CE300E Ion Exc

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Experiment Instructions

CE 300 Ion Exchange


Demonstration Unit
DTP_12
09/2006

CE 300 ION EXCHANGE DEMONSTRATION UNIT


All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 02/2005

Experiment Instructions

Please read and follow the safety regulations before the first installation!

Publication-no.: 918.000 00 D 300 12 (A) DTP_12

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CE 300 ION EXCHANGE DEMONSTRATION UNIT

Table of contents
1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

2 Description of the unit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3

2.1 Unit layout . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3


2.2 Setting up . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2.2.1 Filling the exchanger pipes . . . . . . . . . . . . . . . . . . . . . . . . . . 6
2.3 Shutdown . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

3 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

3.1 Health hazards . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9


3.2 Hazards to unit and function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9

4 Principles of ion exchange . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

4.1 Physical and chemical principles. . . . . . . . . . . . . . . . . . . . . . . . . . . 11


4.2 Take up capacity of ion exchangers . . . . . . . . . . . . . . . . . . . . . . . . 15
4.3 Regeneration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
4.4 Applications of ion exchangers . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
4.4.1 Water softening. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
4.4.2 Dealkalisation of water . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
4.4.3 Total demineralisation of water . . . . . . . . . . . . . . . . . . . . . . 21

5 Experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23

5.1 Exchanging cations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23


5.2 Exchanging anions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
5.3 Series connection of cation and anion exchangers . . . . . . . . . . . . . 28
5.4 Regeneration. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 30
5.5 Notes on further experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34

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6 Appendix . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

6.1 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37


6.2 Tables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 02/2005

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1 Introduction

The CE 300 “Ion exchange demonstration unit"


facilitates experiments relating to water softening
and demineralisation of water.

The experiments are performed with regenerative


ion exchanger resins. It is equipped with both cat-
ion and anion exchangers in strong and weak ba-
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 02/2005

sic or acidic versions.

The range of experiments covers:


– Water softening and water demineralisation
using ion exchange
– Regeneration of ion exchangers

The ion exchanger material is located in bulk in two


separate plastic pipes for cations and anions. The
water is fed through the pipes by a pump.
The exchangers can be used individually or com-
bined in series.
The conductivity measurement is used to measure
the water hardness or the progress of the ion ex-
change.

The table-top unit is equally well suited for per-


forming clear demonstration experiments and lab-
oratory experiments during practical training.
However, it is designed exclusively for training and
educational purposes and is not intended for
industrial use.

1 Introduction 1
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2 Description of the unit

2.1 Unit layout

1container pipes for ion


exchanger
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flow meter
2

measuring
tank with
conductivity 3
measuring
sensor

pump 5
switch
9 collecting tank
conductivity
4
meter
supply tank with
exp. H2O 8 6 intake
rinsing H2O pump 7 pipe
regeneration ( giris)
solution
Fig. 2.1 CE300 unit diagram

1 Container pipes for ion exchanger


2 Flow meter
3 Measuring tank with conductivity measuring sensor
4 Conductivity meter
5 Pump switch
6 Intake pipe
7 Pump
8 Supply tank with experimental water, rinsing water
and regeneration solution
9 Collecting tank

2 Description of the unit 3


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1 The CE300 ion exchange demonstration unit
consists of two transparent plastic pipes (1)
screwed onto a panel. The pipes are filled with ion
exchanger substances to perform experiments.
2 A supply tank (8) with four compartments provides
the substances required for experiments. These are:
– Water for experiments
3
– Cleaning water for rinsing
– Dilute hydrochloric acid
7
– Dilute sodium hydroxide for regeneration
6 These liquids are transported to the pipes via
8 9 hoses using a pump (7).
The hose system features numerous adjusting
Inside:
valves that allow every possible combination of
flows to the exchanger pipes.
– Water for experiments
The substances are selected using an intake pipe
– Cleaning water for rinsing (6), which is simply inserted into the relevant com-
– Dilute hydrochloric acid partment of the tank.
– Dilute sodium hydroxide To allow the volume of liquid delivered by the pump
for regeneration to be determined, all substances flow through a
flow meter (2).
After passing the ion exchanger, the liquids enter a
measuring tank (3), where an add-on unit (4) is
used to measure their conductivity. Finally, the liq-
uid is collected in the collecting tank (9).
The demonstration unit thus works independently
of the mains water supply and only needs a mains
electricity connection to operate the pump.
The conductivity meter is powered by a built-in
battery.

