SIST EN ISO 21068-2:2008
(Main)Chemical analysis of silicon-carbide-containing raw materials and refractory products - Part 2: Determination of loss on ignition, total carbon, free carbon and silicon carbide, total and free silica and total and free silicon (ISO 21068-2:2008)
Chemical analysis of silicon-carbide-containing raw materials and refractory products - Part 2: Determination of loss on ignition, total carbon, free carbon and silicon carbide, total and free silica and total and free silicon (ISO 21068-2:2008)
This part of ISO 21068 specifies analytical techniques for the determination of change in mass by thermal treatment at specified temperatures, and methods for the determination of the total carbon content, free carbon, silicon carbide, silicon, total silica and free silica content of silicon-carbide-containing raw materials and refractory products.
Chemische Analyse von Siliciumcarbid enthaltenden Rohstoffen und feuerfesten Erzeugnissen - Teil 2: Bestimmung des Glühverlustes und Gehaltes an Gesamtkohlenstoff, freiem Kohlenstoff und Siliciumcarbid, des Gehaltes an gesamtem und freiem Silicium(IV)-oxid sowie an gesamtem und freiem Silicium (ISO 21068-2:2008)
Dieser Teil von ISO 21068 legt die Analysenverfahren für die Bestimmung der Massenänderung durch Wärmebehandlung bei festgelegten Temperaturen sowie Verfahren für die Bestimmung des Gehaltes an Gesamtkohlenstoff, freiem Kohlenstoff und Siliciumcarbid, des Gehaltes an gesamtem und freiem Silicium(IV)-oxid sowie an gesamtem und freiem Silicium von Siliciumcarbid enthaltenden Rohstoffen und feuerfesten Erzeugnissen fest.
Analyse chimique des matières premières et des produits réfractaires contenant du carbure de silicium - Partie 2: Détermination de la perte au feu, du carbone total, du carbone libre et du carbure de silicium, de la silice totale et libre, et du silicium total et libre (ISO 21068-2:2008)
L'ISO 21068-2:2008 spécifie des techniques d'analyse permettant de déterminer la variation de masse apportée par un traitement thermique à des températures spécifiées ainsi que des méthodes permettant de déterminer la teneur totale en carbone, ainsi que la teneur en carbone libre, carbure de silicium, silicium, silice totale et en silice libre de carbure de calcium contenant des matières premières et des produits réfractaires.
Kemijska analiza surovin in ognjevzdržnih izdelkov s silicijevim karbidom - 2. del: Določevanje ostanka po žarenju, celokupnega ogljika, prostega ogljika in silicijevega karbida, celokupne in proste silike in celokupnega in prostega silicija (ISO 21068-2:2008)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 21068-2:2008
01-december-2008
.HPLMVNDDQDOL]DVXURYLQLQRJQMHY]GUåQLKL]GHONRYVVLOLFLMHYLPNDUELGRPGHO
'RORþHYDQMHRVWDQNDSRåDUHQMXFHORNXSQHJDRJOMLNDSURVWHJDRJOMLNDLQ
VLOLFLMHYHJDNDUELGDFHORNXSQHLQSURVWHVLOLNHLQFHORNXSQHJDLQSURVWHJDVLOLFLMD
,62
Chemical analysis of silicon-carbide-containing raw materials and refractory products -
Part 2: Determination of loss on ignition, total carbon, free carbon and silicon carbide,
total and free silica and total and free silicon (ISO 21068-2:2008)
Chemische Analyse von Siliciumcarbid enthaltenden Rohstoffen und feuerfesten
Erzeugnissen - Teil 2: Bestimmung des Glühverlustes und Gehaltes an
Gesamtkohlenstoff, freiem Kohlenstoff und Siliciumcarbid, des Gehaltes an gesamtem
und freiem Silicium(IV)-oxid sowie an gesamtem und freiem Silicium (ISO 21068-2:2008)
Analyse chimique des matières premières et des produits réfractaires contenant du
carbure de silicium - Partie 2: Détermination de la perte au feu, du carbone total, du
carbone libre et du carbure de silicium, de la silice totale et libre, et du silicium total et
libre (ISO 21068-2:2008)
Ta slovenski standard je istoveten z: EN ISO 21068-2:2008
ICS:
81.080 Ognjevzdržni materiali Refractories
SIST EN ISO 21068-2:2008 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 21068-2:2008
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SIST EN ISO 21068-2:2008
EUROPEAN STANDARD
EN ISO 21068-2
NORME EUROPÉENNE
EUROPÄISCHE NORM
August 2008
ICS 81.080
English Version
Chemical analysis of silicon-carbide-containing raw materials
and refractory products - Part 2: Determination of loss on
ignition, total carbon, free carbon and silicon carbide, total and
free silica and total and free silicon (ISO 21068-2:2008)
Analyse chimique des matières premières et des produits Chemische Analyse von Siliciumcarbid enthaltenden
réfractaires contenant du carbure de silicium - Partie 2: Rohstoffen und feuerfesten Erzeugnissen - Teil 2:
Détermination de la perte au feu, du carbone total, du Bestimmung des Glühverlustes und Gehaltes an
carbone libre et du carbure de silicium, de la silice totale et Gesamtkohlenstoff, freiem Kohlenstoff und Siliciumcarbid,
libre, et du silicium total et libre (ISO 21068-2:2008) des Gehaltes an gesamtem und freiem Silicium(IV)-oxid
sowie an gesamtem und freiem Silicium (ISO 21068-
2:2008)
This European Standard was approved by CEN on 11 July 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 21068-2:2008: E
worldwide for CEN national Members.
