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Dow
Liquid Separations
DOWEX
Ion Exchange Resins

DOWEX ion exchange resins for

HFCS deashing and polishing

Technical Manual
DOWEX ion exchange resins for HFCS deashing and polishing

Table of Contents Page

Corn Sweetener Processing _______________________________________________________________________1
Operating Guidelines _____________________________________________________________________________2
Typical conditions during syrup service _____________________________________________________________2
Regenerating deashing resins ____________________________________________________________________2
Regenerating DOWEX* 88 and DOWEX MONOSPHERE* 88 strong acid cation resins _______________________5
Regenerating DOWEX 66 and DOWEX MONOSPHERE 77 weak base anion resins _________________________7
Regenerating mixed bed polishers ________________________________________________________________9
Troubleshooting ________________________________________________________________________________11
Troubleshooting deashing systems _______________________________________________________________12
Troubleshooting mixed-beds ____________________________________________________________________17
Resin Properties ________________________________________________________________________________18
Pressure drop as a function of flow rate ___________________________________________________________19
Backwash expansion characteristics ______________________________________________________________21
Storage and Handling____________________________________________________________________________24
How to get more information on Dowex products and Dow support services______________________________25
Tables
Table 1 Suggested operating conditions for DOWEX deashing and mixed-bed polishing resins_______________2
Table 2 Recommended regenerants for DOWEX deashing and mixed-bed polishing resins _________________6
Table 3 Recommended quality of regenerants _____________________________________________________6
Table 4 Relative selectivity of DOWEX 88 for cations _______________________________________________7
Table 5 Typical resin properties for DOWEX deashing and mixed-bed polishing resins ____________________18
Figures
Figure 1 Sweetening-off deashing systems ________________________________________________________3
Figure 2 Comparing sweetening-off curves for dextrose deashing ______________________________________4
Figure 3 Backwashing deashing resins ___________________________________________________________4
Figure 4 Countercurrent vs. cocurrent regeneration _________________________________________________5
Figure 5 Cation and anion rinses ________________________________________________________________7
Figure 6 Weak base anion regeneration and rinsing _________________________________________________8
Figure 7 Series and recirculation rinsing __________________________________________________________8
Figure 8 Sweetening-off and regeneration of mixed beds _____________________________________________9
Figure 9 Rinsing and blowdown of mixed beds ____________________________________________________10
Figure 10 Resin mixing in mixed beds ____________________________________________________________10
Figure 11 Recycle rinsing of mixed beds __________________________________________________________10
Figure 12 Troubleshooting abrupt deashing problems - Short Cycles ____________________________________12
Figure 13 Troubleshooting abrupt deashing problems - Poor Syrup Quality _______________________________13
Figure 14 Troubleshooting abrupt deashing problems - High As-Is Color _________________________________14
Figure 15 Troubleshooting abrupt deashing problems - High After-Heat Color _____________________________15
Figure 16 Troubleshooting abrupt deashing problems - High Pressure Drop ______________________________16
Figure 17 Troubleshooting mixed bed polishers - poor syrup quality_____________________________________17
Figure 18 Pressure drop with DOWEX 88 resin_____________________________________________________19
Figure 19 Pressure drop with DOWEX 66 resin_____________________________________________________19
Figure 20 Pressure drop with DOWEX MONOSPHERE 88 and MONOSPHERE 77 resins___________________19
Figure 21 Pressure drop with DOWEX 88 MB resin _________________________________________________20
Figure 22 Pressure drop with DOWEX 22 resin_____________________________________________________20
Figure 23 Backwash expansion of DOWEX 88 resin_________________________________________________21
Figure 24 Backwash expansion of DOWEX MONOSPHERE 88 resin ___________________________________21
Figure 25 Backwash expansion of DOWEX 66 resin_________________________________________________21
Figure 26 Backwash expansion of DOWEX MONOSPHERE 77 resin ___________________________________22
Figure 27 Backwash expansion of DOWEX 88 MB resin _____________________________________________22
Figure 28 Backwash expansion of DOWEX 22 resin_________________________________________________23

*Trademark of The Dow Chemical Company

Corn Sweetener Processing
The use of DOWEX ion exchange resins in corn sweetener processing

Millhouse Starch Slurry Gelatinization Dextrinization Saccharification

Adsorbent Decolorization Vacuum Filtration

DOWEX* OPTIPORE* SD-2 Adsorbent Evaporation or Membrane Separation
(some systems) of Insolubles

Dextrose Side Deashing

DOWEX MONOSPHERE* 88
Cation Resin

DOWEX MONOSPHERE 77 Evaporation Isomerization

Anion Resin (some systems)

Fructose Side Deashing

Adsorbent Decolorization
DOWEX MONOSPHERE 88
DOWEX OPTIPORE SD-2 Adsorbent
Cation Resin

DOWEX MONOSPHERE 77
Evaporation 42% Fructose Product
Anion Resin

Mixed Bed Polishing Separation

DOWEX 22 DOWEX MONOSPHERE

80-90% Fructose Blending
Anion Resin 99 Resin
DOWEX 88MB
Cation Resin Mixed Bed Polishing
80-90% Glucose
DOWEX 22
Anion Resin
DOWEX 88MB
Raffinate Cation Resin
(Recycled in Process)

Evaporation

55% HFCS Product

1
Operating Guidelines they operate must be maintained
within certain parameters. In particu-
Typical conditions during syrup lar, DOWEX products vary in their
service temperature sensitivity. Table 1 pro-
vides data on suggested operating
To obtain optimum performance and conditions such as maximum syrup
long life from DOWEX ion exchange temperatures.
resins, the conditions under which

Table 1 – Suggested operating conditions for DOWEX deashing and mixed-bed polishing resins

DOWEX 88 DOWEX DOWEX 66 DOWEX DOWEX 88 MB DOWEX 22

strong acid MONOSPHERE weak base MONOSPHERE strong acid strong base
cation 88 anion 77 cation anion
strong acid weak base
cation anion

Maximum syrup 200° F 200° F 140° F 140° F 200° F 115° F

Temperature 93°C 93°C 60°C 60°C 93°C 46°C
(H+ form) (H+ form) (FB form) (FB form) (H+ form) (OH- form)

Bed Depth, 36 inches 36 inches 36 inches 36 inches 36 inches 36 inches

(minimum) 91 cm 91 cm 91 cm 91 cm 91 cm 91 cm

Regenerant 6-7 lbs/cu. ft. 5-6 lbs/cu. ft. 5-6 lbs/cu. ft. 4-5 lbs/cu. ft. 6-7 lbs/cu. ft. 4-5 lbs/cu. ft.
Level 96-112 kg/m3 80-96 kg/m3 80-96 kg/m3 64-80 kg/m3 96-112 kg/m3 64-80 kg/m3
(100% basis)

Regenerant 7% HCl 7% HCl 4% NaOH 4% NaOH 7% HCl 4% NaOH

Concentration

Regenerant 200°F 200°F 140°F 140°F 200°F 115°F

Temperature 93°C 93°C 60°C 60°C 93°C 46°C
(max.)

