EN 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 determination of gravimetric silica (ISO 10058-1:2008)

ISO 10058-1:2008 specifies apparatus, reagents, dissolution and gravimetric silica analysis for the chemical analysis of magnesite and dolomite refractory products and raw materials.

Chemische Analyse von feuerfesten Erzeugnissen aus Magnesit und Dolomit (Alternative zur Röntgenfluoreszenzanalyse) - Teil 1: Geräte, Reagenzien, Aufschluss und gravimetrische Bestimmung von Silicium(IV)-oxid (ISO 10058-1:2008)

Dieser Teil von ISO 10058 legt die Geräte, Reagenzien, den Aufschluss und die gravimetrische Bestimmung
von Silicium(IV)-oxid für die chemische Analyse von feuerfesten Erzeugnissen und Rohstoffen aus Magnesit
und Dolomit fest.
Dieser Teil von ISO 10058 gilt für die nach Tabelle 1 angegebenen Bestimmungsbereiche.
ISO 10058 legt die Verfahrensweisen für die chemische Analyse von feuerfesten Erzeugnissen und
Rohstoffen aus Magnesit und Dolomit innerhalb der Bestimmungsbereiche nach Tabelle 1 fest.

Analyse chimique des produits de magnésie et de dolomie (méthode alternative à la méthode par fluorescence de rayons X) - Partie 1: Appareillage, réactifs, mise en solution et détermination de la teneur en silice par gravimétrie (ISO 10058-1:2008)

L'ISO 10058-1:2008 spécifie l'appareillage, les réactifs, la mise en solution et la détermination de la teneur en silice par gravimétrie pour l'analyse chimique des matières premières et produits réfractaires contenant de la magnésie et de la dolomie.

Kemijska analiza magnezitnih in dolomitnih ognjevzdržnih izdelkov (alternativa rentgenski fluorescenčni metodi) - 1. del: Aparati, reagenti, raztapljanje in gravimetrična silika (ISO 10058-1:2008)

General Information

• Status: Published
• Publication Date: 30-Nov-2008
• Withdrawal Date: 29-Jun-2009
• ICS: 73.080 - Non-metalliferous minerals
• ICS: 81.080 - Refractories
• Technical Committee: CEN/TC 187 - Refractory products and materials
• Drafting Committee: CEN/TC 187/WG 4 - Chemical analysis
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 01-Dec-2008
• Due Date: 22-Mar-2009
• Completion Date: 01-Dec-2008
• Ref Project: SIST EN ISO 10058-1:2009 - 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 (ISO 10058-1:2008)

Relations

• Replaces: EN ISO 10058:1996 - Magnesites and dolomites - Chemical analysis (ISO 10058:1992)
• Effective Date: 22-Dec-2008

Overview

EN 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 determination of gravimetric silica. This CEN/ISO standard specifies the laboratory equipment, reagent quality, sample preparation, decomposition/dissolution techniques and the gravimetric determination of silica (SiO2) for magnesite and dolomite refractory products and raw materials. It is intended as a wet‑chemical alternative to X‑ray fluorescence (XRF) analysis.

Key topics and technical requirements

• Scope and applicability: Procedures apply to magnesite and dolomite refractories within defined ranges (examples: SiO2 0.1–10% by mass; MgO 30–99.9%; CaO 0.01–60%; LOI up to 60%). Values are expressed after loss on ignition (LOI) correction.
• Apparatus: Normal laboratory glassware and equipment as referenced in ISO 26845 (general requirements for wet chemical analysis, AAS and ICP‑AES).
• Reagents and solution standards: Requirement to use analytical‑grade reagents and distilled (or equivalent) water. The standard details preparation and verification of standard volumetric solutions (e.g., CyDTA, zinc, EDTA) and stock oxide solutions (Al2O3, CaO, Cr2O3, Fe2O3 and dilutions).
• Sample preparation and LOI: Instructions for sample treatment and gravimetric measurement of loss on ignition prior to chemical determinations.
• Decomposition and dissolution methods: General decomposition techniques and two principal dissolution routes:
  • Fusion methods (alkali/flux fusion) for complete dissolution of refractory matrices.
  • Hydrofluoric acid attack for silicate breakdown where appropriate.
• Silica determination: Gravimetric separation and weighing procedures for SiO2 quantification, calculation and expression of results, and guidelines for test reporting.
• Quality and reference documents: Normative references include ISO 6353 series (reagent specifications) and ISO 26845.

