SIST EN ISO 21587-3:2008

Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) - Part 3: Inductively coupled plasma and atomic absorption spectrometry methods (ISO 21587-3:2007)

This set of standards will describe methods for the chemical analysis of aluminosilicate refractory products and raw materials, using traditional ("wet") methods, ICP-AE spectrometry and FAA spectrometrymethods for the chemical analysis of aluminosilicate refractory products and raw materials. The methods are applicable to the determination of the following: silicon(IV) oxide (SiO2) aluminium oxide (Al2O3) iron(III) oxide (total iron oxide calculated as Fe2O3) titanium(IV) oxide (TiO2) manganese(II) oxide (MnO) calcium oxide (CaO) magnesium oxide (MgO) sodium oxide (Na2O) potassium oxide (K2O) chromium(III) oxide (Cr2O3) zirconium oxide (ZrO2) phosphorous(V) oxide (P2O5) This part of ISO 21587 gives alternatives to the X-ray flluorescence (XRF) method given in ISO 12677:2003, Chemical analysis of refractory products by XRF - Fused cast bead method.

Chemische Analyse feuerfester Erzeugnisse aus Alumosilicat (Alternative zum Röntgenfluoreszenzverfahren) - Teil 3: Verfahren mit induktiv gekoppeltem Plasma und Atomabsorptionspektrometrie (ISO 21587-3:2007)

Dieser Teil von ISO 21587 legt Verfahren der Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP AES) und der Flammenatomabsorptionsspektrometrie (FAAS) für die chemische Analyse von feuer¬festen Erzeugnissen und Rohstoffen aus Alumosilicat fest.
Die Verfahren gelten für die folgenden Bestimmungen:
   Silicium(IV) oxid (SiO2);
   Aluminiumoxid (Al2O3);
   Eisen(III) oxid (Gesamteisengehalt, berechnet als Fe2O3);
   Titan(IV) oxid (TiO2);
   Mangan(II) oxid (MnO);
   Calciumoxid (CaO);
   Magnesiumoxid (MgO);
   Natriumoxid (Na2O);
   Kaliumoxid (K2O);
   Chrom(III) oxid (Cr2O3);
   Zirkoniumoxid (ZrO2);
   Phosphor(V) oxid (P2O5).
Dieser Teil von ISO 21587 gibt Alternativen zur Röntgenfluoreszenzanalyse (RFA), die in ISO 12677:2003, Chemische Analyse von feuerfesten Erzeugnissen durch RFA — Schmelzaufschluss Verfahren, festgelegt ist.

Analyse chimique des produits réfractaires d'aluminosilicates (méthode alternative a la méthode par fluorescence de rayons X) - Partie 3: Méthodes par spectrométrie d'absorption atomique (AAS) et spectrométrie d'émission atomique avec plasma induit par haute fréquence (ICP-AES) (ISO 21587-3:2007)

L'ISO 21587-3:2007 spécifie des méthodes par spectrométrie d'absorption atomique (AAS) dans la flamme et spectrométrie d'émission atomique avec plasma induit par haute fréquence (ICP-AES), pour l'analyse chimique des produits et matières premières réfractaires d'aluminosilicates.
Les méthodes s'appliquent au dosage des éléments suivants:
la silice(IV) (SiO2)l'alumine (Al2O3)l'oxyde de fer(III) (oxyde de fer total calculé en tant que Fe2O3)l'oxyde de titane(IV) (TiO2)l'oxyde de manganèse(II) (MnO)l'oxyde de calcium (CaO)la magnésie (MgO)l'oxyde de sodium (Na2O)l'oxyde de potassium (K2O)l'oxyde de chrome(III) (Cr2O3)l'oxyde de zirconium (ZrO2)l'oxyde de phosphore(V) (P2O5)
L'ISO 21587-+:2007 fournit une méthode alternative à la méthode par fluorescence de rayons X (FRX) donnée dans l'ISO 12677:2003.

