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Micromeritics ASAP2060

User Familiarization Training


Sains Gunaan UiTM
9 May 2017

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Particle Characterization is the analysis of the particles physical
parameters affecting properties of products and processes

COMPANY BACKGROUND

Founded by Warren Hendrix and Dr. Clyde Orr

Company was incorporated in 1962 50 years in the business


50 years of experience in designing, manufacturing, distributing, and servicing
innovative analytical instrumentation in the fields of particle science and technology

Expanded our headquarters from ~7,250 m2 to ~13,000 m2 in July 2008 doubled


our manufacturing capacity and support centers

Provide support to our entire global operations from our headquarters in


Norcross, Georgia

Micromeritics was awarded ISO 9001 certification in February 1994.


Micromeritics has achieved the ISO 9001:2008 certification. We are dedicated
to ongoing improvements and quality and customer satisfaction at all levels of
our operations.

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MACHINE SHOP

LABORATORY
FINAL ASSEMBLY

Worldwide Distribution & Support Network

3
Our Customers

Micromeritics In Malaysia
Local Lab in Shah Alam
Lab Services
User Training
Local expertise for application support
Highly skilled local technical team

4
Surface Area and Porosity

Non-porous solid Porous solid


Low specific surface area High specific surface area
Low specific pore volume High specific pore volume

Pore Classification
Accessibility - Open Pores/Closed Pores
Open Pores accessible to external fluid/Gas adsorption
Closed Pores Not assessible but affect the bulk density
Open Pores Through Pores / Blind Pores
Through Pores open channel at 1 location, extend into particle and re-emerge
at different location ( e.g. c-e-c, c-e-d )
Blind Pores Dead end Pores ( e.g b and f )

Reference : F. Rouquerol J.Rouquerol & K.Sing

5
Pore Classification
By Shapes

Ink Bottle
Cyclindrical

Slit

Wedge

Pore Size Classification

Pore size classification:

6
Adsorptive, Adsorbate, Adsorbent
Adsorptive

Adsorbate

adsorbent

Physisorption Vs Chemical Adsorption

7
Physisorption Vs Chemical Adsorption

Absorptive Gas and Cryogenic


Temperature
Gases Cryogenic Temperature
Nitrogen( N2 ) Liquid Nitrogen(77K ), Liquid Argon(87K)

Argon ( Ar ) Liquid Nitrogen(77K ), Liquid Argon(87K)

Kryton Liquid Nitrogen(77K ), Liquid Argon(87K)

Carbon Dioxide ( CO2) Dry Ice / Circulating Water Bath @ 0 C

8
Commonly Used Adsorptives for Surface Area
and Pore size Analysis
Nitrogen: at 77.35 K (liquid nitrogen temperature, T/Tc = 0.61)
pore size analysis of micro-,meso and macropores
surface area analysis

Argon: at 77.35 K (T Tr = - 6.5 K; Tr : bulk triple point


temperature; T/Tc = 0.50)
at 87.27 K (liquid argon temperature, T/Tc = 0.57 )
pore size analysis of micro- , meso- and macropores
surface area analysis

CO2 : at 195 K (T/Tc = 0.63)


at 273 K (T/Tc = 0.89) pore size analysis of micropores
of widths < 1.5 nm (particularly for microporous carbons)

Krypton : at 77.35 K (T Tr = - 38.5 K) measurement of very low


surface areas
at 87.27 K (T Tr = - 28.5 K) pore size analysis of thin
micro/mesoporous films (M. Thommes et al, 2005)

Argon Adsorption at 87.27 K


Due to weaker attractive fluid-wall interactions (and
the lack of a quadrupole moment), argon fills
micropores of dimensions 0.4 nm 0.8 nm at much
higher relative pressures, (.i.e., at least 1.5 decades
higher in relative pressures) as compared to
nitrogen.
High resolution adsorption isotherm of high
accuracy can be measured over the complete micro-
mesopore range, in less time.

