Saturday, 1 June 2013

Experiment 3 : Adsorption of Solution


DEFINITION OF ADSORPTION 

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 (the 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.

OBJECTIVE 

In this experiment, adsorption of iodine from solution is studied and Langmuir equation is used to estimate the surface area of activated charcoal sample.



MATERIALS AND APPARATUS 

12 conical flasks, 6 centrifuge tubes, measuring cylinders, analytical balance, Beckman J6M/E centrifuge, burettes, retort stand and clamps, pasteur pipettes, iodine solutions (specified in Table 1), 1% w/v starch solution, 0.1 M sodium thiosulphate solution, distilled water and activated charcoal.

Using burettes or measuring cylinders, fill 12 conical flasks (labeled 1-12) with 50 ml mixtures of iodine solutions (A and B) as stated in the Table 1.

Table 1: Solution A: Iodine (0.05 M)
Solution B: Potassium iodide (0.1 M)



Flask
Volume of solution A (ml)
Volume of solution B (ml)
1 and 7
10
40
2and 8
15
35
3 and 9
20
30
4 and 10
25
25
5 and 11
30
20
6 and 12
50
0


Set 1: Actual concentration of iodine in solution A (X)

For flasks 1-6:
1) Add 1-2 drops of starch solution as an indicator.
2) Titrate using 0.1 M sodium thiosulfate solution until the colour of the
solution changes from dark blue to colourless.


The colour of the solution changes from dark blue to colourless.

3) Record the volume of the sodium thiosulphate used.


Set 2: Concentration of iodine in solution A at equilibrium (C).

For flasks 7-12:
1) Add 0.1g activated charcoal.
2) Cap the flasks tightly. Swirl or shake the flask every 10 minutes for 2 hours.


3) After 2 hours, transfer the solutions into centrifuge tubes and label them accordingly.
4) Centrifuge the solutions at 3000 rpm for 5 minutes and transfer the resulting supernatant into new conical flasks. Label each conical flask accordingly.
5) Repeat steps 1,2 and 3 as carried out for flasks 1-6 in Set 1.

GENERAL NOTES:

Titration equation:
I2 + 2Na2S203 = Na2S4O6 + 2NaI
Na2S2O3 = ½ I2


Given:
1 mole iodine = 2 x 126.9 g
1 ml 0.1 M  Na2S2O3 = 0.01269 gI


       (1 mole  Na2S2O3 =½ mole I2
                         mole I2)
If the amount of activated charcoal used is Y gram, therefore the total mole of iodine
adsorbed by 1 g of activated charcoal (N) is given by the following equation:
N = (X-C) x 50/1000 x 1/y


Results:

Flask
Volume of Na2S2O3 (mL)
1
8.7
2
12.6
3
17.6
4
21.2
5
26.1
6
43.6
7
7.5
8
8.3
9
14.8
10
18.6
11
18.6
12
38.4

DISCUSSION: 

According to the Free Online Dictionary definition, adsorption is a process that occurs when a gas or liquid solute accumulates on the surface of an adsorbent solid or a liquid, forming a molecular or atomic film which is known as the adsorbate. The adsorption from liquid phase can take place in liquid-solid interface, liquid-liquid interface and liquid-vapour interface. Based on this experiment, the adsorption from liquid phase is carried out in the liquid-solid interface. Activated charcoal is used as the adsorbent in this experiment. The Langmuir isotherm is used to calculate the surface area of the charcoal and the calculations are shown below. The Langmuir isotherm is an isotherm derived from a kinetic mechanism, which is based on four hypotheses. The hypotheses are the surface of the adsorbent is uniform, adsorbed molecules do not interact with one another, all adsorption occurs through the same mechanism and at the maximum adsorption, only a monolayer is formed, whereby the molecules of adsorbate do not deposit on other and only presence on the free surface of the adsorbent.


QUESTIONS:
Molecular weight of iodine, I2 : 253.8 gmol-1

1. Calculate N for iodine in each flask.

N=(X-C)x50/1000x1/y (y=0.1g)
ml 0.1M Na2S2O3= 0.01269g I
No. mole = Mass / Molecular weight

Concentration of iodine in solution A,(X)
Concentration of iodine in solution A,(C)
N=(X-C)x50/1000x1/y (y=0.1g)
Flask 1
Mole of iodine = 8.7 ml x 0.01269 gml-1/253.8 gmol-1
        = 4.35 x 10-4 mol
X= 4.35 x 10-4 mol / (50 ml/1000 ml)
   = 0.0087 M

Flask 7
Mole of iodine = 7.5 ml x 0.01269 gml-1/253.8 gmol-1
        = 3.75 x 10-4 mol
C= 3.75 x 10-4 mol / (50 ml/1000 ml) = 0.0075 M
For flask 1 and 7
N= (0.0087 -0.0075) x 50/1000 x 1/0.1
   = 0.0006 molg-1

