CHAPTER - 2

EXPERIMENTAL TECHNIQUES

2.1 VISCOSITY MEASUREMENTS :

Viscosity is the internal resistance that exists within a liquid, a very

important characteristic of both liquid and gases. It is important in studies of oils
and organic liquids and have lot of importance in science and technology.
Instruments called as viscometers have been developed to measure viscosity The
fluid flow can be set up by dragging fluid with a sliding or rotating surface,
forcing the liquid to pass through capillary or between two parallel plates, falling
body through the fluids. Viscometers are categorized depending upon initiation
and maintenance of fluid flow. Different viscometers are as follows.

Concentric cylinders and plate and cone type of viscometers are of

rotational type viscometers. They consist of concentric cylinders having a small
gap in between them. Inner cylinder is fixed and outside cylinder rotates at
variable angular velocities. In fixed outer cylinder viscometer, the inner cylinder
rotates at a constant speed having wrapped by a wire at each end. By using
different mass weights force is exerted and number of revolutions are counted.
Time required is proportional to the viscosity of liquid under test. In plate and
cone type, the top plate is generally stationary. Cone is on the top.

In falling ball method, a ball of suitable density and radius is allowed to

fall through a known distance and required time is measured. Cylinder must have
suitable diameter so as to avoid surface effect on the ball. Time required is related
to viscosity.

Falling cylinder method is similar to falling ball method. Flat ended solid
circular cylinder falls freely in vertical direction through testing fluid. This
method is used in liquids where visual observation is possible. In opaque liquids,
sensing techniques are implemented.

There are two types of methods commonly used to determine viscosity.

26
I) CAPILLARY FLOW METHOD [1-6] :

This is a very satisfactory method for determining viscosity of liquids.

This method involves the measurement of the volume and rate of flow of the fluid
through a long cylindrical tube of circular cross section. The total volume (V),
which flows past across any section in time t, is:

---(2.1)

This is known as Hagen-Poiseuille equation. Where P is driving pressure

between any two points in a capillary, l is the length of capillary, is the
coefficient of viscosity and r is the radius of capillary.

II ) FALLING BALL METHOD[1,5,7] :

The falling ball method consists of cylindrical tube filled with the fluid of
unknown viscosity. A ball of suitable density and radius is allowed to fall along
the axis of the tube. The time at which the ball passes regularly spaced horizontal
calibration marks is recorded and is further related to the viscosity of the fluid
through suitable mathematical equations.

In the present study, the capillary flow method was employed to determine
the viscosity of fluid at various temperatures. The usual form of this simple, yet
accurate, apparatus for calculating viscosities of different liquids is as shown in
figure 2.1.

The Ubbelohde viscometer [8-11] used in present investigation differs

from Ostwald and Cannon-Fenske viscometers in the provision of a suspended
level 'H' at the junction of the capillary 'C' and the bulb ‘G’. The left hand limb of
the U tube is essentially a pipette with two defining marks 'A' and 'B' and a
capillary 'C' through which the liquid contained in bulb 'D' flows under gravity
back into the 'E' in the right hand limb. This feature, which is obtained by
exposing suspended level to the atmosphere, ensures that the liquid issuing from
the capillary adheres as a film to the wall of the bulb 'G'. It is claimed that this
device eliminates loading and surface tension errors.

27
 A definite volume of liquid is employed and delivered into tube 'F' from a
calibrated pipette. The quantity of liquid should be such that when the liquid is
sucked up into the left hand limb until the meniscus stands above the mark 'A',
then the meniscus on the right stands at the bottom of the bulb 'E'. This liquid is
released from this position and allowed to flow back. When the meniscus passes
mark 'A', a stopwatch is started and when it reaches mark 'B' the stopwatch is
stopped and the time of out flow is noted. The stopwatch is with an accuracy of
0.01 s. The volume flow from 'A' to 'B' in time 't' is given by the equation 2.1.
The determination of absolute viscosity of a liquid with the help of equation 2.1
does involve the accurate measurement of 'P', 't', 'r', and 'I'. It is usually sufficient
to compare the viscosity of liquid with that of water or other standard liquids by
measuring the time taken for equal volumes of the two liquids to flow through the
same capillary under pressure due to their own weights. The densities of both
liquids must be known. The absolute viscosity of the liquid can then be obtained
knowing the viscosity of the standard liquid.
The viscosity values were determined using the relation…
 =(at-b/t) ---(2.2)
Where  is the viscosity,  is density of the liquid, t is flow time, a and b are the
constants for a given viscometer. The viscometer was calibrated with triply
distilled water. The constants a and b were obtained by measuring the flow times
of triply distilled water at temperatures 298.15, 303.15, 308.15, and 313.15 K.