Applications and users

• Who uses it: Analytical laboratories, refractory manufacturers, raw material suppliers, quality control personnel, materials scientists, metallurgists and regulatory bodies.
• Practical uses:
  • Quality control of magnesite and dolomite refractory bricks, castables and raw minerals.
  • Routine laboratory analysis where XRF is not available or as a confirmatory wet‑chemical method.
  • R&D and failure analysis requiring precise silica determination and chemical composition profiling.

Related standards

• ISO 10058 series:
  • Part 2: Wet chemical analysis
  • Part 3: FAAS and ICP‑AES methods
• ISO 26845:2008 - General requirements for wet chemical analysis, AAS and ICP‑AES
• ISO 6353 parts - Reagent specifications

Keywords: EN ISO 10058-1:2008, chemical analysis, magnesite, dolomite, refractory products, gravimetric silica, dissolution, hydrofluoric acid, fusion, wet chemical analysis, quality control.

Standards Content (Sample)

SLOVENSKI STANDARD
01-marec-2009
1DGRPHãþD
SIST EN ISO 10058:1998
.HPLMVNDDQDOL]DPDJQH]LWQLKLQGRORPLWQLKRJQMHY]GUåQLKL]GHONRYDOWHUQDWLYD
UHQWJHQVNLIOXRUHVFHQþQLPHWRGLGHO$SDUDWLUHDJHQWLUD]WDSOMDQMHLQ
JUDYLPHWULþQDVLOLND,62
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 (ISO 10058-1:2008)
Einführendes Element - Haupt-Element - Teil 1: Teil-Titel (ISO 10058-1:2008)
Analyse chimique des produits de magnésie et de dolomie (méthode alternative à la
méthode par fluorescence de rayons X) - Partie 1 : Appareillage, réactifs, mise en
solution et détermination de la teneur en silice par gravimétrie (ISO 10058-1:2008)
Ta slovenski standard je istoveten z: EN ISO 10058-1:2008
ICS:
71.040.40 Kemijska analiza Chemical analysis
73.080 Nekovinske rudnine Non-metalliferous minerals
81.080 Ognjevzdržni materiali Refractories
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN ISO 10058-1
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 1:
Apparatus, reagents, dissolution and determination of
gravimetric silica (ISO 10058-1:2008)
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 1: Appareillage, réactifs, mise en solution Röntgenfluoreszenzanalyse) - Teil 1: Geräte, Reagenzien,
et détermination de la teneur en silice par gravimétrie (ISO Aufschluss und gravimetrische Bestimmung von
10058-1:2008) Silicium(IV)-oxid (ISO 10058-1:2008)
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 10058-1:2008: E
worldwide for CEN national Members.

Contents Page
Foreword .3

Foreword
This document (EN ISO 10058-1:2008) 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 10058-1:2008 has been approved by CEN as a EN ISO 10058-1:2008 without any
modification.
INTERNATIONAL ISO
STANDARD 10058-1
First edition
2008-12-01
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
Analyse chimique des produits de magnésie et de dolomie (méthode
alternative à la méthode par fluorescence de rayons X) —
Partie 1: Appareillage, réactifs, mise en solution et détermination de la
teneur en silice par gravimétrie

Reference number
ISO 10058-1:2008(E)
©
ISO 2008
ISO 10058-1:2008(E)
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ii © ISO 2008 – All rights reserved

ISO 10058-1:2008(E)
Contents Page
Foreword .iv
1 Scope.1
2 Normative references.1
3 Terms and definitions .2
4 Apparatus.2
5 Reagents.2
6 Sample preparation .6
7 Determination of loss on ignition (gravimetric) .6
8 Decomposition of the sample and preparation of solutions used in the analysis.6
8.1 General decomposition techniques .6
8.2 Dissolution methods by fusion.6
8.3 Dissolution methods by hydrofluoric acid attack.8
9 Calculation and expression of test results.10
10 Examination and adoption of test results.10
11 Test report.11
Annex A (informative) References for stock solutions and blank solutions in ISO 10058-1:2008 .12

