Vous êtes sur la page 1sur 17

SASO DIN 51562-1:2016

DIN 51562-1: 1999

Determination of kinematic viscosity using the Ubbelohde


viscometer – Part 1: Apparatus and measurement procedure

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 51562-1: 1999 “Determination of
kinematic viscosity using the Ubbelohde viscometer – Part 1: Apparatus
and measurement procedure” 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.
SAUDI STANDARD SASO DIN 51562-1: 2016

Determination of kinematic viscosity using the


Ubbelohde viscometer – Part 1: Apparatus and measurement
procedure

1- Scope and field of application


This standard specifies the design and use of Ubbelohde suspended level
viscometers with ring measuring marks that indicate the flow volume. Such
viscometers are used to determine the kinematic viscosity of Newtonian
liquids that are sufficiently transparent to enable the meniscus of the liquid
to be observed during measurement.
NOTE: Special automatic measuring devices also allow viscosity
measurements of opaque liquids (cf. DIN 51366).

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

1
SAUDI STANDARD SASO DIN 51562-1: 2016

ISO 3585 : 1991 Borosilicate glass 3.3 - Properties


ASTM D 2162-79 Standard method of basic calibration of master
viscometers and viscosity oil standards
3. Concepts
The following concepts apply, in addition to those defined in DIN 1319-1
and DIN 1342-1.
3.1 Viscosity Standard
A material measure or measuring device which represents the viscosity unit
(e.g. when calibrating a viscometer).
3.2 Standard viscometer
For the purposes of this standard, an Ubbelohde capillary viscometer that
is traceable to the national viscosity standard.
NOTE: See subclause 8.1 for a description of the Ubbelohde viscometer.
3.3 Standard Newtonian liquid
A Newtonian liquid whose change in viscosity with time is sufficiently
small so that it is suitable as a viscosity standard.
3.4 Standard viscosity sample
A sample of a standard Newtonian liquid whose viscosity has been
measured and recorded at one or more temperatures using standard
viscometers; the traceability of the viscosity values thus obtained to the
national viscosity standard shall have been documented. This sample can
thus be used as a material measure.
4 Symbols and units
See tables 1 and 2 for symbols and units used in this standard.
For the purposes of this standard, the Reynolds number, Re, is given by (1):

(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)

2
SAUDI STANDARD SASO DIN 51562-1: 2016

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

Symbol Quantity SI unit Other legal


units
)1 Shear rate at the internal wall of
s-1
capillary
(for Newtonian liquids)

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

hm Mean pressure head m mm

k Coverage factor (cf. DIN 1319-3)

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

Relative uncertainty of viscosity

3
SAUDI STANDARD SASO DIN 51562-1: 2016

Relative uncertainty of viscometer


constant

Uv Temperature coefficient of kinematic K-1 cm3


viscosity

V Flow volume m3 cm3


Δt H Kinetic energy correction s

εt Relative difference of flow times in a


series of measurements using one
viscometer
εv Relative difference between viscosities
measured with two viscometers

ᶹ Kinematic viscosity m2 /s
2
mm2 /s
2

ᵨ Density of liquid Kg/m 3 g/cm3


Shear stress at internal wall of capillary Pa

1) Dw may also be used instead of .

Table 2: Guideline values for viscometer dimensions and specifications


Interna Viscome
l Flow ter
diamet volume constant Measuring range, Re for a for a for
Viscomete er of , , ᶹ, flow flow time ᵨ=1
r size no. capillar V, K, time of 200 s, g/cm3,
y, in mm2/s of 200 s in s-1
in cm3 in in Pa
in mm mm2/s2

0 0.36 5.7 0.001 0.35 to 1 500 6200 1.3

0c 0.47 5.7 0.003 0.7 to 3 130 2800 1.7

0a 0.53 5.7 0.005 1 to 5 70 1900 1.9

I 0.63 5.7 0.01 2 to 10 30 1100 2.2

Ic 0.84 5.7 0.03 6 to 30 7 500 3.0

.Ia 0.95 5.7 0.05 10 to 50 4 340 3.4

II 1.13 5.7 0.1 20 to 100 1.6 200 4.0

IIc 1.50 5.7 0.3 60 to 300 0.40 90 5.3

IIa 1.69 5.7 0.5 100to 500 0.21 60 60.

III 2.01 5.7 1 200to1000 0.09 36 7.1

4
SAUDI STANDARD SASO DIN 51562-1: 2016

IIIc 2.65 5.7 3 600to3000 0.023 16 9.4

IIIa 3.00 5.7 5 1000to5000 0.012 11 10.6

IV 3.60 5.4 10 2000to10000 0.005 0.4 12.8

IVc 4.70 5.7 30 6000to30000 0.001 2.8 16.6

Iva 5.34 5.7 50 10000to50000 0.0007 1.9 18.9

V 6.3 5.7 100 20000to100000 0.0003 1.2 23.2

7- Theoretical basis of method


The method is based on the following equation derived from the Hagen-
Poiseuille law, taking account of the kinetic energy correction (also known
as the 'Hagenbach correction'; see DIN 53012):

(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).

