Ion Exchange Resin Testing

John Greene
Consultant
Introduction

Power Industry Background (MUWTP and CPP)

Consider the Life Cycle of Ion Exchange Resins

From Manufacture through to eventual Disposal

One Possible Approach

Consider Ion Exchange Resin Testing as part of a

RESIN MANAGEMENT PROGRAMME

Do you want to pay me now or pay later?

Content

Introduction
When to Test
Why Test
How to Test
Routine Tests
Specialised Testing
Sampling
Test Results
Conclusions
Questions
When to Test

Manufacturing/Production

Pre-delivery

Before Loading into Service Vessel

Periodically

Troubleshooting

Prior to Disposal
Manufacturer and Production

Sampling and Testing for :

Quality Assurance

Traceability etc

Specification Compliance
Resin Specification 1

Resin Properties:

Application e.g. Softening

Polymer Structure

Appearance

Functional Groups

Ionic Form
Typical Resin Specification for Cation Resin

Total Capacity, Na+ Form (min) 1.8eq/l

Moisture Retention, Na+ form 48 53%
Mean Diameter 725 125 m
Uniformity Coefficient (max) 1.7
Reversible Swelling, Na+ to H+ 4%(max)
Temperature limit, H+ form 120 C
Temperature Limit, Na+ form 140 C
Pre Delivery Samples

Special Applications

Check for Compliance with Specification

Procurement Contract

Demonstrate Informed Client

Prior to Loading into Service Vessel

Last Chance !!

ARCHIVE SAMPLES

No of Batches

No of bags

Visual Inspection

Visual Microscopy
Periodically

Expected Resin Life?

2 years ? 5years ? 10 Years ?

Condition Monitoring Programme

Helps to identify a potential problem before it becomes a

performance issue

Trending Analysis

Forward Planning, Purchases and Budgets

Troubleshooting and Problem Solving

Plant Performance Problems

Investigations

Resin Sampling and Testing

One part of the Process

Caution
Resin Testing

Routine Tests

More Specialised Testing

Routine Tests

Visual Inspection
Microscopic Inspection
Separating the Resin
Cation Capacity (total, strong and weak)
Anion Capacity (total, strong and weak)
Particle Size Distribution
% Moisture retention
Visual Inspection

% Perfect Beads
% Cracked Beads
% Broken Beads
Surface Condition
Gel or Macroporous
Particle Size Distribution
Supernatant Liquor
Slide with portrait image image at users
discretion
Capacity - Cation Resins

Capacity

Total

Strong

Weak (by difference)

% Moisture Retention
Cation Capacity - Strong

CH2 CH CH2

SO3-H+
Cation Capacity - Weak

CH CH2 CH CH2 CH CH2

CO2H CO2H

CH CH2 CH CH2 CH CH2

CO2H CO2H
Crosslinked Acrylic Acid
Cation Resin Degradation
60
% Retained Moisture

50

40
0 1 2 3 4 5
TIME
Anion Resins

Capacity

Total

Strong

Weak (by difference)

Anion Capacity - Strong

CH2 CH CH2

Type I
CH2 Cl-
+
H3C N CH3

CH3
Anion Capacity - WEAK

CH2 CH CH2

CH2

H3C N

CH3
Degradation of Anion Resins

100

TOTAL

75 STRONG
% Remaining Capacity

50

25
WEAK

0
0 1 2 3 4 5 6
TIME
Particle Size

Standard Mesh (wet or dry)

Visible Light or Laser

Optical Cell

Parallel light

Gel resins

Macroporous resins
Resin Bead Size Distribution

Number of beads

Uniformity coeff 1.5 to 1.9

30 0 60 0 90 0 12 00 m
 Uniform Beads
No of Beads

Uniformity coeff. 1.2

450 600 750 900 m

 40
Particle Size 1

1
30
1
Number of Beads

20 1

0
10
0

0 0
200

300

400

500

600

700

800

900

1000
Bead Size / microns
Particle Size

45 100

40 90

80

Cumulative Percentage
35
Number of Beads

70
30
60
25
50
20
40
15
30
10 20

5 10

0 0
100

200

300

400

500

600

700

800

900

1000
Bead Size / microns
 Statistics of Measurement

660
Harmonic Mean

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20

650

640
Anion Kinetics

Condensate Polishing Plants (CPP)

High Flow
Anion Kinetics

Chloride

Sulphate

Carbon Dioxide
 Exchange Kinetics

B
A
B AResin
B
Bead
 MTC = V ln(C/C0)
SZA

MTC = Mass Transfer Coefficient (m/s)

C0 = inlet anion concentration (mg/l)

C = outlet anion concentration (mg/l)

V = volumetric flow rate (m3/s)

S = specific surface area of anion resin (m 2/m3)

Z = depth of resin bed (m)

A = cross section of resin bed (m2)

Specific Surface Area

S = 3.9
dHMS
dHMS = harmonic mean diameter (m)

MTC = Constant x dHMS ln(C/C0)

Effect of pH on MTC

2.5
Cl SO4
2
M T C (10- 4 m s-1)

1.5

0.5

0
4 5 6 7 8 9 10
Influent pH
Column Tests

Various Sizes

Small Scale Laboratory

Pilot Plant

Follower Rigs on Plant

 Hydrazine Breakthrough for Resin A
110

90
Hydrazine Concentration (ppm)

70

50

30

10

-10
0 100 200 300 400 500 600 700 800 900
Time (mins)
 Breakthrough Curve for Resin A

90

80

70

Hydrazine
Concentration (ppm)

60

50

40

30

20

10
Ammonia
0

-10
0 500 1000 1500 2000 2500 3000 3500 4000 4500

Time (mins)
 ORGANICS

Organic Extractables

Organic Fouling
 Organic Fouling Measurement(KMnO4 method)

Principle
Oxidise with potassium permanganate
Boil in acidic conditions
Titrate excess KMnO4
There is no direct
relation between
KMnO4 and TOC
Procedure measurement
100ml water + 2 ml 5 N H2SO4
Add 20 ml of 0.0125 N KMnO4
Boil for 10 minutes
Add 20 ml of 0.0125 N Mohrs salt {(NH4)2Fe(SO4)26H2O}
Titrate the excess of Mohrs salt with 0.0125 N KMnO4
Read volume required for titration = y ml
Organic matter = 4 y in mg/L as KMnO4 or y in mg/L as O2
Sampling

Most Important left to the end!

Should be Representative

Representative of What?

Whole Bed

Top of the Bed

Bottom of the Bed

Conclusions 1

See Resin Testing as one part of the bigger picture

Condition Monitoring proactive

Trouble shooting reactive

Trending
 Conclusions 2

Resin Testing is only one weapon in the armoury

Best used in conjunction with other Plant Monitoring Tools

Generally modern resins are strong and robust

Causes of Plant Performance Problems frequently lie elsewhere

 QUESTIONS