Samyang Corporation

31 Jong-ro 33-
gil, Jongno-gu,
Seoul, Korea
Tel: 82-2-740-
7732~7,7742
Fax: 82-2-740-
7790
www.samyangc
orp.com

Date: December 03 2021

Test Method for Ion Exchange Resin

Samyang Corporation 31 Jong-ro 33-gil, Jongno-gu, Seoul, South Korea Tel/Fax: 82-2-740-7742/7790, www.samyangcorp.com
 Test method for ion exchange resin

1 Preparation of stock solution

Prior to experiments, remove suspended solids, oils, and oxidizers from the stock
solution brought into contact with the ion exchange resin.

2 Selection of resin brand

There are two methods for selecting a resin brand while checking adsorption behavior:
the batch method and the column method. Each of these methods is described below.

2.1 Batch method

The batch method is a simple technique as an initial screening to test which resin
brand suits the intended purpose.
Place about 10 mL of conditioned resin into a beaker or Erlenmeyer flask, and pour
in the specified amount of stock solution. The preparation of the conditioning is
described later on section 3.3. Stir or shake vigorously enough for the resin
to float and rest for the resin to react about 0.5–2 hours. Then check the adsorption
effect by filtering the supernatant from the resin slurry and analyze the filtrate.
The adsorption rate can be calculated by conducting in fixed intervals.
Take a note on use of a magnetic stirrer as it may cause crushing of the resin.

2.2 Column method

Fill a column with 10–20 mL of the conditioned resin, and allow stock solution to
flow at a flow velocity of SV 5–20. Sample a fixed amount of the treated liquid,
analyze, and check effectiveness. Use a low flow velocity if the molecular weight of
the adsorbed material is high, or if the viscosity of the liquid is high.

Samyang Corporation 31 Jong-ro 33-gil, Jongno-gu, Seoul, South Korea Tel/Fax: 82-2-740-7742/7790, www.samyangcorp.com
 3 Determination of test conditions
Once a particular type of resins is chosen, conduct a column liquid passage test to check
liquid passage conditions for industrialization purposes and to optimize regeneration
conditions.
(As a special case, industrialization may be done using the batch method.)

3.1 Experimental equipment

In the case of a small-scale experiment for resin selection, as indicated above, it is
convenient to use a 10–15 mm (dia.) glass column for the experiment, but for this
experiment, use a column with a diameter of about 20 mm or more, and set the
height of the layer filled with ion exchange resin to 60 cm or higher. In addition, when
performing backwashing, the column must have backwashing space roughly the same
as the resin layer height.

(If the purpose is not to collect design data, then a scale smaller than the above
conditions is fine, and there is no need to perform backwashing.)

Care is needed when using a PVC or acrylic column because there are restrictions on
factors such as solvents used and experiment temperature.

Fix the column perpendicular to the support stand etc. Fig. 1 shows an example of
the experimental equipment.

If there is no pump, the stock solution container can be placed at a location higher
than the column, and liquid allowed to flow due to gravity.

When using a resin with large changes in volume due to the ion form, such as
weakly acidic cation exchange resin or weakly basic anion exchange resin, there is a
risk of column damage due to swelling pressure of the resin. Therefore, please
consider to use a large-diameter glass column in such a case.

Samyang Corporation 31 Jong-ro 33-gil, Jongno-gu, Seoul, South Korea Tel/Fax: 82-2-740-7742/7790, www.samyangcorp.com
 Fig. 1: Equipment

3.2 Resin filling method

When filling resin into the column, take the specified amount of resin, obtained by
accurately measuring volume in water beforehand using a measuring cylinder, and
add while in the slurry state into the column filled with water (Fig. 2).
At this time, be careful not to allow air bubbles into the resin layer. If air bubbles
get in, insert a rod or similar tool, and remove the air bubbles.

Fig. 2: Resin filling method

Samyang Corporation 31 Jong-ro 33-gil, Jongno-gu, Seoul, South Korea Tel/Fax: 82-2-740-7742/7790, www.samyangcorp.com
 3.3 Resin conditioning
The ion form of a typical strongly acidic resin or strongly basic resin is a salt (Na or Cl)
form. Also, even some weakly acidic resins and weakly basic resins have a salt form.
Therefore, the following regeneration procedure must be performed as resin
conditioning before use.

The amounts of regeneration agent used are as follows. These are twice the
amounts for normal regeneration.

Strongly acidic resin 300–500 g-HCl/L-R

Strongly basic resin 300–500 g-NaOH/L-R
Weakly acidic resin 100–150 g-HCl/L-R
Weakly basic resin 100–150 g-NaOH/L-R

*When an ion exchange resin is first used, there is elution of trace amounts
of impurities. The procedure for quickly reducing these elutes is also called
conditioning. The procedure for this purpose involves repeating the regeneration
and salt load steps 2–3 times.

3.4 Steps of ion exchange resin procedure

As a typical example of the regeneration/liquid passage procedures, the following
shows the procedure steps. For details on each step, see "4. Experiment
procedure" below.

Samyang Corporation 31 Jong-ro 33-gil, Jongno-gu, Seoul, South Korea Tel/Fax: 82-2-740-7742/7790, www.samyangcorp.com
 Backwashing Expansion rate is 1.3–1.5 times the resin layer height. 15–30 min

Settling down 5-10 min

Water draining About 5 cm above the resin surface

Regeneration See 4.4

Expulsion 1.5–2 BV at same flow velocity as regeneration step

Washing (1) 30–60 min at same flow velocity as liquid passage step

Sweetening on 1–2 BV at same flow velocity as liquid passage step

See 4.8
Liquid passage

1–2 BV at same flow velocity as liquid passage step

Sweetening off

Washing (2) 15–30 min at same flow velocity as liquid passage step

Samyang Corporation 31 Jong-ro 33-gil, Jongno-gu, Seoul, South Korea Tel/Fax: 82-2-740-7742/7790, www.samyangcorp.com
4.0 Experiment Procedure
The following explains the experiment procedure for the column method, but
steps 4.1 Backwashing – 4.2 Settling down can be omitted depending on the
situation. In addition, if there is no need to recover liquid, there is no need to
perform 4.7 sweetening on and 4.9 sweetening off.