Flask 2
Mole of iodine = 12.6 ml x 0.01269 gml-1/253.8 gmol-1
        = 6.30 x 10-4 mol
X=6.30 x 10-4 mol / (50 ml/1000 ml)
= 0.0126 M

Flask 8
Mole of iodine = 8.3 ml x 0.01269 gml-1/253.8 gmol-1
        = 4.15 x 10-4 mol
C= 4.15 x 10-4 mol / (50ml/1000 ml)
   = 0.0083 M

For flask 2 and 8
N= (0.0126-0.0083) x 50/1000 x 1/0.1
   = 0.00845 molg-1
Flask 3
Mole of iodine = 17.6 ml x 0.01269 gml-1/253.8 gmol-1
          = 8.8 x 10-4 mol
X= 8.8 x 10-4 mol / (50 ml/1000 ml)
   = 0.0176 M

Flask 9
Mole of iodine = 14.8 ml x 0.01269 gml-1/253.8 gmol-1
          = 7.4 x 10-4 mol
C= 7.4 x 10-4 mol / (50 ml/1000 ml)
   = 0.0148 M

For flask 3 and 9
N= (0.0176-0.0148) x 50/1000 x 1/0.1
   = 1.4 x 10-3 molg-1

Flask 4
Mole of iodine = 21.2 ml x 0.01269 gml-1/253.8 gmol-1
          = 1.06 x 10-3 mol
X= 1.06x 10-3 mol / (50 ml/1000 ml)
   = 0.0212 M
Flask 10
Mole of iodine = 18.6 ml x 0.01269 gml-1/253.8 gmol-1
          = 9.3 x 10-4 mol
C= 9.3 x 10-4 mol / (50 ml/1000 ml)
   = 0.0186 M

For flask 4 and 10
N= (0.0212-0.0186) x 50/1000 x 1/0.1
   = 1.3 x 10-3 molg-1


Flask 5
Mole of iodine = 26.1 ml x 0.01269 gml-1/253.8 gmol-1
        = 1.305 x 10-3 mol
X= 1.305 x 10-3 mol / (50 ml/1000 ml)
   = 0.0261 M

Flask 11
Mole of iodine = 18.6 ml x 0.01269 gml-1/253.8 gmol-1
        = 9.3 x 10-4 mol
C= 9.3 x 10-4 mol / (50 ml/1000 ml)
   = 0.0186 M

For flask 5 and 11
N= (0.0261-0.0186) x 50/1000 x 1/0.1
   = 3.75 x 10-3 molg-1

Flask 6
Mole of iodine = 43.6 ml x 0.01269 gml-1/253.8 gmol-1
        = 2.18 x 10-3 mol
X= 2.18 x 10-3 mol / (50 ml/1000 ml)
   = 0.0436M     
Flask 12
Mole of iodine = 38.4 ml x 0.01269 gml-1/253.8 gmol-1
        =1.92 x 10-3 mol
C= 1.92 x 10-3 mol / (50 ml/1000 ml)
   = 0.0384M

For flask 6 and 12
N= (0.0436-0.0384) x 50/1000 x 1/0.1
   = 2.6 x 10-3 molg-1

 

2) Plot amount of iodine adsorbed (N) versus balance concentration of solution (C) at equilibrium to obtain adsorption isotherm.


Flasks


X (M)
C (M)
Y (g)
N (mol)
1 and 7
0.0087
0.0075
0.1
0.0006
2 and 8
0.0126
0.0083
0.1
0.00845
3 and 9
0.0176
0.0148
0.1
1.4 x 10-3
4 and 10
0.0212
0.0186
0.1
1.3 x 10-3
5 and 11
0.0261
0.0186

0.1
3.75 x 10-3
6 and 12
0.0436
0.0384

0.1
2.6 x 10-3


click to enlarge

3) According to Langmuir theory, if there is no more than a monolayer of iodine adsorbed on the charcoal,

C/N = C/Nm + I/KNm
Where C   =        concentration of solution at equilibrium 
                    Nm=       number of mole per gram charcoal required
   K  =        constant to complete a monolayer

Plot C/N versus C, if Langmuir equation is followed, a straight line with slope of 1/Nm and intercept of 1/KNm is obtained.
Obtain the value of Nm, and then calculate the number of iodine molecule adsorbed on the monomolecular layer. Assume that the area covered by one adsorbed molecule is 3.2 x 10-19 m2, Avogadro no. = 6.023 x 1023 molecule, calculate the surface area of charcoal in m2g-1.



Concentration Of Solution, C (M)
Amount Of Iodine Adsorbed, N (molg-1)
C/N (M/molg-1)
0.0075
0.0006
12.500
0.0083
0.00845
0.982
0.0148
1.4 x 10-3
10.571
0.0186
1.3 x 10-3
14.307
0.0186

3.75 x 10-3
4.96
0.0384

2.6 x 10-3
14.770
click to enlarge


Calculate the surface area of charcoal in m2g-1.

