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Experiment No. 1

ADSORPTION OF ACETIC ACID IN ACTIVATED CARBON

Group I:

Cientos, Justine V.

Esparagoza, Johnil D.

Da-anton, Irish Marie D.

Gallos, Ma. Ines M.

Ortiz, Dyryl S.

Paduano, Angelo R.

Valenzuela, Earl Emmanuel T.

November 20, 2019

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ABSTRACT

In adsorption processes one or more components of a gas or liquid stream are adsorbed on the
surface of a solid adsorbent and a separation is accomplished. This experiment was conducted to
determine the adsorption isotherm of acetic acid on activated carbon and to determine the
adsorption constant (k) and the maximal adsorbed amount (Amax) of acetic acid per gram of
activated carbon. Coefficient of determination for linear, freundlich, and Langmuir isotherms
are taken as 0.4988, 0.8414, 0.9704, respectively. Langmuir isotherm with coefficient of
determination of 0.9704 is closest to 1 which the most accurate compared to the other two.
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I. THEORY
In adsorption processes one or more components of a gas or liquid stream are adsorbed
on the surface of a solid adsorbent and a separation is accomplished. In commercial processes,
the adsorbent is usually in the form of small particles in a fixed bed. The fluid is passed through
the bed and the solid particles adsorb components from the fluid. When the fluid is almost
saturated, the flow in this bed is stopped and the bed is regenerated thermally or by other
methods so that desorption occurs. The adsorbed material (adsorbate) is thereby recovered and
the solid adsorbent is ready for another cycle of adsorption.

The equilibrium between the concentration of a solute in the fluid phase and its
concentration on the solid resembles somewhat the equilibrium solubility of a gas in a liquid.
Data are plotted as adsorption isotherms as shown in figure below. The concentration in the solid
phase is express as q, kg adsorbate (solute)/kg adsorbent (solid), and in the fluid phase (gas or
liquid) as c, kg adsorbate/m3 fluid.

Data that follow a linear law can be expressed by an equation similar to Henry’s law:

q = Kc

where K is a constant determined experimentally, m3/kg adsorbent. This linear isotherm is not
common, but in the dilute region it can be used to approximate data for many systems.

The Freundlich isotherm equation, which is empirical, often approximates data for many
physical adsorption systems and is particularly useful for liquids:

q = Kcn

where K and n are constants and must be determined experimentally. If a log-log plot is made for
q versus c, the slope is the dimentionless exponent n. The dimensions of K depend on the value
of n. This equation is sometimes used to correlate data for hydrocarbon gases on activated
carbon.

The Langmuir isotherm has a theoretical basis and is given by the following, qo and K are
imperical constants:

q=
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where qo is kg adsorbate/kg solid and K is kg/m3. The equation was derived assuming that there
are only a fixed number of active sites available for adsorption, that only a monolayer is formed,
and that the adsorption is reversible and reaches an equilibrium condition. By plotting 1/ q versus
1/c, the slope is K/qo and the intercept is 1/ qo.

Almost all adsorption systems show that as temperature increased, the amount
adsorbed by the adsorbent decreases strongly. This is useful since adsorption is normally at room
temperatures and desorption can be attained by raising the temperature.

II. OBJECTIVES:
1) To determine the adsorption isotherm of acetic acid on activated carbon,
2) To determine the adsorption constant (k) and the maximal adsorbed amount (Amax) of
acetic acid per gram of activated carbon.

