SIST EN ISO 20565-3:2009

Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) - Part 3: Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma emission spectrometry (ICP-AES) (ISO 20565-3:2008)

This part of ISO 20565 specifies flame atomic absorption spectrometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods for the chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials. It is applicable in the ranges of determination given in Table 1. ISO 20565 gives alternatives to the X-ray fluorescence (XRF) method given in ISO 12677.

Chemische Analyse von chromhaltigen feuerfesten Erzeugnissen und chromhaltigen Rohstoffen (Alternative zum Röntgenfluoreszenzverfahren) - Teil 3: Flammenatomabsorptionsspektrometrie (FAAS) und Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES) (ISO 20565-3:2008)

Diese Internationale Norm legt chemische Analysenverfahren für chromhaltige feuerfeste Erzeugnisse und Rohstoffe fest, die für die in Tabelle 1 angegebenen Bereiche anwendbar sind.
Tabelle 1  Bereich für die Bestimmung
Bestandteil   Bereich   Bestandteil   Bereich
   Massenanteil in Prozent      Massenanteil in Prozent
SiO2   0,5 bis 10   MgO   15 bis 85
Al2O3   2 bis 30   Na2O   0,01 bis 1
Fe2O3   0,5 bis 25   K2O   0,01 bis 1
TiO2   0,01 bis 1   Cr2O3   2 bis 60
MnO   0,01 bis 1   ZrO2   0,01 bis 0,5
CaO   0,01 bis 3   P2O5   0,01 bis 5
ANMERKUNG   Diese Werte werden behandelt, nachdem der Glühverlust bestimmt wurde.
Diese Norm enthält Festlegungen für folgende Analysen:
a)   Glühverlust (LOI);
b)   Silicium(IV) oxid (SiO2);
c)   Aluminiumoxid (Al2O3);
d)   Eisen(III) oxid (Gesamteisengehalt berechnet als Fe2O3);
e)   Titan(IV) oxid (TiO2);
f)   Mangan(II) oxid (MnO);
g)   Calciumoxid (CaO);
h)   Magnesiumoxid (MgO);
i)   Natriumoxid (Na2O);
j)   Kaliumoxid (K2O);
k)   Chrom(III) oxid (Cr2O3)
l)   Zirkoniumoxid (ZrO2);
m)   Phosphor(V) oxid (P2O5);
n)   Bor(III) oxid (B2O3).

Analyse chimique des produits réfractaires contenant du chrome et des matériaux bruts contenant du chrome (méthode alternative a la méthode par fluorescence de rayons X) - Partie 3: Spectrométrie d'absorption atomique dans la flamme (FAAS) et spectrométrie d'émission atomique a plasma couplé par induction (ICP-AES) (ISO 20565-3:2008)

L'ISO 20565-3:2008 spécifie des méthodes pour l'analyse chimique des produits réfractaires contenant du chrome et des matières premières contenant du chrome par spectrométrie d'absorption atomique dans la flamme (FAAS) et par spectrométrie d'émission atomique avec plasma induit par haute fréquence (ICP-AES).

Kemijska analiza kromovih ognjevzdržnih izdelkov in kromovih surovin (alternativa rentgenski fluorescenčni metodi) - 3. del: Plamenska atomska absorpcijska spektrometrija (FAAS) in emisijska spektrometrija z induktivno sklopljeno plazmo (ICP-AES) (ISO 20565-3:2008)

General Information

• Status: Published
• Public Enquiry End Date: 30-Jan-2007
• Publication Date: 08-Mar-2009
• ICS: 71.040.40 - Chemical analysis
• ICS: 81.080 - Refractories
• Technical Committee: IKER - Ceramics
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 09-Jan-2009
• Due Date: 16-Mar-2009
• Completion Date: 09-Mar-2009
• Ref Project: EN ISO 20565-3:2008 - Chemical analysis of chrome-bearing refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method) - Part 3: Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) (ISO 20565-3:2008)

