EN ISO 3262-19:2000
(Main)Extenders for paints - Specifications and methods of test - Part 19: Precipitated silica (ISO 3262-19:2000)
Extenders for paints - Specifications and methods of test - Part 19: Precipitated silica (ISO 3262-19:2000)
This part of ISO 3262 specifies requirements and corresponding methods of test for precipitated silica.
Füllstoffe für Beschichtungsstoffe - Anforderungen und Prüfverfahren - Teil 19: Gefällte Kieselsäure (ISO 3262-19:2000)
Dieser Teil von ISO 3262 legt Anforderungen und die entsprechenden Prüfverfahren für gefällte Kieselsäure fest.
Matières de charge pour peintures - Spécifications et méthodes d'essai - Partie 19: Silice précipité (ISO 3262-19:2000)
La présente partie de l'ISO 3262 prescrit les spécifications et les méthodes d'essai correspondantes pour la silice
précipitée.
Polnila za barve - Specifikacije in metode preskušanja - 19. del: Oborjeni kremen (ISO 3262-19:2000)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-januar-2001
Polnila za barve - Specifikacije in metode preskušanja - 19. del: Oborjeni kremen
(ISO 3262-19:2000)
Extenders for paints - Specifications and methods of test - Part 19: Precipitated silica
(ISO 3262-19:2000)
Füllstoffe für Beschichtungsstoffe - Anforderungen und Prüfverfahren - Teil 19: Gefällte
Kieselsäure (ISO 3262-19:2000)
Matieres de charge pour peintures - Spécifications et méthodes d'essai - Partie 19: Silice
précipité (ISO 3262-19:2000)
Ta slovenski standard je istoveten z: EN ISO 3262-19:2000
ICS:
87.060.10 Pigmenti in polnila Pigments and extenders
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
INTERNATIONAL ISO
STANDARD 3262-19
First edition
2000-04-15
Extenders for paints — Specifications
and methods of test —
Part 19:
Precipitated silica
Matières de charge pour peintures — Spécifications et méthodes d'essai —
Partie 19: Silice précipitée
Reference number
ISO 3262-19:2000(E)
©
ISO 2000
ISO 3262-19:2000(E)
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ii © ISO 2000 – All rights reserved
ISO 3262-19:2000(E)
Contents Page
Foreword.iv
1 Scope .1
2 Normative references .1
3 Term and definition .1
4 Requirements and test methods .2
5 Sampling.2
6 Determination of silica content .3
7 Determination of carbon content .5
8 Determination of residue on sieve.7
9 Test report .9
ISO 3262-19:2000(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 3262-19 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)
iv © ISO 2000 – All rights reserved
ISO 3262-19:2000(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
INTERNATIONAL STANDARD ISO 3262-19:2000(E)
Extenders for paints — Specifications and methods of test —
Part 19:
Precipitated silica
1 Scope
This part of ISO 3262 specifies requirements and corresponding methods of test for precipitated 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 787-2:1981, General methods of test for pigments and extenders — Part 2: Determination of matter volatile at
105 °C.
ISO 787-5:1980, General methods of test for pigments and extenders — Part 5: Determination of oil absorption
value.
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 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 5794-1:1994, Rubber compounding ingredients — Silica, precipitated, hydrated — Part 1: Non-rubber tests.
1)
ISO 15528:— , Paints, varnishes and raw materials for paints and varnishes — Sampling.
3 Term and definition
For the purposes of this part of ISO 3262, the following term and definition apply:
3.1
precipitated silica
amorphous silica precipitated by reaction of sodium silicate solution with a mineral acid and/or carbon dioxide
1) To be published. (Revision of ISO 842:1984 and ISO 1512:1991)
ISO 3262-19:2000(E)
4 Requirements and test methods
For precipitated 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. 95 95 See clause 6
%(m/m)
a
max. 0,2 min. 0,3 See clause 7
Carbon content
Organic surface coating? — No Yes See clause 7
Matter volatile at 105 °C, max. %(m/m) 8 ISO 787-2
%(m/m)
Loss on ignition 3 to 8 3 to 15 ISO 3262-1
b
g/100 g 120 ISO 787-5
Oil absorption value ,min.
