Ion-Resins Regeneration
Ion-Resins Regeneration
Fouled Ion
Exchange
Resins
Contents
Sodium Hypochlorite 9
Hydrochloric Acid 16
Sodium Chloride 17
Abbreviations 19
BEST PRACTICES 2
Pictured: Elution study shows resin fouling.
Increased regenerant quantities, regeneration frequency and elevated regeneration temperature may
reduce fouling by preventing foulants from gaining a permanent hold.
A good operating practice is to ensure that all resin in the ion exchange units is regularly contacted
with sufficient regenerant and subject to a regular cleaning procedure.
• Faults in the operating process. Incorrect conditions of regeneration, failure to operate the plant
according to instructions, faulty backwash procedures, and inconsistent rinse volumes and
regenerating concentrations are relatively easy to ensure all functions are operating correctly.
• Malfunction of the plant engineering hardware. This is the most difficult condition to diagnose —
requiring unit shut down, removal of the resin and thorough inspection and testing.
If bed levels, water chemistry, operating processes and engineering hardware check out
satisfactorily, a sample of resin should then be examined.
A bed volume (BV) is the amount of resin that needs to be treated. For example, if the vessel holds
100 ft3 of resin, that is the BV.
To obtain a representative sample of the resin contents of a mixed bed, please refer to our brochure
on this subject at https://bit.ly/3zg84kX.
BEST PRACTICES 4
Analyses will report aging and fouling of sampled resin. If required, various procedures are
available to clean resins. This document covers cleaning procedures for the following:
• Fouling by oil
Bacteria contamination
Work done by the Degussa Technical Applications Department in conjunction with Chemiewerk
Homburg AG determined that peracetic acid is suitable as a disinfectant for deionizers because
of its wide spectrum of attack. Using a 0.1% peracetic acid solution in water with a reaction
time of one hour, a slime and mold concentration of 104–105/mL was reduced to almost zero.
The short rinsing time after using peracetic acid is of importance (typically about 45 minutes
or 10–15 BV).
Experiments have shown that in addition to excellent disinfection action, peracetic acid has
minimal effect on the ion-exchange properties of cation or anion resins.
BEST PRACTICES 6
If peracetic acid is used as a disinfectant, the following procedure should be used for both cation
and anion resin in regenerable systems.
• Ensure anion resins are fully exhausted as peracetic acid performs best at a pH < 8.
• Make up 1 bed volume (BV) of peracetic acid solution containing 0.1% peracetic acid.
• When all the peracetic acid has been injected, close all valves and retain the disinfectant for
at least one hour to soak the resin and pipe work.
• Carry out a displacement rinse using raw water for at least 60 minutes at 5 BV/h, followed
by a fast flush for 30 minutes.
Once the influent source is eliminated, the next step is to flush the system out. Often, a 24-
hour flush at design flow is enough to clean up a system adequately to pass bacteria tests. If a
24-hour flush at full flow is not feasible due to site conditions, try to flush as much volume as
reasonably possible, and pull bacterial samples.
Please note — single-use resin systems should not be backwashed. If there is enough biological
activity to cause clogging, evaluate if solids can be physically removed from the top of the vessel
with a vacuum or a net. Make sure all equipment is sterilized before use to ensure no more
bacteria is introduced into the system.
Chlorine should never be used with anion resin as a disinfectant for several reasons. First, the
chlorine is consumed before a chlorine residual can be established throughout the bed, so the
full bed is not disinfected. While the chlorine is consumed, the chlorine is also breaking chemical
bonds in the resin. Functionality of the resin is lost, and chemicals like nitrosamines will be formed
and released.
For these reasons, hydrogen peroxide is more commonly used as it is less oxidative than chlorine,
yet it still has oxidative and biocidal efficiency necessary to get a system back in service. Use only
Food Grade ANSI/NSF 60 certified products for potable water systems.
To disinfect a drinking water system using a single-use anion ion exchange resin, follow
these steps.
• Before hooking up any equipment or hosing, ensure it has been disinfected and rinsed.
• Drain about one third of the water that is above the resin in the vessel to leave freeboard space
in the vessel for any foaming that may occur.
• Establish a vent path (for possible foaming) with a resin screen to prevent resin spillage
• Determine the amount of peroxide need to create a solution of 0.1% or 1000 ppm of
hydrogen peroxide.
• The basis of the volume of solution will be around half the total volume of the vessel.
• Start recirculation of the vessel with a flow rate of 5 BV/h (0.6 USGPM/cu ft) discharged to a drain
approved for chemical waste disposal.
• Inject the hydrogen peroxide into the system, preferably in the recirculation pump suction.