Substitute 5% Na2CO3 5% Na2CO3 7% Na2CO3

Regenerants @ 7-8 lbs/ft3 @ 6-7 lbs/ft3 @ 5-6 lbs/ft3
(112-128 kg/m3) (96-112 kg/m3) (80-96 kg/m3)

5% NH4OH 5% NH4OH
@ 5-6 lbs/ft3 @ 4-5 lbs/ft3
(80-96 kg/m3) (64-80 kg/m3)

When to regenerate deashing breakthrough, is determined by mea- Regenerating deashing resins

resins suring the conductivity and/or the pH While specific configurations of
of the syrup as it leaves the primary deashing units vary in the industry,
In a double pass system, when the
deashing anion unit. When the con- the basic principles involved in
primary deashing unit becomes
ductivity increases to around 20-30 regeneration are relatively standard.
exhausted to the point where syrup
micromhos per centimeter or the pH This section offers a broad overview
quality drops below an acceptable
drops to around 4.5, it is generally of the process. Specific procedures
level, it is taken off-line and replaced
time to regenerate the unit. may vary, and additional steps may
with the secondary unit. An off-line,
regenerated unit then becomes the be required, depending on the
secondary unit. This point, called design and operation of your system.

2
Never use oxidizing agents such as Sweetening-off waste. The use of deionized (con-
nitric acid, perchlorates, or hydrogen When the on-line deashing unit densate) water is not essential for
peroxide with ion exchange resins. reaches breakthrough, the syrup sweetening-off; however, hard (raw)
The reaction can cause slight to feed is discontinued and water (gen- water will further exhaust the resins.
severe degradation of the resin, pos- erally at the process flow rate) is A rule of thumb for water usage is to
sibly producing explosive reaction used to push the syrup off the resin use the water of highest conductivity
products. Also, the use of H2SO4 to bed (Figure 1). The full strength for sweetening off and save the best
regenerate cation resins is typically syrup exiting the bed during the early water for regeneration final rinse.
discouraged because CaSO4 can stage of sweetening-off goes forward Due to better resin kinetics,
precipitate in the ion exchange resin. in the process. On the dextrose side, DOWEX MONOSPHERE ion
Since the performance of ion when sweetwater (diluted syrup) exchange resins sweeten-off more
exchange resins is dependent on starts to exit the bed, it can often be efficiently, resulting in 30-40% less
proper regeneration, it is important to put back into the process. With fruc- sweetwater and 40-60% less waste-
closely monitor your regeneration tose side deashing, however, sweet- water generated per cycle on both
procedures. For example, routinely water is not generally recycled the dextrose and fructose sides.
have your quality assurance lab because it contaminates the glucose Figure 2 shows the shorter, steeper
check regenerant quality and con- stream with fructose. When the dis- sweetening-off profile of a DOWEX
centration. Also be sure that meters, solved solids concentration of the MONOSPHERE 88 and 66 resin pair
pumps, and valves are working and syrup gets down to a fraction of a compared with conventional deash-
are maintained properly. percent, the effluent is switched to ing resin pair.

Figure 1 – Sweetening-off deashing systems

Water

Cation Anion
Resin Resin

Full Strength
Syrup Process

Sweet Water

Waste

3
Figure 2 – Comparing sweetening-off curves for dextrose deashing
This graph tracks the dextrose side
cation-anion effluent during sweetening-off.
Notice the shorter, steeper profile of
3.0 360
DOWEX MONOSPHERE resins. More effi-
cient rinsing and longer service cycles each
2.5 300 lead to significant reductions in sweetwater
and wastewater.
2.0 240

grams ds/liter
Lbs ds/gal

1.5 180
DOWEX
1.0 MONOSPHERE Standard resins 120
resins
0.5 60

0 0
0 0.4 0.8 1.2 1.6 2.0
Bed Volumes

Backwashing decreased when using colder water.

The next step is backwashing, fluidiz- Backwash expansion curves for
ing the bed by pumping water upflow. DOWEX resins are provided on
By lifting and separating the beads, pages 21-23 to help you determine
backwashing aids in thorough clean- the expansion of your beds at a
ing of the bed and also allows the given temperature and flow rate.
beads to reclassify in the bed, improv-
ing flow distribution. Backwashing
removes residual syrup, resin fines,
microorganisms, and other matter to
allow good regenerant contact and Figure 3 – Backwashing deashing resins
flow through the bed (Figure 3).
A minimum 50% expansion of the Waste
Waste
bed volume during backwashing is
recommended; 100% expansion is
even better.
Unscreened backwash outlets are
most effective because they allow the Expanded
contaminants to freely exit the bed;
however, backwash expansion must
be monitored carefully to ensure that Cation Anion
resin beads don’t escape the bed. Settled Resin Resin
This is particularly true with anion
resins, which are less dense than
cation resins.
Problems sometimes occur when
the water temperature is lower than
normal because colder water will Deionized Deionized
expand the resin bed more at a given Water Water
flow rate. Flow rates should be

