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Isotherm Test Rev2

Isotherm Test Rev2

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MEASURING

ADSORPTIVE
CAPACITY OF
POWDERED
ACTIVATED
CARBON
Introduction.
Norit Americas Inc. produces over 150 different varieties of
activated carbon. This diverse product line provides many
options for carbon adsorption. Isotherm testing can aid in the
process of choosing the best carbon for your purification needs.
Pore volume
available to
both adsorbates
and solvent.
Pore volume
available only
to solvent and
smaller adsor-
bate molecules.
Porosity
available only
to solvent.
Pore size
too small
for adsorption
of impurities
from liquids.
Electron microscope photo of steam activated carbon.
A powdered carbon’s ability to remove impurities
from a liquid is evaluated using laboratory scale
batch treatment tests or “ Isotherms”. Data from
these laboratory adsorption tests may be used to
calculate the carbon’s capacity for impurity removal,
or its “adsorptive capacity”. These laboratory scale
tests are also useful to identify the best performing
carbon type and to define the relative economics of
powdered carbon treatment.
The same laboratory procedures can also be used
as an initial screening of granular carbons, provided
they are ground to a fine powder before testing.
Normally, granular carbon is used in columns or
tanks, with the process liquid flowing continuously
through the bed of granular carbon. As a result, a
laboratory batch adsorption test at equilibrium will
not give accurate data for design of a granular
carbon adsorption system. Pilot column tests are
required to accomplish this and define process
economics when granular carbon is used. The pro-
cedure for running pilot column tests is described
in brochure number NA00-4 and can be obtained
by calling Norit Americas Inc.
Liquid Phase Adsorption Theory.
Knowledge of the adsorption process will provide a better
understanding of the dynamics of using carbon in a particular
purification application. Therefore, it is important to have an
overview of liquid phase adsorption theory and how it relates to
laboratory testing.
In a batch treatment process using powdered acti-
vated carbon, adsorption of impurities from a liquid
is essentially an equilibrium phenomenon. The first
step of the process involves migration or diffusion
of the impurities into the porous cavities within the
carbon particles. Once inside the pore structure,
the impurity molecules are attracted to the internal
pore surfaces by weak electrostatic forces known
as van der Waals’ forces. This “ physical adsorp-
tion” of impurity molecules onto the internal surface
of the pore structure is the most common type of
adsorption and is reversible. Physical adsorption
can be an advantage in some separation scenarios
in which the adsorbed material is the desired
product. After adsorption, a change in processing
conditions may cause the product to desorb from
the carbon. Gold recovery and antibiotic production
are two examples of this.
In some cases, the adsorbed material may interact
with active sites on the carbon pore surfaces and
form chemical bonds with the surface. This process
is called chemisorption and is considered irreversible.
Powdered activated carbon usually works well in
applications involving removal of trace contami-
nants from liquids. Evaluating the economics of the
process requires answering two questions:
will carbon adsorb the impurity to an acceptable
level and what is the cost? Most organic chemical
impurities are adsorbed on carbon to some extent.
To determine how well activated carbon will purify
your process liquid, you must determine the carbon’s
“ adsorptive capacity”. This is done in the laboratory
by conducting an adsorption isotherm test.
Standard laboratory analytical tests such as Iodine
Number, Phenol Value, or Surface Area can be
misleading as a predictor of carbon performance.
These “ surrogate” tests do not necessarily relate
to a carbon’s ability to adsorb the specific impurities
in your process stream. For example, the Iodine
Number test procedure measures removal of iodine
from a standard solution. Carbons with the highest
Iodine Number value are frequently not the best
choice for color removal in food processing or for
taste and odor removal from potable water. What
must be done to select the best carbon for your
application is to conduct an adsorption isotherm
