1

Experiment No.- 1

BLAINE APPARATUS

Aim:
To determine porosity and specific surface area for a given powder.

Introduction:
There are several operations in Chemical Engineering which deal with bed of non-
porous particles. Determination of specific surface of a non-porous powder is a
commonly accepted method for finding particle size of that powder. There are several
ways of doing this, an air permeability method (Blain’s method) is one those.

For example, the fineness of cement is measured as specific surface. Specific surface
is expressed as the total surface area in square meters of all the cement particles in one
kilogram of cement. The higher the specific surface is, the finer cement will be.

Theory:
Surface area per unit mass is an important parameter used to characterize particles and
this characterization is important in several areas of chemical engineering. In this
experiment, we will measure the surface area of particles using a simple Blaine’s
apparatus which uses the dependence of pressure drop across a packed bed on the
effective size of the particle.

For a single phase flowing through a packed bed, the pressure drop across the packed
bed is given by Ergun’s equation:

p 1.75U o 2 (1 −  ) 150 U o (1 −  ) 2
= +
L d P 3 d P 2 3

Where
∆p is the pressure drop across the bed,
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L is the length of the bed (not the column),

dP is the equivalent spherical diameter of the packing,
ρ is the density of fluid,
μ is the dynamic viscosity of the fluid,
Uo is the superficial velocity
Ԑ is the void fraction (porosity) of the bed.

Reynolds number for porous medium is given by

U o Dp
Re PM =
 (1 −  )
Kozeny-Carman equation describes the laminar flow. It is valid for low Reynold’s
number which is given by:

p 150U o (1 −  ) 2 L
=
 d P 2 3 
Using Ergun’s equation pressure drop across a packed bed is related to the effective
diameter of the particle and porosity of the bed. The effective diameter of the particle
can be related to the surface area per unit volume using the following relationship –

6
Sv =
dP

Substituting the above equation in Ergun’s equation at low Reynolds number we get,

p 4.17 Sv 2  (1 −  ) 2 U 0
=
L 3
1/2
 p 3 
Sv =  
 4.17 L (1 −  ) U 0 
2

The surface area per unit volume measured in the above relation is related to the
surface area of the particle per unit mass via the true density of the particle phase -
Sv
.
P
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In the experiment, we will make direct observations for the pressure drop across a
packed bed along with the velocity of the fluid in the Blaine’s apparatus. Porosity will be
related to the bulk density and true density of the particulate phase in the packed bed
which will be calculated separately. The other constants like length of the bed and
viscosity of the fluid are already known.

Experimental Setup:

The apparatus consists of a U-tube with an opening connected to a Vacuum Pump, a

Powder Holder attached to one end and a Plunger to be placed on top of the powder
holder as shown in figure below. The vacuum pump is used to create a pressure
differential between the two arms of the manometer, which then drives the air to flow
through the powder held in the powder holder. This in turn reduces the level in the
manometer arm corresponding to that end.

Fig 1. Blaine’s Apparatus

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The pressure difference across the powder holder is calculated by measuring the levels
in the manometer arms and the rate of air flow is calculated by measuring the rate of
change of the water level in the same. With these measurements, the specific surface
area of the powder can then be found by using the Ergun equation.

Requirements:
Specific gravity bottle, measuring cylinder (10 ml), CaCO3 powder, vernier caliper, filter
paper.

Experimental Procedure:
Estimation of True Density of powder
Measure the following
1. Weight of empty specific gravity bottle W0
2. Weight of bottle + powder W1
3. Add carefully liquid such that there is no air bubble
4. Weight of bottle+ Powder & liquid W2
5. Clean the bottle thoroughly
6. Weight of bottle + liquid W3
7. Calculate true density of the Powder by the given equation.
(𝑊 −𝑊 )
𝜌𝑡𝑠 = (𝑊 −𝑊 1)−(𝑊0 −𝑊 ) × 𝜌𝑙𝑖𝑞 ...… (1)
3 1 2 1

Estimation of Bulk density of powder

1. Find the empty weight of 10 ml measuring jar Wo
2. Fill the jar with some powder (half level) and tap the jar up to 7 times.
3. Note down the volume occupied by the powder V
4. Find the weight of the jar + powder Wp
5. The bulk density of the Powder is given by weight/volume of the powder-

bs =
(W p – Wo )
V
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Estimation of Porosity and Specific Surface Area

1. Measure diameter, (dh) and depth of the powder holder, (Lh).
2. Measure the plunger length, (Lp).
3. Cut a filter paper equivalent to plunger diameter.
4. Slowly put the punched disc and the filter paper into the powder holder and observe
that they are placed horizontally one above the other.
5. Weigh the powder holder along with the plunger, filter paper and punched disc, W0.
6. Calculate approximately the quantity of powder required, given the bulk density of the
powder from Eq. 2.