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SIST EN ISO 21068-2:2008
EN ISO 21068-2:2008 (E)
Contents Page
Foreword.3
2
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SIST EN ISO 21068-2:2008
EN ISO 21068-2:2008 (E)
Foreword
This document (EN ISO 21068-2:2008) 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 February 2009, and conflicting national standards shall be withdrawn
at the latest by February 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.
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 21068-2:2008 has been approved by CEN as a EN ISO 21068-2:2008 without any
modification.
3
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SIST EN ISO 21068-2:2008
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SIST EN ISO 21068-2:2008
INTERNATIONAL ISO
STANDARD 21068-2
First edition
2008-08-01
Chemical analysis of silicon-carbide-
containing raw materials and refractory
products —
Part 2:
Determination of loss on ignition, total
carbon, free carbon and silicon carbide,
total and free silica and total and free
silicon
Analyse chimique des matières premières et des produits réfractaires
contenant du carbure de silicium —
Partie 2: Détermination de la perte au feu, du carbone total, du carbone
libre et du carbure de silicium, de la silice totale et libre, et du silicium
total et libre
Reference number
ISO 21068-2:2008(E)
©
ISO 2008
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SIST EN ISO 21068-2:2008
ISO 21068-2:2008(E)
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ii © ISO 2008 – All rights reserved
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SIST EN ISO 21068-2:2008
ISO 21068-2:2008(E)
Contents Page
Foreword .v
Introduction.vi
1 Scope.1
2 Normative references.1
3 Terms and definitions .1
4 Determination of change in mass.2
4.1 General .2
4.2 Determination of the loss on drying at 250 °C (LOD ) gravimetric method.2
250
4.3 Determination of the loss on calcination in argon (LOI ) .3
Ar
4.4 Determination of the change in mass by heat pretreatment in air.5
4.5 Determination of the change in mass at 750 °C (LOI ).6
750
4.6 Determination of loss on ignition at 850 °C (LOI ).7
850
4.7 Determination of loss on ignition at 1 050 °C (LOI ) .7
1 050
5 Determination of the total carbon content.8
5.1 General .8
5.2 Combustion techniques.9
5.3 Detection techniques .12
5.4 Detection methods .17
6 Determination of free carbon content .24
6.1 General .24
6.2 Sample decomposition by combustion .24
6.3 Detection techniques .24
6.4 Direct detection methods .24
6.5 Indirect detection methods.29
6.6 Direct determination of free carbon by wet oxidation.33
7 Determination of silicon carbide content, SiC.33
7.1 General .33
7.2 Determination of silicon carbide, SiC, by indirect quantitative method.34
7.3 Determination of silicon carbide, SiC, by direct quantitative method .34
7.4 Determination of silicon carbide SiC by ignition method at 750 °C.35
7.5 Determination of silicon carbide, SiC, by chemical method.36
8 Determination of total silicon content via silica.38
8.1 Principle.38
8.2 Reagents.38
8.3 Apparatus.38
8.4 Procedure.39
8.5 Blank test.39
8.6 Calculation .40
9 Determination of free silicon content.40
9.1 Principle.40
9.2 Pretreatment with hydrochloric acid .40
9.3 Silicon determination by hydrogen evolution .40
9.4 Silicon determination by silver displacement .43
10 Determination of silica content, SiO .45
2
10.1 General .45
10.2 Determination of free and/or combined silica content, SiO .45
2
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SIST EN ISO 21068-2:2008
ISO 21068-2:2008(E)
10.3 Determination of free silica, SiO .46
2
10.4 Determination of surface silicon dioxide, SiO .46
2
11 Expression of results .46
12 Test report .46
Annex A (informative) Examples of CRMs for calibration of carbon analyser .47
Bibliography .48
iv © ISO 2008 – All rights reserved
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SIST EN ISO 21068-2:2008
ISO 21068-2:2008(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 21068-2 was prepared by Technical Committee ISO/TC 33, Refractories.
