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PUROLITE SERVICE BULLETIN
D I S I N F E C T I O N T R E AT M E N T P R O C E D U R E S
IRON (AND MANGANESE) FOULING
ORGANIC FOULING
OIL FOULING
THE FOULING OF ION
EXCHANGE RESINS AND
METHODS OF CLEANING
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INDEX
INTRODUCTION
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D I S I N F E C T I O N T R E AT M E N T P R O C E D U R E S
Page 4-5
IRON (AND MANGANESE) FOULING
Page 6-7
Page 1
ORGANIC FOULING
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OIL FOULING
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INTRODUCTION
Most types of ion exchange resins can become polluted or
contaminated with suspended solids. Precipitations can occur
as a result of changes in pH, and/or concentration of relatively
insoluble salts. Also adsorption or ion exchange of other species
which are not easily removed by the normal regeneration
procedures can cause gradual accumulation and fouling of the
resin.
It should be emphasised that regular cleaning treatments can
prevent accumulation of fouling and therefore extend resin life.
Increased quantities of regenerant and increased frequency (and
elevated temperatures) of regeneration can reduce fouling, by
preventing contaminants from gaining a permanent hold.
It is good operating practice to ensure that all resin in the ion
exchange units is regularly contacted with sufficient regenerant
and is subject to regular cleaning procedure.
If, in spite of these precautions, deterioration in plant performance is experienced, the following can be the major causes:1
Loss of resin from the operating units.
Change in feed analysis. If the concentration of ions to be
removed is increased, it follows that throughput will be
reduced proportionally.
Faults in the operating process; incorrect conditions of
regeneration; failure to operate to plant instructions.
Malfunction of the plant engineering hardware
Resin pollution or degradation.
Of the above, (4) is the hardest to diagnose. Under (2) it is good
practice to check the feed analysis regularly and adjustments
may then be made to plant operation to accommodate any
changes. It is also relatively easy to check (3) on backwash procedures, rinse volumes and regenerant concentration to ensure
all functions are being operated correctly. If (1), (2), (3) and (4)
check out satisfactorily then a sample of resin should be examined.
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Resin Sampling
Evaluation of resin and the conclusions will depend on how the
sample is taken. It is preferable to ensure that the sample used
for testing is representative of the bulk from which it was taken,
or if this is not thought to be desirable or possible, the method
used to obtain the sample should be supplied to the analyst. To
obtain a representative sample of the resin contents of a mixed
bed, or other unit fitted with air mixing, the resin should be
mixed for 5 minutes and the sample taken after mixing. Where
there is no mixing facility, beds are generally in the classified
state as a result of regular backwash operation. Depending on
the mode of regeneration and service, pollution of a surface
sample can vary significantly and both the content of pollution
and resin grading can be un-representative. Hence it is necessary to obtain multiple samples at different bed depths and
remix, or obtain a core sample and mix before submission of a
sample for analysis.
Procedures for Cleaning
Various procedures can be employed to clean fouled resins
depending upon the nature of the foulant. These procedures are
detailed in this publication.
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D I S I N F E C T I O N T R E AT M E N T P R O C E D U R E S
INTRODUCTION
FORMALDEHYDE
Under certain conditions when contaminated water sources in
particular are being fed to ion exchange systems the resins may
become fouled either with bacteria or algae.
If formaldehyde is to be used as disinfectant the following
procedure should be followed:-
Where contamination of resin beds is observed one of the following procedures can be considered:
PERACETIC ACID
Peracetic acid, a derivative of hydrogen peroxide, displays a very
wide bandwidth of attack against microbes. Research has shown
that peracetic acid will be used to an ever increasing degree in
the field of human medicine due to its bacterial, fungicidal, sporicidal and anti-virus action.
Because of the wide spectrum of attack peracetic acid has been
shown to be very suitable as a wide bandwidth disinfectant for
deionsers. (Result of work done by Degussa Technical
Applications Department in conjunction with Chemiewerk
Homburg). Using a peracetic acid solution of strength 0.2% (in
water, with a reaction time of one hour), - a slime concentration
of 104 - 105/ml- including mould-was reduced to almost zero. The
short rinsing time after using peracetic acid is of importance
(typically about 45 minutes or 10-15BV).
