Extenders - Specifications and methods of test - Part 20: Fumed silica (ISO 3262-20:2021)

This document specifies requirements and corresponding methods of test for fumed silica.

Füllstoffe für Beschichtungsstoffe - Anforderungen und Prüfverfahren - Teil 20: Pyrogenes Siliciumdioxid (ISO 3262-20:2021)

Dieses Dokument legt Anforderungen und die entsprechenden Prüfverfahren für pyrogenes Siliciumdioxid fest.

Matières de charge - Spécifications et méthodes d'essai - Partie 20: Silice pyrogénée (ISO 3262-20:2021)

Polnila - Specifikacije in preskusne metode - 20. del: Pirogeni silicijev dioksid (kremenčev dim) (ISO 3262-20:2021)

General Information

Status
Published
Public Enquiry End Date
02-Apr-2020
Publication Date
09-May-2021
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
03-May-2021
Due Date
08-Jul-2021
Completion Date
10-May-2021

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SLOVENSKI STANDARD
SIST EN ISO 3262-20:2021
01-junij-2021
Nadomešča:
SIST EN ISO 3262-20:2001

Polnila - Specifikacije in preskusne metode - 20. del: Pirogeni silicijev dioksid

(kremenčev dim) (ISO 3262-20:2021)

Extenders - Specifications and methods of test - Part 20: Fumed silica (ISO 3262-

20:2021)
Füllstoffe für Beschichtungsstoffe - Anforderungen und Prüfverfahren - Teil 20:
Pyrogenes Siliciumdioxid (ISO 3262-20:2021)

Matières de charge - Spécifications et méthodes d'essai - Partie 20: Silice pyrogénée

(ISO 3262-20:2021)
Ta slovenski standard je istoveten z: EN ISO 3262-20:2021
ICS:
87.060.10 Pigmenti in polnila Pigments and extenders
SIST EN ISO 3262-20:2021 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN ISO 3262-20:2021
---------------------- Page: 2 ----------------------
SIST EN ISO 3262-20:2021
EN ISO 3262-20
EUROPEAN STANDARD
NORME EUROPÉENNE
April 2021
EUROPÄISCHE NORM
ICS 87.060.10 Supersedes EN ISO 3262-20:2000
English Version
Extenders - Specifications and methods of test - Part 20:
Fumed silica (ISO 3262-20:2021)

Matières de charge - Spécifications et méthodes d'essai Füllstoffe für Beschichtungsstoffe - Anforderungen und

- Partie 20: Silice pyrogénée (ISO 3262-20:2021) Prüfverfahren - Teil 20: Pyrogenes Siliciumdioxid (ISO

3262-20:2021)
This European Standard was approved by CEN on 19 March 2021.

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. Up-to-date lists and bibliographical references

concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN

member.

This European Standard exists 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-CENELEC Management

Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 3262-20:2021 E

worldwide for CEN national Members.
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SIST EN ISO 3262-20:2021
EN ISO 3262-20:2021 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

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SIST EN ISO 3262-20:2021
EN ISO 3262-20:2021 (E)
European foreword

This document (EN ISO 3262-20:2021) has been prepared by Technical Committee ISO/TC 256

"Pigments, dyestuffs and extenders" in collaboration with Technical Committee CEN/TC 298 “Pigments

and extenders” the secretariat of which is held by DIN.

This European Standard shall be given the status of a national standard, either by publication of an

identical text or by endorsement, at the latest by October 2021, and conflicting national standards shall

be withdrawn at the latest by October 2021.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN ISO 3262-20:2000.

