FprEN 12802

SLOVENSKI STANDARD
01-februar-2009
0DWHULDOL]DR]QDþHYDQMHYR]LãþD/DERUDWRULMVNHPHWRGH]DLGHQWLILNDFLMR
Road marking materials - Laboratory methods for identification
Straßenmarkierungsmaterialien - Laborverfahren für die Identifikation
Produits de marquage routier - Méthodes de laboratoire pour identification
Ta slovenski standard je istoveten z: prEN 12802
ICS:
93.080.20 Materiali za gradnjo cest Road construction materials
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
DRAFT
prEN 12802
NORME EUROPÉENNE
EUROPÄISCHE NORM
September 2008
ICS 93.080.20 Will supersede EN 12802:2000
English Version
Road marking materials - Laboratory methods for identification
Produits de marquage routier - Méthodes de laboratoire
pour identification
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee CEN/TC 226.
If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations which
stipulate the conditions for giving this European Standard the status of a national standard without any alteration.
This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other language
made by translation under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the
same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
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.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and
shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2008 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 12802:2008: E
worldwide for CEN national Members.

prEN 12802:2008 (E)
Contents
Foreword.4
1 Scope .5
2 Normative references .5
3 Terms and definitions .5
4 Sampling.7
5 Test methods.7
Annex A (normative)  Paint – Test method for the determination of the solids content .12
A.1 Principle.12
A.2 Apparatus .12
A.3 Reagents.12
A.4 Procedure .12
A.5 Test result.13
Annex B (normative) Paint, thermoplastics and cold plastics – Test method for the determination and
identification of organic constituents.14
B.1 Principle.14
B.2 Apparatus .14
B.3 Solvents being used.15
B.4 Procedure .15
B.5 Test results.16
Annex C (normative) Paint, thermoplastic and cold plastic – Test method for the determination and
identification of inorganic constituents .18
C.1 Principle.18
C.2 Apparatus .18
C.3 Reagent.18
C.4 Procedure .18
C.5 Calculation and expression of results (carbonate content as part of the inorganic
constituents) .19
Annex D (normative) Paint, thermoplastics and cold plastics – Test method for the determination of
the titanium (IV) dioxide content.20
D.1 Principle.20
D.2 Apparatus .20
D.3 Reagents.20
D.4 Preparation of the solutions .21
D.5 Procedure .21
Annex E (normative) Paint, thermoplastics and cold plastics – Test method for the determination of
the glass bead content.23
E.1 Principle.23
E.2 Apparatus .23
E.3 Reagent.23
E.4 Procedure .23
E.5 Calculation and expression of results.24
Annex F (normative) Paint and cold plastics – Test method for the determination and identification of
solvents .25
F.1 Principle.25
F.1.1 Total Solvent Content.25
F.1.2 Solvent Identification .25
F.2 Apparatus .25
F.3 Reagents.25
F.4 Procedure .26
F.5 Test results.26
F.5.1 Total Solvent Content.26
F.5.2 Solvent Identification .26
Annex G (normative) Paint – Test method for the determination of viscosity (Krebs-Stormer method) .27
G.1 Principle.27
prEN 12802:2008 (E)
G.2 Apparatus .27
G.3 Procedure .27
G.4 Expression of results .28
Annex H (normative) Paint, thermoplastics and cold plastics – Test method for the determination of
the ash content .31
H.1 Scope and field application .31
H.2 References .31
H.3 Sampling.31
H.4 Apparatus .31
H.5 Procedure .31
H.6 Calculation and expression of results.32
H.7 Test report .32

prEN 12802:2008 (E)
Foreword
This document (prEN 12802:2008) has been prepared by Technical Committee CEN/TC 226 “Road equipment”,
the secretariat of which is held by AFNOR.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 12802:2000.

prEN 12802:2008 (E)
1 Scope
This European Standard describes laboratory methods for the identification of road marking materials used in
horizontal signalization. It is not necessary, unless required, to perform all of the tests described.