ISO 21068 consists of the following parts, under the general title Chemical analysis of silicon-carbide-
containing raw materials and refractory products:
⎯ Part 1: General information and sample preparation
⎯ Part 2: Determination of loss on ignition, total carbon, free carbon and silicon carbide, total and free silica
and total and free silicon
⎯ Part 3: Determination of nitrogen, oxygen and metallic and oxidic constituents
© ISO 2008 – All rights reserved v
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SIST EN ISO 21068-2:2008
ISO 21068-2:2008(E)
Introduction
[6]
ISO 21068, Parts 1 to 3, have been developed from the combination of a Japanese standard JIS 2011 and
work items originally developed within CEN. Because there is a wide variety of laboratory equipment in use,
the most commonly used methods are described.
[2] to [5]
This part of ISO 21068 is applicable to the analysis of all refractory products classified in ISO 10081
[1]
(shaped) and ISO 1927 (unshaped) and raw materials containing carbon and/or silicon carbide. Therefore,
this part of ISO 21068 covers the full range of analysis from pure silicon carbide to oxidic refractory
composition with a low content of silicon carbide and/or nitrides. Primarily, this part of ISO 21068 provides
methods to distinguish between different carbon-bound types like total carbon (C ) and free carbon (C )
total free
and derives from these two the silicon carbide content.
If free carbon is present, this part of ISO 21068 includes different types of temperature treatment, in order to
determine the mass changes gravimetrically. Frequently, the resulting residue is used for other determinations.
The determination of other groups of analytes described in this part of ISO 21068 are free metals, free silicon
(Si ), free aluminum (Al ), free magnesium (Mg ), free iron (Fe ) and the group of oxides from main to
free free free free
trace components.
This part of ISO 21068 also describes the chemical analysis of SiO , total Si, oxygen and nitrogen and other
2
oxidic-bound metals which typically occur in the materials.
This part of ISO 21068 represents a listing of analytical methods which is approximately structured according
to material composition. However, it is still the user who should prove the applicability of the method,
depending on the material and analytical requirements.
vi © ISO 2008 – All rights reserved
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SIST EN ISO 21068-2:2008
INTERNATIONAL STANDARD ISO 21068-2:2008(E)
Chemical analysis of silicon-carbide-containing raw materials
and refractory products —
Part 2:
Determination of loss on ignition, total carbon, free carbon and
silicon carbide, total and free silica and total and free silicon
1 Scope
This part of ISO 21068 specifies analytical techniques for the determination of change in mass by thermal
treatment at specified temperatures, and methods for the determination of the total carbon content, free
carbon, silicon carbide, silicon, total silica and free silica content of silicon-carbide-containing raw materials
and refractory products.
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 5725-2, Accuracy (trueness and precision) of measurement methods and results — Part 2: Basic method
for the determination of repeatability and reproducibility of a standard measurement method
ISO 9286:1997, Abrasive grains and crude — Chemical analysis of silicon carbide
ISO 10060, Dense, shaped refractory products — Test methods for products containing carbon
ISO 21068-1:2008, Chemical analysis of silicon-carbide-containing raw materials and refractory products —
Part 1: General information and sample preparation
EN 12698-1:2007, Chemical analysis of nitride bonded silicon carbide refractories — Part 1: Chemical
methods
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 21068-1 apply.
© ISO 2008 – All rights reserved 1
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SIST EN ISO 21068-2:2008
ISO 21068-2:2008(E)
4 Determination of change in mass
4.1 General
The determination of change in mass is defined as a loss or increase in mass caused by heat treatment.
Several methods are distinguished based on the sample material, temperature and atmosphere. The
determination of change in mass is carried out by a gravimetric method. Heat treatments in air will lead to a
loss of volatile matter and carbon and an increase of mass due to oxidation, whereas a heat treatment in
argon will only lead to a loss of volatile matter.
