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2.2.10. Viscosity - Rotating Viscometer Method

This document provides information about methods for measuring viscosity, including the capillary viscometer method and rotating viscometer method. It describes the principles, equipment, procedures, calculations, and key parameters for each method. The document contains detailed technical information intended for those performing viscosity measurements.
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0% found this document useful (0 votes)
179 views3 pages

2.2.10. Viscosity - Rotating Viscometer Method

This document provides information about methods for measuring viscosity, including the capillary viscometer method and rotating viscometer method. It describes the principles, equipment, procedures, calculations, and key parameters for each method. The document contains detailed technical information intended for those performing viscosity measurements.
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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EUROPEAN PHARMACOPOEIA 11.0 2.2.10.

Viscosity - Rotating viscometer method

01/2019:20209 Calculate the viscometer constant (k) in square millimetres


per second squared, using the following expression :
η
k=
ρt
η = dynamic viscosity of the certified reference material, in
2.2.9. CAPILLARY VISCOMETER millipascal seconds ;
METHOD ρ = density of the certified reference material, in milligrams
per cubic millimetre ;
PRINCIPLE t = flow time for the certified reference material to drop
The determination of viscosity is carried out using a from the upper mark to the lower mark, in seconds.
suspended-level (Ubbelohde-type) capillary viscometer of
appropriate size at a temperature of 20.0 ± 0.1 °C, unless Calculate the mean of the values obtained.
otherwise prescribed. The time required for the level of the Method
liquid to drop from one mark to the other is measured. Charge the viscometer (Figure 2.2.9.-1) through tube L with
a sufficient quantity of the liquid to be examined (previously
EQUIPMENT brought to 20 °C unless otherwise prescribed) to fill bulb A
The principal components of an Ubbelohde-type capillary while ensuring that the level of liquid in bulb B is below
viscometer(2). are shown in Figure 2.2.9.-1. the exit to ventilation tube M. Immerse the viscometer in
the upright position in a water-bath at 20.0 ± 0.1 °C (unless
otherwise prescribed) and allow to stand for not less than
L M N 30 min to allow the temperature to reach equilibrium. Close
tube M and draw the level of the liquid in tube N up to a level
about 8 mm above mark E. Keep the liquid at this level by
closing tube N and opening tube M. Open tube N and, using a
stopwatch, measure the time required, to at least the nearest
1/5 of a second, for the level of the liquid to drop from mark E
to mark F.
D The flow time of the liquid to be examined is the mean of
E 3 consecutive measurements. The result is valid if the relative
standard deviation of the 3 measurements is not more than
C 2.0 per cent.
F
Calculation
Calculate the kinematic viscosity (ν) (2.2.8), in square
millimetres per second, using the following expression :
ν = kt
k = viscometer constant, in square millimetres per second
squared ;
R t = flow time of the liquid to be examined, in seconds.
Calculate the dynamic viscosity (η) (2.2.8), in millipascal
seconds, using the following expression :
η = kρt

B ρ = density of the liquid to be examined at the temperature


used for the viscosity measurement, in milligrams
per cubic millimetre.
A The density may be obtained by multiplying the relative
density of the liquid to be examined by 0.99820 (measurement
at 20 °C) or 0.99704 (measurement at 25 °C).

01/2008:20210

Figure 2.2.9.-1. – Suspended-level (Ubbelohde-type) capillary


viscometer

PROCEDURE
2.2.10. VISCOSITY - ROTATING
Select a capillary viscometer of appropriate size to obtain a
minimum flow time of 200 s. VISCOMETER METHOD
Calibration The principle of the method is to measure the force acting on
a rotor (torque) when it rotates at a constant angular velocity
Capillary viscometers are calibrated at regular intervals as (rotational speed) in a liquid. Rotating viscometers are used
defined in the quality management system and dictated by the for measuring the viscosity of Newtonian (shear-independent
frequency of use of the equipment and the application. viscosity) or non-Newtonian liquids (shear dependent
Calibrate the instrument at the temperature used for the viscosity or apparent viscosity). Rotating viscometers can be
measurement by using at least 2 certified reference materials divided in 2 groups, namely absolute and relative viscometers.
matching the viscosity range of the viscometer. In absolute viscometers the flow in the measuring geometry is
(2) The European Pharmacopoeia describes the system proposed by the International Organization for Standardization (ISO)

General Notices (1) apply to all monographs and other texts 33


2.2.10. Viscosity - Rotating viscometer method EUROPEAN PHARMACOPOEIA 11.0

well defined. The measurements result in absolute viscosity α = angle in radians between the flat disk and the cone,
values, which can be compared with any other absolute values. τ = shear stress in pascals (Pa),
In relative viscometers the flow in the measuring geometry
is not defined. The measurements result in relative viscosity γ = shear rate in reciprocal seconds (s-1).
values, which cannot be compared with absolute values or
other relative values if not determined by the same relative
viscometer method.
Different measuring systems are available for given viscosity
ranges as well as several rotational speeds.

