EUROPEAN PHARMACOPOEIA 10.0 2.2.9.

Capillary viscometer method

In the conventional system adopted by the Pharmacopoeia, the

specific optical rotation is expressed by its value without units ;
the actual units, degree millilitres per decimetre gram When the limits for optical rotation or specific optical rotation
[(°)·ml·dm− 1·g− 1] are understood. are expressed as the dried substance, the anhydrous substance
or the solvent-free substance, the result must be corrected for
EQUIPMENT loss on drying (2.2.32), water content (2.5.12 or 2.5.32) or
The polarimeter typically consists of : content of solvent as appropriate.
– a light source, for example a sodium discharge lamp, a
light-emitting diode (LED) or another light source capable
of providing radiation at the desired wavelength (589 nm
unless otherwise prescribed in the monograph) ; if the light
source is polychromatic, a means of isolating the required
wavelength is necessary, e.g. an optical filter ; 04/2018:20208
– a polariser and an analyser ;
– a sample cell with a path length of 1.00 dm, unless otherwise
specified in the monograph ;
– a detection system to measure the angle of optical rotation,
which must be capable of giving readings to at least the 2.2.8. VISCOSITY
nearest 0.01°, unless otherwise specified in the monograph ;
– a temperature control system that indicates the temperature The dynamic viscosity or viscosity coefficient η is the tangential
with a readability of 0.1 °C ; it may be embedded in the force per unit surface, known as shearing stress τ and expressed
polarimeter (e.g. a Peltier system) or be an external unit in pascals, necessary to move, parallel to the sliding plane, a
(e.g. a cycle-cryostat), and must be able to maintain layer of liquid of 1 square metre at a rate (v) of 1 metre per
the temperature of the liquid to within ± 0.5 °C of that second relative to a parallel layer at a distance (x) of 1 metre.
prescribed.
The ratio dv/dx is a speed gradient giving the rate of shear D
EQUIPMENT PERFORMANCE expressed in reciprocal seconds (s− 1), so that η = τ/D.
The accuracy of the scale is checked near the value to be The unit of dynamic viscosity is the pascal second (Pa·s).
measured or over an appropriate range, usually by means of The most commonly used submultiple is the millipascal
certified quartz plates. Other certified reference materials may second (mPa·s).
also be suitable (e.g. sucrose solutions).
The kinematic viscosity v, expressed in square metres per
Optical rotation measurements may be used to quantify the
second, is obtained by dividing the dynamic viscosity η by the
amount of an enantiomer or the ratio of enantiomers present
density ρ expressed in kilograms per cubic metre, of the liquid
in a sample. For that purpose, the linearity must be checked,
measured at the same temperature, i.e. v = η/ρ. The kinematic
for example using sucrose solutions.
viscosity is usually expressed in square millimetres per second.
PROCEDURE A capillary viscometer may be used for determining the
Determine the zero of the polarimeter and the angle of rotation viscosity of Newtonian liquids and a rotating viscometer for
of the liquid at a wavelength of 589 nm and a temperature determining the viscosity of Newtonian and non-Newtonian
of 20 ± 0.5 °C, unless otherwise prescribed. The zero of the liquids. Other viscometers may be used provided that the
polarimeter is determined with the sample cell closed. accuracy and precision are at least as satisfactory as those
For neat liquids, the zero is determined with an empty sample obtained with the viscometers described in the related
cell. chapters.
For solutions, the zero is determined with the sample cell
filled with the same solvent as that used for the solution to be
examined and measured at the same temperature. The sample
preparation procedure is prescribed in the monograph.
Calculate the specific optical rotation at temperature t and 01/2019:20209
wavelength λ using the following formulae.
For neat liquids, the density of the liquid is taken into account :
α
[α]tλ =
l·ρt
For solutions : 2.2.9. CAPILLARY VISCOMETER
1000α METHOD
[α]tλ =
l·c
α PRINCIPLE
= angle of rotation measured at temperature t
and wavelength λ, in degrees ; The determination of viscosity is carried out using a
l = path length of the polarimeter sample cell, in suspended-level (Ubbelohde-type) capillary viscometer of
decimetres ; appropriate size at a temperature of 20.0 ± 0.1 °C, unless
otherwise prescribed. The time required for the level of the
ρt = density determined at the temperature of liquid to drop from one mark to the other is measured.
measurement t, in grams per cubic centimetre ;
for the purposes of the Pharmacopoeia, density
is replaced by relative density (2.2.5) ; EQUIPMENT
c = concentration of the solution, in grams per The principal components of an Ubbelohde-type capillary
litre. viscometer(1). are shown in Figure 2.2.9.-1.
(1) The European Pharmacopoeia describes the system proposed by the International Organization for Standardization (ISO)