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CO2 Micropore Analysis of Porous Carbons
at 273.15 K
At elevated temperatures and higher absolute pressure (P0 =
26200 Torr) CO2 can access micropores, which are not
accessible for nitrogen at 77 K.
Fast analysis: due to higher diffusion rate equilibrium is
achieved faster as compared to nitrogen adsorption at 77 K
dramatic decrease in analysis time i.e., 3-5 h for CO2
versus 30-50 h N2.
No need for high vacuum system with turbomolecular pump;
10-3 torr vacuum is sufficient.
No need for a low-pressure transducer; 1000 Torr transducer is
sufficient.

General Process Flow for Gas adsorption Analysis:-

Sample Preparation Prepare sample into sample tube

Degas Clean Sample before adsorption

Analysis Dose Gas and determine adsorption


- Produce Isotherm

Data Reduction using Generate Process Isotherm data to get results


Models ( BET, BJH, t-plot, Report ( Surface area, Pore Size/Volume distribution
Harvath Kawazoe, DFT etc)

Slide 20

10
Definition of Saturation Pressure
P0 , P0 - Saturation pressure ( of
the cryogen)
Psat Saturation pressure of the
adsorptive

Saturation Pressure & Bath Temperature

N2

Gas = N2
Bath Temp. = LN2(77K)
P0 = 1 atm (~760mmHg)

CO2

Gas = CO2
Bath Temp = Chilled water@0C
P0 = 34.4 atm (~26142mmHg)

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Physisorption

Relative Pressure ( P/P0)


Convenient way to study adsorption isotherm regardless of Gases/Bath
Scale from 0 1 ( Completely Saturate )
Gas adsorption mechanism occurred at specific P/P0
Example:
Micropore Filling : << 0.01 P/P0
Monolayer Formation ( Surface Area Determination ) : 0.05 P/P0 to 0.3 P/P0
Multiple Layer Formation : > 0.1 P/P0
Mesopore Pore filling : up to ~ 1 P/P0
Example 1 : N2 in Liquid Nitrogen
P0 of N2 at -196C is 760mmHg
76mmHg of N2 = 76/760 = 0.1 P/P0

Example 2 : CO2 at Different Bath Temperature


P0 of CO2 at -78C is 760mmHg
P0 of CO2 at -0C is 26485 mmHg
76mmHg of CO2 @-78C = 76/760 = 0.1 P/P0
76mmHg of CO2 @ 0C = 76/26485 = 0.003 P/P0

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Isotherm
The amount of gas adsorbed is a
function of
The strength of interaction between gas
and solid (intrinsic)
Temperature (fixed)
Pressure (controlled variable)
expressed as relative pressure P/Po

Sample Preparation - Degas


Purpose:
To remove absorbed volatile contaminants from sample ( Moisture, CO2 etc )
Clean surfaces accessibility of pores and surface

Methods:
1. Heat/Vacuum
2. Heat/Flow Inert Gas

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The Major Component of Gas adsorption Instrument
Degas System (Flow/Vacuum)
Analysis System
Accessories ( Dewar , sample tube )
Vacuum System

Flow / Vacuum Degas


Performance Considerations
Economical Considerations
Time

Mesopore Micropore

14
Volumetric Gas Adsorption Measurement
Remove adsorbed
Degas Sample Contamination Determine Saturation
Psat Pressure
Measurement Can be manually
Transfer from Degas port to Analysis Port entered

Remove all gases Remove N2 gas


Evacuate Sample Evacuate Sample prior to start analysis
prior to next step

Freespace Dosing Pressure Dosing N2 gas


Measurement pressure targets
Points
Measured Volume
Determine Warm/Cold adsorbed
Freespace using Helium gas
Can be manually entered Vol

