Chemical analysis of refractories containing alumina, zirconia, and silica - Refractories containing 5 percent to 45 percent of ZrO2 (alternative to the X-ray fluorescence method) - Part 3: Flame atomic absorption spectrophotometry (FAAS) and inductively coupled plasma emission spectrometry (ICP -AES) (ISO 21079-3:2008)

This part of ISO 21079 specifies flame atomic absorption spect rophotometry (FAAS) and inductively coupled plasma emission sp ectrometry (ICP-AES) methods for the analysis of AZS (alumina, zirconia, and silica) refractory products (containing 5 % to 45 % of ZrO2) and raw materials. This part of ISO 21079 is not applicable to MgO-based refractories. This part of ISO 21079 gives alternatives to the X-ray fluorescence (XRF) method give n in ISO 12677.

Chemische Analyse von aluminiumoxid-, zirkomiumoxid- und silicium(IV)-oxidhaltigen feuerfesten Erzeugnissen - Feuerfeste Erzeugnisse mit einem Massenanteil an ZrO2 von 5 % bis 45 % (Alternative zum Röntgenfluoreszenzverfahren) - Teil 3: Flammenatomabsorptionsspektrophotometrie (FAAS) und Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES) (ISO 21079-3:2008)

Dieser Teil von ISO 21079 legt die Verfahren der Flammenatomabsorptionsspektrophotometrie (FAAS) und Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP AES) für die Analyse von feuerfesten Erzeugnissen (mit 5 % bis 45 % ZrO2) und Rohstoffen fest, die AZS (Aluminiumoxid, Zirkoniumoxid und Silicium(IV) oxid) enthalten.
Dieser Teil von ISO 21079 gilt nicht für feuerfeste Erzeugnisse, die auf MgO basieren.
Dieser Teil von ISO 21079 stellt eine Alternative zum Röntgenfluoreszenzverfahren (RFA) nach ISO 12677 dar.

Analyse chimique des matériaux réfractaires contenant de l'alumine, de la zircone et de la silice - Matériaux réfractaires contenant de 5 % à 45 % de ZrO2 (méthode alternative à la méthode par fluorescence de rayons X) - Partie 3: Spectrométrie d'absorption atomique dans la flamme (FAAS) et spectrométrie d'émission atomique avec plasma induit par haute fréquence (ICP-AES) (ISO 21079-3:2008)

L'ISO 21079-3:2008 spécifie des méthodes par spectrométrie d'absorption atomique dans la flamme (FAAS) et spectrométrie d'émission atomique avec plasma induit par haute fréquence (ICP-AES) pour l'analyse des matières premières et produits réfractaires AZS (alumine, zircone et silice), contenant de 5 % à 45 % de ZrO2 (zircone).
L'ISO 21079-3:2008 n'est pas applicable aux matériaux réfractaires à base de MgO.
L'ISO 20179:2008 fournit des méthodes alternatives à la méthode d'analyse par fluorescence de rayons X, spécifiée dans l'ISO 12677.

Kemijska analiza ognjevzdržnih izdelkov, ki vsebujejo aluminijev oksid, cirkonijev oksid in silicijev oksid - Ognevzdržni izdelki vsebujejo 5 % do 45 % ZrO2 (alternativa rentgenski fluorescenčni metodi) - 3. del: Plamenska atomska absorpcijska spektrometrija (FAAS) in emisijska spektrometrija z induktivno sklopljeno plazmo (ICP -AES) (ISO 21079-3:2008)

General Information

Status
Published
Publication Date
03-Aug-2008
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
07-May-2008
Due Date
12-Jul-2008
Completion Date
04-Aug-2008