ISO 10058-1:2008(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 10058-1 was prepared by Technical Committee ISO/TC 33, Refractories.
This first edition of ISO 10058-1, together with ISO 10058-2 and ISO 10058-3, 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

INTERNATIONAL STANDARD ISO 10058-1:2008(E)

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
1 Scope
This part of ISO 10058 specifies apparatus, reagents, dissolution and gravimetric silica analysis for the
chemical analysis of magnesite and dolomite refractory products and raw materials.
This part of ISO 10058 is applicable to the ranges of determination given in Table 1.
ISO 10058 specifies procedures for the chemical analysis of magnesite and dolomite refractory products and
raw materials 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 MgO 30 to 99,9
Al O 0,05 to 10 Na O 0,01 to 1
2 3 2
Fe O 0,01 to 10 K O 0,01 to 1
2 3 2
TiO 0,01 to 1 Cr O 0,01 to 3
2 2 3
MnO 0,01 to 1 ZrO 0,01 to 1
CaO 0,01 to 60 P O 0,01 to 5
2 5
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 6353-1, Reagents for chemical analysis — Part 1: General test methods
ISO 6353-2, Reagents for chemical analysis — Part 2: Specifications — First series
ISO 6353-3, Reagents for chemical analysis — Part 3: Specifications — Second series
ISO 26845:2008, 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 10058-1:2008(E)
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 26845 apply.
4 Apparatus
Normal laboratory apparatus and other apparatus as defined in ISO 26845.
5 Reagents
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only
distilled water or water of equivalent purity.
Reagents shall conform to the requirements of ISO 6353-1, ISO 6353-2 and ISO 6353-3 as appropriate.
Specific requirements for reagents are given in the appropriate clause.
Use reagents that are defined in ISO 26845 and the following.
5.1 Standard volumetric solutions.
5.1.1 Standard volumetric CyDTA solution, c(CyDTA) = 0,01 mol/l.
Add 8 ml of sodium hydroxide solution (100 g/l) and approximately 150 ml of water to 3,65 g of
trans-1,2-cyclohexanediamine -N,N,N′,N′ -tetraacetic acid monohydrate (CyDTA), and dissolve by heating.
After cooling, dilute to 1 000 ml with water; approximately 25 ml of water are required.
Determine the exact strength of this solution by titration against the standard volumetric zinc solution,
c(Zn) = 0,01 mol/l.
5.1.2 Standard volumetric zinc solution, c(Zn) = 0,01 mol/l.
Wash the surface of the zinc (purity greater than 99,9 % by mass) with hydrochloric acid (1+3) and dissolve
the oxidized layer; subsequently, wash with water, ethanol and diethyl ether in succession, then dry in a
desiccator. Weigh 0,65 g (recorded to the nearest 0,000 1 g) of zinc and transfer it to a 300 ml beaker. Cover
with a watch glass. Add 20 ml of water and 5 ml of nitric acid carefully, and heat to dissolve on a steam bath.
After cooling, dilute to 1 000 ml in a volumetric flask with water.
Calculate the factor, F, of this zinc solution using Equation (1).
mA
F=× (1)
0,653 8 100
where
m is the mass of the weighed zinc, in grams (g);
A is the purity of the zinc, as a percentage by mass (%).
5.1.3 Standard volumetric EDTA solution, c(EDTA) = 0,02 mol/l.
Dissolve 7,5 g of EDTA Na (ethylenediamine-tetraacetic acid disodium salt dihydrate) in 1 l of water. Store in
a plastic bottle.
2 © ISO 2008 – All rights reserved