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2.2 Setting up

– Set up the demonstration unit on an even,


solid table.
– Position the collecting tank underneath the
unit to ensure proper discharge of the liquids.
– Place the supply tank on the table and fill the
compartments with the required substances:
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 02/2005

• Water for experiments


• Demineralised water for cleaning and
rinsing the exchanger and the hose
system
• Dilute hydrochloric acid for regenera-
tion of cation exchangers,
concentration 5...10%
• Dilute sodium hydroxide for regenera-
tion of anion exchangers,
concentration 2...4%
– Connect the demonstration unit to the mains
electricity supply. The pump is turned on us-
ing the pump switch (5) as required.

2 Description of the unit 5


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2.2.1 Filling the exchanger pipes

For filling, based on the dimensions of the pipes:


1 cm filling level = 3.53 ml exchanger substance
1 ml exchanger substance = 2.8 mm filling level

– Unscrew the two union nuts on the ends of


Plastic pedestal
the pipe by turning them.
– Remove plastic pipe.
If the pipes stick, the fixing bolts in the rele-
vant plastic pedestal on the rear of the panel
must be loosened slightly.
– Now fill the plastic pipe with the ion
exchanger substance as required.
Union nuts – Replace the plastic pipe and tighten the un-
ion nuts again. If necessary, also tighten the
fixing bolts in the plastic pedestals on the rear
of the panel.

NOTE! Due to the manufacturing process, brand


new ion exchanger substance always contains
solvent and separating agents (e.g. ammonia
etc.). When fresh exchanger substance has been
added, this must first be rinsed with demineralised
water before the ion exchanger can be used.
– To do this, adjust the valves on the unit so
that the rinsing water is fed in at the foot of
the relevant pipe and is discharged at the
head of the pipe.
– Then use the pump to rinse the exchanger
substance with at least 5 litres of demineral-
ised water from the corresponding compart-
ment in the supply tank.

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– After rinsing, completely drain all liquids from


the exchanger pipes.
– After this procedure, the relevant ion
exchanger is ready for experiments.

2.3 Shutdown
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– After performing experiments, turn off the


pump and disconnect the demonstration unit
from the mains electricity.
– Completely drain all liquids from the ex-
changer pipes.
– Drain all compartments in the supply tank
if the unit will not be used for a long period
of time.

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3 Safety

3.1 Health hazards

DANGER! Electrical components


There is a risk of electric shock!
Before opening the pump switch housing, discon-
nect the unit from the mains electricity.
Protect the pump switch housing from moisture
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and dampness.

DANGER! Caustic liquidsAcids and alkalis used.


Serious skin burns possible. Wear protective
gloves and goggles when filling and handling.

DANGER! Substances hazardous to health


Exchanger substances are hazardous to health if
swallowed or inhaled.
Do not eat or smoke during experiments. Avoid
skin contact with the substances.
Wear protective gloves and goggles when filling
and handling.

3.2 Hazards to unit and function

DANGER! Caustic liquids


Spilt chemicals can damage the unit. Wipe away
any spilt chemicals immediately! If necessary,
rinse again afterwards.

3 Safety 9
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4 Principles of ion exchange

4.1 Physical and chemical principles


surrounding
Ion exchange involves ions from a liquid being
bonded onto the surface of a suitable solid and
other ions being given up to the liquid in return.
This enables substances to be removed from solu-
tions. The solid that takes up the ions from the liq-
uid is known as the ion exchanger.
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Ion exchanger substances are mainly synthetically


manufactured, capillary active plastics, e.g. poly-
styrene or polyacrylic acid resin with attached re-
active groups with loosely bonded exchangeable
ions.
They are used in the form of tiny balls or granules
approx. 1 to 3 mm in diameter. The liquid to be puri-
fied is normally passed in bulk through a container.

The take up of the unwanted ions from an aque-


ous solution by the ion exchanger is known as
exhaustion.

