SIST EN ISO 21079-1:2008
(Main)Chemical analysis of refractories containing alumina, zirconia and silica - Refractories containing 5 percent to 45 percent of ZrO2 (alternative to the X-ray fluorescence method) - Part 1: Apparatus, reagents and dissolution (ISO 21079-1:2008)
Chemical analysis of refractories containing alumina, zirconia and silica - Refractories containing 5 percent to 45 percent of ZrO2 (alternative to the X-ray fluorescence method) - Part 1: Apparatus, reagents and dissolution (ISO 21079-1:2008)
This set of standards will give methods for the chemical analysis of AZS (alumina, zirconia, and silica) refractory products and raw materials, using traditional ("wet") methods, ICP-AE spectrometry and FAA spectrometry. It covers apparatus, reagents and dissolution methods.
Chemische Analyse von aluminiumoxid-, zirkoniumoxid- und silicium(IV)-oxidhaltigen feuerfesten Erzeugnissen - Feuerfeste Erzeugnisse mit einem Massenanteil an ZrO2 von 5% bis 45% (Alternative zum Röntgenfluoreszenzverfahren) - Teil 1: Geräte, Reagenzien und Aufschluss (ISO 21079-1:2008)
Dieser Teil von ISO 21079 legt chemische Analysenverfahren für feuerfeste Erzeugnisse und Rohstoffe (mit 5 % bis 45 % ZrO2) fest, die AZS (Aluminiumoxid, Zirkoniumoxid und Silicium(IV) oxid) enthalten, indem traditionelle (nasschemische) Verfahren, Atomemissionsspektrometrie (ICP AES) und Flammenatom¬absorptionsspektrometrie (FAAS) angewendet werden. Er legt die Geräte, Reagenzien und Aufschlussverfahren fest.
Der jeweilige Bestimmungsbereich ist in Tabelle 1 angegeben.
Tabelle 1 — Bestimmungsbereich
Bestandteil Bereich
Massenanteil in % Bestandteil Bereich
Massenanteil in %
LOI –1 bis 40 MgO 0,01 bis 2
SiO2 0,1 bis 45 Na2O 0,01 bis 3
Al2O3 1 bis 80 K2O 0,01 bis 1
Fe2O3 0,01 bis 2 Cr2O3 0,01 bis 3
TiO2 0,01 bis 5 ZrO2 5 bis 45
CaO 0,01 bis 2 HfO2 0,01 bis 2
ANMERKUNG Die angegebenen Werte sind, außer denen für LOI, bezogen auf den Zustand nach der Bestimmung des Glühverlustes.
Dieser Teil von ISO 21079 gilt nicht für feuerfeste Erzeugnisse, die auf MgO basieren.
ANMERKUNG Dieser Teil von ISO 21079 stellt eine Alternative zum Röntgenfluoreszenzverfahren (RFA) nach ISO 12677 dar.
Analyse chimique des matériaux réfractaires contenant de l'alumine, de la zircone et de la silice - Matériaux réfractaires contenant de 5 % à 45 % de ZrO2 (méthode alternative à la méthode par fluorescence de rayons X) - Partie 1: Appareillage, réactifs et dissolution (ISO21079-1:2008)
L'ISO 21079:2008 spécifie des méthodes d'analyse chimique des matières premières et produits réfractaires AZS (alumine, zircone et silice), contenant de 5 % à 45 % de ZrO2 (zircone) à l'aide des méthodes classiques («par voie humide»), par spectrométrie d'émission atomique avec plasma induit par haute fréquence (ICP-AES) et par spectrophotométrie d'absorption atomique dans la flamme (FAAS). Elle fournit des méthodes alternatives à la méthode d'analyse par fluorescence de rayons X, spécifiée dans l'ISO 12677.
L'ISO 21079‑1:2008 spécifie l'appareillage, les réactifs et les méthodes de dissolution utilisés.
Elle n'est pas applicable aux matériaux réfractaires à base de MgO.