test on your specific process stream.
There are several important factors that must be
considered when evaluating adsorptive capacity.
In most process streams, there are numerous types
of impurities present at different concentration levels.
All of these impurities are competing with each other
in the adsorption process. Since different impurity
types are adsorbed at different rates and in different
amounts, it is very important that laboratory tests
be conducted using the actual process liquid. An
accurate measurement of a carbon’s adsorptive
capacity also requires duplication of the actual plant
processing conditions in the laboratory. Physical
and chemical properties such as pH, temperature,
impurity concentration, and viscosity can affect
adsorption and must be duplicated in your labora-
tory isotherm testing. Additionally, the physical size
distribution of the carbon samples tested must be
consistent because carbon particle size affects the
rate of adsorption.
Measuring Adsorptive Capacity.
Laboratory tests for measuring adsorptive capacity are
designed to be rapid screening methods for determining the
performance of activated carbon. For batch treatment using
powdered carbon, results from laboratory isotherm tests con-
ducted at equilibrium will correlate directly with full scale plant
process performance. The laboratory tests can accurately
measure adsorptive capacity of different types of activated carbon
and identify the carbon type with the best cost performance.
To achieve accurate results, the adsorption measurements
must be made under equilibrium conditions. Therefore, Step 1
in your laboratory testing is to determine the minimum contact
time required to establish equilibrium conditions.
STEP 1: Determine the Test Conditions.
An activated carbon sample must reach adsorption
equilibrium to measure its total adsorptive capacity.
Normally, a contact time of one hour is sufficient.
However, applications involving viscous liquids, low
temperatures, or impurities that are difficult to adsorb
might require longer contact times. To determine
the optimum contact time, you should expose a
series of liquid samples to the same carbon treat-
ment dosage for different time periods using test
conditions that match the plant process (impurity
type, concentration, pH, temperature, etc.).
The lab procedure commonly used is as follows:
1. Laboratory tests must be run on samples of the
actual process liquid and actual plant processing
conditions must be duplicated as closely as possible.
2. A predetermined weight of carbon is added to
each of five bottles. The amount of carbon used is
typically 0.1% to 0.5%, by weight, for treating
process liquids, which usually have relatively high
concentrations of impurity present. For potable
water or wastewater with less than 5 ppm of impu-
rity, the carbon dosage used may be in the range
of 5 to 200 ppm. The carbon dosage used in these
contact time tests should be near the smallest
dosage you expect to use in the adsorptive capacity
tests, which will be conducted later.
3. Transfer 200 mL (or 200 grams) of the process
liquid to each of the bottles and seal the bottle.
4. Agitate the samples at the same process temper-
ature and test conditions for different time periods.
Contact times of 10, 20, 30, 60, and 120 minutes
may be used.
5. After mixing the carbon and liquid for the specified
contact time, immediately filter each sample to
separate the process liquid from the carbon.
Analyze the filtrate to determine the impurity
remaining in the solution. You can analyze the
residual impurities by any number of methods,
depending on the impurity of interest. Commonly
used analytical methods include spectrophotometry,
titration, chromatography, or gravimetric methods.
6. Prepare a graph with the impurity removed (or
remaining) on the Y-axis vs. the carbon contact
time on the X-axis. The test results will produce a
plot as shown in Figure 1. There is usually a sharp
break in the curve at the optimum contact time.
Contact times in excess of this value have a very
limited effect on removal of additional impurity or
increases in carbon adsorptive capacity.
When evaluating several different carbon samples,
you will find it necessary to determine the contact
time for each carbon type. This is particularly true
when comparing samples with different particle sizes.
CONTACT TIME (min)
I
M
P
U
R
I
T
Y