General Notices (1) apply to all monographs and other texts 27

2.2.10. Viscosity - Rotating viscometer method EUROPEAN PHARMACOPOEIA 10.0

L M N 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.
The flow time of the liquid to be examined is the mean of
3 consecutive measurements. The result is valid if the relative
standard deviation of the 3 measurements is not more than
D 2.0 per cent.
E
Calculation
C Calculate the kinematic viscosity (ν) (2.2.8), in square
F millimetres per second, using the following expression :
ν = kt
k = viscometer constant, in square millimetres per second
squared ;
t = flow time of the liquid to be examined, in seconds.
Calculate the dynamic viscosity (η) (2.2.8), in millipascal
R seconds, using the following expression :
η = kρt
ρ = density of the liquid to be examined at the temperature
used for the viscosity measurement, in milligrams
per cubic millimetre.
B
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).
A

01/2008:20210

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

viscometer 2.2.10. VISCOSITY - ROTATING
PROCEDURE VISCOMETER METHOD
Select a capillary viscometer of appropriate size to obtain a The principle of the method is to measure the force acting on
minimum flow time of 200 s. a rotor (torque) when it rotates at a constant angular velocity
Calibration (rotational speed) in a liquid. Rotating viscometers are used
for measuring the viscosity of Newtonian (shear-independent
Capillary viscometers are calibrated at regular intervals as viscosity) or non-Newtonian liquids (shear dependent
defined in the quality management system and dictated by the viscosity or apparent viscosity). Rotating viscometers can be
frequency of use of the equipment and the application. divided in 2 groups, namely absolute and relative viscometers.
Calibrate the instrument at the temperature used for the In absolute viscometers the flow in the measuring geometry is
measurement by using at least 2 certified reference materials well defined. The measurements result in absolute viscosity
matching the viscosity range of the viscometer. values, which can be compared with any other absolute values.
Calculate the viscometer constant (k) in square millimetres In relative viscometers the flow in the measuring geometry
per second squared, using the following expression : is not defined. The measurements result in relative viscosity
η values, which cannot be compared with absolute values or
k= other relative values if not determined by the same relative
ρt viscometer method.
η = dynamic viscosity of the certified reference material, in Different measuring systems are available for given viscosity
millipascal seconds ; ranges as well as several rotational speeds.
ρ = density of the certified reference material, in milligrams APPARATUS
per cubic millimetre ;
The following types of instruments are most common.
t = flow time for the certified reference material to drop
CONCENTRIC CYLINDER VISCOMETERS (ABSOLUTE
from the upper mark to the lower mark, in seconds.
VISCOMETERS)
Calculate the mean of the values obtained. In the concentric cylinder viscometer (coaxial double cylinder
Method viscometer or simply coaxial cylinder viscometer), the viscosity
Charge the viscometer (Figure 2.2.9.-1) through tube L with is determined by placing the liquid in the gap between the
a sufficient quantity of the liquid to be examined (previously inner cylinder and the outer cylinder. Viscosity measurement
brought to 20 °C unless otherwise prescribed) to fill bulb A can be performed by rotating the inner cylinder (Searle type
while ensuring that the level of liquid in bulb B is below viscometer) or the outer cylinder (Couette type viscometer),
the exit to ventilation tube M. Immerse the viscometer in as shown in Figures 2.2.10.-1 and 2.2.10.-2, respectively. For
the upright position in a water-bath at 20.0 ± 0.1 °C (unless laminar flow, the viscosity (or apparent viscosity) η expressed
otherwise prescribed) and allow to stand for not less than in pascal-seconds is given by the following formula :
30 min to allow the temperature to reach equilibrium. Close
1 æ M ö÷æç 1 1 ö
çç 2 - 2 ÷÷÷÷ = k
tube M and draw the level of the liquid in tube N up to a level M
η= çç ÷
about 8 mm above mark E. Keep the liquid at this level by ç ÷
ω è 4πh øçè R i R o ÷ø ω

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