According to the CEN-CENELEC Internal Regulations, the national standards organizations of the

following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,

Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,

Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of

North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the

United Kingdom.
Endorsement notice

The text of ISO 3262-20:2021 has been approved by CEN as EN ISO 3262-20:2021 without any

modification.
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SIST EN ISO 3262-20:2021
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SIST EN ISO 3262-20:2021
INTERNATIONAL ISO
STANDARD 3262-20
Second edition
2021-03
Extenders — Specifications and
methods of test —
Part 20:
Fumed silica
Matières de charge — Spécifications et méthodes d'essai —
Partie 20: Silice pyrogénée
Reference number
ISO 3262-20:2021(E)
ISO 2021
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SIST EN ISO 3262-20:2021
ISO 3262-20:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 3262-20:2021
ISO 3262-20:2021(E)
Contents  Page

Foreword ..........................................................................................................................................................................................................................................v

1  Scope ................................................................................................................................................................................................................................. 1

2  Normative references ...................................................................................................................................................................................... 1

3  Terms and definitions ..................................................................................................................................................................................... 1

4  Requirements and test methods .......................................................................................................................................................... 2

5  Sampling ........................................................................................................................................................................................................................ 2

6  Determination of silica content ............................................................................................................................................................ 2

6.1 Principle ........................................................................................................................................................................................................ 2

6.2 Reagents........................................................................................................................................................................................................ 3

6.3 Apparatus .................................................................................................................................................................................................... 3

6.4 Procedure .................................................................................................................................................................................................... 3

6.4.1 Number of determinations...................................................................................................................................... 3

6.4.2 Test portion .......................................................................................................................................................................... 3

6.4.3 Determination .................................................................................................................................................................... 3

6.5 Expression of results .......................................................................................................................................................................... 4

6.6 Precision ....................................................................................................................................................................................................... 4

7  Determination of aluminium oxide, titanium (IV) oxide and iron (III) oxide

contents by spectrometry ........................................................................................................................................................................... 4

7.1 Principle ........................................................................................................................................................................................................ 4

7.2 Reagents and materials ................................................................................................................................................................... 4

7.3 Apparatus .................................................................................................................................................................................................... 5

7.4 Procedure .................................................................................................................................................................................................... 6

7.4.1 Preparation of standard matching solutions ........................................................................................... 6

7.4.2 Spectrometric measurement ................................................................................................................................. 6

7.4.3 Calibration graph ............................................................................................................................................................. 7

7.4.4 Preparation of the test solution .......................................................................................................................... 7

7.4.5 Determination of aluminium, titanium and iron .................................................................................. 7

7.4.6 Determination of the total loss on ignition ............................................................................................... 7

7.5 Expression of results .......................................................................................................................................................................... 8

7.5.1 Calculation of the concentration of each element ............................................................................... 8

7.5.2 Calculation of the oxide content for each element ............................................................................. 8

7.6 Precision ....................................................................................................................................................................................................... 9

8  Determination of carbon content ....................................................................................................................................................... 9

8.1 Principle ........................................................................................................................................................................................................ 9

8.2 Reagents and materials ................................................................................................................................................................... 9

8.3 Apparatus .................................................................................................................................................................................................10

8.4 Procedure .................................................................................................................................................................................................10

8.4.1 Preparation of apparatus .......................................................................................................................................10

8.4.2 Calibration ..........................................................................................................................................................................10

8.4.3 Determination .................................................................................................................................................................10

8.5 Expression of results .......................................................................................................................................................................10

8.6 Precision ....................................................................................................................................................................................................11

9  Determination of chloride content .................................................................................................................................................11

9.1 Principle .....................................................................................................................................................................................................11

9.2 Reagents.....................................................................................................................................................................................................11

9.3 Apparatus .................................................................................................................................................................................................11

9.4 Procedure .................................................................................................................................................................................................12

9.4.1 Number of determinations...................................................................................................................................12

9.4.2 Test portion .......................................................................................................................................................................12

9.4.3 Determination .................................................................................................................................................................12

9.5 Expression of results .......................................................................................................................................................................12

© ISO 2021 – All rights reserved iii
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SIST EN ISO 3262-20:2021
ISO 3262-20:2021(E)

9.6 Precision ....................................................................................................................................................................................................13

10  Test report ................................................................................................................................................................................................................13

iv © ISO 2021 – All rights reserved
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SIST EN ISO 3262-20:2021
ISO 3262-20:2021(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.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

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. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 256, Pigments, dyestuff and extenders,

in collaboration with the European Committee for Standardization (CEN) Technical Committee CEN/

TC 298, Pigments and extenders, in accordance with the Agreement on technical cooperation between

ISO and CEN (Vienna Agreement).