APPARATUS
The following types of instruments are most common.
CONCENTRIC CYLINDER VISCOMETERS (ABSOLUTE
VISCOMETERS)
In the concentric cylinder viscometer (coaxial double cylinder
viscometer or simply coaxial cylinder viscometer), the viscosity
is determined by placing the liquid in the gap between the
inner cylinder and the outer cylinder. Viscosity measurement
can be performed by rotating the inner cylinder (Searle type
viscometer) or the outer cylinder (Couette type viscometer),
as shown in Figures 2.2.10.-1 and 2.2.10.-2, respectively. For
laminar flow, the viscosity (or apparent viscosity) η expressed
in pascal-seconds is given by the following formula :

1 æ M ö÷ æç 1 1 ö÷÷ M
η= çç ÷ ç - 2÷
=k
ω çè 4πh ÷ø ççè R 2
R ÷ø÷ ω Figure 2.2.10.-1
i o

M = torque in newton-metres acting on the cylinder


surface,
ω = angular velocity in radians per second,
h = height of immersion in metres of the inner cylinder
in the liquid medium,
Ri = radius in metres of the inner cylinder,
Ro = radius in metres of the outer cylinder,
k = constant of the apparatus, expressed in radians per
cubic metre.
For non-Newtonian liquids it is indispensable to specify the
shear stress (τ) or the shear rate (γ) at which the viscosity is
measured. Under narrow gap conditions (conditions satisfied
in absolute viscometers), there is a proportional relationship
between M and τ and also between ω and γ :

τ = AM γ = Bω

where A and B are constants for the instrument and are


calculated from the following expressions :
Figure 2.2.10.-2
– for concentric surface : CONE-PLATE VISCOMETERS (ABSOLUTE VISCOMETERS)
In the cone-plate viscometer, the liquid is introduced into the
1 R i2 + R o2 R i2 + R o2 gap between a flat disc and a cone forming a define angle.
A= B=
4πh R i2R o2 R o2 - R i2 Viscosity measurement can be performed by rotating the cone
or the flat disc, as shown in Figures 2.2.10.-3 and 2.2.10.-4,
– for cone-plates : respectively. For laminar flow, the viscosity (or apparent
viscosity) η expressed in pascal-seconds is given by the
3 1 following formula :
A= B=
2πR 3 α æ M ö æ 3α ö÷ M
η = çç ÷÷÷ çç =k
M = torque in Newton-metres acting on the cone or çè ω ø çè 2πR 3 ÷÷ø ω
cylinder surface,
ω M = torque in Newton-metres acting on the flat disc or
= angular velocity in radians per second,
cone surface,
Ri = radius in metres of the inner cylinder, ω = angular velocity in radians per second,
Ro = radius in metres of the outer cylinder, α = angle in radians between the flat disc and the cone,
R = radius in metres of the cone, R = radius in metres of the cone,
h = height of immersion in metres of the inner cylinder k = constant of the apparatus, expressed in radians per
in the liquid medium, cubic metre.

34 See the information section on general monographs (cover pages)


EUROPEAN PHARMACOPOEIA 11.0 2.2.10. Viscosity - Rotating viscometer method

Constants A, B of the apparatus (see under concentric cylinder


viscometers).

Figure 2.2.10.-3

Figure 2.2.10.-6

In a general way, the constant k of the apparatus may be


determined at various speeds of rotation using a certified
viscometer calibration liquid. The viscosity η then corresponds
to the formula :
Figure 2.2.10.-4

SPINDLE VISCOMETERS (RELATIVE VISCOMETERS)

In the spindle viscometer, the viscosity is determined by M


η=k
rotating a spindle (for example, cylinder- or disc-shaped, ω
as shown in Figures 2.2.10.-5 and 2.2.10.-6, respectively)
immersed in the liquid. Relative values of viscosity (or
apparent viscosity) can be directly calculated using conversion
factors from the scale reading at a given rotational speed.
METHOD

Measure the viscosity (or apparent viscosity) according to the


instructions for the operation of the rotating viscometer. The
temperature for measuring the viscosity is indicated in the
monograph. For non-Newtonian systems, the monograph
indicates the type of viscometer to be used and if absolute
viscometers are used the angular velocity or the shear rate at
which the measurement is made. If it is impossible to obtain
the indicated shear rate exactly, use a shear rate slightly higher
and a shear rate slightly lower and interpolate.

With relative viscometers the shear rate is not the same


throughout the sample and therefore it cannot be defined.
Under these conditions, the viscosity of non-Newtonian
liquids determined from the previous formula has a relative
character, which depends on the type of spindle and the
angular velocity as well as the dimensions of the sample
container (Ø = minimum 80 mm) and the depth of immersion
of the spindle. The values obtained are comparable only if
the method is carried out under experimental conditions that
Figure 2.2.10.-5 are rigorously the same.

General Notices (1) apply to all monographs and other texts 35

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