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 20565-3:2009
01-april-2009
.HPLMVNDDQDOL]DNURPRYLKRJQMHY]GUåQLKL]GHONRYLQNURPRYLKVXURYLQ
DOWHUQDWLYDUHQWJHQVNLIOXRUHVFHQþQLPHWRGLGHO3ODPHQVNDDWRPVND
DEVRUSFLMVNDVSHNWURPHWULMD)$$6LQHPLVLMVNDVSHNWURPHWULMD]LQGXNWLYQR
VNORSOMHQRSOD]PR,&3$(6,62
Chemical analysis of chrome-bearing refractory products and chrome-bearing raw
materials (alternative to the X-ray fluorescence method) - Part 3: Flame atomic
absorption spectrometry (FAAS) and inductively coupled plasma emission spectrometry
(ICP-AES) (ISO 20565-3:2008)
Chemische Analyse von chromhaltigen feuerfesten Erzeugnissen und chromhaltigen
Rohstoffen (Alternative zum Röntgenfluoreszenzverfahren) - Teil 3:
Flammenatomabsorptionsspektrometrie (FAAS) und Atomemissionsspektrometrie mit
induktiv gekoppeltem Plasma (ICP-AES) (ISO 20565-3:2008)
Analyse chimique des produits réfractaires contenant du chrome et des matériaux bruts
contenant du chrome (méthode alternative a la méthode par fluorescence de rayons X) -
Partie 3: Spectrométrie d'absorption atomique dans la flamme (FAAS) et spectrométrie
d'émission atomique a plasma couplé par induction (ICP-AES) (ISO 20565-3:2008)
Ta slovenski standard je istoveten z: EN ISO 20565-3:2008
ICS:
71.040.40 Kemijska analiza Chemical analysis
81.080 Ognjevzdržni materiali Refractories
SIST EN ISO 20565-3:2009 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------

SIST EN ISO 20565-3:2009

---------------------- Page: 2 ----------------------

SIST EN ISO 20565-3:2009
EUROPEAN STANDARD
EN ISO 20565-3
NORME EUROPÉENNE
EUROPÄISCHE NORM
December 2008
ICS 81.080

English Version
Chemical analysis of chrome-bearing refractory products and
chrome-bearing raw materials (alternative to the X-ray
fluorescence method) - Part 3: Flame atomic absorption
spectrometry (FAAS) and inductively coupled plasma atomic
emission spectrometry (ICP-AES) (ISO 20565-3:2008)
Analyse chimique des produits réfractaires contenant du Chemische Analyse von chromhaltigen feuerfesten
chrome et des matières premières contenant du chrome Erzeugnissen und chromhaltigen Rohstoffen (Alternative
(méthode alternative à la méthode par fluorescence de zum Röntgenfluoreszenzverfahren) - Teil 3:
rayons X) - Partie 3: Méthodes par spectrométrie Flammenatomabsorptionsspektrometrie (FAAS) und
d'absorption atomique dans la flamme (FAAS) et Atomemissionsspektrometrie mit induktiv gekoppeltem
spectrométrie d'émission atomique avec plasma induit par Plasma (ICP-AES) (ISO 20565-3:2008)
haute fréquence (ICP-AES) (ISO 20565-3:2008)
This European Standard was approved by CEN on 8 November 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 20565-3:2008: E
worldwide for CEN national Members.

---------------------- Page: 3 ----------------------

SIST EN ISO 20565-3:2009
EN ISO 20565-3:2008 (E)
Contents Page
Foreword .3

2

---------------------- Page: 4 ----------------------

SIST EN ISO 20565-3:2009
EN ISO 20565-3:2008 (E)
Foreword
This document (EN ISO 20565-3:2008) 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 June 2009, and conflicting national standards shall be withdrawn at
the latest by June 2009.
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 20565-3:2008 has been approved by CEN as a EN ISO 20565-3:2008 without any
modification.

3

---------------------- Page: 5 ----------------------

SIST EN ISO 20565-3:2009

---------------------- Page: 6 ----------------------

SIST EN ISO 20565-3:2009

INTERNATIONAL ISO
STANDARD 20565-3
First edition
2008-12-01


Chemical analysis of chrome-bearing
refractory products and chrome-bearing
raw materials (alternative to the X-ray
fluorescence method) —
Part 3:
Flame atomic absorption spectrometry
(FAAS) and inductively coupled plasma
atomic emission spectrometry (ICP-AES)
Analyse chimique des produits réfractaires contenant du chrome et des
matières premières contenant du chrome (méthode alternative à la
méthode par fluorescence de 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 20565-3:2008(E)
©
ISO 2008

---------------------- Page: 7 ----------------------

SIST EN ISO 20565-3:2009
ISO 20565-3:2008(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.