2 Normative references
This European 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 publications are listed hereafter. For
dated references, subsequent amendments to or revisions of these publications apply to this European Standard
only when incorporated in it by amendment or revision. For undated references the latest edition of the publication
referred to applies.
ENV 13459-1, Road marking materials – Quality control – Part 1: Sampling from storage and testing

EN 1423, Road marking materials – Drop on materials – Glass beads, antiskid aggregates and mixtures of the two

EN 1424, Road marking materials – Premix glass beads

EN 1790, Road marking materials – Preformed road markings

ISO 2555, Plastics. Resins in the liquid state or as emulsions or dispersions. Determination of apparent viscosity by
the Brookfield Test method
ISO 2811-1, Paints and varnishes – Determination of density – Part 1: Pyknometer method

ISO 2811-2, Paints and varnishes – Determination of density – Part 2: Immersed body (plummet) method

ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results – Part 2: Basic method for
the determination of repeatability and reproducibility of a standard measurement method

ISO 11890-2, Paints and varnishes. Determination of volatile organic compound (VOC) content. Gas
chromatographic method
ISO 15528, Paints, varnishes and raw materials for paints and varnishes. Sampling
3 Terms and definitions
For the purpose of this European Standard the following terms and definitions apply.

3.1
paints
a liquid product containing suspended solids. It can be supplied in single or multicomponent systems. When
applied it produces a cohesive film by the process of solvent evaporation, or solvent evaporation and a chemical
process.
3.1.1
solvent paints
solvent paints are liquid products containing solids and liquid additives suspended in an organic solvent. They can
be supplied in single or multi-component systems. The solids comprise are inorganic and/or organic fillers,
pigments and additives
3.1.1.1
high Solid paints (HS)
high Solid paints are liquid products containing solids and liquid additives suspended in a solution of the binder in
an organic solvent. The content of solvents is limited to 25% weight by weight.

prEN 12802:2008 (E)
3.1.1.2
single-Component-High Solid paints (SCHS)
the cohesive film of a single-component High Solid is formed only by evaporation of the solvent and physical
curing.
3.1.1.3
multi-Component-High Solid paints (MCHS)
multi-component-High Solid paints consist of two or more components. The cohesive film is formed after mixing all
components by the evaporation of the solvent and a chemical reaction. The Application is possible within the pot-
life-time.
3.1.2
waterborne Paints
a liquid product containing suspended solids in an aqueous liquid. It can be supplied in single or multicomponent
systems. When applied it produces a cohesive film by the process of aqueous liquid evaporation and /or chemical
process
3.1.2.1
dispersions
dispersions are liquid or viscous products containing solids and liquid additives dispersed in an aqueous liquid. The
aqueous liquid consists of the binder polymers and mainly of water. The solids comprise inorganic and/or organic
fillers, pigments and additives. The content of volatile organic solvents is limited to 2 % weight by weight, the total
amount of volatile organic compounds (VOC) is limited to 3 % weight by weight.

3.1.2.2
dispersion paints
the volatile component is mainly water. The content of organic solvents is limited to 2 % weight by weight, the total
amount of volatile organic compounds (VOC) is limited to 3 % weight by weight.
The solid content is lower than 80 % weight by weight. The cohesive film of a dispersion paint is produced by the
process of water evaporation.
3.1.2.3
high solid dispersions
the volatile component of a high solid dispersion is mainly water with a content lower than 20 % weight by weight,
the content of solids is equal to or higher than 80 % weight by weight. The content of organic solvents is limited to 2
% weight by weight, the total amount of volatile organic compounds (VOC) is limited to 3 % weight by weight. The
cohesive film of a High-Solid dispersion is produced by the process of water evaporation and a chemical cross-
linking reaction.
3.2
cold plastics
cold plastics are viscous products supplied in two or multi-component forms (at least one main component and a
hardener system). They are free from solvents. The cohesive film is formed after mixing of all components only by
a chemical reaction. Following the reaction the liquid becomes a solid.

3.2.1
cold-setting reactive materials (cold plastics)
cold plastics consist of a minimum of two components. One component contains a hardener and another
component the accelerator. Depending on the system the components are mixed in various ratios. The application
is only possible within the pot-life-time.

3.2.2 energy Induced Curing Materials (EICM)
energy induced curing materials produce a cohesive film under the influence of energy
(e.c. heat, UV-radiation).
prEN 12802:2008 (E)
3.3
thermoplastics
a solvent-free marking substance supplied in block, granular or powder forms. It is heated to a molten state and
then applied. It forms a cohesive film by cooling.

