Nom: NGUYEN LUU MINH

Prénom: THIEN

REPORT OF CHARACTERIZATION OF THE POROSITY FROM NITROGEN

ADSORPTION MEASUREMENTS LABORATORY CLASSES

A) SHORT DESCRIPTION OF A N2 ADSORPTION-DESORPTION EXPERIMENT

B) TREATMENT OF THE RESULTS OBTAINED FROM A N2 ADSORPTION-DESORPTION
EXPERIMENT.
The provided data is given below:

1
Nom: NGUYEN LUU MINH
Prénom: THIEN

1. Specify the type of porous material?

The type of porous material is meso porous due to the appearance of capillary
condensation (indicated by the hysteresis loop in isotherm plot)

2. Calculate its specific surface area?

Choose the isotherm value in relative pressure range: 0.05 < P/Ps < 0.3

Relative Pressure Vol Adsorbed

P/Ps (cm3/g STP)
0.06 145.47
0.08 151.15
0.10 158.69
0.12 164.17
0.14 169.20
0.16 173.92
0.18 178.31
0.20 182.70
0.25 191.54

Linearization of BET equation:

𝑃
𝑃 1 𝐶−1𝑃 𝑃𝑠 1 𝐶−1𝑃
= + → = +
𝑉(𝑃𝑆 − 𝑃) 𝑉𝑚 𝐶 𝑉𝑚 𝐶 𝑃𝑠 𝑃 𝑉𝑚 𝐶 𝑉𝑚 𝐶 𝑃𝑠
𝑉 (1 − )
𝑃𝑠
𝑃
𝑃𝑠 𝑃
𝐶𝑎𝑙𝑙 𝑦 = ,𝑥 = 𝑤𝑒 ℎ𝑎𝑣𝑒
𝑃 𝑃𝑠
𝑉 (1 − )
𝑃𝑠
1 𝐶−1
𝑦= + 𝑥
𝑉𝑚 𝐶 𝑉𝑚 𝐶

2
Nom: NGUYEN LUU MINH
Prénom: THIEN

We make a new table:

𝑃
𝑃 𝑃𝑠
𝑃𝑠 𝑃
𝑉 (1 − )
𝑃𝑠
0.06 4.43E-04
0.08 5.46E-04
0.10 7.03E-04
0.12 8.35E-04
0.14 9.70E-04
0.16 1.11E-03
0.18 1.25E-03
0.20 1.39E-03
0.25 1.71E-03

1 𝐶−1
𝑃𝑙𝑜𝑡 𝑖𝑡 𝑜𝑛 𝑒𝑥𝑐𝑒𝑙, 𝑎𝑛𝑑 𝑢𝑠𝑖𝑛𝑔 𝑡𝑟𝑒𝑛𝑑𝑙𝑖𝑛𝑒 𝑡𝑜 𝑜𝑏𝑡𝑎𝑖𝑛 𝑎𝑛𝑑
𝑉𝑚 𝐶 𝑉𝑚 𝐶

y = 0.0068x + 2E-05
R² = 0.9995
0.0018
0.0016
0.0014
0.0012
0.001
0.0008
0.0006
0.0004
0.0002
0
0 0.05 0.1 0.15 0.2 0.25 0.3

1
= 2. 10−5 𝑐𝑚 3 @𝑆𝑇𝑃
𝑉𝑚 𝐶 𝑉 = 146.62
→{ 𝑚 𝑔𝑠𝑎𝑚𝑝𝑙𝑒
𝐶−1
= 0.0068 𝐶 = 341
{ 𝑉𝑚 𝐶

Change adsorbed volume of monolayer to mole N2 adsorb (mono layer)

3
Nom: NGUYEN LUU MINH
Prénom: THIEN

𝑐𝑚 3 @𝑆𝑇𝑃 1 𝑚𝑜𝑙 −3
𝑚𝑜𝑙
𝑛𝑁2 = 146.62 × = 6.55. 10
𝑔𝑠𝑎𝑚𝑝𝑙𝑒 22414 𝑐𝑚 3 @𝑆𝑇𝑃 𝑔𝑠𝑎𝑚𝑝𝑙𝑒

Calculate surface area:

𝐴 = 𝑛𝑁2 × 𝑁𝐴 × 𝐴𝑁2 𝑀𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 = 6.55. 10−3 × 6. 1023 × 16.2 = 6.36. 1022 Å = 636 𝑚2

