SASO DIN 51562-3:2016

DIN 51562-3: 1985

Determination of kinematic viscosity using the Ubbelohde

viscometer – Part 3: Viscosity relative increment at short
flow times

The Saudi Standards, Metrology and Quality Organization

THIS DOCUMENT IS A DRAFT SAUDI STANDARD CIRCULATED FOR
COMMENT. IT IS, THEREFORE SUBJECT TO CHANGE AND MAY NOT BE
REFERRED TO AS A SAUDI STANDARD UNTIL APPROVED BY THE BOARD
OF DIRECTORS.

ICS: 17.060
 Foreword

The Saudi Standards, Metrology and Quality Organization (SASO) has

adopted the DIN standard No. DIN 51562-3: 1985 “Determination of
kinematic viscosity using the Ubbelohde viscometer – Part 3: Viscosity
relative increment at short flow times” issued by the DIN. The text of this
international standard has been translated into Arabic so as to be
approved as a Saudi standard without introducing any technical
modification.

Introduction

See Explanatory notes for connection with International Standard ISO

1628:1984, published by the International Organization for
Standardization (ISO).
This standard assumes knowledge of DIN 51562 Part 1. The information
provided therein regarding the designation of the viscometer and the
general test procedure is not repeated in the present standard.
SAUDI STANDARD SASO DIN 51562-3: 2016

Determination of kinematic viscosity using the Ubbelohde viscometer

– Part 3: Viscosity relative increment at short flow times

1. Scope and field of application

DIN 51562 Part 1 specifies a minimum flow time of 200 s for the volume
between the filling marks, as in almost all standards dealing with capillary
viscometers.
Even greater flow times are specified for cases where the Hagenbach
correction at 200 s is not negligibly small.
The specification of minimum flow times leads to difficulties in fields
where short flow times have in practice been customary and required.
When frequent measurements are made in practice, flow times for pure
solvents of above 200 s are too long, especially when determining the
Staudinger function (viscosity number, see clause 2) of polymer solutions
(e.g. in accordance with the DIN 53728 standard series), since the flow
times of the solutions are even higher and, additionally, there are
difficulties in the handling of the capillaries.
Experience has shown that for such measurements it is better to operate
with wider capillaries and shorter flow times.
This standard specifies a method of determining and applying the
Hagenbach correction, which is essential at low viscosities and short flow
times, and offers, together with experimental instructions, a uniform
working base.
2. Concepts (see also DIN 1342)
The viscosity relative increment is defined by

(1)
where
 is the viscosity of the solution;
s is the viscosity of the solvent;
x is the viscosity ratio.
When the viscosity relative increment is related to the concentration by
mass of the substance dissolved in the solution, βi, the concentration-
related viscosity relative increment, Jv, called Staudinger function
(viscosity number), is obtained.

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SAUDI STANDARD SASO DIN 51562-3: 2016

(2)
The concentration by mass, βi , is mostly expressed in g/cm3, the
Staudinger function, Jv, in cm3/g.
3 Calculation of viscosity relative increment and Staudinger function
From flow times measured by the Ubbelohde viscometer, the kinematic
viscosity, v, which is the ratio of dynamic viscosity,  , to density ,ϱ, is
immediately obtained.
Provided that the differences in density between the solvent and the
solution are small, Jv can be calculated from the ratio of the kinematic
viscosities or that of flow times which are proportional to these
viscosities.

(3)
where
t is the flow time of the solution;
ts is the flow time of the solvent.
Only flow times corrected in accordance with clause 5 shall be used for t
and ts in equation (3), not the flow times measured.
4 Hagenbach correction
If the actual flow time is shorter than the minimum flow time tG1 specified
in DIN 51562 Part 1, the individual values for the Hagenbach correction,
ΔtHi , are to be determined for every capillary viscometer using suitable
standard liquids of known viscosity, as follows:

(4)
where
tgi is the flow time measured using the standard liquid, i;
vi is the kinematic viscosity of the standard liquid;
K is the apparatus constant of the viscometer.
In accordance with DIN 51562 Part 1, the flow times and the Hagenbach
corrections shall be expressed in s, the kinematic viscosities in mm2/s )*
and the apparatus constants in mm2 /s2.
By linear interpolation between the values of ΔtH1 and ΔtH2 determined for
the two standard liquids i = 1 and i = 2 having flow times tg1 and tg2
respectively, the Hagenbach correction ΔtH shall be calculated for another
flow time, tg , using equations (5) and (6) (see also figure 1):

)* Previously centistokes (cSt); 1 cSt= 1 mm2/s.