Depending on the nature of the active groups, a


distinction is made between:
• Cation exchangers, if the active groups are
acidic in nature and can exchange cations
(e.g. Ca2+, Mg2+ or Na+).
• Anion exchangers, if the active groups are
basic in nature and can exchange anions
(e.g. SO42-, NO3- or Cl-).

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Depending on the function, a distinction is also


made between:
– Weak acidic and
– Strong acidic cation exchangers
and between
– Weak basic
– Medium basic and
– Strong basic ion exchangers.

The general principle of ion exchangers is that


some ions are bonded more strongly to the ion
exchanger substance than others. Particles with a
higher charge have a stronger attraction. For ex-
ample, in an ion exchanger Na+ is displaced by
Ca2+ but in turn Ca2+ is displaced by Al3+. The
stronger ion expels the weaker from the sub-
stance. Therefore, the unwanted ions in the solu-
tion are always attracted more strongly than the
ions that are present in an unexhausted state,
which are given up during the exchange process.
For example, removing Ca2+ cations and HCO3-
anions from untreated water involves the following
processes:

Cation exchanger CE

Anion exchanger AE

The H+ ions and OH- ions given up to the


exchanger combine into water
H+ + OH- ⇒ H20
The water that flows through the ion exchanger is
then free of foreign ions.

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The ion exchange is a reversible process. There-


fore, with an exchanger that is partially exhausted
but still capable of taking up ions, a counter ion ef-
fect can occur. This involves giving up ions already
bonded to the ion exchanger to the surrounding
water if there is no more flow of water to the
exchanger mass.
For example, if soft water free of earthy bases is in
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 02/2005

contact with a partially exhausted softening mass


for a long period, the soft water becomes impure
again with earthy bases from the exchanger.
After rinsing and repeated water flow, perfect wa-
ter is again discharged.

Measuring technique :
• Conductivity measurement
Aqueous solutions of salts conduct electrical cur-
rent as they contain free moving ions. All sub-
stances that conduct electrical current have a
measurable specific electrical conductivity. (This
is the inverse of the specific electrical resistance.)
Even traces of ions increase the conductivity of
pure water by several powers of ten. Accordingly,
electrical conductivity is used as a measure of the
purity of water. In many measuring situations, it is
used as an overall parameter for measuring
dissolved inorganic substances.

The unit of conductivity is:

1
Ω S
=
m m

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However, in practice the units mS/ or µS/cm are


cm
normally used:

1S/m = 100 S/cm


= 100,000 mS/cm
= 100,000,000 µS/cm

The electrolytic conductivity is measured to moni-


tor the function of desalination plants, for example.
Pure water has a minimum electrolytic conductivity
in the pH range 6.8 to 7.2. Even tiny quantities of
ions increase the conductivity significantly. Thus,
exhaustion of the ion exchanger or a defect can be
reliably identified.

• Analytical hardness calculation


There are applications in which measurement of
the electrolytic conductivity does not allow a sound
conclusion on the water hardness because it is not
clear which type of ions is causing the conductivity
(e.g. section 4.4.1 “Water softening”). In this case,
the hardness must be determined in an alternative
way using chemical methods, e.g.
– Titration
– Test strips
– Water analysis kits

3 types of hardness calculation:

titration
test strips
analysis kit

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4.2 Take up capacity of ion exchangers

The capacity of an exchanger is the quantity of


ions that one litre of the exchanger substance can
take up from an aqueous solution. It is specified
using the volumetric capacity in mmol/ml or in
equivalents eq/ltr.

In practice, the theoretical total capacity of an


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exchanger material cannot be fully utilised for vari-


ous reasons. The usable capacity (NVK) is there-
fore used; this is not a constant value as it de-
pends greatly on:
– Water composition (ions available)
– Specific load (ratio between exchanger
quantity and volumetric flow of water to be
purified)
– Water temperature
– Excess regenerating agent from prior regen-
eration process

The theoretical water quantity from which ions can be exchanged is calculated
from the NVK as follows:

VH 2O =
NVK ⋅ VT
×
[mmol ml] ⋅ [ml ] = [ltr ]
kH2 0 [mmol ltr ]
VH 2O : Exchangeable water quantity

k H 2O : Concentration of ions to be exchanged in water


NVK : Usable volumetric capacity of exchanger material
VT : Volume of exchanger material

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4.3 Regeneration

The capacity of the ion exchanger substance is


limited. The substance is exhausted when all ac-
tive groups of its ions have been given up. The ion
exchanger is then completely exhausted. How-
ever, the exhaustion of the ion exchanger filling in
a system can be removed. Giving up or expelling
the ions from the exchanger material is known as
regeneration.