In addition to the excellent disinfection action, peracetic acid
(according to experiments) has a minimal effect on the ionexchange properties of cation or anion resins.
Make up 3BV* of formaldehyde solution containing 0.5%
formaldehyde. Commercial formaldehyde (called formalin)
contains 40% formaldehyde and should therefore be diluted
approximately 80 times. Alternatively arrange the regenerant
injection system to provide a solution of injection strength
0.5%. The ion exchange plant manufacturer will provide
advice as to how this can be accomplished.
Inject 1BV of disinfectant at a flow rate of 5BV/h discharging
to drain.
If possible, drain down the unit to a level about 50mm above
the resin surface.
Inject a second BV of disinfectant at the same rate and retain
in the unit for a period of at least eight hours and preferably
in the unit overnight. Formaldehyde should be detectable by
smell at any drain valve.
Flush the unit to drain using raw water until no formaldehyde
is detectable at the drain by Schiffs Test.
Regenerate the resins TWICE (double regeneration) and
return the unit to service.
*1BV = 1 litre per litre of resin.
If peracetic acid is used as a disinfectant the following procedure
should be followed for both cation and anion resin.
Ensure anion resins are fully exhausted as peracetic acid
performs best at a pH below 8.
Make up one bed volume (BV)* of peracetic acid solution
containing 0.2% peracetic acid.
Inject 1BV of disinfectant at a flow rate of 5BV/h, with
displacement discharged to drain.
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 5BV/h, followed by a fast flush for 30 minutes.
Regenerate the resins once and return the unit to service.
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D I S I N F E C T I O N T R E AT M E N T P R O C E D U R E S
SODIUM HYPOCHLORITE
Availability
The most convenient packout of sodium hypochlorite is in the
form of small carboys/containers.
Preparation
For resin sterilisation a 1% available chlorine solution should be
used. This is obtained by diluting the commercially available
hypochlorite.
Treatment Procedure
The column should be regenerated with brine before
treatment in order to convert all resin to the exausted form (a
double or triple regeneration is often required). It
should be ensured particularly that cation resin is fully
exhausted before treatment so that there is no possibility of
production of chlorine gas.
The minimum volume of solution required to treat the bed is
3 bed volumes (i.e. 3 times the resin volume installed in the
unit).
The first bed volume should be passed through the bed at
normal regeneration flow rate or approximately 4 bed
volumes per hour (4BV/h).
A portion of the second bed volume should be retained in the
bed, but for no more than 2 hours.
The third bed volume should be passed through the bed at
the same rate as the first bed volume.
The sodium hypochlorite should now be displaced at a rate
of approximately 4BV/h with softened water and then rinsed
thoroughly to drain to remove any trace of sodium hypochlorite. At least 8-10 bed volumes will be required.
The resin should be triple regenerated before returning to
service.
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Caution
It should be noted that this form of treatment may cause slight
de-crosslinking of the resin matrix and therefore frequent treatments are not advised.
The procedure is not recommended for phenolic, polycondensation, and chelate resins.
In the case of anion resins, the oxidising effect of the sodium
hypochlorite is on the amine groups and therefore disinfection in
sodium hypochlorite should only be considered in extreme cases
and then only on a once off basis.
Please note:
Suitable safety precautions should be taken when using sodium
hypochlorite and drains into which the waste is to discharged
should be free from acids or other chemicals which may react
adversely with the dilute hypochlorite discharge.
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IRON (AND MANGANESE) FOULING
INTRODUCTION
SODIUM DITHIONITE TREATMENT
Iron can be present in several different forms in water. For example in the case of un-aerated borehole water iron can be present
in the ferrous state (Fe++) but on oxidation it is converted into the
ferric form (Fe+++).
Sodium dithionite is a powerful reducing agent and when applied
to an iron fouled resin bed will reduce any ferric iron present to
the soluble ferrous form. Thus the bed can be freed from iron
during a normal aqueous cycle.
Iron can also be complexed with organic matter; in which case it
is present as an anionic complex.
We would recommend the following procedure for applying the
sodium dithionite to a resin bed :-
Normally iron present in the ferric state is removed by cation
resin operated either in the sodium or hydrogen forms.
The sodium dithionite should be added to water (and not the
reverse) so as to form a 4% solution.
