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ISO 2012 All rights reserved

Document type: International Standard


Document subtype:
Document stage: (20) Preparatory
Document language: E

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Version 2.4e - RC2

ISO/TC 256/SC N
Date: 2012-06-04
ISO/WD 8780-7
ISO/TC 256/SC /WG 6
Secretariat: DIN
Methods of dispersion for assessment of dispersion characteristics
Part 7: Dispersion in a low-viscosity binder system using an oscillatory
shaking machine


Warning
This document is not an ISO International Standard. It is distributed for review and comment. It is subject to
change without notice and may not be referred to as an International Standard.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of
which they are aware and to provide supporting documentation.
ISO/WD 8780-7
ii ISO 2012 All rights reserved

Copyright notice
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ISO/WD 8780-7
ISO 2012 All rights reserved iii

Contents Page
Foreword ............................................................................................................................................................ iv
Introduction ...................................................................................................... Fehler! Textmarke nicht definiert.
1 Scope ...................................................................................................................................................... 1
2 Normative references ............................................................................................................................ 1
3 Apparatus ............................................................................................................................................... 1
4 Binder system ........................................................................................................................................ 3
5 Sampling................................................................................................................................................. 3
6 Millbase................................................................................................................................................... 3
6.1 Composition of the millbase ................................................................................................................ 3
6.2 Volume of the millbase ......................................................................................................................... 3
7 Volume of the grinding beads .............................................................................................................. 4
8 Procedure ............................................................................................................................................... 4
8.1 Filling the container .............................................................................................................................. 4
8.2 Dispersion .............................................................................................................................................. 4
8.3 Stabilization of the millbases ............................................................................................................... 4
8.4 De-aeration of millbases ....................................................................................................................... 4
9 Precision................................................................................................................................................. 5
10 Test report .............................................................................................................................................. 5

ISO/WD 8780-7
iv ISO 2012 All rights reserved

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 8780-7 was prepared by Technical Committee ISO/TC 256, Pigments, dyestuffs and extenders.
ISO 8780 consists of the following parts, under the general title Methods of dispersion for assessment of
dispersion characteristics:
Part 1: Introduction
Part 2: Dispersion using an oscillatory shaking machine
Part 3: Dispersion using a high-speed impeller mill
Part 4: Dispersion using a bead mill
Part 5: Dispersion using an automatic muller
Part 6: Dispersion using a triple-roll mill
Part 7: Dispersion in a low-viscosity binder system using an oscillatory shaking machine
WORKING DRAFT ISO/WD 8780-7

ISO 2012 All rights reserved 1

Methods of dispersion for assessment of dispersion
characteristics Part 7: Dispersion in a low-viscosity binder
system using an oscillatory shaking machine
1 Scope
This International Standard specifies a dispersion method that serves in combination with the assessment
methods ISO 8781-1 and ISO 8781-2 to assess the dispersion characteristics of pigments in low viscosity,
liquid media mostly solvent-borne for grinding in bead mills, sand mills, etc., if necessary also with dissolvers.
The advantages of the shaking machine used for evaluation of dispersion are:
small millbases can be used;
simultaneously dispersion of more than one millbase under the same apparatus conditions.
By this method it is possible to assess the dispersion of multiple pigment samples in the same binder system,
however, it is not recommended for optimizing the millbase composition, i.e. the search for an optimum ratio
of pigment : binder : solvent. This is not the intention of this International Standard.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 2431, Paints and varnishes Determination of flow time by use of flow cups
ISO 8780-2, Pigments and extenders Methods of dispersion for assessment of dispersion characteristics
Part 2: Dispersion using an oscillatory shaking machine
ISO 8781-1, Pigments and extenders Methods of assessment of dispersion characteristics Part 1:
Assessment from the change in tinting strength of coloured pigments
ISO 8781-2, Pigments and extenders Methods of assessment of dispersion characteristics Part 2:
Assessment from the change in fineness of grind
ISO 15528, Paints, varnishes and raw materials for paints and varnishes Sampling
3 Apparatus
Ordinary laboratory apparatus and glassware, together with the following:
3.1 Shaking machine
in which the containers are subjected to 660 ( 40) reciprocating strokes per minute.
The containers with the millbases are fixed to the table of the shaking machine, which is set in motion driven
by an eccentric drive. The oscillating geometry is oval in vertical direction and moves from rear to front.
3.2 Holder
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consists of two horizontal plates, one on top of the other, which can be adjusted to the desired height.
The containers are sandwiched between these plates. It is advised to fix the containers by means of a jar
holder.
To avoid displacement of the containers if not securely tightened and prevent breaking (esp. with glass
bottles) it is advised, to put a rubber sheet between the metal plate and the millbase container and another
sheet under the jar holder.
The metal plate of the holder has a size of 325 mm wide and 330 mm long.
The position of the container has no influence on the degree of dispersion. However, if temperature
differences depending on the position of the container are observed (see 3.5), the efficiency of dispersion in
the containers can be different.
3.3 Containers
of a suitable type
For comparative evaluations, shape and size of the containers as agreed upon by the parties involved shall be
identical.
NOTE Suitable are glass bottles up to 400 ml with twist off caps lined with polyethylene. If agreed upon, smaller glass
bottles with screw caps (with PE liners) or PE bottles may be used.
3.4 Grinding beads
of a suitable type
Type and size of the grinding beads shall be identical if two of more tests will be compared and should be
agreed upon between the parties.
NOTE Suitable are glass beads with a diameter of (3 +/- 0.5) mm and a density of (2,6 +/-) g/cm
3
. If agreed upon,
also zirconium- or steel beads or glass beads with different diameters can be used. New, unused beads shall be
conditioned by shaking them in a mill base (see clause 6) for approximately 60 min, sieved and cleaned prior to the use for
comparative testing.
3.5 Cooling device
for cooling of the millbases (Temperature control)
(If necessary for constant temperature of the millbases)
After finishing of the dispersion, the temperature of the millbases is a function of the dispersion time and the
number of containers shaken at the same time. This assumes that samples have the same millbase
composition and same grinding beads. Depending on the position in the holder (middle or edge) significant
temperature differences can arise without cooling.
In such cases, it is necessary to use a fan to create cooling and equal temperatures, to allow a comparison
between different millbases.
3.6 Balance, 0,01 g precision
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ISO 2012 All rights reserved 3

