SIST EN ISO 3451-1:2019

Plastics - Determination of ash - Part 1: General methods (ISO 3451-1:2019)

This document specifies general methods, with suitable test conditions, for the determination of the
ash of a range of plastics. The particular conditions chosen can be included in the specifications for the
plastic material in question.
Particular conditions applicable to poly(alkylene terephthalate) materials, unplasticized cellulose
acetate, polyamides and poly(vinyl chloride) plastics, including some specific filled, glass-fibrereinforced
and flame-retarded materials, are specified in ISO 3451-2, ISO 3451-3, ISO 3451-4 and
ISO 3451-5.

Kunststoffe - Bestimmung der Asche - Teil 1: Allgemeine Grundlagen (ISO 3451-1:2019)

Plastiques - Détermination du taux de cendres - Partie 1: Méthodes générales (ISO 3451-1:2019)

Le présent document spécifie des méthodes générales et les conditions d'essai appropriées correspondantes qui permettent de déterminer le taux de cendres d'une gamme de plastiques. Les conditions particulières choisies peuvent figurer dans les spécifications relatives au matériau plastique considéré.
Les conditions particulières applicables aux matières poly(téréphtalates d'alkylène), à l'acétate de cellulose non plastifié, aux polyamides et au poly(chlorures de vinyle), y compris certaines matières contenant des charges spécifiques, renforcées de fibres de verre et ignifugées, sont spécifiées dans l'ISO 3451‑2, l'ISO 3451‑3, l'ISO 3451‑4 et l'ISO 3451‑5.

Polimerni materiali - Določevanje pepela - 1. del: Splošne metode (ISO 3451-1:2019)

Ta dokument določa splošne metode, s primernimi preskusnimi pogoji, za določevanje
pepela v polimernih materialih. Izbrani pogoji se lahko vključijo v specifikacije za uporabljeni polimerni material.
Posebni pogoji, ki se uporabljajo za materiale na osnovi poli(alkilentereftalata), za nemehčani celulozni acetat, poliamide in za materiale na osnovi mehčanega polivinilklorida, vključno z nekaterimi specifičnimi polnjenimi materiali, ojačenimi s steklenimi vlakni in z ognjeodpornimi materiali, so določeni v standardih ISO 3451-2, ISO 3451-3, ISO 3451-4 in ISO 3451-5.

General Information

• Status: Published
• Public Enquiry End Date: 27-Jun-2018
• Publication Date: 27-Mar-2019
• ICS: 83.080.01 - Plastics in general
• Technical Committee: IPMA - Polimer materials and products
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 15-Mar-2019
• Due Date: 20-May-2019
• Completion Date: 28-Mar-2019
• Ref Project: EN ISO 3451-1:2019 - Plastics - Determination of ash - Part 1: General methods (ISO 3451-1:2019)

Relations

• Revised: SIST EN ISO 3451-1:2008 - Plastics - Determination of ash - Part 1: General methods (ISO 3451-1:2008)
• Effective Date: 04-May-2016
• Replaces: SIST EN ISO 3451-1:2008 - Plastics - Determination of ash - Part 1: General methods (ISO 3451-1:2008)
• Effective Date: 13-Mar-2019

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 3451-1:2019
01-maj-2019
1DGRPHãþD
SIST EN ISO 3451-1:2008
3ROLPHUQLPDWHULDOL'RORþHYDQMHSHSHODGHO6SORãQHPHWRGH,62

Plastics - Determination of ash - Part 1: General methods (ISO 3451-1:2019)
Kunststoffe - Bestimmung der Asche - Teil 1: Allgemeine Grundlagen (ISO 3451-1:2019)
Plastiques - Détermination du taux de cendres - Partie 1: Méthodes générales (ISO 3451
-1:2019)
Ta slovenski standard je istoveten z: EN ISO 3451-1:2019
ICS:
83.080.01 Polimerni materiali na Plastics in general
splošno
SIST EN ISO 3451-1:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 3451-1:2019

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SIST EN ISO 3451-1:2019


EN ISO 3451-1
EUROPEAN STANDARD

NORME EUROPÉENNE

March 2019
EUROPÄISCHE NORM
ICS 83.080.01 Supersedes EN ISO 3451-1:2008
English Version

Plastics - Determination of ash - Part 1: General methods
(ISO 3451-1:2019)
Plastiques - Détermination du taux de cendres - Partie Kunststoffe - Bestimmung der Asche - Teil 1:
1: Méthodes générales (ISO 3451-1:2019) Allgemeine Verfahren (ISO 3451-1:2019)
This European Standard was approved by CEN on 15 February 2019.

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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, 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
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 3451-1:2019 E
worldwide for CEN national Members.