In the case of hydrogen form cation resin representing the first
stage of a demineralisation system the iron is removed from the
water but eluted on regeneration with mineral acid. With softening resin the situation is different, as the ion exchange resin
removes the iron from the water but the regeneration procedure
using 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.
Caution should be shown when mixing the sodium dithionite
because strong fumes of an obnoxious nature are evolved
during the mixing process. Sufficient solution should be
mixed so that when applied to the resin bed there is sufficient
to fully immerse the whole of the resin. The resin should be
agitated so that the sodium dithionite solution is evenly
distributed throughout the bed.
In the case of iron being present as organo/iron complexes the
complex is present as an anion and is therefore removed from
solution by the anion resin.
Because the anion resin is being regenerated with caustic soda,
whilst the organic matter may be substantially removed each
regeneration cycle, the iron is retained on the resin. The accumulation of iron on the resin causes the anion resin to become
iron fouled.
It is recommended that where the iron content of a water is higher than 0.5ppm some form of pre-treatment is used in order to
reduce the iron level down to less than 0.1ppm.
Air should not be used for agitation purposes as this will tend
to oxidise the sodium dithionite.
The dithionite should be allowed to remain in contact with
the resin bed for a minimum of 3 hours but 6 hours if possible.
After this period drain and rinse the unit thoroughly in a
downflow fashion after pressuring the unit and then backwash
for a full 30 minutes in order to remove any extraneous matter.
After this last procedure the unit should be regenerated in the
normal way prior to it being returned to service.
Because of the relative instability of sodium dithionite solution
a method utilising sodium tripolyphosphate has been found
to be even more effective than using sodium dithionite alone.
Remedial Action
Cation Resin
When using sulphuric acid constantly while iron is present in the
feedwater some accumulation of iron on the resin might take
place causing a reduction in performance.
In these cases, treatment with hydrochloric acid should be considered providing the internal construction of the units and attendant pipe work make this possible.
In the case of accumulation of iron on base exchange softening
resin, again either hydrochloric acid or sodium dithionite treatment may be considered.
In this instance the solution should be made up of 2%
sodium dithionite 2% sodium tripolyphosphate. The resultant
solution retains its iron removal power for a period of up to
sixteen hours because of its greater stability.
In instances where a preventive procedure may be considered
we would recommend the addition of a 1 gram of sodium
dithionite to every 100 grams of sodium chloride used during
the regeneration sequence.
However, we would emphasise that the same precaution
should be taken in both the preventing of oxidation of the
sodium dithionite by addition immediately prior to brine
injection and also in the method of addition to brine solution.
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IRON (AND MANGANESE) FOULING
HYDROCHLORIC ACID TREATMENT
The general characteristics of sodium dithionite together with
the precautionary procedures are as follows:Characteristics of sodium dithionite
Sodium dithionite will decompose under the influence of heat or
moisture. For this reason sodium dithionite should be kept in
sealed watertight containers and stored in a cool dry place.
Under such conditions this material can be stored over a prolonged period with negligible loss in activity. Care should be
exercised in handling sodium dithionite since, on contact with
water, this product decomposes quite rapidly forming gases
which can ignite spontaneously.
For this reason Sodium Dithionite is classified as a flammable
solid and is shipped under the appropriate caution label.
Because of the above mentioned, any material which is spilled
should be promptly cleaned up and the site washed with copious
amounts of water. Partially used containers represent a definite
fire hazard.
When fighting a sodium dithionite fire the burning material
should be deluged with water since too little water may be worse
than none at all. Carbon dioxide and dry fire extinguishers are
valueless since the product provides for its own oxygen for combustion.
Caution
Full details of the recommended procedure for storing and handling sodium dithionite should be obtained from the supplier and
these recommendations strictly adhered to so as to ensure full
compliance with local Health and Safety Regulations.
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In many instances it is not possible to treat softening resins with
hydrochloric acid in situ because of the materials of construction of the softening unit.
However, where it is possible, 6% hydrochloric acid should be
utilised and three bed volumes applied retaining the middle bed
volume in contact with the resin for a period in excess of two
hours (warming to 40C is beneficial).
The resin should then be regenerated twice with 10% brine solution, before putting back into service.
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ORGANIC FOULING
INTRODUCTION
It is well known that anion resins are susceptible to fouling by the
humic and fulvic acids sometimes found in surface waters.
