Abstract

The aim of this report is to demonstrate the experiment of adsorption of oxalic acid on activated
carbon, in a medium of aqueous solution. And the verification of the Freundich isotherm
hypothesis. The current report enhances the study of adsorption, chemisorption and
physisorption. 4 samples with different concentrations of oxalic acid were prepared and the
activated carbon is added (1 gram) to each sample, and left on shaker for 30 min. to reach
equilibrium. Furthermore, the samples are filtered and titration by standardized KMnO4 on the
samples to deduce the concentration. Using the given equations related to the experiment, a
graph is plotted (logC) against (logx/m) in which an expected straight line is resulted, were the
slope of this line (n) represents the type of adsorption and the intercept (k) represents the rate
of reaction.
 1. Introduction

1.1. Adsorption and Absorption

Two important processes that take place between different phases are absorption and
adsorption. A lot of people mistake those two processes to be alike when they are two entirely
different processes. Absorption is a process in which a substance’s molecules diffuse or
penetrate into the bulk of another material, solid or liquid, to result in the formation of
compounds or solutions. In other words, the molecules that penetrated into the volume of
another substance, may actually become part of the original substance itself. An example of
absorption could be the absorption of water by a dry sponge. (Shukla, 2012)

Adsorption is a completely different process than absorption. It is all about the adhesion forces
on the surface causing the particles to stick on it only and not penetrate. The molecules gather
on the adsorbent’s surface and are not consumed by it which results in high concentration of
the adsorbate on the surface. When a substance is adsorbed on the surface, it is no longer free
to move as before. It can be said that its movement have been restricted by the adsorbent, and
the entropy of the adsorbate decreases.

Another important factor that has a role in the rate of adsorption is the nature of the adsorbent
and adsorbate. For the adsorbate, gases that can be easily liquefied, such as ammonia, have
higher tendency to be adsorbed than elemental gases such as nitrogen. As for the adsorbent,
the higher the porosity of it cause the surface area to be higher and therefore can adsorb more
amounts than non-porous material. An example of an excellent adsorbent is charcoal. (Mantell,
1951)

Figure 1.1 shows clearly the difference between absorption and adsorption while figure 1.2
shows the difference in mechanisms of both processes:
 Figure 1. Absorption Vs Adsorption

Figure 2.: (a) mechanism of absorption, (b) mechanism of adsorption

Table 1.comparison between adsorption and absorption

Adsorption Absorption
Definition Accumulation of molecules on Assimilation of molecules through a
the surface of a solid or liquid solid or liquid’s bulk
Phenomenon Surface Bulk
Temperature Better at low temperatures No effect
Heat Exchange Exothermic process Endothermic process
Rate of Reaction Increases until equilibrium is Uniform rate
reached
Concentration Higher on the surface than in Equal throughout the material
bulk
Example Ammonia adsorbed by charcoal Ammonia absorbed by water forming
ammonium hydroxide
 1.2. Types of Adsorption
Due to the nature of existing forces between the adsorbent and adsorbate, adsorption can be
divided into two categories, chemical adsorption (Chemisorption) and physical adsorption
(Physisorption). (IUPAC, 2002)

1.2.1. Physical Adsorption

This type occurs when the type of attraction force between molecules is Vander Waal forces.
The force of attraction in this type of adsorption between the adsorbent and adsorbate is very
weak and can be reversed easily by an increase in temperature or a decrease in pressure.

1.2.2. Chemical Adsorption

This type occurs when the forces of attraction between the adsorbent and adsorbate is very
strong and has almost the same strength as that of a chemical bond. Due to the very strong
forces of attraction between the molecules and the surface, this adsorption process cannot be
easily reversed.

Table 2. Comparison between Physical and Chemical adsorption (IUPAC, 2002)

Physisorption Chemisorption

Low heat of adsorption usually in the range of High heat of adsorption in the range of 40-
20-40 kJ mol-1 400 kJ mol-1

Forces of attraction are similar to chemical

Force of attraction are Van der Waal's forces
bond forces

Takes place at low temperatures and decreases

Favours high temperature
with increasing temperature

Reversible Irreversible

The extent of adsorption is generally not

It is related to the ease of liquefaction of the gas
related to liquefaction of the gas

It is not very specific It is highly specific

It forms multi-molecular layers It forms monomolecular layers

It does not require any activation energy It requires activation energy

Favours high pressure and desorption may Favours high pressure but desorption does
happen when pressure is decreased not happen if pressure decreases

Figure 3. Physical Vs Chemical Adsorption

 2. Experimental Procedure

1. Four samples of different Oxalic acid concentrations were prepared:

Sample 1 – 100 % oxalic acid (0.5 N)
Sample 2 – 75% oxalic acid, 25% water (0.375 N)
Sample 3 – 50% oxalic acid, 50%water (0.25 N)
Sample 4 – 25% oxalic acid, 75% water (0.125 N)
2. Add 1 gram of charcoal to each sample
3. Place it on the shaker for 30 minutes
4. After the 30 minutes, filter out the charcoal and collect the filtrate in another flask
5. Titrate 10 ml of the filtrate of each sample with potassium permanganate until it reaches an
end point (from colourless to faint pink).
 3. Experimental Results

The following equations will be used to calculate both log(C) and log(x/m), to plot a graph
between both parameters to conduct the slope and intercept of the resulted line.

