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International Standard: Paints, Varnishes and Plastics - Determination of Non-Volatile-Matter Content

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INTERNATIONAL ISO
STANDARD 3251

Fourth edition
2008-02-15

Paints, varnishes and plastics —


Determination of non-volatile-matter
content
Peintures, vernis et plastiques — Détermination de l'extrait sec

Reference number
ISO 3251:2008(E)

© ISO 2008
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ISO 3251:2008(E)

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ISO 3251:2008(E)

Contents Page

Foreword............................................................................................................................................................ iv
1 Scope ..................................................................................................................................................... 1
2 Normative references ........................................................................................................................... 1
3 Terms and definitions........................................................................................................................... 2
4 Apparatus .............................................................................................................................................. 2
5 Sampling ................................................................................................................................................ 3
6 Procedure .............................................................................................................................................. 3
7 Supplementary test conditions ........................................................................................................... 4
8 Expression of results ........................................................................................................................... 4
9 Precision ................................................................................................................................................ 5
10 Test report ............................................................................................................................................. 5
Annex A (informative) Commonly used test parameters ................................................................................ 6
Bibliography ....................................................................................................................................................... 7

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ISO 3251:2008(E)

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 3251 was prepared by Technical Committee ISO/TC 35, Paints and varnishes, Subcommittee SC 10,
Test methods for binders for paints and varnishes, in collaboration with Technical Committee CEN/TC 139,
Paints and varnishes.

This fourth edition cancels and replaces the third edition (ISO 3251:2003), which has been technically revised.
The main changes are as follows:

a) The heating time, heating temperature and test-portion mass have to be agreed in each case. The tables
giving values of these parameters have therefore been moved to an informative annex where they are
intended to serve as proposals. Values suitable for reactive systems such as car refinish paints have
been added.

b) The precision data have been corrected.

iv © ISO 2008 – All rights reserved


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INTERNATIONAL STANDARD ISO 3251:2008(E)

Paints, varnishes and plastics — Determination of non-volatile-


matter content

1 Scope
This International Standard specifies a method for determining the non-volatile-matter content by mass of
paints, varnishes, binders for paints and varnishes, polymer dispersions and condensation resins such as
phenolic resins (resols, novolak solutions, etc.).

The method is also applicable to formulated dispersions containing fillers, pigments and other auxiliaries (e.g.
thickeners and film-forming agents). For the method to be usable for unplasticized polymer dispersions and
rubber latices, the non-volatile residue (which consists essentially of the polymeric material and of small
quantities of auxiliaries such as emulsifiers, protective colloids, stabilizers, solvents added as film-forming
agents and — especially for rubber latex concentrate — preserving agents) has to be chemically stable under
the test conditions. For plasticized samples, the residue, by definition, normally includes the plasticizer.

NOTE 1 The non-volatile-matter content of a product is not an absolute quantity but depends upon the temperature
and period of heating used for the determination. Consequently, when using this method, only relative and not true values
for non-volatile-matter content are obtained owing to solvent retention, thermal decomposition and evaporation of low
molecular mass constituents. The method is therefore primarily intended for testing different batches of the same type of
product.

NOTE 2 This method is suitable for synthetic rubber latices provided heating for a specific period of time is considered
appropriate (ISO 124 specifies heating until the loss in mass of a 2 g test portion following successive periods of heating is
less than 0,5 mg).

NOTE 3 In-house methods for determining non-volatile matter often include drying with infrared or microwave radiation.
Standardization of such methods is not possible, since they are not generally applicable. Some polymer compositions tend
to decompose during such treatment and therefore give incorrect results.

ISO 3233 and ISO 23811 specify methods for determining the volume of non-volatile matter in paints,
varnishes and related products.

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 123, Rubber latex — Sampling

ISO 124, Latex, rubber — Determination of total solids content

ISO 1513, Paints and varnishes — Examination and preparation of samples for testing

ISO 2431, Paints and varnishes — Determination of flow time by use of flow cups

ISO 15528, Paints, varnishes and raw materials for paints and varnishes — Sampling

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ISO 3251:2008(E)

3 Terms and definitions


For the purposes of this document, the following terms and definitions apply.

3.1
non-volatile matter
NV
residue by mass obtained by evaporation under specified conditions

[ISO 4618:2006]

4 Apparatus
Ordinary laboratory apparatus, together with the following:

4.1 For paints, varnishes, binders for paints and varnishes and polymer dispersions:

Flat-bottomed dish, of metal or glass, inner diameter of base (75 ± 5) mm, height of rim at least 5 mm.

Dishes having different diameters may be used by agreement between the interested parties. The agreed dish
diameter shall be adhered to within ± 5 %.

NOTE 1 For rubber latices, lipless dishes with covers are recommended.

NOTE 2 For very viscous polymer dispersions or latices, it is recommended that aluminium foils are used which are
about 0,1 mm thick, cut into rectangles of about (70 ± 10) mm × (120 ± 10) mm that can be folded in half, thus allowing the
viscous liquid to be spread by gently squeezing the halves together.

4.2 For liquid crosslinking resins (phenolic resins):

Flat-bottomed dish, of metal or glass, inner diameter of base (75 ± 1) mm, height of rim at least 5 mm, for
use with a test portion of 3 g.

Dishes of different diameters may be used provided the mass of the test portion m, in grams, is calculated
from the following equation in order to ensure comparable film thicknesses:

2
⎛ d ⎞
m = 3×⎜ ⎟ (1)
⎝ 75 ⎠

where

d is the diameter, in millimetres, of the dish base;

3 is the nominal mass of the test portion (3 g);

75 is the nominal diameter of the dish (75 mm).

4.3 Air oven, designed to carry out the test in safe conditions, and capable of being controlled at the
specified or agreed temperature (see Clause 7) to within ± 2 °C (for temperatures up to 150 °C) or ± 3,5 °C
(for temperatures above 150 °C and up to 200 °C). The oven shall be fitted with forced-ventilation equipment,
except in the case of phenolic resins when an oven with natural convection with a perforated metal shelf
placed at one-third of the height of the oven may be used.

WARNING — To protect against explosion or fire, products containing flammable volatile substances
should be handled with care. National regulations should be followed.

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