)1See ASTM D 2162-79.

5
SAUDI STANDARD SASO DIN 51562-1: 2016

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

6
SAUDI STANDARD SASO DIN 51562-1: 2016

An automatically-controlled constant-temperature bath shall be used which


is preferably capable of accommodating several viscometers
simultaneously. The top plate of the bath (used to support the upper plate
of the viscometer holder) shall be flat, i.e. it shall not deviate more than 1°
from the horizontal )2 . The temperature of the bath liquid shall not vary by
more than 0,02 °C during measurement.
During the measurement, the temperature over the length of the viscometer
shall not differ by more than 0,01 °C from the measured bath temperature.
NOTE: This can be checked, for example, by determining the temperature
distribution in the bath - with the viscometer(s) in it - using a sufficiently
sensitive temperature sensor that has been calibrated against the
thermometer used to measure the bath temperature.
The bath shall be protected from direct sunlight or direct artificial light,
since this may falsify the temperature reading. The thermometer and bath
shall therefore be illuminated by low-radiation fluorescent tubes.

2)
The plate may be adjusted by means of adjustment screws, and horizontality may be checked with a
spirit level.

7
SAUDI STANDARD SASO DIN 51562-1: 2016

Figure 1: Ubbelohde viscometer (schematic)


8.5 Automatic measuring device
The automatic measuring device used shall have a constant that has been
determined by calibration. In this case, the measuring marks are optional,
although any marks provided shall not interfere with the automatic
detection of the passage of the meniscus.
When using viscometers with ring marks, bear in mind that the viscometer
constant referring to measurements made with the ring marks differs from
that referring to automatic measurements. The latter is only valid when the
automatic device is used for calibration.
Automatic measuring devices that are also capable of automatically
draining the old sample, cleaning the viscometer, and filling it with the new
sample - and which thus have an additional rinsing tube - deviate from the
viscometer design specified in subclause 8.1. Such devices may only be
used if steps are taken to ensure that the cleaning of the viscometer does not
affect the validity of the constant.

8
SAUDI STANDARD SASO DIN 51562-1: 2016

The uncertainty of measurement specified in clause 14 applies to


measurements made with automatic measuring devices only if they fulfil
the requirements specified above for non-automatic viscometers.
9. Viscometer calibration
Calibration shall be performed as specified in DIN 51562-4 by means of
comparison with standard viscometers or by determining the viscometer
constants using viscosity standards of Newtonian liquids. The user may
perform calibration, but only if defined measuring conditions are
maintained. In this case, the uncertainties of the viscometer constants shall
be calculated as specified in DIN 51562-4 on the basis of the uncertainties
for various influence quantities.
The interval between recalibrations will depend on the nature of the
viscometer, its use, and the properties of the liquid to be measured; this
interval shall be no greater than five years. For automatic measuring
devices, the interval between recalibrations shall not exceed one year, and
the viscometer constants should be checked between calibrations. A
particularly simple way of doing this is to place calibrated viscometers with
measuring marks in the automatic measuring device. The flow time is then
visually determined, with the help of a stopwatch, at the same time as
automatic determination (direct comparison). The constant of the automatic
measuring device is calculated from the viscosity determined visually and
the automatically measured flow time.
NOTE: If measurements are made on products which may leave deposits
and thus influence the viscometer constant, the viscometer shall be checked,
cleaned (if necessary; cf. subclause 11.3 b)) and then recalibrated at shorter
intervals.
10 Sampling
Sampling and sample preparation shall be according to the relevant
regulations or standards for the liquid to be measured. Depending on the
viscometer size, about 15 to 20 ml of liquid will be needed per filling.
11 Preparations for measurement
11.1 Sample preparation
A sample prepared as in clause 10 will not require further treatment. High-
viscosity liquids may be warmed to facilitate filling, provided this does not
result in any change in the liquid's viscosity at the test temperature.
NOTE: For measurements near the solidification point of the liquid or of
one of its components, non-Newtonian behaviour can be expected.
Unless specified, the sample shall only be filtered if particles present in it
may affect the measurement. In such cases, a note to this effect indicating
the pore size of the filter used shall be included in the test report.
When handling hazardous substances, regulations governing work safety
and the disposal of dangerous material shall be observed.