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SAUDI STANDARD SASO DIN 51562-3: 2016

(5)

(6)
Flow time tg shall lie between flow times tg1 and tg2.

Curve a- correction equation (3) as in DIN 51652 , Part 1(validity range d)

Curve b -true form of the individual Hagenbach correction
Curve c - straight line to be interpolated from equation (5); it intersects
curve bat points.

Figure 1. Example of the individual Hagenbach correction for an

Ubbelohde viscometer No. Oc in accordance with DIN 51562 Part 1
Figure 1 represents an example of a typical form of the individual
Hagenbach correction for an Ubbelohde viscometer No. Oc in accordance
with DIN 51562 Part 1, in which the transition from the capillary to the
suspended level is funnel-shaped.

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SAUDI STANDARD SASO DIN 51562-3: 2016

5 Correction of the measured flow times

To determine the Staudinger function (viscosity number) by equation (3),
the measured flow times of the solvent, tgs, and the solution, tg , shall be
corrected using the Hagenbach correction in accordance with clause 4 (see
equations 7 and 8).

t=tg -ΔtH (7)

ts=tgs -ΔtHs (8)
where the subscript s represents the solvent.
6 Limitation of correction method
For Ubbelohde viscometer No. 0 in accordance with DIN 51562 Part 1,
the method is applicable for the shortest flow times attainable in practice.
For all other viscometers, attention shall be paid in cases of short flow
times (see table 1) to disturbances which announce the imminent collapse
of the suspended level. Figure 2 illustrates these disturbances in a
simplified form.

Table 1. Limiting values of the measured flow time, tg , and the

Reynolds number, Re, in accordance with DIN 53012, up to which
generally no suspended level disturbances occur

Ubbelohde viscometer as in No.

DIN 51562 Part 2 0c oa I Ic
Limiting value of tg , in s 100 75 60 60
Corresponding Reynolds number Re 500 500 300 100
Note. In some viscometers, the disturbances can occur even at slightly
longer flow times, although the visual examination of the lower end of the
capillary does not suggest such disturbances.

7 Apparatus and reagents

The following apparatus and reagents shall be used.
7.1 Ubbelohde viscometer with suspended level in accordance with DIN
51562 Part 1. For measuring polymer solutions, viscometers shall be used
for which the surface tension correction is sufficiently small (see also
Explanatory notes). Viscometers with a lower capillary end, which is
either sharp-edged or funnel shaped, may also be used.
To reduce uncertainty of measurement, automatic measuring devices for
the determination of flow times shall preferably be used. Determination of
the Hagenbach correction shall be carried out in the same order as the
tests.

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SAUDI STANDARD SASO DIN 51562-3: 2016

7.2 Thermometer in accordance with DIN 51562 Part 1.

a) Undisturbed flow, measurement is usable

b) Commencement of a disturbance at an excessively high flow rate
c) Progress of the disturbance at an even higher flow rate Measurement
d) Collapse of the suspended level cannot be used

Figure 2. Formation of the suspended level

The illustration shows the liquid alone without the glass wall of the
viscometer enclosing it .
7.3 Constant-temperature liquid circulator as specified in DIN 12879 Part
1, capable of maintaining the test temperature constant to within 0,01 °C.
See DIN 51562 Part 1 for further details.
7.4 Timing device with an uncertainty of measurement of 0,02 s. The time
base of the electronic measuring device shall be constant to 10-4 and shall
correspond to the nominal value.
7.5 Two to three low-viscosity standard liquids (see Explanatory notes)
covering a range of kinematic viscosity which includes the kinematic
viscosities of the solutions to be tested. The values of the ratio of surface
tension to density of the standard liquids and of the solvent shall differ by
less than 2 cm3 /s2 .
7.6 A solvent (not a mixture, if possible) of an agreed degree of purity,
suitable for preparing the solution to be tested shall be used. The surface
tension and density at the test temperature shall be known. The use of one
of the standard liquids as solvent is very advantageous.
8 Preparation of measurement
8.1 Preparation of viscometer
The apparatus constant, K, shall be determined in compliance with the
specifications given in DIN 51562 Part 1.

