Experiment No: 3

Experiment Name: Chemisorption studies using CO as adsorbate

I. Aim: To determine the metal dispersion and active metal surface area of Ni/AC catalyst by CO pulse
Chemisorption

II. Procedure:

(A) Starting instrument

1. Open carrier gas (Helium) cylinder.

2. Switch on the computer.
3. Switch on chemisorb and Press A make sure that carrier gas He is flowing through the TCD.
4. Make path ' Bypass' mode and Delay in 'short' mode.
5. Adjust the gas flow to 30 cm3/min
6. Wait for 30-45 minute for stabilization.
7.
(B) Pulse chemisorption experiment procedure:

1. Take a quartz sample tube and make sure that it is clean and dry.
2. Insert small amount of quartz wool in the bottom of the sample tube.
3. Weight out 20-50mg of sample.
4. Connect the sample tube in the preparation port.
5. Slide the heating mantle upward around the sample tube and gently push the clip.
6. Specify the desired temperature (150oC) using the Temp Set dials.
7. Press Prep Gas button for preparation gas (Helium).
8. After competition of degassing, set temp set dials to 000 and switch off preparation button.
9. After removing the sample tube from preparation port immediately connect to analysis port.
10. Reduce the sample with H2/Ar at the reduction temperature (300oC) for 1 h.
11. After complete reduction the flushed out by He gas at a temperature 200oC for 1h.
12. Cool the sample to the room temperature.
13. Open TPx software (it will display a menu)
14. Click on File then open then sample information and Enter the serial no to create a file.
15. Select sample information and give the sample name, mass, comment then save and close.
16. Select analysis condition for Co pulse chemisorption.
17. Select wait for baseline stable then start recording.
18. Inject 0.5cm3of 10%Co/He
19. Repeat until the sample is saturated(suggest constant peak area)
20. Click Report option to get the final report.

III. Results and Analysis:

I. Instrument name (Make and Model):
II. Sample name:
III. Sample amount:
IV. Analysis gas:
V. Carrier gas:
VI. Temperature:
VII. Pulse volume:
Table 1: Observations
Serial No. Pulse No Volume adsorbed Area

(a) Total volume chemisorbed: ______________________________

(b) % metal dispersion: _____________________________________
(c) Active metal surface area per gm of sample: ___________________

VI. Precautions to be taken:

1. Never switch on the instrument without any carrier gas
2. For best results, the ChemiSorb 2720 should be free of air before performing analyses. Purging should
be performed when: it is initially put into operation and has been idle for several days
3. Each and every injection should be steady.
4. Certain catalysts, when heated and exposed to reducing or oxidizing gases can give off noxious and
corrosive gases.
5. Use of reagent-grade gases is always recommended.

VII. Example analysis:

Aim: CO chemisorption on 0.5 wt % Platinum on Alumina
Result:
(a) Sample name: 0.5 wt % Platinum on Alumina
(b) Sample amount: 1gm
(c) Analysis gas: 10%Co/He
(d) Carrier gas: He
(e) Temperature: 22oC
(f) Pulse volume: 0.5cm3

a. Volume of Active Gas Injected From a Syringe 10 %CO /He

Vinj = Vsyr × ( Tstd/Tamb) × ( Pstd/Pamb) ×( %A/100)

Vsyr = syringe volume injected =0.5 cm3

Tstd = ambient temperature =22oC
Tamb = standard temperature 273K
Pamb = ambient pressure =743mmHg
Pstd = standard pressure=760mmHg
%A = % active gas =10%

Vinj = 0.5 cm3 × [273K / (22 +273K)] × (743 mmHg / 760mmHg) × (10/100) = 0.0453cm3

b. Calculating Volume Chemisorbed:

Vinj = volume injected= 0.0453 cm3

 m = mass of the sample = 1 gm
Ai = area of peak i =0.00648

Vads = 0.1847cm3/g m

c. % Metal Dispersion:

Sf = stoichiometry factor, CO on Pt=1

Vads = volume adsorbed=0.l803 cm3/gm
Vg = molar volume of the gas at STP= 22414 cm3/mol
m.w. = molecular weight of the metal =195.078 amu
%M = % metal =0.5%

d. Active Metal Surface Area (per gram of sample)

Sf = stoichiometry factor, CO on Pt=1

Vads = volume adsorbed= 0.1803 cm3/g
Vg = molar volume of the gas at STP= 22414 cm3/mol
NA = Avogadro’s number = 6.023 x 1023 molecules/mol

ࢾm = cross-sectional area of active metal atom =0.08 nm2