IX Maintenance and Troubleshooting

Bill Carlin

Maintenance & Troubleshooting

Content
Maintenance

Record keeping
Monitoring
Vessel integrity
Resin integrity

Resin analysis/Director services

Problematic Impurities

Maintenance
-Recordkeeping

Maintenance
-Record Keeping
Changes in the following may affect running time or throughput :

Feed water composition:

Minor salinity increase: proportional reduce running time
x% more salinity means x% shorter cycle
Radical water composition changes: Re-assess whole plant
Feed water temperature:
Variations >10C may affect resin operating capacity
(WAC & WBA particularly sensitive to low temperature)
High temperature decreases silica removal.

Maintenance
-Record Keeping
Loss of capacity

After a long time in operation, gradual decrease of anion exchange

resin capacity. May need to adjust running time or replace resin

Pressure drop

Pressure drops >2.5 bar (35 psi) should be avoided due to possible
equipment or resin damage.
If the pressure drop in a vessel increases > 50 %, the resin should be
backwashed to avoid channeling and resin damage.

Loss of resin replace immediately

Rinse water consumption

After regenerant injection, monitor the slow (displacement) rinse water

volume required to reach 150 S/cm.
If the volume > 1.5 times the value for new resins, fouling or crosscontamination may have occurred and a cleaning should be made.

Maintenance
-Monitor Input

Feed water analysis & Temperature

Condition of the ion exchange resins
Resin height
Regenerant Conditions
(level, concentrations, etc.)
Pretreatment Operating Data
(residual Cl2, level of suspended solids, dosing chemical
consumption)
Maintenance log
records routine maintenance, mechanical failures, equipment replacements,
calibration of gauges and meters, all IX cleanings

Maintenance
-Monitor output

Conductivity
pH
Silica
Throughput
Flows
Unusual incidents
Check rinse water consumption ~ every 15 cycles
(for resin fouling)

DI Run Length vs. River Conductivity

700

230
220
210

500
200
400

190

300

180
170

200
160
100

0
Apr'93

150

Jun'93

Aug'93

DI Runs

Oct'93

Dec'93

Feb'94

140
Apr'94

River Conductivity

Conductivity (S/cm)

Volume (m3)

600

DI Run Length vs. River Conductivity

700

230
220
210

500
200
400

190

300

180
170

200
160
100

0
Apr'93

DI Runs

Conductivity (S/cm)

Volume (m3)

600

150

Jun'93

Aug'93

Oct'93

River Conductivity

Dec'93

Feb'94

140
Apr'94

Conductivity* DI Run Length (/1000)

Maintenance
-Monitor output
Anion effluent conductivity

SAC
Free Mineral Acidity

Free Mineral Acidity

Na (anion effluent conductivity)

End of
rinse

Production run

Bedvolumes

Na leakage

pH

2 RH + Ca++

R2Ca + 2 H+

RH + Na+

RNa + H+

2 RNa + Ca++

R2Ca + 2 Na+

In effluent:
H+ = key cation until exhaustion
All anions still present

Breakthrough

As exhaustion approaches,

[Na] increases.
Free Mineral Acidity (FMA) e.g. HCl, H2SO4, HNO3, respectively decreases, with [Na+]
pH at outlet of the SAC resin is low (2 to 4) until near exhaustion, then [H +] & pH
Conductivity at the outlet of the SBA resin downstream reflects Na+ leakage from the
SAC resin: remains low until Na+ appear at the outlet of the cation column.
11

Maintenance
-Monitor output
120

12 pH

60

120

12 pH

60

SBA

SBA
100

100

10

10
pH

40

20
Silica
Conductivity (increase due to acids)

0
End of
rinse

Production run

RCl + OH

2 ROH + SO4=

R2SO4 + 2 OH

ROH+ HSiO3

RSiHO3

2RSiHO3 + SO4=

R2SO4 + HSiO3

20

4
Silica
Conductivity (increase due to NaOH)

0
End of
rinse

Breakthrough

If SBA breaks first =>

H2SiO3 , etc. in effluent

ROH + Cl

40

20

2
Bedvolumes

60

40

20

80

Conductivity S/cm

60

40

Silica g/L

Silica g/L

80

Conductivity S/cm

pH

Production run

2
Bedvolumes
Breakthrough

If SAC breaks first =>

NaOH, NaHSiO3 in effluent
In effluent:
H+ = key cation unless SAC breaks first giving Na leakage
Key anion = OH- until exhaustion
H + + OHH2O
st
1 anion to break through = HSiO3