These organic species, because of the relatively large molecular
weights, become trapped within the resin matrix (to a greater or
lesser degree depending upon the resin) and specific procedures
have to be employed to cause recovery of the original ion
exchange properties of the resin.
Iron/Organic Complexes
This subject is covered to some extent in the section on iron
fouling.
Occasionally the presence of iron is detected on the anion resin.
This can arise from an iron/organic complex being present in the
raw feed water.
The symptoms of organic fouling include long rinse requirements, poor capacity and, in the case of strong base resins,
higher silica leakage.
In these cases, it is advisable to consider treatment of 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.
Treatment
The most common forms of treatment involve the use of brine
solution; the procedure is as follows :-
It is extremely important that all traces of hydrochloric acid are
removed from the unit before introduction of the caustic soda
regenerant.
The resin should be treated at the end of the normal
exhaustion cycle.
It is important to ensure that the materials of construction are
suitably resistant to hydrochloric acid.
Three bed volumes of 10% w/v brine solution containing 2%
w/v caustic soda should be prepared.
One bed volume should be introduced into the ion exchange
unit at a flow rate not exceeding 2 BVs per hour followed by
a second bed volume - this second bed volume should be
retained in the unit for as long as possible, but at least 4
hours. Some agitation, if possible, should be employed
periodically 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 per hour
and the resin thoroughly rinsed with clean water until free
from brine.
The resin should be subject to at least two complete
regeneration cycles before being put back on line.
N.B. Brine at minimum 35C should be employed or preferably as
high as 60C so as to produce a better organic elution effect.
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OIL FOULING
CLEAN UP OF OIL FOULED RESIN
Introduction
The cleaning of resins fouled by oil is extremely difficult. If the
resins are heavily fouled it may be impossible to clean them up
sufficiently well in order to make them suitable for ongoing use.
However the following procedure is recommended for lightly
fouled ion exchange resins and inert polymers.
Procedure
The procedure uses a low foaming nonionic-surfactant.
Initially, the fouled resin should be thoroughly backwashed,
the unit drained and then filled with a solution containing no
more than 0.1% of surfactant.
The treatment is more effective if the solution is administered
at approximately 40C. Using lower temperature may produce
considerable foaming.
More efficient cleaning action will result if air is introduced to
the resin bed causing agitation while the resin soaks in the
surfactant solution. Agitation should be continued for
approximately half an hour. Following this the unit should
again be thoroughly backwashed and rinsed downflow until
foaming disappears completely. Here again it is helpful if the
first part of the rinse utilises water at approximately 40C.
The resin should then be thoroughly regenerated and rinsed
before proceeding to the next service cycle.
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Page 2
SALES OFFICES & BUSINESS CENTRES:
U.S.A.
The Purolite Company, 150 Monument Road, Bala Cynwyd,
Philadelphia PA 19004.
Telephone: (1) 610-668-9090, Toll Free: 800-343-1500,
Telex: 291718, Telefax: (1) 610-668-8139.
Texas
The Purolite Company, 1700 West Loop South, Suite 740,
Houston, TX 77027.
Toll Free: 800-562-6488, Telefax: (1) 713-627-7890
California
The Purolite Company, 22632 Golden Springs Drive, Suite 190,
Diamond Bar, CA 91765.
Telephone: (1) 909-396-5253, Telefax: (1) 909-396-5258
MEXICO
Purolite International, S.A. De C.V., World Trade Center,
Montecito 38 Piso 33-19, Mexico City, D.F. 03810.
Telephone: (52) 5-488-0905, Telefax: (52) 5-488-0906
CANADA
The Purolite Company, 625 Wabanaki Drive, Unit #2, Kitchener,
Ontario N2C 2G3.
Telephone: (1) 519-896-6674, Toll Free: (1) 800-461-1500
Telefax: (1) 519-896-6679
UNITED KINGDOM
Purolite International Limited, Kershaw House, Great West Road,
Junction with Lampton Road, Hounslow, TW5 0BU.
Sales - Telephone: (44) 181-570-4454, Telefax: (44) 181-572-7726
European Marketing - Telephone (44) 181-577-1222,
Telefax: (44) 181-577-1136
GERMANY
Purolite Deutschland GmbH, Harkortstrasse 25, 40880 Ratingen.
