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ChE 323L - Physical Chemistry Laboratory 1 Manual

Viscosity Measurement by Falling Sphere Method

Viscosity Measurement of Liquids and Solutions By Falling Sphere Method


Measurement of viscosity is one of the ways to investigate the rates with which reactants can come together in
solution. One application in which viscosity measurement is employed is catalysis by enzymes. In this case, the
viscosity of the medium is being monitored and is related to the changes in composition and/or concentration of
the components in the medium. In many cases, viscosity is an important parameter in fluid dynamics. The viscosity
of a liquid may be measured by a number of methods, including the determination of the rate of flow through a
capillary, the rate of settling of a sphere in a liquid, and the force required to turn one of two concentric cylinders at
a certain angular velocity. In this experiment, the viscosity of a certain liquid is measured using the falling sphere
method. The effect of temperature on viscosity is also studied.

1. Introduction
Viscosity is a measure of the resistance that a fluid offers to an applied shearing force. Consider
two parallel planes in which one is moving while the other is stationary (Figure 1). When the top plane
moves to the y-direction at a constant speed relative to the bottom plane while maintaining a constant
distance, the layer of the fluid immediately adjacent to the moving plane moves with the velocity of this
plane. The layer next to the stationary plane is also stationary, however, the velocity of the in-between
planes changes linearly with distance. The viscosity, , is defined by the hypothetical equation

where,

d y
dz

Equation 1

F = force per unit area required to move one plane relative to the other
dvy/dz = velocity gradient (i.e., the rate of change of velocity with respect to distance
measured perpendicular to the direction of flow) and is negative since the velocity
decreases in successive layers away from the moving plane

Fluids whose behavior is described by the equation above are called Newtonian fluids. These
fluids follow Newtons law of viscous flow. However there are fluids that deviate from this behavior.
They are the non-Newtonian fluids. There are certain factors that govern a fluids resistance to flow.
Momentum transfer governs the viscosity of gases while intermolecular forces dictate the viscosity of
liquids.
Liquids with greater IMF have higher viscosity. It is also true that an increase in molecular
complexity would likely lead to an increase in viscosity. The factors, which affect the viscosity of liquids,
are temperature and pressure. In this experiment, viscosity measurements are done at atmospheric
pressure but the temperature is varied.
_____________________________________________________ Department of Chemical Engineering
University of San Carlos

ChE 323L - Physical Chemistry Laboratory 1 Manual


Viscosity Measurement by Falling Sphere Method

Although the viscosity is easily defined in terms of the hypothetical equation above,
experimental techniques are available for practical applications. These techniques involve measurement
of viscosity by determining the rate of flow through a tube, the torque on a disk that is rotated in a fluid,
or other experimental methods. In this experiment, the viscosity of a certain liquid at different
temperatures is determined by measuring the rate of settling of a sphere of known density in that liquid.
The force causing the sphere to settle in the fluid is equal to its effective mass of the sphere times the
acceleration due to gravity. The effective mass is the mass of the sphere minus the mass of the fluid it
displaces. When the rate of settling of the sphere in the liquid is constant, the retarding force is equal to
the force due to gravity and the equation is known as the Stokes Law equation (Equations 2 and 3). This
method is highly valuable for solutions of high viscosity.

Moving plane

vy

Stationary plane
Figure 1. Velocity gradient in a fluid due to a shearing action

4 3
dx
r 0 g 6r
3
dt

Equation 2

dx 2r 2 0 g

dt
9

Equation 3

where, = density of the sphere [kg/m3]


0 = density of the medium [kg/m3]
r = radius of the sphere [m]
= viscosity of the liquid [Pa.s]
x = distance traveled by the ball [m]
t = time of travel [s]
g = gravitational constant [m.s-2]

_____________________________________________________ Department of Chemical Engineering


University of San Carlos

ChE 323L - Physical Chemistry Laboratory 1 Manual


Viscosity Measurement by Falling Sphere Method

2. Experimental Design
General procedure
Prepare a water bath that is maintained at 40oC. (NOTE: Use distilled water in the preparation of
the water bath to prevent formation of scales.) Meanwhile familiarize the parts of the falling ball
viscometer and practice with the ball release mechanism. Make sure that the viscometer tube is clean
and dry. Fill the viscometer tube with the liquid whose viscosity is to be determined. Assemble the
falling ball viscometer setup (Figure 2). Fully immerse the glass tube with the liquid in the water bath.
Only the lower part of the plastic screw cap should be touched by the clamp. Wait for a few minutes for
the liquid sample to achieve the same temperature as the water bath. Measure the time of settling of
the sphere. Measure the density of the sample at the said temperature. Calculate the viscosity of the
liquid. Clean and dry the viscometer and ball for next use. Perform another run at 30oC. For each
temperature setting a duplicate run should be made.

