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RUN I RUN II
Ion exchange is a reversible chemical reaction where an ion (an atom or molecule
that has lost or gained an electron and thus acquired an electrical charge) from solution is
exchanged with a similarly charged ion attached to an immobile solid particle. These solid
ion exchange particles are either naturally occurring inorganic zeolites or synthetically
produced organic resins.
Ion exchange often uses resin to change this ion charge. It is known as ion
exchange resin. Ion exchange resin is a polymerized hydrocarbon compound which is in
the form of small beads, insoluble in water or other organic solvent, and usually has white
or yellowish colour. It contains cross-linking bond, and functional groups which make it
enables to ions on the water exchange with ion exchange resins’ charge. In industry, ion
exchange resins are widely used in separation, purification, deionization, and
demineralization processes.
Ion exchange resin has several characteristics, such as:
• Selectivity
Selectivity showed activity on certain ion. The main factor of selectivity is ion
charge and radius. Selectivity will determine the separation capability of an ion in
solution which same ion charge.
• Porosity
Describe varies pores size of capillary canal in resin. These pores are the area of
water absorbed. Porosity can influence ion capacity and selectivity.
• Resin stability
Physical and chemical stability involve resistance and strength friction, resistance
of osmotic effect in service and regeneration.
• Crosslinking degree
This degree describes quantitative size of total crosslinking inside polymer.
Crosslinking degree has range from 4% to 16% and influences solubility, exchange
capacity, selectivity, chemical resistance and oxidation.
Based on its functional groups, ion exchange resin can be distinguished into:
a. Cation Exchange Resin
Cation exchange resin is a high molecular weight, cross-linked polymer containing
sulfonic, phenolic, carboxylic, etc, groups as an integral part of the resin and an
equivalent number of cations. This kind of resins can exchange all kinds of cation
in a solution, therefore, it has low selectivity.
b. Anion Exchange Resin
Anion exchange resin is a polymer containing amine groups an integral parts of
polymer lattice and an equivalent number of anions, such as chloride, hydroxyl, or
sulphate ions.
Resins can be classified as strong or weak acid cation exchanger and strong or
weak base anion exchangers. The kinds and different for each the type of resin, such as:
Strong acid cation Weak acid cation Strong base anion Weak base anion
resin resin resin resin
Groups of Sulfonate carboxylat Ammonium R-NH2-
function quartener
(R-SO3H) (-COOH) (R-R3N+:OH-)
START-UP
First of all, wet cotton placed at the bottom of column to prevent resin going out
from the column. Then, the column is filled with resin KOH exchange resin. There are two
variations of resin height: 7 cm and 10 cm. The resins must always be immersed in water
or a solution. When it becomes dry, the resin would not swell. It makes the pores shrink,
and causes ion exchange performance is not effective.
Then, the tank is filled with 3 liters of demineralized water which is streamed into
the column. Then, the flow rate of the solution which passes the resins is controlled on
constant flow rate. This experiment is done with flow rate 25 BV. For the 7 cm resin
height, it equals to 20.62 mL/minute, whereas for the 7 cm resin height, it equals to 29.45
mL/minute. BV is bed volume which includes particles volume, pores volume, and volume
form bulk density. The purpose of constant flow rate is to make sure that resin contact time
solution is constant during the process.
The high of the water above resin has to be constant because it will effect the
pressure which affect the flow rate and ion exchange condition.
SERVICE
Service is the main process in ion exchange. In this process, the ions in the solution
will be exchanged with the ions in the resin. In this experiment, ion exchange occurs
between Mg2+ ions and Ca2+ ions (from hard water) with Na+ ions (from resin). The
reaction is :
Mg2+ + R-Na Na+ + R-Mg
Ca2+ + R-Na Na+ + R-Ca
Initially. Practicants prepared 3 L hard water 4000 ppm consist of 1000 ppm
MgSO4 and 3000 ppm CaSO4. Then the demineralized water in the storage tank used
before replaced by hard water. Then the hard water was streamed from the hole in the
bottom of the tank through the hose to the hole upside the ion exchange column. The flow
rate used is the one which was determined before. The process of ion exchange occurred
when the solution passed the ion exchange resin. The first 50 mL of outcome water was
disposed because it still contained the demineralized water from start-up process before.
After that, every 25 mL outcome water was collected and 10 mL from this water was taken
to be titrated with EDTA. In this experiment, practicants did duplo for the titration.
The titration is used to determine the concentration of the outcome water. The
titrate that used in this experiment is EDTA solution with 0.15 M concentration. 10 mL
sample (outcome water) was placed in the erlenmeyer and then added with 14 drops of
NH4Cl and half spatula of EBT than it was titrated with EDTA. EDTA was chosen as the
titrate because EDTA has some superiority; EDTA always react with metal logams with
ratio 1: 1, the reaction runs perfectly, and EDTA can react with some metals fast. The
equilibrium of EDTA solution is:
H4Y ↔ H3Y- ↔ H2Y2- ↔ HY3- ↔ Y4-
Every single form of this EDTA produces or needs the ion H+ so that the pH of solution
contains of each form of EDTA will be different. NH4Cl was added in purpose to maintain
the pH balance in the solution so that the optimal condition of titration (pH 8 – 12) could
be reached. In this titration the optimal pH is 10, because in pH 10, the EDTA is in the Y4-
which is used in the reaction happened in titration between the sample solution and EDTA.