Kemijska analiza aluminijev silikatnih ognjevzdržnih izdelkov (alternativa rentgenski fluorescenčni metodi) - 3. del: Metode induktivno sklopljene plazme in atomske absorpcijske spektrometrije (ISO 21587-3:2007)

General Information

• Status: Published
• Publication Date: 06-Mar-2008
• ICS: 81.080 - Refractories
• Technical Committee: IKER - Ceramics
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 15-Oct-2007
• Due Date: 20-Dec-2007
• Completion Date: 07-Mar-2008
• Ref Project: EN ISO 21587-3:2007 - Chemical analysis of aluminosilicate refractory products (alternative to the X-ray fluorescence method) - Part 3: Inductively coupled plasma and atomic absorption spectrometry methods (ISO 21587-3:2007)

Relations

• Replaces: SIST ENV 955-4:1998 - Chemical analysis of refractory products - Part 4: Products containing silica and/or alumina (Analysis by Flame Atomic Absorption Spectrometry (FAAS) and Inductively Coupled Plasma Atomic Emission Spectrography (ICP)
• Effective Date: 01-Mar-2008

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 21587-3:2008
01-april-2008
1DGRPHãþD
SIST ENV 955-4:1998
.HPLMVNDDQDOL]DDOXPLQLMHYVLOLNDWQLKRJQMHY]GUåQLKL]GHONRYDOWHUQDWLYD
UHQWJHQVNLIOXRUHVFHQþQLPHWRGLGHO0HWRGHLQGXNWLYQRVNORSOMHQHSOD]PHLQ
DWRPVNHDEVRUSFLMVNHVSHNWURPHWULMH,62
Chemical analysis of aluminosilicate refractory products (alternative to the X-ray
fluorescence method) - Part 3: Inductively coupled plasma and atomic absorption
spectrometry methods (ISO 21587-3:2007)
Chemische Analyse feuerfester Erzeugnisse aus Alumosilicat (Alternative zum
Röntgenfluoreszenzverfahren) - Teil 3: Verfahren mit induktiv gekoppeltem Plasma und
Atomabsorptionspektrometrie (ISO 21587-3:2007)
Analyse chimique des produits réfractaires d'aluminosilicates (méthode alternative a la
méthode par fluorescence de rayons X) - Partie 3: Méthodes par spectrométrie
d'absorption atomique (AAS) et spectrométrie d'émission atomique avec plasma induit
par haute fréquence (ICP-AES) (ISO 21587-3:2007)
Ta slovenski standard je istoveten z: EN ISO 21587-3:2007
ICS:
81.080
SIST EN ISO 21587-3:2008 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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EUROPEAN STANDARD
EN ISO 21587-3
NORME EUROPÉENNE
EUROPÄISCHE NORM
September 2007
ICS 81.080 Supersedes ENV 955-4:1997
English Version
Chemical analysis of aluminosilicate refractory products
(alternative to the X-ray fluorescence method) - Part 3:
Inductively coupled plasma and atomic absorption spectrometry
methods (ISO 21587-3:2007)
Analyse chimique des produits réfractaires Chemische Analyse feuerfester Erzeugnisse aus
d'aluminosilicates (méthode alternative à la méthode par Alumosilicat (Alternative zum
fluorescence de rayons X) - Partie 3: Méthodes par Röntgenfluoreszenzverfahren) - Teil 3: Verfahren mit
spectrométrie d'absorption atomique (AAS) et induktiv gekoppeltem Plasma und
spectrométrie d'émission atomique avec plasma induit par Atomabsorptionspektrometrie (ISO 21587-3:2007)
haute fréquence (ICP-AES) (ISO 21587-3:2007)
This European Standard was approved by CEN on 13 September 2007.
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
© 2007 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 21587-3:2007: E
worldwide for CEN national Members.

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EN ISO 21587-3:2007 (E)






Foreword



The text of ISO 21587-3:2007 has been prepared by Technical Committee ISO/TC 33
"Refractories” of the International Organization for Standardization (ISO) and has been taken
over as EN ISO 21587-3:2007 by 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 March 2008, and conflicting national
standards shall be withdrawn at the latest by March 2008.

This document supersedes ENV 955-4:1997.

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 United
Kingdom.


Endorsement notice

The text of ISO 21587-3:2007 has been approved by CEN as EN ISO 21587-3:2007 without any
modifications.