• Verify concentration of hydrogen peroxide with test strips at the outlet sample port. Approach
the injection slowly. Be careful not to overdose the peroxide into the resin bed.
• Recirculate the system for a minimum of one to two hours. Check the concentration periodically.
• Rinse or flush the vessel to a zero residual of hydrogen peroxide at the outlet sample port,
discharging to a drain approved for chemical waste disposal.
BEST PRACTICES 8
• This is typically about 45 minutes or 10–15 BV when flushing at full flow.
• Continue to flush, if possible, while awaiting sample results. If continuous flushing is not
achievable, the resin should be flushed a minimum of 5 BV’s at a flowrate greater than
6 USGPM/SQFT every 24 hours.
Sodium Hypochlorite
Sodium hypochlorite is widely available in the form of small carboys and containers. For resin
sterilization, a 0.1% available chlorine solution should be used. This is obtained by diluting the
commercially available hypochlorite.
• Regenerate the column with brine before treatment to convert all resin to the exhausted form
(a double or triple regeneration is often required.) Note that cation resin will produce chlorine
gas if not properly exhausted before treatment.
• The minimum volume of solution required to treat the bed is 3 BV (i.e. 3 times the resin
volume installed in the unit).
• Pass the first bed volume through the bed at normal regeneration flow rate, or approximately
4 BV/h (0.5 USGM/ft3).
• Retain a portion of the second bed volume in the bed for no more than 2 hours.
• Pass the third bed volume through the bed at approximately 4 BV/h.
• Displace the sodium hypochlorite at a rate of approximately 4 BV/h with softened water,
then rinse thoroughly to remove any trace of sodium hypochlorite. At least 8–10 bed volumes
are required.
The procedure is also not recommended for phenolic, polycondensation and chelate resins.
For anion resins, the oxidizing effect of the sodium hypochlorite is on the amine groups, and
therefore disinfection in sodium hypochlorite should only be considered in extreme cases on a
once-off basis.
Suitable safety precautions should always be taken when using sodium hypochlorite.
Additionally, all environmental laws and regulations should be followed when discharging waste
into drains. All discharge areas should be free from acids or other chemicals that may react
adversely with the dilute hypochlorite discharge.
Iron can also be complexed with organic matter; in which case it is present as an anionic complex.
Normally, iron present in the ferric state is removed by cation resin operated in either the sodium
or hydrogen forms.
In the case of hydrogen form cation resin representing the first stage of a demineralization
system, the iron is removed from the water and eluted on regeneration with mineral acid. The
situation is different with softening resin. Here, the ion exchange resin removes the iron from the
water, but the regeneration procedure — which uses brine — does not elute the accumulated iron
from the resin during the regeneration cycle. Consequently, the iron accumulates on the resin
from cycle to cycle and steadily causes progressive iron fouling.
In the case of iron being present as organic/iron complexes, the complex is present as an anion,
and is removed from the solution by the anion resin.
Because anion resin is regenerated with caustic soda, the iron is retained on the resin
even though organic material is substantially removed with each regeneration cycle. This
accumulation of iron on the resin causes the anion resin to become iron fouled.
BEST PRACTICES 10
When iron content of water is > 0.5 mg/L (0.5 ppm), it is recommended that some form of
pre-treatment is used to reduce the ion level to < 0.1 ppm.
The use of sulfuric acid while iron is present in feed water can result in an accumulation
of iron on the resin and cause reduction in performance. In these cases, treatment with
hydrochloric acid should be considered providing the internal construction of the units and
attendant pipe work are compatible with hydrochloric acid.
In cases where iron accumulates on softening resin, either hydrochloric acid or citric acid
treatment can be considered for treatment. When iron content of water is > 0.5 mg/L
(0.5 ppm), it is recommended that some form of pre-treatment is used to reduce the ion level
to < 0.1 mg/L (0.1 ppm). An alternative option is to use special Purolite resins, called Shallow
Shell technology — or SST®. The SAC or WAC versions are able to treat water with up to
20 mg/L (20 ppm) of Fe2+.
Online cleaning with citric acid is a simple procedure and requires a chemical feed system
comprised of a small tank and a chemical feed pump. 50% citric acid is used for both on-line
and off-line cleaning procedures.
In the case of a WAC or SAC resin operating in the hydrogen form (acid regeneration), the
solution is pumped into the backwash inlet at a dosage of 9 mL/L-R (9 oz/ft3-R). In the case
of a SAC operating in the sodium form (salt regeneration), the same dosage is used, but the
citric acid is metered into the brine dilution water or add the full amount of citric acid into the
brine tank.