R
E
M
O
V
E
D

(
%
)
Figure 1
CONTACT TIME TEST RESULTS
Step 2: Obtain Your Adsorption Data.
Once the optimum contact time is determined, the
next step is to measure the total adsorptive capacity
of the activated carbon. This must be done using
the actual process liquid and running the tests at
actual process conditions that exist in the full-scale
plant. You should also establish a treatment goal
for impurity removal to provide a basis for selection
of the range of carbon dosages to use. This may
be an arbitrary number to obtain an acceptable
product quality level or it may be a number estab-
lished by a regulation governing the process.
Impurity removal levels may range from 50% to
over 99%, depending on the nature of the impurity
to be removed.
The following method may be used to measure
the adsorptive capacity of a carbon sample.
1. Different amounts of carbon are added to six
bottles. At least one of the bottles should contain
sufficient carbon to remove impurities to a concen-
tration level that is below the desired treatment
goal. Carbon dosages may range from a low of
0.05% to 5% when treating process liquids.
Dosages for water and wastewater treatment
are usually significantly lower.
2. Add 200 mL (or 200 grams) of the test liquid to
each bottle, and seal the bottle. Test liquid (200
mL) is also added to a bottle containing no carbon,
to act as a control sample.
3. Agitate the samples under identical process condi-
tions for the optimum contact time determined earlier.
4. Immediately filter the samples to remove the
carbon from the solution.
5. Analyze the samples using the best method
for determining the residual impurity level you are
trying to reach.
If at least one of the carbon treated samples meets
the impurity removal goal, you are ready to interpret
the test results. If the target level is not reached,
you may need to repeat the test with higher carbon
dosages. In the event you are still unable to meet
your treatment goal with higher carbon dosages,
different process conditions or techniques may
be required.
Step 3: Interpret Your Results.
Carbon Dosage Method
There are two basic approaches to interpreting the
test results for carbon adsorptive capacity. The
first is to directly plot the amount of impurity
remaining vs. the carbon dosage. Ideally, this will
produce a plot as shown in Figure 2. This “ linear
scale” Isotherm Plot can be used to determine the
required carbon dosage. Locate on the curve the
targeted impurity remaining level, and draw a
vertical line down to the X-axis to identify the
required carbon dosage. You may also calculate
the adsorptive capacity or “ carbon loading”
at this carbon dosage as follows:
Adsorptive
Wt. Impurity Adsorbed
Capacity
Carbon Weight
This simplified isotherm technique may be used to
compare the performance of different carbon sam-
ples and to identify the most cost-effective carbon.
You could also use it to determine how impurity
removal and adsorptive capacity are influenced by
changes in process conditions, such as pH, tem-
perature, impurity concentration, or impurity type.
Freundlich Adsorption Equation Method
Sometimes the lab isotherm data does not produce
a plot that is easy to interpret, as indicated in
Figure 2. The curve may be very flat at high levels
of impurity removal. This makes it difficult to deter-
mine the carbon usage rate accurately. In such
cases, a different approach is used to evaluate the
data based on the Freundlich Adsorption Equation.
This equation describes mathematically the rela-
tionship between the amount of impurity adsorbed
at equilibrium and the impurity concentration. It is
usually written as follows:
X/M = KC
1/n
X = Amount of impurity adsorbed at equilibrium
M = Weight of carbon used
C = Concentration of impurity remaining in liquid
K & n = Constants specific to test conditions and
the carbon type used
When expressed in logarithmic form, this empirical
equation becomes a straight line equation with a
slope of 1/n and Y-axis intercept of log K. A loga-
rithmic scale plot of X/M on the Y-axis and C on the
X-axis usually results in a straight line. Such plots
are referred to as Freundlich Adsorption Isotherms.
CARBON DOSAGE, g/200mL
I
M
P
U
R
I
T
Y

R
E
M
A
I
N
I
N
G
,

m
g
/
L
Figure 2
ADSORPTION ISOTHERM
=
An adsorption isotherm plotted on a logarithmic
scale often makes it easier to determine carbon
loading at the desired level of impurity removal.
Figure 3 is an example of a Freundlich Isotherm plot.
Adsorption isotherms provide useful information for
estimating performance in a full scale process
stream. First, they help determine if it is possible to
reach a desired purity level with activated carbon
treatment. This is especially important when multi-
ple impurities are present and one or more impuri-
ties are poorly adsorbed. Second, isotherms allow
calculation of carbon loading (X/M) at equilibrium,
which has a major impact on process economics.
Note that Figure 3 and the Freundlich equation
show that carbon loading depends upon the equi-
librium concentration of impurity remaining in the
process liquid. Carbon loading will be higher at
higher impurity concentrations.
Adsorption isotherms can also be used to predict
the relative performance of different types of car-
bon. The position and slope of the isotherm lines
reveal how well one carbon performs relative to
another carbon. A higher isotherm line means that
carbon has better adsorptive capacity than one
with a lower isotherm line. When the isotherm line
is nearly horizontal, it means the carbon has good
adsorption of impurity throughout a wide range of
impurity concentration. A nearly vertical isotherm
line shows poor adsorptive properties at lower
impurity concentrations.
The following sample problem and calculation will
illustrate how you may make effective use of the
Freundlich Adsorption Isotherm to determine a car-
bon’s adsorptive capacity. It also shows how to
compare the relative performance of two different
types of powdered activated carbon.
Sample Calculation.
A process liquid contains 400 ppm (mg/L) of an
impurity that must be reduced by 95%. Laboratory
adsorption tests were conducted with two types of
carbon (A and B) to determine if the desired impuri-
ty removal could be achieved. The purification goal
is less than 20 mg/L of impurity remaining after
carbon treatment. A tabulation of the test results
is given in Table 1.
The test data from Table 1 are plotted on a logarith-
mic scale in Figure 4, which shows the adsorption
isotherms for Carbon A and Carbon B. Both carbons
achieved the desired level of purification (less than
20 mg/L of impurity remaining). You can easily see
IMPURITY REMAINING, mg/L
C
A
R
B
O
N