III. EQUIPMENTS/APPARATUS/MATERIALS NEEDED/SAFETY DEVICES & PPE

A. Equipment & Apparatus Needed:
1) 6 boiling flasks (250 ml),
2) 6 Erlenmeyer flash (250 ml)
3) 6 funnels,
4) 3 burettes (50ml),
5) 10 titrimetric flasks,
6) 3 pipettes,
7) holders for funnels,
8) holders for burettes,
9) spoon,
10) rubber stoppers
B. Materials and supplies:
1) filter paper,
2) glazed paper for weighing,
3) acetic acid solution (concentration = 1 mol dm-3),
4) NaOH solution (concentration = 0.2 mol dm-3),
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5) activated carbon,
6) phenolphthalein
C. Safety gear/apparel:
1) Rubber gloves
2) Safety glasses or goggles

IV. EXPERIMENT PROCEDURES :

Fig. 1.1 Preparation of Aqueous Solutions

1) Prepare aqueous solutions of acetic acid into numbered flasks following the scheme given
in Table 1. The total volume of each solution is 60 ml. Use flasks fitted with stoppers.
Table 1.1
Scheme for acetic acid dilution

Flask No. 1 2 3 4 5 6
Acetic acid (ml) 6 12 18 30 42 60
Distilled H2O (ml) 54 48 42 30 18 0
Total volume (ml) 60 60 60 60 60 60

2) Transfer 10 ml of the solution from each flask into numbered titrimetric flask, so final
volume of acetic acid solution is VA = 50 ml per flask.
3) Determine the actual concentration of acetic acid in flasks by titration in this way:
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4) For titration, modify the volume in each titrimetric flask. Take away defined volume of
the solution, to obtain in each flask the volume as given in Table 2

Table 1.2
Volumes of the acetic acid solutions used for titration before and after the adsorption

Titrimetric flask No. 1 2 3 4 5 6

Volume V (ml) 10 10 5 5 5 2

5) Add 2-3 drops of phenolphthalein and titrate with NaOH.

6) Once the endpoint has been reached, read the burette and record the volume of the base
Xi0 (ml) that was required to reach the endpoint in Table 3.
7) Calculate the actual concentration of acetic acid Ci0 in the flask No. 1 – 6, respectively,
and write it down in Table 3.
8) Using a suitable balance and glazed paper, weigh 6 portions of activated carbon (5 g each
portion). The accuracy of weighing must be 0.01 g.
9) Put activated carbon into numbered flasks with stoppers (1 portion per flask). Plug up the
flasks, and shake them. Wait for 20 minutes, the process of adsorption is in progress. Mix
the mixtures in each stoppered flasks several times by shaking within this period.
(Remark: The process of adsorption is a function of time too. It is important to put
charcoal into flasks at the same time, to provide adsorption for the same period in each
flask).
10) Filter the mixtures into clean and dry flasks. To avoid disturbing effect of adsorption of
acetic acid into filtering paper, remove away the first portion of filtration, app. 5 ml.
11) Determine the final concentration of acetic acid Ci in each of the flasks after adsorption:
From each solution, transfer the required volume into clean and dry titrimetric flask,
following Table 1.2.
12) Repeat points 5-7, and from the consumed base Xi (ml) determine the concentration of
acetic acid ci after adsorption.
13) Finishing experiment, wash carefully used flasks, pipettes, etc.
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V. CONDUCT OF THE EXPERIMENT

For preparing of aqueous solutions of acetic acid, all apparatus and chemicals were
prepared. For dilution of acetic acid, 6 flasks with fitted stoppers were used to prepare 6
solutions of acetic acid with different volumes of acetic acid and water and with the total volume
of 60 mL each. After that 10 ml of the solution from each flask was transferred into numbered
titrimetric flask, so final volume of acetic acid solution is VA = 50 ml per flask. Then every
solution was titrated with NaOH, once the endpoint was reached the volume of the base was
recorded and calculated to determine the actual concentration of acetic acid in each flask. 6
portions of 5g activated carbon were weighed and put in every flask with stopper and shake to
mix the solution well. Letting it for 20 minutes for the process of adsorption is in progress. The
solution was mixed several times. Then the mixtures were filtered into clean and dry flasks.
After that the final concentrations of acetic acid Ci in each of the flasks were determined.