Linear regression analysis of a plot of  t / against t2 for pure water at

four temperatures provides estimates of the constants a and b as slope and
intercept of the plot with a correlation coefficients of 0.999. Knowledge of a and b
allows determination of viscosities from the flow time and densities of liquids.

2.1.1 PRACTICAL DETAILS :

A viscometer was selected having a flow time of approximately 300

o
seconds at 25 C. It was first thoroughly cleaned with warm chromic acid so that
there were no obstructions in the capillary and the liquid ran clearly without
leaving drops behind. It was then thoroughly washed by drawing distilled water
through it followed by distilled acetone and finally dried by aspirating clean hot

28
air through it. Compressed air was not used because foreign particles or traces of
oil might cause serious errors. The viscometer was fastened accurately vertical in
a glass sided thermostat as shown in photograph. The mark 'A' was well below the
surface of water. A piece of rubber tubing, cleaned internally to remove dust, was
attached to the tube 'A' and used when sucking the liquid into the left hand limb.
o
The temperature of the thermostat was controlled within 0.01 C. A mechanical
stirrer was used to maintain a uniform temperature of the thermostat. A suitable
quantity of the liquid under investigation, usually 25 cc measured exactly, was
introduced into the viscometer with a pipette and allowed 10-15 minutes to reach
the temperature of the thermostat. The liquid was then sucked up and released and
the time of out flow between the marks was determined with an electronic
stopwatch reading to 0.01 s. The flow time measurement was repeated a number
of times (usually 5-6 times). The different readings did not deviate from the mean
by more than 0.2 s. To determine the influence of temperature on viscosity, the
time of out flow was measured at the interval of 5 oC between 25 and 40oC.

A small error may arise in these measurements due to the change of

volume of the liquid owing to expansion but this may be neglected provided that
during the out flow period, the lower meniscus lies inside the bulb 'E' so that the
change of level is small. For purpose of calculating absolute viscosities, densities
of liquids at various temperatures were required. These were determined by
means of a pycnometer. The viscometer was calibrated separately at each
temperature with an exactly same volume of a liquid of known viscosity and
density, usually water, the density and viscosity of which were taken from
literature [12]. From the densities and times of flow, absolute viscosities of the
liquid mixtures were calculated with the help of the equation 2.2. Since all flow
times were greater than 200 seconds, the kinetic energy correction is not applied.
To evaluate viscometer constant, the length of the capillary of the viscometer ( )
term is to be corrected as ’ = + 0.05r where “r” being the radius of the
viscometer capillary. Since “ ” is much larger (150-160 mm) as compared to “r”
(0.5 mm), i.e. = ’ and hence end effect in viscometer are negligible. Accuracy
of the viscosity measurements was 0.001 mPa.s.

29
FIGURE 2.1 Ubbelohde Viscometer

30
2.2 DENSITY MEASUREMENTS :

The density of a liquid or liquid mixture is defined as the mass per unit
volume and is generally expressed as g.cm-3 in CGS or more appropriately as
kg.m-3 in SI.

Density of liquid is generally measured either by a density bottle or by

pycnometer or by determining buoyancy action on a 'sinker' immersed in a liquid
(principle of Archemedes). When sufficient accuracy is not required density is
some times measured by the rate of rise or fall of a small-immersed quartz-float of
pre- arranged overall density. When sufficient amount of liquid is available, the
density can be determined, approximately, by means of hydrometer. In the present
study a bicapilary pycnometer was used for the density measurements. Therefore
a brief survey of various pycnometers is given below.