ISO 10058-1:2008(E)
Determine the factor, F, of the 0,02 mol/l standard volumetric EDTA solution as follows.
Transfer 50 ml of 0,01 mol/l zinc solution, obtained in 5.1.2, to a 300 ml beaker and add 50 ml of water. Drop
in sodium hydroxide solution (100 g/l) of up to pH 6 to pH 8 and add 2 ml of buffer solution (pH 10) and, while
stirring, add 3 to 4 drops of Eriochrome Black T solution as an indicator and titrate with 0,02 mol/l standard
volumetric EDTA solution. Observe and record the end point, which is when the reddish purple colour of the
solution is altered to blue.
Calculate the factor, F, of the 0,02 mol/l standard volumetric EDTA solution using Equation (2).
f × 50
F = (2)
2 ×V
where
f is the factor of 0,01 mol/l standard volumetric zinc solution;
V is the volume of 0,02 mol/l standard volumetric EDTA solution, in millilitres (ml).
5.2 Standard solutions.
5.2.1 Standard aluminium oxide solution, Al O 1 mg/ml.
2 3
Wash the surface of a sufficient amount of aluminium metal (approximately 0,6 g to 0,7 g), purity of more than
99,9 % by mass, with hydrochloric acid (1+4) to dissolve the oxidized layer. Then wash with water, ethanol
and diethyl ether in succession, and dry in a desiccator. Weigh 0,529 2 g of aluminium and transfer it to a
250 ml beaker. Cover the beaker with a watch glass, add 20 ml hydrochloric acid (1+1), and heat to dissolve.
After cooling, dilute to 1 000 ml with water in a volumetric flask.
5.2.2 Standard calcium oxide solution, CaO 1 mg/ml.
Dissolve 1,785 g of pure calcium carbonate that has been previously dried at 150 °C for 2 h, in a slight excess
of diluted hydrochloric acid (1+4) in a 250 ml beaker, covered with a watch glass. Boil to expel carbon dioxide,
cool and dilute to 1 000 ml with water in a volumetric flask.
5.2.3 Standard chromium(III) oxide solution, Cr O 1 mg/ml.
2 3
Dry between 2 g to 3 g of potassium dichromate at 110 °C for at least 2 h. Weigh 1,935 5 g of this and
dissolve in water. Dilute to 1 000 ml with water in a volumetric flask.
5.2.4 Dilute standard chromium(III) oxide solution, Cr O 0,025 mg/ml.
2 3
Pipette 25 ml of the standard chromic oxide solution (1 mg/ml) to a 1 000 ml volumetric flask and dilute to the
mark with water. Prepare this solution freshly when required.
5.2.5 Standard iron(III) oxide solution, Fe O 1 mg/ml.
2 3
Wash the surface of a sufficient amount of iron metal (purity greater than 99,9 % by mass) with hydrochloric
acid (1+4). Then dissolve the oxidized layer, wash with water, ethanol, and diethyl ether in succession. Dry in
a desiccator. Weigh 0,699 4 g of this, transfer to a beaker (200 ml) and cover with a watch glass. Add 40 ml of
hydrochloric acid (1+1) and heat on a steam bath until dissolved. After cooling, dilute to 1 000 ml with water in
a volumetric flask.
5.2.6 Dilute standard iron(III) oxide solution, Fe O 0,2 mg/ml.
2 3
Pipette 200 ml of the standard iron(III) oxide solution (Fe O 1 mg/ml) into a 1 000 ml volumetric flask and
2 3
dilute to the mark with water. Prepare this solution freshly when required.
ISO 10058-1:2008(E)
5.2.7 Dilute standard iron(III) oxide solution, Fe O 0,04 mg/ml.
2 3
Pipette 40 ml of the standard iron(III) oxide solution (Fe O 1 mg/ml) into a 1 000 ml volumetric flask and
2 3
dilute to the mark with water. Prepare this solution freshly when required.
5.2.8 Standard magnesium oxide solution, MgO 1 mg/ml.
Wash the surface of a sufficient amount of magnesium metal (purity greater than 99,9 % by mass) with
hydrochloric acid (1+1) to dissolve the oxidized layer. Wash with water, ethanol and diethyl ether in
succession and dry in a desiccator. Weigh 0,301 5 g of the washed magnesium, transfer to a 200 ml beaker
and cover with a watch glass. Add 20 ml of hydrochloric acid (1+1), and heat on a steam bath until dissolved.
After cooling, transfer to a 500 ml volumetric flask, and dilute to the mark with water.
5.2.9 Standard manganese(II) oxide solution, MnO 1 mg/ml.
Wash the surface of a sufficient mass of manganese metal (purity greater than 99,9 % by mass) with
hydrochloric acid (1+3) to dissolve the oxidized layer. Then wash with water, ethanol, and diethyl ether in
succession and dry in a desiccator. Weigh 0,774 5 g of this metal, transfer to a 200 ml beaker and cover with
a w
...