4.1 Backwashing
This is performed to discharge, to the outside of the column, the
suspended solid (SS) component mixed in during liquid passage and
the resin crushed during use, and to improve contact efficiency with
the regeneration agent by loosening the compacted resin layer.
Perform backwashing with an upward flow at a flow velocity so that
the resin layer expands by 1.3–1.5 times, until the water flowing out is
transparent. The backwashing expansion rate varies in each case
depending on the brand used and the water temperature, so set flow
velocity based on DIAION Data Sheets.

4.2 Settling down

This step allows the resin layer, expanded due to backwashing, to naturally settle.

4.3 Water draining

After the settling down step is finished, this process drains off water at the top of
the column to a position about 5 cm above the resin surface. This is done to avoid
dilution of the regeneration agent.

4.4 Regeneration
This step converts a resin in the salt form to the regenerated form. The type of
regeneration agent and the amount used varies in each case depending on the resin
used.
Typical regeneration agent concentrations are as follows.

Strongly acidic resin 3–8% HCl or H2SO4

Strongly basic resin 3–8% NaOH
Weakly acidic resin 0.5–5% HCl
Weakly basic resin 0.5–5% NaOH

Samyang Corporation 31 Jong-ro 33-gil, Jongno-gu, Seoul, South Korea Tel/Fax: 82-2-740-7742/7790, www.samyangcorp.com
 Time needed to supply regeneration agent is roughly 30 min with a strongly acidic
resin. In the case of a strongly basic resin, roughly 45 min is a good guideline.
Even if the regeneration level is raised to a fixed level or higher, it is not possible to
obtain a regeneration effect corresponding to the amount of regeneration agent
used. Therefore, it is typical to perform management using the following
regeneration rates and amounts of regeneration agent used.

Samyang Corporation 31 Jong-ro 33-gil, Jongno-gu, Seoul, South Korea Tel/Fax: 82-2-740-7742/7790, www.samyangcorp.com
 Regeneration rate Amount of
regeneration agent
used
Strongly acidic resin 50–70% 100–300 g/L-R
Type I 30–50%
Strongly basic resin Type II 50–70% 100–300 g/L-R
Weakly acidic resin 80–100% 60–120 g/L-R
Weakly basic resin 80–100% 60–120 g/L-R

*The regeneration method above is for resin which has adsorbed impurities (unnecessary
material). The resin may also be used in cases where valuable material is adsorbed using special
chemicals. In those cases, there are two approaches: eluting the target material using an
appropriate eluent and then performing elution; or performing elution and regeneration together.

4.5 Expulsion
This step is an extension of regeneration. Here, unreacted regeneration agent remaining in
the column is expelled using pure water at the same flow velocity as regeneration. The amount
of pure water used is 1.5–2 times the amount of ion exchange resin.

4.6 Washing (1)

This step is for completely removing regeneration agent remaining in the column. Normally, this
is performed for 30–60 min at the same flow velocity as the liquid passage process. The
process up to this step completes the regeneration process.

4.7 Sweetening on
When performing treatment with a special chemical liquid, water in the resin layer is steadily
replaced due to the liquid being passed through. "Sweetening on" refers to this replacement
step.

4.8 Liquid passage

Recovery as treatment liquid begins from the point where the chemical liquid at the column
outlet reached or exceeded a certain concentration, and continues until ion leakage occurs and
the specified liquid quality is no longer obtained. This process is called liquid passage. Flow
velocity during liquid passage is SV20–50 in ordinary water treatment. In other cases it is SV10 or
lower.

Samyang Corporation 31 Jong-ro 33-gil, Jongno-gu, Seoul, South Korea Tel/Fax: 82-2-740-7742/7790, www.samyangcorp.com
 4.9 Sweetening off
In treatment with chemical liquid, this is the process of replacing the stock solution in the column
with water after passing through the chemical liquid. The term applies until the outlet stock
liquid concentration is at or below the specified concentration. This portion is recovered as
treatment liquid or sweet water.

4.10 Washing (2)

In treatment with chemical liquid, this is performed in the same way as washing after
regeneration. The amount of washing water used is about 1/2 that used after regeneration.

5 Check items for equipment development

Assuming that actual equipment will be developed, check factors such as liquid passage flow rate,
temperature, treatment amount, regeneration level, service life, etc., and set optimal treatment
conditions. Items to be checked are indicated below, but it is difficult to estimate life with ordinary
column tests. Therefore, perform other tests such as accelerated cycle tests, long-term testing using
a pilot plant, or a sample hanging test is actual equipment is in operation.

*Liquid passage conditions *Regeneration conditions

-Treatment amount -Chemical type
-Liquid quality -Amount used
-Flow velocity -Concentration
-Temperature -Flow velocity
-pH, etc. -Temperature

A pilot plant may be operated to recheck and evaluate design conditions, and to manufacture
samples for distribution. Normally, the plant is 1/10 the scale of the actual equipment, and even a large
pilot plant operates with resin amounts of about 50–100 L.

Samyang Corporation 31 Jong-ro 33-gil, Jongno-gu, Seoul, South Korea Tel/Fax: 82-2-740-7742/7790, www.samyangcorp.com