SIST EN ISO 21078-2:2008
(Main)Determination of boron(III) oxide in refractory products - Part 2: Acid extraction method for the determination of boron(III) oxide in binder components (ISO 21078-2:2006)
Determination of boron(III) oxide in refractory products - Part 2: Acid extraction method for the determination of boron(III) oxide in binder components (ISO 21078-2:2006)
This standard specifies methods of determining boron trioxide in oxidic raw materials for and constituents of ceramics, glass and glazes in concentrations of 0,01 % or greater. The samples are digested or determined analytically using one of three methods.
Bestimmung des Gehaltes an Bor(III)-oxid in feuerfesten Erzeugnissen — Teil 2: Säureextraktionsverfahren zur Bestimmung des Bor(III)-oxid-Gehaltes in Binderkomponenten (ISO 21078-2:2006)
Dosage de l'oxyde de bore(III) dans les produits réfractaires - Partie 2: Méthode d'extraction acide pour le dosage de l'oxyde de bore(III) dans les composants de liant (ISO 21078-2:2006)
L'ISO 21078-2:2006 spécifie des méthodes de dosage de l'oxyde de bore(III) contenu dans la phase liante des réfractaires aluminosilicates, utilisant une méthode d'extraction acide.
Elle est applicable pour les réfractaires contenant moins de 1 % (fraction massique) d'oxyde de bore(III).
Kemijska analiza borovega (III) oksida v ognjevzdržnih izdelkih - 2. del: Metoda kislinske ekstrakcije ugotavljanja borovega (III) oksida v vezivnih sestavinah (ISO 21078-2:2006)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 21078-2:2008
01-marec-2008
Kemijska analiza borovega (III) oksida v ognjevzdržnih izdelkih - 2. del: Metoda
kislinske ekstrakcije ugotavljanja borovega (III) oksida v vezivnih sestavinah (ISO
21078-2:2006)
Determination of boron(III) oxide in refractory products - Part 2: Acid extraction method
for the determination of boron(III) oxide in binder components (ISO 21078-2:2006)
Bestimmung des Gehaltes an Bor(III)-oxid in feuerfesten Erzeugnissen — Teil 2:
Säureextraktionsverfahren zur Bestimmung des Bor(III)-oxid-Gehaltes in
Binderkomponenten (ISO 21078-2:2006)
Dosage de l'oxyde de bore(III) dans les produits réfractaires - Partie 2: Méthode
d'extraction acide pour le dosage de l'oxyde de bore(III) dans les composants de liant
(ISO 21078-2:2006)
Ta slovenski standard je istoveten z: EN ISO 21078-2:2007
ICS:
81.080
SIST EN ISO 21078-2:2008 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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EUROPEAN STANDARD
EN ISO 21078-2
NORME EUROPÉENNE
EUROPÄISCHE NORM
October 2007
ICS 81.060.01; 81.040.01
English Version
Determination of boron(III) oxide in refractory products - Part 2:
Acid extraction method for the determination of boron(III) oxide
in binder components (ISO 21078-2:2006)
Dosage de l'oxyde de bore(III) dans les produits réfractaires Bestimmung des Gehaltes an Bor(III)-oxid in feuerfesten
- Partie 2: Méthode d'extraction acide pour le dosage de Erzeugnissen - Teil 2: Säureextraktionsverfahren zur
l'oxyde de bore(III) dans les composants de liant (ISO Bestimmung des Bor(III)-oxid-Gehaltes in
21078-2:2006) Binderkomponenten (ISO 21078-2:2006)
This European Standard was approved by CEN on 16 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 21078-2:2007: E
worldwide for CEN national Members.
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EN ISO 21078-2:2007 (E)
Foreword
The text of ISO 21078-2:2006 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 21078-2:2007 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 April 2008, and conflicting national
standards shall be withdrawn at the latest by April 2008.