Evacuate Sample Remove He gas


prior to next step End
p/p0

Freespace Measurement
Is the voids volume inside sample tube not occupied by samples
Quantity of gas absorbed by sample must subtract freespace .
Freespace is sensitive to temperature variation ( Need constant
temperature throughout analysis)
Measure using He gas
Freespace perform ONCE b4 analysis LN2 dissipates during analysis(
hence changing the cold/warm space

Warm Zone

FIlled with He Cold Zone


LN2

Dewar

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Freespace Measurement
Pressure
Manifold P
Transducer Ideal Gas Law
NN
Sample Valve PV = nRT
NN

nads = ndosed -
NN
NN
NN
NN
NN N

nfreespace
N
NN
NN
N

N
NN
N
N

N
nads = (PV/RT)man. - (PV/RT)cell
NN
N N
NN
N
N
N
NN
N
N
NN
N
N
N
N N
N
N N
N
N N
NN
N
N
N
N N
N
N
N
NN N NN N
N N
N N N
N
N NN
N N
N N
N
N N
N N

Cryogen Control Freespace Measurement

Warm Zone
Warm Zone

Cold Zone
LN2 LN2
Cold Zone

Dewar Dewar

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Freespace :Low Surface Area
Freespace error Worst case for
Low surface area
Minimize Free-space Errors K
NN
NN
NN
Psat for Kr K NN
NN

NN
2.5 mm Hg at 77.3 K K
NN N
NN
N
K NN
Psat for N2 K
N
N
N
760 mm Hg at 77.3 K K NN
N
N
NN

Relative free-space error Kr/N2


K N N
NN
K N
N
N
2.5/760 = 1/300
K N N
N
N
K N N
N
N
K N
N N
K N
N N
N
K N N
NN
N
K N
K N
N N
N
N
N
K N
N NNN N
K N N
N N N
N

Micromeritics Freespace Solution


Patented Isotherml Jacket
Advantages
Fixed Cold / Warm Freespace throughout analysis as long
As the liquid Nitrogen touches the Isothermal Jacket
Durable solution - Last a lifetime
Warm Move movement during analysis No abrupt change
Freespaceof temperature
Very effective for long analysis duration
Can be refill during analysis - Extends the analysis time
Cold freespace

beyond the dewar capacity

Disadvantages
Large Cold Freespace - Disadvantages for very low
Surface areas samples . Low surface areas sample more
Sensitive to freespace error

T = 77K T = 77K

17
The method of liquid nitrogen level
control in the Competitor Q

Liquid
sensor
The Dewar is raised
by the elevator as
cryogen evaporates End of
by use of a analysis

thermistor. Middle
part
The Dewar cannot
be refilled for
extended analyses.

Cooler

The signal from the liquid


sensor makes the Dewar
elevator raise

Physisorption

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Physisorption

Physisorption

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Volumetric Gas Adsorption Method
Gas Law
PV = nRT
nads = ndosed - nfreespace
nads = (PV/RT)man. - (PV/RT)cell

Gas Adsorption Mechanism

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IUPAC Classification of Adsorption
Isotherms

Type I Isotherm Microporous Samples


Limiting value (plateau) due to filled
pores and essentially zero external
area.

Steep initial region due to very


strong adsorption, for example in
micropores.

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Gas Adsorption

Type II Isotherm Macroporous Samples

Absence of hysteresis indicates adsorption


on and desorption from a non-porous
surface

Low slope region in middle of


isotherm indicates first few
multilayers
Rounded knee indicates approximate
location of monolayer formation.

Type IV Isotherm Mesoporous Samples

Hysteresis indicates capillary


condensation in mesopores

Low slope region in middle of


isotherm indicates first few
multilayers
Rounded knee indicates
approximate location of monolayer
formation.

