Department of Petrochemical Engineering: Catalyst Lab Report (2020 - 2021)

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TECHNICAL COLLEGE OF ENGINEERING - DUHOK

Department of Petrochemical Engineering

CATALYST LAB REPORT

(2020 – 2021)

Fourth Year

This report prepared by

Mohammed SALAH

FALAK ALI

BARFI FAQH

RAYHAN RASHED

Date of Exp:

13/10/2020

Date of Sub. :

20/10/2020
Objective:

► determination of adsorption isotherm of acetic acid on activated charcoal


► determine the adsorption constant (k)
► the maximal adsorbed substance amount of acetic acid per gram of charcoal
(amax) of langmuir isotherm.

Introduction:

Adsorption is a process that occurs when a gas or liquid solute accumulates on


the surface of a solid or a liquid (adsorbent), forming a molecular or atomic film
(adsorbate). It is different from absorption, in which a substance diffuses into a
liquid or solid to form a solution. The term sorption encompasses both
processes, while desorption is the reverse process. Adsorption is operative in
most natural physical, biological, and chemical systems, and is widely used in
industrial applications such as activated charcoal, synthetic resins and water
purification. Similar to surface tension, adsorption is a consequence of surface
energy. In a bulk material, all the bonding requirements (be they ionic, covalent
or metallic) of the constituent atoms of
the material is filled. But atoms on the (clean) surface experience a bond
deficiency, because they are not wholly surrounded by other atoms. Thus it is
energetically favorable for them to bond with whatever happens to be
available. The exact nature of the bonding depends on the details of the species
involved, but the adsorbed material is generally classified as exhibiting
physisorption or chemisorption. Physisorption or physical adsorption is a type of
adsorption in which the adsorbate adheres to the surface only through Van der
Waals (weak intermolecular) interactions, which are also responsible for the
non-ideal behavior of real gases.
Chemisorption is a type of adsorption whereby a molecule adheres to a surface
through the formation of a chemical bond, as opposed to the Van der Waals
forces which cause physisorption. Adsorption is usually described through
adsorption isotherms, that is, functions which
connect the amount of adsorbate on the adsorbent, with its pressure (if gas) or
concentration (if liquid). One can find in literature several models describing
process of adsorption, namely Freundlich isotherm, Langmuir isotherm, BET
isotherm, etc. We will deal with Langmuir
isotherm in more details:
Langmuir isotherm
In 1916, Irving Langmuir published an isotherm for gases adsorbed on solids,
which retained his name. It is an empirical isotherm derived from a proposed
kinetic mechanism. It is based on four hypotheses:
1. The surface of the adsorbent is uniform, that is, all the adsorption sites are
equal.
2. Adsorbed molecules do not interact.
3. All adsorption occurs through the same mechanism.
4. At the maximum adsorption, only a monolayer is formed: molecules of
adsorbate do not deposit on other, already adsorbed, molecules of adsorbate,
only on the free surface of the adsorbent.

Calculation
Titration #1:

Conical Flask #1

6ml Acetic acid + 54ml of DW

From burette:
Vi = 0
Vf = 5.6
Soo M1 * V1= M2 * V2
0.2*5.6=M2 *5 ➔ M2 = 0.224 g

Titration #2:

Conical Flask #2
12ml acetic acid + 48ml DW

From burette
Vi = 5
Vf = 13.8
V1=8.8
M1 * V1=M2 * V2=➔ M2 = 0.352 g
Titration #3:

Conical Flask #3

18ml Acetic acid + 42ml DW

From burette

Vi=0 & Vf=7 ➔ V1 = 7


M1 * V1 = M2 * V2➔ M2=0.28 g

Titration #4:

Conical Flask #4

30ml Acetic acid + 30ml DW

From burette
Vi=7 & Vf=18.5➔ V1= 11.5
M1 * V1=M2 * V2➔ M2= 0.46 g

Titration #5:

