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A Practical Guide to Investigating Operating Problems on
In-situ Regenerated Polishing Mixed Beds
Brian Windsor and David Hayhurst
ABSTRACT
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ThIS paper looks back at the historical problems that are stili being frequently encountered on polishing mixed beds, ir
Ihese bemg typically apparent as very long rinse times to quality after regeneration, or consistently poor treated waler 3.
quality (high conductivity). Over 95 % of mixed bed problems are caused by one or more problems in the following
four areas of regeneration: poor resin separation, inadequate slow displacement rinsing, poor drain cont rol prior to
remixing, and air blowers. This article is designed to help plant chemists and operators in troubleshooting mixed bed A
problems by Identifying the issues involved, as well as to give all readers a better understanding of polishing mIXed Sl
bed operation. dt
INTRODUCTION
Most ion exchange issues are rarely due to problems with
the resins themselves, but are primarily due to aspects of
the operation of the plant. The units which prOVide the
biggest challenge to operators of make+up deminerailsa+
1IOn plant are polishing mixed beds. These problems were,
in the main, identified twenty to thirty years ago in the
power industry.
Recent years have seen a recurrence of these issues, with
customers requiring on site support for troubleshooting
mixed bed problems more frequently than for any other
type of unit. In the vast majority of cases the problem of
poor quality is due to one or more of the four problems
outlined below, and thus thiS article is deSigned to serve
as a troubleshooting refresher to plant chemists and oper+
aters.
Mixed Bed Performance
When treating partially demineralised water which has
passed through a cation and anion stage or reverse osmo-
sis plant, the polishing of this water should result In a final
treated water quality that complies with that defined in
at all times.
ConductiVity IS very temperature sensitive so any meas-
urement needs to be with a temperature compensated
Instrument and any silica guarantee can only relate to
reactive silica. Non-reactive (collOidal silica) is not fully
removed by conventional mixed bed Ion exchange resins.
C 2012 by Waesseri GmbH. All rights reserved.
282
Conductivity at 25 "c {I-IS , cml1 0.06-0.1
$odIum !mgL-'j < 0.01
Reactive silica
[mg L-Ij
< 0.02
Table 1
TyptCal make-up plant pollsl1ln9 mixed bed quality.
To achieve thiS quality polishing mixed beds should never
be run to exhaustion and the service cycle should be
terminated on time or throughput well before any increase
in conductiVity or reactive silica is seen. This way the
resins are maint ained in optimum condition and almost
fully regenerated, and this premature regeneration does
not add much to the operating costs of running the plant,
as the bulk of the costs is in the acid and caUstiC used in
the preceding cation and anion units.
REGENERANT INJECTION OPTIONS
While the valve arrangements are similar on all mixed bed
designs, some companies do carryout the regeneration
slightly differently. The biggest difference is often in the
regenerant injection stages.
The modern way of "1htrodUClng the regenerant, after sep-
arating the resin into Its cation and aOion components, is
to have the acid and caustic Inlection occurring
ously, WIth the caustic introduced from the top and the
aCid from the bottom and with both regenerants leaVing
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VIa the centre collection system located at the interface of
the two resin components. The slow (displacement) nnses
follow the same route.
Other systems are designed uSing the same regenerant
inJectton points but do not carry out the mjectlon Simulta-
neously. These designs usually introduce the caustic first
and have an upward water buffef"'flow through the cahon
component to stop caustic migration. likewise the caustic
nnse provides a downflow buffer dUring upward acid
inJectIOn. Another vanallon is where the caustic and acid
Injection are carned out totally separately, and here the
acid is introduced downflow through the centre collection
system.
All the above commonly encountered designs have been
successfully employed In achieving the water quahty
defined in Table 1. Regardless of the system used, this
article covers the main operating problems encountered
on polishing mixed beds employing in-Situ regeneratton.
provides a diagrammatic representation of these
alternative designs used in introducing regenerant.
(a) (b)
F"9Jre 1
AlternatIVe regenerant tntnxlucllon methods_
(a) SIITlUltaneouS acid/caUSlic regeneratIOn
(b) caustIC tn)ElCtlon with water buffer
(e) acid In,ectJon vIa centre system
MIXED BED REGENERATION CYCLES
(e)
Once the unit is taken off hne and the unit is isolated vnlet
and outlet valve closed) the first step IS a backwash,
Mixed beds should ideally have more than 100 % free-
board (space above the bed) and the backwash, intro-
duced into the bottom of the unit. leaves through a back-
wash strainer at the top (which also often acts as the inlet
distributor for the water In normal operation) . The back-
wash can have up to three functions.
Where the water is all derived from a preceding anion col -
umn, no solids should be present. Here the backwash is
reqUIred 10 decompact the bed, loosen the resin for better
regenerant contact and most importantly to separate the
intimately mixed resin Inlo its two separate components of
cation and anion resin. If the mixed bed uses a separating
inert of intermediate denSity, then the backwash will sepa-
rate the bed into the three components.
