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mc2note-poresize-mesoporosity

The document discusses the determination of pore size distribution in mesoporous solids using gas adsorption methods, specifically the BJH model. It outlines the experimental setup, including the use of nitrogen gas at 77 K and the analysis of adsorption isotherms to derive pore characteristics. The findings indicate a main pore size of 12.6 nm and emphasize the importance of sample preparation for accurate results.

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0% found this document useful (0 votes)
2 views2 pages

mc2note-poresize-mesoporosity

The document discusses the determination of pore size distribution in mesoporous solids using gas adsorption methods, specifically the BJH model. It outlines the experimental setup, including the use of nitrogen gas at 77 K and the analysis of adsorption isotherms to derive pore characteristics. The findings indicate a main pore size of 12.6 nm and emphasize the importance of sample preparation for accurate results.

Uploaded by

Tony Ngo
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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MC² – Material and Chemical Characterisation Facility

Materials Characterisation

Determining the pore size


distribution of mesoporous solids
Introduction
Porous solids have a wide range of adsorption isotherm, experimentally obtained
applications according to the size and as follows. Successive doses of a gas probe,
shape of their pores: water purification, typically N2 at 77 K, are sent to the solid
hydrogen storage, catalysis of chemical material, preliminarily dried and evacuated.
reactions, etc. They are therefore commonly The amount of gas molecules that can be
described by their pore size distribution, adsorbed onto the surface of the solid is
which relates the amount of pore volume for derived from the evolution of the pressure in
each pore diameter. In particular, mesopores the system. The cumulative amount of gas
are defined as pores in the approximate adsorbed plotted with respect to the pressure
diameter range 2 nm to 50 nm. The pore size is the adsorption isotherm.
distribution is usually derived from a gas

Experimental details
 Method: Analysis of mesopores by gas material, dried for 3 h at 350 °C under
adsorption, ISO 15901-2:2006(E) [1] vacuum (unrestricted from 1.33⋅10-2 mbar)
 Instrument: Micromeritics 3Flex  Amount of sample: 230 mg
 Adsorptive gas: N2 at 77 K  Sample holder: glass tube of 12 mm outer
 Sample: reference silica-alumina porous diameter with a seal frit

20
Amount adsorbed (mmol/g)

15 desorption

10

adsorption
5

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Relative pressure

Adsorption isotherm of the reference silica-alumina porous solid. According to the classification of
standard physisorption isotherms (IUPAC [2]) this is a type IV isotherm with a hysteresis loop of
type H2: it is the signature of a mesoporous solid. The adsorption and desorption branches are
different, and a hysteresis loop with non-parallel branches is observed, typical of pores whose size
distribution is wide and shape is not well defined.
MC² – Material and Chemical Characterisation Facility
Materials Characterisation

Results
The adsorption isotherm already contains

Differential pore volume (cm³/g/log nm)


readable information concerning the size 1.2
and shape of the pores. But a precise pore
size distribution can be derived from it
using the Barrett, Joyner and Halenda
(BJH) model. This is an algebraic
0.8
procedure that takes into account the
capillary condensate present in the
mesopores as well as the multilayer film
adsorbed on the walls of the pores. [1]
0.4
In the end the pore size distribution on
the right is obtained. One peak is visible,
which corresponds to the main pore size
of the distribution: 12.6 nm in diameter.
The area under the peak represents the 0
total pore volume in the solid: 0.65 cm³/g. 1 10 100
Pore diameter (nm)

Conclusion
 The distribution of pore size of a  Pore sizes screened by this method range
mesoporous solid can be extracted from the from 2 nm to 150 nm. For larger pores
measurement of its adsorption isotherm mercury intrusion may be used.
using the BJH model.  This method only works on porous solids
 The BJH model is only valid for well-defined that have been dried beforehand, in order
pore shapes, with minimal interconnection to clean the surface and the pores from any
between the pores. adsorbed molecule. This can be done under
 The quantity needed for that experiment is vacuum or dry gas sweeping, and at high
rather large: at least several hundreds of temperature too. If the porous solid cannot
mg and it needs to be known within 2 % undergo drying, thermoporometry may be
error, as the results are always presented in used: it uses calorimetry instead of
specific units. volumetry.

[1] Pore size distribution and porosity of solid materials by mercury porosimetry and gas adsorption —
Part 2: Analysis of mesopores and macropores by gas adsorption, ISO 15901-2:2006(E)
[2] Sing K.S.W., Everett D.H., Haul R.A.W., Moscou L., Pierotti R.A., Rouquérol J. and Siemieniewska T.,
IUPAC Recommendations 1984: Reporting Physisorption Data for Gas Solid Systems with Special
Reference to the Determination of Surface Area and Porosity, Pure & Applied Chemistry 57, 1985, pp. 603-
319

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