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Jeff Yee

Hayden Robbins
Mohammed Al Hashim

Adsorption of Acetic Acid with Activated Carbon


Experiment 6

Objective

To study the effects of activated carbon in adsorption processes and to


determine the maximum amount of adsorption (qmax).

Introduction

Sorption refers to the action of either absorption or adsorption. It is the effect of


gases or liquids being incorporated into a material of a different state and adhering to
the surface of another molecule.

Sorption processes are very important in the fate and transport of contaminants
in the environment and also in the removal of contaminant, usually with the use of
reactors, for the following removal purposes:

● Removal of color from dye mill wastewater


● Removal of surface activate reagents from water
● Removal of total organic carbon from industrial wastewater
● Removal of taste or odor constituents, or both, from the potable water
Absorption is the incorporation of a substance in one state into another of a
different state (e.g. liquids being absorbed by a solid or gases being absorbed by a
liquid). Adsorption is the physical adherence or bonding of ions and molecules onto the
surface of another molecule or in another word adsorption is a surface phenomenon in
which the rate and the extent of adsorption are functions of the surface area of the
solids used.

Activated carbon is a generally made from a wood product or coal by heating to


temperatures between 300-1000℃ in one of a variety of possible gaseous atmosphere
such as CO2, air or water vapor, and then by rapid quenching in the air or water.
Activated carbon is a material with an exceptionally high surface area of approximately
500 m2 in 1 gram due to a high degree of microporosity. Sufficient activation for useful
applications may come solely from the high surface area, though often further chemical
treatment is used to enhance the absorbing properties of the material.

In this experiment Langmuir Isotherm plot will be used to estimate the maximum
amount of adsorption (qmax).

Langmuir Isotherm relates the coverage or adsorption of molecules on a solid


surface to gas pressure or concentration of a medium above the solid surface at a fixed
temperature. Langmuir Isotherm assumes that a single adsorbate binds to a single site
of the adsorbent, and that all surface sites on the adsorbent have the same affinity for
the adsorbate.
Langmuir Isotherm equation was developed by Irving Langmuir in 1916 and it states
that:
𝑏𝐶
Langmuir 𝑞 = 𝑞 𝑚𝑎𝑥 𝑥 1+𝑏𝐶

Where When C is the concentration of contaminant in the liquid after adsorption (molar
or mg/l)
q is the mass of sorbed molecules per mass of sorbent (mole or mg per gram sorbent)
b = Langmuir equilibrium constant
q 𝑚𝑎𝑥 =maximum adsorbed amount, mol/g
In order to calculate the amount adsorbed, q, the equation below can be used:
(𝐶 −𝐶)𝑉
𝑜
q=
𝑚
where,
q = amount adsorbed, mmol/g of activated sludge carbon, mol/g
Co = aqueous concentration before adsorption, mol/L
C = aqueous concentration after adsorption, mol/L
m = weight of activated carbon, g
V = volume of sample, L
Figure 1 below show the Langmuir Isotherm plot (which can be later used to estimate
qmax or Ƭmax)
In the above graph;

● Region I represents the free adsorbent surface. In this region, adsorption


increase with increase in the concentration of aqueous solution after adsorption.
● Region II indicates that the most of the adsorption surfaces are full. In this region,
adsorption increased non-linearly with increase in the concentration of aqueous
solution.
● Region III indicates that all the adsorption surfaces are full. In this region, rate of
adsorption neither decrease nor increase with increase in the concentration of
aqueous solution.

Reagents

● Acetic acid solution with concentration of 1N.


● Activated carbon
● Aqueous sodium hydroxide solution (0.1N)
● Phenolphthalein indicator

Procedures

1. Dilute 1N acetic acid to 0.8, 0.4, 0.2, 0.1, 0.05 and 0.025 N. The final volume of
each concentration is 100 ml.
2. Transfer about 50.00 ml of different concentrations of diluted acetic acid solution
into a clean 250 ml Erlenmeyer flask. Prepare a series of each solution and
name one series, set I.
3. Transfer different volume (ml) of different concentrations of diluted acetic acid
solution into a clean 250 ml Erlenmeyer flask. Prepare a series of each solution
and name one series, set II.
4. Measure 1.0000 g activated carbon and transfer to set I of solutions. Stoppers
the flasks and place them in the shaker, shaking for 1.5 hours at 150 rpm.
5. For set II, measure the indicated volumes (Vo) of each sample solution and dilute
the rest with DI water to 50 ml in a clean, labeled Erlenmeyer flask.
6. Titrate the prepared solutions in step 3 against NaOH solution (0.1N) in order to
detect the precise concentration of acetic acid solution in each flask (Co). Make
sure to add three drops of the phenolphthalein indicator before you start the
titration. As you reach the end point the color of the colorless solution will turn
pale pink.
7. Record the volume of the NaOH solution use (V) at the end point in the provide
table.
8. Filter the solutions in set I and transfer them to clean, labeled 250 ml Erlenmeyer
flasks.
9. Follow step 3 and 4 above in order to detect the precise concentration of acetic
acid solution in each flask (C).
Results