Fig. 1.2 Acetic acid

solutions
Fig. 1.3 Activated carbon sample Fig. 1.4 0.2M NaOH
solution

Fig. 1.5 Titration of Fig. 1.6 Determining Fig. 1.7 Conduct of the experiment
the solution of volume
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VI. PRESENTATION, ANALYSIS/DISCUSSION OF RESULTS AND CONCLUSION

Table 1.3
Volume of 0.2 M NaOH as Titrant and Acetic acid Concentration Before and After the
Adsorption Process
Xi 0 Ci 0 Xi Ci
Flask No.
(mL) (mol/L) (mL) (mol/L)
1 0.5 (10 mL Sample) 0.010 0.5 (10 mL Sample) 0.008
2 1.4 (10 mL Sample) 0.028 1.1 (10 mL Sample) 0.022
3 1.2 (5 mL Sample) 0.048 0.9 (5 mL Sample) 0.036
4 1.9 (5 mL Sample) 0.076 1.3 (5 mL Sample) 0.052
5 2.4 (5 mL Sample) 0.096 1.6 (5 mL Sample) 0.064
6 1.5 (2 mL Sample) 0.150 1.0 (2 mL Sample) 0.1

Table 1.4
Data Points for Linear Freundlich and Langmuir Isotherms
c q
log c log q 1/c 1/q
(kg adsorbate/m3 fluid) (kg adsorbate/ kg adsorbent)
0.120 0.00024 -0.920 -3.619 8.319 4159.734
0.361 0.00072 -0.443 -3.142 2.773 1386.578
0.721 0.00072 -0.142 -3.142 1.387 1386.578
1.442 0.00144 0.159 -2.841 0.693 693.289
1.923 0.00192 0.284 -2.716 0.520 519.967
3.005 0.00120 0.478 -2.920 0.333 831.947

0.0025
q,(kg adsorbate/kg adsorbent)

0.002

0.0015

0.001 y = 0.0004x + 0.0005

R² = 0.4988
0.0005

0
0 0.5 1 1.5 2 2.5 3 3.5
3
c,(kg adsorbate/m fluid)

Fig. 1.8 Plot of Data for the Linear Isotherm

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log q,(kg adsorbate/kg adsorbent)

-1 -0.8 -0.6 -0.4 -0.2 0 0.2 0.4 0.6
-0.5

-1

-1.5

-2
y = 0.5668x - 3.0081
-2.5
R² = 0.8414
-3

-3.5

-4
log c, (kg adsorbent/m3 fluid)

Fig. 1.9 Plot of Data for the Freundlich Isotherm

4500.00
4000.00
1/q, (kg adsorbate/kg adsorbent)

3500.00
3000.00
2500.00
2000.00
1500.00 y = 435.27x + 478.89
1000.00 R² = 0.9704

500.00
0.00
0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00
1/c, (kg adsorbent/m3 fluid)

Fig. 1.10 Plot of Data for the Langmuir Isotherm

Analysis/Discussion of Results:
The tables above show the different isotherms used for determining the degree of
adsorption. The data is plot and the coefficient of determination, r2, is used as comparison for
accuracy of isotherms and to choose which fits the most. Coefficient of determination for linear,
freundlich, and Langmuir isotherms are taken as 0.4988, 0.8414, 0.9704, respectively.
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Conclusion:
Out of the three, Langmuir isotherm with coefficient of determination of 0.9704 is closest
to 1. In conclusion, this best fits the data plot, and is the more accurate to be used in comparison
to others.

VII. APPENDIX AND REFERENCES

Raw Data:

Molarity of NaOH = 0.2 M

Molar Mass of Acetic Acid = 60.1 g/mol
Mass of Activated Carbon = 5 g
Calculations:

Concentration of Solute =

ci = = 0.01 mol/L cf = = 0.008 mol/L

Note: For titrations before and after adsorption, the same calculation is used.

Concentration of Solute on the Fluid Phase: c = ( )

c=( ) = 0.120 kg adsorbate/m3 fluid

Concentration of Solute on the Solid Phase: q =

q= = 0.00024 kg adsobate/kg adsorbent

Note: For all Trials, the same calculation is used.
References:

Transport Processes and Unit Operations, 3rd Edition by Geankoplis

Unit Operations, 5th Edition by McCabe and Smith