4
Regenerating DOWEX 88 and Figure 4 – Countercurrent vs. cocurrent regeneration
DOWEX MONOSPHERE 88
strong acid cation resins Cocurrent Countercurrent
Two methods of regenerating are in
common use: cocurrent (in the same 7% HCI Waste &
Acid
direction as syrup flow) and counter- at 5.7 Recovery
current (opposite syrup flow). We Ibs/cu. ft.
recommend countercurrent cation
regeneration at normal regenerant Na Na Na Na Na
loads, particularly for single pass sys- Ca Mg Ca Mg Ca Ca Mg Ca Mg Ca
tems, because it results in lower Na Na Na Na Na
sodium leakage when the unit is
returned to service. Salt "heel"
Since 100% regeneration of the
resin is not economical, a small per- Waste & Acid Recovery 7% HCI at 6 Ibs/cu. ft.
centage of exchange sites will still be
occupied by salts. With cocurrent
regeneration, these residual salts
(called the salt heel) end up at the Cation resin regeneration Acid contact time is also important
bottom of the bed and can result in efficiency to regeneration efficiency. We rec-
higher than acceptable sodium leak- Prudent operation of ion exchange ommend a minimum of 45 minutes
age when the bed is returned to systems is a trade-off between appar- acid pumping time to allow mass
syrup service (Figure 4). ent short-term savings and long-term action to take place.
With countercurrent regeneration, operating costs. The most important Regeneration efficiency is also
the salt heel ends up at the top of the factor in cation resin regeneration effi- dependent on the purity of the acid
bed, and even if the syrup picks up ciency is the acid concentration. and dilution water. Table 3 gives the
some of this salt, it will be removed Since the resin’s active sites have a minimum purity requirements for
by the more fully regenerated resin greater affinity for the salts they have regenerants commonly used with
lower in the bed. Salt leakage due to picked up than for hydrogen ions, a DOWEX resins.
cocurrent regeneration is more pro- sufficient acid concentration is Regeneration efficiency is reduced
nounced in single pass systems than required to overwhelm and drive the by increased amounts of calcium and
in double pass systems (at equiva- salts off these sites. Technically, this magnesium loaded on the resin
lent acid loads). is called mass action. Even though because of the high selectivity of the
With both methods of regenera- 40% over the stoichiometric amount of cation resin for these salts (Table 4).
tion a build-up of calcium and/or acid will not completely regenerate the Extra acid (120-140% of the recom-
magnesium may occur on the resin resin, the use of additional excess mended load) may be required to dis-
over several cycles. This may acid is not justified by the economics. place these salts.
require extra heavy acid dosages on The standard recommendation for Bead size also affects the regen-
a periodic basis in order to maintain regenerating DOWEX 88 strong acid eration efficiency. Larger beads
normal operating capacities. cation resins is 7% hydrochloric acid require longer acid contact time for
(2N) at 6-7 pounds of 100% HCl per complete regeneration than smaller
cubic foot of resin.1 These conditions beads. Because they permit a small-
have proven to be the most efficient er average size bead to be used with-
and economic for routine regeneration out excessive pressure drop,
in most systems. Higher concentra- DOWEX MONOSPHERE resins
tions or loads will regenerate the regenerate more efficiently than stan-
resins more completely, but the mini- dard DOWEX resins. This can result
mal capacity gained is generally not in higher operating capacity and 15-
worth the extra cost in acid. Lower 20% longer service cycles. Longer
concentrations or loads will result in cycles translate into fewer regenera-
inefficient regeneration of the ion tions in a given time span, significant-
exchange resins’ capacity and ly reducing regenerant costs and
reduced lifetime due to irreversible increasing resin lifetimes.
accumulation of impurities.

1For DOWEX MONOSPHERE 88 resin, the recommended load drops to 5-6 pounds per cubic foot.

5
Table 2 – Recommended regenerants for DOWEX deashing and mixed-bed polishing resins

DOWEX 88 DOWEX DOWEX 66 DOWEX DOWEX 88 MB DOWEX 22

strong acid MONOSPHERE weak base MONOSPHERE strong acid strong base
cation 88 anion 77 cation anion
strong acid weak base
cation anion
3
Regenerant 6-7 lbs. HCl/cu. 5-6 lbs. HCl/cu. 5-6 lbs. NaOH/cu. ft. 4-5 lbs. (64-80 kg/m ) 6-7 lbs./cu. ft. 4-5 lbs.
1
level ft. ft. 7-8 lbs. NaOH/cu. ft. HCl NaOH/cu. ft.
3
(100% basis) (112-128 kg/m ) 6-7 lbs. 5-6 lbs.
3 3 3
96-112 kg/m 80-96 kg/m Na2CO3/cu. ft. Na2CO3/cu. ft. 96-112 kg/m Na2CO3/cu. ft.
5-6 lbs. 4-5 lbs.
NH4OH/cu. ft. NH4OH/cu. ft.

Regenerant 7% HCl 7% HCl 4% NaOH 4% NaOH 7% HCl 4% NaOH

concentration 5% Na2CO3 5% Na2CO3 7% Na2CO3
(minimum) 5% NH4OH 5% NH4OH

Regenerant 200° F 200° F 140°F 140°F 200° F 115°F

temperature 93°C 93°C 60°C 60°C 93°C 46°C
(max)
1
Assuming a minimum 90% equipment efficiency.

Table 3 – Recommended quality of regenerants

Caustic Soda Hydrochloric Acid Ammonium Hydroxide Soda Ash
(NaOH) (HCl) (NH4OH) (Na2CO3)

100% Basis Grade: Technical Liquid ammonia Grade: Technical,

gassified and white powder
dissolved in water
<1200 ppm NaCl 28% (18° Be”) HCl is generally pure enough Typical analysis:
for regeneration of weak
<3000 ppm Na2CO3 <100 ppm Fe 99% Na2CO3
base anion resins.
<30 ppm NaClO3 <100 ppm organics as O2 2100 ppm NaCl
consumed

<10 ppm Fe <5 ppm oxidants as Cl2 200 ppm Na2SO4

<2000 ppm Na2SO4 <4000 ppm sulfate 22 ppm Fe2O3

<100 ppm SiO2

6
Table 4 – Relative selectivity of Figure 5 –Cation and Anion Rinses
DOWEX 88 for cations
H+ = 1 Slow Rinse Fast Rinse
Na+ = 2
K+ = 3 Water
Mg++ = 3 dome lateral
Ca++ = 6