This second edition cancels and replaces the first edition (ISO 3262-20:2000), which has been

technically revised.
The main changes compared to the previous edition are as follows:
— the main title has been changed from "Extenders for paints" to "Extenders";

— in Table 1, carbon content has been revised and organic surface has been refined;

— in 6.3.4, magnesium perchlorate has been changed to an example for a desiccant;

— in 8.2.3, suitable examples for carbon steel have been added;

— the text has been editorially revised and the normative references have been updated.

A list of all parts in the ISO 3262 series can be found on the ISO website.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
© ISO 2021 – All rights reserved v
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SIST EN ISO 3262-20:2021
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SIST EN ISO 3262-20:2021
INTERNATIONAL STANDARD ISO 3262-20:2021(E)
Extenders — Specifications and methods of test —
Part 20:
Fumed silica
1  Scope

This document specifies requirements and corresponding methods of test for fumed silica.

2  Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements 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 648, Laboratory glassware — Single-volume pipettes

ISO 787-2, General methods of test for pigments and extenders — Part 2: Determination of matter volatile

at 105 °C

ISO 787-9, General methods of test for pigments and extenders — Part 9: Determination of pH value of an

aqueous suspension

ISO 787-11, General methods of test for pigments and extenders — Part 11: Determination of tamped

volume and apparent density after tamping

ISO 787-18, General methods of test for pigments and extenders — Part 18: Determination of residue on

sieve — Mechanical flushing procedure
ISO 1042, Laboratory glassware — One-mark volumetric flasks

ISO 3262-1, Extenders — Specifications and methods of test — Part 1: Introduction and general test methods

ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 3819, Laboratory glassware — Beakers

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

ISO 18451-1, Pigments, dyestuffs and extenders — Terminology — Part 1: General terms

3  Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 18451-1 and the following apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
3.1
fumed silica

amorphous silica produced from silicon halides by high-temperature flame hydrolysis

© ISO 2021 – All rights reserved 1
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SIST EN ISO 3262-20:2021
ISO 3262-20:2021(E)
4  Requirements and test methods

For fumed silica complying with this document, the essential requirements are specified in Table 1 and

the conditional requirements are listed in Table 2.

In order to determine the pH value in an aqueous suspension, a 1 + 1 mass fraction mixture of water

and methanol is used.
Table 1 — Essential requirements and test methods
Characteristic Unit Requirement Test method
Grade A Grade B
according to
Silica content, min. 99,8 Clause 6
Oxide content
max. 0,05
— Al O
2 3
Clause 7
% mass
— TiO max. 0,03
fraction
— Fe O max. 0,003
2 3
a b
Carbon content <0,3 ≥0,3 Clause 8
Chloride content max. 0,025 Clause 9
Organic surface treatment or
— No Yes Clause 8
surface coating
% mass
Residue on 45 µm sieve max. 0,05 Not applicable ISO 787-18
fraction
% mass
Matter volatile at 105 °C max. 3 max. 1 ISO 787-2
fraction
% mass
Loss on ignition max. 2,5 max. 10 ISO 3262-1
fraction
pH value of aqueous suspension — 3,6 to 4,5 3,4 to 8 ISO 787-9
The carbon content is also part of the loss on ignition.
Usually does not exceed 15 %.
Table 2 — Conditional requirements and test methods
Characteristic Unit Requirement Test method
Grade A Grade B
according to
Apparent density after tamping g/ml ISO 787-11
To be agreed between
To be agreed between
2 the interested parties
Specific surface area m /g
the interested parties
5  Sampling
Take a representative sample of the product to be tested according to 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 impurities is

not required.
2 © ISO 2021 – All rights reserved
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SIST EN ISO 3262-20:2021
ISO 3262-20:2021(E)
6.2  Reagents

WARNING — Hydrofluoric acid is corrosive and toxic. The related operations shall be

performed in fume hood. This document does not point out all possible safety problems. It is

the responsibility of the user to take proper safety and health measures and to determine the

applicability of regulatory limitations prior to use.

