SIST EN ISO 3262-20:2001
(Main)Extenders for paints - Specifications and methods of test - Part 20: Fumed silica (ISO 3262-20:2000)
Extenders for paints - Specifications and methods of test - Part 20: Fumed silica (ISO 3262-20:2000)
This part of ISO 3262 specifies the requirements and the corresponding methods of test for fumed silica.
Füllstoffe für Beschichtungsstoffe - Anforderungen und Prüfverfahren - Teil 20: Pyrogenes Siliciumdioxid (ISO 3262- 20:2000)
Dieser Teil von ISO 3262 legt Anforderungen und die entsprechenden Prüfverfahren für pyrogenes Siliciumdioxid fest.
Matieres de charge pour peintures - Spécifications et méthodes d'essai - Partie 20: Silice pyrogénée (ISO 3262-20:2000)
La présente partie de l'ISO 3262 prescrit les spécifications et les méthodes correspondantes pour la silice
pyrogénée.
Polnila za barve - Specifikacije in metode preskušanja - 20. del: Prekajeni kremen (ISO 3262-20:2000)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 3262-20:2001
01-januar-2001
Polnila za barve - Specifikacije in metode preskušanja - 20. del: Prekajeni kremen
(ISO 3262-20:2000)
Extenders for paints - Specifications and methods of test - Part 20: Fumed silica (ISO
3262-20:2000)
Füllstoffe für Beschichtungsstoffe - Anforderungen und Prüfverfahren - Teil 20:
Pyrogenes Siliciumdioxid (ISO 3262- 20:2000)
Matieres de charge pour peintures - Spécifications et méthodes d'essai - Partie 20: Silice
pyrogénée (ISO 3262-20:2000)
Ta slovenski standard je istoveten z: EN ISO 3262-20:2000
ICS:
87.060.10 Pigmenti in polnila Pigments and extenders
SIST EN ISO 3262-20:2001 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 3262-20:2001
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SIST EN ISO 3262-20:2001
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SIST EN ISO 3262-20:2001
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SIST EN ISO 3262-20:2001
INTERNATIONAL ISO
STANDARD 3262-20
First edition
2000-04-15
Extenders for paints — Specifications
and methods of test —
Part 20:
Fumed silica
Matières de charge pour peintures — Spécifications et méthodes d'essai —
Partie 20: Silice pyrogénée
Reference number
ISO 3262-20:2000(E)
©
ISO 2000
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SIST EN ISO 3262-20:2001
ISO 3262-20:2000(E)
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ii © ISO 2000 – All rights reserved
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SIST EN ISO 3262-20:2001
ISO 3262-20:2000(E)
Contents Page
Foreword.iv
1 Scope .1
2 Normative references .1
3 Term and definition .2
4 Requirements and test methods .2
5 Sampling.3
6 Determination of silica content .3
7 Determination of aluminium oxide, titanium(IV) oxide and iron(III) oxide contents by spectrometry.4
8 Determination of carbon content .9
9 Determination of chloride content .11
10 Test report .13
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SIST EN ISO 3262-20:2001
ISO 3262-20:2000(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 3.
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 part of ISO 3262 may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
International Standard ISO 3262-20 was prepared by Technical Committee ISO/TC 35, Paints and varnishes,
Subcommittee SC 2, Pigments and extenders.
Together with the other parts (see below), this part of ISO 3262 cancels and replaces ISO 3262:1975, which has
been technically revised. Part 1 comprises the definition of the term extender and a number of test methods that
are applicable to most extenders, whilst part 2 and the following parts specify requirements and, where appropriate,
particular test methods for individual extenders.
ISO 3262 consists of the following parts, under the general title Extenders for paints — Specifications and methods
of test:
� Part 1: Introduction and general test methods
� Part 2: Barytes (natural barium sulfate)
� Part 3: Blanc fixe
� Part 4: Whiting
� Part 5: Natural crystalline calcium carbonate
� Part 6: Precipitated calcium carbonate
� Part 7: Dolomite
� Part 8: Natural clay
� Part 9: Calcined clay
� Part 10: Natural talc/chlorite in lamellar form
� Part 11: Natural talc, in lamellar form, containing carbonates
� Part 12: Muscovite-type mica
� Part 13: Natural quartz (ground)
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SIST EN ISO 3262-20:2001
ISO 3262-20:2000(E)
� Part 14: Cristobalite
� Part 15: Vitreous silica
� Part 16: Aluminium hydroxides
� Part 17: Precipitated calcium silicate
� Part 18: Precipitated sodium aluminium silicate
� Part 19: Precipitated silica
� Part 20: Fumed silica
� Part 21: Silica sand (unground natural quartz)
� Part 22: Flux-calcined kieselguhr
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SIST EN ISO 3262-20:2001
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SIST EN ISO 3262-20:2001
INTERNATIONAL STANDARD ISO 3262-20:2000(E)
Extenders for paints — Specifications and methods of test —
Part 20:
Fumed silica
1 Scope
This part of ISO 3262 specifies requirements and corresponding methods of test for fumed silica.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of
this part of ISO 3262. For dated references, subsequent amendments to, or revisions of, any of these publications
do not apply. However, parties to agreements based on this part of ISO 3262 are encouraged to investigate the
possibility of applying the most recent editions of the normative documents indicated below. For undated
references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain
registers of currently valid International Standards.