The possibility of regeneration is based on the fact


that, like most chemical reactions, ion exchange is
a reversible process.
Actually, the forward and back reactions in the
exchanger material always occur simultaneously
(chemical equilibrium). However, the forward re-
action is predominant when using the ion
exchanger. To regenerate exhausted ion
exchangers, extreme force must therefore be ap-
plied. It is possible to force the back reaction, re-
generation, by adding an excess of “weaker” ions;
the amount of weaker ions displaces the stronger
ions.
With a cation exchanger, this is done with acid, us-
ing hydrochloric acid (H+ + CI-).

With an ion exchanger, an alkali is used, preferably


sodium hydroxide (Na+ OH-).

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The quantitative conclusions on the capacity


of ion exchanger materials apply in reverse for
regeneration.

Regeneration results in a liquid that, in addition


to excess acid or alkali, contains a high concen-
tration of the exchanged ions.
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The regenerating agent can be fed to the resin


as a parallel flow (same flow direction as for ex-
haustion) or as a counter flow. Reverse flow re-
generation enables a better effect to be
achieved with a lower quantity of regenerating
agent. The exchanger resin must be rinsed be-
fore and after regeneration.

Oil, grease, iron and manganese compounds


and organic substances can block the active
groups in the exchanger and thus impair the per-
formance of the exchanger.

4 Principles of ion exchange 17


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4.4 Applications of ion exchangers

4.4.1 Water softening yumsaltma


Untreated water

Regeneration with
NaCl solution

Softened
water
Suyun yumaldılması Ca2+ v onun
aradan qaldırılmasını nzrd tutur
Mg2+ suda hll olunan torpaq sas
kationları, Water softening involves eliminating the Ca2+ and
hng çöküntülrinin yıılmasına sbb Mg2+ earthy base cations dissolved in the water,
ola bilr
borularda v avadanlıqlarda. which can cause the build up of limescale deposits
n çox istifad ediln üsul (msln, evlrd) in pipes and equipment.
natrium ionları il mübadil etmkl
yumalmadır. The most frequently used method (e.g. in house-
Tmizlnmmi su dyidiricidn keçir holds) is softening by exchanging for sodium ions.
sütun. Burada Na+ ionları suya
keçir The untreated water flows through an exchanger
v bunun müqabilind Ca2+ v Mg2+ column. Here, the Na+ ions switch into the water
ionları balanır.
and in return the Ca2+ and Mg2+ ions are bonded.

Prosesdn sonra suyun trkibind After the process, the water contains Na+ cations
Na+ kationları var and various anions. It does not change the salt
v müxtlif anionlar. Duzunu content of the water. This method enables water to
dyimir
suyun trkibi. Bu üsul suya be softened to <0.01mmol/ltr in terms of the Ca2+
imkan verir and Mg2+ earthy base ions.
<0,01 mmol/- qdr yumaldılmalı
Ca2+ baxımından ltr The exhausted cation exchanger is normally re-
v Mg2+ torpaq sas ionları generated using saturated common salt solution
(NaCl). Tüknmi kation dyidiricisi, adtn, doymu ümumi duz
mhlulundan istifad edrk yenidn yaradılır
(NaCl)

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4.4.2 Dealkalisation of water

Untreated water
(Regeneration with dilute
hydrochloric acid)
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CO2
degasification
Dealkalised
water

Dealkalisation is the method of removing hydro-


gen carbonates (HCO3- ) dissolved in the water. In
water with a higher hydrogen carbonate content,
the previous type of softening is not normally suffi-
cient. For example, to obtain feed water for boilers
or heating water, it is also necessary to remove the
hydrogen carbonate ions.
A weak acidic cation exchanger is used to remove
the cations (Ca2+, Mg2+, Na+), which are bonded to
hydrogen carbonate ions. Corresponding quanti-
ties of H+ ions are given up. The excess HCO3-
ions then combine with the H+ ions to form CO2
gas, which dissolves in the water.