NOTE Additional materials to those described in 3.1 to 3.3 can include, if recommended by the manufacturer,
primers which are liquid products which may contain solids and liquid additives suspended in an organic solvent or
in water. The solids comprise inorganic and/or organic fillers, pigments and additives. The content of volatile
organic solvents is not limited.
Primers are used to precoat road surfaces before the road marking system is applied. They improve the adhesion
of the road marking and protect against disintegration, discolouring etc. caused by incompatible compounds in the
road surface.
4 Sampling
Samples representative of each component of the material shall be taken from storage in accordance with ENV
13459-1. Smaller representative samples, of sufficient quantity to carry out all the tests required, shall be taken
from the larger samples. For paints and cold plastics approximately 1 l of the basic component shall be taken.

In the case of thermoplastic in powder form sufficient quantity shall be taken in accordance with ENV 13459-1 so
that it can be melted in a metal container and mixed to a homogeneous mass. After cooling and casting into solid
sheets or blocks, representative samples of approximately 1 kg of homogeneous solid material shall be taken for
testing.
5 Test methods
5.1 General
The standard test methods are listed in 5.2 to 5.4.

Alternative quantitative analytical test methods may be used providing that:

– the resulting values are comparable to those obtained using the standard methods; and,
– the repeatability of the alternative methods, determined in accordance with ISO 5725-2, can be shown to
be not less than that of the methods given in this standard.

5.2 Paint
5.2.1 Density
The density of the paint shall be determined using, either the method laid down in ISO 2811-1, or an alternative
method complying with 5.1.
5.2.2 Solids content
The solids content of the paint, expressed as a percentage, shall be determined using, either the method described
in annex A, or an alternative method complying with 5.1.

5.2.3 Organic content and identification

The type of organic materials, and the content expressed as a percentage, of the paint shall be determined using,
either the method described in annex B, or an alternative method complying with 5.1.

5.2.4 Inorganic content and identification

The type of inorganic materials, and the content expressed as a percentage, of the paint shall be determined using,
either the method described in annex C, or an alternative method complying with 5.1.

prEN 12802:2008 (E)
5.2.5 Titanium dioxide content

The titanium dioxide content of the paint, expressed as a percentage, shall be determined, either by the method
described in annex D, or an alternative method complying with 5.1.

5.2.6 Glass bead content
The glass bead content of the paint, expressed as a percentage, shall be determined, either as described in annex
E, or an alternative method complying with 5.1.

5.2.7 Solvent content and identification

The type of solvent, and the content expressed as a percentage, of the paint shall be determined using, either the
method described in annex F, or an alternative method complying with 5.1.

5.2.8 Viscosity
The viscosity of the paint shall be determined using, either the method described in annex G, or an alternative
method complying with 5.1.
5.2.9 Ash content
The ash content of the paint shall be determined using, either the method described in annex H, or an alternative
method complying with 5.1.
5.3 Thermoplastics
5.3.1 Density
The density of the thermoplastics shall be determined using, either the method laid down in ISO 2811-2, or an
alternative method complying with 5.1.

5.3.2 Organic content and identification

The type of organic materials, and the content expressed as a percentage, of the thermoplastics shall be
determined using, either the method described in annex B, or an alternative method complying with 5.1.

5.3.3 Inorganic content and identification

The type of inorganic materials, and the content expressed as a percentage, of the thermoplastics shall be
determined using, either the method described in annex C, or an alternative method complying with 5.1.

5.3.4 Titanium dioxide content

The titanium dioxide content of the thermoplastics, expressed as a percentage, shall be determined, either by the
method described in annex D, or an alternative method complying with 5.1.

5.3.5 Glass bead content
The glass bead content of the thermoplastics, expressed as a percentage, shall be determined, either as described
in annex E, or an alternative method complying with 5.1.

5.3.6 Ash content
The ash content of the thermoplastics shall be determined using, either the method described in annex H, or an
alternative method complying with 5.1.

prEN 12802:2008 (E)
5.4 Cold plastics
5.4.1 Density
The density of the cold plastics shall be determined using, either the method laid down in ISO 2811-2, or an
alternative method complying with 5.1.

5.4.2 Organic content and identification

The type of organic materials, and the content expressed as a percentage, of the cold plastics shall be determined
using, either the method described in annex B, or an alternative method complying with 5.1.

