EN ISO 12677:2003

SLOVENSKI STANDARD
01-november-2003
Kemijska analiza ognjevzdržnih izdelkov z XRF – Metoda z vlito talino (ISO
12677:2003)
Chemical analysis of refractory products by XRF - Fused cast bead method (ISO
12677:2003)
Chemische Analyse von feuerfesten Erzeugnissen durch Röntgenflureßenz -
Schmelzaufschluss-Verfahren (ISO 12677:2003)
Analyse chimique des matériaux réfractaires par fluorescence de rayons X - Méthode de
la perle fondue (ISO 12677:2003)
Ta slovenski standard je istoveten z: EN ISO 12677:2003
ICS:
81.080 Ognjevzdržni materiali Refractories
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN ISO 12677
NORME EUROPÉENNE
EUROPÄISCHE NORM
May 2003
ICS 81.080
English version
Chemical analysis of refractory products by XRF - Fused cast
bead method (ISO 12677:2003)
Analyse chimique des matériaux réfractaires par Chemische Analyse von feuerfesten Erzeugnissen durch
fluorescence de rayons X - Méthode de la perle fondue Röntgenflureszenz - Schmelzaufschluss-Verfahren (ISO
(ISO 12677:2003) 12677:2003)
This European Standard was approved by CEN on 16 April 2003.
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 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
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versions.
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© 2003 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 12677:2003 E
worldwide for CEN national Members.

CORRECTED  2003-07-02
Foreword
This document (EN ISO 12677:2003) has been prepared by Technical Committee ISO/TC 33
"Refractories" in collaboration with Technical Committee CEN/TC 187 "Refractory products and
materials", the secretariat of which is held by BSI.
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 November 2003, and conflicting national
standards shall be withdrawn at the latest by November 2003.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of
the following countries are bound to implement this European Standard: Austria, Belgium, Czech
Republic, Denmark, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,
Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and
the United Kingdom.
Endorsement notice
The text of ISO 12677:2003 has been approved by CEN as EN ISO 12677:2003 without any
modifications.
NOTE Normative references to International Standards are listed in Annex ZA (normative).
Annex ZA
(normative)
Normative references to international publications
with their relevant European publications
This European Standard incorporates by dated or undated reference, provisions from other
publications. These normative references are cited at the appropriate places in the text and the
publications are listed hereafter. For dated references, subsequent amendments to or revisions of
any of these publications apply to this European Standard only when incorporated in it by
amendment or revision. For undated references the latest edition of the publication referred to
applies (including amendments).
NOTE Where an International Publication has been modified by common modifications, indicated
by (mod.), the relevant EN/HD applies.
Publication Year Title EN Year
ISO 10058 1992 Magnesites and dolomites - Chemical EN ISO 10058 1996
analysis
INTERNATIONAL ISO
STANDARD 12677
First edition
2003-05-01
Chemical analysis of refractory products
by XRF — Fused cast bead method
Analyse chimique des matériaux réfractaires par fluorescence de
rayons X — Méthode de la perle fondue

Reference number
ISO 12677:2003(E)
©
ISO 2003
ISO 12677:2003(E)
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ii © ISO 2003 — All rights reserved

ISO 12677:2003(E)
Contents Page
Foreword. iv
1 Scope. 1
2 Normative references. 1
3 Types of material. 1
4 Principle. 2
5 Sample grinding. 2
6 Apparatus. 3
7 Loss on ignition (and/or drying). 3
8 Flux. 4
9 Fusion casting procedures . 5
10 Calibration. 8
11 Corrections. 16
12 Reproducibility and repeatability. 19
13 Accuracy as measured using certified reference materials. 21
14 Definitions of limits of detection . 22
15 Test report. 22
Annex A (normative) Calibration range and required detection limits . 24
Annex B (normative) Corrections for tungsten carbide grinding media . 28
Annex C (informative) Examples of fluxes/flux ratios . 30
Annex D (normative) Examples of CRM to be used to check synthetic calibrations. 32
Annex E (normative) Examples of SeRM . 37
Annex F (normative) Equation for theoretical calculations . 42
Annex G (normative) Certified reference materials (CRMs). 43
Annex H (normative) Method of interference correction used to compensate for the effects of
co-existing components when using SeRM for calibration. 46
Annex I (informative) Standard deviations achieved with certified reference materials . 71
Bibliography . 74

ISO 12677:2003(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 2.
The main task of technical committees is to prepare International Standards. 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 document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 12677 was prepared by Technical Committee ISO/TC 33, Refractories.

iv © ISO 2003 — All rights reserved

INTERNATIONAL STANDARD ISO 12677:2003(E)

Chemical analysis of refractory products by XRF — Fused cast
bead method
1 Scope
This International Standard specifies a method for chemical analysis of refractory products and materials, and
technical ceramics composed of oxides, including the determination of oxide at levels between 0,01 % and
99 % by means of the XRF fused cast bead method.
NOTE Constituents at concentrations greater than 99 % (on a dried basis) should be reported on by difference,
provided that all likely minor constituents and any loss on ignition have been determined. These figures should also be
checked by direct determination.
2 Normative references
The following referenced documents are indispensable for the application 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 Guide 34:2000, General requirements for the competence of reference material producers
ISO 565, Test sieves — Metal wire cloth, perforated metal plate and electroformed sheet — Nominal sizes of
openings
ISO 10058, Magnesites and dolomites — Chemical analysis
ISO/IEC Directives (1992) — Part 2: Methodology for the development of International Standards — Annex B
Mention of reference materials
EN 955-2, Chemical analysis of refractory products — Part 2: Products containing silica and/or alumina (wet
method)
3 Types of material
High alumina W 45 % Al O
2 3
Alumino-silicate 7 % to 45 % Al O
2 3
Silica W 93 % SiO
Zircon
Zirconia and zirconates
Magnesia
Magnesia/alumina spinel (∼ 70/30)
ISO 12677:2003(E)
Dolomite
Limestone
Magnesia/chromic oxide
Chrome ore
Chrome alumina
Alumina/magnesia spinel (∼ 70/30)
Zirconia-alumina-silica cast material (AZS)
Calcium silicates
Calcium aluminates
Magnesium silicates
A list of elemental ranges and required detection limits are given in Annex A. Some of the above material
types can be accommodated on to common calibrations (see 10.3.4).
4 Principle
The powdered sample is fused with a suitable flux to destroy its mineralogical and particulate composition.
The resultant melt is cast into the shape of a glass bead which is then introduced into an XRF spectrometer.
The intensities of the fluorescent X-rays of the required elements in the bead are measured and the chemical
composition of the sample is analysed by reference to previously determined calibration graphs or e
...