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College of Engineering
Chemical Engineering Department
Manila
Section: 51026
Experiment No. 7
CHEMICAL EQUILIBRIUM
Date of Experiment: July 3, 2018
Submitted by:
Submitted to:
Adsorption
Manz Agdalpen, Ariadna Agoto, Melissa Mae Carpio
a
Department of Chemical Engineering, College of Engineering, Adamson University, 900 San Marcelino, Ermita, Manila 1000, Philippines
Article history: The experiment aimed to determine the equilibrium constant for the mixture of
Date Performed: July 3, 2018 iron (III) and thiocynate, to form a complex, ferric thiocyanate. The relative
Date Submitted: July 8, 2018 amounts of the ions participating in the reaction can be judged from the solution
color, since in neutral to slightly acidic solutions, Fe+3 is light yellow, NCS– is
colorless, and FeNCS+2 is red. If the solution is initially reddish, and the
equilibrium shifts to the right (more FeNCS+2), the solution becomes darker red,
Keywords: Adsorbate, Adsorbent, while if the equilibrium shifts to the left (less FeNCS+2), the solution becomes
Adsorption, Concentration, Equilibrium lighter red or straw yellow. In order to find the concentration of the unknown, we
constant used a standard and compared heights, by either removing or adding solution to
the standard until the color of the solutions to be equal. The experiment also
aimed to apply the Beer-Lambert law and Le Châtelier principle in order to
obtain the equilibrium constants of each solution by using an spectrophotometry.
1.0 Introduction tendency to attract and retain the molecular species with
The term of adsorption is used to specify that the adsorbate which it comes in contact with the surface. Adsorption is
(gas or liquid) is bound onto the adsorbent (solid surface). essentially a surface phenomenon.
This is different from absorption, in which the molecule Adsorption is a term which is completely different from
goes into the interior of the solid. In the case of adsorption, absorption. While absorption means uniform distribution
the process is defined as physical adsorption if the of the substance throughout the bulk, adsorption
adsorbate is held by weak, Van der Waals type of forces essentially happens at the surface of the substance. When
on the surface. If bond formation between the adsorbate both Adsorption and absorption processes take place
and the adsorbent is observed, the process is commonly simultaneously, the process is called sorption.
known as chemical adsorption. The amount adsorbed per Adsorption process involves two components Adsorbent
gram of solid influenced by the specific area of the solid, and Adsorbate. Adsorbent is the substance on the surface
the equilibrium solute concentration in the solution or of which adsorption takes place. Adsorbate is the
pressure in the case of adsorption from the gas phase, the substance which is being adsorbed on the surface of
temperature, and the nature of the molecules involved. adsorbent. Adsorbate gets adsorbed.
𝑥 3.0 Methodology
log ( ) = log 𝐾 + 𝑛𝑙𝑜𝑔𝐶
𝑚 The objective of the experiment was to determine the
equilibrium constant for the formation of ferric
Equation 2: Logarithmic form of Freundlich Adsorption
Isotherm thiocyanate. The calculations were made using the
equations presented above.
Where (x/m) is the weight of the absorbed material per
gram of adsorbent and C is the concentration of the 3.1 Materials and Reagents
solution at equilibrium. The term k and n are constants to This experiment required 20 mL 0.2 M Fe(NO3)3, 40 mL
be evaluated from experimental data in each case. 0.002 M KCNS, and distilled water as reagents. For the
There are some limitations of Freundlich adsorption materials, we used 6 test tubes, 10 mL graduated cylinder,
isotherm. Experimentally it was determined that extent of 50 mL graduated cylinder, ruler, mirror, pipette, aspirator,
adsorption varies directly with pressure till saturation and some white paper.
pressure (Ps) is reached. Beyond that, the point rate of
adsorption saturates even after applying higher pressure. 3.2 Procedure
Thus Freundlich Adsorption Isotherm fails at higher Five (5) dry test tubes of identical size were labelled. By
pressure. serial dilution, solutions of ferric nitrate were prepared. A
20ml of 0.20M Fe(NO3)3 was placed in a 25ml graduated
Langmuir Isotherm cylinder. The 8ml of this solution was transferred into test
The Langmuir equation is based on the assumption that the tube 1. The remaining solution in the graduated cylinder
solid surface is completely uniform. Deviations from the was added with water to bring the volume back to 20ml.