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SIST EN ISO 3451-1:2019
EN ISO 3451-1:2019 (E)
Contents Page
European foreword . 3

2

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SIST EN ISO 3451-1:2019
EN ISO 3451-1:2019 (E)
European foreword
This document (EN ISO 3451-1:2019) has been prepared by Technical Committee ISO/TC 61 "Plastics"
in collaboration with Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by
NBN.
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 September 2019, and conflicting national standards
shall be withdrawn at the latest by September 2019.
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 3451-1:2008.
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, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 3451-1:2019 has been approved by CEN as EN ISO 3451-1:2019 without any
modification.


3

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SIST EN ISO 3451-1:2019

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SIST EN ISO 3451-1:2019
INTERNATIONAL ISO
STANDARD 3451-1
Fifth edition
2019-02
Plastics — Determination of ash —
Part 1:
General methods
Plastiques — Détermination du taux de cendres —
Partie 1: Méthodes générales
Reference number
ISO 3451-1:2019(E)
©
ISO 2019

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SIST EN ISO 3451-1:2019
ISO 3451-1:2019(E)

COPYRIGHT PROTECTED DOCUMENT
© ISO 2019
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: [phone]
Fax: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved

---------------------- Page: 8 ----------------------

SIST EN ISO 3451-1:2019
ISO 3451-1:2019(E)

Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents (for methods B and C only) . 2
6 Apparatus . 2
7 Procedure. 3
7.1 Test portion . 3
7.2 Test conditions . 4
7.3 Method A — Direct calcination . 5
7.4 Method B — Calcination following sulfuric acid treatment after burning . 5
7.5 Method C — Calcination following sulfuric acid treatment before burning . 6
7.6 Method D —Automated instrument method . 6
8 Number of tests . 7
9 Expression of results . 7
10 Precision . 7
11 Test report . 8
Bibliography . 9
© ISO 2019 – All rights reserved iii

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SIST EN ISO 3451-1:2019
ISO 3451-1:2019(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 61, Plastics, Subcommittee SC 5, Physical-
chemical properties.
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.
This fifth edition cancels and replaces the fourth edition (ISO 3451-1:2008), which has been technically
revised by adding an automated instrument method (Method D).
A list of all parts in the ISO 3451 series can be found on the ISO website.
iv © ISO 2019 – All rights reserved

---------------------- Page: 10 ----------------------

SIST EN ISO 3451-1:2019
INTERNATIONAL STANDARD ISO 3451-1:2019(E)
Plastics — Determination of ash —
Part 1:
General methods
SAFETY PRECAUTIONS — Persons using this document should be familiar with normal laboratory
practice, if applicable. This document does not purport to address all of the safety concerns, if
any, associated with its use. It is the responsibility of the user to establish appropriate safety
and health practices.
1 Scope
This document specifies general methods, with suitable test conditions, for the determination of the
ash of a range of plastics. The particular conditions chosen can be included in the specifications for the
plastic material in question.
Particular conditions applicable to poly(alkylene terephthalate) materials, unplasticized cellulose
acetate, polyamides and poly(vinyl chloride) plastics, including some specific filled, glass-fibre-
reinforced and flame-retarded materials, are specified in ISO 3451-2, ISO 3451-3, ISO 3451-4 and
ISO 3451-5.
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 472, Plastics — Vocabulary
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 472 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/
4 Principle
It is possible to determine the ash of an organic material by four main methods (methods A, B, C and D).
a) Direct calcination, i.e. by burning the organic matter and heating the residue at high temperature
until constant mass is reached, which may be carried out by two different procedures:
— burning with, for example, a Bunsen burner and one or more calcining steps in a muffle furnace
(method A);
— burning and calcining as one single step in a muffle furnace (method A — rapid ashing), if it can
be demonstrated that the rapid ashing yields the same results as method A.
© ISO 2019 – All rights reserved 1

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SIST EN ISO 3451-1:2019
ISO 3451-1:2019(E)