2

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INTERNATIONAL ISO
STANDARD 21587-3
First edition
2007-03-01

Chemical analysis of aluminosilicate
refractory products (alternative to the
X-ray fluorescence method) —
Part 3:
Inductively coupled plasma and atomic
absorption spectrometry methods
Analyse chimique des produits réfractaires d'aluminosilicates (méthode
alternative à la méthode par fluorescence de rayons X) —
Partie 3: Méthodes par spectrométrie d'absorption atomique (AAS) et
spectrométrie d'émission atomique avec plasma induit par haute
fréquence (ICP-AES)





Reference number
ISO 21587-3:2007(E)
©
ISO 2007

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ISO 21587-3:2007(E)
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ii © ISO 2007 – All rights reserved

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ISO 21587-3:2007(E)
Contents Page
Foreword. iv
1 Scope . 1
2 Normative references . 2
3 Determination of residual silica in solution by ICP/AES . 2
4 Determination of iron(III) oxide by ICP/AES. 4
5 Determination of titanium(IV) oxide by ICP/AES . 6
6 Determination of manganese(II) oxide by ICP/AES. 6
7 Determination of calcium oxide by ICP/AES. 7
8 Determination of magnesium oxide by ICP/AES . 9
9 Determination of sodium oxide by ICP/AES . 9
10 Determination of potassium oxide by ICP/AES . 10
11 Determination of chromium(III) oxide by ICP/AES . 11
12 Determination of zirconium oxide by ICP/AES . 11
13 Determination of phosphorus(V) oxide by ICP/AES . 12
14 Determination of calcium by AAS . 14
15 Determination of magnesium oxide by AAS. 16
16 Determination of sodium oxide by AAS . 17
17 Determination of potassium oxide by AAS. 18
18 Determination of manganese oxide by AAS . 18
19 Determination of chromium(III) oxide by AAS . 20
20 Test report . 21

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ISO 21587-3:2007(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 21587-3 was prepared by Technical Committee ISO/TC 33, Refractories.
ISO 21587 consists of the following parts, under the general title Chemical analysis of aluminosilicate
refractory products (alternative to the X-ray fluorescence method):
⎯ Part 1: Apparatus, reagents, dissolution and gravimetric silica
⎯ Part 2: Wet chemical analysis
⎯ Part 3: Inductively coupled plasma and atomic absorption spectrometry methods

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INTERNATIONAL STANDARD ISO 21587-3:2007(E)

Chemical analysis of aluminosilicate refractory products
(alternative to the X-ray fluorescence method) —
Part 3:
Inductively coupled plasma and atomic absorption
spectrometry methods
1 Scope
This part of ISO 21587 specifies inductively coupled plasma/atomic emission (ICP/AE) spectrometry and
flame atomic absorption (FAA) spectrometry methods for the chemical analysis of aluminosilicate refractory
products and raw materials.
The methods are applicable to the determination of the following:
⎯ silicon(IV) oxide (SiO )
2
⎯ aluminium oxide (Al O )
2 3
⎯ iron(III) oxide (total iron oxide calculated as Fe O )
2 3
⎯ titanium(IV) oxide (TiO )
2
⎯ manganese(II) oxide (MnO)
⎯ calcium oxide (CaO)
⎯ magnesium oxide (MgO)
⎯ sodium oxide (Na O)
2
⎯ potassium oxide (K O)
2
⎯ chromium(III) oxide (Cr O )
2 3
⎯ zirconium oxide (ZrO )
2
⎯ phosphorous(V) oxide (P O )
2 5
This part of ISO 21587 gives alternatives to the X-ray flluorescence (XRF) method given in ISO 12677:2003,
Chemical analysis of refractory products by XRF — Fused cast bead method.