12

Monitoring Conductivity
- Not Enough
Silica being a weak acid does not have as high a conductance as Na

Silica, ppb

Conductivity, S/cm

Sodium, ppb

Conductivity, S/cm

10

0.0548

0.01

0.0548

40

0.0549

0.0550

160

0.0553

10

0.12

640

0.0566

100

1.1

1000

0.0576

1000

10.9

Monitoring pH
pH out of each bed in a pretreatment system can give critical info
especially when troubleshooting

Weak Acid Cation Bed

Cation Bed

Should be low <3 (depends on TDS) understanding baseline is important

Change upward from typical baseline pH indicates increase in cation
leakage, should correspond to higher conductivity and pH out of anion
resin

Weak Base Anion Bed

Should be low <4 for 10-30% of the run (depends on FMA)

Will baseline at ~ 4.5
Change upward from 4.5 indicates breakthrough

Should be between 4 and 7 depending on alkalinity

Drop in pH from baseline indicates exhaustion or channeling

Strong Base Anion Bed

Should be between 7.5 and 9

Below 7 indicates exhaustion or channeling
Higher than 9 indicates chemical hideout, leaky NaOH valve, or problem
with SAC resin

Maintenance
-Vessel integrity

Vessel Integrity
-Unit Distributor Inspection
Inlet Distributor
Flow Must be Evenly Distributed Across Bed
No Bent or Incorrectly Aimed Laterals
Splash Plates Intact
Regenerant Distributor
Flow Must be Evenly Distributed Across Bed
No Bent or Incorrectly Aimed Laterals
Outlet Distributor
If the Inlet Distributor is in Good Condition an Uneven Bed
Surface After the Service Run Indicates Lower Distributor
Blockage.

M-16

Examples of Channeling

Concave

Convex

Diagonal

M-15

Vessel Integrity
-Unit Lining Inspection
Check Walls, Base and Top for Tears or Bubbles
Check Wherever Laterals Enter Vessel or Are Braced
Check Walls of Vessel in Vicinity of Regeneration Lateral for
Bubbles Caused by Regenerant

M-17

Maintenance
-Resin integrity

Analytical testing of resin

The purpose is to:

Troubleshoot
Track resin condition
Determine if resin needs to be replaced
Examine resin condition SEPARATE from the operating unit
Look for changes from new resin
Make INTERPRETATIONS about performance

Courtesy of The Dow Chemical Co All

rights reserved.

Sampling
Sample after regeneration and rinse
Pre-regeneration samples maybe necessary for troubleshooting but
not routine testing.

Core samples preferred

Not necessary for mixed bed samples

Use clean, plastic container

Tape lid onto container to avoid spilling during
shipment
Label container with paper label
Sharpie right on plastic container can get smudged

Make up demin resin analysis

Water Retention Capacity (WRC)
Total Capacity
Cation Resin Total Weight Capacity
Anion Resin Strong, Weak, Total Capacity

Fe Loading on Cation Resin

Organic Loading on Anion Resin
Bead Integrity - WUB

CPP resin analysis

WRC
Total Capacity
Cation Resin Total Weight Capacity
%H and Na form sites

Anion Resin Strong, Weak, Total Capacity

%OH, HCO3, Cl, SO4 form sites

Fe and Cu Loading on Cation Resin

Anion Resin Kinetics/MTC
Bead Integrity WUB
Special Testing

Water retention capacity

Problem: SAC Increase > 3%

Cause: Oxidation (decrosslinking)
Symptoms:
Softening of the resin

Decrease in particle density

Increased pressure differential
High resin makeup
Organic fouling of anion resin
Source of SULFATE in feed to boiler!!!

