Experiment 4: Measurement of Viscosity of NR Latex

4.1 Objective
4.1.1 To determine the viscosity of the NR latex according to MS 281: Part 15:1992.
4.1.2 To measure the effect of spindle speed and spindle number on viscosity of
natural rubber latex.

4.2 Introduction
Havae Latex which is comprised of rubber particles and a dispersed phase in aqueous
serum known as “viscoids”, exhibits significant viscosity change when treated with
ammonia, sodium sulphite, formaldehyde or distilled water. The NR latex is a highly
specified material and is characterized by properties that are significant to the user.
Viscosity of latex significantly influences processing conditions and final rubber product
properties. Therefore, understanding factors affecting viscosity of latex is beneficial.
(Perez, 1993)

Viscosity is the measure of flow or the internal friction for a liquid system. This friction
becomes apparent when a layer of fluid is made to move in relative to another layer. The
greater the friction, the greater the amount of force require to cause this movement
which is called shear. Shearing occur whenever the fluid is physically moved or
distributed. The higher the viscous fluids, therefore, require more force to move than less
viscous materials. The viscosity of latex can be very complex as the latex is hetero-
phase system. (Athey, 1991)

The Brookfield viscometer is probably one of the most commonly used rotational
viscometers. It consists of a series of spindles which are immersed into a large vat of
fluid and enables scale deflection to be measured for a given rotational speed of the
spindle. A viscosity value can then be found from a table provided by the manufacturers;
however, a corresponding shear rate is not given. This viscosity value is the viscosity of
the Newtonian fluids. This means that Brookfield R.V.T is essentially a quality control
instrument whereby data is given in terms of scale deflection, spindle number and speed
of rotation rather than a viscometric shear stress-shear rate relationship. (Williams, 1984)

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For many industrial applications, it is important to obtain accurate results with the least
expensive and most versatile instrument. Of those mentioned, the Brookfield Synchro-
Lectric Viscometer introduced in 1981 is probably the best available compromise
between accuracy and price. The variety of attachments available allows coverage of a
broad range of shear rate and viscosity. In the older style Brookfield instruments, many
of which are available in laboratories and plants today, a dial deflection (0 to 100) by an
appropriate factor which are obtained from a “Factor Finder” supplied with the instrument
and should only be used for Newtonian fluids since the “dial viscosity” and the apparent
viscosity are identical only in this case. (David& Meyer, 2000)

Latex is a non-Newtonian fluid. The viscosity measured is not an absolute value. Most
latex exhibits decreasing viscosity with increasing shear rate and for this reason any
reference to latex viscosity should include a description of the method of measurement,
the rate of shear (if known) and the test temperature. The viscosity of particular latex is a
function of its origin, including the clone from which it was derived, and of the
composition of the latex serum, its total solids concentration, and the means of
preservation. (Perez, 1993)

Besides that, the reading of the latex viscosity must be taken by clamping both pointer
and scale of the viscometer where the rotation of spindle is stopped. Thus, it is not
suitable to measure the viscosity associated with non-Newtonian flow behavior
continuously. The viscometer also can be affected by turbulence and angle of immersion
of the spindle. (Blackley, 1997)

4.3 Materials
Old natural rubber (NR) latex, Acrylonitrile rubber (NBR) latex and Distilled water

4.4 Equipment
Brookfield Synchro-Lectric viscometer RV 200 Type R, Beaker, Glass rod, Spindle
number 2 and 3 and Filter.

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4.5 Procedure
1. The spindle of number 2 was attached to the motor shaft securely, while the guard
was attached securely to the motor housing of the viscometer.
2. The spindle and guard were inserted carefully into the NR latex sample until the
surface of the sample was at the mid-point of the groove on the spindle shaft. The
procedure was carried out in such a way as to avoid air being trapped,
3. The spindle was placed vertically in the sample and in the centre of the beaker.
4. The rotational speed of the instrument was selected at 5, 10, 20, 50 and 100 rpm
respectively.
5. The viscometer motor was switched on and the equilibrium reading was taken to the
nearest unit scale division.
6. The experiment was repeated with NR latex with spindle of number 3.
7. The procedure from 1 to 6 is repeated by using NBR latex.
8. All the readings were obtained and tabulated.