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Type III Isotherm - Macroporous Samples

Low C Value - Little Affinity for Surface


BET not applicable

Lack of knee represents extremely weak


adsorbate-adsorbent interaction

Type V Isotherm - Mesoporous Samples


Low C Value - Little Affinity for Surface
BET not applicable

Lack of knee represents extremely weak


adsorbate-adsorbent interaction

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Type VI Isotherm - Stepped Isotherm
Strong Interaction with Surface
Uniform non porous surface

Particle Properties Surface Area & Porosity


Industries Examples
Oil & Gas All chemical reaction required catalyst.
Surface area & porosity define the efficiency of the catalyst
Environmental Control Control release of green house / Toxic gas
removal to environment
Filtration Drinking water, dioxin removal from food etc
Future Energy Fuel cell required H2 storage material etc
Ideally, need material with high surface area with the right pore structure
For the intended purpose in order to maximize the efforts

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This image cannot currently be display ed.

ASAP 2060
Dedicated Micropore and
Low Surface Area Analyzer

Designed to Perform
The ASAP 2060 is a research grade, single-port,
dedicated, true micropore (0.1 mmHg) and low
surface area instrument

1. This is an instrument built for the purpose of providing


research grade results for microporous or low surface
area samples at a very affordable cost .

2. The ASAP 2060 is available with MicroActive Data


software. Its fully compatible with Windows 7, 8, 32-bit
and 64-bit Windows operating systems.

3. A unique option, is that up to four ASAP 2060s can be


operated sharing a single turbo pumping station and
manifold system. Software control permits the shared
vacuum system to operate without compromising
results to each unit within the system.

4. An available solutions kit has an ASAP 2060 that


includes a FlowPrep 6-postion degasser, and regulator
expansion kit.

ASAP 2060

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Std. 0.1mmHg and Proprietary transducer
10mmHg transducers system delivers quick
response , stability and
improved S/N
Stainless-steel manifold
provides optimized
internal volumes for Up to 4 instruments
highly accurate can share a single
measurements turbo vacuum system
with optional manifold
kit
MicroActive Interactive
Data Software
Proven Isothermal
Jacket Cold Zone
Control

Long duration,
Six analysis gas inlets >80 hr. refillable
with dedicated helium dewar
free-space ports

ASAP 2060

for ASAP 2060

Extensive range of reports- Extensive range of


NFDLT models for calculating pore size distributions.
Includes over 19 physisorption reports

Overlay multiple runs and Mercury Intrusion Data -


MicroActive for ASAP 2060 provides the ability to
overlay up to 25 runs. Included is the option to import
mercury intrusion data to provide analysis data in the
micro to macropore range in a single report

User selectable data ranges- Permits user to select


data ranges through the graphic interface permitting
direct modeling for BET, t-Plot, Langmuir, DFT
interpertation.

User defined reports- With powerful Python


programming language users can develop their own
extensions to standard reports to fully customize
results data to meet their individual application needs.

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Optional
Optional Iso-
Chiller- Controller
Dewar Thermo-electric
Liquid recirculation Chiller-Dewar
system for accurate Peltier thermo-electric
temperature control controlled
through the use of temperature device
an external
refrigerated
circulation bath
Temp. range: 5 C to 75 C (lab temp <27 C)
Cooling Capacity: Approx. 80W at 0 C, 120W at 25 C
Minimum Controllable Resolution : 0.1 C
Temp. Stability : 0.1 C

Optional
MicroPrep
In-situ degassing
High quality, digital control unit regulates
heating mantle to desired set-
temperature
Temp. range: ambient to 250 C
Ramp rate: 10 C/min.
Temp. Stability : 5 C

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Specifications

Pressure Measurement:
0 to 950 mmHg

Transducers:
1000 mmHg, 10.0 mmHg and 0.1 mmHg

Resolution: Up to 1 x 10-7 torr


(0.1 mmHg transducer)

System Capacity:
Single Port, Up to four Individual
Instruments can share a single
turbo vacuum system

Cryogen System: 3 L, > 80 hr. dewar

Electrical Requirements:
150A max, 50/60Hz, 100-240V

Dimensions:
Width: 36.5 cm
Depth: 58.5 cm
Height: 93.0 cm

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What Surface Area means ?