5.4.3 Inorganic content and identification

The type of inorganic materials, and the content expressed as a percentage, of the cold plastics shall be
determined using, either the method described in annex C, or an alternative method complying with 5.1.

5.4.4 Titanium dioxide content

The titanium dioxide content of the cold plastics, expressed as a percentage, shall be determined, either by the
method described in annex D, or an alternative method complying with 5.1.

5.4.5 Glass bead content
The glass bead content of the cold plastics, expressed as a percentage, shall be determined, either as described in
annex E, or an alternative method complying with 5.1.

5.4.6 Solvent content and identification

The type of solvent, and the content expressed as a percentage, of the cold plastics shall be determined using,
either the method described in annex F, or an alternative method complying with 5.1.

5.4.7 Viscosity
The viscosity of the cold plastics shall be determined using, either the method laid down in ISO 2555 with a Type A
viscosimeter, or an alternative method complying with 5.1.

5.4.8 Ash content
The ash content of the cold plastics shall be determined using, either the method described in annex H, or an
alternative method complying with 5.1.

5.5 Preformed road markings
The identification methods for preformed road markings are laid down in EN 1790

5.6 Premix glass beads
5.6.1 Granulometry
The granulometry of the glass beads shall be determined using the method laid down in
Clause 4 of EN 1424.
5.6.2 Refractive index
The refractive index class of the glass beads shall be determined using the method laid down in Clause 4 of EN
prEN 12802:2008 (E)
5.6.3 Resistance to water, hydrochloric acid, calcium chloride and sodium sulfide

The glass beads shall not develop any surface haze or dulling when in contact with any of the following: water,
hydrochloric acid, calcium chloride and sodium sulfide, using the method laid down in Clause 4 of EN 1423

5.6.4 Defective beads
The percentage of defective glass beads shall be determined using the method laid down in Clause 4 of EN 1424

5.6.5 Surface Treatment
The surface treatment of the glass beads shall be determined using the method laid down in Clause 4 of EN 1424
5.7 Drop on materials
5.7.1 Drop on glass beads
5.7.1.1 Granulometry
The granulometry of the glass beads shall be determined using the method laid down in Clause 4 of
EN 1423.
5.7.1.2 Refractive index
The refractive index class of the glass beads shall be determined using the method laid down in Clause 4 of
EN 1423.
5.7.1.3 Resistance to water, hydrochloric acid, calcium chloride and sodium sulfide

The glass beads shall not develop any surface haze or dulling when in contact with any of the following: water,
hydrochloric acid, calcium chloride and sodium sulfide, using the method laid down in Clause 4 of EN 1423

5.7.1.4 Defective beads
The percentage of defective glass beads shall be determined using the method laid down in Clause 4 of EN 1423.

5.7.1.5 Surface Treatment
The surface treatment of the glass beads shall be determined using the methods laid down in Clause 4 of EN 1423.

5.7.2 Drop on antiskid aggregates

5.7.2.1 Friability index
The friability index of the antiskid aggregates shall be determined using the method laid down in Clause 5 of
EN 1423.
5.7.2.2 Granulometry
The granulometry of the antiskid aggregates shall be determined using the method laid down in Clause 5 of
EN 1423.
5.7.2.3 Colour co-ordinates and luminance factor

If the antiskid aggregate is not transparent, the chromaticity co-ordinates and the luminance factor shall be
determined using the method laid down in Clause 5 of EN 1423.

5.7.3 Mixture of glass beads and antiskid aggregates

In a mixture of glass beads and antiskid aggregates the glass beads shall conform to Clause 4 of EN 1423 and the
antiskid aggregates shall conform to Clause 5 of EN 1423. The tests on the glass beads and the antiskid
aggregates to be incorporated in mixtures shall be conducted separately before mixing.
prEN 12802:2008 (E)
5.8 Tolerances
Tolerances are as shown in Table 1.

For the initial testing of a material, tolerances apply to the manufacturers declared values for the properties tested
and the initial test results shall be within the tolerances in Table 1.

When the values fall inside the tolerances then the values initially declared by the manufacturer are considered to
be verified.
When values fall outside of the tolerances there are four possibilities:
- the manufacturer can decide that the test be terminated
- by agreement between the participants the test can be repeated with the same samples
- by agreement between the participants the test can be repeated with new samples
- by agreement between the participants the manufacturer can submit revised declared values

For re-identification of a material it may not be necessary to test all of the values, the reference values for the
properties tested shall be the values declared by the manufacturer.