Kemijska analiza ognjevzdržnih izdelkov, ki vsebujejo aluminijev oksid, cirkonijev oksid in silicijev oksid - Ognevzdržni izdelki vsebujejo 5 % do 45 % ZrO2 (alternativa rentgenski fluorescenčni metodi) - 1. del: Aparati, reagenti in raztapljanje (ISO 21079-1:2008)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 21079-1:2008
01-september-2008
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DOWHUQDWLYDUHQWJHQVNLIOXRUHVFHQþQLPHWRGL GHO $SDUDWLUHDJHQWLLQ
UD]WDSOMDQMH ,62
Chemical analysis of refractories containing alumina, zirconia and silica - Refractories
containing 5 percent to 45 percent of ZrO2 (alternative to the X-ray fluorescence method)
- Part 1: Apparatus, reagents and dissolution (ISO 21079-1:2008)
Chemische Analyse von aluminiumoxid-, zirkoniumoxid- und silicium(IV)-oxidhaltigen
feuerfesten Erzeugnissen - Feuerfeste Erzeugnisse mit einem Massenanteil an ZrO2 von
5% bis 45% (Alternative zum Röntgenfluoreszenzverfahren) - Teil 1: Geräte, Reagenzien
und Aufschluss (ISO 21079-1:2008)
Analyse chimique des matériaux réfractaires contenant de l'alumine, de la zircone et de
la silice - Matériaux réfractaires contenant de 5 % à 45 % de ZrO2 (méthode alternative
à la méthode par fluorescence de rayons X) - Partie 1: Appareillage, réactifs et
dissolution (ISO21079-1:2008)
Ta slovenski standard je istoveten z: EN ISO 21079-1:2008
ICS:
71.040.40 Kemijska analiza Chemical analysis
81.080 Ognjevzdržni materiali Refractories
SIST EN ISO 21079-1:2008 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 21079-1:2008
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SIST EN ISO 21079-1:2008
EUROPEAN STANDARD
EN ISO 21079-1
NORME EUROPÉENNE
EUROPÄISCHE NORM
April 2008
ICS 81.080; 71.040.40
English Version
Chemical analysis of refractories containing alumina, zirconia
and silica - Refractories containing 5 percent to 45 percent of
ZrO2 (alternative to the X-ray fluorescence method) - Part 1:
Apparatus, reagents and dissolution (ISO 21079-1:2008)
Analyse chimique des matériaux réfractaires contenant de Chemische Analyse von aluminiumoxid-, zirkoniumoxid-
l'alumine, de la zircone et de la silice - Matériaux und silicium(IV)-oxidhaltigen feuerfesten Erzeugnissen -
réfractaires contenant de 5 % à 45 % de ZrO2 (méthode Feuerfeste Erzeugnisse mit einem Massenanteil an ZrO2
alternative à la méthode par fluorescence de rayons X) - von 5% bis 45% (Alternative zum
Partie 1: Appareillage, réactifs et dissolution (ISO 21079- Röntgenfluoreszenzverfahren) - Teil 1: Geräte, Reagenzien
1:2008) und Aufschluss (ISO 21079-1:2008)
This European Standard was approved by CEN on 12 April 2008.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the CEN Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the
official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
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EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2008 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 21079-1:2008: E
worldwide for CEN national Members.
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SIST EN ISO 21079-1:2008
EN ISO 21079-1:2008 (E)
Contents Page
Foreword.3
2
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SIST EN ISO 21079-1:2008
EN ISO 21079-1:2008 (E)
Foreword
This document (EN ISO 21079-1:2008) 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 October 2008, and conflicting national standards shall be withdrawn at
the latest by October 2008.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech
Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.
Endorsement notice
The text of ISO 21079-1:2008 has been approved by CEN as a EN ISO 21079-1:2008 without any
modification.
3
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SIST EN ISO 21079-1:2008
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SIST EN ISO 21079-1:2008
INTERNATIONAL ISO
STANDARD 21079-1
First edition
2008-04-15
Chemical analysis of refractories
containing alumina, zirconia and silica —
Refractories containing 5 % to 45 %
of ZrO (alternative to the X-ray
2
fluorescence method) —
Part 1:
Apparatus, reagents and dissolution
Analyse chimique des matériaux réfractaires contenant de l'alumine,
de la zircone et de la silice — Matériaux réfractaires contenant de 5 %
à 45 % de ZrO (méthode alternative à la méthode par fluorescence de
2
rayons X) —
Partie 1: Appareillage, réactifs et dissolution
Reference number
ISO 21079-1:2008(E)
©
ISO 2008
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SIST EN ISO 21079-1:2008
ISO 21079-1:2008(E)
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ii © ISO 2008 – All rights reserved
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SIST EN ISO 21079-1:2008
ISO 21079-1:2008(E)
Contents Page
Foreword. iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions. 2
4 Apparatus . 2
5 Reagents. 2
5.1 General. 2
5.2 Standard solutions specific to ISO 21079 . 2
6 Sampling. 4
7 General procedures. 5
8 Determination of loss on ignition. 5
9 Decomposition of the sample and preparation of solutions used in the analysis . 5
9.1 General decomposition techniques. 5
9.2 Dissolution methods by fusion . 5
9.3 Dissolution methods by hydrofluoric acid attack . 8
10 Expression of test results. 10
11 Examination and adoption of test results .10
12 Test report . 11
Annex A (informative) References for stock solutions and blank solutions in this part of
ISO 21079. 12
Bibliography . 13
© ISO 2008 – All rights reserved iii
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SIST EN ISO 21079-1:2008
ISO 21079-1:2008(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 21079-1 was prepared by Technical Committee ISO/TC 33, Refractories.