3. Calculate the Kevin radii corresponding to the two extremities of the hysteresis
loop, and that of corresponding to the inflexion point in the desorption curve?
Kevin radius is expressed as follows:
−2𝛾𝑐𝑜𝑠𝜃
𝑟𝐾 =
𝑃
𝑅𝑇𝑙𝑛 ( )
𝑃𝑠
3 points of P/Ps is 0.45, 0. 65, 0.86 respectively, so the Kevin radii corresponding is:
𝑃 −2(8.85 × 10−5 ) × 34.65 × cos(0) 𝑛𝑚
@ = 0.45, 𝑟𝐾 = × (109 ) = 1.19 𝑛𝑚
𝑃𝑠 83144 × 77.4 × 𝑙𝑛(0.45) 𝑚
𝑃 −2(8.85 × 10−5 ) × 34.65 × cos(0) 𝑛𝑚
@ = 0.65, 𝑟𝐾 = × (109 ) = 2.21 𝑛𝑚
𝑃𝑠 83144 × 77.4 × 𝑙𝑛(0.65) 𝑚
𝑃 −2(8.85 × 10−5 ) × 34.65 × cos(0) 𝑛𝑚
@ = 0.86, 𝑟𝐾 = × (109 ) = 6.32 𝑛𝑚
𝑃𝑠 83144 × 77.4 × 𝑙𝑛(0.86) 𝑚

4. Calculate the adsorbed thickness for the 3 associated values of P/Ps. What can you
conclude?
N2 adsorbed layer thickness t is expressed as follows:
1/3
−5
𝑡 (𝑛𝑚) = 0.343 × [ ]
𝑃
ln ( )
𝑃𝑠
3 points of P/Ps is 0.45, 0. 65, 0.86 respectively, so the Kevin radii corresponding is:
1
3 1
𝑃 −5 −5 3
@ = 0.45, 𝑡(𝑛𝑚) = 0.343 × [ ] = 0.343 × [ ] = 0.63 𝑛𝑚
𝑃𝑠 𝑃 ln(0.45)
ln ( )
𝑃𝑠
1
3 1
𝑃 −5 −5 3
@ = 0.65, 𝑡(𝑛𝑚) = 0.343 × [ ] = 0.343 × [ ] = 0.78 𝑛𝑚
𝑃𝑠 𝑃 ln (0.45 )
ln ( )
𝑃𝑠
1
3 1
𝑃 −5 −5 3
@ = 0.86, 𝑡(𝑛𝑚) = 0.343 × [ ] = 0.343 × [ ] = 1.1 𝑛𝑚
𝑃𝑠 𝑃 ln(0.45)
ln ( )
𝑃𝑠

4
Nom: NGUYEN LUU MINH
Prénom: THIEN

5. Calculate the pore volume and then the porosity assuming that the solid skeleton is
made of single oxide (density of SiO2 equal to 2.2 g.cm-3)

P saturation is obtained from isotherm plot, Psat = 767.76 mmHg  Volume

adsorbed saturation Vs = 418.83 cm3@STP/g_sample
Total pore volume is:
𝑉𝑃 = 0.001557 × 𝑉𝑆 = 0.001557 × 418.83 = 0.65 cm3_pore/g_sample
Density of dense silica is 2.2 g/cm3
Specific volume of dense silica is:
1
𝑉𝑠𝑘𝑡 = = 0.45 𝑐𝑚3_𝑠𝑜𝑙𝑖𝑑/𝑔_𝑠𝑎𝑚𝑝𝑙𝑒
2.2
Porosity of the sample is:
𝑃𝑜𝑟𝑒 𝑉𝑜𝑙𝑢𝑚𝑛 𝑃𝑜𝑟𝑒 𝑣𝑜𝑙𝑢𝑚𝑛
Porosity = =
𝑆𝑎𝑚𝑝𝑙𝑒 𝑉𝑜𝑙𝑢𝑚𝑛 𝑃𝑜𝑟𝑒 𝑣𝑜𝑙𝑢𝑚𝑛 + 𝑆𝑘𝑒𝑙𝑒𝑡𝑜𝑛 𝑣𝑜𝑙𝑢𝑚𝑛
0.65
𝑃𝑜𝑟𝑜𝑠𝑖𝑡𝑦 = = 0.588 = 58.8%
0.65 + 0.455