b) Calcination after sulfation, which may be carried out by two different procedures:
— with sulfuric acid treatment after burning, i.e. by burning the organic matter, transforming the
inorganic residue into sulfates with concentrated sulfuric acid and heating the residue at high
temperature until constant mass is reached. This is the common method of obtaining “sulfated
ash” (method B);
— with sulfuric acid treatment before burning, i.e. by heating the organic matter together with
concentrated sulfuric acid up to temperatures where fuming and subsequent burning of the
organic matter occur, and finally heating the residue at high temperature until constant mass is
reached (method C). This procedure may be used if volatile metal halides are liable to evaporate
during burning of the organic matter. It is not applicable to silicones or fluorine-containing
polymers.
c) Automated instrument method (method D).
In each case, the final step of the procedure is calcination at a pre-defined temperature (see 7.2).
NOTE The mass of the ash can vary with the temperature of calcination. For example, higher temperatures
such as 850 °C convert calcium carbonate and other carbonates to their oxides and thus give lower values for
the ash.
5 Reagents (for methods B and C only)
During the analysis, use only reagents of analytical grade and only distilled water or water of
equivalent purity.
5.1 Ammonium carbonate, anhydrous.
5.2 Ammonium nitrate, approximately 10 % (by mass) solution.
3
5.3 Sulfuric acid, concentrated 98 %, ρ = 1,84 g/cm .
WARNING — Highly corrosive. Handle with suitable skin and eye protection in a fume cupboard.
Reacts exothermically with water.
5.4 Sulfuric acid, 50 % (by volume) solution.
WARNING — Handle with care. Prepare by slowly adding the concentrated acid to water.
6 Apparatus
some of the listed items may not be necessary for each method.
6.1 Crucible, made of silica, porcelain, ceramics, fibres, quartz, glass or platinum, thereof, inert to the
material tested and suitable for the temperatures used. The use of a crucible lid/watch-glass may be
beneficial for samples producing a fine particulate ash.
6.2 Gas burner, or other appropriate heat source.
6.3 Muffle furnace, powered by electric resistance heat
...

SLOVENSKI STANDARD
oSIST prEN ISO 3451-1:2018
01-junij-2018
3ROLPHUQLPDWHULDOL'RORþHYDQMHSHSHODGHO6SORãQHPHWRGH,62',6

Plastics - Determination of ash - Part 1: General methods (ISO/DIS 3451-1:2018)
Kunststoffe - Bestimmung der Asche - Teil 1: Allgemeine Grundlagen (ISO/DIS 3451-
1:2018)
Plastiques - Détermination du taux de cendres - Partie 1: Méthodes générales (ISO/DIS
3451-1:2018)
Ta slovenski standard je istoveten z: prEN ISO 3451-1
ICS:
83.080.01 Polimerni materiali na Plastics in general
splošno
oSIST prEN ISO 3451-1:2018 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
oSIST prEN ISO 3451-1:2018

---------------------- Page: 2 ----------------------
oSIST prEN ISO 3451-1:2018
DRAFT INTERNATIONAL STANDARD
ISO/DIS 3451-1
ISO/TC 61/SC 5 Secretariat: DIN
Voting begins on: Voting terminates on:
2018-04-05 2018-06-28
Plastics — Determination of ash —
Part 1:
General methods
Plastiques — Détermination du taux de cendres —
Partie 1: Méthodes générales
ICS: 83.080.01
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 3451-1:2018(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 2018

---------------------- Page: 3 ----------------------
oSIST prEN ISO 3451-1:2018
ISO/DIS 3451-1:2018(E)

COPYRIGHT PROTECTED DOCUMENT
© ISO 2018
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, Switzerland
Tel. [phone]
Fax [phone]
[e-mail]
www.iso.org
Published in Switzerland
ii © ISO 2018 – All rights reserved

---------------------- Page: 4 ----------------------
oSIST prEN ISO 3451-1:2018
ISO/DIS 3451-1:2018(E)

Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents (for methods B and C only) . 2
6 Apparatus . 2
7 Procedure. 3
7.1 Test portion . 3
7.2 Test conditions . 4
7.3 Method A — Direct calcination . 5
7.4 Method B — Calcination following sulfuric acid treatment after burning . 5
7.5 Method C — Calcination following sulfuric acid treatment before burning . 6
7.6 Method D —Automated instrument method . 6
8 Number of tests . 7
9 Expression of results . 7
10 Precision . 7
11 Test report . 8
© ISO 2018 – All rights reserved iii

---------------------- Page: 5 ----------------------
oSIST prEN ISO 3451-1:2018
ISO/DIS 3451-1:2018(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 on 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 the following
URL: www .iso .org/ iso/ foreword .html.
This document was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-
chemical properties.
This fifth edition cancels and replaces the fourth edition (ISO 3451-1:2008), which has been technically
revised by adding an automated instrument method (Method D).
A list of all parts in the ISO 3451- series can be found on the ISO website.
iv © ISO 2018 – All rights reserved