ISO 21079 consists of the following parts, under the general title Chemical analysis of refractories containing
alumina, zirconia and silica — Refractories containing 5 % to 45 % of ZrO (alternative to the X-ray
2
fluorescence method):
⎯ Part 1: Apparatus, reagents and dissolution
⎯ Part 2: Wet chemical analysis
⎯ Part 3: Flame atomic absorption spectrophotometry (FAAS) and inductively coupled plasma emission
spectrometry (ICP-AES)
iv © ISO 2008 – All rights reserved
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SIST EN ISO 21079-1:2008
INTERNATIONAL STANDARD ISO 21079-1:2008(E)
Chemical analysis of refractories containing alumina, zirconia
and silica — Refractories containing 5 % to 45 % of ZrO
2
(alternative to the X-ray fluorescence method) —
Part 1:
Apparatus, reagents and dissolution
1 Scope
This part of ISO 21079 specifies methods for the chemical analysis of AZS (alumina, zirconia, and silica)
refractory products (containing 5 % to 45 % of ZrO ) and raw materials, using traditional (“wet”) methods,
2
inductively coupled plasma atomic emission (ICP-AE) spectrometry and flame atomic absorption (FAA)
spectrometry. It covers apparatus, reagents and dissolution methods.
The range of determination is given in Table 1.
Table 1 — Range of determination (% by mass)
Component Range Component Range
LOI –1 to 40 MgO 0,01 to 2
SiO 0,1 to 45 Na O 0,01 to 3
2 2
Al O 1 to 80 K O 0,01 to 1
2 3 2
Fe O 0,01 to 2 Cr O 0,01 to 3
2 3 2 3
TiO 0,01 to 5 ZrO 5 to 45
2 2
CaO 0,01 to 2 HfO 0,01 to 2
2
NOTE The values other than LOI are on an ignited basis.
This part of ISO 21079 is not applicable to MgO-based refractories.
NOTE This part of ISO 21079 gives alternatives to the X-ray fluorescence (XRF) method given in ISO 12677.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 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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SIST EN ISO 21079-1:2008
ISO 21079-1:2008(E)
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 26845 apply.
4 Apparatus
Ordinary laboratory apparatus and the apparatus given in ISO 26845.
5 Reagents
5.1 General
Prepare the following reagents, and those given in ISO 26845, as necessary.
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only
distilled water or water of equivalent purity.
Reagents should conform to the requirements of ISO 6353-1, ISO 6353-2 and ISO 6353-3, as appropriate.
5.2 Standard solutions specific to ISO 21079
Traceable standard solutions may be used in place of the following.
5.2.1 Aluminium oxide standard solution, Al O 1 mg/ml.
2 3
Wash the surface of a sufficient amount of aluminium metal (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 into a 250 ml beaker. Cover
with a watch glass, add 20 ml of hydrochloric acid (1+1), and heat to dissolve. After cooling, dilute to 1 000 ml
in a volumetric flask with water.
5.2.2 Calcium oxide standard solution, CaO 1 mg/ml.
Dissolve 1,785 g of pure calcium carbonate, previously dried at 150 °C, in a slight excess of dilute
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 in a volumetric flask.
5.2.3 Chromium(III) oxide standard solution, Cr O 1 mg/ml.
2 3
Dry about 2 g to 3 g of potassium dichromate, K Cr O , at 110 °C. for at least 2 h. Weigh 1,935 g of this and
7
2 2
dissolve in water, diluting to 1 000 ml in a volumetric flask.
5.2.4 Diluted chromium(III) oxide standard solution, Cr O 0,025 mg/ml.
2 3
Dilute 25 ml of the chromium(III) oxide standard solution (1 mg/ml), to 1 000 ml in a volumetric flask. Prepare
this solution freshly when required.
5.2.5 CyDTA (trans-1,2-cyclohexanediamine-N,N,N',N'-tetraacetic acid monohydrate) standard
solution, 0,02 mol/l.
Add 16 ml of sodium hydroxide solution (100 g/l) and 150 ml of water to 7,30 g of CyDTA, and dissolve by
heating. After cooling, dilute to 1 000 ml with water.
2 © ISO 2008 – All rights reserved
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SIST EN ISO 21079-1:2008
ISO 21079-1:2008(E)
5.2.6 EDTA standard solution, 5 g/l.
Dissolve 5 g of EDTANa (ethylenediamine-tetraacetic acid disodium salt, dihydrate) in water and dilute to
2
1 000 ml in a volumetric flask. Store in a plastics bottle.