H+ + HCO3- ⇒ CO2 + H2O


yaratmaq , baslatmaq
DEGAZIFICATION --prosesi As the CO2 can promote corrosion, it is expelled in a
ile downstream dan CO2 qazi downstream CO2 degasification process.
xaric edilir
This process reduces the salt content in the water. It
Bu proses suda duzun miqdarını azaldır. O is therefore referred to as partial demineralisation.
buna gör d qismn demineralizasiya adlanır.

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Yumaldılmı suyun trkibind hl d H+, SO4 The softened water still contains H+, SO42-, CI- and
var
2-, CI- v NO3- ions, but without cations from the earthy
NO3 base group these do not form any deposits.
- ionlar, lakin torpaqdan kationlar
olmadan The exhausted cation exchanger is normally re-
baza qrupu bunlar heç bir depozit tkil generated using a slight excess of dilute hydro-
etmir.
chloric acid (HCl).
Tüknmi kation dyidiricisi normal olaraq
az miqdarda seyreltilmi hidroklor turusu
(HCl) istifad edrk yenidn yaradılır.

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4.4.3 Total demineralisation of water

Untreated water

CO2
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degasi-
fication

Demineralised
water

Diagram of a total C - Strong acidic cation exchanger


demineralisation A1 - Weak basic anion exchanger
treatment unit A2 - Strong basic anion exchanger

Total demineralisation by ion exchange can be


used to produce chemically pure water. This pro-
cess has almost completely replaced distillation of
water as a demineralisation method.
Demineralised water has a conductivity value of
less than 10µS/cm.
In its simplest form, it involves a strong acidic cat-
ion exchanger and a strong basic anion exchanger
in series. The cation exchanger gives up the ap-
propriate quantities of H+ ions, while the anion
exchanger gives up the appropriate quantities of
OH- ions. These combine to form water:

H+ + OH- ⇒ H2O

In certain special cases, it is advisable to separate


the filters into weak and strong levels for capacity
reasons. Strong basic anion exchangers can only

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take up anions from mineral acids such as Cl-,


SO42- or NO3-.
Strong basic anion exchangers are also able to re-
move silicic acid (SiO 32-) and carbonic acid
(CO32-). To prevent excessive loading of the
strong basic anion exchanger with carbonic acid,
for water with hydrogen carbonate content
(HCO3-) of above around 2mmol/ltr, CO2 degasifica-
tion is incorporated.
The figure below illustrates all possible variations
for total demineralisation of water.

Weak Strong Weak CO2 Strong


acidic acidic basic degasi- basic
fication

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5 Experiments

5.1 Exchanging cations

(Softening)
In this experiment, only the cations will initially be
exchanged from an experimental water (tap water)
loaded with ions.
The aim is to reduce the hardness of the water pri-
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marily by removing the Ca2+ and K+ cations.

• Preparation
– Provide experimental water and demineral-
ised rinsing water in the supply tank.
– Fill one of the exchanger pipes with weak
acidic cation exchanger material
(~40 ... 60mm filling level = ~14 ... 21ml).
– Adjust the valves on the unit so that the ex-
perimental water is fed in at the head of the
exchanger pipe and flows out into the mea-
suring tank at the foot of the pipe.
– If fresh exchanger substance is used, the
material in the exchanger pipe must first be
rinsed with demineralised water.
– Ascertain and note the conductivity of the ex-
perimental water. In addition, use an alterna-
tive method to ascertain and note the hard-
ness of the experimental water.

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• Performing the experiment


– Turn on the pump and allow the experimental
water to flow through the exchanger pipe
(~80ml/min).
– At regular intervals (approx. 1 min) note the
conductivity of the discharged water.
– At regular intervals (3-5 min) take a sample of
the discharged water. (To do this, the inlet
hose can be disconnected from the measur-
ing tank.) Ascertain and note the hardness of
the water sample.
– Perform the experiment until the hardness of
the discharged water approximately equates
to that of the experimental water. The
exchanger substance is then exhausted.
– Ascertain and note the hardness of the last
water discharged from the exchanger.

