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Characterization of the porosity f

Submitted by : Imtisal-e-Noor
Sample: T 50

Question 1

Description of N2 Adsorption desorption experiment:

For the characterization of the porous material, N2 adsorption-desorption on


and porosity by using N2 adsorption-desorption equipment.In this process, n
between nitrogen and adsorbent) which adsorbes on the surface of the porou
between 0-100 k Pa for good results. Equipment basically uses the volumetric
of the porous material . And number of molecules gives us the specific surfac
required to stabilize the system before starting the experiment ,with the help
equipment there are two volume chambers seperated by a valve with volume
expansion of gas between two specific volumes.Glass tube is used for the me
of the volume chamber. This glass tube is closed with the help of crok to isola
constant temperature. The amount of gas adsorbed is determined by measur
automatically measures the change in pressure. After the introduction of N2 w
also be calculated. N2 is introduced step by step for further measurements. A
equilibrium pressure can be measured before and after dosing, density of fre
manifold has a lower pressure.The specific amount of gas confined can also b
Question 2- part 1

Specify the type of porous material:

According to IUPAC classification pores, it is IV b type sample. Sample given


the mesopores of the sample and there is a hystersis occurs in N2 adsorption
curvature upon emptying.
Relative pressures
0.009837994
0.030476486
0.062878068
0.077667817
0.100368317
0.120798387
0.140952501
0.161312431
0.181878688
0.202778849
0.247468769
0.303896847
0.358300895
0.400322097
0.450043075
0.499213042
0.548629635

Pressure (mm Hg)


7.39525
22.90975
47.26751
58.38624
75.45219
90.81154
105.96404
121.27168
136.73448
152.07315
186.04991
228.47688
269.38348
300.98138
338.37128
375.34747
412.53058

0.598659443
0.653148056
0.715626278
0.766208851
0.818239743
0.839010414
0.850718025
0.862803316
0.87549289
0.900013596
0.925358108
0.931431581
0.937621486
0.944051703
0.950137913
0.974453596
0.980339436
0.989936459
0.994806719

450.17917
491.18912
538.20325
576.26025
615.40857
631.04712
639.86969
648.97681
658.53894
677.001
696.08392
700.67108
705.34607
710.20209
714.79956
733.11188
737.55945
744.79944
748.52295

0.972437357
0.932412841
0.906753787

731.7157
701.61755
682.32776

0.900380914
0.876112446
0.851174413
0.826029647
0.80094614
0.751202447
0.700988286
0.650953737
0.600842414
0.551087526
0.502432613
0.455189571
0.419393687
0.4006340626
0.364062627
0.338707454
0.32186929
0.300782083

677.53375
659.26282
640.4903
621.56262
602.68146
565.24506
527.45691
489.80319
452.09253
414.65088
378.03665
342.45676
315.51321
301.39502
273.8775
254.7998
242.12964
226.26347

0.270864853
0.251271825
0.220816759
0.200879973
0.190980364

203.75711
189.01833
166.10861
151.11124
143.66429

0.186580498
0.166045649
0.143895228
0.127388973
0.123264121
0.100639351
Question 2- part 2

140.35451
124.90724
108.24467
95.8279
92.72499
75.70559

Calculate its specific surface area


BET equation:
(P/Ps)/(V*(1-(P/Ps)))=(C-1/Vm*C)(P/Ps)+(1/Vm*C)
Relative pressure range :0.05<P/Ps<0.35
from BET curve we get :
and we know:
and
where
and
so
then
and
as Vm = V monolayer
as

and V molar =
no. of moles =
Avagadro's Number=
no. of molecules=
Adsorption Cross section of nitrogen =

and

specific surface area=

Question 2- part 3&4 Calculate the Kelvin Radii:

we can use Kelvin equation for calulation of Kelvin Radii = rk=(-2Vcos)/(RT


where
Quantity
Molar volume of
condensate
Wetting angle on the
material
Surface tension of
condensate
Temperature
Saturation pressure
Ideal gas Constant

and

we can use Hasley Equation tocalculate the thickness


Points from curve
first intersection point
2nd intersection point
inflexion point

Conclusion :