Table 1 - Tolerances
Parameter Maximum relative deviation Maximum absolute deviation
Solids content - ± 2
Density - Paint: ± 0,04 g/cm³
- Cold plastic: ± 0,06 g/cm³
- Thermoplastic: ± 0,1 g/cm³
Organic constituents 10% ± 2
Calcium Carbonate ± 3
Inorganic constituents - ± 3
Titanium dioxide For TiO concentrations≥ 10% For TiO concentrations ≤10 %
2 2
Tolerance = 10% Tolerance = 1
Glass beads* 20% ± 5
Solvent content ± 3
Viscosity Cold plastic: 20%
Paint: ± 10 units
Ash Content - ± 3
* Experimental values which are only applicable if the glass bead content is ≥ 10%. It is not possible
to set tolerances if the percentage of glass beads is less than 10%.

prEN 12802:2008 (E)
Annex A
(normative)
Paint – Test method for the determination of the solids content
A.1 Principle
The volatile constituents of the paint are evaporated at 105 °C. The residual solids are weighed and the solids
content calculated.
A.2 Apparatus
a) Cooling equipment, refrigerator or water bath with thermostat at approximately +10 °C;

b) porcelain plates with a diameter of approx. 40 mm an a high of 20 mm to 30 mm;

c) analytical balance, with an accuracy of 0,001 g, with zero point correction;

d) warming cupboard, with forced fresh air ventilation and flame-proof interior capable of being heated to 105 °C ±
2 °C;
e) desiccator, with drying agent, e.g. silica gel.

A.3 Reagents
Thinner consisting of a suitable solvent / thinner as recommended by the manufacturer.

A.4 Procedure
A.4.1 Carry out two determinations.

A.4.2 Mark porcelain plates with numbers. Record the mass of the empty plates (L) to the nearest 0,001 g. Place
approximately 2 g of the paint, pre-cooled to 10 °C and homogenized, in the plate with a spoon. Weigh to the
nearest 0,001 g (mass M ).
Place the plates containing the sample in a warming cupboard at a temperature of 105 °C ± 2 °C and store there
for at least 3 h or until constant mass is reached. Constant mass is reached when, after the sample has been in the
warming cupboard for a further 1,5 h, the mass loss is less than 0,2 % of the initial mass. Cool the plate to room
temperature in the desiccator, and weigh to the nearest 0,001 g.

Use the solid residue remaining in the plate as the basis for determining the organic content of the paint in
accordance with annex B.
prEN 12802:2008 (E)
A.5 Test result
The percentage solids content of the paint by mass, S, shall be calculated according to the following equation:

100 (M −L )
2 S
S =
M −L
1 S
where:
M1 is the initial mass of paint together with the empty plate, in grams;

M2 is the final mass of solid together with the plate, in grams;

L is the mass of the empty plate, in grams.

If the results of the individual determinations differ by more than 0, 5% by mass the procedure shall be repeated.
The mean of the two individual results shall be calculated and the solids content given rounded to the nearest 0,1
% by mass.
prEN 12802:2008 (E)
Annex B
(normative)
Paint, thermoplastics and cold plastics – Test method for the determination
and identification of organic constituents

B.1 Principle
Separation of the binder, insoluble organic and inorganic constituents from the specimen by solvent extraction,
centrifuging and combustion. The binder type of paints and thermoplastics is identified by IR spectra using a
potassium bromide (KBr) pellet or window.
The binder type of cold plastics is identified using ISO 11890 – 2 “Determination of volatile organic compound
(VOC), part 2:Gaschromatographic method”

The inorganic constituents are kept for further IR examination (annex C), determination of titanium dioxide (annex
D) and the glass bead content (annex E).
B.2 Apparatus
)
a) Centrifuge, high-speed, 10 000g ;

b) centrifuge bowls, steel bowls or glass tubes, each with a capacity of 80 cm ;

c) spatula;
d) warming cupboard, with forced ventilation, capable of being heated to 105 °C ± 10 °C;

e) rotary evaporator;
f) glass flask, with a capacity of 500 ml, with ground glass neck;