When only small quantities of liquids are available or where greater

accuracy is required, the density of liquid is best determined by means of vessels
of accurately known definite volume, called pycnometers. These are made in
varying shapes. The pycnometer, invented by Spengel and modified by Ostwald,
is very popular for accurate density measurements. Perkins, Bonsfield and many
others have altered forms of pycnometers. Most of pycnometers are of single
capillary and usually used to determine the density of liquid at fixed temperature.

2.2.1 PRACTICAL DETAILS :

A bicapillary pycnometer (fig. 2.2) with a bulb volume of 15 cc was

chosen for the present work [13-23].

The pycnometer was washed thoroughly with fresh chromic acid to

remove any obstructions in the capillary that enabled a smooth flow of liquid
without drops sticking behind. Subsequently the pycnometer was washed with
distilled water and then with acetone and dried with a stream of warm air from hot
blower. It was then kept in an oven at about 60 oC for half an hour. The weights of
empty pycnometer and pycnometer filled with experimental liquids were taken on
an Adair Dutt balance having a sensitivity of 0.01 mg. The pycnometer was
calibrated with freshly prepared triply distilled water. The pycnometer was filled

31
with air-bubble free triply distilled water by dipping the end of 'A' limb with the
water taken in beaker. Water was filled up to mark 'D' in limb 'B' by capillary
action.

The pycnometer was mounted accurately vertical in a glass sided

thermostat. The temperature of the thermostat was controlled within 0.01oC. The
height of water in limbs 'A' and 'B', say h1 and h2 were noted at various
temperatures with the help of travelling microscope that could read to 0.01mm.
From the known densities of water at various temperatures and the weights of the
water taken in the pycnometer, corresponding volumes of water were calculated.
The volumes were plotted against the total height (h1+h2) of water levels, yielding
a straight line. This served as a calibrating curve for pycnometer.

Pycnometer was removed from the thermostat and cleaned as above. It

was then filled with experimental liquids and mounted in the thermostat. The
procedure was repeated to find the total height (h1 + h2) for experimental liquids
at various temperatures. From their total height, the corresponding volumes of
liquids under investigation were obtained from the calibration curve and the
corresponding densities thus determined.

The density measurements for each experimental liquid were repeated at

least three to four times and the results averaged. This procedure enabled us to get
an uncertainty of  gm/cm3 in density measurements.

32
FIGURE 2.2 Bi-capillary Pycnometer

33
34
2.3 SPEED OF SOUND MEASUREMENTS :

The speed of sound (U) of liquids is determined by simple and direct

device called ultrasonic interferometer. The ultrasonic waves in liquids and
mixtures are conducted by different method [24-27] The principle used in the
measurements of speed of sound is based on the accurate determination of the
wavelength (λ) in a medium. The ultrasonic waves of known frequency (f) are
produced by a quartz crystal fixed at the bottom of the cell. A movable metallic
plate kept parallel to the quartz crystal reflects these waves. If the separation
between these two plates is exactly a whole multiple of the ultrasonic wavelength,
standing waves are formed in the medium. This acoustic resonance gives rise to
an electrical signal on the generator driving quartz crystal, and the anode current
of the generator becomes a maximum.

If the distance is increased or decreased and the variation is exactly one

half the wave length ( )or a multiple of it, an anode current becomes maximum.

From the knowledge of wavelength and frequency, speed of sound can be

obtained by the relation:
Velocity = (Wave length) (frequency)
U=f ---(2.3)

In the present investigation, F-81 ultrasonic interferometer operating at a

frequency of 2 MHz was used [29-36]. Working of the interferometer was
checked by measurements of speed of sound in pure liquids such as water,
benzene, methylbenzene, Isopropylbenzene, fluorobenzene and comparing with
the precise literature values. The agreement was with in ±1ms-1. Therefore our
speeds of sound measurements in the present investigation are precise with in
±1ms-1.