𝑁 ∗ 𝑉)𝑜𝑥𝑎𝑙𝑖𝑐 = 𝑁 ∗ 𝑉)𝐾𝑚𝑁𝑂4 , Where N are : 0.5, 0.375, 0.25, 0.125

𝑚𝑎𝑠𝑠(𝑥) = 𝑁 ∗ 𝑉 ∗ 𝐸𝑞. 𝑊𝑡

𝐶 = 𝑁 ∗ 63

- Note that the mass of activated carbon (m) is equal to 1g

Table 3. Calculation steps for log(c) and log(x/m)

Flask`# VKmNO4) VKmNO4) X x (g) x/m C = Log(x/m) Log(C)

Before After (Vb – N*63
VA)
ml
1 10 9.5 0.5 0.01575 0.01575 33.39 -1.803 1.524
2 7.5 7.25 0.25 0.005906 0.005906 24.57 -2.229 1.390
3 5 4.85 0.15 0.002363 0.002363 16.38 -2.627 1.214
4 2.5 2.4 0.1 7.88*103 7.88*103 8.19 -3.103 0.913

0 Log(C) vs Log(x/m)
0 0.5 1 1.5 2
-0.5

-1
Log(x/m)

-1.5 y = 2.0766x - 5.0575

R² = 0.9751
-2

-2.5

-3

-3.5
Log(C)
Figure 4. graphically illustration of log(c) vs log(x/m)
 4. Discussion and Conclusion

To conclude it all, this experiment was conduct for the study of adsorption of oxalic acid on
activated carbon, with respect to the experimental procedures and results, the report’s aims to
verify the freundlish isotherm and to determine both the type of adsorption (either monolayer
or multilayer) and the rate of reaction (k). 4 samples with different concentrations of oxalic
acid was prepared and activated carbon (1g) was added to each sample as the type of adsorbent.
This particular type of adsorbent was considered due to its high surface area and capability of
high sorption rates where each 1 gram of activated carbon is able to adsorb 500ml. However,
it was recommended to use different mases of activated carbon, to demonstrate the influence
of it on the experiment. Using the given equation to determine the; Normality; mass and
Concentration. A graph was plotted between log(C) and log(x/m). these values are
implemented relying on the freundlish equation (at constant temperature) in which the straight
line resulted from the plotted graph will be helpful in determining the required parameters. The
slope of the straight line equals to 2.0766 as shown in Figure 4, which represents the type of
adsorption (n), since the value of (n) >1, therefore it is a Multilayer. Additionally, the intercept
of the straight line represents the rate of reaction, where log(k) = 5.0575  k = 114156.33.
Such a value for the rate of reaction is unreliable, which indicates that the results implemented
for this experiment contains error in calculations. However, a trial was made to plot the graph
again with different valued, by multiplying the standard normalities by 10-3, and different
values of (C) are obtained, after plotting the graph the intercept was obtained to be 1.1734.
since log(k) = 1.1734  k = 14.9. The value of the rate of reaction calculated is not for sure
the right answer, yet such a value makes sense and is more reliable than the previous trial.
5. Sources of Error

1) The solution prepared in the laboratory before carrying out the experiment was not
preparing accurately; such an error was deduced when titrating with KMnO4 took
longer than usual.
2) The number of samples used in the experiment (4 samples) were not sufficient enough
for further study of the experiment. It is recommended to test at least 6 samples for the
sake of deducing more accurate results.
3) The masses of activated carbon added to the sample should varies, to be able to study
the effect of variation of the activated carbon.
4) The time allowed for shaking (30 min.) was not adjusted correctly, students were not
able to maintain correct time for shaking the sample.
 6. References

IUPAC. (2002, september 5). Retrieved from

http://old.iupac.org/reports/2001/colloid_2001/manual_of_s_and_t/node16.html

Mantell, C. L. (1951). Adsorption. New York: Mcgraw-hill Book company Inc.

Shukla, A. (2012, March 28). Slideshare. Retrieved from

https://www.slideshare.net/iitabhinav84/surface-chemistry