SIST EN ISO 10058-3:2009

Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray fluorescence method) - Part 3: Flame atomic absorption spectrometry (FAAS) and inductively coupled plasma emission spectrometry (ICP-AES) (ISO 10058-3:2008)

This part of ISO 10058 specifies atomic absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods for the chemical analysis of magnesite and dolomite refractory products and raw materials. It is applicable to components within the ranges of determination given in Table 1.

Chemische Analyse von feuerfesten Erzeugnissen aus Magnesit und Dolomit (Alternative zur Röntgenfluoreszenzanalyse) - Teil 3: Flammenatomabsorptionsspektroskopie (FAAS) und Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES) (ISO 10058-3:2008)

Dieser Teil von ISO 10058 legt im Rahmen der chemischen Analyse für feuerfeste Erzeugnisse und Rohstoffe aus Magnesit und Dolomit die Vorgehensweise bei der Atomabsorptionsspektroskopie (AAS) und bei der Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP AES) fest, die für die in Tabelle 1 angegebenen Bereiche anwendbar ist.
Tabelle 1  Bereich für die Bestimmung
Bestandteil   Bereich
Massenanteil in %   Bestandteil   Bereich
Massenanteil in %
SiO2      0,1   bis    10   Na2O   0,01 bis 1
Al2O3      0,05 bis 10   K2O   0,01 bis 1
Fe2O3      0,01 bis 10   Cr2O3   0,01 bis 3
TiO2      0,01 bis   1   ZrO2   0,01 bis 1
MnO      0,01 bis   1   P2O5   0,01 bis 5
CaO      0,01 bis   10      
ANMERKUNG   Die angegebenen Werte sind bezogen auf den Zustand nach der Bestimmung des Glühverlustes.
Nach diesem Teil von ISO 10058 werden im Rahmen der chemischen Analyse die folgenden Bestimmungen durchgeführt:
a)   Silicium(IV) oxid (SiO2);
b)   Aluminiumoxid (Al2O3);
c)   Eisen(III) oxid (Gesamteisengehalt, berechnet als Fe2O3);
d)   Titan(IV) oxid (TiO2);
e)   Mangan(II) oxid (MnO);
f)   Calciumoxid (CaO);
g)   Natriumoxid (Na2O);
h)   Kaliumoxid (K2O);
i)   Chrom(III) oxid (Cr2O3)
j)   Zirkoniumoxid (ZrO2);
k)   Phosphor(V) oxid (P2O5).

Analyse chimique des produits de magnésie et de dolomie (méthode alternative a la méthode par fluorescence de rayons X) - Partie 3: Méthodes par spectrométrie d'absorption atomique dans la flamme (FAAS) et par spectrométrie d'émission de plasma a couplage inductif (ICP-AES) (ISO 10058-3:2008)

L'ISO 10058-3:2008 spécifie des méthodes de spectrométrie d'absorption atomique dans la flamme (FAAS) et de spectrométrie d'émission atomique à plasma induit par haute fréquence (ICP-AES) pour l'analyse chimique des produits et des matières premières réfractaires de magnésie et de dolomie.

Kemijska analiza magnezitnih in dolomitnih ognjevzdržnih izdelkov (alternativa rentgenski fluorescenčni metodi) - 3. del: Plamenska atomska absorpcijska spektrometrija (FAAS) in emisijska spektrometrija z induktivno sklopljeno plazmo (ICP-AES) (ISO 10058-3:2008)

General Information

• Status: Published
• Publication Date: 09-Feb-2009
• ICS: 71.040.40 - Chemical analysis
• ICS: 73.080 - Non-metalliferous minerals
• ICS: 81.080 - Refractories
• Technical Committee: IKER - Ceramics
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 19-Dec-2008
• Due Date: 23-Feb-2009
• Completion Date: 10-Feb-2009
• Ref Project: EN ISO 10058-3:2008 - Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray fluorescence method) - Part 3: Flame atomic absorption spectrophotometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) (ISO 10058-3:2008)

