Technical Bulletin

Chemicals / TB72A / 05-2009

Evaluation of Activated Carbon in Liquid Phase Applications

Preparation of Isotherms

1. Introduction

In liquid phase applications, activated carbon is predominantly used as an adsorbent for the removal of
organic impurities. The affinity of activated carbon for organic species depends on the size and polarity of
the organic species to be removed and the pore structure and surface chemistry of the carbon used.
The adsorption capacity (the amount of organic adsorbed per gram carbon) of activated carbon depend on:
• the physical and chemical appearance of the target compounds,
• the initial concentration of the target compounds,
• the equilibrium final concentration of the target compounds,
• competing adsorption of organic species other than the target compounds,
• temperature,
• pH of process liquor.

As there are thousands of applications for powdered and granular activated carbon and hundreds of grades
it is often essential to perform lab. scale tests in order to find the most suitable and economical grade for
any specific application.

This technical bulletin contains the complete method for the laboratory evaluation of powdered and
granular activated carbon by means of the adsorption isotherm technique. It is a general procedure,
suitable for any type of application and any type of activated carbon.

2. General

If you are evaluating activated carbon for the first time, it is recommended to contact Norit®. We can assist
you in making a preliminary selection of two or three carbon types most suitable for your initial laboratory
tests.

It is essential to perform the tests using the actual solution to be purified in your plant. Type and origin of
the impurities may differ substantially, even from production line to production line.

Any particles or suspended material can influence the purification process. Preferably the solution to be
treated is pre-filtered prior to contact with carbon to minimize distortion of the results.

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3. The Evaluation of Powdered Activated Carbon

3.1. General

Different carbon quantities are added to a series of batches containing the liquid to be purified. The
batches are equilibrated during a specified contact time under conditions representing practical operation
as closely as possible. Thus, a relation between carbon dosage versus final concentration of the compound
of interest reveal. Generally, carbon performance under practical conditions may be simulated quite well.
Depending on the experimental set up, test results yield:
• Selection of most cost effective carbon grades (price/performance wise).
• Optimization of conditions (contact time, pH, temperature).

3.2. Determine the optimum contact time

The first step in the evaluation of powdered activated carbon is to determine the optimum contact time in
which equilibrium conditions are reached. These tests should be performed using the actual process liquid
at the actual process temperature.
This first step may be ignored by assuming an optimum contact time of one hour. However, for applications
involving viscous liquids (> 4 cP), low temperatures or impurities difficult to remove, a contact time more
than one hour is preferred.

The following lab procedure is commonly used:

• Add 200 ml samples of the test solution to each of six 300 ml Erlenmeyer flasks. If only a small
amount of test solution is available, use 100 ml in 200 ml flasks.
• Heat the flasks to the normal process temperature.
• Add a fixed amount of activated carbon to 5 of the flasks, the 6th one is the blank. The amount of
carbon used is usually between 0.2 to 0.5 g/100ml or somewhere near the smallest dosage
expected to use in the adsorption isotherm tests that follows.
• Agitate the samples for varying time periods. Contact times of 10, 20, 40, 60 and 120 minutes may
be used. These time periods are chosen on the basis of general industrial experience.
• After mixing, immediately filter each of the six samples.
• Analyse the filtrate to determine the amount of impurity remaining in the solution. You can use
any standard method depending on the species of interest.
• Plotting the % impurity removed vs. the contact time will yield a curve that usually has a sharp
break at the level of optimum contact time. Use this contact time in the second step of this
method.

If you are evaluating several different carbon types, it is sometimes necessary to determine the optimum
contact time for each carbon type. Especially when comparing samples with different particle sizes. In
figure 1 an example of a contact time curve has been included.

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 IMPURITY REMOVED (%) 100

50

0
0 30 60 90 120
CONTACT TIME (min)

Figure 1: Contact time curve

3.3 Obtaining an adsorption isotherm

After establishing the optimum contact time, the second step is the preparation of an adsorption isotherm.
Again, the tests should be performed using the actual process liquid at the actual process temperature. The
following method will help you determine the adsorption capacity of a carbon sample:

• Prepare a series of five 300 ml Erlenmeyer flasks, containing a certain amount of carbon. Typical
the amount of carbon range from 0.10 to 2.0 grams. This range must include at least one point
with sufficient carbon to adsorb the impurities to a level below the target level.
• Add 200 ml of the test liquid to be purified to each flask. Add 200 ml of test liquid to an empty
flask as blank.
• Agitate the samples at the normal process temperature during the optimum contact time
determined earlier. If the optimum contact time was not established then agitate for one hour.
• Immediately filter each of the six samples.
• Analyse the filtrate to determine the amount of impurity remaining in the solution. You can use
any standard method depending on the species of interest.

Repeat this method for each of the activated carbon grades tested.
If the target level of the impurity is not reached, the tests have to be repeated with higher carbon dosages.
If you are still not reaching your target level, it is recommended to contact Norit®

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3.4 Interpreting the results

Next step is the interpretation of the test results. The common method is to prepare a graph in which the
impurity remaining is plotted against the carbon dosage. Ideally, this will produce a graph as shown in
figure 2.