On some occasions return condensate IS introduced for
polishing and is mixed With the water from the anion col-
umn. The condensate can contam suspended solids and
in thiS case the backwash is also required to remove the
solids from the bed. Under these circumstances the back-
wash step is normally longer to ensure the bed Is clear of
solids.
After separallon the beds are allowed to settle and reform
Into the separate components. The bed settle step can
last 5 to 10 min depending on the volume and type of
resins used. Gel resins settle more quickly than macro-
porous resins.
The next stage IS regenerant injection utilizing any of the
routes described earlier in the paper. Acid regeneration
levels are typically between 50 and 70 g. L _1 , while caustic
regeneration levels are typically higher between 60 and
60 g L -, On some occasions systems are encountered
where the caustic IS warmed slightly. This tends 10 be
observed on older plants and was introduced to help in
the removal of silica from Ihe anion component. Today It is
rarely used unless the silica loading IS very high. The typi-
cal ragenerant flow rate is 2 to 4 bed volumes (BV) per
hour and the regenerant concentrations are tYPically 4 %
for caustic Injection and 5 % for acid injection for either
sulphuric or hydrochloric acids.
The slow (displacement) rinse is carried out at a similar
flow rate as the ragenerant injection and is deSigned to
remove the vast bulk of regenerant effiCiently. By usmg a
similar flow rate the rinse water follows the same path as
the regenerant from the distributor and hence good plug
flow would be expected to be achieved.
Having rinsed the bulk of the chemical from the two com-
ponents the resins must be remixed. This is done by first
draining down the water level to just above the bed and
then Introducing an air mix stage to mix the resins. The air
is normally supplied by separate low pressure air blowers
or occasionally via site air. The alf needs to be clean and
oit free; an air velOCity of around 110m
3
. m-
2
. h-
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IS
required within the unit and usually a pressure around
5 ""'.
Once remixed the unit IS refilled. Usually the Inillal fill IS via
the caustic distnbutor first so as not to disturb the bed and
then once the bed is well covered With water a higher lIow
rate IS used from the top of the unit to complete the filling.
283
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The final stage is a rinse to drain to achieve final quality.
This nnse is usually quite quick as any trace acid from the
cation resin IS removed by the anion component while any
caustic from the anion component IS collected by the
cation resin. Some plants have a rinse recycle stage to
reduce nnse water reqUirements further.
A typical mixed bed arrangement is illustrated In flgy[Q...Z.
~ water 0UIIet

, ... .. = = = r F = = ~ = ~
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Treated wat ... outlel
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TYPICal mIXed bed arrangement.
POOR MIXED BED PERFORMANCE
It IS very unusual for any ion exchange to be working per-
feelly and then suddenly begin to perform very badly.
When this type of catastrophic failure occurs. it IS usually a
relatively Simple problem. can normally be found very eas-
Ily and is usually due to a problem on lhe previous regen-
erallon. The recommended first action is to put the mixed
bed through a double regeneration to ensure the resin is
fully regenerated and the resins are both in the besl possi-
ble condition. Hopefully this will address the problem.
A double regeneration can be performed by carrying out
the full regeneration procedure twice (back to back). or to
qUicken the process, puttmg the unit Into regeneration and
284
after the chemical draw step, stopping the regeneration
and refilling the chemical measures. The chemical inJec-
tion step can Ihen be repeated and the unit allowed to
proceed through the remainder of the regeneration cycle.
The Important action dunng this double regeneration IS for
an expenenced operator who understands how the plant
works to check some of the basics. First, befOf8 starting
the double regeneration, check that the resin level IS cor-
rect (easy If there is a top sight glass) to make sure the unit
has not lost any resin. Lost resin can affect not only the
Unit's capacity between regenerations but also the inter-
face pOSItion after backwashing and the resin mixing
stage, all of which Will result in poor quality. The operator
should also check that the chemical measures are filling
correctly and the full amount of ragenerant IS bemg
applied during the chemical draw stage. The valve
sequences must be confirmed as correet and opening and
closing at the light time. In addition the air blower must be
working correctly, the air relief valve should not have lifted
and thus the lull air flow should pass to the vessel for resin
mixing.
Hopefully, when the regeneration cycle has been repeated
and if no issues have been Identified. the mixed bed Will
return on tine with no quality issues. If however the prob-
lems persiSt or if the problem has been a slow deteriora-
hon In performance. then a more detailed investigation is
required.
The major problems reported on mixed beds can mainly
be split into the folloWing categories:
- very long nnse times to quality
- poor water quality (high conductivity) at all times.
Dunng regeneratIOn there are four areas which can lead to
poor quality and over 95 % of mixed bed problems are
caused by one or a combination of the issues listed below.