A) HIGH FREQUENCY GENERATOR :

This interferometer (photograph 2.4) is designed to excite the quartz

crystal fixed at the bottom of the measuring cell at its resonance frequency to
generate an ultrasonic wave in the experimental liquid, filled in the measuring
cell. A micrometer, to observe the changes in current and two controls for the

35
purpose of sensitivity regulation and initial adjustment of the micrometer are
provided on the panel of the high frequency generator.

B) MEASURING CELL :

The interferometer cell (fig 2.5) is a specially designed double

walled cell for maintaining the temperature of the liquid constant during the
experiment. A fine micrometer screw has been provided at the top, which can
raise or lower the reflector plate in the liquid in the cell through a known distance.
It has quartz- crystal fixed at its bottom. The maximum capacity of the cell is 12
cc. The instrument was adjusted in the following manner:
1) The cell was inserted in the square base socket and clamped to it with the help
of a screw provided on one of its sides,
2) The knurled cap of the cell was unscrewed and lifted away from the double
walled cell. The experimental liquid was poured in the middle portion of the cell
and the knurled cap was screwed.
3) Water at desired temperature, from a thermostat, was circulated through two
chutes in double wall of the cell, and
4) The high frequency generator was connected to the cell by a co-axial cable.

2.3.1 PRACTICAL DETAILS :

The interferometer was initially adjusted with the help of two knobs
provided on the high frequency generator, one marked with Adj and other with
Gain. With knob marked Adj, the position of needle on the Ammeter was adjusted
and knob marked Gain was used to increase the sensitivity of the instruments for
greater deflection if desired. The interferometer cell was filled with the
experimental liquid and connected to the output terminal of the high-frequency
generator through a shielded cable. Water was circulated around the measuring
cell from a thermostat maintained at constant temperature (0.01 K). When the
liquid attained the temperature of the bath, the micrometer screw was slowly
moved till the anode current meter showed a maximum.

For increasing the accuracy of the measurement, several such maxima

were counted (n) by changing the distance between the transducer and the

36
reflector. The total distance (d) moved by the reflector was used to calculate the
wavelength () with the help of the equation:

---(2.4)

The frequency of the crystal ‘f ’is accurately known (2 MHz). The sound
velocity, U, in the liquid was calculated with the help of equation 2.3

37
38
39
2.4 IR SPECTRUM :

FTIR spectra were recorded on a FTIR spectrometer (Model SHIMADZU

8400s pc) by using KBr pellet in the region 4000-400 cm-1 (30-2.5μm). For the
FTIR technique measurement of a single spectrum is faster because the
information at all frequencies is collected simultaneously. This allows multiple
samples to be collected and averaged together resulting in an improvement in
sensitivity.

2.5 PURIFICATION :

Even though the purity of substance is not a crucial factor in

measurements of density [28], it is very important for viscosity measurements.
Therefore, all chemicals were used after purification:

1) t-Butanol (s.d.fine chem. purity 99.5 )

2) Benzene (s.d.fine chem. purity 99 )
3) Chlorobenzene (s.d.fine chem., purity 99.5)
4) Toluene (s.d.fine chem. purity 99 )
5) o-Chlorotoluene (s.d. fine chem. Purity 99% )
6) p-Chlorotoluene (s.d. fine chem. Purity 99% )
7) o-Xylene (s.d.fine chem., purity 99)
8) m-Xylene (s.d. fine chem. Purity 99% )
9) p-Xylene (s.d. fine chem. Purity 99% )
10) Nitrobenzene (s.d.fine chem., purity 99)
11) Aniline (s.d.fine chem. purity 99 )

All the chemicals were used after single distillation. The purity of the
solvents, after purification was ascertained by comparing their experimental
density, viscosity and ultrasonic velocity with the corresponding literature values
at 298.15 K (Table 2.1). From the Table 2.1, it could be said that, our
experimental values matched very well with those of literature.

40
2.6 PREPARATION OF LIQUID MIXTURES :

Binary and ternary liquid mixtures were prepared by mixing known

masses of each liquid in airtight stoppered glass bottles. The measurements were
made on a AND single pan electronic balance to an accuracy of ± 0.01 mg. The
more volatile component (pentyl and isopentyl acetate) was filled directly into the
bottle and the closed bottle was weighed. The other component (alkanols) was
injected into the bottle through the stopper by means of a syringe. This method
allowed negligible vapour loss and contamination. The possible error in mole
-4
fraction is calculated to be less then ±1x 10 . The preferential evaporation of
solvents from the mixture was kept to a minimum as evidenced by reproducible
measurements of the physical properties of these liquid mixtures over a time
interval of 1 or 2 days.