The reaction equilibrium is :
MIn- (violet) + H+ + Y4- ↔ HIn2- (blue) + MY2-
While Y describes as EDTA, and MY2- describes complex metal-EDTA.
4-
Ce/Co 2
BACKWASH
The purpose backwashing is remove solid and gas which is caused by hard water
that passed through resin (ion exchange process), separate crumpled resin, organized resin,
and also turned back distribution flow pass through the column. In backwash, the bottom
hole in the column is connected with under of the column carbon and the top of column
carbon is connected to valve with connector of hose. When the valve was opened, the
water will flow from the valve to the carbon column (from top to the bottom).
The outlet water from carbon column is free of Ca(ClO)2 (calcium hypochlorite).
Calcium hypochlorite will damage the resins, therefore it must have been removed before
the tap water flow into this column. The outlet water from carbon column will flow to the
bottom of resin column and fluidize the resin. During fluidization, the wet cotton at the
bottom of resin column must be suppressed so as not fluidized simultaneously. If the wet
cotton was fluidized together with the resin, after the fluidization is ended, the wet cotton
may be above the resin bed, and the resins can pass the column.
During fluidization (approximately 5 minutes), the resin will be is fluidized, the
height of the fluidized resin must be measured. Then, stop the water and wait 5 minutes
until the resin precipitated, height of resin is measured. From experiment data, is got:
RUN 1 RUN 2
h before fluidization 7 cm 10 cm
h when fluidization 9 cm 14 cm
h after fluidization 7,5 cm 10,5 cm
% fluidization 28,57%% 40 %
% expansion 7,1429% 5%
From this data, can be seen if the height of the fluidized resin in run 1 is lower than
run 2 because the water flow rate in run 2 was bigger than in run 1. But as the resin in run
2 is more saturated than in run 1, the % expansion is smaller than run 1.
After resin precipitation, there will be three phenomenons can be occurred:
a. Bubbling
Bubbling is occurred because flow rate of the fluid is bigger than minimum
velocity. The particle and bubble will merge and build an empty space.
b. Slugging
The bubbles which have the same size with the column diameter will merge and
slugging occurs. Slugging will divide the resins bed into some layer and there is an
empty space between the layers.
c. Channeling
Channeling is caused by aggregation effect of cohesion force between the particles.
From the experiment, bubbling and slugging was occurred in both run 1 and run 2.
REGENERATION
Regeneration is the process done to restore the resin capability after the resin
saturated from used in the service process. The regeneration only can restore the resin
capability near 100% but not exactly 100%. This process must be done so that resin can be
use for service process again.
The regeneran requirements are:
• Regeneran must have the ions that can be exchange to the saturated resin.
• The reaction between regeneran and resin must be reversible, the regeneration
reaction from regeneran must be the opposite of the service reaction.
• Regeneran must be easy to made or found and is not expensive.
The regeneration procedure is similar to the service procedure, it is only the
solution streamed that is different. In regeneration, the solution streamed is the regeneran,
in this experiment used NaCl as the regeneran. The reaction equilibrium occurred in the
regeneration process:
R-Mg2+ + 2NaCl 2R-Na+ + MgCl2
R-Ca2+ + 2NaCl 2R-Na+ + CaCl2
In this experiment, NaCl used had 9000 ppm concentration. While the first 50 mL
outcome water was disposed, the 25 mL after was collected and taken 10 mL to be titrated
using EDTA. From the titration, the concentration of outcome water could be calculated
and the breakthrough curve could be made. The ideal breakthrough curve is shown in the
picture below:
2 Ce/Co
V
Area 1 : The resin is still saturated from the service process before. Its capability to
exchange the ions is still low.
Area 2 : The resin capability begin to be restored as the ions of the resin restored from the
regeneran used.
Area 3 : The resin is in nearly its initial condition, which means the regeneration
completed.
Regeneration efficiency shows how near the regeneran can restore the resin to its
initial condition. The higher regeneration efficiency the closer resin to its initial condition.
From this experiment, the regeneration efficiency got:
% efficiency regeneration RUN I RUN II
Calculation method 6.0585 % 10.8188 %
Graphical method 3,888.10-5 % 0.44203 %
This result shows that the regeneration can not restore resin to its 100% initial
condition. The result from run I is lower than the result of run II, it is because the resin in
run II had higher column height so that the ions that can be exchanged is more than in run
II which column height is lower.