Poor Resin Separ ation
Today the resin suppliers produce graded products of dif-
ferent denSity whereby mixed bed resin separation into
the two components on backwashlng IS achieved very
eaSily. It is cntlcal that the interface between the lighter
anion resin (on the top) and the heavier cation resin (on the
bottom) IS locateOin the correct poSItion. This is because
it IS impor1ant that the sodium hydrOXide (caustic soda)
used to regenerate Ihe anion component does not cootaC1
cation resin as it will convert it to the sodium form; likewise
It IS Important that the acid - usually either sulphuric acid
or hydrochloric acid - does not contact anion resm as rt
Will be converted to the sulphate or chlonde form depend-
Ing on the acid used. Of the two, anion contamination with
acid causes more long-term problems than a little caustic
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A Practical GUide , In II,. Ro CIted Po h 19 M xc::l 3eds PPCIUI
In cootact with cation resin. Therefore, when commiSSion-
ing a new resin charge it is usually impossible to get the
Interface exactly on the midpoint of the centre laterals and
so the recommendation IS that the lateral slightly favours
the cation resin (but is not buried in the cation!). This will
stili give very good performance as slight sodium contami -
nation of the cation IS not highly detrimental to perlor-
mance.
Obviously from this information operators should realise
that special care should be taken when !oading/commls-
SiOfling new mixed bed charges. Purolite have produced a
written guide to assist companies loading mixed bed
resins to ensure good performance.
All mixed beds should have a minimum of one Sight glass
located In line With the centre laterals so that operators
can check the interlace position. It is recommended that
when there is no resin In the unit, the poSition of the lateral
should be carefully drawn/marked on the sight glass to
show the position when the bed is full of resin. This
enables operators to check the position routinely and thiS
IS very important when there is a mixed bed quality prob-
lem.
If the Interface is too low and the bed has backwashed
correctly, then t he most likely cause Is loss of some of the
cation resin. While this must be investigated to find the
cause of the loss, short term the problem can be cor-
rected by adding some more bags of cation resin to the
bed and giVing the unit a double regeneratIOn. If the resm
loss IS small and results from minor damage to a centre
lateral Of bottom lateral, then it is possible to collect the
lost resin by putting a bag filter over the drain outlet to
recover the resin and to use the collected resin to top up
the bed regularly until a full repair can be accommodated.
ObviOUSly maJOf losses cannot be handled In this manner
and a full repa.1r must be undertaken.
Where lost anion resin is identified, i.e. the resin bed is low
but the cation interlace is In the correct poSition, then thiS
usually means ellher the backwash rate is too high. forCing
anion resin out of the column (or damaged top strainer), or
Ihere is damage at the centre lateral causing anion resin
loss during caustiC Injection and slow nnse.
If the Interface is too high, this can be due to resin comll'9
Into the bed from the preceding unit, but is more likely
caused by trapped anion within the cation component.
ThiS is where the backwash rate is too low (it usually
occurs in the summer with higher water temperatures) and
requires an Increased rate to expand the cation fully so
thai entrapped anion resin can escape.
If lhe backwash flow IS increased 100 much and the flow
rate falls, thiS is because the rate is too high and the lighter
anion resin has been pushed around the top strainer/ col-
--
lector cauSing blockage: therefore the rate needs reducing
a httle.
If however the backwash wor1<.s well and the resin inter-
face is in ItS correct position, then we need to look at other
likely causes.
Inadequate Slow Di splacement Rinsing
As we have seen, there are different routes used on mixed
beds for tnlroducing acid and caustic, the most popular
being Slmullaneous injection WIth the regenerant and slow
rinses leaving from the buried centre drain.
However. regardless of the system used there IS never a
conductiVity meter on the centre drain and the COnductiV-
Ity at the end of the slow nnse is not monitored. It should
be relatively low shOWing that all the regenerant chemIcals
have been washed from the bed. Normally the syslem Jusl
relies on the fact that suffiCient slow rinse has been Intro-
duced when Originally commiSSIoned. Unfortunately, col-
lecllonldlslnbulion systems do get blocked and flow rates
and pressures do change. So after haVlf'lg gone to all the
trouble of making sure the beds are perfectly separated to
stop contamtnalton, It would be counter-productive to
leave lots of regenerant in either component before remix-
ing!
ThiS has been found to be a common cause of quality
problems 00 many mixed beds, and on some occaSions, if
the laterals/nozzles are not too badly blocked, the Issue
has been addressed temporarily Just by extending the
slow rinse stage. A full inspection of distnbutors and col -
lectors to make sure they are clear and working correctly
can then be made when time allows.