Falling ball type


viscometer

Water bath

HEATER/ STIRRER
Timer

Figure 2. Setup for viscosity measurement by falling ball method

Density Measurement Using the Liquid Densitometer


The density of liquid samples can be determined using a densitometer (Kern Instruments). To
determine the density of liquids using the densitometer, first, place the small-diameter beaker (55 mm)
on the metal platform. Then, attach the thermometer to the rim of the beaker using the retainer clip.
Carefully suspend the disk with the glass plummet, which hangs on one wire, from the frame. Tare the
_____________________________________________________ Department of Chemical Engineering
University of San Carlos

ChE 323L - Physical Chemistry Laboratory 1 Manual


Viscosity Measurement by Falling Sphere Method

balance. Fill the beaker with the liquid sample so that the liquid is 10 mm above the glass plummet.
Record the buoyancy displayed with a negative sign. The negative weight displayed by the balance
corresponds to the buoyancy acting on the glass plummet in the liquid. Read off the temperature and
record it.
The glass plummet has as a volume of 10 cm3. To determine the density of the liquid, mentally
shift the decimal point of the current density display one place to the left.
The Falling Ball Type Viscometer
The viscometer is manufactured by Gilmont Instruments (a division of Barnant Company,
Barrington, IL, USA). The tube (10 inches long and 1 inch in diameter) is made of high precision bore
glass tubing with stabilizing beads (Figure 3). There are three different tube sizes, each one covering a
different range of viscosity. Two high precision balls, one of glass and one of stainless steel, are supplied
with each instrument to extend the range. The ball is observed with red lines, called fiduciary lines,
permanently fused into the glass.

Cap with
rubber cork

Figure 3. Gilmont Instruments falling ball type viscometer


[Gilmont Instruments, Barnant Company, USA, GB-104234, Edition 06]
In this experiment, the stainless steel ball (type 316) is used. Scrupulously clean and dry the
instrument. Add the ball to the tube and assemble the parts as in the diagram (Figure 3).

_____________________________________________________ Department of Chemical Engineering


University of San Carlos

ChE 323L - Physical Chemistry Laboratory 1 Manual


Viscosity Measurement by Falling Sphere Method

Filling the Tube with Liquid


Unscrew cap. Then remove the ball from the tube. Slowly and carefully pipette the test liquid
(10-15 mL) into the tube until nearly full (approximately inch from the top of the flange). Use a stand
or holder for the tube for convenience during pipetting. A test tube rack may be used for this purpose.
Ensure that no air bubbles are present. The liquid should be clear of particles and filtered if necessary.
Particles in the liquid will interfere with the motion of the ball and reduce the accuracy of measurement.
Now, carefully add the ball and allow it to drop into the tube. Carefully replace the cap with rubber cork.

Taking a Reading
Invert the instrument full of liquid until the ball reaches the before release position. Restore
the instrument to its normal vertical position. It is now ready for taking a reading. For the most accurate
work, the viscosity tube should be immersed in a constant temperature bath with a transparent window
to observe the fiduciary lines (Figure 1). At elevated temperatures the cap should be removed to permit
excess liquid to pass through the capillary vent. Air and gas bubbles should also be vented after
equilibrium is reached. Then the cap is replaced.
Measure the time of descent between the two sets of fiduciary lines. Repeat measurements can
be made by removing the viscometer from the bath and inverting to return the ball to the before
release position and turning to the closed position. With good technique measurements should be
reproducible from 0.2% to 1.0% depending upon the time of descent.

Calculating the Viscosity


For a falling ball viscometer, calculate the viscosity by using the simple formula

= K (t -) t
where,

t
K

= viscosity of the liquid in centipoises [cP]


= density of ball [g/mL]
2.53 for the glass
8.02 for stainless steel
16.6 for tantalum
= density of liquid [g/mL] at a certain temperature
= time of descent [min.]
= viscosity constant [cP.mL/g-min.]

The approximate K for size 1=0.3, size 2=3.3 and size 3=3.5. In this experiment, size 1 is used.

_____________________________________________________ Department of Chemical Engineering


University of San Carlos

ChE 323L - Physical Chemistry Laboratory 1 Manual


Viscosity Measurement by Falling Sphere Method

3. Questions and Calculations


a) Compare Poiseuille equation with Stokes Law equation. Why is the Stokes Law equation most
valuable in the determination of viscosity for viscous liquids?
b) From the results obtained, explain the effect of temperature on the viscosity of liquids at constant
pressure.
c) If the experiment is conducted at constant temperature, what is the expected effect of pressure on
the measured viscosity of the liquid?
d) Compare the effects of temperature and pressure on the viscosity of gases to that of liquids.
e) Explain why liquids have greater resistance to flow than gases?
f) Aside from the applications mentioned in the Introduction, what are other applications where the
measurement of viscosity is employed? Mention at least three applications.

4. Bibliography
Gilmont Instruments, Barnant Company. Falling Ball Type Viscometer Operating Instructions Manual,
GB-104234, Edition 06.
Atkins, P. and de Paula, J. (2002). Atkins Physical Chemistry (7th ed.). Oxford, UK: Oxford University
Press, pp. 826-833.
Silbey, R.J. and Alberty, R.A. (2001). Physical Chemistry (3rd ed.). New York: John Wiley & Sons, Inc., pp.
650-651 and 742-744.

_____________________________________________________ Department of Chemical Engineering


University of San Carlos

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