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SLOVENSKI STANDARD
SIST EN ISO 21079-3:2008
01-oktober-2008
.HPLMVNDDQDOL]DRJQMHY]GUåQLKL]GHONRYNLYVHEXMHMRDOXPLQLMHYRNVLGFLUNRQLMHY
RNVLGLQVLOLFLMHYRNVLG2JQHY]GUåQLL]GHONLYVHEXMHMRGR=U2
DOWHUQDWLYDUHQWJHQVNLIOXRUHVFHQþQLPHWRGL GHO3ODPHQVNDDWRPVND
DEVRUSFLMVNDVSHNWURPHWULMD )$$6 LQHPLVLMVNDVSHNWURPHWULMD]LQGXNWLYQR
VNORSOMHQRSOD]PR ,&3$(6  ,62
Chemical analysis of refractories containing alumina, zirconia, and silica - Refractories
containing 5 percent to 45 percent of ZrO2 (alternative to the X-ray fluorescence method)
- Part 3: Flame atomic absorption spectrophotometry (FAAS) and inductively coupled
plasma emission spectrometry (ICP -AES) (ISO 21079-3:2008)
Chemische Analyse von aluminiumoxid-, zirkomiumoxid- und silicium(IV)-oxidhaltigen
feuerfesten Erzeugnissen - Feuerfeste Erzeugnisse mit einem Massenanteil an ZrO2 von
5 % bis 45 % (Alternative zum Röntgenfluoreszenzverfahren) - Teil 3:
Flammenatomabsorptionsspektrophotometrie (FAAS) und Atomemissionsspektrometrie
mit induktiv gekoppeltem Plasma (ICP-AES) (ISO 21079-3:2008)
Analyse chimique des matériaux réfractaires contenant de l'alumine, de la zircone et de
la silice - Matériaux réfractaires contenant de 5 % à 45 % de ZrO2 (méthode alternative
à la méthode par fluorescence de rayons X) - Partie 3: Spectrométrie d'absorption
atomique dans la flamme (FAAS) et spectrométrie d'émission atomique avec plasma
induit par haute fréquence (ICP-AES) (ISO 21079-3:2008)
Ta slovenski standard je istoveten z: EN ISO 21079-3:2008
ICS:
71.040.40 Kemijska analiza Chemical analysis
81.080 Ognjevzdržni materiali Refractories
SIST EN ISO 21079-3:2008 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 21079-3:2008

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SIST EN ISO 21079-3:2008
EUROPEAN STANDARD
EN ISO 21079-3
NORME EUROPÉENNE
EUROPÄISCHE NORM
April 2008
ICS 81.080; 71.040.40

English Version
Chemical analysis of refractories containing alumina, zirconia,
and silica - Refractories containing 5 percent to 45 percent of
ZrO2 (alternative to the X-ray fluorescence method) - Part 3:
Flame atomic absorption spectrophotometry (FAAS) and
inductively coupled plasma emission spectrometry (ICP -AES)
(ISO 21079-3:2008)
Analyse chimique des matériaux réfractaires contenant de Chemische Analyse von aluminiumoxid-, zirkomiumoxid-
l'alumine, de la zircone et de la silice - Matériaux und silicium(IV)-oxidhaltigen feuerfesten Erzeugnissen -
réfractaires contenant de 5 % à 45 % de ZrO2 (méthode Feuerfeste Erzeugnisse mit einem Massenanteil an ZrO2
alternative à la méthode par fluorescence de rayons X) - von 5 % bis 45 % (Alternative zum
Partie 3: Méthodes par spectrométrie d'absorption Röntgenfluoreszenzverfahren) - Teil 3:
atomique dans la flamme (FAAS) et spectrométrie Flammenatomabsorptionsspektrophotometrie (FAAS) und
d'émission atomique avec plasma induit par haute Atomemissionsspektrometrie mit induktiv gekoppeltem
fréquence (ICP-AES) (ISO 21079-3:2008) Plasma (ICP-AES) (ISO 21079-3:2008)
This European Standard was approved by CEN on 12 April 2008.
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 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 Management Centre has the same status as the
official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2008 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 21079-3:2008: E
worldwide for CEN national Members.

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SIST EN ISO 21079-3:2008
EN ISO 21079-3:2008 (E)
Contents Page
Foreword.3

2

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SIST EN ISO 21079-3:2008
EN ISO 21079-3:2008 (E)
Foreword
This document (EN ISO 21079-3:2008) 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 October 2008, and conflicting national standards shall be withdrawn at
the latest by October 2008.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
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, Cyprus, Czech
Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.
Endorsement notice
The text of ISO 21079-3:2008 has been approved by CEN as a EN ISO 21079-3:2008 without any
modification.