The fact that Na+, K+, Mg++, and Ca++ all have Water
a higher affinity for the resins’ active sites than
the hydrogen ion is the basis for the cation feed lateral
resins’ ability to effectively remove unwanted
salts from the syrup stream. Because regen-
eration must overcome these selectivity ratios,
the concentration and contact time of the
regenerant must be sufficient to overwhelm
the sites with hydrogen ions and force these
salts off. Waste Waste
or Water Recovery
Cation resin rinsing
Following regeneration are two rinse Regenerating DOWEX 66 and the regenerant at the discharge. The
steps: a slow rinse and a fast rinse DOWEX MONOSPHERE 77 weak subsequent fast rinse is continued
(Figure 5). The slow rinse is per- base anion resins until the discharge conductivity or pH
formed in the same direction as the drops below the syrup cycle break-
regenerant flow. The purpose of the In regenerating DOWEX 66 and
through point.
slow rinse step is to extend the con- DOWEX MONOSPHERE 77 resins,
Rinse requirements for weak base
tact time of the acid. This time exten- the objective is to remove the acids
anion resins increase over time as
sion improves regeneration efficiency picked up during syrup service (i.e.
the resin progressively fouls.
and allows the displaced salts time to sulfuric, nitric, hydrochloric, and
Ammonium hydroxide-regenerated
diffuse out of the interior of the resin organic acids). Regeneration is
resins give the lowest rinse require-
beads and into the rinse stream. almost always done downflow (Figure
ments. On the other hand, ammoni-
Slow rinse is performed at regenera- 6). With the proper regenerant con-
um hydroxide-regenerated resins
tion flow rates using condensate or centration and good flow distribution,
tend to foul out more rapidly.
deionized water. The slow rinse is weak base anion resins can be regen-
typically continued until there is a erated with nearly 100% efficiency.
Series and recirculation rinsing
noticeable acid dilution (the pH rises). The minimum regeneration recom-
mendations are 4% sodium hydroxide Series rinsing of cation and anion
Following the slow rinse, a fast beds can be used to conserve rinse
rinse at 2 to 4 times the slow rinse at 5-6 pounds per cubic foot for
DOWEX 66 and 4-5 pounds per cubic water (Figure 7). Series rinsing can
flow rate is performed to wash the also provide deionized water for sub-
residual, dilute acid off the resin. This foot for DOWEX MONOSPHERE 77.
Alternatively, 5% soda ash or 5% sequent rinses and dilutions. Series
rinse is continued until the effluent rinsing involves pumping rinse water
quality reaches the desired level, ammonium hydroxide can be used as
specified in Table 2. As with cation through the cation and the anion
typically 3-5 pH. The water used for beds in series.
this rinse must be of especially high resin regeneration, 45 minutes pump-
ing time is recommended as a mini- Recirculation rinsing is sometimes
quality (condensate or deionized performed when rinse requirements
water). Poor quality rinse water will mum.
become excessive (i.e., older resins)
partially exhaust the regenerated and continuous pumping of new
resin before the resin is even returned Rinsing weak base anion resins
rinse water isn’t economically justi-
to syrup service. If the cation resin The slow and fast steps of rinsing
fied. Recirculation rinsing involves
has been kept reasonably clean, part anion resins are generally performed
pumping rinse water through the
of the rinse water can usually be in the same manner as previously
cation and anion beds in a closed
recovered for subsequent acid dilu- described for cation resins. The slow
loop. During this process, the resid-
tion and/or rinse water. rinse is performed at the regeneration
ual acid coming off the cation bed is
flow rate until noticeable dilution of
removed by the anion resin. At the
same time, the residual caustic com-

7
ing off the anion bed is neutralized Figure 6 – Weak base anion regeneration and rinsing
when returned to the cation bed.
Recirculation rinsing helps to achieve
low conductivity effluent during the
sweetening-on step. It can also help Regeneration Slow
4% Caustic Soda Rinse
reduce salt leakage during the syrup
or
cycle. However, recirculation rinsing Water
5% Soda Ash
consumes a small amount of the
or
cation and anion resin capacities.
5% Ammonium
Hydroxide
Sweetening-on deashing systems
The sweetening-on procedure is
essentially the opposite of the sweet-
ening-off procedure. When the on-
line unit pair in the primary position
reaches breakthrough, the regenerat- Waste Waste
ed unit pair is switched to syrup ser-
vice. For a double-pass system, the
secondary unit pair is moved into the
primary position and the fresh unit is
brought into the secondary position.
Series and recirculation rinsing are techniques to minimize water use
Thus, sweetening-on is accomplished
in-line, at the process flow rate. The
effluent from the fresh unit pair is typ- Figure 7 – Series and recirculation rinsing
ically handled as treated water and
waste. Next comes sweetwater. Series Rinse
Finally, when the syrup concentration
D.I.Water
is high enough, the treated syrup is
sent forward in the process. At the
same time the fresh unit pair is
sweetening-on, the exhausted unit Cation Anion
pair is sweetening-off.

Cross-regenerating deashing
resins Waste & Treated
Weak base anion resins generally Water Recovery
require cross-regeneration with 7%
HCl and 4% NaOH approximately
every 6 weeks, on average. Cross-
regeneration helps clean up organic
fouling and extends the life of the
Cation Anion
resin.

Caustic brine cleaning of anion

resins
For highly fouled resin, soaking the
Recirculation Rinse
resin in a 2% caustic soda/10% sodi-
um chloride brine solution will help
restore the resin’s capacity. This treat-
ment may be done every 6 months or ed only when the cleaning has been We also recommend cross-
so to keep the resin in good condition. done at regular intervals starting when regeneration of strong acid cation
Caustic brine cleaning is recommend- the resin was new. resins periodically, using caustic
soda, rinsing, then regenerating with
hydrochloric acid.