L
O
A
D
I
N
G
,

m
g
/
g
Figure 3
FREUNDLICH ADSORPTION ISOTHERM
IMPURITY REMAINING, mg/L
X
/
M
,

m
g
/
g
Carbon A
Carbon B
Figure 4
ADSORPTION ISOTHERM
that Carbon A is the best performing carbon,
because at all impurity concentrations the amount
of impurity adsorbed per unit weight of carbon
(X/M) is higher than the corresponding value for
Carbon B. Carbon usage rates are calculated for
each carbon as illustrated below.
1. Determine carbon loading (X/M) directly from
the isotherm plots at the desired final impurity level
(20 mg/L).
Carbon A X/M = 74 mg/g
Carbon B X/M = 48 mg/g
2. Calculate impurity removal. This is the same for
both carbons: 400 mg/L – 20 mg/L = 380 mg/L
3. Carbon usage rate is determined by dividing the
amount of impurity removed (380 mg/L) by the car-
bon loading (X/M).
Carbon A Usage = 380/74 = 5.1 g carbon/L
Carbon B Usage = 380/48 = 7.9 g carbon/L
From the calculated results, it is apparent that
approximately 55% more Carbon B is required to
achieve the same treatment results as obtained
with Carbon A. Finally, the unit prices of each carbon
type can be used to determine the most cost-effec-
tive activated carbon for this purification application.
Conclusion.
Laboratory adsorption testing is the only way you
can determine how effective an activated carbon
will be in your purification process. Accurate, unbi-
ased testing on the actual process liquid at plant
process conditions will provide data that you can
use confidently. This type of testing is the only
effective way to compare carbons for a particular
application.
Norit Americas Inc. produces the most diverse
product line of activated carbon in the world. With
over 80 years of technological expertise, we are
one of the most experienced manufacturers of pow-
dered, granular, and extruded activated carbons.
Norit Americas Inc. has the capabilities and the
resources to recommend the right carbon for your
purification needs.
Carbon
Dosage
(g/200mL)
0
0.08
0.16
0.32
0.64
1.95
Carbon
Dosage
(g/L) (M)
0
0.4
0.8
1.6
3.2
9.75
Impurity
Removed
(mg/L) (X)
0
152
236
308
366
390
Impurity
Removed / Unit
Weight of Carbon
(mg/g) (X/M)
0
380
295
193
114
40
Concentration
of Impurity
Remaining
(mg/L) (C)
400
248
164
92
34
10
Carbon
Dosage
(g/200mL)
0
0.08
0.16
0.32
0.64
3
Carbon
Dosage
(g/L) (M)
0
0.4
0.8
1.6
3.2
15
Impurity
Removed
(mg/L) (X)
0
120
200
280
340
391
Impurity
Removed / Unit
Weight of Carbon
(mg/g) (X/M)
0
300
250
175
106
26
Concentration
of Impurity
Remaining
(mg/L) (C)
400
280
200
120
60
9
C
A
R
B
O
N

A
C
A
R
B
O
N

B
Table 1
ISOTHERM DATA
©2001 NORIT NA00-3 2000
Norit Nederland BV
Amersfoort, The Netherlands
Telephone: 31334648911
Telefax: 31334617429
Norit (U.K.) Ltd.
Glasgow, Scotland
Telephone: 441416418841
Telefax: 441416410742
Norit (France) S.a.r.l.
Paris, France
Telephone: 33145910808
Telefax: 33148673603
Norit Italia S.p.A
Ravenna, Italy
Telephone: 39544451514
Telefax: 39544451283
Norit Deutschland G.m.b.H.
Düsseldorf, Germany
Telephone: 49211906020
Telefax: 49211161115
N.V. Norit Belgium S.A.
Brussels, Belgium
Telephone: 3226750645
Telefax: 3226751119
Norit (Japan) Co. Ltd.
Minato-Ku, Tokyo, Japan
Telephone: 81352952850
Telefax: 81352952860
Norit Singapore Pte. Ltd.
Singapore, Singapore
Telephone: 657353066
Telefax: 657353166
Norit Americas Inc.
3200 West University Avenue
Marshall, TX 75670
800-641-9245
Telephone: 903-923-1000
Telefax: 903-923-1003
www.norit-americas.com
e-mail: info@norit-americas.com

www.norit-americas.com

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