Standardize against calcium as follows.
Pipette 25 ml of standard calcium solution (1 mg/ml) into a 500 ml conical flask, add 10 ml of potassium
hydroxide solution, and dilute to about 200 ml. Add about 0,015 g of screened calcein indicator and titrate with
the EDTA solution (5 g/l), from a fluorescent green colour to pink.
Standardize against magnesium as follows.
Pipette 25 ml of standard magnesium solution (1 mg/ml), into a 500 ml conical flask. Add 20 drops of
hydrochloric acid (concentrated) and 20 ml of ammonia solution (concentrated), and dilute to about 200 ml.
Add about 0,04 g of methylthymol blue complexone indicator and titrate with the EDTA solution (5 g/l).
5.2.7 Hafnium oxide standard solution, HfO 1 mg/ml.
2
Transfer 1,5 g of hafnium oxide (of a purity more than 99,9 % by mass) into a 20 ml platinum crucible, ignite at
1 050 °C ± 25 °C for 1 h and cool in a desiccator. Weigh 0,500 0 g of the ignited residue into a 75 ml platinum
crucible. After adding 3,0 g of anhydrous sodium carbonate, add 2,0 g of boric acid and mix.Then carry out
melting at 1 050 ± 25 °C in an electric muffle furnace. After cooling, add 55 ml of sulfuric acid (1+9) and heat
until dissolved on a steam bath. After cooling, dilute to 500 ml in a flask with water.
5.2.8 Iron(III) oxide standard solution, Fe O 1mg/ml.
2 3
Wash the surface of a sufficient amount of iron metal (purity greater than 99,9 %) with hydrochloric acid (1+4).
Then dissolve the oxidized layer, and wash with water, ethanol and diethyl ether in succession. Then dry in a
desiccator. Weigh 0,699 4 g of this, transfer to a beaker (200 ml), and cover with a watch glass. Add 30 ml of
hydrochloric acid (1+1), and heat on a steam bath until dissolved. After cooling, dilute to 1 000 ml in a
volumetric flask with water.
5.2.9 Diluted iron(III) oxide standard solution, Fe O 0,04 mg/ml.
2 3
Transfer 40 ml of the iron(III) oxide (1 mg/ml) standard solution to a 1 000 ml volumetric flask and dilute to the
mark with water. Prepare this solution freshly as required.
5.2.10 Magnesium oxide standard solution, MgO 1 mg/ml.
Wash the surface of a sufficient amount of magnesium metal (purity, more than 99,9 % by mass) with
hydrochloric acid (1+1) to dissolve the oxidized layer. Then 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 10 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.
5.2.11 Potassium oxide standard solution, K O 1 mg/ml.
2
Transfer 1 g to 1,5 g of potassium chloride into a platinum crucible (e.g. 30 ml) and ignite at 600 °C ± 25 °C for
approximately 60 min. Allow the crucible and contents to cool in a desiccator. Weigh 0,791 4 g of this and
transfer to a 200 ml beaker. Dissolve in 100 ml of water, transfer to a 500 ml volumetric flask, and dilute to the
mark with water.
© ISO 2008 – All rights reserved 3
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SIST EN ISO 21079-1:2008
ISO 21079-1:2008(E)
5.2.12 Silicon(IV) oxide standard solution, SiO 1 mg/ml.
2
Weigh 0,7 g to 1,0 g of silicon(IV) oxide (purity, greater that 99,9 % by mass) in a platinum crucible (e.g.
30 ml) and heat for 30 min at 1 150 °C ± 50 °C. Cool in a desiccator and then weigh 0,500 0 g of this
silicon(IV) oxide into a platinum crucible (e.g. 30 ml). Fuse the silicon(IV) oxide with 3,0 g of anhydrous
sodium carbonate. Cool and wipe the outside of the crucible, and dissolve in warm water (150 ml) in a plastics
200 ml beaker while stirring using a plastic rod. Cool and dilute without heating to 500 ml in a volumetric flask.
Transfer this solution to a plastic bottle immediately.
5.2.13 Diluted silicon(IV) oxide standard solution, SiO 0,04 mg/ml.
2
Dilute 10 ml of silicon(IV) oxide standard solution (1,0 mg/ml) to 250 ml with water.
5.2.14 Sodium oxide standard solution, Na O 1 mg/ml.
2
Transfer 1 to 1,5 g of sodium chloride into a platinum crucible (e.g. 30 ml) and ignite at 600 °C ± 25 °C for
approximately 60 min. Allow the crucible and contents to cool in a desiccator. Weigh 0,942 9 g of this and
transfer to a 200 ml beaker. Dissol
...
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