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SAUDI STANDARD SASO DIN 51562-3: 2016

The experimental determination of the Hagenbach correction as specified

in clause 4 using standard liquids (see subclause 7 .5) is to be considered a
special case of calibration of the viscometer for the field of application of
this standard.
8.2 Preparation of samples
The pretreatment of the sample supplied and the preparation of the
solution are governed by the relevant standards or they are to be agreed
upon.
The test solution shall be free from undissolved constituents. The agreed
concentration by mass, βi , at the agreed preparation temperature of the
solution shall be kept to 0,1 %.
The use of filters (folded filters, fritted glass filters) in the filling of the
viscometer reduces the risk of disturbances due to particles suspended in
the liquid. When charging the viscometer through the filter, the first 10 ml
shall be discarded in order to avoid fluctuations in its concentration.
9 Procedure
The measurement of flow times tgs (solvent) and tg (test solution) shall be
carried out using the same viscometer.
For this purpose, the capillary with the most suitable diameter shall be
selected. The measurement shall be carried out as specified in DIN 51562
Part 1.
The flow times of the pure solvent shall be measured using a liquid taken
from the same container as the liquid used for preparing the solutions.
The number of measurements carried out on one and the same viscometer
charge shall be not less than 3 and, because of solvent evaporation, not
more than 5. If the flow times differ by more than 0,1 % within this
measurement series, this may be due to external influences.
In such a case, the measurement shall be repeated after cleaning the
viscometer.
Note. Disturbances due to solvent evaporation are more readily prevented
if pressure rather than suction is applied.
10 Inter-laboratory testing
When inter-laboratory tests of the viscosity relative increment are to be
carried out on the same substances, the conditions specified in subclauses
10.1 to 10.3 shall be observed.
10.1 Sampling
All laboratories shall proceed in compliance with the same specifications
for, or agreements on, the substances to be tested in respect of
a) sampling,
b) sample preparation,
c) solution preparation.

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SAUDI STANDARD SASO DIN 51562-3: 2016

10.2 Procedure
All laboratories shall observe the following standard test conditions:
a) agreed type of viscometer type in accordance with DIN 51562 Part 1;
b) agreed solvent (degree of purity and composition);
c) agreed concentration of the substance to be tested;
d) agreed test temperature;
e) application of the Hagenbach correction in accordance with this
standard using the same standard liquids.
1 0.3 Expression of result
The test result shall include the following information:
a) identification of sample and its preparation in accordance with
subclause 10.1 ;
b) test parameters in accordance with subclause 1 0.2;
c) relative viscosity and/or the Staudinger function (viscosity number) in
compliance with the specifications relating to the test report covering the
substance tested;
d) specifically agreed details, e.g. information concerning the apparatus
constant, form of the lower end of capillary (sharp-edged or funnel-
shaped); type of determination of flow times (manual or automatic).
11 Precision
The precision cannot be characterized by values specified in DIN 51562
Part 1. Irrespective of the inherent uncertainty of measurement caused by
the samples themselves, these values are increased by:
a) higher relative variations when measuring short flow times;
b) the procedure of determining the difference between solution and
solvent flow times when calculating the viscosity relative increment (see
Explanatory notes);
c) the uncertainty of the Hagenbach correction.

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SAUDI STANDARD SASO DIN 51562-3: 2016

Standards referred to
DIN 1342 Part 2 Viscosity of Newtonian liquids
DIN 12879 Part 1 Electrical laboratory apparatus; constant-temperature
liquid circulators; general and safety requirements, testing
DIN 51562 Part 1 Viscometry; determination of kinematic viscosity using
the standard design Ubbelohde viscometer
DIN 53012 Viscometry; capillary viscometry of Newtonian fluids;
sources of errors and corrections
DIN 53728 Testing of plastics; determination of viscosity of solutions

Other documents
[1] Bauer, H.; Meerlender, G. Precise viscosity measurements of
Newtonian liquids with v < 1 mm2/s for the selection of suitable standards.
Rheol. Acta 23 (1984), pp. 514 to 521.