ISO 648:1977, Laboratory glassware — One-mark pipettes.
ISO 787-2:1981, General methods of test for pigments and extenders — Part 2: Determination of matter volatile at
105 °C.
ISO 787-9:1981, General methods of test for pigments and extenders — Part 9: Determination of pH value of an
aqueous suspension.
ISO 787-11:1981, General methods of test for pigments and extenders — Part 11: Determination of tamped volume
and apparent density after tamping.
ISO 787-18:1983, General methods of test for pigments and extenders — Part 18: Determination of residue on
sieve — Mechanical flushing procedure.
ISO 1042:1998, Laboratory glassware — One-mark volumetric flasks.
ISO 3262-1:1997, Extenders for paints — Specifications and methods of test — Part 1: Introduction and general
test methods.
ISO 3696:1987, Water for analytical laboratory use — Specification and test methods.
ISO 3819:1985, Laboratory glassware — Beakers.
1)
ISO 15528:— , Paints, varnishes and raw materials for paints and varnishes — Sampling.
1) To be published. (Revision of ISO 842:1984 and ISO 1512:1991)
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SIST EN ISO 3262-20:2001
ISO 3262-20:2000(E)
3 Term and definition
For the purposes of this part of ISO 3262, the following term and definition apply:
3.1
fumed silica
amorphous silica produced from silicon halides by high-temperature flame hydrolysis
4 Requirements and test methods
For fumed silica complying with this part of ISO 3262, the essential requirements are specified in Table 1 and the
conditional requirements are listed in Table 2.
Table 1 — Essential requirements
Requirement
Characteristic Unit Test method
Grade A Grade B
Silica content, min. 99,8 See clause 6
Oxide content
0,05
—Al O ,max.
2 3
—TiO ,max.
%(m/m) 0,03 Seeclause7
2
—Fe O ,max.
0,003
2 3
a
max. 0,2 min. 0,3 See clause 8
Carbon content
Chloride content, max. 0,025 See clause 9
Organic surface coating? — No Yes See clause 8
Residueon45μmsieve,max. %(m/m) 0,05 Not applicable ISO 787-18
Matter volatile at 105 °C, max. %(m/m) 3 1 ISO 787-2
Loss on ignition, max. %(m/m) 2,5 10 ISO 3262-1
b
pH value of aqueous suspension — 3,6 to 4,5 3,4 to 8 ISO 787-9
a
The carbon content is also part of the loss on ignition.
b
Usea1:1 (m/m) mixture of water and methanol.
Table 2 — Conditional requirements
Requirement
Characteristic Unit Test method
Grade A Grade B
Apparent density after
g/ml ISO 787-11
tamping
To be agreed between the interested
parties
2
Specific surface area To be agreed between the
m /g
interested parties
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SIST EN ISO 3262-20:2001
ISO 3262-20:2000(E)
5 Sampling
Take a representative sample of the product to be tested, as described in ISO 15528.
6 Determination of silica content
6.1 Principle
A test portion is ignited, weighed and treated with sulfuric acid and hydrofluoric acid. The silicon tetrafluoride thus
formed is evaporated off and the silica content is calculated from the resulting loss of mass.
As the silica content is very high, a previous separation from the impurities is not required.
6.2 Reagents
Use only reagents of recognized analytical grade and only water of at least grade 3 purity as defined in ISO 3696.
6.2.1 Sulfuric acid, diluted 1� 1.
Add 1 part by volume of concentrated sulfuric acid, approximately 96 % (m/m), ρ� 1,84 g/ml, slowly to 1 part by
volume of water.
6.2.2 Hydrofluoric acid, concentrated, approximately 40 % (m/m), ρ� 1,13 g/ml.
6.3 Apparatus
Use ordinary laboratory apparatus and glassware, together with the following:
6.3.1 Platinum dish.
6.3.2 Muffle furnace, capable of being maintained at (1 000� 20) °C.
6.3.3 Infrared evaporator.
6.3.4 Desiccator, containing magnesium perchlorate as desiccant.
6.4 Procedure
6.4.1 Number of determinations
Carry out the determination in duplicate.