To check thiS problem, take samples of the water leaving
the unit at the end of slow rinses and check the conductiV-
ity - t1 should be low, preferably less than 50 cm-
I
On
some units conductiVities exi l ing the centre drain at the
end of the slow rinse of over 1 000 cm-
I
have been
observed, resulting in major cross contamination after the
remixing stage!
Poor Drain Control Prior to Remixing
Over the last 30 years, Purolite have, like all other major
resin producers, spent considerable time producing better
mixed bed grades which separate more easily and in
some cases use lower backwash flow rates. Conversely,
they are a little more difficult to remix.
Therefore ensuring that the remiXing stage works periectly
IS highly cntlcal If operalors are 10 achieve a correctly
mixed resin charge to return to service.
285
PPCHlM Gu je to Illvest J.]tmg C :>c "8Ilog:mbl 5)fl In sllu RogcneTated Polishing M,xed Beds
~
Rather surprisingly perhaps, the height that the water 15
above the bed when starting the air mix IS very critical. II
should be only a few centimeters above the bed (3 to 4 in).
If It IS below the top of the bed, the air will not remix the
bed, and this is easily eVident by looking through the cen-
tre sight glass. However, the most common problem is
that the water height is too high for modern resins.
Some years ago, engineering companies would include a
separate drain down valve from the shell of the unit with a
strainer that ran to drain. This exactly controlled the height
of the water on dram down and when the line was no
longer pasSing water it would be clear that the water was
at the correct height for a full resin bed and the aIr blower
could be started 10 air miX the bed.
Today, this valve is rarely seen, as almost every company
has Ined 10 reduce costs by omitting this valve and
instead relying on setting the system up on commission-
ing with drain down via the centre dram and bottom drain
outlets and the control system keeping these open for a
certain fixed time. This will never work consistently over
the hfe of the mixed bed!
During the life of a mixed bed unit, laterals become
blocked, damaged. or replaced, valves are serviced or
replaced, resin types are changed and different grades
used. Water denSity also changes With temperature so
drain down can be a little slower in the winter. All of these
factors will mean that it is likely that too much water can
be left in the bed.
When there IS a httle too much water in the bed the air mix
always appears to go well With lots of movement and so
operators are usually pleased. In fact some operators start
the air blowers early as they know the mixing looks better
when there IS more water in the bed. Unfortunately, thOugh
the mix is better, when the air mix is stopped the reSin has
expanded into the full volume, and as resins are designed
to separate better, the cation resin is often much heavier,
particularly if you have a combination of a gel cation with a
macroporous anion resin. The cation Will fall very qUickly
and form a separate cation layer below the mixed portion
of the bed. With no anion resin present to mop up trace
aCid from the beads dunng the final rinse stage, the rinse
will become poor, very long and have an acid pH.
Measuring pH on the final rinse is therefore a good way of
identifying this issue.
Unfortunately. depending on the deSign. getting the water
height poSItion right on your bed can be very difficult I' you
have no top sight glass above the resin bedl
Some companies resolve thiS problem by extending the
air blower mixing stage after the dram down and then they
introduce another drain down before the end of the air
mul. ThiS locks the fully mixed resins in place when the
286
water level falls below the bed level and stops the second-
ary separation of the catton component.
Air Blowers
Earlier it was noted that a velOCity In the bed of around
110 m
3
. m-2 h- ' is required for good mixing and the air
blowers have to have sufficient head to blow this velocity
against the head of water and resin. Atr blower failures are
not uncommon, and problems like lifting relief valves due
to high back pressure will cause loss of flow.
Always check air blowers and maintain them in good con-
dition, and check for ptpework damage from the blowers
to the unit In case some air is being lost. All these have
been Identified on sites over the last 20 years as bemg the
cause of mixed bed problems.
A modern trend IS to use site air from compressors and
not to use dedicated blowers. However, this has also been
found to be a problem if the mixed bed demand for air
mixing (which is an Infrequent demand) COinCIdes With
other major demands on site, as it can lead to a poor mix
poor perlormance and is almost Impossible to identIfy as
the repeat regeneratIOn does not coincide and the mixing
works well.
CONCLUSiON
Hopefully thiS paper has given an insight to plant opera
tors/managers on troubleshooting mixed bed problems by
Identifying the issues the authors of this paper come
across as well as gIVen all readers a better understanding
a' polishing mixed bed operation.
While the paper was specific to In-Situ make-up mixed
beds, many of the points raised would also apply to exter-
nal regenerated umts. External regeneration however has
one other major issue which needs care. That is, during
transfer of the mixed resin from the regeneration vessels
the resin can easily separate in the service unit if the trans-
fer velocity is wrong for the given pipe size and more
importantly if the transfer water is not drained away imme-
diately from the service unit as the resin is transferred
back.
Paper presented at the Annual BIAPWS Symposium on
Power Plant Chemistry, ChUwell, Nottingham, UK, March
28-29, 2012.
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