Figure 2: Adsorption isotherm of powdered activated carbon

Using this graph the carbon dosage required to meet your purity requirements can readily be seen.
This simplified method can be used to compare the performance of different powdered carbon samples
and help you find the most promising sample on a cost-performance basis.

4. The Evaluation of Granular Activated Carbon

4.1. General

For an isotherm study granular activated carbon (GAC) is ground first before testing. The principle of the
test is similar to the test for powdered activated carbon. Isotherms tests provides an indication of the
maximum amount of impurity a granular activated carbon can adsorb, it can not give definite scale up data
for a GAC operation due to several factors:
• In a GAC column, dynamic adsorption occurs along an adsorption wave front where the impurity
concentration changes.
• GAC rarely becomes totally exhausted in a column.
• Ground GAC exhibits a significant greater rate of adsorption than a normal GAC.
• Effects of recycling with regeneration can not be studied
Thus the test is an indicative method basically for preselection purposes only.
For accurate performance tests and process design purposes read technical bulletin
TB 72B "Pilot column tests with granular carbon". For further information about performing
column tests please contact Norit.

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4.2. Obtaining an adsorption isotherm

Tests with ground granular activated carbon should be performed using the actual process liquid at the
actual process temperature. The contact time should be sufficient to reach equilibrium.

• Grind the carbon so that 95 % will pass through a 44 µm/325 mesh sieve. Dry the ground sample
at 120°C overnight in an oven.
• Prepare a series of five 300 ml Erlenmeyer flasks, containing a certain amount of carbon. Typical
the amount of carbon range from 0.10 to 2.0 grams. This range must include at least one point
with sufficient carbon to adsorb the impurities to a level below the target level.
• Add 200 ml of the test liquid to be purified to each flask. Add 200 ml of test liquid to an empty
flask as blank.
• Agitate the samples at the normal process temperature during the chosen contact time.
• Immediately filter each of the six samples.
• Analyse the filtrate to determine the amount of impurity remaining in the solution. You can use
any standard method depending on the species of interest.

4.3. Interpreting the results

The commonly used method of evaluating the test results is the Freundlich Equation. This equation
mathematically describes adsorption attained under equilibrium conditions. The Freundlich Equation is
usually written in the following form:

q = K * C 1/n
e

where:
q = amount of impurity adsorbed per amount of carbon used (mg/g).
Ce = concentration of impurity remaining (mg/l).

K and n are constants specific to the equilibrium conditions.

A plot of q (carbon loading) vs Ce (impurity remaining) on log-log scale usually yields a straight line as can
be seen in figure 3.

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 Figure 3: Freundlich isotherm of granular carbon

By extrapolating the Freundlich isotherm to the influent concentration the maximum achievable carbon
loading (mg/g) can be found. From the impurity removal and the carbon loading follows the carbon usage rate
(g/l):

Co - Ct
Carbon usage rate = _____________
Carbon loading

where:
C0 = influent impurity concentration (mg/l)
Ct = target impurity concentration (mg/l)

Adsorption isotherms help to determine if it is possible to reach a desired purity level with activated carbon.
Also, isotherms present a carbon loading value defined as the amount of impurity per unit weight of carbon.

The position and slope of each line reveal how well a carbon will perform compared to other carbons
evaluated. Generally, a line higher up on the graph means that this carbon will have a higher adsorption
capacity than one lower on the graph. A more vertical line indicates good adsorptive properties at the influent
concentration but poor adsorptive properties particularly at lower concentrations. A nearly horizontal line
indicates better adsorption throughout a wider range of concentrations.
In general, the carbon which exhibits the steeper slope will be more effective during well designed column
operations.

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 In some cases the Freundlich isotherm will be non-linear. In particular in case of a residual non-adsorbable
fraction of the target compounds the isotherm will show a sudden change in slope.

If there are still questions about performing isotherms please contact Norit

5. Laboratory Tips

Following are some useful laboratory tips based on our own experiences. They will help you produce more
reliable data.

• Check the amount of solution that has evaporated during the test and correct the volume before
measuring the impurity. This is of considerable importance at higher temperatures.
• Be sure that all the activated carbon is filtered off.
• Use screw cap Erlenmeyer flasks when testing with volatile species.
• Check the pH of the test solution before and after carbon treatment and the activated carbon
used, if your product is pH sensitive.
• If there are tight limits for mineral impurities in the liquid to be purified, check then before and
after carbon treatment.
• In recording and evaluating data, always express dose rate in terms of mass of activated carbon
per unit of material to be purified. For example the unit for applications such as sugar refining is
weight based on dry material, for glycerin the unit is volume based.
• It is important to obtain isotherms that cover the entire range of concentrations especially with
Freundlich isotherms.

Caution: For health and safety related aspects of a Norit activated carbon, please refer to the corresponding Material Safety Datasheet (MSDS),
which is available on request.

This information is provided as a convenience and for informational purposes only. No guarantee or warranty as to this information, or any
product to which it relates, is given or implied. Cabot disclaims all warranties express or implied, including merchantability or fitness for a
particular purpose as to (i) such information, (ii) any product or (iii) intellectual property infringement. In no event is Cabot responsible for, and
Cabot does not accept and hereby disclaims liability for, any damages whatsoever in connection with the use of or reliance on this information or
any product to which it relates.

This Technical Bulletin (Issue 05-09) replaces previous issues.

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