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ICS: 17.060
Foreword
3- Normative references
This Standard incorporates, by dated or undated reference, provisions
from other publications. These normative references are cited at the
appropriate places in the text, and the titles of the publications are listed
below. For dated references, subsequent amendments to or revisions of any
of these publications apply to this standard only when incorporated in it by
amendment or revision. For undated references, the latest edition of the
publication referred to applies.
DIN 1319-1 Basic concepts in metrology - General concepts
DIN 1319-3 Basic concepts in metrology - Evaluating measurements
of a single measurand and expression of uncertainty
DIN 1342-1 Viscosity - Rheological concepts
DIN 51366 Determination of kinematic viscosity of petroleum
products using the Cannon-Fenske viscometer for opaque liquids
DIN 51562-3 Determination of kinematic viscosity using the Ubbelohde
viscometer - Relative change in viscosity at short flow times
DIN 51562-4 Determination of kinematic viscosity using the Ubbelohde
viscometer - Calibration of viscometers and determination of uncertainty of
measurement
DIN 53012 Capillary viscometry of Newtonian liquids - Sources of
error and corrections
DIN 53017 Determination of temperature coefficient of viscosity of
liquids
ISO 3105 : 1994 Glass capillary kinematic viscometers - Specifications
and operating instructions
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SAUDI STANDARD SASO DIN 51562-1: 2016
(1)
Note that equation (1) only applies when the units given in column 4 of
table 1 are used.
The following equations apply to the shear stress and shear rate,
respectively:
(2)
(3)
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5- Measuring range
This method is suitable for measuring kinematic viscosities within a range
of 0,35 to 100000 mm2 /s (see table 2), with flow times ranging from 200 s
to 1000 s at temperatures from 10 °C to 100 °C.
When using the viscometer at temperatures or flow times outside the above
ranges, additional errors of measurement may occur which are not included
in the uncertainty of measurement specified in clause 14.
6- Principle
The viscosity of the test liquid is determined by measuring the time it takes
for the sample, whose volume is defined by two ring-shaped measuring
marks, to flow laminarly through a capillary under the influence of gravity.
As a result of the suspended level, the mean pressure head is independent
of the filling volume, while the influence of surface tension (see DIN
53012) can generally be neglected.
Table 1: Symbols, quantities and units
g
Acceleration due to gravity at the point 2
of m/s
measurement
g`
Acceleration due to gravity at the point 2
of m/s
calibration
K Viscometer constant m2 /s
2
mm2 /s
2
l Capillary length m mm
n Number of single measurements (flow
times) in a measurement series
R Capillary radius m mm
Re Reynolds number
t Flow time s
tmax , tmin
Longest and shortest flow times in a
series of n single measurements s
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ᶹ Kinematic viscosity m2 /s
2
mm2 /s
2
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(4)
For long flow times or greater viscometer sizes, Δt H may be disregarded
(see clause 14).
8- Apparatus
The following apparatus shall be used.
8.1 Ubbelohde suspended level viscometer
The viscometer (see figure 1) shall be made of 3.3 borosilicate glass as in
ISO 3585 and consist of a ventilation tube (1), a capillary tube (2), a filling
tube (3), an upper reservoir (4), a timing bulb (5), a capillary (6) which
opens into the dome (7) of the suspended level bulb (8), an equalization
tube (9) and a lower reservoir (10). The sample to be measured flows
through the suspended level bulb from the capillary as thin film (suspended
level) through the equalization tube back to the lower reservoir.
The ventilation tube shall be attached to the suspended level bulb at a point
that is below the dome and sufficiently remote from the lower end of the
capillary; this will ensure that the axial symmetry of the suspended level is
not disturbed.
The filling marks (MF) indicate the quantity of sample to be poured in,
while the measuring marks (M1 and M2) delineate the sample's flow volume
and determine the mean pressure head. To compensate for the influence of
surface tension, the ratio of the radius of the dome of the suspended level
bulb to that of the timing bulb shall be 0,751 )1. The internal diameter of the
equalization tube shall be large enough for equalization to effectively take
place between the suspended level bulb and the lower reservoir, even in the
case of high-viscosity liquids (i.e. the ventilation tube remains open during
measurement).
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The viscometer design specified here largely conforms to ISO 3105, which
also specifies dimensions that are not of metrological relevance.
As the measuring range of a single viscometer is smaller than the overall
measuring range specified in clause 5, viscometers of various sizes are used
to cover the entire range. These viscometers have different capillary
diameters and, consequently, different constants; see table 2 for viscometer
specifications. The actual viscometer constant shall not deviate from the
values given in table 2 by more than 10 %.
Measuring marks, filling marks, the manufacturer's name, viscometer size
number and an identification number shall be permanently marked on the
viscometer by the manufacturer.
The viscometer shall be held in a fixed position in the bath by means of a
holder equipped with a flat supporting plate at the top. The deviation of the
capillary axis from the normal of this supporting plate shall not exceed 1 °
(see subclause 8.4).
8.4 Temperature measuring device
The device used to determine the temperature in the constant-temperature
bath shall allow the measurement to be carried out with an uncertainty of
0,02 °C.
NOTE: These requirements are fulfilled, for example, by calibrated liquid
glass thermometers having scale intervals of 0,01 °C and a freezing point
marking, with regard to the correction for the difference between the
immersion depth during calibration and that during measurement. For
greater accuracy, calibrated platinum resistance thermometers are suitable.
