CH 3510: Mechanical Operations Lab

Experiment: Determination of specific

surface area of non porous materials

B Narasimhan: CH11B043
Naveenraaj K.P: CH11B044
Raghuveer P: CH11B045

AIM:
To determine the specific surface area of non - porous material using Blaines Apparatus.

APPARATUS:
Blaines apparatus A U-tube manometer with glycerin, vacuum pump, filter paper, specific
gravity bottle, measuring cylinder, stop-watch, given non porous material (Calcium carbonate
and Titanium Oxide), Vernier callipers

THEORY
The components of Blaines Apparatus are: a U-tube manometer, permeability cell, a plunger,
perforated disc, plunger rubber stopper, rubber tube 30cm long, packet of 12 filter paper disc
incorporated. The rubber tube of the Blaines apparatus is connected to a vacuum pump.
This apparatus is used specifically for finding the air permeability specific surface of non
porous materials as a measure of their fineness (usually cement)

Fig 1: Blaines Apparatus

Source:
http://zealinternational.com/cement/zi1002.asp

To find the specific surface of the given material, we first need the pressure drop across the
packed bed. The pressure drop can be obtained using the Kozeny Carman equation.

=

Here is the pressure drop, is the total height of the bed, is the superficial or "emptytower" velocity, is the viscosity of the fluid, is the porosity of the bed, is the sphericity of
the particles in the packed bed, and is the diameter of the related spherical particle. This
equation holds for flow through packed beds with particle Reynolds numbers up to
approximately 1.0

The modified form of this equation to find specific surface from the apparatus is:

S =Specific surface area

k = Equipment constant = 839.2 kg2/s2m5
t= true density of material
t = time taken
hb= bed height
= porosity of the bed
Porosity of the bed is found out by the following formula:
= (

= porosity of the bed

m = mass of the material
dh = inner diameter
hb = bed height
t = true density of material

To find the porosity of the bed, we need to calculate the true density and the bulk density.

Bulk density calculation

Weight of the empty measuring cylinder.

wo

Weight of the measuring cylinder with the given material up to v

wp

Bulk Density,

= ( )/

True Density calculation

Weight of empty specific gravity bottle:

w0

Weight of bottle + material:

w1

Weight of the bottle + material + liquid:

w2

Weight of bottle + liquid:

w3

True Density,

EXPERIMENTAL PROCEDURE

1. The bulk density of the given material is found by finding the values of wo, wp and
substituting them in the above equation
2.

The true density of the material is estimated by finding w0, w1, w2 and w3 and using the
equation for true density

3. The dimensions (inner diameter and height) of the powder holder are found using Vernier
calipers
4. Using the bulk density known, a weight of the material that will fill 25 % of the holder (upto
one fourth of its height) is taken and put in the powder holder, the bottom of which contains
a filter
5. The holder is placed above the U-tube manometer of the Blaines apparatus and the plunger
over the packed bed.
6. The vacuum pump is used to create vacuum on one side of the manometer.
7. Once vacuum is created the pump is switched off and the plunger is removed.

8. The time of descent of the glycerine between two levels (say x 1 and x2) is measured using a
stop-watch. This becomes t for the modified Kozeny Carman equation
9. This procedure is repeated with material filling 50 % and 75 % of the holder
DATA, OBSERVATIONS AND CALCULATIONS

Bulk Density Calculations

1. CaCO3
wo = 27.28 g

wp = 29.36 g

v = 4 cc

b = 2.08/4 = 0.52 g/cc

2. TiO2
wo = 27.25 g

wp = 29.89 g

v = 4 cc

b = 2.64/4 = 0.66 g/cc

True Density Calculations

1. CaCO3
w0 = 9.68 g

w1 = 9.88 g

w2 = 15.11 g

w3 = 14.99 g

w2 = 14.97 g

w3 = 14.79 g

t = 0.2/(5.31 5.23) = 2.5 g/cc

2. TiO2
w0 = 9.68 g

w1 = 9.91 g

t = 0.23/(5.11 5.06) = 4.6 g/cc

Dimensions of powder holder

Inner Diameter: 11.9 mm
Height: 4.78 cm
25 % ht: 1.195 cm ~ 1.2 cm

Weights corresponding 25 %, 50 % and 75 % of holder height:

CaCO3 : 0.82 g, 1.64 g and 2.46 g respectively

TiO2 : 1.04 g, 2.08 g and 3.12 g respectively

Table 1: Time taken for glycerine to drop to marked levels (t)

a. For CaCO3

Time Taken (sec)

% Filled

25% (h = 1.2 cm)

50% (h = 2.4cm)

75% (h = 3.6cm)

Trial 1

10.66

22.16

37.50

Trial 2

9.91

21.93

37.06

Trial 3

10.43

21.22

37.09

Average

10.33

21.77

37.22

Porosity

0.7542

0.7542

0.7542

Specific Surface

2624.42

2693.99

2886.93

(cm2/g)
Average Specific Surface = 2735.11 cm2/g

b. For TiO2

Time Taken (sec)

% Filled

25% (h = 1.2 cm)

50% (h = 2.4cm)

75% (h = 3.6cm)

Trial 1

8.87

17.5

32.1

Trial 2

9.10

17.09

31.87

Trial 3

17.01

31.94

Average

8.99

17.05

31.91

Porosity

0.8306

0.8306

0.8306

Specific Surface

2231.37

2172.89

2427.13

(cm2/g)
Average Specific Surface = 2277.13 cm2/g

RESULT:
The specific surface areas of the given powders (CaCO3) and (TiO2) came to be 2735.11 cm2/g
and 2277.13 cm2/g respectively. While the specific surface obtained for Calcium Carbonate is in
the range reported by literature (about 2000 3000 cm2/g), the value for Titanium dioxide is
much lower than reported in literature. The reported value is of the order of 101 to 102 m2/g while
the experimentally determined ones are off by an order of 10 to the lower limit.
SOURCES OF ERROR AND PRECAUTIONS

Care must be taken to prevent the packed bed from falling into the apparatus

Parallax error while noting the movement of glycerine in the manometer must be avoided

Stop-watch measurements must be accurate