COPYRIGHT PROTECTED DOCUMENT


©  ISO 2008
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or
ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail [e-mail]
Web www.iso.org
Published in Switzerland

ii © ISO 2008 – All rights reserved

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

SIST EN ISO 20565-3:2009
ISO 20565-3:2008(E)
Contents Page
Foreword. iv
1 Scope .1
2 Normative references .2
3 Instrumental methods using inductively coupled plasma emission spectrometry
(ICP-AES) .2
4 Instrumental methods using flame absorption spectrophotometry (FAAS) .10
5 Test report .14
Bibliography .15




© ISO 2008 – All rights reserved iii

---------------------- Page: 9 ----------------------

SIST EN ISO 20565-3:2009
ISO 20565-3:2008(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 20565-3 was prepared by Technical Committee ISO/TC 33, Refractories, in collaboration with Technical
Committee CEN/TC 187, Refractory products and materials.
ISO 20565 consists of the following parts, under the general title Chemical analysis of chrome-bearing
refractory products and chrome-bearing raw materials (alternative to the X-ray fluorescence method):
⎯ Part 1: Apparatus, reagents, dissolution and determination of gravimetric silica
⎯ Part 2: Wet chemical analysis
⎯ Part 3: Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma atomic emission
spectrometry (ICP-AES)

iv © ISO 2008 – All rights reserved

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

SIST EN ISO 20565-3:2009
INTERNATIONAL STANDARD ISO 20565-3:2008(E)

Chemical analysis of chrome-bearing refractory products and
chrome-bearing raw materials (alternative to the X-ray
fluorescence method) —
Part 3:
Flame atomic absorption spectrometry (FAAS) and inductively
coupled plasma atomic emission spectrometry (ICP-AES)
1 Scope
This part of ISO 20565 specifies flame atomic absorption spectrometry (FAAS) and inductively coupled
plasma atomic emission spectrometry (ICP-AES) methods for the chemical analysis of chrome-bearing
refractory products and chrome-bearing raw materials.
It is applicable in the ranges of determination given in Table 1.
ISO 20565 gives alternatives to the X-ray fluorescence (XRF) method given in ISO 12677.
Table 1 — Range of determination (% by mass)
Component Range
SiO
0,5 to 10
2
Al O
2 to 30
2 3
Fe O
0,5 to 25
2 3
TiO
0,01 to 1
2
MnO 0,01 to 1
CaO 0,01 to 3
MgO 15 to 85
Na O
0,01 to 1
2
K O
0,01 to 1
2
Cr O
2 to 60
2 3
ZrO
0,01 to 0,5
2
P O
0,01 to 5
2 5
LOI −0,5 to 5
NOTE These values are after the loss on ignition (LOI)
has been taken into account.
© ISO 2008 – All rights reserved 1

---------------------- Page: 11 ----------------------

SIST EN ISO 20565-3:2009
ISO 20565-3:2008(E)
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 20565-1:2008, Chemical analysis of chrome-bearing refractory products and chrome-bearing raw
materials (alternative to the X-ray fluorescence method) — Part 1: Apparatus, reagents, dissolution and
determination of gravimetric silica
ISO 26845, Chemical analysis of refractories — General requirements for wet chemical analysis, atomic
absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES)
methods
3 Instrumental methods using inductively coupled plasma emission spectrometry
(ICP-AES)
3.1 Determination of residual silica in stock solutions (S1) by ICP-AES
3.1.1 Principle
The residual silica remaining in solution in solutions (S1) is determined using ICP-AES.
3.1.2 Reagents
Prepare the following reagents in addition to any reagents described in ISO 20565-1:2008, Clause 5, that are
necessary.
3.1.2.1 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.
3.1.2.2 Matrix solution 2.
Carry out the procedure given in ISO 20565-1:2008, 9.2.2.3, without the sample, but omit heating the fusion
mixture or anhydrous sodium carbonate. The equivalent solution to stock solution (S1) is referred to as matrix
solution 2.
3.1.2.3 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 2 (3.1.2.2) and dilute to the mark with water.
In Table 2, a typical example of the preparation of solutions is shown. In accordance with the compositions of
the samples, and the type and capabilities of the instrument used, an appropriate series of solutions for
calibration is prepared.
2 © ISO 2008 – All rights reserved