3

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SIST EN ISO 21079-3:2008

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SIST EN ISO 21079-3:2008

INTERNATIONAL ISO
STANDARD 21079-3
First edition
2008-04-15

Chemical analysis of refractories
containing alumina, zirconia, and silica —
Refractories containing 5 % to 45 %
of ZrO (alternative to the X-ray
2
fluorescence method) —
Part 3:
Flame atomic absorption
spectrophotometry (FAAS)
and inductively coupled plasma emission
spectrometry (ICP-AES)
Analyse chimique des matériaux réfractaires contenant de l'alumine, de
la zircone et de la silice — Matériaux réfractaires contenant de 5 % à
45 % de ZrO (méthode alternative à la méthode par fluorescence de
2
rayons X) —
Partie 3: Méthodes par spectrométrie d'absorption atomique dans la
flamme (FAAS) et spectrométrie d'émission atomique avec plasma
induit par haute fréquence (ICP-AES)




Reference number
ISO 21079-3:2008(E)
©
ISO 2008

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SIST EN ISO 21079-3:2008
ISO 21079-3:2008(E)
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All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
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Published in Switzerland

ii © ISO 2008 – All rights reserved

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SIST EN ISO 21079-3:2008
ISO 21079-3:2008(E)
Contents Page
Foreword. iv
1 Scope . 1
2 Normative references . 1
3 Instrumental methods using ICP-AES. 1
3.1 Determination of residual silica in solution by ICP-AES . 1
3.2 Determination of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide,
calcium oxide, magnesium oxide, chromium(III) oxide and hafnium oxide using stock
solutions (S1), (S’1) or (S’’1) by ICP-AES. 3
3.3 Determination of calcium oxide, magnesium oxide, sodium oxide and potassium oxide
using stock solutions (S4) by ICP-AES . 7
4 Instrumental methods using Flame Atomic Absorption Spectrometry (FAAS). 8
4.1 Determination of calcium oxide, magnesium oxide, sodium oxide and potassium oxide
using stock solutions (S3) by FAAS . 8
4.2 Determination of chromium(III) oxide by FAAS spectrometry. 10
5 Calculation and expression of test results .12
6 Test report . 12
Bibliography . 13

© ISO 2008 – All rights reserved iii

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SIST EN ISO 21079-3:2008
ISO 21079-3:2008(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 21079-3 was prepared by Technical Committee ISO/TC 33, Refractories.
ISO 21079 consists of the following parts, under the general title Chemical analysis of refractories containing
alumina, zirconia, and silica — Refractories containing 5 % to 45 % of ZrO (alternative to the X-ray
2
fluorescence method):
⎯ Part 1: Apparatus, reagents and dissolution
⎯ Part 2: Wet chemical analysis
⎯ Part 3: Flame atomic absorption spectrophotometry (FAAS) and inductively coupled plasma emission
spectrometry (ICP-AES)

iv © ISO 2008 – All rights reserved

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SIST EN ISO 21079-3:2008
INTERNATIONAL STANDARD ISO 21079-3:2008(E)

Chemical analysis of refractories containing alumina, zirconia,
and silica — Refractories containing 5 % to 45 % of ZrO
2
(alternative to the X-ray fluorescence method) —
Part 3:
Flame atomic absorption spectrophotometry (FAAS) and
inductively coupled plasma emission spectrometry (ICP-AES)
1 Scope
This part of ISO 21079 specifies flame atomic absorption spectrophotometry (FAAS) and inductively coupled
plasma emission spectrometry (ICP-AES) methods for the analysis of AZS (alumina, zirconia, and silica)
refractory products (containing 5 % to 45 % of ZrO ) and raw materials.
2
This part of ISO 21079 is not applicable to MgO-based refractories.
This part of ISO 21079 gives alternatives to the X-ray fluorescence (XRF) method given in ISO 12677.
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 21079-1:2008, Chemical analysis of refractories containing alumina, zirconia and silica — Refractories
containing 5 % to 45 % of ZrO (alternative to the X-ray fluorescence method) — Part 1: Apparatus, reagents
2
and dissolution
ISO 26845, Chemical analysis of refractories — General requirements for wet chemical analysis, atomic
absorption spectrometry (AAS) and inductively coupled plasma (ICP) methods
3 Instrumental methods using ICP-AES
3.1 Determination of residual silica in solution by ICP-AES
3.1.1 Principle
The residual silica remaining in solution in solutions (S1) or (S’1) is determined using ICP-AES.
3.1.2 Reagents
3.1.2.1 General
Prepare the reagents given in 3.1.2.2 to 3.1.2.4. and those specified in ISO 26845, as necessary.
© ISO 2008 – All rights reserved 1