• Evaluation and results


The comparison shows that the hardness values
for the water have fallen considerably after pass-
ing through the cation exchanger. This is to be ex-
pected as the exchanger substance has predomi-
nantly removed Ca2+ and K+ cations from the wa-
ter and replaced them with H+ ions.

However, the conductivity of the water hardly ap-


pears to change as it passes through the ion
exchanger. This is also to be expected as ulti-
mately no ions are removed from the water, it is
only the type of ions dissolved in it that changes.
The conductivity is not therefore impaired.

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The experimental water has thus been identifiably


softened but the ion load has not been reduced.
This result could only be identified by ascertaining
the hardness. The method of measuring the con-
ductivity is obviously inadequate for verifying and
monitoring this type of softening.
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 02/2005

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5.2 Exchanging anions

(Dealkalisation)
In this experiment, only the anions will initially be
exchanged from an experimental water (tap water)
loaded with ions.
The aim is to primarily remove the HCO3- ions
from the water.

• Preparation
– Provide experimental water and demineral-
ised rinsing water in the supply tank.
– Fill one of the exchanger pipes with weak ba-
sic anion exchanger material (~40 ... 60mm
filling level = ~14 ... 21ml).
– Adjust the valves on the unit so that the ex-
perimental water is fed in at the head of the
exchanger pipe and flows out into the mea-
suring tank at the foot of the pipe.
– If fresh exchanger substance is used, the
material in the exchanger pipe must first be
rinsed with demineralised water.
– Ascertain and note the conductivity of the ex-
perimental water before the experiment. In
addition, use an alternative method to ascer-
tain and note the hardness of the experimen-
tal water.

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• Performing the experiment


– Turn on the pump and allow the experimental
water to flow through the exchanger pipe
(~80ml/min).
– At regular intervals (approx. 1 min) note the
conductivity of the discharged water.
– At regular intervals (3-5 min) take a sample of
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 02/2005

the discharged water. (To do this, the inlet


hose can be disconnected from the measur-
ing tank.) Ascertain and note the hardness of
this water sample.
– Perform the experiment for at least 20 minutes.

• Evaluation and results


The comparison shows that the hardness values
for the water have not changed after passing
through the anion exchanger. This is to be ex-
pected as the water hardness is primarily related to
Ca2+ and K+ cations and these were not removed
from the experimental water at all during this
experiment.

However, the HCO3-- ions are presumed to have


been replaced with OH- ions. This presumption is
based on the fact that the conductivity of the water
discharged from the exchanger has actually in-
creased noticeably. The OH- ions are more loose
in a solution than HCO3- ions. This is the reason
for the increase in conductivity.

The experimental water appears to have been


dealkalised. However, this conclusion is only
speculative as the fundamental measuring meth-
ods for verifying and monitoring simple removal of
anions are obviously inadequate.

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5.3 Series connection of cation and anion exchangers

(Total demineralisation)
In this experiment, all mineral ions will be ex-
changed as completely as possible from an experi-
mental water (tap water) loaded with ions.
To do this, the two exchanger methods from sec-
tions 5.1 and 5.2 are combined.

• Preparation
– Provide experimental water and demineral-
ised rinsing water in the supply tank.
– Fill one of the exchanger pipes with cation
exchanger material
(~40 ... 60mm filling level = ~14 ... 21ml).
– Fill the second exchanger pipes with basic
anion exchanger material
(~40 ... 60mm filling level = ~14 ... 21ml).
– If fresh exchanger substance is used, the ma-
terial in both exchanger pipes must first be
rinsed separately with demineralised water.
– Adjust the valves on the unit so that the ex-
perimental water is fed in at the head of the
first exchanger pipe and flows out at the foot
of the pipe. The discharged water should
then be fed to the head of the second
exchanger pipe and then from the foot of this
pipe to the measuring tank.
– Ascertain and note the conductivity of the ex-
perimental water before the experiment. In
addition, use an alternative method to ascer-
tain and note the hardness of the experimen-
tal water.