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 21078-2:2006 has been approved by CEN as EN ISO 21078-2:2007 without any
modifications.
2
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INTERNATIONAL ISO
STANDARD 21078-2
First edition
2006-12-01
Determination of boron(III) oxide in
refractory products —
Part 2:
Acid extraction method for the
determination of boron(III) oxide in binder
components
Dosage de l'oxyde de bore(III) dans les produits réfractaires —
Partie 2: Méthode d'extraction acide pour le dosage de l'oxyde de
bore(III) dans les composants de liant
Reference number
ISO 21078-2:2006(E)
©
ISO 2006
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ISO 21078-2:2006(E)
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ISO 21078-2:2006(E)
Contents Page
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Preparation of the test sample . 1
5 Reagents . 2
6 Mass of test portion for extraction . 2
7 Preparation of the test solution . 2
8 Blank solution . 3
9 Classification of determination methods . 3
10 Determination of boron(III) oxide by sodium hydroxide titrimetry . 3
11 Determination of boron(III) oxide by inductived coupled plasma/atomic emission
spectrometry . 5
12 Curcumine absorption spectrophotometry (Rothocyanine method) . 6
13 Quality assurance and control . 9
14 Expression of test results . 9
15 Test report . 10
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ISO 21078-2:2006(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 21078-2 was prepared by Technical Committee ISO/TC 33, Refractories.
ISO 21078 consists of the following parts, under the general title Determination of boron(III) oxide in refractory
products:
— Part 1: Determination of total boric oxide in oxidic materials for ceramics, glass and glazes
— Part 2: Acid extraction method for the determination of boron(III) oxide in binder components
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INTERNATIONAL STANDARD ISO 21078-2:2006(E)
Determination of boron(III) oxide in refractory products —
Part 2:
Acid extraction method for the determination of boron(III) oxide
in binder components
1Scope
This part of ISO 21078 specifies procedures of chemical analysis for the determination of boron(III) oxide used
as a binder component added to aluminosilicate refractories, using an acid extraction method.
1%
It is applicable for refractories containing less than (mass fraction) of boron(III) oxide.
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 31-0, Quantities and units — Part 0: General principles
ISO 836, Terminology for refractories
ISO 3310-1, Test sieves — Technical requirements and testing — Part 1: Test sieves of metal wire cloth
ISO 3696, Water for analytical laboratory use — Specification and test methods
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 836 and the following apply.
3.1
dry unshaped refractories
dry particles and/or powder of unshaped refractories
4 Preparation of the test sample
4.1 Refractory brick or its raw material
Sampling is carried out in accordance with the contract between the user and producer. A specified quantity
taken from a lot of the sample is crushed to pass through a 6,7 mm sieve (see ISO 3310-1) and reduced to
about 100 g by riffling or quartering. Then all the reduced sample is ground to pass through a 300µm sieve
(see ISO 3310-1).
4.2 Unshaped refractories
Prepare two approximately 100 g portions of the sample for analysis (both dry and wet), and crush to pass
through a 300µm sieve (see ISO 3310-1), in accordance with the following procedure in 4.3 to 4.5.
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ISO 21078-2:2006(E)
4.3 Dry unshaped refractories
Take one bag or 50 kg of the sample from a lot and reduce to about 100 g as above, and crush to pass through
a 300µmsieve.
4.4 Laboratory sample
The laboratory sample from 4.1 or 4.2 is reduced to approximately 25 g by quartering, and ground to pass
through a 106µm sieve. This is the test sample for analysis. It is transferred into a container [e.g. a flat weighing
bottle (50 mm× 30 mm) or sample tube (50 mm× 25 mm)], and dried in a desiccator with silica gel desiccant
for a minimum of 8h.
4.5 Weighing of test portion
The specified quantity of the test portion for chemical analysis shall be weighed to the nearest 0,1 mg using an
analytical balance and recorded.
Carry out the extraction process in duplicate.