Conical Flask #5

40ml acetic acid + 20ml DW

From burette
Vi=18.5 & Vf=32.7 ➔ V1= 14.2
M1 * V1=M2 * V2➔ M2= 0.568 g

Titrations after adsorptions process and filtrate the solution


Titration #1:
From burette
Vi= 32.7 & Vf= 34.5 ➔ V1 = 1.8
M1 * V1=M2 * V2
0.2*1.8=M2*5➔ M2 = 0.072 g

Titration #2:

From burette
Vi=34.5 & Vf=43➔ V1 = 8.5
M1 * V1=M2 * V2➔ M2 = 0.34 g

Titration #3:

From burette
Vi= 43 & Vf= 49.7➔ V1 = 6.7
M1*V1=M2*V2➔ M2 = 0.268 g

Titration #4:

From burette
Vi=0 & Vf=9 ➔ V1 = 9
M1*V1=M2*V2➔ M2 = 0.36 g

Titration #5:

From burette
Vi=13.5 & Vf=25.2 ➔ V1 = 11.7
M1*V1=M2*V2➔ M2 = 0.468 g

To Find Mi use:
(𝑪𝒂 − 𝑪𝒇) ∗ 𝑽𝑨
𝑴𝒊 =
𝒈 ∗ 𝟏𝟎𝟎𝟎
Where:
(Ca-Cf)= Cad
g=1
VA = 55
Soo
(𝟎.𝟏𝟓𝟐)∗𝟓𝟓
1. Mi = ➔ Mi = 0.00836
𝟏∗𝟏𝟎𝟎𝟎

(𝟎.𝟎𝟏𝟐)∗𝟓𝟓
2. Mi = ➔ Mi = 0.00066
𝟏∗𝟏𝟎𝟎𝟎

(𝟎.𝟎𝟏𝟐)∗𝟓𝟓
3. Mi = ➔ Mi = 0.00066
𝟏∗𝟏𝟎𝟎𝟎

(𝟎.𝟏)∗𝟓𝟓
4. Mi = ➔ Mi = 0.0055
𝟏∗𝟏𝟎𝟎𝟎

(𝟎.𝟏)∗𝟓𝟓
5. Mi = ➔ Mi = 0.0055
𝟏∗𝟏𝟎𝟎𝟎

1/ Cad:
1. 6.5789
2. 83.3333
3. 83.3333
4. 10
5. 10

Final Result’s in table


No. Ca Cf Ca – Cf=Cad Mi 1/Cad 𝟏 %=
𝑪𝒂𝒅
∗ 𝟏𝟎𝟎
𝑪𝒂
(mol/L) (mol/L) (mol/L) (mol/g) (L/mol) 𝑴𝒊
(g/mol)

1 0.224 0.072 0.152 0.00836 6.5789 119.617 67.86%

2 0.352 0.34 0.012 0.00066 83.3333 1515.15 3.4%

3 0.28 0.268 0.012 0.00066 83.3333 1515.15 4.2%

4 0.46 0.36 0.1 0.0055 10 181.818 21.7%

5 0.568 0.468 0.1 0.0055 10 181.818 17.6%


Result’s in graph
1600
y = 18.181804x + 0.0002201
1400

1200
1/Mi, (g/mol)

1000

800

600

400

200

0
0 20 40 60 80 100
1/Cad, (L/mol)