---------------------- Page: 6 ----------------------
oSIST prEN ISO 3451-1:2018
DRAFT INTERNATIONAL STANDARD ISO/DIS 3451-1:2018(E)
Plastics — Determination of ash —
Part 1:
General methods
SAFETY PRECAUTIONS — Persons using this document should be familiar with normal laboratory
practice, if applicable. This document does not purport to address all of the safety concerns, if
any, associated with its use. It is the responsibility of the user to establish appropriate safety
and health practices and to ensure compliance with any regulatory requirements.
1 Scope
This document specifies general methods, with suitable test conditions, for the determination of the
ash of a range of plastics (resins and compounds). The particular conditions chosen may be included in
the specifications for the plastic material in question.
Particular conditions applicable to poly(alkylene terephthalate) materials, unplasticized cellulose
acetate, polyamides and poly(vinyl chloride) plastics, including some specific filled, glass-fibre-
reinforced and flame-retarded materials, are specified in ISO 3451-2, ISO 3451-3, ISO 3451-4 and
ISO 3451-5.
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 472, Plastics — Vocabulary
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 472 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
4 Principle
It is possible to determine the ash of an organic material by four main methods:
— direct calcination, i. e. by burning the organic matter and heating the residue at high temperature
until constant mass is reached, which may be carried out by two different procedures:
— burning with e.g. a Bunsen burner and one or more calcining steps in a muffle furnace (method A);
— burning and calcining as one single step in a muffle furnace (method A — rapid ashing), if it can be
demonstrated that the rapid ashing yields the same results as method A;
— calcination after sulfation, which may be carried out by two different procedures:
© ISO 2018 – All rights reserved 1

---------------------- Page: 7 ----------------------
oSIST prEN ISO 3451-1:2018
ISO/DIS 3451-1:2018(E)

— with sulfuric acid treatment after burning, i. e. by burning the organic matter, transforming the
inorganic residue into sulfates with concentrated sulfuric acid and heating the residue at high
temperature until constant mass is reached. This is the common method of obtaining “sulfated ash”
(method B);
— with sulfuric acid treatment before burning, i.e. by heating the organic matter together with
concentrated sulfuric acid up to temperatures where fuming and subsequent burning of the organic
matter occur, and finally heating the residue at high temperature until constant mass is reached
(method C). This procedure may be used if volatile metal halides are liable to evaporate during
burning of the organic matter. It is not applicable to silicones or fluorine-containing polymers.
— automated instrument method (method D).
In each case, the final step of the procedure is calcination at 600 °C, 750 °C, 850 °C or 950 °C until
constant mass is reached (see 7.2).
NOTE The mass of the ash may vary with the temperature of calcination. For example, higher temperatures
such as 850 °C will convert calcium carbonate and other carbonates to their oxides and thus give lower values for
the ash.
5 Reagents (for methods B and C only)
During the analysis, use only reagents of analytical grade and only distilled water or water of
equivalent purity.
5.1 Ammonium carbonate, anhydrous.
5.2 Ammonium nitrate, approximately 10 % (by mass) solution.
3
5.3 Sulfuric acid, concentrated 98 %, ρ = 1,84 g/cm .
WARNING — Highly corrosive. Handle with suitable skin and eye protection in a fume cupboard.
Reacts exothermically with water.
5.4 Sulfuric acid, 50 % (by volume) solution.
WARNING — Handle with care. Prepare by slowly adding the concentrated acid to water.
6 Apparatus
Some of the listed items may not be necessary for each method.
6.1 Crucible, made of silica, porcelain, ceramics, fibres , quartz, glass or platinum, thereof, inert to
the material tested and suitable for the temperatures used. The use of a crucible lid/watch-glass may be
beneficial for samples producing a fine particulate ash.
6.2 Gas burner, or other appropriate heat source.
6.3 Muffle furnace, powered by electric resistance heated or by microwave heating, capable of being
maintained at 600 °C ± 25 °C, 750 °C ± 50 °C, 850 °C ± 50 °C or 950 °C ± 50 °C, as appropriate.
6.4 Analytical balance, accurate to 0,1 mg.
2 © ISO 2018 – All rights reserved

---------------------- Page: 8 ----------------------
oSIST prEN ISO 3451-1:2018
ISO/DIS 3451-1:2018(E)

6.5 For automated instruments, the following requirements apply:
— fully automatic analysis instrument with integrated drying oven, muffle furnace, analytical balance
and a sample turntable;
— loss of weight during the drying and ashing process is preferably continuously monitored during the
ashing process;
— the built-in analytical balance can weigh each sample in turn, and recorded by the software;
— instrument should have a method to correct the mass difference caused by buoyancy, thus the
weighing can be took in different temperature, samples do not need to be cooled down during test;
— having a furnace that operates at the prescribed temperature, and capability to maintain a constant
temperature constant to within ±5°C;
— having a holder for one or more crucibles, e.g. by using a turntable, or an automatic way to introduce
and extract the crucibles consecutively into and from the furnace;
— temperature and sample mass ranges in accordance with the experimental requirements;
— recording device capable of automatically recording the sample
...