Table 1: Dilution of acetic acid

Initial Volume of Target Volume of Volume of


concentration target acetic concentration initial acetic water added
of acetic acid acid (mL) of acetic acid acid required (mL)
(N) (N) (mL)

1.00 100.00 0.80 80.00 20.00

1.00 100.00 0.40 40.00 60.00

1.00 100.00 0.20 20.00 80.00

1.00 100.00 0.10 10.00 90.00

1.00 100.00 0.05 5.00 95.00

1.00 100.00 0.025 2.50 97.50

Table 2: Acetic acid concentration before adsorption

Standard NAOH titrant concentration 0.1 N

Labeled Volume of Initial read Final read of Volume of Actual


acetic acid acetic acid of NaOH NaOH titrant NaOH titrant concentration
concentration used (mL) titrant (mL) (mL) used (mL) of acetic acid
(N) - in flask (Co; N)

0.8 5.00 12.31 34.52 22.21 0.4442

0.4 5.00 33.72 44.90 11.18 0.2236

0.2 5.00 44.99 50.02 5.03 0.1006

0.1 10.00 39.62 44.99 5.37 0.0537

0.05 10.00 36.61 39.62 3.01 0.0301

0.025 15.00 34.52 36.61 2.09 0.0139


Table 3: Acetic acid concentration after adsorption

Standard NAOH titrant concentration 0.1 N

Labeled Volume of Initial read Final read of Volume of Actual


acetic acid acetic acid of NaOH NaOH titrant NaOH titrant concentration
concentration used (mL) titrant (mL) (mL) used (mL) of acetic acid
(N) - in flask (C; N)

0.8 5.00 22.80 43.50 20.70 0.414

0.4 5.00 16.40 25.80 9.40 0.188

0.2 5.00 18.20 22.80 4.60 0.092

0.1 10.00 14.00 18.20 4.20 0.042

0.05 10.00 14.20 16.40 2.20 0.022

0.025 20.00 13.10 14.20 1.10 0.0055

Table 4: Adsorption of acetic acid using activated carbon

Remark: molar concentration and normal concentration of acetic acid are the same

Diluted acetic Vo (mL) Co (mol/l) C (mol/l) Amount of Q (mol/g)


acid Volume of Actual Actual activated
concentration acetic acid concentration concentratio carbon
(N) in a/c flask of acetic acid n of acetic used (g)
before acid after
adsorption adsorption

0.8 50.00 0.4442 0.414 1.0000 0.00151

0.4 50.00 0.2236 0.188 1.0038 0.00177

0.2 50.00 0.1006 0.092 1.0006 0.04567

0.1 50.00 0.0537 0.042 1.0008 0.00058

0.05 50.00 0.0301 0.022 1.0013 0.00041

0.025 50.00 0.0139 0.0055 1.0049 0.00042

Sample Calculations
Table 1: Dilution of Acetic Acid:
Volume of Acetic Acid (1.00 N) needed:
𝑀 𝑉 𝑀 𝑉0.8𝑁
𝑉2 = 𝑀1 𝑉1 𝑉1.00𝑁 = 0.80𝑁 = (0.80N)(100mL)/1.00N = 80.00 mL
2 2 𝑀 1.00𝑁

Volume of DI Water needed:


𝑉𝐷𝐼 = 𝑉𝑇𝑜𝑡𝑎𝑙 − 𝑉0.80𝑁 = 100.00 mL - 80.00 mL = 20.00 mL

Table 2: Acetic Acid Concentration before Adsorption


Final Volume of NaOH titrant used:
V 𝑁𝑎𝑂𝐻 = V 𝑓 - V 𝑖 = 34.52 mL - 12.31 mL = 22.21 mL

Actual Concentration of Acetic Acid:


(𝑉 ∗ 𝐶 𝑁𝑎𝑂𝐻 ) 22.21𝑚𝐿 ∗ 0.1𝑁
C 𝑜 = 𝑁𝑎𝑂𝐻 = 5.00 𝑚𝐿 = 0.4442 N
𝑉 𝐶𝐻3𝐶𝑂𝑂𝐻

Table 3: Acetic Acid Concentration after Adsorption:


Final Volume of NaOH titrant used:
V 𝑁𝑎𝑂𝐻 = V 𝑓 - V 𝑖 = 43.50 mL - 22.80 mL = 20.70 mL

Actual Concentration of Acetic Acid:


(𝑉 ∗ 𝐶 𝑁𝑎𝑂𝐻 ) 20.70𝑚𝐿 ∗ 0.1𝑁
C 𝑜 = 𝑁𝑎𝑂𝐻 = 5.00 𝑚𝐿 = 0.414 N
𝑉 𝐶𝐻3𝐶𝑂𝑂𝐻

Table 4: Adsorption of Acetic Acid Using Activated Carbon:


Amount of Adsorption:
(𝐶 𝑜 −𝐶)𝑉 𝑜 (0.442𝑚𝑜𝑙/𝑙 − 0.414𝑚𝑜𝑙/𝑙)(50.00𝑚𝐿 ∗ 1𝐿/1000𝑚𝐿)
q=𝑚 = = 0.00151 mol/g
𝑎𝑐𝑡𝑖𝑣𝑎𝑡𝑒𝑑𝑐𝑎𝑟𝑏𝑜𝑛 1.0000𝑔

Graph
Estimated Qmax (from graph) = 0.000285 mol/g

Figure 1: Amount of Adsorption (Q) vs. Actual Acetic Acid Concentration Before
Adsorption (Co).

Discussion

Adsorption is observed because an adsorbent solid is mixed with a liquid solution


that contains dissolved substances; this acts as an adsorbate. The activated charcoal
removes a part of the acetic acid once it is agitated, and therefore decreases the
amount of concentration of acetic acid in the solution. The acetic acid adsorbed
increases with the concentration of the adsorbate. Activated carbon filtration effectively
removes certain organic (carbon containing) compounds in water. When observing the
formula for acetic acid (CH3COOH), the numerous amounts of carbon are apparent,
making it easier for the activated carbon to remove the contaminants. The isotherm
observed from the acetic removal using activated carbon was the Langmuir model.
Because the graph produced from the experimental data obtained in this lab resembles
that of the Langmuir model, it can be noted that this lab followed this specific adsorption
isotherm. The graph illustrated in Figure 1 reveals that the maximum amount of
adsorption (Qmax) for this lab was 0.000285 mol/g. Referring to the shape of Figure 1,
region I behaves linearly due to the rapid increase of how much acetic acid is adsorbed
while having a relatively free adsorbent surface. Once the surface fills with the
adsorbate, the amount of acetic acid adsorbed increases, while the rate of adsorption
decrease (as observed in region II). Over time, the adsorbent surface becauses full and
the amount of adsorbed remains constant, regardless of increasing the concentration
(region III). If you reflect this situation graphically, a parabolic pattern is obtained and
Qmax is shown as a constant line. The increase of acetic acid concentration will
increase the amount of adsorption occurring at equilibrium until a limiting value is
reached (Qmax). When the removal of other contaminants is necessary, the maximum
amount adsorbed with change. The contaminants that are more easily adsorbed by the
activated carbon will be removed in larger amounts compared to those that are less well
absorbed. This is due to the fact that adsorption isotherms are characterized by their
ability to remove a specific contaminant, thus the Qmax value would change based on
the desired contaminant that needs to be removed.
Rapid adsorption would create a graph where region I would be decrease in size,
due to the decreased time of the free adsorbent surface. Because adsorption increases
with the increase in the concentration of the aqueous solution after adsorption, region I
would reflect a shorter period of this linear increase. Region II would reflect a smaller
section where the adsorption surfaces are full, because the contaminant is more easily
absorbed by the activated carbon. Although this is a non-linear increase, a smaller
curve would represent this rapid adsorption. Taking all of these predictions into
consideration, equilibrium would be reached at a fairly lower rate which would create a
lower Qmax, and therefore a decrease in the value where the graph appears to be
constant. A higher Qmax is favored over a lower Qmax in environmental engineering,
due efficiently removing a larger amount of contaminants. If the threshold for absorbing
contaminants is increased, it will take the adsorption sites on the activated carbon to
become fuller of contaminants, which will reduce the the contaminants in the water by
using less materials. Some errors that occurred during this experiment caused one pair
of data (0.4442,0.00151) to be thrown out in order to obtain Qmax graphically. This
error can be attributed to human error in the dilution of CH3COOH and over-titration.

Conclusion

This lab consisted of studying the effects of activated carbon in adsorption


processes. In this process, the adsorbent was activated carbon, while the adsorbate
was acetic acid. The adsorption effects of activated carbon was measured by variably
diluting the acetic acid. The maximum amount of adsorption (Qmax) observed
graphically was 0.000285 g/mol.