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 (H SO), CAS-No 7664-93-9 , diluted 1 + 1.
2 4

Add 1 part by volume of concentrated sulfuric acid, approximately 96 % mass fraction ρ ≈ 1,84 g/ml,

slowly to 1 part by volume of water.

6.2.2  Hydrofluoric acid (HF), CAS-No 7664-39-3, concentrated, approximately 40 % mass fraction

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 for example 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 (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 takes

approximately 2 h) and allow to cool in the desiccator (6.3.4). Weigh the test portion again (m ).

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 ).
1) CAS-No – Chemical Abstracts Service Registry Number.
© ISO 2021 – All rights reserved 3
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SIST EN ISO 3262-20:2021
ISO 3262-20:2021(E)
6.5  Expression of results

Calculate the silica content w (SiO ), expressed as a mass fraction in percent, using Formula (1):

mm−
w SiO = ×100 (1)
where
m is the mass, in grams, of the test portion after ignition;
m is the mass, in grams, after treatment with hydrofluoric acid and ignition.

Calculate the mean of the two determinations and report the result to the nearest 0,1 %.

6.6  Precision
No precision data are available at the time of publication.
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 volatized 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.

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 shall 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 according to ISO 3696.
7.2.1  Sulfuric acid (H SO), CAS-No 7664-93-9, diluted 1 + 1.
2 4

Add 1 part by volume of concentrated sulfuric acid, approximately 96% mass fraction, ρ ≈ 1,84 g/ml,

slowly to 1 part by volume of water.

7.2.2  Hydrofluoric acid (HF), CAS-No 7664-39-3, concentrated, approximately 40 % mass fraction,

ρ ≈ 1,13 g/ml.

7.2.3  Hydrochloric acid (HCl), CAS-No 7647-01-0, concentrated, approximately 30 % mass fraction,

ρ ≈ 1,15 g/ml.

7.2.4  Hydrochloric acid (HCl), CAS-No 7647-01-0, diluted, approximately 3 % mass fraction,

ρ ≈ 1,01 g/ml.
4 © ISO 2021 – All rights reserved
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SIST EN ISO 3262-20:2021
ISO 3262-20:2021(E)
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 µg 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 % volume fraction.
7.2.9  Acetylene (C H), commercial grade, in a steel cylinder.
2 2
7.2.10 Compressed air.
7.2.11 Dinitrogen oxide (NO), commercial grade, in a steel cylinder.
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
...

SLOVENSKI STANDARD
oSIST prEN ISO 3262-20:2020
01-marec-2020

Polnila - Specifikacije in preskusne metode - 20. del: Pirogeni silicijev dioksid

(kremenčev dim) (ISO/DIS 3262-20:2020)

Extenders - Specifications and methods of test - Part 20: Fumed silica (ISO/DIS 3262-

20:2020)
Füllstoffe für Beschichtungsstoffe - Anforderungen und Prüfverfahren - Teil 20:
Pyrogenes Siliciumdioxid (ISO/DIS 3262-20:2020)

Matières de charge - Spécifications et méthodes d'essai - Partie 20: Silice pyrogénée