If rk is samll we can not neglect thickness because th


Question 2- part -5

Calculate Pore Volume and Porosity

As my sample is amorphous silicon dioxide (assuming


that solid skeleton is made up of single oxide ) with a
density
Pore Volume
pore volume = Vads*(34.65/22400) cm3/g
as from the curve (Vads vs P/Ps) we can know that
at P/PS=1
pore volume
% Porosity
% Porosity = Vpores/(Vpores+(1/Density of solid))
% Porosity

erization of the porosity from Nitrogen Adsorption Measurements


EM3E

on experiment:

material, N2 adsorption-desorption on the porous material is a type of intrusive method which gives us Spec
desorption equipment.In this process, nitrogen gas behaves like an adsorbate( it is also an inert gas so there
ch adsorbes on the surface of the porous material.The specific temperature at which this determination is do
Equipment basically uses the volumetric method of adsorption in which equipment measures how many mole
f molecules gives us the specific surface area of the adsorbent by using Adsorption Cross section area of nitr
e starting the experiment ,with the help of pump and degassing for the sample prepration depends on the ex
mbers seperated by a valve with volumes V1 and V2 respectively and sample is placed and Basically pressur
c volumes.Glass tube is used for the measurement of sample volume ,which is in powdered form that helps t
e is closed with the help of crok to isolate the sample from atmosphere and it is at controllable temperature
gas adsorbed is determined by measuring Pressure of the gas at precise volume. And vaccum system is con
pressure. After the introduction of N2 we can measure the free volume is measured corresponding to the vo
ep by step for further measurements. After equilibrium is achieved, the valve is open therefore allowing the
d before and after dosing, density of free gas is determined at each step.In case of desorption, the reactor ha
ecific amount of gas confined can also be calculated with respect to the total amount of the gas that will be a

s, it is IV b type sample. Sample given is a mesoporous material associated with Network perculation. In this
e is a hystersis occurs in N2 adsorptionprocess in meso pores of sample because the curvature of meniscus

Volume absorbed (cm3/g)


49.1041
56.9116
63.0865
65.162
67.9549
70.1585
72.1796
74.0719
75.876
77.6219
81.3791
86.0452
90.7556
94.6843
99.8861
106.0834
114.1321

Elapsed time (mins)


1:31
2:09
2:17
2:24
2:29
2:34
2:38
2:43
2:48
2:52
2:57
3:03
3:09
3:15
3:21
3:29
3:36
3:48

124.9448
137.9267
145.6777
146.8485
147.3098
147.5057
147.5905
147.6905
147.7736
147.9638
148.1849
148.256
148.3221
148.3763
148.4324
148.7513
148.8674
149.1031
149.2552

3:58
4:09
4:17
4:21
4:25
4:29
4:33
4:37
4:41
4:45
4:49
4:53
4:57
5:01
5:05
5:09
5:13
5:17
5:29

148.7586
148.2248
147.949

5:34
5:38
5:42
5:44
5:48
5:53
5:57
6:01
6:05
6:09
6:12
6:16
6:20
6:24
6:29
7:05
7:20
7:27
7:33
7:38
7:43
7:48
7:50
7:56
8:00
8:05
8:10
8:14

147.8577
147.6425
147.4254
147.2327
147.0136
146.6149
146.1852
145.6975
145.1538
144.5168
143.3646
114.1183
97.6958
94.8495
90.9849
88.7251
87.2663
85.4767
82.9726
81.3469
78.8364
77.1267
76.24

75.8497
74.0485
72.0133
70.4
69.9809
67.5547

8:17
8:22
8:27
8:32
8:35
8:40

/Ps)))=(C-1/Vm*C)(P/Ps)+(1/Vm*C)
ure range :0.05<P/Ps<0.35
y=0.016x-5*10^-5
y=(P/Ps)/(V*(1-(P/Ps)))
x=P/Ps
a=C-1/Vm*C

0.016

b=1/Vm*C

0.00005

Vm*C

20000

C
Vm

321
62.3052959502
22400
0.0027814864
6.02E+23
1675050425567420000000
1.62E-19

Vm/V molar=
Na=
no. of moles*Na=
oss section of nitrogen =
no. of molecules* adsorption
cross section of the N2

271.3581689419

ion of Kelvin Radii = rk=(-2Vcos)/(RTln(P/Ps)


Symbol

Numerical Value

34.65

T
Ps
R

8.85E-05
7.74E+01
7.60E+02
8.31E+00

asley Equation tocalculate the thickness= t= 0.343(-5/ln(P/Ps))^(1/3)


P/Ps

rk(m)
0.4006
0.7009
0.5257

0.000000001
2.68161988601425E-009
1.48209117163498E-009

e can not neglect thickness because thickness is considerable in calculation of rp.

is amorphous silicon dioxide (assuming


eton is made up of single oxide ) with a

= Vads*(34.65/22400) cm3/g
rve (Vads vs P/Ps) we can know that
Vads
Vpore

2.2

149.5
0.2312578125

Vpores/(Vpores+(1/Density of solid))
33.7207219056

dsorption Measurements

e of intrusive method which gives us Specific Surface area, Pore size, pore volume
n adsorbate( it is also an inert gas so there will be no chemical reaction occurs
perature at which this determination is done, is 77 K and the pressure should be in
which equipment measures how many molecules of nitrogen are adsorbed in pores
using Adsorption Cross section area of nitrogen gas. In this equipment, vaccum is
r the sample prepration depends on the extent upto which vaccumis created. In this
nd sample is placed and Basically pressure is measured before and after the
me ,which is in powdered form that helps to reduce the free volume is placed in one
phere and it is at controllable temperature while the rest of the equipment is at
precise volume. And vaccum system is connected with computer so that it can
lume is measured corresponding to the volume of the bath .Number of moles can
d, the valve is open therefore allowing the gas to be exposed to the sample. The
h step.In case of desorption, the reactor has high pressure while the staying
o the total amount of the gas that will be available for adsorbtion.