How to Get more Surface Area / Mass ???

What Surface Area means ?

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How can Surface Area be determined
???
Irving Langmuir presented the Langmuir model
for surface area to determine the monolayer
capacity of gas adsorbed on surface.
Brunaeur, Emmett, Teller improved the model
to includes multi layer adsorption before
monolayer is formed
BET becomes the more universally used model
for surface area determination

Langmuir Model
Aims to explain chemisorption giving rise to Type I
isotherm
All sites are energetically identical
Gas adsorbed to the surface 1 molecule layer only
Va bP

Vm 1 bP

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BET Surface Area Model

BET comes after Brunauer, Emmett and Teller


How BET can be used to determine Surface
Area ?

Where the word BET comes from ?

31
Random adsorption

The BET Equation

32
BET transformation

Determining the surface area from Nm


specific surface area Avogadros number
(m2/g) (molecules/mol)

S = nmAmN

area occupied by one


monolayer molecule (m2/molecule)
capacity (mol/g)

N Avagadros number 6.023 x 1023 molecules/mol

33
Properties of Adsorbates for
Physisorption Measurements

Adsorbate Boiling Point (K) Am (nm2/molecule)

N2 77.3 0.162
Ar 87.4 0.142
CO2 194.5 0.17
Kr 120.8 0.152

BET Transformation Plot

Isotherm Plot BET TransformationPlot

34
Important Factors when using BET model

visual check for linearity


X[(Po/P)-1]
1

negative intercepts are unacceptable

relative pressure, P/Po


Reference : S.Lowell, J.Shields , M. Thomas, M. Thommes

Important Factors when using BET model


Select points which is on the linear range for BET transformation plot.
Suitable data range 0.05 P/P0 0.30 P/P0 *
Try to use at least 5 data points
Should have good coefficient correlation > 0.99
Must have positive C value for model to be valid
*Note : For some microporous sample, need to use data range <0.15 P/P0

Reference : S.Lowell, J.Shields , M. Thomas, M. Thommes

35
Limitations of BET Surface Area Method

Optimize BET model for Microporous Material -


Rouquerol BET Plot
How to optimize BET plot for micropore material;
Plot n ads( P0-P) vs (P/P0 )
The n ads( P0-P) should continuously increase together with p/p;
if not, the pressure range should be narrowed

Reference : F. Rouquerol J.Rouquerol & K.Sing

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Capillary Condensation - Determination of
Mesoporosity

37
38
39
40
How the pore volume is being determined
Determination of total pore volume at this point all pores are filled with liquid.
The total amount of liquid condensed inside the pore is equivalent to the total pore volume

41
Desorption
Desorption is carried out by reducing the
pressure after reaching the atmospheric
pressure or the saturation pressure. The
desorption branch differs from the adsorption
branch due to the shape of the pores.
The shape of the hysteresis will depend on the
shape of the pores

42
43
44
Adsorptio, Condensation,Hysterisis
behaviour of a Fluid into a single Cylindrical
Mesopore

Hysteresis Classification - IUPAC

45
Hysteresis Loop Type H1
the adsorption and desorption branch almost vertical and
approximately parallel.
characteristic of porous materials consisting
of agglomerates or packing of uniform spheres and
tidy. ie materials that have a very narrow distribution of pore
size
also characteristic of materials
with pores of cylindrical geometry with a uniform pore size

Example: SB-15

Hysteresis Loop Type H2


Difficult to interpret
in general characteristic of materials that have pores like
bottleneck" or materials with interconnected network of
pores
also occurs in materials with non-uniform size and shape

Example : Inorganic Oxides

46
Hysteresis Loop Type H3
Characteristics of porous material consists of
aggregates of plate-like particles give rise to
slit-shaped pores