RINSING
Rinsing process uses demin water for cleaning. The purpose of rinsing is remove
the residue of ions trapped in resins also to remove the residue of regenerant (NaCl). There
are 2 method of rinsing:
• Fast rinsing : to wash ions residue
• Slow rinsing : to push ion residue out from resin and throw away the cleaning
residue
First, 3L demin water pour into in the storage tank and initial pH is measured. pH
meter display the initial pH of demin water is 6,7. Afterwards, every 25 mL of outlet water
from ion exchange column is collected, and the pH of each sample is measured until three
times constant. When the pH has been constant, the pH value of non-polluter demin water
in this experiment is 4,98, it will not reach the initial pH value as the regeneration will not
restore all ion exchange capacity. This shows that residues inside the resin are decreased.
CHAPTER IV
CONCLUSION
1. http://en.wikipedia.org/wiki/Ion_chromatography
2. http://jurnal.sttn.batan.ac.id/wp-content/uploads/2008/06/8-dyah-hal-95-104.pdf
3. http://nciz.org.nz/ChemPrcesses/water/13D.pdf
4. http://www.freshwatersystems.com
5. http://www.remco.com/ix.htm
6. http://www.skataspe.com/gs_bedvolume.asp
7. Lawrence F. Drbal, Patricia G. Boston, Kayla L. Westra, Black & Veatch, Power
plant engineering, Springer, 1996
8. Skoog, Douglas.A, et.al, Analytical Chemistry An Introduction
9. Vogel, Textbook of Quantitative Chemical Analysis, 5th edition
APPENDIX A
PHYSICAL AND LITERATURE DATA
Flow rate = 25 BV
Diameter of column = 3 cm
Height of resin Run I = 7.5 cm
Run II = 10 cm
[EDTA] = 0. 1316 M
Mr EDTA = 372.24 g/mol
[MgSO4.7H2O] = 0.1 M
Mr MgSO4.7H2O = 246 g/mol
RUN I
3. SERVICE
• Making hard water
[hard water] = 4000 ppm; MgSO4 : CaSO4 = 1 : 3
V hard water = 3 L
m hard water = 4000 mgL ×3 L=12000 mg=12 g
m MgSO4 = 14 ×12 g=3 g
m CaSO4 = 34 ×12 g=9 g
Mr hard water = 0.25 x 120+0.75 x 136 (0.25+0.75=132 g/mol
• Breakthrough curve
[EDTA] . V EDTA = [hard water] . V hard water
0,1316 M. 0,4 mL = [hard water] . 10 mL
[hard water] = 0,005264 M x 132 gmol × 1000 mgg = 694,848ppm
Ce/Co = 694,848/4000 = 0,173712
• Total operation capacity determination
Operation volume = 525 mL
Resin volume = 49,49 mL
Co = 4000 ppm = 4 g/L
Σ Ce/Co.Vs = 0,0640563 L
Total operation capacity = Co .VopV resin – Co . CeCo.VsV resin
= 4 gL . 0,525 L49,48.10-3 L – 4 gL . 0,0640563
L49,48 . 10-3 L = 37,263 g/L
• Total operation capacity determination (with 5% leakage) can not be determined as the
leakage of the resin is higher than 5%.
• Total operation capacity determination (with 10% leakage)
V op = 0,125 L
Co = 4000 ppm
Ce/Co.Vs = 0,00173712
Operation capacity = Co .VopV resin – Co . CeCo.VsV resin
= 4 gL . 0,525 L49,48.10-3 L – 4 gL . 0,00173712
L49,48 . 10-3 L = 42,3 g/L
4. BACKWASH
% fluidisasi = h during fluidization- h before backwash h before backwash x
100% = 9 cm-7 cm7 cm ×100%= 28,57%
% ekspansi = h after backwash -h before backwashh before backwash x 100% =
7,5 cm-7 cm7 cm ×100%= 7,1429%
5. REGENERATION
• [NaCl] initial = Co = 9000 ppm
V NaCl = 9000 mg/L x 3 L = 27 gram
• Breakthrough curve
1 mol Na+ ~ 1 mol EDTA
[NaCl] = 0,1316 M ×1,25 mL10 mL=0,01645 M
= 0,01645 molL ×58,5 gmol ×1000 mgg = 962,325 ppm
Ce/Co = 962,3259000 = 0,106925
• Regeneration capacity
Calculation methods
Σ Ca2+ dan Mg2+ out = Vs . Ca2+dan Mg2+Mr air sadah x valensi
= 0,0041454 mg x 1 g1000 mg132 g/mol x 2 =
3,1406.10-8 eq
Graphic method
Area under curve = 31,81 mL
M ion out from regeneration = L . Co = 31,81.10-3 L . 4 gL . 158,5 g/mol = 2,175.10-3
mol
M ion passes resin = Co . Vop = 4 gL x 0,525 L . 158,5 g/mol = 0,0359 mol
Regeneration efficiency = M ion out from regeneration M ion passes resin x
100%
= 2,175.10-30,0359 x 100% = 6,0585%