Total capacity
Tells you:

How many sites are present per unit mass or volume

Does not tell you:

How long your runs should be

Whether or not the capacity is accessible
Whether or not the resin is being adequately regenerated

Total capacity
Problem: SBA: loss of > 20% Total Cap
SBA: conversion to Weak Base
Cause: Loss of chemical functionality

WB: cannot remove silica

Symptoms:

Loss of operating capacity

Short runs

Site analysis
Cation - % Na, % H
Anion - %OH, %HCO3, %Cl, %SO4, etc.
Problems
High leakage
Low operating capacity

Causes
Poor Regeneration
Poor Separation
High Cl in NaOH

Physical integrity
- Whole bead

Problem: Osmotic shock and physical attrition

Resin shrink and swell as they change forms

Osmotic stress on the resin is very strong

Shrink/swell too fast causes beads to break
Transfer to and from vessels causes physical attrition
WBA are particularly susceptible

Action Levels
85 to 90% Increase testing; Plan to replace within ~12 months
< 85 % Replace as soon as possible

Symptoms:

Loss of resin
Increased pressure drop
Channeling
High mixed bed Na leakage
RESIN ESCAPE: to next bed or to product
Separation problems in MB

Fouling/Precipitation (DI)
Types:
Fe, Silica, Organic Compounds,
Calcium Sulfate, Barium Sulfate,
Mud, Dirt, Filth, Algae/Bacteria

Symptoms:

Higher pressure drop

Channeling
Loss of operating capacity
Higher baseline leakage

Organic loading (DI)

Problem: Effective loss of Strong Base Capacity
CH3 CH3
N+
CH3 CH2

Anion resin

CH2
CH2

CH2
CH2 CH
3
N+
CH
3
CH3
OO
C
O

CH2 CH
3
N+
CH
O CH3
3
C
O
CH2

NH2
CH2

CH2
CH2

O
CH2

CH3

Organic acid

Symptoms:
Long rinse to conductivity
Reduced throughput to silica endpoint

O-

Effects of organic fouling

Problems in plant operation
During anion regeneration with
NaOH

Rinse is long
Na leakage increases
SiO2 leakage increases
Capacity decreases
Moisture content decreases

S/cm

convert to -COONa

60
50
40
30
20
10
0

SBA resin rinse

Long rinse
OK

0 2 4 6 8 10 12 14 16 18 20
Bedvolumes

Poly-electrolyte fouling
Cationic or Anionic polyelectrolytes used in pre-treatment can be
serious cause of resin surface fouling
Cationic polymers foul cation resin
See high leakage of Ca and Mg but not necessarily Na leakage

Not easy to detect by normal testing. Watch for the symptoms...

Recovering from fouling

SiO2
8% NaOH soak for at least 8 hrs
preferably at 50C

Natural Organic
10% NaCl/2% NaOH soak for at least 8 hrs
Repeat soaks may be necessary
Use frequently and routinely for high organic waters

Iron or CaSO4
10% HCl soak for at least 4 hrs
Repeat soaks may be necessary
Materials of construction must be compatible

Mass Transfer Coeficient (MTC)

Ion exchange processes are film diffusion limited
Measures the rate at which ions diffuse from the feed solution to the
resin surface.
Reduction in MTC indicates resin fouling.

Why does anion MTC degrade with use?

Anion Resin
Surface

Cl

SO4

Surface Foulant

+
+
+
+
+

++

++
+
+

Anion Exchange Resin Bead

negative charge
35

MTC Test Concept

Flow through column test

Run on MB at flow rate simulating CPP, 50 gpm/ft2 (120 m/h)
Bed depth set to get measurable leakage for new resin
Challenge the MB with inlet containing SO4
Measure SO4 leakage (cation conductivity)
Calculate SO4 MTC using conditions of test
Be sure to include anion resin particle size

Now a standard test:

ASTM test method, D6302-98

Take home message

Watch for the signs / trends
Your system will give warning signs before most major problems
Problems due to resin degradation typically develop over time
Sudden problems tend to indicate equipment issues or changes to
feed water or regen conditions

Sample for resin analysis routinely

If you start to see a trend, dont wait for a major problem
Investigate possible causes of trend - We can help
Send resin samples to Dow for analysis

Thank You!

For more information please visit our web site or

contact your local Dow representative.
http://www.dowwaterandprocess.com/