Example : Mesoporous
Activated Carbon

Hysteresis Loop Type H4


Characteristics of porous material in the form
of narrow slits
Uniform pore size distribution

Example : Microporous
Activated Carbon

47
What can be determined by adsorption
and/or by desorption ???

By adsorption, the cavity size


of a pore can be determined

By desorption, the neck size


of the pore can be determined

Lower Limit of Hysteresis Tensile


Strength Problem
For Mesopores desorption hysteresis - there is a lower limit ( 0.42 P/P0 for N2 )
Mechanical stability limit for capillary condensed liquid
spontaneous evaporation of pore liquids

Reference: S.J Gregg and K.S.W Sing (1982)

48
Low Pressure Hysteresis ?
Non Closure /Opened desorption observed in some samples
Chemisorption
Change in volume of the adsorbent
e.g swelling of the non-rigid pores

Reference: S.J Gregg and K.S.W Sing (1982)

Application
How the pore size in solids can affect ts
applications?

Lets see an example where million of dollars


can be involved. The pore size of a catalyst in
the oil industries

49
Example : Catalysts

Example : MCM41

50
Effect of impregnation

Change in the Adsorption Isotherm after


impregnation

51
Porosity models
Mesopore
BJH
Based on Kelvin equation & Thickness Curve
Valid from 2 to 300 nm.
Dollimore & Heal
Micropore
t-plot
MP Method
HK
Dubinin
Unified Theory for Mesopore & Micropore
DFT

52
N2 Adsorption Isotherms & Pore Volume Distributions Isotherm Linear Plot
Isotherm Linear Plot
12 mm Tube N1 Silica-Alumina ADS-DES with FS - Adsorption 12 mm Tube N1 Silica-Alumina ADS-DES with FS - Desorption
SBA-15 - Adsorption SBA-15 - Desorption
400
600

500

300
Q u a n ti t y A d s o r b e d ( c m /g S T P )

Q u a n ti ty A d s o r b e d ( c m /g S T P )
400

200
Alumina Silica SBA15
300

200
100

100

0
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Relative Pressure (P/Po) 0
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Relative Pressure (P/Po)
BJH Desorption dV/dlog(w) Pore Volume
Harkins and Jura : Faas Correction BJH Desorption dV/dlog(w) Pore Volume
Silica Alumina - M - Port 1 : 12 mm Tube N1 Silica-Alumina ADS-DES with FS
Harkins and Jura : Faas Correction
4 SBA-15

3
d V /d lo g ( w ) P o r e V o lu m e ( c m /g )

d V /d l o g ( w ) P o r e V o l u m e ( c m /g )
Alumina Silica
2
4
SBA15

1
2

0 0
1 5 10 50 100 500 1,000 1 5 10 50 100 500 1,000
Pore Width () Pore Width ()

N2 Adsorption Isotherms & Pore Volume Distributions


Isotherm Linear Plot
Isotherm ACS-5860 - Adsorption ACS-5860 - Desorption
1,000
Q u a n tity A d s o r b e d (c m /g S T P )

800
Q u a n ti ty A d s o r b e d ( c m / g S T P )

100 600

Y-Zeolite MOF
400

200

0
0.000 0.001 0.002 0.003 0.004 0.005 0.006 0.007 0.008 0.009 0.010
0
Relative Pressure (P/Po) 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Relative Pressure (P/Po)

Horvath-Kawazoe Differential Pore Volume Plot


dV/dlog(W) Pore Volume vs. Pore Width
Cylinder Pore Geometry (Saito-Foley)
HY Zeolite Tube Kr6 w/ FS @ end of analysis Port 1 dV/dlog(W) Pore Volume
0.15

4
d V /d l o g ( W ) P o r e V o l u m e ( c m /g )

0.10 3
S m o o t h e d d V / d w ( c m /g )