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Explanatory notes
This standard has been prepared by NMP 831 Technical Committee
Viskosimetrie because it was felt that ISO 1628-1984, Guidelines for the
standardization of methods for determination of viscosity number and
limiting viscosity number of polymers in dilute solution. Part 1: General
conditions, dealing with the same range of problems, did not offer an
adequate solution of the problems involved. According to ISO 1628, the
Hagenbach correction, ΔtH , should not exceed 3% of flow time tg ; the
correction is neglected. This may result in an uncertainty of measurement
of the viscosity number of 4% to 6 %. Since in many cases the change in
viscosity number over the whole manufacturing range of a product is less
than 10 %, this limit of error is considered too high.
The Ubbelohde viscometers referred to in ISO/R 1628 do not correspond
to those specified in DIN 51562 Part 1, but to Ubbelohde viscometers
specified in International Standard ISO 3105, Glass capillary viscometers;
specification and operating instructions.
The kinematic viscosities of suitable standard liquids of a defined degree
of purity have been published [1]. For example, for determining the
viscosity of polycarbonate (PC) dissolved in dichloromethane, the
standard liquids specified in table 2 are recommended.
Table 2. Standard liquids used for the experimental determination of
the Hagenbach correction when measuring the viscosity of dissolved
polycarbonate.
Surface
Degree of Measuring Kinematic
Tension/
Substance purity temperature viscosity
oc density
mm2/s
cm3/s2
Dichloromethane Analytical
25.00 0.3142 21.0
grade
Trichloroethylene Analytical
25.00 0.3693 20.0
grade
Tetrachloroethylene Analytical
25.00 0.5257 18.5
grade

differ only slightly from each other. This is the reason why some
deviations have a significant influence on the final result , as illustrated in
the following example of calculation. In an Ubbelohde viscometer No. Oc
in accordance with DIN 51562 Part 1, having an apparatus constant, K, of
0,003201 and being provided with a funnel-shaped lower capillary end,
the measured flow time tgs is 103,46 s and tg is 127,18 s. The differences
in density between the solution and the solvent should be negligibly small.
After the individual Hagenbach correction has been applied, the corrected
flow times are t = 122,48 s and ts = 97,90 s. It follows that the relative
viscosity is 1,2511 and the viscosity relative increment is 0,2511.
Example a): A deviation,t, of + 0,3 s in tg causes a deviation of + 0,24 %
in x, but of + 1,19 % in x -1.

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Example b): Ignoring the Hagenbach correction for solution and solvent
flow times would result in a deviation of - 8,68 % in x -1; the Hagenbach
correction will be 3,7% of the solution flow time and 5,4 % of the solvent
flow time.
Example c): An incorrect value of the apparatus constant, K, only takes
effect indirectly through the Hagenbach correction. If the value taken for
the apparatus constant is too high by 1 %, a deviation in x - 1 of - 0,04%
will result.
The error of capillary rise (see DIN 53012) due to surface tension σ
cannot always be ignored when using Ubbelohde viscometers. If liquids
with widely varying values of the ratio surface tension to density, σ /ϱ,
(see the example of calculation above equation ( 10)) are used for
determining the individual Hagenbach correction as specified in clause 4,
constant K* as defined in equation (9) shall be used in equation (4) instead
of constant K. Since large differences in the ratio of surface tension to
density are mostly caused by large differences in density, the correction
for the buoyancy of the air, 1– ϱL/ϱ , is also to be taken into consideration.

(9)
where
σ0/ϱ0 is a reference value to be chosen as appropriate, ϱL is the density of
air, ϱ is density of the liquid for which constant K* is valid and constant x
is a measure of deviation from the ideal surface tension compensation for
the particular Ubbelohde viscometer in question.
x can be determined from the measurements carried out on two liquids
with the same kinematic viscosity but different values of σ/ϱ .
The following have been found suitable [1]:
a) analytical grade anhydrous acetone at 24,63°C with σ/ϱ = 29 cm3/s2,
v = 0,3850 mm2/s and ϱ = 0,786 g/cm3 ;
b) analytical grade trichloroethylene at 20,00°C with σ/ϱ = 19,5 cm3/s2,
v = 0,3850 mm2/s and ϱ = 1,464 g/cm3.
With σ0/ϱ0 = 29 cm3/s2 x is to be calculated using equation ( 1 0) :

(10)
where
tT is the measured flow time, in s, for trichloroethylene at 20,00°C;
tA is the measured flow time, in s, for acetone at 24,63°C;
K is the uncorrected apparatus constant, in mm2/s2;
x is the correction factor allowing for the surface tension, in s2/cm3.
For viscometer No. Oc, the values of x , determined from equation (10),
frequently lie between - 1 .10-4 s2/cm3 and - 2. 10-4 s2/cm3, but values of

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SAUDI STANDARD SASO DIN 51562-3: 2016

up to - 5.10-4 s2/cm3 have also been observed. For measurements carried

out on polymer solutions (see subclause 7.1), the correction allowing for
surface tension remains sufficiently small, if | x| is less than 2.10-4 s2/cm3.

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