8
Regenerating Mixed Bed Polishers top. After backwashing, the bed is For DOWEX 22 strong base
Regeneration of mixed bed polishers allowed to settle, resulting in two anion resin, the minimum
is more complicated than regeneration distinct layers. recommendation is 4% sodium
of split beds because the anion and hydroxide at 4-5 lbs/ cu. ft. or
cation resins are intimately mixed Chemical addition 7% soda ash at 5-6 lb/cu. ft.
during syrup service. As part of the The resins are regenerated by pump-
regeneration the cation and anion ing caustic soda or sodium carbon- Rinsing and blowdown of mixed
beads must be separated prior to ate through the anion resin from the beds
regenerant chemical contact. For top of the bed while pumping Following regeneration, a slow rinse
quality guidelines, refer to Table 3, hydrochloric acid through the cation is performed maintaining the same
Page 6. resin from the bottom. Excess flow directions as the regenerants
regenerants meet at the central later- (Figure 9). Next, a fast rinse is per-
Sweetening-off and backwashing al, neutralize each other, and are formed from the top and bottom of
The first step in regeneration of mixed sent to waste. Since this procedure the bed simultaneously. Both rinses
bed polishers (Figure 8) is sweeten- requires that the interface of the two require demineralized or deionized
ing-off in essentially the same manner resins occurs precisely at the same water. A blowdown of the liquid head
previously described for deashing level as the lateral discharge, it is to just above the resin level is typical-
units. critical that the correct cation resin ly performed after rinsing to accom-
Next, the resins are backwashed. volume is maintained in the bed. modate the subsequent mixing step.
Backwashing causes the denser, larg- The minimum recommendation
er cation resin beads to migrate to the for regeneration of DOWEX 88MB
lower portion of the expanded bed, strong acid cation resin is
while the anion resin beads rise to the 6-7 lbs/cu ft of 7% hydrochloric acid.

Figure 8 – Sweetening-off and regeneration of mixed beds

Waste

Water

Cation Anion
&
Anion
Mix Cation

Full Strength
Process
Backwash Water
Sweet Water
Waste
Caustic

Anion
Waste
Cation
Acid

9
Remixing mixed beds for syrup Figure 9 – Rinsing and blowdown of mixed beds
service
Complete and intimate mixing of the Fast Rinse
Slow Rinse
cation and anion resins is essential Deionized Water

for proper operation of mixed beds.

Typically, the resin bed is first Deionized
Water Waste
expanded using air and water simul- Waste & Water
Recovery
taneously to mix the resins (Figure
10). Once the resins are intimately Blowndown
Air
mixed, water addition is stopped but
Deionized Deionized
air continues to be blown into the Water Water
bed until the bed can finish settling
without significant separation of the
anion resin from the mixture. The
system is vented, and the bed starts
to settle. As it settles, water is
drained off at a rate which keeps the Water Recovery
water level just above the top of the
resins. This keeps the anion resins
from separating near the top of the
bed. Usually this sequence is part of Figure 10 – Resin mixing in mixed beds
the automatic operating program, but
in some systems it is performed Air-Water Mix Air Mix Air Drain
manually. Water Recovery Vent Vent

Recycle rinsing of mixed beds

A recycle rinse is also commonly
used with mixed beds because it
helps achieve a low conductivity
Water
effluent during sweetening-on and Recovery
syrup service (Figure 11). Because
the performance requirements of
mixed bed polishers are more strin-
Deionized Air Air
gent than with deashing beds, efflu- Water & Air
ent rinse water conductivity should
ideally be below 10 micromhos/cm
near the end of the rinse. At the
completion of the recycle rinse a Figure 11– Recycle rinsing of mixed beds
blowdown of the liquid head is used
to remove the water to just above the Fill
resin level in systems operated with Deionized Vent
air domes. Water Recycle Rinse

Blowndown
Air

Water Recovery

10
Troubleshooting cause of the problem. In fact, many In addition to the standard tests, we
potential problems can be identified have the capability of running a wide
Troubleshooting deashing systems through routine resin analysis before variety of non-standard tests to assist
they show up in the form of short you in troubleshooting your system.
Abrupt vs. gradual problems cycles or poor syrup quality. That’s Syrup samples can also be evaluated
The following troubleshooting flow why we encourage processors to for resin-related quality problems.
charts will help you determine the take advantage of our Resin Check-
cause of problems which occur Up Service. System profiling helps you fine-
abruptly in deashing and mixed-bed tune your system
polishing units. These charts also Our Resin Check-Up Service System profiling is another service
suggest corrective action. Abrupt helps you obtain optimum results available to users of DOWEX resins.
problems are those which occur within from DOWEX resins We start by taking syrup samples at
a few minutes, hours, days, or even
This analytical service covers various points in the system over a
weeks. These problems are distin-
every critical operating characteristic complete cycle. The special battery of
guished from the gradual decrease in
of your resin. These analyses allow tests we perform on these samples
unit performance which results from
us to help you maximize the remain- gives us the information we need to
normal aging and occurs over much
ing usable life of the resin. Each time help you fine-tune your system for
longer periods of time (months and
you send samples to our lab you’ll economical operation and consistent-
years).
receive a complete report which ly high syrup quality.
The value of routine analysis and includes itemized listings of the oper-
ating characteristics as well as rec-
good record-keeping
ommendations for remedial steps, if
When problems do occur, the task required. We also maintain a histori-
of troubleshooting will be greatly sim- cal database on your resins which
plified if you regularly sample and can prove extremely valuable in pre-
analyze your resins and keep good dicting or troubleshooting possible
records on your system. This will problems.
allow you to compare current perfor- Our lab offers one of the most
mance with normal operation to deter- complete analytical services available
mine the extent and sometimes the for producers of nutritive sweeteners.

11
Figure 12: Troubleshooting abrupt deashing problems - Short Service Cycles

Possible Causes
Cation Unit or Anion Unit Problem? & Suggested Actions
First determine if the problem is coming from
the cation bed or the anion bed by sampling Poor Cation Regeneration
the anion discharge at service breakthrough.
Check acid strength, load, quality, and
flow rates (regenerant dilution and
contact time). Check rinse water and
dilution water quality. See Table 3,
page (6).

Check resin bed levels

If low, top off with new resin.
High Feed Ash
Check for excess enzyme activator
addition or excessive pH adjustment
Symptoms upstream. Check if feed syrup or anion
regenerant is leaking to product line.
Breakthrough on Cation Unit
If pH is greater than 4 and there is high
pH > 4 conductivity, then salt breakthrough is
probably occuring on the cation unit. Poor Flow Distribution
Check for mechanical problems that
could affect flow during regeneration or
syrup service such as leaky valves or
Breakthrough on Anion Unit broken distribution laterals.
If pH is below 4, then acid
pH < 4 breakthrough is probably occuring
on the anion unit.
Poor Anion Regeneration
Check base strength, load, quality, and
flow rates (regenerant dilution and
contact time). Check rinse water and
dilution water quality. See Table 3,
page (6).