Relations

• Replaces: SIST EN ISO 10058:1998 - Magnesites and dolomites - Chemical analysis (ISO 10058:1992)
• Effective Date: 01-Mar-2009

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 10058-3:2009
01-marec-2009
1DGRPHãþD
SIST EN ISO 10058:1998
.HPLMVNDDQDOL]DPDJQH]LWQLKLQGRORPLWQLKRJQMHY]GUåQLKL]GHONRYDOWHUQDWLYD
UHQWJHQVNLIOXRUHVFHQþQLPHWRGLGHO3ODPHQVNDDWRPVNDDEVRUSFLMVND
VSHNWURPHWULMD)$$6LQHPLVLMVNDVSHNWURPHWULMD]LQGXNWLYQRVNORSOMHQRSOD]PR
,&3$(6,62
Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray
fluorescence method) - Part 3: Flame atomic absorption spectrometry (FAAS) and
inductively coupled plasma emission spectrometry (ICP-AES) (ISO 10058-3:2008)
Chemische Analyse von feuerfesten Erzeugnissen aus Magnesit und Dolomit
(Alternative zur Röntgenfluoreszenzanalyse) - Teil 3:
Flammenatomabsorptionsspektroskopie (FAAS) und Atomemissionsspektrometrie mit
induktiv gekoppeltem Plasma (ICP-AES) (ISO 10058-3:2008)
Analyse chimique des produits de magnésie et de dolomie (méthode alternative a la
méthode par fluorescence de rayons X) - Partie 3: Méthodes par spectrométrie
d'absorption atomique dans la flamme (FAAS) et par spectrométrie d'émission de
plasma a couplage inductif (ICP-AES) (ISO 10058-3:2008)
Ta slovenski standard je istoveten z: EN ISO 10058-3:2008
ICS:
71.040.40 Kemijska analiza Chemical analysis
73.080 Nekovinske rudnine Non-metalliferous minerals
81.080 Ognjevzdržni materiali Refractories
SIST EN ISO 10058-3:2009 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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EUROPEAN STANDARD
EN ISO 10058-3
NORME EUROPÉENNE
EUROPÄISCHE NORM
December 2008
ICS 73.080 Supersedes EN ISO 10058:1996
English Version
Chemical analysis of magnesite and dolomite refractory
products (alternative to the X-ray fluorescence method) - Part 3:
Flame atomic absorption spectrophotometry (FAAS) and
inductively coupled plasma atomic emission spectrometry (ICP-
AES) (ISO 10058-3:2008)
Analyse chimique des produits de magnésie et de dolomie Chemische Analyse von feuerfesten Erzeugnissen aus
(méthode alternative à la méthode par fluorescence de Magnesit und Dolomit (Alternative zur
rayons X) - Partie 3: Méthodes par spectrométrie Röntgenfluoreszenzanalyse) - Teil 3:
d'absorption atomique dans la flamme (FAAS) et Flammenatomabsorptionsspektroskopie (FAAS) und
spectrométrie d'émission atomique avec plasma induit par Atomemissionsspektrometrie mit induktiv gekoppeltem
haute fréquence (ICP-AES) (ISO 10058-3:2008) Plasma (ICP-AES) (ISO 10058-3:2008)
This European Standard was approved by CEN on 1 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 10058-3:2008: E
worldwide for CEN national Members.

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EN ISO 10058-3:2008 (E)
Contents Page
Foreword .3

2

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EN ISO 10058-3:2008 (E)
Foreword
This document (EN ISO 10058-3:2008) 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.
This document supersedes EN ISO 10058:1996.
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 10058-3:2008 has been approved by CEN as a EN ISO 10058-3:2008 without any
modification.