6.4.2 Test portion
Weigh, to the nearest 0,2 mg, approximately 1 g (m ) of the sample (see clause 5) into the tared platinum dish
0
(6.3.1).
6.4.3 Determination
Ignite the test portion in the muffle furnace (6.3.2) at (1 000 � 20) °C to constant mass (this should take
approximately 2 h) and allow to cool in the desiccator (6.3.4). Weigh the test portion again (m ).
1
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SIST EN ISO 3262-20:2001
ISO 3262-20:2000(E)
Wet the ignited test portion in the platinum dish with 2 ml to 3 ml of water, add 1 ml of sulfuric acid (6.2.1) and 15 ml
of hydrofluoric acid (6.2.2) and evaporate to a syrup on the infrared evaporator (6.3.3), taking care to avoid loss by
spitting. Allow to cool and wash the sides down with small quantities of water. Then add a further 10 ml of
hydrofluoric acid and evaporate to dryness. If the evaporation of the silicon tetrafluoride is not complete, add a
further 10 ml of hydrofluoric acid and evaporate to dryness again.
Heat the residue until white fumes are no longer evolved, then ignite for 30 min in the muffle furnace at
(1 000� 20) °C. Remove from the furnace, allow to cool in the desiccator and weigh to the nearest 0,2 mg (m ).
2
6.5 Expression of results
Calculate the silica content w(SiO ), expressed as a percentage by mass, using the equation
2
()mm�
12
w( )= � 100
SiO
2
m
1
where
m is the mass, in grams, of the test portion after ignition;
1
m is the mass, in grams, after treatment with hydrofluoric acid and ignition.
2
Calculate the mean of the two determinations and report the result to the nearest 0,1 %.
6.6 Precision
No precision data are currently available.
7 Determination of aluminium oxide, titanium(IV) oxide and iron(III) oxide contents by
spectrometry
7.1 Principle
A test portion is treated with sulfuric acid and hydrofluoric acid in a platinum dish. The resulting silicon tetrafluoride
is volatilized and the residue is dissolved in hydrochloric acid. After diluting with water to a constant, known volume,
the Al, Ti and Fe impurities are determined either by flame atomic absorption spectrometry (FAAS) or by inductively
coupled plasma atomic emission spectrometry (ICP-AES), depending on which instrument is available in the
laboratory.
NOTE The advantages of the ICP-AES method include its wide dynamic range and multi-element capabilities. Both
methods (FAAS and ICP-AES) are relative analytical techniques. For quantitative analytical results, both measurement
techniques must be calibrated using standard matching solutions.
7.2 Reagents and materials
Use only reagents of recognized analytical grade except for acids, which shall be ultrapure, and use only water of
at least grade 3 purity as defined in ISO 3696.
7.2.1 Sulfuric acid, diluted 1 + 1.
Add 1 part by volume of concentrated sulfuric acid, approximately 96 % (m/m), ρ� 1,84 g/ml, slowly to 1 part by
volume of water.
7.2.2 Hydrofluoric acid, concentrated, approximately 40 % (m/m), ρ� 1,13 g/ml.
7.2.3 Hydrochloric acid, concentrated, approximately 30 % (m/m), ρ� 1,15 g/ml.
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SIST EN ISO 3262-20:2001
ISO 3262-20:2000(E)
7.2.4 Hydrochloric acid, dilute, approximately 3 % (m/m), ρ� 1,01 g/ml.
7.2.5 Caesium chloride buffer solution.
Dissolve 50 g of caesium chloride in approximately 500 ml of water and add 50 ml of concentrated hydrochloric
acid (7.2.3). Make up to 1 000 ml with water and mix well.
7.2.6 Standard stock solutions, containing 1,000 g/l of aluminium, titanium and iron, respectively.
Store each solution in a fluorinated-polyethylene/polypropylene (FEP) bottle.
7.2.7 Standard solutions, containing 10 mg of the element per litre.
Prepare these solutions on the day of use.
Pipette 1 ml of the appropriate standard stock solution (see 7.2.6) into a 100 ml one-mark volumetric flask, add
10 ml of concentrated hydrochloric acid (7.2.3), make up to the mark with water and mix well.
1 ml of the standard solution contains 10�g of the element concerned.
Prepare a more dilute or more concentrated standard solution, if necessary, depending on the concentration of Al,
Ti or Fe in the product under test.
7.2.8 Ethanol, 96 % (V/V).
7.2.9 Acetylene (C H ), commercial grade, in a steel cylinder.
2 2
7.2.10 Compressed air.
7.2.11 Dinitrogen oxide (N O), commercial grade, in a steel cylinder.
2
7.3 Apparatus
Use ordinary laboratory apparatus and glassware, together with the following:
7.3.1 Flame atomic absorption spectrometer (FAAS), suitable for measurements at the following wavelengths:
� 309,3 nm for al
...
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