(ISO/DIS 3262-20:2020)
Ta slovenski standard je istoveten z: prEN ISO 3262-20
ICS:
87.060.10 Pigmenti in polnila Pigments and extenders
oSIST prEN ISO 3262-20:2020 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
oSIST prEN ISO 3262-20:2020
---------------------- Page: 2 ----------------------
oSIST prEN ISO 3262-20:2020
DRAFT INTERNATIONAL STANDARD
ISO/DIS 3262-20
ISO/TC 256 Secretariat: DIN
Voting begins on: Voting terminates on:
2020-01-31 2020-04-24
Extenders — Specifications and methods of test —
Part 20:
Fumed silica
Matières de charge pour peintures — Spécifications et méthodes d'essai —
Partie 20: Silice pyrogénée
ICS: 87.060.10
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
ISO/CEN PARALLEL PROCESSING
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 3262-20:2020(E)
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 2020
---------------------- Page: 3 ----------------------
oSIST prEN ISO 3262-20:2020
ISO/DIS 3262-20:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 4 ----------------------
oSIST prEN ISO 3262-20:2020
ISO/DIS 3262-20:2020(E)
Contents  Page

Foreword ........................................................................................................................................................................................................................................iv

1  Scope ................................................................................................................................................................................................................................. 1

2  Normative references ...................................................................................................................................................................................... 1

3  Terms and definitions ..................................................................................................................................................................................... 1

4  Requirements and test methods .......................................................................................................................................................... 2

5  Sampling ........................................................................................................................................................................................................................ 2

6  Determination of silica content ............................................................................................................................................................ 2

6.1 Principle ........................................................................................................................................................................................................ 2

6.2 Reagents........................................................................................................................................................................................................ 3

6.3 Apparatus .................................................................................................................................................................................................... 3

6.4 Procedure .................................................................................................................................................................................................... 3

6.5 Expression of results .......................................................................................................................................................................... 4

6.6 Precision ....................................................................................................................................................................................................... 4

7  Determination of aluminium oxide, titanium (IV) oxide and iron (III) oxide

contents by spectrometry ........................................................................................................................................................................... 4

7.1 Principle ........................................................................................................................................................................................................ 4

7.2 Reagents and materials ................................................................................................................................................................... 4

7.3 Apparatus .................................................................................................................................................................................................... 5

7.4 Procedure .................................................................................................................................................................................................... 6

7.5 Expression of results .......................................................................................................................................................................... 8

7.6 Precision ....................................................................................................................................................................................................... 8

8  Determination of carbon content ....................................................................................................................................................... 9

8.1 Principle ........................................................................................................................................................................................................ 9

8.2 Reagents and materials ................................................................................................................................................................... 9

8.3 Apparatus .................................................................................................................................................................................................... 9

8.4 Procedure .................................................................................................................................................................................................10

8.5 Expression of results .......................................................................................................................................................................10

8.6 Precision ....................................................................................................................................................................................................10

9  Determination of chloride content .................................................................................................................................................11

9.1 Principle .....................................................................................................................................................................................................11

9.2 Reagents.....................................................................................................................................................................................................11

9.3 Apparatus .................................................................................................................................................................................................11

9.4 Procedure .................................................................................................................................................................................................11

9.5 Expression of results .......................................................................................................................................................................12

9.6 Precision ....................................................................................................................................................................................................12

10  Test report ................................................................................................................................................................................................................12

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oSIST prEN ISO 3262-20:2020
ISO/DIS 3262-20:2020(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.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

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. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 256, Pigments, dyestuff and extenders.

This second edition cancels and replaces the first edition (ISO 3262-20:2000), which has been

technically revised.
The main changes compared to the previous edition are as follows:
— the main title has been changed from "Extenders for paints" to "Extenders";

— in Table 1 carbon content has been revised and organic surface has been refined;

— in 6.3.4 magnesium perchlorate has been changed to an example for a desiccant;
— in 8.2.3 suitable examples for carbon steel have been added;

— the text has been editorially revised and the normative references have been updated.

A list of all parts in the ISO 3262 series can be found on the ISO website.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2020 – All rights reserved
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oSIST prEN ISO 3262-20:2020
DRAFT INTERNATIONAL STANDARD ISO/DIS 3262-20:2020(E)
Extenders — Specifications and methods of test —
Part 20:
Fumed silica
1  Scope

This document specifies requirements and corresponding methods of test for fumed silica.