From the graph the gradient is used to determine the number of mole per gram charcoal required (Nm)

Gradient, m =  (10.571-0) M/molg-1 ÷ (0.0148-0) M
            =  714.26 gmol-1

In general the gradient is equal to 1/ Nm, therefore

1/Nm = 714.26
Nm = 1/714.26
       = 1.4x10-3molg-1

From the Nm 1.4x10-3molof iodine is adsorbed in 1 g of charcoal. Therefore, the number of mol of iodine molecules that adsorbed on the monomolecular layer is 

= 1.4x10-3mol/1g =1.4x103mol.

The number of molecules of the iodine molecules
= number of mole of iodine molecules x Avogadro no.
=1.4x10-3mol x 6.023x 1023
=8.4325 x 1020 molecules of iodine

Assume the surface covered by one adsorbed molecules is 3.2x 10-19 m2
1 molecules of iodine = 3.2x 10-19 m2 adsorbed on the charcoal layer.

Therefore, 8.4325 1020 molecules of iodine
= (3.2x 10-19 m2)  x (8.4325 x 1020)

= 269.84 m2g-1 adsorbed on the charcoal layer

4) Discuss the results of the experiment. How do you determine experimentally that equilibrium has been reached after shaking for 2 hours?



The way to determine that the equilibrium has been reached after shaking for 2 hours is by observing the colour changes in the flask. The iodine will undergo colour change from dark brown to light brown at certain period of time after the flask is shook for every 10 minutes for 2 hours. The light brown colour of the iodine will not change until the end of the reaction and this marks the equilibrium point of the reaction. There is a change in the colour of the iodine throughout the reaction due to the adsorption of iodine by the activated charcoal. The equilibrium of the reaction can also be determined by observing the colour change of the sodium thiosulfate solution using titration method. The sodium thiosulfate solution will change colour from dark blue to colourless to mark the point of equilibrium of the reaction.
           
            Based on results obtained from the experiment, there are many errors that cause the results of the experiment to be lack of accuracy. Firstly, there are parallax error that occurs when recording the readings from the burette. This is due to the wrong position of the eye to the meniscus level of the solution. Secondly, the time taken for the flask to be shaken for every 10 minutes for two hours is shorten to one hour and 30 minutes only. This will definitely affect the accuracy of the readings obtained in the experiment. Moreover, there a few person who are in charge of shaking all the flasks at all time which have different speed and strength in shaking the flasks. This will cause the consistency of the readings to be affected. The activated charcoal maybe accidentally spilled when the charcoal is added to the flask. This will affect the readings obtained from this experiment. The centrifuge tubes and the flasks may not be capped tightly and this also causes the spillage of the solution. 

PRECAUTIONS


1. We must make sure that our eyes are directly perpendicular on the meniscus of the solution when we are recording our readings. This is to prevent parallax errors from occurring.

2. The flasks have to be shaken for every 10 minutes for 2 hours instead of shaking the flasks for 1 hour and 30 minutes only. This is to improve the accuracy of readings obtained in the experiment.

3. The same person must be in charge to shake all the flasks at all time so that the speed and the strength used to shake the flasks are the same. This will improve the consistency of the readings obtained.

4. The flasks have to be capped tightly to prevent the spillage of solution. The spillage of solution will affect the accuracy of readings obtained.

5. The same person must be in charge of titrating the volume of thiosulphate solution in each of the conical flask so that the change in the colour of the solution can be determined by the same person. This is to ensure that accuracy of readings is improved. 

6. A filter funnel must be used to add the activated charcoal into the flask respectively. This is to prevent the activated charcoal from spill and increases the accuracy of the results obtained. 


CONCLUSION 

The purpose of carrying out this experiment is to identify the surface area of the charcoal by studying the adsorption of iodine from solution process. The Langmuir equation is used to calculate the surface area of the charcoal. The Nm value is 1.4x103 g mol-1. The number of molecules of iodine adsorbed onto the monomolecular layer is 8.4325 x 1020 molecules of iodine. The surface area of charcoal is 269.84 m2g-1.

REFERENCES 


  1. Florence Alexander T and Attwood David. 2006. Physicochemical Principles of Pharmacy. Fourth Edition. MacMillan Press Ltd. Great Britain. Page 194 until 200  
  2. Aulton M. E. 2002. Pharmaceutics The Science Of Dosage Form Design. Second Edition. Churchhill Livingstone Press. Spain. Page 65 until 68
  3. http://en.wikipedia.org/wiki/Adsorption
  4. http://www.rpi.edu/dept/chem-eng/Biotech-Environ/Adsorb/adsorb.htm
  5. http://www.fpharm.uniba.sk/fileadmin/user_upload/english/Physical_Chemistry/5-Adsorption.pdf
  6. http://www.le.ac.uk/chemistry/thermodynamics/pdfs/500/Topic0140.pdf
  7. http://www.scribd.com/doc/33000065/Adsorption-in-Physical-Pharmacy