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• Performing the experiment


– Turn on the pump and allow the experimental
water to flow through the two exchanger
pipes connected in series (~80ml/min).
– At regular intervals (approx. 1 min) note the
conductivity of the discharged water.
– At regular intervals (3-5 min) take a sample of
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 02/2005

the discharged water. (To do this, the inlet


hose can be disconnected from the measur-
ing tank.) Ascertain and note the hardness of
this water sample.
– Perform the experiment until the conductivity
of the discharged water approximately
equates to that of the experimental water.
The exchanger substances are then ex-
hausted.

• Evaluation and results


Both the conductivity and hardness values for the
water are significantly reduced after passing
through both ion exchangers.
This result is both expected and intended.
Most of the cations have apparently been ex-
changed for H+ ions and the anions for OH- ions.
These neutralise one another and form water. The
ions are thus effectively exchanged and the exper-
imental water is demineralised.
The conductivity measurement is obviously a suit-
able method for monitoring the demineralisation
quality.

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5.4 Regeneration

Each ion exchanger material has a limited ex-


changing capacity. Once all active groups are sat-
urated with foreign ions, the material is exhausted.
It can be regenerated by expelling the exchanged
ions.
Anion exchanger substances are regenerated us-
ing strong anions, normally OH- or CL- ions.
Cation exchanger substances are normally regen-
erated using acids, e.g. dilute hydrochloric acid.

On the CE300 demonstration unit, the exchanger


substances are regenerated using the following
chemicals:
• Cation exchanger
– Dilute hydrochloric acid, 5 ... 10%
• Anion exchanger
– Dilute sodium hydroxide, 2 ... 4%

• Preparation
– Provide dilute hydrochloric acid, 5 ... 10%,
dilute sodium hydroxide, 2 ... 4% and demin-
eralised rinsing water in the supply tank.
– Fill one of the exchanger pipes with the cation
or anion exchanger material to be regenerated
(~40 ... 60mm filling level = ~14 ... 21ml).

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– Adjust the valves on the unit so that the re-


generating solution is fed in at the head of the
exchanger pipe and flows out into the mea-
suring tank at the foot of the pipe.
– Choose the appropriate regenerating solu-
tion for the relevant ion exchanger material in
the supply tank (intake pipe).
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 02/2005

• Method
– Turn on the pump and allow the regenerating
solution to flow through the exchanger pipe
(~40ml/min).
– Perform the experiment for approx. 3 ... 5 min-
utes. The exchanger substance is then regen-
erated.
– ATTENTION!After regeneration, the rele-
vant exchanger pipe must always be rinsed
with demineralised water until the conductiv-
ity of the discharged rinsing water no longer
shows any significant deviation from that of
the demineralised water fed in.
– To confirm and verify the regeneration pro-
cess, an ion exchange experiment can then
be performed as described in 5.1 or 5.2.

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• Example quantitative analysis


What is the minimum amount of time for regenerat-
ing an exchanger substance? Example:

Given: Anion exchanger substance, weak basic


Exchanging capacity NVK = 1,0 mmol
ml
Exchanger volume VT = 40 ml

Regenerating solution, dilute sodium hydroxide


Concentration c =OH 2% = 0,5 mmol
ml
Regenerating solution flow rate

VR = 20 ml
min

Desired results: Regeneration time tR

• Quantity of ions to be exchanged


1.0 mmol
mI = NVK ⋅ VT = ml ⋅ 40 ml = 40 mmol

The minimum quantity of OH ions that must be available for regeneration


is therefore also:
mOH = mI = 40 mmol

The following volume of regenerating solution is required:


• mOH 40 mmol
VR = = = 80 ml
c OH 0,5 mmol
ml

This results in a theoretical regeneration time tR of:


V 80 ml
tR = • R = ml
= 4 min
VR 20 min

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While this theoretical calculated value for tR is only


of limited use, it does provide at least a reference
point for the time dimension that needs to be used
as a basis.
The above analysis requires the ion exchange pro-
cess in the exchanger substance to be spontane-
ous and optimal with no losses. However, this is
not the case in practice. Therefore, regeneration
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 02/2005

must always be performed with an excess of the


ions offered. This applies to both the concentra-
tion of the regenerating solution and to the
regeneration time.