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ISO 21587-3:2007(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 21587-1:2007, Chemical analysis of aluminosilicate refractory products (alternative to the X-ray
fluorescence method) — Part 1: Apparatus, reagents, dissolution and gravimetric silica
ISO 21587-2:2007, Chemical analysis of aluminosilicate refractory products (alternative to the X-ray
fluorescence method) — Part 2: Wet chemical analysis
ISO 26845, Chemical analysis of refractories — General requirements for wet chemical analysis, atomic
absorption spectrometry and inductively coupled plasma methods
3 Determination of residual silica in solution by ICP/AES
3.1 Principle
The residual silica remaining in stock solutions (S1) or (S′1) is determined using ICP/AES.
3.2 Reagents
Prepare the reagents specified in ISO 26845 and ISO 21587-1 and the following.
3.2.1 Aluminium oxide solution, Al O 5 mg/ml.
2 3
Weigh 2,65 g of aluminium (purity, more than 99,5 % by mass, having Si, less than 0,001 % by mass) into a
platinum dish (e.g. 100 ml). Cover the dish with a watch glass, add approximately 100 ml of hydrochloric acid
(1+1) and heat on a steam bath in order to dissolve the metal. After cooling, dilute to 1 l in a volumetric flask
with water.
3.2.2 Matrix solution 1.
Transfer an appropriate aliquot portion of the aluminium oxide solution (5 mg/ml) into a 500 ml volumetric flask
and dilute to the mark with water. Prepare this solution freshly whenever needed.
NOTE The amount of the aluminium oxide solution to be used is determined by the chemical composition of the
sample. For example, use 35 ml for the aluminium oxide solution of a sample containing 35 % by mass of aluminium oxide.
3.2.3 Matrix solution 2 or 2′.
Carry out the procedure given in 4.2.2.3 or 4.2.3.3 of ISO 21587-1:2007 without the sample, but omit heating
the fusion mixture or anhydrous sodium carbonate. The solution equivalent to stock solution (S1) or (S′1) is
referred to as matrix solution 2 or 2′, as applicable.
3.2.4 Series 2 solution for calibration.
Transfer appropriate amounts of aliquot portions of dilute standard silicon(IV) oxide solution (0,2 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 and either matrix solution 2 or 2′, respectively, and dilute to the mark with water.
Table 1 is shown as an example.
NOTE In Table 2, a typical example of the preparation of solutions is shown. Prepare an appropriate series of
solutions for calibration in accordance with the compositions of the samples, and the type and capabilities of instrument
used.
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ISO 21587-3:2007(E)
Table 1 — Example of Series 2 solution for calibration
Calibration Matrix Matrix solution Dilute standard Concentration of
solution solution 1 2 or 2′ silicon(IV) oxide solution
Series 2 solution
No. ml ml ml SiO mg/100 ml
2
1 10 10 0 0
2 10 10 1 0,2
3 10 10 2 0,4
4 10 10 5 1,0
5 10 10 10 2,0
6 10 10 15 3,0

3.3 Procedure
Determine the silicon(IV) oxide remaining in solution (S1) or (S′1) (4.2.2.3 or 4.2.3.3 in ISO 21587-1:2007) 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.
This solution, for the determination of dissolved silicon(IV) oxide, is referred to as diluted stock solution (S1d)
or (S1′d).
Spray a portion of diluted stock solution (S1d) or (S1′d) into the argon plasma flame of the inductively coupled
plasma/atomic emission (ICP/AE) spectrometer, and measure the emission intensity at, for example, the
wavelength of 251,61 nm.
3.4 Blank test
Carry out the procedure in 3.3 with blank solution (B1) or (B′1). The diluted blank solution equivalent to diluted
stock solution (S1d) or (S1′d) is referred to as diluted blank solution (B1d) or (B1′d).
3.5 Plotting the calibration graph
Using the calibration solution Series 2, carry out the emission procedure described in 3.3. Plot the relation
between the emission intensity and the mass of oxide, and 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.
3.6 Calculation
Calculate the mass fraction of silicon(IV) oxide, w , as a percentage, from the amount of silicon(IV) oxide
SiO
2
derived from the figures obtained from 3.3 and 3.4 and the calibration described in 3.5 using the equation:
500
mm−+m−m×
()()
12 3 4
10
w=× 100 (1)
SiO
2
m