High Feed Ash

Check for excess enzyme activator
addition or excessive pH adjustment
upstream. Check if cation regenerant
(acid) is leaking to product line.

High Organic Acids &

Microbial Contamination
Check for microbe buildup ahead of
and on anion bed. If found, backwash
around screening devices; clean up
and regenerate cation and anion beds;
clean up surge tanks, heat
exchangers, etc.

12
Figure 13: Troubleshooting abrupt deashing problems - Poor Syrup Quality

Cation Unit or Anion Unit Problem?

First determine if the problem is in the
Possible Causes &
cation bed or the anion bed by Suggested Actions
checking the anion discharge during
the syrup run. Poor Cation Regeneration
Check acid strength, load, quality, and flow
rates (regenerant dilution and contact
time). Check rinse water and dilution
water quality - If OK, increase acid dosage.

Check resin bed levels.

If low, top off with new resins.
Poor Flow Distribution
Symptoms Check for mechanical problems that could
affect flow during regeneration or syrup
service such as leaky valves or broken
Leakage from Cation Unit distribution laterals - If OK, increase acid
If pH is equal to or greater than normal dosage.
and there is high conductivity, the
pH ≥ normal problem is generally with the cation unit.
Regenerant Leakage to Line
Alkali regenerant leaking to the product
Leakage from Anion Unit line will cause a high pH that has nothing
to do with the cation bed. Check for
If pH is below normal, the problem is leaking valves.
pH < normal generally with the anion unit.

Poor Anion Regeneration or

Poor Flow Distribution
Check base strength, load, quality, and
flow rates (regenerant dilution and
contact time). Check rinse water and
dilution water quality - If OK, boost
regenerant dosage.

Regenerant Leakage to Line

Acid regenerant leaking to the product
line will cause a low pH that has nothing
to do with the anion bed. Check for
leaking valves.

High Organic Acids &

Microbial Contamination
Check for microbe buildup ahead of and
on anion bed. If found, backwash around
screening devices; clean up and
regenerate cation and anion beds; clean
up surge tanks, heat exchangers, etc.

13
Figure 14: Troubleshooting abrupt deashing problems - High As-is Color

Problem Possible Causes Suggested Actions

See Figure 13, "Troubleshooting

Poor Operation Poor Syrup Quality"
of Cation Unit (cation branch)

Poor Operation See Figure 13, Troubleshooting

of Anion Unit Poor Syrup Quality
(anion Branch)
Color (operational)
High Reduce Temperature or
Temperature Increase Flow Rate

Long Reduce Time or Decrease

Retention Recycle
Time

Weak Base Anion Resin

with Excessive Call your Dow Technical Service
Salt Splitting Capacity Representative for Assistance

See Figure 13, "Troubleshooting

Poor Syrup Quality"
Poor Cation Performance (cation branch).
with New Anion Resin
Pink Color
(high pH environment) Pink color due to mismatch
of cation and anion
resin operating capacities. Replace Cation Resin

Check Rinse Effectiveness

Caustic in
Vessel and/or Lines

Check for Anion

Regenerant Leakage

14
Figure 15: Troubleshooting abrupt deashing problems - High After-Heat Color

Suggested Actions

See Figure 13, "Poor Syrup

Problem Possible Causes Quality"
Follow Cation Unit branch of chart
(pH≥ normal).
High After-Heat Protein Leakage
(heat treated) Color from
Cation Unit

Check for Increases in

Incoming Protein
Check for enzymes or corn protein.

15
Figure 16: Troubleshooting abrupt deashing problems - High Pressure Drop

Suggested Actions
Check for Plugging
Check line valving, strainers,
and distribution laterials for
mechanical problems or
plugging that can inhibit flow.

Possible Causes

Defective Operating Devices

Plugged valves, screens, and Remove Cell Masses
distribution laterials are the Remove cell masses from the top
most common cause of of resin beds by backwashing
abrupt pressure drop. (bypassing screen devices),
and/or mechanical removal
(skimming bed tops).

An Abrupt Rise In
Pressure Drop Increase Service Temperature
Microbial Contamination
This is usually due to a defective Increase the ion exchange system
operating device. Typically, Pressure drop due to microbial
buildup generally builds up service temperature to 46oC
problems caused by (115oF).
contamination or resin breakage gradually.
will gradually appear over a
period of weeks or months.

Add SO2 to Feed

Add 100 ppm SO2 to ion
exchange feed on periodic basis
to minimize microbial activity and
block browning reactions.

Resin Breakage
If resin breaks up rapidly, Terminate Runs on Color
something is wrong in the system
that needs to be corrected. For Terminate extra long runs on
example, an oxidizer such as color rather than conductivity
oxygen or chlorine may be or pH.
entering the system.

Check For Resin Fines

Sample the resin bed and check
for fines after the regeneration
cleanup sequence. Remove fines
by backwashing, bypassing
screening devices.

16
Troubleshooting Mixed-beds
Figure 17: Troubleshooting abrupt problems - Poor Syrup Quality

Possible Causes
& Suggested Actions

Insufficient Cation Resin

Regeneration
Symptoms Check regenerant strength,
quality, and flow rates. Check
rinse water quality.
If pH is Greater than Normal
and/or Cation Leakage -
The problem is generally
with the cation resin. Regenerant
Cross-Contamination
If the cation/anion resin
interface is high, the anion
regenerant will contaminate the
Cation or Anion Problem? top portion of the cation resin,
putting it into the sodium form
First determine if the problem is and causing salt leakage.
in the cation or the anion resin
by checking the syrup quality at
the discharge from the unit.
Insufficient Anion
Resin Regeneration
Check regenerant strength,
quality, and flow rates. Check
rinse water quality.
If pH is Less than Normal
(4-6) and/or Anion Leakage -
The problem is generally
with the anion resin. Regenerant
Cross-Contamination
If the cation/anion resin
interface is too low, the cation
regenerant will contaminate the
lower portion of the anion resin,
causing chloride leakage when
the unit is returned to service.

17
Resin Properties
This section provides typical resin
properties as well as pressure drop
and backwash expansion charts for
DOWEX resins.