equation indicate lack of uniformity in the surface. It An 8ml of the new solution in the graduated cylinder was
relates the coverage or adsorption of molecules on a solid transferred into test tube 2. The procedures were repeated
surface to gas pressure or concentration of a medium until 5 different concentrations of Fe(NO3)3 were obtained.
above the solid surface at a fixed temperature. The An 8 mL of 0.002 M KCNS was added to every test tube
obtained and a change in color from cloudy-yellow to (Continuation)
blood-red was observed. Then, one of the cuvettes were replaced with the
Each test tube was wrapped with white paper to lessen the Mixture 1 that contains undiluted FeCNS2+ placed in
a cuvette filled with around 2/3 of the total volume.
external light sources that may affect the perception of The measurement of absorbance was then recorded by
a printer directly connected to the spectrophotometer.
color. Test tube 1 served as the standard. By looking down The measurement of absorbance was gathered from
400 nm to 700 nm with 20 nm intervals. The
into the solutions in the test tube, the color intensities of experiment was repeated with Mixture 2, 3, 4 and 5 as
the sample.
the solutions in test tubes 1 and 2 were compared. This
process was aided by placing the test tubes in the presence
The data gathered were then tabulated and
of smartphone flashlight; a mirror can also be used in this plotted with respect to the absorbance and
process. wavelength.
The height of the solution in test tube 2 was adjusted by 4.0 Results and Discussion
the addition of some 0.002 M KCNS solution until the Test Tube
1 2 3 4 5
No.
observed color intensities appeared equal. The heights of
Before 0.025 0.0125 0.00625
0.1M 0.05 M
the solutions in test tubes 1 and 2 were measured using a [Fe3+] M M M
Mixing 0.002 0.002
ruler. The procedures for measuring the heights were 0.002 M 0.002 M 0.002 M
[CNS-] M M
repeated for test tubes 3, 4 and 5. By assuming that the hs (height
10.2
of xxx 10.6 cm 9.6 cm 8.5 cm
entire limiting reagent in test tube 1 was converted to the cm
standard)
hu (height
complex, the concentration of the complex in the test tubes of xxx 11.1 cm
11.1
11.1 cm 11.1 cm
cm
2-5 was calculated using Beer-Lambert’s law. unknown)
0.049045 0.0240 0.01163 5.484 x
[Fe3+] xxx
M 81 M 5M 10-3 M
3.3 Theoretical Framework 4.5 x 10-5 8.1 x 1.35 x 2.34 x
[CNS-] xxx
M 10-5 M 10-4 M 10-4 M
9.55 x 10-4 9.19 x 8.65 x 7.66 x
[FeCNS2+] M
M 10-4 M 10-4 M 10-4 M
Serial dilution of
ferric nitritrate
Based on the data, the absorbance of each concentration of tube 1 with the original concentration of ferric nitrate. the
the sample has its maximum y-value; means has its highest height of the solutions in each is increasing with
peak. In other concentrations, the absorbance reaches decreasing molarity of diluted Ferric nitrate in each test
above 1.0 (too much high). This means that the sample is tube. Intensity of colors was the same and it can be
need to be diluted because the linear absorbance range of assumed that the 5 test tubes are in chemical equilibrium
most spectrometers is between 0.1 and 1.0. Greater than with one another.