4.6 Result& Discussion

In the study of flow behavior, it is more common to describe the variation of viscosity as
a function of shear rate (spindle speed). The Brookfield device can be used with the
expectation of about 10% precision. Besides, spindle number is another parameter that
will give significance to the experimental result.

1500
Viscosity (mPa.s)

1000

500 Spindle number 2

Spindle number 3
0
0 20 40 60 80 100 120
Spindle speed (rpm)

Figure 1: Comparison of viscosity of NR latex using spindle number 2 and 3 at different

spindle speed

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Figure 1 shows that both NR latices with different spindle number exhibits similar trend
of variation that is decreasing viscosity with the increasing of the spindle speed. Besides,
it can be observed that the viscosity of the NR latex tested by spindle number 3 is higher
than the spindle number 2. Hence, the decreasing viscosity of NR latex with shear rate
indicates that the NR latex exhibit shear thinning effect (pseudo-plastic) as most
polymers solution and melted polymers will do.

The viscosity of the both NR lattices shows the highest value at the slowest spindle
speed (5.0 rpm) used. At the early stage without apparent shearing force, the latex
particle is extensively entangled without the alteration on the molecular chain of the
sample. This can be explained by the shearing force produced at the slowest speed is
finite and insufficient to cause any chain orientation on the latex particles. As the speed
of spindle increase, more shearing force is generated and hence enough to do some
alteration on the molecular chain.

When the spindle shaft is rotated, the latex particles at the molecular level are interfered
by the dragging force applied by the shaft. The shear rate applied on the latex particles
lead to molecular orientation where the chain entanglement of the latex is reduced
dramatically. Subsequently, the slippage between the latex particles are readily to occur
which can increase the average distance between the latex particles. The free volume
between the adjacent particles is now increases causing the latex particles are now
more dispersed than before. At low shear rates, Brownian motion of the rubber latexes
made them to rotate and they interfere strongly with one another so the viscosity is high.
As the shear rate increased, the rubber latices were became deformable and aligned
with the direction of flow, so that they interfere less with one other and the viscosity
decreased.

Figure 2 shows the variation of viscosity as a function of shear rate in NBR latex. When
discussing the viscosity of synthetically made latex, it is different from the natural clone
Havae latex due to difference in molecular structure, molecular weight, molecular weight
distribution and chain polarity. All these parameters have on effects on the viscosity of
NBR latex.

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 120
Viscosity (mPa.s)

100
80
60
Spindle number2
40
20 Spindle number 3
0
0 20 40 60 80 100 120
Spindle speed (rpm)

Figure 2: Comparison of viscosity of NBR latex using spindle number 2 and 3 at different
spindle speed

NBR latex shows the abnormal trend of viscosity change as a function of shear rate.
Although a clear trend for both NBR lattices cannot be made, from Figure 2, it is obvious
to observe that the viscosity of the NBR latex tend to increase at fastest spindle speed.
This can be explained by the NBR latex being shorter molecular weight polymer are
more prone to heat sensitization effect compared to NR latex with higher molecular
weight. This is especially the case where spindle number 2 with larger diameter will
generate more shear. The shearing force that generated on the NBR latex system will
cause the viscosity to decrease until a point where accumulated kinetic energy in the
latex system is sufficient to overcome the repulsive force between latex particles in the
emulsion system. More kinetic energy is generated in the latex system and latex
destabilization is increased. When the latex is destabilized, latex flocculation occurs
where micro-coagulation of latex results in small aggregates of rubber. The occurrence
of the latex aggregates causing the dragging force applied by the shaft and the torque
developed increase. This leads to a significant increase of viscosity.

However, by making comparison, heat sensitization of the NR latex is lower due to

higher molecular weight and broader molecular weight distribution. NR latex particles in
the latex system that are long and entangled are stable in the thermal condition and

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higher kinetic energy is needed to supplied to increase the frequency and violence of the
latex particles collision in order to form small flocculate as NBR latex.

There are some external factors that attribute to the experiment result. The same latex
sample is used throughout the test conducted causing an accumulation of the shearing
force effect. The same latex sample is used to test the effect of every spindle speed
causing the effect from previous spindle speed test will be add up to the effect of next
spindle speed tested. Therefore, the latex should be regularly changed during the
experiment conducted in order to increase the accuracy of the result.