3

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INTERNATIONAL ISO
STANDARD 10058-3
First edition
2008-12-01


Chemical analysis of magnesite and
dolomite refractory products (alternative
to the X-ray fluorescence method) —
Part 3:
Flame atomic absorption
spectrophotometry (FAAS) and
inductively coupled plasma atomic
emission spectrometry (ICP-AES)
Analyse chimique des produits de magnésie et de dolomie (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 10058-3:2008(E)
©
ISO 2008

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ISO 10058-3:2008(E)
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ii © ISO 2008 – All rights reserved

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ISO 10058-3:2008(E)
Contents Page
Foreword .iv
1 Scope.1
2 Normative references.1
3 Instrumental methods using ICP-AES.2
3.1 Determination of residual silica in stock solutions (S1) by ICP-AES .2
3.2 Determination of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide,
manganese(II) oxide, calcium oxide, chromium(III) oxide and zirconium oxide using stock
solutions (S1) or (S′1) by ICP-AES.3
3.3 Determination of sodium oxide and potassium oxide using stock solutions (S4)
by ICP-AES.6
3.4 Determination of phosphorus(V) oxide by ICP-AES.7
4 Instrumental methods using FAAS .9
4.1 Determination of manganese(II) oxide, calcium oxide and chromium(III) oxide by FAAS .9
4.2 Determination of calcium oxide, sodium oxide and potassium oxide using stock solutions
(S3) by FAAS.11
5 Test report.13

© ISO 2008 – All rights reserved iii

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ISO 10058-3:2008(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 10058-3 was prepared by Technical Committee ISO/TC 33, Refractories.
This first edition of ISO 10058-3, together with ISO 10058-1 and ISO 10058-2, cancels and replaces
ISO 10058:1992 which has been technically revised to include the increasing use of flame atomic absorption
spectrophotometry (FAAS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) methods
as well some improvements in the wet chemical analyses procedures developed in Japan.
ISO 10058 consists of the following parts, under the general title Chemical analysis of magnesite and dolomite
refractory products (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 spectrophotometry (FAAS) and inductively coupled plasma atomic
emission spectrometry (ICP-AES)

iv © ISO 2008 – All rights reserved

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INTERNATIONAL STANDARD ISO 10058-3:2008(E)

Chemical analysis of magnesite and dolomite refractory
products (alternative to the X-ray fluorescence method) —
Part 3:
Flame atomic absorption spectrophotometry (FAAS) and
inductively coupled plasma atomic emission spectrometry
(ICP-AES)
1 Scope
This part of ISO 10058 specifies atomic absorption spectrometry (AAS) and inductively coupled plasma
atomic emission spectrometry (ICP-AES) methods for the chemical analysis of magnesite and dolomite
refractory products and raw materials.
It is applicable to components within the ranges of determination given in Table 1.
Table 1 — Range of determination (percentage by mass)
Component Range Component Range
SiO 0,1 to 10 Na O 0,01 to 1
2 2
Al O 0,05 to 10 K O 0,01 to 1
2 3 2
Fe O 0,01 to 10 Cr O 0,01 to 3
2 3 2 3
TiO 0,01 to 1 ZrO 0,01 to 1
2 2
MnO 0,01 to 1 P O 0,01 to 5
2 5
CaO 0,01 to 10 — —
LOI 0,01 to 60 — —
NOTE These values are after the loss on ignition (LOI) has been taken into account.
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 10058-1:2008, Chemical analysis of magnesite and dolomite refractory products (alternative to the X-ray
fluorescence method) — Part 1: Apparatus, reagents, dissolution and 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
© ISO 2008 – All rights reserved 1