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ISO 21587-3:2007(E)
where
m is the mass, in g, of the test portion (4.2.2.2 or 4.2.3.2 in ISO 21587-1:2007);
m , m are the mass, in g, differences in 4.2.2.3 or 4.2.3.3 in ISO 21587-1:2007;
1 2
m is the mass, in g, of silicon(IV) oxide in diluted stock solution (S1d or S′1d) as described in 3.3.
3
m is the mass, in g, of silicon(IV) oxide in diluted blank solution (B1d or B′1d) as described in 3.4.
4
4 Determination of iron(III) oxide by ICP/AES
4.1 Principle
The emission intensity of iron is measured by an ICP/AE spectrometer on solutions S1 or S′1, obtained from
4.2.2.3 or 4.2.3.3 of ISO 21587-1:2007.
4.2 Reagents
Any of the reagents described in 4.1, 4.2 and 4.3 of ISO 21587-1:2007 and the following are required.
4.2.1 Aluminium oxide solution, Al O 2 mg/ml.
2 3
Dilute aluminium oxide solution (10 mg/ml) with water to a concentration of one-fifth.
4.2.2 Mixed standard solution 2, Fe O 0,04 mg/ml, TiO 0,04 mg/ml, MnO 0,01 mg/ml, Cr O
2 3 2 2 3
0,01 mg/ml, ZrO 0,01 mg/ml.
2
Transfer 40 ml each of the standard iron(III) oxide solution (1 mg/ml) and the standard titanium(IV) oxide
solution (1 mg/ml), and 10 ml each of the standard manganese(II) oxide solution (1 mg/ml), the standard
chromium(III) oxide solution (1 mg/ml) and the standard zirconium oxide solution (1 mg/ml), to a 1 000 ml
volumetric flask and dilute to the mark with water.
4.2.3 Matrix solution 2 or 2′.
See 3.2.3.
4.2.4 Series 3 solutions for calibration.
Transfer appropriate aliquot portions of mixed standard solution 2 into each of several 100 ml volumetric
flasks. Add 10 ml of matrix solution 2 or matrix solution 2′, 5 ml of internal standard solution (Sc 0,1 mg/ml,
Y 0,1 mg/ml), and a specified amount of aluminium oxide solution (2 mg/ml), respectively, and dilute to the
mark with water.
NOTE An example of the preparation of solutions is shown in Table 2. Prepare an appropriate series of solutions for
calibration in accordance with the composition of the samples, and the type and capabilities of instrument used.
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ISO 21587-3:2007(E)
Table 2 — Example of Series 3 solution for calibration
(mass fraction of aluminium oxide is 30 %)
Matrix Internal Aluminium Mixed
Solution for
solution 2 standard oxide standard Concentration of solution
calibration
or 2′ solution solution solution 2
No. ml ml ml ml mg/100 ml
   Fe O TiO MnO Cr O ZrO
2 3 2 2 3 2
1 10 5 3 0 0,00 0,00 0,00 0,00 0,00
2 10 5 3 1 0,04 0,04 0,01 0,01 0,01
3 10 5 3 2 0,08 0,08 0,02 0,02 0,02
4 10 5 3 3 0,12 0,12 0,03 0,03 0,03
5 10 5 3 4 0,16 0,16 0,04 0,04 0,04
6 10 5 3 5 0,20 0,20 0,05 0,05 0,05
7 10 5 3 10 0,40 0,40 0,10 0,10 0,10
8 10 5 3 15 0,60 0,60 0,20 0,20 0,20
9 10 5 3 20 0,80 0,80 0,30 0,30 0,30