Y-Zeolite MOF
2

0.05

0.00
1 5 10 50 100 500 1,000 0
Pore Width () 1 5 10 50 100 500 1,000
Pore Width ()

53
Capillary Condensation in
Mesopores
Sorption behavior in mesopore ( 2 50nm )
Depend on fluid wall interaction
Attractive interaction between fluid-fluid molecules
Pore Condensation - Phenomena whereby gas condenses into liquid phase
in the pore at the pressure less than the Saturation pressure of bulk liquid

Mesopore Porosity Model Based on


Kelvin Equation
Thickness Equation

Kelvin Equation for Nitrogen


p 2VL 1 VL = 34.6810-6 m3/mol
ln
p 0
RT rm = 8.88 mN/m
1
Relative pressure p/p0

0.8

0.6

0.4

0.2

0
0.1 1 10 100 1000 10000
dm (nm)
micro meso macro
Catalysis and Catalysts - Physical Adsorption

54
BJH -Pore Size Determination

BJH -Pore Size Determination

55
BJH -Pore Size Determination

BJH -Pore Size Determination

56
Mesopore Porosity Model
BJH Model
Modified Kelvin Equation
Thickness Curve

Mesopore : BJH Model

57
Mesopore : BJH Model

Mesopore : BJH Model

58
Summary of Common Adsorptive Gas Table
Adsorptive Bath Sat. Microporosity Surface Area Mesoporosity Comments
Gas Pressure
Nitrogen Liquid ~760mmHg Yes Yes Yes Most
Nitrogen( 77K) commonly used

Argon Liquid ~193mmHg Yes Yes Not suitable Good for


Nitrogen( 77K) Micropore
analysis but
longer analysis
time
Argon Liquid ~760mmHg Yes Yes Yes Good for
Argon(87K) Micropore
analysis but
longer analysis
time

CO2 Ice bath ( OC) ~26142mmHg Yes No No Used for


micropore esp.
Carbon
-Faster analysis
results
-- Does not
required high
vacuum
Kripton Liquid ~2.4mmHg No Yes No Best for low
Nitrogen( 77K) surface

Summary of Models
Model Parameter Suggested Analysis Range Remark

Langmuir Surface Area 0.05 0.3 P/P0 Suitable for Monolayer capacity

BET Surface Area 0.05 0.3 P/P0 Most commonly used for
surface area

BJH Mesopore Pore Distribution >0.35P/P0, Pore Volume Valid for mesopore
@0.995P/P0

HK Micropore Pore Distribution Ultra low P/P0 Valid for micropore


region, up to 0.01P/P0

DA Micropore Pore Distribution, Micropore Volume Ultra low P/P0 Valid for micropore
region, up to 0.01P/P0

DR Micropore Surface Area, Monolayer Capacity Ultra low P/P0 Valid for micropore
region, up to 0.01P/P0

MP Method Average Pore Radius, Cum. Surface Area/Pore > 0.1 P/P0 Get micropore info without ultra
volume low dosing
T- Plot Micropore / External surface Area > 0.1 P/P0 Get micropore info without ultra
low dosing
DFT Pore Distribution / Surface energy All adsoption pts Valid for both
mesopore/micropore run

Slide 118

59
Summary Report

Reference
1. Gas Adsorption and Characterization of Powders and Porous Material,
J.Kenvin, Micromeritics Instrument Corporation
2. Internal Presentation Simon Yunes , Micromeritics Instrument Corporation
3. Analytical Methods in Fine Particle Technology , Paul A.Webb, Clyde Orr ( 1997)
4. Characterization of Porous Solids and Powders : Surface Area, Pore Size and Density
by S. Lowell, J.E Shields, M.A Thomas & Thommes (2004)
5. Adsorption, Surface Area and Porosity by S.J Gregg and K.S.W Sing (1982)
6. Adsorption by Powders and Porous Solids :
Principle, Methodology and Application, F. Rouquerol, J.Rougurol, K.S.W Sing(1999)

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