4 Binder system
The binder/solvent system controls the ease of dispersion and millbase viscosity, so the binder system shall
be agreed upon.
5 Sampling
Take a sample of the pigment to be tested as described in ISO 15528.
6 Millbase
6.1 Composition of the millbase
For the dispersion method according to this International Standard, it is mandatory that the grinding beads can
move freely in the millbase during the dispersion process.
NOTE This is ensured, for example, when after the dispersing step the flow time of the millbase is not longer than
100 s, measured according to ISO 2431 with flow cup ISO 2431 No. 5. To fill the ISO cup the millbases of 2 identical
dispersions are necessary.
If the ease of dispersion of multiple pigments is to be compared, the millbases shall show the same flow
behaviour. Therefore different millbase compositions may be needed. The most suitable concentration of
pigment, binder, and solvent in the millbase may not be known.
For a given binder system - that means at a defined ratio of binder : solvent, with the option of putting in
additives; the suitable pigment concentration Pk can be determined, if not known, by means of some
preliminary trials.
Guidance for suitable pigment concentrations:
Inorganic pigments Pk > 40 %
Inorganic and organic pigments Pk 10 % to 40 %
Organic pigments and carbon blacks Pk < 10 %
6.2 Volume of the millbase
The millbase (beads excluded) shall occupy approximately 30 % of the volume of the container (3.3). The
mass of the pigment and of the binder system may be determined by using the following equations:
Mass m
p
of pigment in grams:
Pk
Pk
V
m
M p
p

+

=

100 1
3 , 0
(1)
Mass m
M
of binder system in grams:
Pk
Pk m
m
p
M
) 100 (
= (2)
where:

p
is the density of the pigment;
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is the density of the binder system;


Pk is the pigment concentration;
V is the volume of the container.
EXAMPLE Calculation of the mass of pigment m
p
:
8 , 68
5 , 1 244 , 0
120
100 1
3 , 0
=
+
=

+

=
Pk
Pk
V
m
M p
p

(3)
EXAMPLE Calculation of the mass of binder m
M
:
2 , 103
40
60 8 , 68
) 100 (
=

=

=
Pk
Pk m
m
p
M
(4)
7 Volume of the grinding beads
The apparent volume of the grinding beads shall be approximately 50 % of the total volume of the container.
This has to be measured precisely and kept constant for all test of a test series.
8 Procedure
8.1 Filling the container
Unless otherwise agreed upon, add the grinding beads (3.4. Apparent volume according to clause 7) to the
container. Add the calculated mass of binder (clause 4 and 6.2). Wet the grinding beads with the binder
system by tilting the container. Then add the required mass of pigment (6.2). Close the container and wet the
pigment by carefully tilting the container.
NOTE If it is difficult to wet the pigment it may be advisable to select a different sequence of preparing the containers.
If necessary, the millbase may be placed into the container first and stirred with a spatula prior to the addition of the
grinding beads.
Complete the preparation of the full set of mill bases as quickly as possible in order to avoid differences in
stirring and wetting time between the samples.
8.2 Dispersion
Immediately after filling the containers clamp the containers in the holder and start the machine for the
dispersion process. Take test portions after the agreed dispersion time to assess the ease of dispersion. The
total mass of these test portions shall not exceed 15% of the initial mass of the millbase. If larger test portions
are required, separate replicates for each time are necessary.
8.3 Stabilization of the millbases
If necessary, the test portions may be stabilized by adding either binder or additives. These additions have to
be agreed upon by parties involved and shall be the same for all samples of a test series.
8.4 De-aeration of millbases
If necessary, the interested parties can take action to de-aerate (escape of enclosed air bubbles) the millbase.
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9 Precision
Statements on precision of the methods of assessment are not able to be given due to the dependence of the
results on the choice of the binder system and the method of dispersion.
10 Test report
The test report shall contain at least the following information:
a) all details necessary to identify the product tested;
b) a reference to this part of ISO 8780 (ISO 8780-7:20xx);
c) size of the container;
d) exact composition of the millbase;
e) type and diameter of the grinding beads;
f) oscillatory frequency (see 3.1.) and dispersion time;
g) any deviation from the procedure specified;
h) the date(s) of the test.

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