ssociated with Network perculation. In this case cappilary condensation occurs in


ample because the curvature of meniscus filling the pores is diiferent than the

Saturation Pressure (mm Hg)

y=(P/Ps)/(V*(1-(P/Ps)))
751.62585
0.0002023404
0.000552339
0.0010635714
0.0012922881
0.0016417655
0.0019583593
0.0022732183
0.0025966544
0.0029299464
0.0032768727
0.0040409454
0.0050737136
0.0061523782
0.0070503965
0.0081925736
0.009396919
0.0106497255

Volume Adsorbed

0.0119384681
0.0136527193
0.0172744306
0.0223177077
0.0305597644
0.0353313934
0.0386117832
0.0425809778
0.0475840735
0.0608348784
0.0836610371
0.0916251175
0.1013413442
0.1137219692
0.1283770779
0.2564310536
0.3349507061
0.659735458
1.2834159046
0.2371694202
0.0930728862
0.0657273528
752.505
0.0611279429
0.0478983751
0.0387943644
0.0322489897
0.0273700252
0.0205936241
0.0160368531
0.0128001492
0.0103702156
0.0084945538
0.0070434265
0.0073213572
0.0073937411
0.0070472677
0.0062920538
0.005772775
0.0054390064
0.0050325914
752.2464
0.0044772353
0.0041255192
0.0035947248
0.0032592665
0.0030963266

(P/Ps)/(V*(1-P/Ps))

0.0030241115
0.0026888647
0.0023340318
0.0020736644
0.0020090391
0.0016564502

cm3/g
cm3/g (STP)
dimension less
no. of molecules / mole
moleclues / g
m2
m2/g (STP)

Units
cm3/mol
degree
N/cm
K
mm Hg
J/mol.K

t(thickness)(m)

alculation of rp.

g/cm3

cm3/g(STP)
cm3/g(STP)

rp=rk+t (m)
6.038524171709E-010
1.64564245286595E-009
8.27306194557472E-010
3.50892608057172E-009
6.79065006762076E-010
2.16115617839706E-009

Adsorption-Desorption Isotherm
160
140
120
100
Volume Adsorbed

ads

80

des

60
40
20
0
0

0.1

0.2

0.3

0.4

0.5

0.6

Relative Pressure (P/Ps)

0.7

0.8

0.9

20
0
0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

Relative Pressure (P/Ps)

BET isotherm
0.0045
0.004

f(x) = 0.0159605173x + 4.53052493560063E-005

0.0035
0.003
0.0025
(P/Ps)/(V*(1-P/Ps))

BET

0.002

Linear (BET)

0.0015
0.001
0.0005
0
0

0.05

0.1

0.15

0.2

Relative pressure (P/Ps)

0.25

0.3

ads
des

0.9

0.9

0.3

BET
Linear (BET)

x
0.0599
0.0781
0.086
0.1006
0.1116
0.1208
0.1364
0.14007
0.16117
0.1873
0.2013
0.2128
0.2373
0.2521
0.2632
0.2873
0.3026
0.3139
0.3378

y
0.000613
0.000774
0.000842
0.000968
0.001063
0.001143
0.00127
0.00131
0.001495
0.00173
0.001858
0.001965
0.002198
0.002343
0.002454
0.002702
0.002864
0.002987
0.003255

BET graph
0.0035
0.003

f(x) = 0.0093734345x + 0.00000958

0.0025
0.002
0.0015
0.001
0.0005
0
0

0.05

0.1

0.15

0.2

0.25

0.3

0.

BET graph

093734345x + 0.00000958

.15

BET graph
Linear (BET graph)

0.2

0.25

0.3

0.35

0.4

0.062878
0.077668
0.100368
0.120798
0.140953
0.161312
0.181879
0.202779
0.247469

0.001064
0.001292
0.001642
0.001958
0.002273
0.002597
0.00293
0.003277
0.004041

BET
0.0045
0.004
0.0035

f(x) = 0.0160403178x + 3.1522684560197

0.003
0.0025
0.002
0.0015
0.001
0.0005
0
0.05

0.1

0.15

0.2

BET

03178x + 3.15226845601979E-005
BET
Linear (BET)

0.15

0.2

0.25

0.3

0.303897 0.005074