.125 dm3

[𝐴𝑛+ 𝑅𝑛 ] 0.0716 M 0.0794 M

[𝑁𝑎 + ] 1.4292 M 2.8200 M

[𝐴𝑛+ ] 0.0236 M 0.0600 M

[𝑁𝑎 + 𝑅] 1.5202 M 1.4969 M

Loading Capacity 0.2149 eq/dm3-resin 0.2383 eq/dm3-resin

Selectivity Coefficient 2.5237 8.8521

Distribution Coefficient 3.0369 1.3239

4.4 Graphical Illustration of Loading Capacity, Selectivity Coefficient and Distribution

Experiment A: Effect of Ion Valency

Figure 4.4.2: Effect of Ion Valency on Selectivity Coefficient

Experiment B: Effect of Concentration

loading capacity [eq/dm3-resin]

Figure 4.4.3: Effect of Test Water Concentration on Loading Capacity

Figure 4.4.4: Effect of Test Water Concentration on Selectivity Coefficient

Figure 4.4.5: Effect of Test Water Concentration on Distribution Coefficient

5.2 Experiment A: Effect of Ion Valency

5.3 Experiment B: Effect of Concentration

5.4 Error Analysis

5.5 Recommendations on Further Improvements

Figure A.1: Experimental Setup

Appendix A.2: Raw Data

Table A.2.1: Raw Data for 0.5M Magnesium Chloride at 30cm3/min

Time [s] Conductivity (mS/cm) CA [M] CA/CA0

215 0.321 -0.0679 -0.14