c
— 3,5 to 9 ISO 787-9
pH value of aqueous suspension
a
The carbon content is also part of the loss on ignition.
b
A test method with higher reproducibility and repeatability is described in ASTM D 2414-97, Standard test method for carbon black —
n-Dibutyl phthalate absorption number. However, the results cannot be compared directly with oil absorption values determined in accordance
with ISO 787-5.
c
For hydrophobic silicas, use a 1:1 (m/m) mixture by mass of water and methanol.
Table 2 — Conditional requirements
Requirement
Characteristic Unit Test method
Grade A Grade B
Residueon45μmsieve, To be agreed
a
max. %(m/m) between the Not applicable
Spray method (see clause 8)
interested parties
Particle size distribution
%(m/m) To be agreed between the interested parties
(instrumental method)
Apparent density after
g/ml ISO 787-11
To be agreed between the interested
tamping
parties
Specific surface area ISO 5794-1:1994, annex D
m /g
a
Only for hydrophylic materials.
5 Sampling
Take a representative sample of the product to be tested, as described in ISO 15528.
2 © ISO 2000 – All rights reserved
ISO 3262-19:2000(E)
6 Determination of silica content
6.1 Principle
A test portion is repeatedly treated with hydrochloric acid and evaporated to dryness. To render the dehydrated
silicic acid thus formed as insoluble as possible, it is then heated for 2 h at (140� 5) °C. Any chlorides present are
removed by extracting the precipitate with hot dilute hydrochloric acid.
The precipitate is ignited at 1 000 °C, giving impure silicon dioxide, which is treated with sulfuric and hydrofluoric
acid. The silicon tetrafluoride formed is evaporated off and the silica content is calculated from the resulting loss in
mass.
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 Hydrochloric acid, concentrated, approximately 32 % (m/m), ρ� 1,16 g/ml.
6.2.2 Hydrochloric acid, diluted 1� 1.
Add 1 part by volume of concentrated hydrochloric acid (6.2.1) to 1 part by volume of water.
6.2.3 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.
6.2.4 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 Dish.
6.3.2 Platinum crucible.
6.3.3 Water bath, capable of being maintained at 100 °C.
6.3.4 Infrared evaporator.
6.3.5 Muffle furnace, capable of being maintained at (1 000� 20) °C.
6.3.6 Drying oven, capable of being maintained at (140� 5) °C.
6.3.7 Filter paper.
The filter paper used for filtration of the silica shall be of such texture as to retain the smallest particles of
2)
precipitate and nevertheless permit rapid filtration.
6.3.8 Desiccator, containing magnesium perchlorate as desiccant.
2) For example Whatman No. 40 or 41 or Schleicher und Schüll No. 589/2 "Weißband".
ISO 3262-19:2000(E)
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 a dish (6.3.1).
6.4.3 Determination
Add slowly 20 ml of concentrated hydrochloric acid (6.2.1) and evaporate to dryness under the infrared evaporator
(6.3.4). Add again 20 ml of concentrated hydrochloric acid and evaporate to dryness. Repeat this step once more.
After the third evaporation, place the dish in the drying oven (6.3.6), maintained at (140� 5) °C, and leave for 2 h.
Remove the dish from the oven and allow to cool. Add 50 ml of 1� 1 hydrochloric acid (6.2.2) to the residue in the
dish and warm it for approximately 20 min on the water bath (6.3.3) at 100 °C. Filter through a suitable filter paper
(6.3.7) and wash the residue on the filter with hot water until the washings are neutral.
Pour the filtrate and washings into the original dish and evaporate to dryness. Repeat this evaporation step another
two times, adding each time 10 ml of concentrated hydrochloric acid to the residue. After the third evaporation, heat
at (140� 5) °C for 2 h in the drying oven.
Add 20 ml
...
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