-1 -1
g) infrared spectrometer, automatically recording FTIR spectrometer, range 4000 cm to 400 cm with an
-1
optical resolving power better than 5 cm throughout the spectral range using an ordinate with a scale of 0
% to 100 % transmission.
h) analytical balance, with an accuracy of 0,001 g, with zero point correction;

i) two erlenmeyer flasks of heat resistant glass, 250 ml or 300 ml capacity;

j) electric muffle furnace, adjustable to 450 °C ± 25 °C;

k) desiccator, with drying agent, e.g. silica gel

l) ultrasonic dissolver or similar device

) -2
g equals 9,81 m x s
prEN 12802:2008 (E)
B.3 Solvents being used
The following solvents shall be used unless otherwise stipulated by the supplier:

• for paints containing organic solvents: mixture of three parts toluene p.a. to one part acetone p.a. by volume;
• for waterborne paints: tetrahydrofurane;
• for thermoplastics: mixture of three parts toluene p.a. to one part acetone p.a. by volume or methylethylketone
• for cold plastics: ethyl acetate.
• Acetone
B.4 Procedure
B.4.1 Separation of binder
Weigh the centrifuge bowls to the nearest 0,01 g (W ). Weigh a portion of approximately at least 10 g to the nearest
0,01 g together with the bowl (W ).
Place a portion of the marking material, carefully homogenized, in a centrifuge tube. Add approximately 25 ml of an
appropriate solvent (see B.3). Seal the tube with a stopper and allow to stand overnight. After standing, stir the
contents of the tube thoroughly with a spatula and centrifuge the mixture at 10 000g to 15000g for 20 min. Decant
the liquid phase into the glass flask. Thin the solid phase with a further 25 ml of solvent, stir again with the spatula,
rinse and centrifuge again. Repeat the procedure three times or until the liquid supernatent is of clear color. Use a
highly volatile solvent the third time (such as acetone). Expose the centrifuge bowls containing the solid phase to
the air for 5 min and dry in the warming cupboard for approximately 2 h.

Cool down the tubes in a desiccator and reweigh them to the nearest 0,01 g (W ).
For dispersions do the extraction with tetrahydrofurane and centrifuge at a low speed of about 1000g, as high
speeds can throw out high molecular components of the binder.

B.4.2 Preparation of spectra
Concentrate the solutions obtained in B4.1 down to about 20 ml in the 500 ml glass flask in a rotary evaporator.

For recording the IR spectrum of the binder of a road marking material, use the binder solutions obtained in B.4.2.
Coat the cuvette window or the potassium bromide (KBr) pellet (both referred to as 'pellet' below) evenly with a
specimen of the solution.
Dip a previously prepared pellet into the liquid obtained from the appropriate extraction and coat it evenly with a
specimen of the solution. As the solvent evaporates, examine the pellet to make sure that the film formed on it is
uniform and homogeneous. There shall be no bubbles or separation. In order to remove the solvent completely,
store the coated pellet for at least 3 h in a warming cupboard at 60 °C ± 2 °C.

Place the pellet in the sample holder of the IR spectrometer and record the IR spectrum. Keep the tracing as a
reference.
If the intensity of the spectrum is too weak, dip the pellet into the solution a second time, dry it and test again.
Repeat the procedure until a spectrum is produced in which the strongest bands have an intensity of 5 % to 15 %
transmittance. If the intensity is to strong, thin with an appropriate solvent.

Record the spectrum in such a way that the strongest absorptions have a transparency between 5 % and 15 %.
The film thickness suitable for evaluation of the spectra shall be determined empirically.

It is imperative that no absorption bands of the solvents are present in the spectrum. If such bands are present
continue the drying of the film.

prEN 12802:2008 (E)
B.4.3 Processing of the solids

The solids from the separation may contain insoluble organic compounds. The are ashed at 450 °± 25 °C in a
muffle furnace and the loss in mass determined. The ash residue is used for the determination of the titanium
dioxide in annex D and inorganic constituents in annex C.

Carry out two determinations.
Weight a empty flask to the nearest 0.001g (W ), Take the residue of the centrifuge tube an place it in the
flask directly in the muffle furnace afterwards and raise the temperature gradually to 450 °C ± 25 °C. Keep the
flask in the furnace for at least 2 h or until constant mass is obtained. Remove the flask containing the
residues, cool in a desiccator and reweigh (W ).
NOTE  The determination should be carried out in a properly functioning fume hood.