2  Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements 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 648, Laboratory glassware — Single-volume pipettes

ISO 787-2, General methods of test for pigments and extenders — Part 2: Determination of matter volatile

at 105 degrees C

ISO 787-9, General methods of test for pigments and extenders — Part 9: Determination of pH value of an

aqueous suspension

ISO 787-11, General methods of test for pigments and extenders — Part 11: Determination of tamped

volume and apparent density after tamping

ISO 787-18, General methods of test for pigments and extenders — Part 18: Determination of residue on

sieve — Mechanical flushing procedure
ISO 1042, Laboratory glassware — One-mark volumetric flasks

ISO 3262-1, Extenders for paints — Specifications and methods of test — Part 1: Introduction and general

test methods
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 3819, Laboratory glassware — Beakers

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

ISO 18451-1, Pigments, dyestuffs and extenders — Terminology — Part 1: General terms

3  Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 18451-1 and the following apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— IEC Electropedia: available at http:// www .electropedia .org/
— ISO Online browsing platform: available at http:// www .iso .org/ obp
3.1
fumed silica

amorphous silica produced from silicon halides by high-temperature flame hydrolysis

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oSIST prEN ISO 3262-20:2020
ISO/DIS 3262-20:2020(E)
4  Requirements and test methods

For fumed silica complying with this document, the essential requirements are specified in Table 1 and

the conditional requirements are listed in Table 2.
Table 1 — Essential requirements
Characteristic Unit Requirement Test method
Grade A Grade B
Silica content, min. 99,8 Clause 6
Oxide content
max. 0,05
— Al O
2 3
Clause 7
%(mass
— TiO max. 0,03
fraction)
— Fe O max. 0,003
2 3
a b
Carbon content < 0,3 ≥ 0,3 Clause 8
Chloride content max. 0,025 Clause 9
Organic surface treatment or
— No Yes Clause 8
surface coating
%(mass
Residue on 45 µm sieve max. 0,05 Not applicable ISO 787-18
fraction)
%(mass
Matter volatile at 105 °C max. 3 max. 1 ISO 787-2
fraction)
%(mass
Loss on ignition max. 2,5 max. 10 ISO 3262-1
fraction)
pH value of aqueous suspension — 3,6 to 4,5 3,4 to 8 ISO 787-9
The carbon content is also part of the loss on ignition.
Usually does not exceed 15 %.
Use a 1:1 (mass fraction) mixture of water and methanol.
Table 2 — Conditional requirements
Characteristic Unit Requirement Test method
Grade A Grade B
Apparent density after tamping g/ml ISO 787-11
To be agreed between
To be agreed between
the interested parties
Specific surface area m /g
the interested parties
5  Sampling
Take a representative sample of the product to be tested according to ISO 15528.
6  Determination of silica content
6.1  Principle

A test portion is ignited, weighed and treated with sulphuric acid and hydrofluoric acid. The silicon

tetrafluoride thus formed is evaporated off and the silica content is calculated from the impurities is

not required.
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oSIST prEN ISO 3262-20:2020
ISO/DIS 3262-20:2020(E)
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 sulphuric acid, approximately 96 % (mass fraction) ρ ≈ 1,84 g/ml,

slowly to 1 part by volume of water.

6.2.2  Hydrofluoric acid, concentrated, approximately 40 % (mass fraction) 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 for example 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 (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 ).

Wet the ignited test portion in the platinum dish with 2 ml to 3 ml of water, add 1 ml of sulphuric 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 ).
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oSIST prEN ISO 3262-20:2020
ISO/DIS 3262-20:2020(E)
6.5  Expression of results

Calculate the silica content w (SiO ), expressed as a percentage mass fraction, using Formula (1):

mm−
w SiO = ×100 (1)
where
m is the mass, in grams, of the test portion after ignition;
m is the mass, in grams, after treatment with hydrofluoric acid and ignition.

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 sulphuric acid and hydrofluoric acid in a platinum dish. The resulting

silicon tetrafluoride is volatized and the residue is dissolved in hydrochloric acid. After diluting with

water to a con
...

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