---------------------- Page: 12 ----------------------

SIST EN ISO 20565-3:2009
ISO 20565-3:2008(E)
Table 2 — Example of series 2 solution for calibration
Solution Matrix solution 2 Diluted silicon(IV) oxide Concentration
No. standard solution of solution
SiO mg/100 ml
ml 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) (see ISO 20565-1) as follows.
Transfer 10 ml of stock solution (S1) to a 100 ml volumetric flask and dilute to the mark with water. This
solution, for the determination of dissolved silicon(IV) oxide, is referred to as diluted stock solution (S1d).
Spray a portion of diluted stock solution (S1d) into the argon plasma flame of the ICP-AE spectrometer, and
measure the emission intensity at, for example, the wavelength of 251,611 nm.
3.1.4 Blank test
Carry out the procedure in 3.1.3 with blank solution (B1) (see ISO 20565-1). The equivalent diluted blank
solution to diluted stock solution (S1d) is referred to as diluted blank solution (B1d).
3.1.5 Plotting of calibration graph
Calibrate the ICP-AE spectrometer using the series 2 solution (3.1.3.3) and 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 solution solutions for each set
of determinations.
3.1.6 Calculation
Calculate the mass fraction of silicon(IV) oxide, w , as a percentage, using Equation (1). Use the mass of
SiO
2
silicon(IV) oxide derived from the figures obtained from 3.1.3 and 3.1.4 and the calibration prepared in 3.1.5.
250
()mm−+()m−m×
12 s b
10
w=×100 (1)
SiO
2
m
where
m is the mass of the test portion (see ISO 20565-1), in grams (g);
m is the first mass from ISO 20565-1:2008, 9.2.2.3.3, in grams (g);
1
m is the second mass from ISO 20565-1:2008, 9.2.2.3.3,, in grams (g);
2
m is the mass of silicon(IV) oxide in diluted stock solution (S1d) as described in 3.1.3, in grams (g);
s
m is the mass of silicon(IV) oxide in diluted blank solution (B1d) as described in 3.1.4, in grams (g).
b
© ISO 2008 – All rights reserved 3

---------------------- Page: 13 ----------------------

SIST EN ISO 20565-3:2009
ISO 20565-3:2008(E)
3.2 Determination of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide,
manganese(II) oxide, calcium oxide, magnesium oxide, chromium(III) oxide and zirconium
oxide using stock solutions (S1) or (S′1) by ICP-AES
3.2.1 Principle
The emission intensities of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide, manganese(II)
oxide, calcium oxide, magnesium oxide, chromium(III) oxide and zirconium oxide are measured by an ICP-AE
spectrometer for stock solutions (S1) (see ISO 20565-1) or (S′1) (see ISO 20565-1). This method should be
applied to components in (S1) or (S′1) in accordance with Table 3.
Table 3 — Application range (% by mass)
Component Range
SiO
0,1 to 10
2
Al O
0,05 to 10
2 3
Fe O
0,01 to 10
2 3
TiO
0,01 to 1
2
MnO 0,01 to 1
CaO 0,01 to 10
Cr O
0,01 to 10
2 3
ZrO
0,01 to 0,5
2
NOTE 1 When solution (S1) is used, the SiO is residual silica.
2
When solution (S′1) is used, the SiO is all of the silicon(IV) oxide.
2
NOTE 2 Determination of calcium oxide by this method cannot be
applied to calcium oxide contents of more than 10 % by mass.

3.2.2 Reagents
Prepare the following reagents in addition to any reagents described in ISO 20565-1:2008, Clause 5, that are
necessary.
3.2.2.1 Mixed standard solution 3, SiO 0,04 mg/ml, Al O 0,04 mg/ml, Fe O 0,04 mg/ml,
2 2 3 2 3
TiO 0,005 mg/ml, MnO 0,005 mg/ml, CaO 0,04 mg/ml, Cr O 0,04 mg/ml, ZrO 0,005 mg/ml.
2 2 3 2
Transfer aliquot portions of standard silicon(IV) oxide (40 ml), aluminium oxide (40 ml), iron(III) oxide (40 ml),
titanium(IV) oxide (5 ml), manganese(II) oxide (5 ml), calcium oxide (40 ml), chromium(III) oxide (40 ml) and
zirconium oxide (5 ml) solutions to a 1 000 ml volumetric flask and dilute to the mark with water.
3.2.2.2 Matrix solution 3 or 3′.
Carry out the procedure given in ISO 20565-1:2008, 9.2.2.3 or 9.2.3.3, without the sample, but omit heating
the fusion mixture or anhydrous sodium carbonate. The equivalent solution to stock solution (S1) or (S′1) is
referred to as matrix solution 3 or 3′ as applicable.
4 © ISO 2008 – All rights reserved

---------------------- Page: 14 ----------------------

SIST EN ISO 20565-3:2009
ISO 20565-3:2008(E)
3.2.2.3 Internal standard solution.
Transfer 10 ml of standard scandium oxide solution (1 mg/ml) and standard yttrium oxide solution (1 mg/ml) to
a 100 ml volumet
...