Table 5 – Typical resin properties for DOWEX deashing and mixed-bed polishing resins

DOWEX 88 DOWEX DOWEX 66 DOWEX DOWEX 88 DOWEX 22

MONOSPHERE MONOSPHERE MB
88 77

Type Strong acid Strong acid Weak base Weak base Strong acid Strong base
cation cation anion anion cation anion,
Type II
Active group Sulfonate Sulfonate Tertiary amine Tertiary amine Sulfonate Quaternary
amine
Ionic form Sodium Sodium Free base Free base Sodium Chloride
(as produced)
Structure Macroporous Macroporous Macroporous Macroporous Macroporous Macroporous
styrene- styrene- styrene- styrene- styrene- styrene-
divinylbenzene divinylbenzene divinylbenzene divinylbenzene divinylbenzene divinylbenzene
Physical form Spheres Uniform spheres Spheres Uniform spheres Spheres Spheres
U.S. standard 16-40 -30 + 40 16-50 -30 + 40 16-35 16-50
mesh (typical) (95%) (95%)
Total capacity 1.8 meq/ml, 1.8 meq/ml, 1.7 meq/ml, 1.60 meq/ml, 1.8 meq/ml, 1.2 meq/ml,
min min min min min min
Weak base 1.50 meq/ml, 1.35 meq/ml,
capacity min min
Water retention 42-48% 42-50% 40-50% 40-50% 42-48% 48-56%
capacity (typical)
Swell, % ~ 5% ~ 5% ~ 22% ~ 20% ~ 5% 12% typical
Na → H form Na → H form Free base → HCl Free base → HCl Na → H form Cl- → OH-

18
Pressure drop as a function of flow rate

The following charts are provided to help you determine pressure drop across beds of DOWEX resins. Possible causes
for excessive pressure drop are discussed on Page 16.

Figure 18 – Pressure drop with DOWEX 88 resin Figure 19 – Pressure drop with DOWEX 66 resin
Pressure Drop as a function of flow Pressure Drop with DOWEX 66 Resin
rate with DOWEX 88 Resin
m/h m/h
0 1.2 2.4 3.7 4.9 6.1 7.3 0 1.2 2.4 3.7 4.9 6.1 7.3
3.0 68 3.0 68
2 cp ~ 40% dissolved solids at 120° F

Pressure Drop (psi/ft of bed depth)

2 cp ~ 40% dissolved solids at 120° F
Pressure Drop (psi/ft of bed depth)

10 cp ~ 60% dissolved solids at 120° F 10 cp ~ 60% dissolved solids at 120° F

(10cp)
(12 cp)

Pressure Drop (kPa/m)

Pressure Drop (kPa/m)
2.0 45 2.0 45
(10cp)

(6cp)

(6cp)
1.0 23 1.0 23

(2cp)
(2cp)

0 0 0 0
0 .5 1.0 1.5 2.0 2.5 3.0 0 .5 1.0 1.5 2.0 2.5 3.0
Flow Rate (gpm/ft2) Flow Rate (gpm/ft2)

Figure 20 – Pressure drop with DOWEX MONOSPHERE 88 and MONOSPHERE 77 resins

Pressure Drop with DOWEX MONOSPHERE 88 and MONOSPHERE 77 Resins

m/h
0 1.2 2.4 3.7 4.9 6.1 7.3
3.5 79
Pressure Drop (psi/ft of bed depth)

3 X 68
Pressure Drop (kPa/m)

2.5 56

2 X 45
X
1.5 34
X +
1 X 23
+
0.5 X 11
+

0 0
0 0.5 1 1.5 2 2.5 3
Flow Rate (gpm/ft2)

2 cp + 4 cp X 6 cp 8 cp X 10 cp 12 cp

19
Figure 21 – Pressure drop with DOWEX 88 MB resin

Pressure Drop with DOWEX 88 MB Resin

(m/h)
0 1.2 2.4 3.7 4.9 6.1 7.3
3 68
Pressure Drop (psi/ft of bed depth)

2.5 56

Pressure Drop (kPa/m)

X
2 45

1.5 X 34
+
1 23
+
X
0.5 11
+

0 0
0 0.5 1 1.5 2 2.5 3
Flow Rate (gpm/ft2)

2 cp + 6 cp X 10 cp 12 cp

Figure 22 – Pressure drop with DOWEX 22 resin

Pressure Drop with DOWEX 22 Resin

(m/h)
0 1.2 2.4 3.7 4.9 6.1 7.3
3 68
X
Pressure Drop (psi/ft of bed depth)

2.5 X 56
Pressure Drop (kPa/m)

2 X 45
+
1.5 X + 34
+
1 X 23
+

+
0.5 X 11
+

0+
X 0
0 0.5 1 1.5 2 2.5 3
Flow Rate (gpm/sq.ft.)

2 cp + 6 cp X 10 cp 14 cp

20
Backwash expansion characteristics

The backwash expansion curves in Figure 24 – Backwash expansion of DOWEX MONOSPHERE 88 resin
this section are provided to help you
determine the expansion of your beds DOWEX* MONOSPHERE* 88 Backwash Expansion Water @ 77 Deg. F 25 Deg. C
at a given temperature and flow rate. (m/h)
Colder water will expand the resins 0 4.9 9.8 14.7 19.6 24.4 29.3 34.2
higher in the bed for a given pump 100
rate. 90
Backwash expansion should be 80
monitored carefully since insufficient
% Bed Expansion
70
expansion will decrease regeneration 60
efficiency. Excessive expansion may 50
lead to resins escaping the bed - a
40
particular concern with anion resins, To determine flow rate at temperature t
30 Ft°Fahrenheit = F77 [1+.008 (t° Fahrenheit - 77)]
which are lighter than cation resins.
20 Ft°Celsius = F25 [1+ 0.014 (t° Celsius - 25)]
More information on resin backwash-
ing and recommendations for bed 10
expansion are given on Page 4. 0
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14
Flow Rate F (gpm/ft2)
Sodium Form

Figure 23 – Backwash expansion of DOWEX 88 resin Figure 25 – Backwash expansion of DOWEX 66 resin

Backwash Expansion Characteristics of DOWEX 88 Resin Backwash Expansion Characteristics of DOWEX 66 Resin
(m/h) (m/h)
0 4.9 9.8 14.7 19.6 24.4 29.3 34.2 0 1.2 2.4 3.7 4.9 6.1 7.3 8.6 9.8 11.0
100 100
Free Base
Typical Wet Screen 90 Form 77°F
Mesh % (25°C)
90 +16 0.0 80
+20 21.4 HCI-H2SO4
+30 64.2 70 Exhausted
% Bed Expansion

80
% Bed Expansion ( Na+ exhausted form)

77°F Form 77°F

+35 11.6 (25°C)
+40 2.3 25°C 60
+50 0.5
70 50
-50 0.0
40
60
30

50 20
To determine flow rate at temperature t
10 Ft°Fahrenheit = F77 [1+.008 (t° Fahrenheit - 77)]
40 Ft°Celsius = F25 [1+ 0.014 (t° Celsius - 25)]
0
0 .5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5
30
Backwash Flow Rate (gpm/sq.ft.)