41
Table 2.1: Comparison of Experimental Density, Viscosity and Speed of
Sound with Literature.
Temp. ×10
-3
kg.m-3 η (mPa.s) u (m.s-1)
Liquid
K Expt. Lit. Expt. Lit. Expt. Lit.
298.15 0.7810 0.781237 4.445 4.44437 1125 1123.542
303.15 0.7750 0.775437 3.379 3.37840 1109 111085
t-Butanol
308.15 0.7700 0.770238 2.642 2.64441 1094 109337
313.15 0.7648 0.764838 2.106 2.10542 1084 108137
298.15 0.8735 0.873562 0.616 0.61647 1300 130050
303.15 0.8682 0.868239 0.568 0.57048 1286 128051
Benzene
308.15 0.8630 0.863245 0.532 0.53149 1258 126052
313.15 0.8574 0.857646 0.502 0.50341 1232 122752
298.15 1.1005 1.100661 0.757 0.75565 1264 126852
303.15 1.0956 1.095562 0.721 0.72366 1240 123852
Chlorobenzene
308.15 1.0893 1.089263 0.679 0.67365 1220 122450
313.15 1.0844 1.084564 0.640 0.64366 1198 119550
298.15 0.8618 0.862353 0.551 0.55256 1304 130459
303.15 0.8576 0.857654 0.527 0.52757 1285 1285.384
Toluene
308.15 0.8532 0.852850 0.492 0.49649 1259 126260
313.15 0.8484 0.848455 0.486 0.48558 1248 124885
298.15 1.0778 1.077539 0.958 0.95789 1304 130290
303.15 1.0726 1.072182 0.892 0.88783 1284 128482
o-Chlorotoluene
308.15 1.0679 1.067846 0.826 0.82883 1262 125990
313.15 1.0631 1.063039 0.767 0.76439 1243 124090
298.15 1.0648 1.064587 0.848 0.85239 1293 -
303.15 1.0597 1.059587 0.785 0.78439 1271 127182
p-Chlorotoluene
308.15 1.0526 1.05239 0.731 0.72639 1249 -
313.15 1.0474 1.04739 0.718 0.72239 1237 -
298.15 0.8756 0.875975 0.755 0.75478 1345 134859
303.15 0.8716 0.871750 0.703 0.69577 1333 133987
o-Xylene
308.15 0.8676 0.867876 0.650 0.65050 1321 132350
313.15 0.8635 0.863377 0.571 0.57739 1310 1297.587

42
Table 2.1 contd :
298.15 0.8601 0.859950 0.585 0.58250 1320 132480
303.15 0.8555 0.855839 0.553 0.55777 1301 130070
m-Xylene
308.15 0.8518 0.851579 0.501 0.50939 1281 128659
313.15 0.8474 0.846750 0.474 0.47339 1267 126059
298.15 0.8562 0.856581 0.602 0.60539 1315 131450
303.15 0.8522 0.852281 0.564 0.56646 1294 128985
p-Xylene
308.15 0.8473 0.847839 0.527 0.52777 1270 127250
313.15 0.8437 0.843681 0.489 0.48839 1259 126186
298.15 1.1982 1.198139 1.801 1.79150 1461 146369
303.15 1.1933 1.193467 1.618 1.61968 1442 144669
Nitrobenzene
308.15 1.1883 1.188349 1.430 1.43739 1423 142350
313.15 1.1834 1.183567 1.252 1.25539 1404 140269
298.15 1.0171 0.017270 3.775 3.77442 1630 163473
303.15 1.0121 1.012970 3.141 3.17072 1615 1614.542
Aniline
308.15 1.0087 1.008471 2.521 2.51039 1599 1595.142
313.15 1.0049 1.004439 2.400 2.40072 1582 158274

43
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