Ws = (d h )2 [ Lh − Lp ]bs (2)
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7. Weigh Ws gm of solid in the balance and slowly fill up the powder holder. It is filled
slowly by pushing the plunger each time a small quantity is added into the powder
holder.
8. Check if the plunger goes completely. Then add little powder so that the plunger is a
little above approximately less than 1mm.
9. Use the gap gauge to measure the gap Lg made by the plunger.
10. Find the weight of the holder along with plunger after filling powder to it, Wt.
11. Keep the holder over the Permeameter tube having rubber cork.
12. Observe that there is no air leakage between the solid holder and the cork.
13. Switch on the Vacuum Pump and operate the glass cork to pull up the liquid.
14. Ensure that the liquid does not cross the top marking.
15. Close the glass cork and remove the plunger from the powder holder. The liquid will
start falling.
16. Note the time taken, t for the liquid level to move from X1 to X2 marking from the top.
17. Remove the solid and clean the Permeameter.
(Wt − W0 )
18. Calculate porosity given by equation  = 1− (3)
( ) ts d h 2 ( Lh − Lp + Lg )
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19. From calculated ‘  ’ & time measured ‘t’, calculate specific surface area.
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0.5
 t 3 
S=K 2 
 ts ( Lh − Lp + Lg ) (1 −  ) 
2 (4)

System parameter, K = 3.4906x105 cm-1/2 sec-1/2

Precautions:
1) Don’t push the plunger into the powder holder very hard otherwise it can tear the
filter paper and powder will start to pass through the holder.

2) Do not let the liquid rise above the permissible height.

3) Make sure that the rubber cork is fitted tightly on the glass tube.

Observations:
Sample- CaCO3 powder
Liquid – Water (density= 1 gm/cc)
1 ) Determination of true density:
Wt. of empty Wt. of bottle Wt. of bottle + Wt. of bottle True density
Sp.Gravity +powder powder+liquid +liquid
(W1 − W0 )
bottle (W gm) (W 2 gm) (W3 gm) ts =  liq
1
(W3 − W0 ) − (W2 − W0 )
(W0 gm)

2 ) Determination of bulk density:

Wt. of 10 ml Wt. of 10 ml measuring jar Volume occupied by Bulk density

(W – Wo )
measuring jar + powder powder after tapping (V)
bs =
p

(Wo gm) (Wp gm) V

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Blaine’s Apparatus
Diameter of the powder holder, (dh) = mm = cm
Depth of the powder holder, (Lh) = cm
Length of the plunger, (Lp) = cm
Weight the powder holder + plunger + filter paper + punched disc, W0 = gm


Quantity of powder needed ( approx.) , Ws = (d h )2 [ Lh − Lp ]bs = gm
4
Gap made by the plunger, Lg = mm = cm
Weight of the holder along with plunger after filling powder to it, Wt = gm

Observation Table:
Time taken, t for the liquid level to move from X1 to X2:
Obs. Time (s) Avg. time (s) (X1 –X2) cm
1
2
3

Results:
Report the bulk density, true density, porosity and the specific surface area for the given
powder. Report the specific surface area in m2/gm (1 m2/gm= 104 cm2/gm).

Sources of errors:

Report the possible sources of error found in the experiment and the observations. Discuss
exactly how these affect the experimental data (i.e. will the readings be larger or will be they be
smaller due to the presence of a particular source).
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Discussion:
The following topics need to be discussed in detail in the report.
1. What is the conclusion of the experiment? Is the objective fulfilled?
2. Give a physical interpretation of your results.
3. Provide any additional suitable inference.

References:
1. V.N.P. le, E.Robins, M.P. Flament, Air Permeability of Powder: A potential tool
for dry powder inhaler formulation development, European Journal of
Pharmaceutics and Biopharmaceutics 76 (2010) 464-469
2. 2. B. Kaye, Permeability technique for characterizing fine powders, Powder
Technology 1 (1) (1967) 11-22