means 99.9% of the available light is being blocked by the experiment. The experiment can be considered as
parts of the visible spectrum. While the "color" of a Mixing 0.002 0.002
0.002 M 0.002 M 0.002 M
[CNS-] M M
substance depends on the person observing it, absorption hs (height
10.2
of xxx 10.6 cm 9.6 cm 8.5 cm
of specific wavelengths depends on the molecular cm
standard)
hu (height
structure of the substance. 11.1
of xxx 11.1 cm 11.1 cm 11.1 cm
cm
unknown)
0.04904 0.0240 0.01163 5.484 x
And base on the data gathered, the application of [Fe3+] xxx
5M 81 M 5M 10-3 M
spectrophotometry is that the proportion of light that is 4.5 x 10- 8.1 x 1.35 x 2.34 x
[CNS-] xxx 5
M 10-5 M 10-4 M 10-4 M
absorbed by a solution of a particular compound is a [FeCNS2+ 9.55 x 9.19 x 8.65 x 7.66 x
M
function of the concentration of that compound. And ] 10-4 M 10-4 M 10-4 M 10-4 M
according to the Beer-Lambert Law, absorbance is Keq xxx 432.71 471.15 550.7 596.92
Test tube 5:
20𝑚𝑙 𝑜𝑓 0.02592𝑀 𝐹𝑒(𝑁𝑂3 )3 − 8𝑚𝑙 𝑡𝑜 𝑡𝑒𝑠𝑡 𝑡𝑢𝑏𝑒 5
= 12𝑚𝑙 0.02592𝑀 𝐹𝑒(𝑁𝑂3 )3 𝑟𝑒𝑚𝑎𝑖𝑛𝑖𝑛𝑔
12𝑚𝑙 0.02592𝑀 𝐹𝑒(𝑁𝑂3 )3 + 8𝑚𝑙 𝐻2 𝑂 = 20𝑚𝑙 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛
12𝑚𝑙 𝑥 0.02592𝑀 𝐹𝑒(𝑁𝑂3 )3 = 𝐶 𝑥 20𝑚𝑙
Image 2: The “then and now” comparative analysis 𝐶 = 0.01552𝑀 𝐹𝑒(𝑁𝑂3 )3
𝑐𝑜𝑛𝑐 ′ 𝑛𝑝𝑟𝑜𝑑𝑢𝑐𝑡
Keq =
𝑐𝑜𝑛𝑐 ′ 𝑛𝑟𝑒𝑎𝑐𝑡𝑎𝑛𝑡
9.55 𝑥 10−4
Keq =
(4.5𝑥10−5)(0.049045)
= 432.71
9.19 𝑥 10−4
Keq =
(8.1𝑥10−5)(0.024081)
= 471.15
8.65 𝑥 10−4
Keq =
(1.35𝑥10−4)(0.011635)
= 550.70
Image 3: Adding of 0.002 KCNS
7.66 𝑥 10−4
Keq =
(2.34𝑥10−4)(5.484𝑥10−3)
= 596.92
Test tube 1:
20𝑚𝑙 𝑜𝑓 0.20𝑀 𝐹𝑒(𝑁𝑂3 )3 − 8𝑚𝑙 𝑡𝑜 𝑡𝑒𝑠𝑡 𝑡𝑢𝑏𝑒 1
= 12𝑚𝑙 0.20𝑀 𝐹𝑒(𝑁𝑂3 )3 𝑟𝑒𝑚𝑎𝑖𝑛𝑖𝑛𝑔
Test tube 2:
20𝑚𝑙 𝑜𝑓 0.12𝑀 𝐹𝑒(𝑁𝑂3 )3 − 8𝑚𝑙 𝑡𝑜 𝑡𝑒𝑠𝑡 𝑡𝑢𝑏𝑒 2
= 12𝑚𝑙 0.12𝑀 𝐹𝑒(𝑁𝑂3 )3 𝑟𝑒𝑚𝑎𝑖𝑛𝑖𝑛𝑔
12𝑚𝑙 0.12𝑀 𝐹𝑒(𝑁𝑂3 )3 + 8𝑚𝑙 𝐻2 𝑂 = 20𝑚𝑙 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛
12𝑚𝑙 𝑥 0.12𝑀 𝐹𝑒(𝑁𝑂3 )3 = 𝐶 𝑥 20𝑚𝑙
𝐶 = 0.072𝑀 𝐹𝑒(𝑁𝑂3 )3
Test tube 3:
20𝑚𝑙 𝑜𝑓 0.072𝑀 𝐹𝑒(𝑁𝑂3 )3 − 8𝑚𝑙 𝑡𝑜 𝑡𝑒𝑠𝑡 𝑡𝑢𝑏𝑒 3
= 12𝑚𝑙 0.072𝑀 𝐹𝑒(𝑁𝑂3 )3 𝑟𝑒𝑚𝑎𝑖𝑛𝑖𝑛𝑔
12𝑚𝑙 0.072𝑀 𝐹𝑒(𝑁𝑂3 )3 + 8𝑚𝑙 𝐻2 𝑂 = 20𝑚𝑙 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛
12𝑚𝑙 𝑥 0.072𝑀 𝐹𝑒(𝑁𝑂3 )3 = 𝐶 𝑥 20𝑚𝑙
𝐶 = 0.0432𝑀 𝐹𝑒(𝑁𝑂3 )3