The pump rate is established based on the dosage and the time to complete the backwash
step (or dilute brine feed if using a SAC in the sodium form). For example, 1,000 liters (35 ft3)
Off-Line Cleaning
Off-line cleaning with citric acid is prescribed when the resin is extremely fouled. This procedure
requires the unit to be out of service for approximately 8 hours. A mixing vessel, drum pump, air lance
and proper safety equipment will be required to perform this cleaning procedure.
Prior to cleaning the resin should be backwashed and regenerated as per normal operating
procedures. This step will help reduce the amount of insoluble and soluble iron in or deposited
on the resin and the tank internals.
The dosage for an off-line cleaning is 600 mL/L-R (0.5 USG/ft3-R) of resin. In the previous example we
used 1,000 liters (35 ft3) of resin, so the off-line procedure would require 190 liters (50 USG) of 50%
citric acid solution.
Open the vessel man way and drain the water to 30 cm (12 in) above the top of the resin bed. Utilizing
a drum pump, slowly pump the entire 190 liters (50 USG) of cleaning solution into the vessel. Drain the
vessel again until the liquid level is approximately 5 cm (2 in) above the top of the resin bed. This step
places the cleaning solution in direct contact with the resin.
With the citric acid solution in contact with the resin bed, air-lance the entire resin bed using clean oil
free plant air. A 2.5 cm (1 in) diameter PVC pipe can be used for the air lance. If the vessel has a gravel
underdrain support, make sure to avoid contact with the air lance. The air-lancing step should be
conducted for 2–3 minutes every ½ hour for 4–6 hours.
BEST PRACTICES 12
Upon completion of the cleaning the vessel should be closed, filled, vented and backwashed with
finished water until clear. After backwashing perform a standard regeneration.
In some circumstances it may be difficult to remove the control head from the softener to add
the citric acid and sparge the resin/cleaning solution. In this case, the saturated brine tank can be
used to prepare the citric acid. Please note that it would be acceptable to mix the 50% citric with
the saturated brine.
Use the system controls to add the cleaning solution to the resin. Be sure to empty the contents
of the saturated brine tank to assure that all of the cleaning solution goes into resin. Soak as
described above for 4 to 6 hours followed by a standard NaCl regeneration.
Citric Acid Cleaning Procedure for Purolite Strong Base Anion (SBA)
Operated in Chloride (Cl-) Form Resin — Dealkalizing,
or Organic Trap
Use of citric acid for restoring capacity of fouled ion exchange resin by removal of organic foulants,
precipitated calcium/magnesium as well as iron and copper oxides.
2. Regenerate with 160 g/L-R (10 lb/ft3-R) of 10% brine solution at 2 LPM/L-R
(0.5 USGPM/ft3-R).
4. Drain the water level to 6” above resin with regenerated resin bed.
5. For 40% citric acid, add 70 ml/L-R (0.5 USG/ft3-R). For example: SBA tank contains
1,000 liters (35 ft3) = add 70 liters (20 USG) to resin bed.
For 90% citric acid, add 25 ml/L-R (0.2 USG/ft3-R). For example: SBA tank contains
1,000 liters (35 ft3) = add 25 liters (7 USG) to resin bed.
6. Drop water level to 2.5 cm (1 in) above resin bed (reducing resin level 13 cm (5 in)
will allow reaction in under bedding).
7. Using air sparging technique, add induced air for 2–3 min. per 1/2 hour for a minimum of 8
hours. Disruption towards the bottom of the bed in an upward directional air flow will create
foam and carbon dioxide (CO2 from citric acid + calcium carbonate reaction). This would
indicate suspected fouling at bottom of bed. You may be able to run the air for longer periods
8. Rinse for at least 30 min. or till effluent water is clear from vessel.
9. Regenerate the unit using a 10% NaCl and 2% Caustic Soda solution of 192–240 g/L
(12–15 lb/ft3) at 2 LPM/L-R (0.5 USGPM/ft3-R) and let resin soak for 8 hours.
10. At end of soak, add 75–85 mL/L-R (7-8 USG/ft3-R) of same solution.
Preventative treatment going forward: Add 3–4 liters (3–4 quarts) 90% citric acid per 100 liters
(3.5 ft3) of resin and leave out caustic during this regeneration.
3. After regeneration is done, open the top manway and drain the water level down to 15 cm
(6 in) above the resin bed.
4. For 40% citric acid, add 70 ml/L-R (0.5 USG/ft3-R). For example: SBA tank contains 1,000
liters
(35 ft3) = add 70 liters (20 USG) to resin bed.
For 90% citric acid, add 25 ml/L-R (0.2 USG/ft3-R). For example: SBA tank contains 1,000
liters
(35 ft3) = add 25 liters (7 USG) to resin bed.