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SIST EN ISO 21079-3:2008
ISO 21079-3:2008(E)
3.1.2.2 Diluted silicon(IV) oxide standard solution, SiO 0,08 mg/ml.
2
Transfer 20 ml of the silicon(IV) oxide standard solution (SiO 1 mg/ml) into a 250 ml volumetric flask, and
2
dilute to the mark with water.
3.1.2.3 Matrix solution 1 or 1’.
Carry out the procedure given in 9.2.2.3 or 9.2.3.3 of ISO 21079-1:2008 without the sample, but omit heating
the fusion mixture or anhydrous sodium carbonate. Designate the solution equivalent to stock solution (S1) or
(S’1) as matrix solution 1 or 1’ as applicable.
3.1.2.4 Series 2 solution for calibration.
Transfer appropriate aliquot portions of diluted silicon(IV) oxide standard solution (0,08 mg/ml) precisely into
several 100 ml volumetric flasks, in accordance with the composition of the samples. Add 10 ml each of matrix
solution 1 or 1’ and dilute to the mark with water.
Table 1 shows a typical example of the preparation of solutions. An appropriate series of solutions for
calibration should be prepared, depending on the compositions of the samples and the types and capabilities
of instrument used.
Table 1 — Example of series 2 solution for calibration
Matrix solution Diluted silicon(IV) oxide Concentration
Solution
1 or 1’ standard solution of solution
No.
ml ml SiO mg/100 ml

2
1 10 0 0
2 10 5 0,4
3 10 10 0,8
4 10 15 1,2
5 10 20 1,6
6 10 25 2,0

3.1.3 Procedure
Determine the silicon(IV) oxide remaining in solution (S1) or (S’1) (see Annex A of ISO 21079-1:2008) as
follows.
Transfer 10 ml of stock solution (S1) or (S’1) to a 100 ml volumetric flask, and dilute to the mark with water.
Designate this solution for the determination of dissolved silicon(IV) oxide as diluted stock solution (S1d) or
(S’1d).
Spray a portion of diluted stock solution (S1d or S’1d) into the argon plasma flame of the inductively coupled
plasma atomic emission (ICP-AE) spectrometer, and measure the emission intensity at an appropriate
wavelength, for example, 251,611 nm.
3.1.4 Blank test
Carry out the procedure in 3.1.3 with blank solution (B1) or (B’1) (see Annex A of ISO 21079-1:2008).
Designate the equivalent diluted blank solution to diluted stock solution (S1d) or (S'1d) as diluted blank
solution (B1d or B'1d).
2 © ISO 2008 – All rights reserved

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SIST EN ISO 21079-3:2008
ISO 21079-3:2008(E)
3.1.5 Plotting the calibration graph
Using the series 2 solution for calibration, carry out the emission procedure described in 3.1.3. Plot the
relation between the emission intensity and mass of oxide, prepare the calibration graph by adjusting the
curve so that it passes through the point of origin.
A new calibration should be carried out using the range of calibration and blank solutions for each set of
determinations.
3.1.6 Calculation
Calculate the mass fraction of silicon(IV) oxide, w(SiO ), expressed as a percentage, using Equation (1) with
2
the amount of silicon(IV) oxide derived from the values obtained from 3.1.3 and 3.1.4 and the calibration
prepared as described in 3.1.5.
500
mm−+m−m×
()()
12 s b
10
w SiO=×100 (1)
()
2
m
where
m is the mass of the test portion obtained in accordance with 9.2.2.2 or 9.2.3.2 of ISO 21079-1:2008, in
grams;
m is the mass obtained in accordance with 9.2.2.3 or 9.2.3.3 of ISO 21079-1:2008, in grams;
1
m is the mass obtained in accordance with 9.2.2.4 or 9.2.3.4 of ISO 21079-1:2008, in grams;
2
m is the mass of sili
...

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