Besides, there are also another one crucial parameter that can be associated with this
experiment which is the spindle number used. Theoretically, the spindle number used
can influence the viscosity of the latex, where higher viscosity of NR latex can be
obtained by using a higher spindle number during the test. There is a range of spindle
number that has significantly different disc diameter. The diameter of the disc increases
with the lowering of the number of the spindle used; so as the surface area. Thus,
spindle number 2 which has the largest disc diameter has the highest contact surface
area with the NR latex. Such larger contact area can significantly interfere the movement
or the arrangement of the latex particles since higher shearing force is produced during
rotation.

As the shear rate increased, the latex particles become deformable and aligned with the
direction of flow, resulting in the decrease in viscosity. On the other hand, smaller
contact area imparted by the larger spindle number (spindle number 3) will contribute to
a lower shearing force on the latex particles and subsequently exhibit lower shear rate.
As a result, the latex particles cannot be readily orientated or aligned from the chain
entanglement. Furthermore, the longer chains of the latex particles are not broken
sufficiently into shorter chains to increase the flow behaviour of the latex. Thus, the
viscosity of the latex is higher by using the larger spindle number or smaller disc
diameter.

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4.7 Conclusion
In conclusion, the latex viscosity depends upon the speed of the spindle. For NR latex,
the shear thinning effect or pseudo-plastic behavior will be dominant that is the viscosity
of NR latex decrease with spindle speed (shear rate). At high spindle speed, the rubber
chains undergo chain scission more aggressively due to higher shear rate that exerted
on the NR latex. Hence the free volume is increase and the latex particle are more
dispersed, subsequently the viscosity of the NR latex decreases. For NBR latex, the
viscosity tends to decrease gradually and up to the point before latex destabilization due
to heat build-up in the latex system.

Besides, the viscosity of NR latex sample will also decrease with the decreasing spindle
number used. This due to a larger contact area with latex is associated with the
decreasing of spindle number used and more shearing force is able to be produced. As
a result, the movement of particles is significantly interfered and the chain scission of the
latex is more likely to occur. Thus, the higher viscosity of the latex sample can be
observed with large spindle number.

References
(1) Athey, R.D. (1911). Emulsion Polymer Technology. New York: Marcel Dekker,
Inc
(2) Blackley, D.C. (1997). Polymer Latices: Science and Technology Vol 1:
Fundamental Principles. New York: Springer.
(3) David, D.B& Mayer, R.R (1990), Rheology Modifiers Handbook: Practical Use
and Application (Materials and Processing Technology). New York: William Andrew
Publishing
(4) Jean Perez. (1993). Natural Latex: Control and Industrial Procedures. Clinical
Reviews in Allergy, Volume 11, 355-361.
(5) R. W, Williams. (1978). Determination of Viscometer Data from The
Brookfield R.V.T. Viscometer, Volume 18, 345-359.

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 Table 1: Viscosity of NR Latex using different spindle speed
Spindle Speed Factor Dial Reading Average Viscosity
number
2 5 80 13 13 13 13 1040
10 40 18 18 18 18 720
20 20 25 25 25 25 500
50 8 39.5 39.5 39.5 39.5 316
100 4 52 55 54 54 214.67
3 5 200 6 6 6 6 1200
10 100 8 8 8 8 800
20 50 11 11 11 11 550
50 20 16.5 17 17 17 336.7
100 10 24 24 17 22 250

Table 2: Viscosity of NBR Latex using different spindle speed

Spindle Speed Factor Dial Reading Average Viscosity
number
2 5 80 0.5 0.5 0.5 0.5 40
10 40 1 1 1 1 40
20 20 2.5 2.5 2.5 2.5 50
50 8 6.5 6.5 7.5 6.8 54.67
100 4 17.5 16 16.5 16.7 66.67
3 5 200 0.5 0.5 0.5 0.5 100
10 100 0.5 0.5 0.5 0.5 50
20 50 1 1 1 1 50
50 20 4 3 4 3.7 73.33
100 10 5.5 6 5.5 5.7 56.67

Useful formulae:
Apparent viscosity= Factor× Dial Reading