The temperature shall be measured as near as possible to the viscometer so
that the requirements stipulated in subclause 8.4 are fulfilled. The
temperature sensor should be immersed to a depth that is 2/3 the depth of
immersion of the viscometer and equal to the depth of immersion during
calibration or verification. Adjustments shall be made, if necessary.
The temperature measuring device shall be recalibrated or reverified at
intervals appropriate for the type of thermometer and the operating
conditions.
8.3 Timing device
The flow time can be measured using a timer (e.g. electronic stopwatch),
by observing the passage of the meniscus, or by using an automatic timing
device (cf. subclause 8.5). The smallest scale interval or digital increment
displayed shall be no greater than 0,01 s and the relative uncertainty of the
time measurement shall not exceed 0,02 %.
NOTE: These requirements are fulfilled by a calibrated timer having a
smallest scale interval or digital increment of 0,01 s.
The timer shall be recalibrated or reverified at intervals appropriate for the
type of timer and the operating conditions.
8.4 Constant-temperature bath
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2)
The plate may be adjusted by means of adjustment screws, and horizontality may be checked with a
spirit level.
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figure 1. Then, suspend the viscometers in the bath, ensuring that the
surface of the bath liquid is about 20 mm above the top of the upper
reservoir.
If the viscometers have not been assigned to specific holders during
calibration, and appropriate markings made, check the vertical position of
the capillary, using a plumb line, for example. The deviation from the
vertical in two planes normal to each other, measured along the entire length
of the capillary, shall be no greater than 2 mm.
After placing the viscometer in the bath, wait until the bath and test liquid
temperatures reach equilibrium. Experience has shown that this requires
about 20 minutes.
Once equilibrium has been reached, close the ventilation tube and bring the
sample to the top rim of the upper reservoir by applying suction to the
capillary tube or pressure to the filling tube. If suction is applied, take
special care to ensure that the liquid is drawn up slowly enough to prevent
any evaporation of components or degassing of the sample.
On completing this operation, open the tubes again. The liquid column will
then break away at the lower end of the capillary and the 'suspended level'
will form.
To prevent a delay in the formation of the suspended level due to liquids
entering the ventilation tube (this can happen especially when highly
viscous liquids are forced upwards), first open only the ventilation and
filling tubes and wait until the suspended level has formed; then, open the
capillary tube to perform the measurement.
Measure the time (flow time) it takes for the lower edge of the sample
meniscus to fall from the upper edge of measuring mark M1 to the upper
edge of measuring mark M2, then wait for the liquid to stop running out of
the capillary.
With each viscometer, carry out at a series of at least three valid
measurements of flow times for one filling. If the flow times are less than
400 s, carry out five or more measurements. If the first flow time deviates
significantly from the subsequent ones, regard it as a trial test, discard it and
make an additional flow time measurement. A deviation is deemed to be
'significant' if the limit value for £t (see equation (7)) is exceeded when the
first flow time is considered, but is not exceeded when this first time is
disregarded.
13 Evaluation
13.1 Kinetic energy correction
For viscometers of sizes 0 to Ia, the measured flow time shall be corrected
by ΔtH , the kinetic energy correction (also called the 'Hagenbach
correction'), as shown in equation (4). ΔtH shall be taken from either the
manufacturer's specifications or the calibration certificate (cf. DIN 51562-
4).
Correction is not necessary if an increased uncertainty of measurement is
permitted (see subclause 14.3).
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(6)
whereby the following condition is to be fulfilled
εt ≤ 2. 10 -3 (7)
Calculate the kinematic viscosity for each viscometer using equation (4),
and then establish the mean of the two viscosities
(8)
as well as the relative difference between the two measured viscosities
(9)
whereby the following condition is to be fulfilled
εv ≤ 2. 10 -3 (10)
If conditions (7) and (10) are fulfilled, n is the kinematic viscosity of the
sample. If condition (7) is not fulfilled even after repeating the
measurement, the determination shall be repeated with another viscometer.
If condition (10) is not fulfilled even after repeating the measurement, the
viscometer constants shall be checked (see clause 9) and, if necessary, the
viscometers recalibrated.
14. Uncertainty of measurement
14.1 Calculation of relative uncertainty of measurement
Equation (11)
(11)
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The relationship between u'v and u'K is shown in table 3 for several
viscosities and for measurements involving one or two viscometers.
For calibrated viscometers, u'v is either to be taken from the calibration
certificate or determined as specified in DIN 51562-4.
If measurement is carried out with only one viscometer, the relative
uncertainty of measurement is given by .
(12)
This yields the values given in column 3 of table 3, which shall also be used
if two viscometers are used, but only one thermometer. In such cases,
however, it shall be ensured that results will not be falsified by residual
contamination of the capillary, by particles present in the test liquid, or by
other effects.
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14.2 Reproducibility
The results of two measurements carried out in accordance with this
standard under reproducibility conditions are considered to be in agreement
if their relative difference is
(13)
NOTE: If the results obtained by two different laboratories under
reproducibility conditions meet the requirements specified in subclause
14.1, and if the relative uncertainty of the viscometer constants, u'K, does
not exceed 0,4 %, both results shall be considered acceptable if the relative
difference does not exceed 0.4 % related to the mean of the results.
14.3 Increased uncertainty
If a kinetic energy correction is not made, the uncertainty of measurement
for viscometers of sizes 0 to I (determined using equation (11)) shall be
increased by the value given in table 4.
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