B.4.4 Processing of the liquid

Weight an empty capsule to the nearest 0.001 g (W )
V is the total volume of the liquid part obtained in B 4.1
Take a small part of the different liquid phase collect in part B 4.1 (V ) In order to have at the end between 1 and 3
grams of binder and put in the capsule on a hotplate at 60°C under a ventilation forced for approximately 12 h –16
h. To finish the evaporation of the volatile part place the capsule in a drying ovent at vacuum regulated at 60°C and
establish the vacuum (1) gradually to prevent the risks of projection during one hour
(1) approximately 16 to 33 mbar.

Continue the evaporation until constant mass is obtained (W ). Be careful to cool the capsule before every
weighting
B.5 Test results
The binder content by mass (B) , shall be determined using the following equation for thermoplastics cold plastic
and paints.
(W −W )×V
W −W
2 1 2
7 6
B = *100 where W =
W V
8 1
The percentage binder + solvent content by mass, B+SC, could be determined (for information only) using the
following equation for thermoplastics and reactive materials:

100(W −W )
2 3
B+SC =
W −W
2 1
where:
W is the mass of the empty centrifuge bowl in grams;
W is the mass of the bowl together with the sample in grams;
W is the mass of the bowl together with the residues in grams.
The percentage of inorganic compounds content by mass, I, shall be determined using the following equation:
100(W −W )
5 4
I =
W −W
2 1
The percentage binder content by mass, B, could be also determined using the following equation for paints and
cold plastics:
prEN 12802:2008 (E)
B =S −I
“S” is the solid content obtained in annex A

If the results of the individual determinations of the binder or inorganic content differ by more than 0,5 % by mass
from the mean, repeat the procedure. The mean of the two individual results shall be calculated and the binder
content given rounded to the nearest 0,1 % by mass.

The percentage of insoluble organic compounds (IC) by mass is given by the difference:

IC =100−()I +B
prEN 12802:2008 (E)
Annex C
(normative)
Paint, thermoplastic and cold plastic – Test method for the determination
and identification of inorganic constituents
C.1 Principle
The inorganic constituents obtained in annex B.4.3 are used for the determination.
In the case of containing glass beads and antiskid materials the pigments and fillers are separated with a standard
sieve, mesh size 0,090 mm.
The pigments and fillers are determined by IR analysis using a KBr pellet.
Furthermore they are used for the determination of titanium dioxide described in annex D.
For the determination of the carbonates –expressed as calcium carbonate – a part of the residue obtained in annex
o
B.4.3 is heated in a furnace up to 1000 C. The loss of weight is used to calculate the carbonate content.
C.2 Apparatus
a) Analytical balance, with an accuracy of 0,001 g, with zero point correction;

b) standard sieve and bottom, mesh size 0,090 mm;

c) agate mortar and pestle
d) desiccator, with drying agent e.g. silica gel;

-1 -1
e) infrared spectrometer, automatically recording FTIR spectrometer, range 4 000 cm to 400 cm ;

f) press;
g) mould, for making pellets;
h) electric muffle furnace, capable of being raised to a temperature of 1000°C ± 20°C;

i) porcelain basins.
C.3 Reagent
Potassium bromide in chromatographic quality
C.4 Procedure
Carry out two determinations.
C.4.1
In the case of containing glass beads and antiskid materials separate the pigments and fillers with a standard sieve
and bottom, mesh size 0,090 mm.
Pulverize the pigments and fillers in the agate mortar. It shall be a homogeneous mixture that is representative of
the composition of the inorganic constituents of the sample materials.

Take a representative sample of approximately 1,5 g to 2,0 g from the sample. Mix this sample in the agate mortar
with approximately 200 mg of KBr and make a pellet from the mixture. Record an IR spectrum of the pellet. Keep
the recorded spectrum for reference.
If the pellets are not to be used immediately for recording the IR spectrum, keep them over a drying agent in a
desiccator.
prEN 12802:2008 (E)
Record the spectrum in such a way that the strongest absorption bands have a transmission between 5 % and 15
%. If the absorption intensities do not lie within this range, determine the amount of sample suitable for evaluation
empirically and record a new spectrum.

C.4.2 Determination of the carbonates

Weigh the porcelain basin (M ), add 3-6 g of the residue obtained in annex B.4.3 and weigh again (M ). Heat
...