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ISO 10058-3:2008(E)
3 Instrumental methods using ICP-AES
3.1 Determination of residual silica in stock solutions (S1) by ICP-AES
3.1.1 Principle
The residual silica remaining in solutions (S1) (see ISO 10058-1:2008, Annex A) is determined using ICP-AES.
3.1.2 Reagents
3.1.2.1 Series 1 solution for calibration.
Transfer appropriate amounts of aliquot portions of dilute silicon(IV) oxide standard solution (0,08 mg/ml)
precisely to several 100 ml volumetric flasks in accordance with the composition of the samples. To each, add
10 ml of matrix solution 1 and dilute to the mark with water. An example is shown in Table 2.
In this table, a typical example of the preparation of solutions is shown. In accordance with the compositions
of the samples, and the types and capabilities of the instrument used, an appropriate series of solutions for
calibration is prepared.
Table 2 — Example of series 1 solution for calibration
Series 1 Matrix solution 1 Dilute silicon(IV) oxide Concentration
solution 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) as follows.
Transfer 10 ml of stock solution (S1) to a 100 ml volumetric flask and dilute to the mark with water.
This solution, which is used for the determination of dissolved silicon(IV) oxide, is designated 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 a wavelength of 251,611 nm.
3.1.4 Blank test
Carry out the procedure in 3.1.3 with blank solution (B1) (see ISO 10058-1:2008, Annex A).
The equivalent diluted blank solution to diluted stock solution (S1d) is designated as diluted blank solution
(B1d).
2 © ISO 2008 – All rights reserved

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ISO 10058-3:2008(E)
3.1.5 Plotting the calibration graph
Using the series 1 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.
Carry out a new calibration 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 , expressed as a percentage, using Equation (1), from
SiO
2
the amount of 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 calculated in accordance with ISO 10058-1:2008, 8.2.2.3.1, in
grams (g);
m is the mass from ISO 10058-1:2008, 8.2.2.3.3, in grams (g);
1
m is the mass from ISO 10058-1:2008, 8.2.2.4, 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
3.2 Determination of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide,
manganese(II) oxide, calcium oxide, chromium(III) oxide and zirconium oxide using stock
solutions (S1) or (S′1) by ICP-AES
3.2.1 Principle
The emission intensity of silicon(IV) oxide, aluminium oxide, iron(III) oxide, titanium(IV) oxide, manganese(II)
oxide, calcium oxide, chromium(III) oxide and zirconium oxide is measured by ICP-AE spectrometer for stock
solutions (S1) or (S′1) (see ISO 10058-1:2008, Annex A). This method should be applied to components in
(S1) or (S′1) in accordance with Table 3.
Table 3 — Range of determination (percentage by mass)
Component Range Component Range
SiO 0,1 to 10 MnO 0,01 to 1
2
Al O 0,05 to 10 CaO 0,01 to 10
2 3
Fe O 0,01 to 10 Cr O 0,01 to 3
2 3 2 3
TiO 0,01 to 1 ZrO 0,01 to 1
2 2
NOTE 1 When solution (S1) is used, the SiO is residual silica. When solution (S′1) is
2
used, the SiO is all of 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.
© ISO 2008 – All rights reserved 3

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ISO 10058-3:2008(E)
3.2.2 Reagents
Reagents given in ISO 10058-1:2008, Clause 5, and the following.
3.2.2.1 Mixed standard solution 1, 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 0,02 mg/ml, ZrO 0,005 mg/ml.
2 2 3 2
Transfer an aliquot portion (1 mg/ml) 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
(20 ml) and zirconium oxide (5 ml) solutions into a 1 000 ml volumetric flask and dilute to the mark with water.
3.2.2.2 Matrix solution 2 or 2′.
Carry out the procedure given in ISO 10058-1:2008, 8.2.2.3 or 8.2.3.3 without the sample, but omit heating
the fusion mixture or anhydrous sodium carbonate.
The equivalent solution to stock solution (S1) or (S′1) is designated as matrix solution 2 or 2′ as applicable.
3.2.2.3 Internal standard solution.
Transfer 10 ml of standard scandium solution (1 mg/ml) and standard yttrium solution (1 mg/ml) into a
volumetric 100 ml flask and dilute to the mark with
...