4.3 Procedure
Transfer a 10 ml aliquot portion of stock solution (S1) or (S′1), as prepared in 4.2.2.3 or 4.2.3.3 of
ISO 21587-1:2007, into a 100 ml volumetric flask. Add 5 ml of internal standard solution (Sc 0,1 mg/ml,
Y 0,1 mg/ml), and dilute to the mark with water. This solution is designated as stock solution (S1′dScY) or
(S1′dSCY).
Spray a portion of stock solution (S1dScY) or (S1′dScY) into the argon plasma flame of an ICP/AE
spectrometer, and measure the iron emission intensity at the appropriate wavelength, for example, 259,94 nm.
4.4 Blank test
Transfer a 10 ml aliquot portion of blank solution (B1) or (B′1), (4.2.2.4 or 4.3.2.4 in ISO 21587-1:2007) and
carry out the procedure given in 4.3. The solution corresponding to stock solution (B1) or (B′1) is designated
as blank solution (B1dScY) or (B′1dScY).
4.5 Plotting the calibration graph
Use Series 3 solutions for calibration. Carry out the procedure described in 4.3 and plot the relation between
the emission intensity and the mass of iron(III) oxide. Prepare the calibration graph by adjusting the curve so
that it passes through the point of origin.
4.6 Calculation
Calculate the mass fraction of iron(III) oxide, w , as a percentage, using the following equation, with
Fe O
2 3
iron(III) oxide that is derived from the emission intensity in 4.3 and 4.4, and the calibration in 4.5.
mm− 500
12
w ×× 100 (2)
Fe O
23
m 10
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ISO 21587-3:2007(E)
where
m is the mass, in g, of iron(III) oxide in stock solution (S1dScY) or (S′1dScY);
1
m is the mass, in g, of iron(III) oxide in blank solution (B1dScY) or (B′1dScY);
2
m is the mass, in g, of the test portion in 4.2.2.2 or 4.3.2.2 of ISO 21587-1:2007.
5 Determination of titanium(IV) oxide by ICP/AES
5.1 Principle
The emission intensity of the titanium is measured by an ICP/AE spectrometer on stock solution (S1dScY) or
(S′1dScY).
5.2 Procedure
Spray a portion of stock solution (S1dScY) or (S′1dScY) (4.3) into the argon plasma flame of an ICP/AE
spectrometer, and measure the titanium emission intensity at a wavelength of 334,94 nm.
5.3 Blank test
Carry out the procedure described in 5.2 for blank solution (B1dScY) or (B′1dScY) obtained in 4.4.
5.4 Plotting the calibration graph
Using the Series 3 solutions (4.2.4), carry out the procedure described in 5.2, and plot the relation between
the emission intensity and titanium(IV) oxide. Prepare the calibration graph by adjusting the curve so that it
passes through the point of origin.
5.5 Calculation
Calculate the mass fraction of titanium oxide(IV), w , as a percentage,, using the following equation with the
TiO
2
amount of titanium(IV) oxide derived from the emission intensity obtained in 5.2 and 5.3, and the calibration in
5.4.
mm−
500
12
w=×× 100 (3)
TiO
2
m 10
where
m is the mass, in g, of titanium(IV) oxide in stock solution (S1dScY) or (S′1dScY);
1
m is the mass, in g, of titanium(IV) oxide in blank solution (B1dScY) or (B′1dScY);
2
m is the mass, in g, of the test portion described in 4.2.2.2 or 4.3.2.2 of ISO 21587-1:2007.
6 Determination of manganese(II) oxide by ICP/AES
6.1 Principle
The emission intensity of manganese from stock solution (S1dScY) or (S′1dScY) is measured by an ICP/AE
spectrometer.
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ISO 21587-3:2007(E)
6.2 Procedure
Spray a portion of stock solution (S1dScY) or (S′1dScY) obtained in 4.3 into the argon plasma flame of an
ICP/AE spectrometer, and measure the emission intensity at a wavelength of 257,61 nm, for example.
6.3 Blank test
Carry out the procedure described in 6.2 using blank solution (B1dScY) or (B′1dScY) obtained in 4.4.
6.4 Plotting the calibration graph
Carry out the procedure described in 6.2 using Series 3 solutions for calibration (4.2.4). Plot the relation
between the emission intensity and the mass of manganese(II) oxide, and prepare the calibration graph by
adjusting the curve so that it passes through the point of origin.
6.5 Calculation
Calculate the mass fraction of manganese(II) oxide, w , as a percentage, using the following equation. Use
MnO
the mass of manganese(II) oxide that is derived from the emission intensity obtained in 6.2. and 6.3. and the
calibration in 6.4.
mm−
500
12
w=×× 100 (4)
MnO
m 10
where
m is the mass, in g, of manganese(II) oxide in stock solution (S1dScY) or (S′1dScY);
1
m is the mass, in g, of manganese(II) oxide in blank solution (B1dScY) or (B′1dScY).
2
m is the mass, in g, of the test portion described in 4.2.2.2 or 4.3.2.2 of ISO 21587-1:2007.
7 Determination of calcium oxide by ICP/AES
7.1 Principle
The emission intensity of calcium in solution (S4) is measured by an ICP/AE spectrometer.
7.2 Series 1 solution for calibration
See 10.2.2 in ISO 21587-2:2007. Transfer aliquot portions of mixed standard solution 1 to each of several
100 ml volumetric flasks. To each, add 5 ml of hydrochloric acid (1+1) and an appropriate amount of standard
solution I of aluminium oxide, and dilute to the mark with water. Typical examples of preparation are shown in
Table 3.
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ISO 21587-3:2007(E)
Table 3 — Example of Series 1 solution for calibration
(mass fraction of aluminium oxide is 30 %)
Solution for Aluminium oxide Hydrochloric Mixed standard
Concentration of solution
calibration solution I acid (1+1) solution 1
No. ml ml ml mg/100 ml
  CaO MgO NaO K O
2 2
1 3 5 0 0 0 0 0
2 3 5 2 0,2 0,2 0,2 0,2
3 3 5 4 0,4 0,4 0,4 0,4
4 3 5 6 0,6 0,6 0,6 0,6
5 3 5 8 0,8 0,8 0,8 0,8
6 3 5 10 1.0 1.0 1.0 1.0
7 3 5 20 2,0 2,0 2,0 2,0
8 3 5 30 3,0 3,0 3,0 3,0
9 3 5 40 4,0 4,0 4,0 4,0
10 3 5 50 5,0 5,0 5,0 5,0
11 3 5 60 6,0 6,0 6,0 6,0