20
To determine flow rate at temperature t
Ft°Fahrenheit = F77 [1+.008 (t° Fahrenheit - 77)]
10
Ft°Celsius = F25 [1+ 0.014 (t° Celsius - 25)]

0
0 2 4 6 8 10 12 14
Flow Rate F (gpm/ft2)

21
Figure 26 – Backwash expansion of DOWEX MONOSPHERE 77 resin

DOWEX* MONOSPHERE* 77 Backwash Expansion

Water @77 Deg. F 25 Deg. C
(m/h)
0 1.2 2.4 3.7 4.9 6.1 7.3 8.6
100 +
90
80
+
% Bed Expansion

70
+
60 +
50
+
40
To determine flow rate at temperature t
30 + Ft°Fahrenheit = F77 [1+.008 (t° Fahrenheit - 77)]
20 Ft°Celsius = F25 [1+ 0.014 (t° Celsius - 25)]
+
10
0
0 0.5 1 1.5 2 2.5 3 3.5
Flow Rate F (gpm/ft2)
Free Base Form + Acid Exhausted Form

Figure 27 – Backwash expansion of DOWEX 88 MB resin

DOWEX 88MB Backwash Expansion

Water @77 Deg. F 25 Deg. C

(m/h)
0 4.9 9.8 14.7 19.6 24.4 29.3 34.2
100
90
80
% Bed Expansion

70
60
50
40
To determine flow rate at temperature t
30 Ft°Fahrenheit = F77 [1+.008 (t° Fahrenheit - 77)]
20 Ft°Celsius = F25 [1+ 0.014 (t° Celsius - 25)]
10
0
0 1 2 3 4 5 6 7 8 9 10 11 12 13 14
Flow Rate (gpm/ft2)
Sodium Form

22
Figure 28 – Backwash expansion of DOWEX 22 resin

DOWEX 22 Backwash Expansion

(m/h)
0 1.2 2.4 3.7 4.9 6.1 7.3 8.6 9.8
100
90
% Bed Expansion (CI¯ form)

80
70
60
50
40
To determine flow rate at temperature t
30 Ft°Fahrenheit = F77 [1+.008 (t° Fahrenheit - 77)]
20 Ft°Celsius = F25 [1+ 0.014 (t° Celsius - 25)]

10
0
0 0.5 1 1.5 2 2.5 3 3.5 4
Flow Rate F (gpm/sq.ft.)
Expansion @ 77 Deg F
25 Deg C

23
Storage and Handling Bringing deashing units back
on-line
Storage 1) Rinse off the NaOH storage solu-
For long shutdowns, cation and anion tion to neutral pH.
deashing resins can be stored in 2) Cation resins - Regenerate with a
place in a manner that provides pro- minimum of 1.5 bed volumes of 7%
tection from microbial growth. The HCl; rinse to neutral pH. Anion
following recommendations will also resins - Cross-clean first with 7%
increase the probability of a trouble HCl; rinse to neutral pH; regenerate
free start-up. with a minimum of 2.2 bed volumes
of 4% NaOH; rinse to neutral.
Cation and anion deashing resin 3) Follow normal procedures from this
preparation and storage point on.
1) Backwash the bed to a minimum
of 50% expansion for as long as it Handling
takes to produce a clear and color- WARNING: Oxidizing agents such
less effluent. as nitric acid attack organic resins
2) Clean up the resin by passing 2 under certain conditions and could
bed volumes of 4% (1N) NaOH result in a slightly degraded resin up
through the bed; rinse to neutral to an explosive reaction. Before using
pH; pass through 1.5 bed volumes strongly oxidizing agents, consult
of 7% (2N) HCl ; rinse to neutral sources knowledgeable in handling
pH.2 such materials.
3) Pass 4% NaOH through the bed
until at least a 0.5% (0.1N) con-
centration is detected in the efflu-
ent. The entire vessel should be
full of 0.5% (minimum) NaOH solu-
tion for protection and cleaning of
the dome space.
4) During the storage period, check
the NaOH solution periodically by
draining some off the bottom of the
vessel. Replace the entire solution
volume with fresh 0.5% NaOH if
there is significant color develop-
ment.

2Pumping rates of the chemicals should be such that there is a minimum contact time of 45 minutes.

24
How to get more information on DOWEX products
and Dow support services
To learn more about DOWEX prod- Dow technical service representa-
ucts, Dow technical support services, tive. You'll talk with someone who
request additional literature, or to get understands your needs and can
help resolving a particular problem, provide the prompt, personal service
simply call us toll-free at you deserve.
1-800-447-4369 or contact your

Warning: Oxidizing agents such as nitric acid attack organic ion exchange resins under certain conditions. This could lead to
anything from slight resin degradation to a violent exothermic reaction (explosion). Before using strong oxidizing agents, consult
sources knowledgeable in handling such materials.

Notice: No freedom from any patent owned by Seller or others is to be inferred. Because use conditions and applicable laws
may differ from one location to another and may change with time, Customer is responsible for determining whether products
and the information in this document are appropriate for Customer’s use and for ensuring that Customer’s workplace and
disposal practices are in compliance with applicable laws and other governmental enactments. Seller assumes no obligation or
liability for the information in this document. NO WARRANTIES ARE GIVEN; ALL IMPLIED WARRANTIES OF
MERCHANTABILITY OR FITNESS FOR A PARTICULAR PURPOSE ARE EXPRESSLY EXCLUDED.

25