Telephone: (49) 2102-46033, Telefax: (49) 2102-443663
FRANCE
Purolite International SARL, 34 Avenue Matignon, 75008 Paris.
Telephone: (33) 1-42-564563, Telex: 648856, Telefax: (33) 1-45-633826
BELGIUM
Purolite Benelux, Industrieweg 11 - Zinkval, 2630 Aartselaar (Antwerp).
Telephone: (32) 3 -870-7298, Telefax: (32) 3-870-7299
SPAIN
Purolite Iberica S.A., Parc Tecnologic del Valles, Centre
Empreses Noves Tecnologies, 08290 Cerdanyola del Valles (Barcelona).
Telephone: (34) 93-582-0266, Telefax: (34) 93-582-0268
EGYPT
Purolite International Middle East, LCC
12 Obour Gardens, 5th Floor, App. No. 55, Saleh Salem Street,
Nasr City, Cairo.
Telephone: (20) 2-4031969, Telefax: (20) 2-4021478
SWEDEN
Purolite Nordiska AG, Hjdrodergatan 5, 21 239 Malm.
Telephone: (46) 40-292130, Telefax: (46) 40-292232
ITALY
Purolite International S.r.l., Viale Coni Zugna 29, 20144 Milan.
Telephone: (39) 02- 481-8145 Telefax: (39) 02-4801-2359
ROMANIA
Purolite Romania, International Business Centre 'Modern',
34-36 Carol I Blvd, 5th Floor, Bucharest.
Telephone: (40) 1-250-5053/5028 Telefax: (40) 1-250-5999
POLAND
Radus Spolka z o.o., ul Przebendowskich 33, 81-543 Gdynia.
Telephone: (48) 58-6248979/58-6649609/58-6649617,
Telefax: (48) 58-6248118
CZECH & SLOVAK REPUBLICS
Purolite International, Nad Mazankou 17, 182 00 Prague 8.
Telephone& Telefax: (420) 2-6881086/2-90010330
RUSSIA
Moscow - Head Office
Purolite International, 10th Floor, 36 Lyusinovskaya Street,
Moscow 113093.
Telephone: (7) 502-2222120 (satellite/ (7) 095-5648120
Telefax: (7) 502-2222121 (satellite)/ (7) 095-5648121 (7) 0957455047.
St. Petersburg
Purolite Interntional Limited, 12A Tabovskaya St,
St. Petersburg, 192007.
Telephone: (7) 812-3278530, Telefax: (7) 812-3279079
UKRAINE
Purolite International Limited, 2 Korolenko Street,
Dnepropetrovsk 320070.
Telephone: (38) 0562-320065/66, Telefax: 0562-320067
KAZAKHSTAN
Purolite RH Limited, 240 Dostyk pr., Almaty 480051
Telephone (7) 327-5811745/2641234, Telefax: (7) 327-5811744
CHINA
Purolite (China) Limited, Chenguan County, Dequin City,
Xhejiang Province, 313200.
Telephone: (86) 572-8422908/8422819, Telefax: (86) 572-8423954
SINGAPORE
Purolite International (Singapore) PTE Limited,
32-04 The Concourse, 300 Beach Road, 199555.
Telephone: (65) 297-0889/297-1453, Telefax: (65) 297-1986
TAIWAN
Purolite International, 16F-2, No. 191, Fu-hsing N. Road, Taipei.
Telephone (886) 2-546-7078, Telefax: (886) 2-546-7069
KOREA
Purolite International (Korea) LLC, Dae Yeon Bldg., Suite 403,
943-30 Daechi-dong, Kangnam-gu, Seoul.
Telephone: (82) 2-3453-7062/7063, Telefax: (82) 2-3453-7064
Web Site. http://www.purolite.com
The Purolite Company and Purolite International Limited have one of the most complete ranges of ion exchange resins worldwide. For further information please
contact your local Purolite office.
All suggestions and recommendations given concerning the use of Purolite products are based on tests and data believed to be reliable. However, as
Purolite cannot control the use of its products by others, no guarantee is either expressed or implied by any such suggestion or recommendation by
Purolite nor is any information contained in this bulletin to be construed as a recommendation to infringe any patent currently valid.
Produced by Hamilton-Rio Design, Epsom, U.K.
PSB/101/5.96
Printed in England