9
SAUDI STANDARD SASO DIN 51562-1: 2016

11.2 Selection of viscometer


Preferably, two viscometers of the same size number shall be selected so
that the flow time is at least 200 s (see DIN 51562-3 if the flow time is
shorter). The use of two viscometers also makes it possible to detect nearly
invisible contamination of a viscometer by comparing the measurement
results (see equation (10)).
11.3 Cleaning viscometers
The viscometer(s) shall be cleaned immediately after each measurement. If
the last measurement took place some time ago, the viscometer shall be
cleaned again prior to measurement. Cleaning shall be performed in such a
manner that the viscometer constant found during calibration is still valid.
In case of doubt, the viscometer
shall be checked using a standard viscosity sample.
a) Cleaning normally contaminated viscometers
Rinse the viscometer repeatedly with a suitable solvent. For instance, when
the viscometer is contaminated with mineral oil or a similar fluid, rinsing
with filtered special boiling-point spirit (SBP spirit) is suitable. The
volatility and purity of the solvent used for the final rinse shall be sufficient
to ensure that no residue is left after drying.
Drying shall be carried out by blowing or using suction to force a dry, dust-
free air stream through the viscometer tubes and/or by placing the
viscometer in an oven or vacuum desiccator for an appropriate time.
If the contamination is due to water-soluble substances, cleaning may be
carried out with demineralized or distilled water.
b) Cleaning heavily contaminated viscometers
The viscometer shall first be cleaned as specified in the first paragraph of
item a) above. It shall then be filled with a chromosulfuric acid cleaning
mixture and left at room temperature for two to three hours, after which it
shall be rinsed thoroughly with demineralized or distilled water several
times and dried as specified in the second paragraph of item a).
Depending on the type of contamination, cleaning with chromosulfuric acid
may be supplemented by cleaning with hydrochloric acid.
Other cleaning agents are permissible if they achieve the same result,
although strongly alkaline cleaning agents may not be used.
NOTE: The determination of the viscosity of silicone oils renders the glass
surface hydrophobic, especially at fairly high temperatures, and this may
result in a change in the viscometer constants. Such viscometers shall be
regarded as heavily contaminated and will require a particularly thorough
cleaning.
12 Procedure
Place the viscometers in suitable holders (e.g. those supplied by the
viscometer manufacturer) and set the bath to the test temperature. Pour
enough sample liquid into each viscometer through the filling tube so that
the liquid level of the sample is between the two filling marks (MF); see
10
SAUDI STANDARD SASO DIN 51562-1: 2016

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).

11
SAUDI STANDARD SASO DIN 51562-1: 2016

13.2 Calculating viscosity


For each series of measurements, calculate the mean flow time
(5)
and the relative difference between the longest and shortest flow
times

(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)

may be used to calculate the relative uncertainty of measurement, u'v, as


a function of the relative uncertainties of the viscometer constants, u'K,
that have been determined as in DIN 51562-4, provided the following
assumptions hold:
- Two capillary viscometers as specified in this standard are used which
have been calibrated as specified
in DIN 51562-4, each having its own thermometer.
- The method and conditions of measurement conform to this standard.

12
SAUDI STANDARD SASO DIN 51562-1: 2016

- Kinetic energy correction is not necessary.


- The temperature coefficient, Uv, of the kinematic viscosity of the test
liquid determined as in DIN 53017 does not exceed 0,1 K-1.
Equation (11) is valid for a coverage factor, k, of 2 (this corresponds to
a confidence level of about 95 %) and represents the most unfavourable
case where n is 3 and εt is 2 .10-3.

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.

Table 3: Relative uncertainty of measurement of the viscosity, u'v ,as a


function of the relative uncertainty, u'k, of the viscometer constants
for determinations made with one or two viscometers
u'v, for measurements using
u'k
2 viscometers 1 viscometers

2 .10 -3 3.5 .10 -3 4.3 .10 -3

4 .10 -3 4.8 .10 -3 5.5 .10 -3

6 .10 -3 6.6 .10 -3 7.1 .10 -3

8 .10 -3 8.4 .10 -3 8.6 .10 -3

1 .10 -2 1.04 .10 -2 1.07 .10 -2

1.5 .10 -2 1.52 .10 -2 1.55 .10 -2

2 .10 -2 2.02 .10 -2 2.04 .10 -2

13
SAUDI STANDARD SASO DIN 51562-1: 2016

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.

Table 4: Increase in the uncertainty of measurement when kinetic


energy correction is neglected
Uncertainty of measurement
Increased by
Viscometer size
no. 2 % for flow times,
3 %for flow times,
in s in s,

0 From 700 to 1000 From 350 to below 700

0c From 400 to 800 From 200 to below 400

0a From 300 to 600 From 200 to below 300

I From 200 to 400

15- Test report


A test report shall be drawn up which shall include at least the following
information:
a) sample identification;
b) measurement temperature;
c) kinematic viscosity, in mm2/s;
d) uncertainty of the kinematic viscosity, determined as in clause 14;
e) the number of viscometers used for measurement;
f) a reference to this standard;
g) date of measurement;

14
SAUDI STANDARD SASO DIN 51562-1: 2016

h) any special observations (e.g. a systematic change in the flow time


during repeat determinations).

15

Vous aimerez peut-être aussi