BEST PRACTICES 14
5. Using Air Sparging technique, add induced air for 2–3 min. per 1/2 hour for a minimum
of 8 hours. Disruption towards the bottom of the bed in an upward directional air flow will
create foam and carbon dioxide (CO2 from citric acid + calcium carbonate reaction). This
would indicate suspected fouling at bottom of bed. You may be able to run the air for longer
periods as the hardness breaks and foaming occurs in less volume.
6. Rinse for at least 30 min. or till effluent water is clear from vessel.
9. Perform a caustic regeneration cycle, hold the caustic inject step for 2x the normal
time setting.
These organic species become trapped within the resin matrix due to their large molecular
weights. Symptoms of organic fouling include long rinse requirements, poor capacity and
in the case of strong base resins, higher silica leakage.
The following treatment helps return the original ion exchange properties of the resin.
• Prepare three bed volumes of 10% w/v brine solution containing 2% w/v caustic soda.
Temperate of the solution should be between 95 °F (35 °C) and 140 °F (60 °C) to ensure
optimal organic elution effect.
• Introduce one bed volume into the ion exchange unit at a flow rate not exceeding 2 BV/h
followed by a second bed volume.
• Retain the second volume in the unit for as long as possible (minimum 4 hours). Periodically
agitate the bed throughout the retention period.
• At the end of the retention period, the last bed volume of brine should be passed through the
resin at a rate of 1 BV/h and the resin rinsed thoroughly with clean water until free from brine.
• Subject the resin to at least two complete regeneration cycles before returning online.
In these cases, it is advisable to treat the anion resin with 6% hydrochloric acid immediately after
the brine treatment. The procedure that should be followed is similar to that given for brining.
It is very important that all traces of hydrochloric acid are removed from the unit before
introducing caustic soda regenerant, and that all parts of the unit that come into contact with
the hydrochloric acid are compatible with and resistant to the acid.
Iron fouling
BEST PRACTICES 16
Sodium Chloride
A. Add one bed volume solution of 15% NaCl to the vessel and allow it to soak for 240 minutes. If the
temperature of the solution can be raised up to 80 ° C (176 ° F), the soak time can be reduced to 120
minutes.
B. Fast rinse the bed for 1.5 bed volumes. If hardness is still leaking above set point, repeat step A above.
C. If hardness leakage after step B is acceptable, proceed with a 90-minute acid regeneration cycle to fully
covert the resin to H+ form.
For best performance, there should be zero oil in feed solutions to the ion exchange resin bed.
Cleaning resins fouled by oil is extremely difficult. If resin is heavily fouled, it may be impossible
to clean them sufficiently to make them suitable for ongoing use. The following procedure uses a
low foaming, non-ionic surfactant and is recommended for lightly fouled ion exchange resins and
inert polymers.
• Drain the unit and fill with a solution containing no more than 0.1% of surfactant. The
treatment is most effective if the solution is administered at approximately 104 °F (40 °C).
Using lower temperatures may produce considerable foaming. Note that it is important to use
surfactant that does not foul resin.
• Cleaning will be more efficient if air is introduced to the resin bed as this causes agitation
while the resin soaks in the surfactant solution. Agitation should continue for approximately
a half an hour.
• Following this, thoroughly backwash the unit and rinse in down-flow mode until the foaming
completely dissipates. Water temperature for the first part of the rinse is optimal at 104 °F (40
°C).
• Finally, thoroughly regenerate and rinse the resin before proceeding to the next service cycle.
Inspecting, sampling and cleaning the resin regularly can prevent the accumulation of
contaminants and severity of resin fouling. This, in turn, will help optimize performance and
prevent permanent degradation of the resin.
BEST PRACTICES 18
Abbreviations
BV Bed volume
BV/h Bed volume per hour
C Celsius
cm Centimeter
F Fahrenheit
ft3 Cubic foot
ft -R
3
Cubic foot of resin
g/L Grams per liter
g/L-R Grams per liter of resin
in Inch
L Liter
lb/ft3 Pound per cubic foot
lb/ft -R3
Pound per cubic foot of resin
LPM Liters per minute
LPM/L-R Liters per minute per liter of resin
L-R Liter of resin
mg/L Milligrams per liter
min Minute
mL Milliliter
mL/L-R Milliliters per liter of resin
MSDS Material safety data sheet
oz Ounce
oz/ft -R3
Ounces per cubic feet of resin
ppm Parts per million
SAC Strong acid cation
SBA Strong base anion
USG United States gallon
USGPM United States gallons per minute
USGPM/ft -R 3
United States gallons per minute per cubic foot of resin
USG/ft3-R United States gallons per cubic foot of resin
WAC Weak acid cation
w/v Weight per volume
BEST PRACTICES 20
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