7.3 Procedure
Spray a portion of stock solution (S4) (4.3.4.3 in ISO 21587-1:2007) into the argon plasma flame of an ICP/AE
spectrometer, and measure the emission intensity at a wavelength of 393,37 nm, for example.
7.4 Blank test
Carry out the procedure described in 7.3 using blank solution (B4).
7.5 Plotting the calibration graph
Carry out the procedure described in 7.3 using Series 1 solutions for calibration. Plot the relation between the
emission intensity and the mass of calcium oxide, and prepare the calibration graph by adjusting the curve so
that it passes through the point of origin.
7.6 Calculation
Calculate the mass fraction of calcium oxide, w , as a percentage, using the following equation. Use the
CaO
mass of calcium oxide derived from the emission intensity obtained in 7.3 and 7.5, and the calibration
described in 7.6.
mm−
12
w=× 100 (5)
CaO
m
where
m is the mass, in g, of calcium oxide in stock solution (S4);
1
m is the mass, in g, of calcium oxide in blank solution (B4);
2
m is the mass, in g, of the test portion (4.3.4.3 in ISO 21587-1:2007).
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ISO 21587-3:2007(E)
8 Determination of magnesium oxide by ICP/AES
8.1 Principle
The emission intensity of magnesium in stock solution (S4) is measured by an ICP/AE spectrometer.
8.2 Procedure
Spray a portion of stock solution (S4) obtained in 4.3.4.3 in ISO 21587-1:2007 into the argon plasma flame of
an ICP/AE spectrometer, and measure the intensity at a wavelength of 279,55 nm.
8.3 Blank test
Carry out the procedure described in 8.2 with blank solution (B4) obtained in 4.3.4.4 in ISO 21587-1:2007.
8.4 Plotting the calibration graph
Use Series 1 solutions for calibration described in 10.2.2 in ISO 21587-2:2007. Carry out the procedure
described in 8.2 and plot the relation between the emission intensity and the mass of magnesium oxide, and
prepare the calibration graph by adjusting the curve so that it passes through the point of origin.
8.5 Calculation
Calculate the mass fraction of magnesium oxide, w , as a percentage, using the following equation by
MgO
using the mass of magnesium oxide derived from the emission intensity obtained in 8.2 and 8.3, and the
calibration described in 8.4.
mm−
12
w=× 100 (6)
MgO
m
where
m is the mass, in g, of magnesium oxide in stock solution (S4);
1
m is the mass, in g, of magnesium oxide in blank solution (B4);
2
m is the mass, in g, of the test portion in 4.3.4.2 in ISO 21587-1:2007.
9 Determination of sodium oxide by ICP/AES
9.1 Principle
The emission intensity of sodium is measured by an ICP/AE spectrometer on stock solution (S4).
9.2 Procedure
Spray a portion of stock solution (S4) obtained in 4.3.4.3 in ISO 21587-1:2007 into the argon plasma flame of
an ICP/AE spectrometer, and measure the intensity at a wavelength of 589,00 nm.
9.3 Blank test
Carry out the procedure described in 9.2 with blank solution (B4) obtained in 4.3.4.4 in ISO 21587-1:2007.
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ISO 21587-3:2007(E)
9.4 Pl
...