Dr. S.S.

BHATNAGAR UNIVERSITY INSTITUTE OF CHEMICAL ENGINEERING AND TECHNOLOGY,

P.U., CHANDIGARH

Title: Andreasen Pipette.

Objective:

 To determine particle size distribution by gravitational settling method using

Andreasen Pipette

Theory:

Andreasen pipette is the most widely used method for sampling from sedimenting
liquids. It is a homogeneous incremental method, since it starts with a uniform
suspension, and analyses the concentration of material at a fixed depth (near the
bottom). An analysis of this kind expresses quantitatively the proportions by weight
of the various sizes of particles present in the slurry.
The Andreasen pipette method of determining grain sizes by sedimentation is a
refinement of the ordinary pipette method. It permits precise results but requires more
time and precision than some other methods because this method is fully based on
gravitational settling of particles in liquid and the effective hydrodynamic radius is
determined

The Andreasen method assumes that particles will sediment at a rate dependent on
their size and further assumes the validity of Stoke´s Law in this respect.
The size distribution of particles characterized by small dimensions is usually given
in terms of the Stokes diameter (dst), i.e., the diameter of the sphere that falls with the
same terminal velocity as the particle in the same fluid and at the same temperature.
In the Andreasen Pipette a sample of the material is dispersed in a liquid and allowed
to settle from time zero. At intervals a sample of fluid is pipetted from a depth h
below the surface. These samples are evaporated to dryness and weighed to give
concentrations. This produces a set of concentrations C(t) and the known initial
concentration C0. At any time t the sample withdrawn will contain particles with
terminal velocities equal to or less than h/t, at their original concentration, larger
particles will have settled below the level of the pipette tip. We therefore have:

B.E. CHEMICAL IInd Year AVIRAL SELI CH12111

Dr. S.S.BHATNAGAR UNIVERSITY INSTITUTE OF CHEMICAL ENGINEERING AND TECHNOLOGY,
P.U., CHANDIGARH

18µu
dst = √(ρ
s −ρ)g
Where,
dst = Stoke’s diameter µ = viscosity of water
u = settling velocity ρ = density of water
𝜌𝑠 = density of the solid

Description Of The Setup:

The apparatus consists of a glass vessel holding about 550 ml of suspension, into
which a 10 ml calibrated pipette dips, the tip being about 4cm from the bottom of the
vessel. A 3-way tap is provided to allow a sample of the liquid to be withdrawn via
the pipette at intervals. The slurry made was of Calcium Carbonate (3%).
Thermometer was used to note down the temperature of water. Setup also consisted
of empty beakers to hold on to the dry residue, an oven and a stopwatch.

Schematic Diagram:

B.E. CHEMICAL IInd Year AVIRAL SELI CH12111

Dr. S.S.BHATNAGAR UNIVERSITY INSTITUTE OF CHEMICAL ENGINEERING AND TECHNOLOGY,
P.U., CHANDIGARH

Procedure:

 The temperature of water is noted down.

 Take 10 empty beakers, wash them, dry them thoroughly and weigh the empty
beakers.
 Slurry of Calcium Carbonate (3%) is made in water. 16.2 g in 540 ml of water.
 The Andreasen pipette is filled with the slurry.
 The container is then agitated by inversion (not by stirring, since this causes
persistent vortices).
 The timer is started when the agitation is complete.
 The samples are sucked at time intervals of 1, 2, 3, 5, 7, 9, 12, 15, 18 and 22 min.
 In order to weigh sample the three way tap is turned so that sample is emptied into
a pre-weighed beaker.
 Now, the beakers are kept in an oven for all the water to evaporate and the residue
to be left.
 The beakers with dry residue are finally weighed.

Recordings:

Temperature of water = 20oC

Density of water = 998.23 kg/m3
Density of Calcium Carbonate = 2711 kg/m3
Viscosity of water = 0.000102 kg/m s
Slurry of CaCO3 in water = 3% = 30g in 1000 ml

B.E. CHEMICAL IInd Year AVIRAL SELI CH12111

Dr. S.S.BHATNAGAR UNIVERSITY INSTITUTE OF CHEMICAL ENGINEERING AND TECHNOLOGY,
P.U., CHANDIGARH

Observations:

S.no Empty Empty beaker Residue(g) Time(min) Height (cm)

beaker(g) +residue(g)
1 27.72 27.81 0.09 1 19.8

2 29.71 29.78 0.07 2 19.4

3 31.78 31.84 0.06 3 19

4 29.58 29.63 0.05 5 18.6

5 27.49 27.51 0.02 7 18.2

6 30 30.01 0.01 9 17.8

7 31.74 31.74 0 12 17.4

8 29.97 29.97 0 15 17

9 27.97 27.97 0 18 16.6

10 30.38 30.38 0 22 16.2

Sample Calculations:

For reading 2

Time = 120 seconds

Ht. travelled by particles = 0.194 m

H
Settling velocity, u =
t
= 0.00161667 m/s

Ws (in 10 ml) = 0.07 g

Ws (in 540 ml) = 3.78 g

B.E. CHEMICAL IInd Year AVIRAL SELI CH12111

Dr. S.S.BHATNAGAR UNIVERSITY INSTITUTE OF CHEMICAL ENGINEERING AND TECHNOLOGY,
P.U., CHANDIGARH

Ws
Wf =
Wt

3.78
= = 0.23333
16.2

18µu
dst = √
(ρ s −ρ)g

= 13.2911498 microns

Calculations:

Time,t(s) Height,H(m) Velocity,v(m/s) Diameter, Wt. residue(in Wt. residue(in Wt. fraction
10 ml)(gm)
ds(μm) 540ml),Wi(gm)

60 0.198 0.0033 18.98931422 0.09 4.86 0.3

120 0.194 0.001616667 13.29115117 0.07 3.78 0.233333333

180 0.9 0.00105 10.71141783 0.06 3.24 0.2

300 0.186 0.000616667 8.20876202 0.05 2.7 0.166666667

420 0.182 0.000428571 6.843270408 0.02 1.08 0.066666667

540 0.178 0.000325926 5.967766392 0.01 0.54 0.033333333

720 0.174 0.000238889 5.109170398 0 0 0

900 0.17 0.000186667 4.516334341 0 0 0

1080 0.166 0.000150926 4.061012647 0 0 0

1320 0.162 0.000120455 3.627978686 0 0 0

B.E. CHEMICAL IInd Year AVIRAL SELI CH12111

Dr. S.S.BHATNAGAR UNIVERSITY INSTITUTE OF CHEMICAL ENGINEERING AND TECHNOLOGY,
P.U., CHANDIGARH

Graph:

 Weight fraction vs. Stoke’s diameter

Wt. fraction vs. Stoke's Diameter

0.33

0.28

0.23
Wt. fraction

0.18

0.13

0.08

0.03

-0.02 0 2 4 6 8 10 12 14 16 18 20

Stoke's Diameter (μm)

B.E. CHEMICAL IInd Year AVIRAL SELI CH12111

Dr. S.S.BHATNAGAR UNIVERSITY INSTITUTE OF CHEMICAL ENGINEERING AND TECHNOLOGY,
P.U., CHANDIGARH

Discussion of Results:

The graph between dst (microns) and Wf is very close to the one predicted. But Wf
(total) is coming equal to 1 which may be due to some error while noting in the
weights of the beakers or some other experimental error that occurred while
performing the experiment.

Source Of Error:

 Least count of the scale was only upto two decimal places.
 Beakers not properly cooled before weighing.
 Poor dispersion.
 Poor initial sampling.

B.E. CHEMICAL IInd Year AVIRAL SELI CH12111