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5.5 Notes on further experiments

Because of its design, the unit allows numerous other experi-


ments to be performed. It is not possible to include examples
of all of these. It is left to the user’s discretion to perform these
alternative experiments independently.
The following notes on possible variations are intended to act
as a guide.

• Varying the contact times in the exchanger. Increasing


the flow rate reduces the dwell time of the water in the
exchanger pipe and thus the contact time with the
exchanger material. On the other hand, the number of
exchangeable ions available increases. The same ap-
plies to ion exchange and regeneration. Determine the
exchange effect with:
– Different flow rates
– Different quantities of exchanger material

• Variation in exchanger material. Determine the ex-


change effect with:
– Strong acidic or basic exchanger substances
– Weak acidic or basic exchanger substances

• Variation in temperature. Ion exchange is an equilibrium


reaction that is influenced by the temperature.

• Variation in flow direction The effect and quality of re-


generation depends on whether it is performed with a
parallel or counter flow. This is based on the flow direc-
tion used for the preceding ion exchange.

34 5 Experiments
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6 Appendix

6.1 Technical data

LxWxH 600 x 500 x 980 mm


Weight: approx. 55 kg
Power supply: 230V / 50Hz
Optional alternatives, see rating plate
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 02/2005

Cation exchanger MERCK 104835 cation exchanger IV


Weak acidic, capacity > 3.2 mmol/
ml

MERCK 104765 cation exchanger IV


Strong acidic, capacity > 1.7 mmol/
ml

Anion exchanger MERCK 115261 AMBERLYST(®) A-21


Weak basic, capacity > 1.0 mmol/
ml

MERCK 104767 anion exchanger III


Strong basic, capacity > 0.9 mmol/
ml

Exchanger columns Material PVC, transparent


Length 400 mm
Internal diameter Ø 21.2 mm
External diameter Ø 25 mm

1mm filling level = 0.353ml exchanger substance


1ml exchanger substance = 2.8mm filling level

Chemical and material requirements


for regeneration: Hydrochloric acid HClaq 5 ...10 %
Sodium hydroxide NaOHaq 2 ... 4 %
for rinsing the exchanger: distilled or demineralised water

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CE 300 ION EXCHANGE DEMONSTRATION UNIT

Pump Capacity ~300 ml/


min

Suction height max. 6 m


(water column)
Head max.10 m
(water column)
Electrical supply 24 VDC

Flow meter Measuring range 20 ... 260 ml/


min

Conductivity measurement Measuring range 0 ... 200 mS/


cm

0 ... 85 °C
Electrical supply Battery operated

Tanks Supply tank 4 x 5 litres


LxWxH 350 x 350 x 210 mm
Collecting tank ~ 25 litres
LxWxH 350 x 350 x 210 mm

Items supplied
1 Complete demonstration unit
1 Conductivity meter
1 Instruction manual

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6.2 Tables

Measured conductivity values for different waters


Ultra-pure water 0.05 ... 0.1 µS/cm
Water from ion exchanger ... 5 µS/cm
Distilled water ... 20 µS/cm
Drinking, ground water 300 ... 800 µS/cm
River, lake water 1 ... 5 mS/cm
All Rights Reserved G.U.N.T. Gerätebau GmbH, Barsbüttel, Germany 02/2005

Sea water ~50 ... 60 mS/cm

The water hardness is primarily related to the K+ and Mg2+


ions contained in the water. The most frequently used units for
water hardness are the French hardness grade (°f)
1°f = 20µS/cm

and the German hardness grade (°dH)


1°dH = 30 µS/cm

Overview of water hardness


in German and French grades
µS/cm °dH °f
0 -140 0-4 0-7
140 - 300 4-9 9 - 15
300 - 500 9 - 15 15 - 25
500 - 640 15 - 19 25 - 32
640 - 840 19 - 25 32 - 42
> 840 > 25 > 42

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CE 300 Worksheet
Date:
Experiment no.:

Participants:
Topic of experiment:

Ion exchanger used: Experimental setup & method

£ Cation exchanger, weak acidic


£ Cation exchanger, strong acidic
£ Anion exchanger, weak basic
£ Anion exchanger, strong basic

Duration of Water
Conductivity hardness
experiment µS
in /cm Comments
in min °f °d

40 6 Appendix

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