5Reagents
Use only reagents of known analytical purity and water conforming to the requirements of grade 2 of ISO 3696
(e.g. double-distilled water).
The boron and borate ion concentrations in the water and the reagents shall be negligible compared with the
lowest concentration to be determined. All solutions are aqueous unless otherwise specified.
NOTE The reagents below are for the extraction process only. Reagents for the determination of B O are listed in the
2 3
appropriate clauses.
5.1 Dilute hydrochloric acid (1 + 1).
Add 1 volume of hydrochloric acid (concentrated, 35 % by mass) to 1 volume of water, then mix and allow to
cool.
5.2 Dilute hydrochloric acid (1 + 50).
Add 1 volume of hydrochloric acid (concentrated, 35 % by mass) to 50 volumes of water.
6 Mass of test portion for extraction
Weigh out 5,0 g of the test sample.
7 Preparation of the test solution
Weigh and transfer the dry sample into a 200 ml plastics beaker. Using a measuring cylinder, add 20 ml of
hydrochloric acid solution (1 + 1) (5.1) and 50 ml of warm water, and mix intimately. Allow to stand for
approximately 30 min± 2 min while stirring, to dissolve the soluble binder components.
Filter with a fine-textured filter paper and wash with warm dilute hydrochloric acid (1 + 50) (5.2). Transfer the
filtrate and washings into a 250 ml volumetric flask, and dilute to the mark with water. Transfer into a plastics
bottle. This solution is referred to as the “test solution” for the determination of boron(III) oxide.
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ISO 21078-2:2006(E)
8 Blank solution
Carry out the procedure given in Clause 7 without the sample. This solution is referred to as the “blank solution”.
9 Classification of determination methods
The determination of boron(III) oxide is carried out using one of the following three methods.
a) Sodium hydroxide titrimetry.
NOTE This method is applied to the sample containing more than (mass fraction) of boron(III) oxide.
0,5 %
b) Inductively coupled plasma atomic emission spectrometry (ICP/AES).
c) Curcumin absorption spectrophotometry (Rothocyanine method).
10 Determination of boron(III) oxide by sodium hydroxide titrimetry
10.1 Principle
A specified volume of test solution is taken and adjusted to pH approximately 5,0. The precipitate containing
silicic acid is filtered off. The filtrate's pH is adjusted to 6,3 and D(–)-mannitol is added to the filtrate. Then, the
+
H ions liberated by the mannitol in the solution are titrated with the sodium hydroxide standard solution until the
solution's pH becomes 6,3 again.
10.2 Reagents
10.2.1 Dilute hydrochloric acid.
Prepare dilute hydrochloric acid (1 + 50) as described in 5.2.
10.2.2 D(–)-Mannitol (C H O ).
6 14 6
10.2.3 Bromocresol purple (C H Br O S) solution, .1 g/l
21 16 2 5
Dissolve 0,1 g of bromocresol purple in water and dilute to approximately 100 ml. Keep this solution in the dark
at a low temperature for a maximum of 7 days.
10.2.4 Boron(III) oxide standard solution, 0,1 mgB O /ml.
2 3
Transfer approximately 0,5 g of boric acid into a 100 ml beaker, spread it as a thin layer and dry for 24 h in a
desiccator with silica gel desiccant. Weigh 0,177 6 g of this dry boric acid and transfer into a 200 ml plastics
beaker. Dissolve in approximately 100 ml of water and dilute precisely to 1 000 ml in a volumetric flask.
10.2.5 Sodium hydroxide standard volumetric solution.
Transfer 50 g of sodium hydroxide into a polyethylene bottle, add 50 ml of water, dissolve while cooling, and put
a seal on it. Keep the sealed bottle for several days, pipette 4,0 ml of the supernatant fraction, and dilute to
2 000 ml in a volumetric flask. Transfer this solution into a polyethylene bottle, using a 25 ml au
...
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