From graph

Slope = 18.181804
Intercept = 0.0002201

𝟏
Intercept=
𝑨𝒎𝒂𝒙

𝟏
0.0002201 = ➔ Amax * 0.0002201=1
𝑨𝒎𝒂𝒙

𝟏
➔ Amax= ➔ Amax = 4543.389
𝟎.𝟎𝟎𝟎𝟐𝟐𝟎𝟏

𝟏 𝟏 𝟏
Slope = ➔ k = 𝑨𝒎𝒂𝒙∗𝑺𝒍𝒐𝒑𝒆 ➔ k = 𝟒𝟓𝟒𝟑.𝟑𝟖𝟗∗𝟏𝟖.𝟏𝟖𝟏𝟖𝟎𝟒
𝑨𝒎𝒂𝒙∗𝒌

➔ K = 0.000012105 mol-1 * ml3


Discussion & Conclusion:
This experiment was conducted to study the adsorption isotherm of
acetic acid by activated carbon. Activated charcoal with presence of 0.4
M acetic acid was used to titrated by 0.1 M sodium hydroxide, NaOH with
phenolphthalein indicator. Adsorption is the adhesion of atoms ions or
molecules from a gas liquid or dissolved solid to a surface. A molecule
that undergoes adsorption is referred to as the adsorbate, the solid is the
adsorbent. Chemisorption is the process commonly known as bond
formation between the adsorbate and the surface. Physical adsorption
involves low heats of adsorption and is enhanced by lowering the
temperature while chemical adsorption involves higher heats of
adsorption and isenhanced by raising the temperature. Similar to surface
tension, adsorption is a consequence of surface energy.

The factors that decide the amount of substance that can be adsorbed
on to activated charcoal are nature of adsorbate and adsorbent, the
surface area of adsorbent activation of adsorbent and experimental
condition such as temperature. Adsorption processes studied through
graphs known as adsorption isotherm. In this experiment, Langmuir
equation is used to estimate the surface area of activated charcoal
sample. Langmuir derived an equation which explained the relationship
between the number of active sites of the surface undergoing adsorption
and pressure.

The possible errors that occur while conducting this experiment is the
position of the eye would not perpendicular to meniscus line which cause
the amount of sodium hydroxide titrated recorded are inaccurate and it
will change overall result of the experiment. Besides, the amount of
charcoal is added is more than needed and not distributed equally over
the solution. This cause the solution not achieved equilibrium. Next, the
charcoal maybe included in supernatant that will affect the amount of
sodium hydroxide needed to change color dorm dark blue to colorless.
Conclusion:
From this experiment, the adsorption of acetic acid in charcoal follows
the Langmuir theory of adsorption isotherm which shows that the
adsorption decreases as the concentration of the acetic acid solution
decrease.

Answer of some question:

Q1/ What are the differences between


between Physical adsorption and chemical adsorption?
Physical absorption occurs when the adsorbate gas molecules are held by
physical forces like Van der Waals forces, and physical adsorption can be
monolayer or multilayer. Chemical adsorption occurs when the absorbate
molecule is held on the adsorbent surface by chemical forces as short covalent
chemical bonding occurs by the sharing of electrons, and is monolayer only.

Q2/ What are the differences between adsorbent and


adsorbate?
The substance which gets absorbed is called absorbate and the substance which
absorbs is called the absorbent ..... For example, when we use a paper towel to
clean the spilled water, the paper absorbs the water, so in this case paper is
absorbent and water is the absorbate.

Q3/ Define the following:


adsorption isobar, adsorption isotherm & adsorption
isostere.

Adsorption asobar: is a graph between the amount adsorbed (x/m)and the


temperature (T) of the adsorbate at constant pressure.
Adsorption isotherm: is a graph or a relation between the amounts of adsorbate
adsorbed on the surface of adsorbent and pressure at a constant temperature.
Different adsorption isotherm was studied by different scientists.

Adsorption isosester: The function relating the equilibrium pressure to the


temperature at a constant value of the amount, or excess amount, of substance
adsorbed by a given amount of solid.
Q4/ What are the differences between adsorption and
Absorption?

ADSORPTION:
► PHENOMENON
It is a surface phenomenon. The process in wich there in adhesion of
► HEAT EXCHANGE. Atoms,ions or molecules from a gas,liquid
It is exothermic reaction. Or dissolved solid to surface
► TEMPERATURE
It is favored by low temp.
► RATE OF REACTION
It is steadily increases and
reaches equilibrium.
► CONCENTRATION
Concentration on the
surface of adsorbent is
different from that in bulk.

ABSORPTION:
► PHENOMENON
It is a bulk phenomenon. The process by wich one substance
► HEAT EXCHANGE Takes up another substance
It is Endothermic reaction. Through minute pores or spaces
► TEMPRATURE. Between them
It is generally not affected bytemp.
► RATE OF REACTION
It occurs at uniform rate.
► CONCENTRATION
It is same throughout the material.

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