Normally, the residue is used for other determinations. Therefore, the change in mass is considered for the
calculation of the analytical result. The analytical method which is applied to the residue depends on the
matrix and the parameters to be determined. It is up to the user to select the appropriate analytical method.
Table 1 gives an overview of methods of determination of change in mass by heat pretreatments and their
different applications.
Table 1 — Methods and application purpose of determination of change in mass
Short title of method Temperature Subclause Application
Attached water and chemically combined water are
Loss on drying (LOD) 250 °C 4.2
250
removed, e.g. in clay containing plastic formulations
Loss on calcination in argon All volatile compounds out of pitch- or resin-bonded
750 °C 4.3
(LOI ) formulations are removed
Ar
Volatile compounds are removed from resin-bonded
200 °C 4.4
formulations
Change in mass in air
Volatile compounds are removed from pitch-bonded
400 °C 4.4
formulations
Change in mass (LOI) 750 °C 4.5 Both procedures are suitable to remove carbon (e.g.
750
graphite) from refractory formulations. If fine-grained
SiC is present, care should be taken because SiC may
Loss on ignition (LOI) 850 °C 4.6
850
be oxidised as well.
Loss or gain of mass; attached water, chemically
Loss on ignition (LOI ) 1 050 °C 4.7 combined water, carbon, organic compounds (e.g.
1 050
pitch, resin), silicon carbide, and metals are removed
4.2 Determination of the loss on drying at 250 °C (LOD ) gravimetric method
250
4.2.1 Principle
The test sample is heated at 250 °C ± 10 °C and the loss of mass from attached water is determined.
4.2.2 Apparatus
4.2.2.1 Heat-resistant container, for example with dimensions 200 mm × 150 mm × 30 mm and made
from stainless steel.
4.2.3 Procedure
Heat the heat-resistant container at 250 °C ± 10 °C for 30 min. Cool in a desiccator, weigh and record its
empty mass , m , to the nearest 0,01 g.
0
Transfer the sample into the container and spread it out flat. Then weigh and record the mass, m , of the
1
container and sample to the nearest 0,01 g.
2 © ISO 2008 – All rights reserved
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SIST EN ISO 21068-2:2008
ISO 21068-2:2008(E)
Place the container without a lid in an air bath and heat it at 250 °C ± 10 °C for 16 h. Allow to cool in a
desiccator. Weigh and record the mass, m , of the container plus the dried sample to the nearest 0,01 g.
2
4.2.4 Calculation
Calculate the loss on drying at 250 °C, LOD , as a percentage by mass, using Equation (1).
250
mm−
12
LOD=×100 (1)
250
mm−
10
where
m is the mass of the empty container, in grams;
0
m is the mass of the container plus the sample before drying, in grams;
1
m is the mass of the container plus the sample after drying, in grams.
2
4.3 Determination of the loss on calcination in argon (LOI )
Ar
4.3.1 Principle
Pretreatment under argon at 750 °C to remove volatile matter. The loss of volatile matter is determined by a
gravimetric method.
The residue (R ) is normally used for determination of C , SiC and C (therefore these parameters will be
Ar total free
additionally indexed with ), and the change in mass has to be considered for the calculation of the result.
Ar
4.3.2 Apparatus
Ordinary laboratory apparatus and the following.
4.3.2.1 U-tube, with ground stoppers and filled with magnesium perchlorate.
4.3.2.2 Resistance furnace, heatable and adjustable at (750 ± 25) °C, in the centre of the heating zone.
4.3.2.3 Thermocouple with display, registering up to 1 200 °C.
4.3.2.4 Ceramic tube, with cones or other gastight connector, with an inner diameter W 16 mm, made
from porcelain, sillimanite, quartz or other suitable material.
4.3.2.5 Open combustion boats, of unglazed ceramic material, the length of which is adapted to the
oven's zone of constant temperature. The boats shall be broad enough to accommodate the amount of
sample required for the determination.
4.3.2.6 Gas flowmeter, with an upper scale reading of around 20 l/h.
The argon-conducting parts, such as tubes and connections, should be made of material proofed against
oxygen diffusion. Preferable materials are glass and copper. Silicone is unsuitable.
4.3.2.7 Test assembly
The test assembly is set up as shown in Figure 1.
© ISO 2008 – All rights reserved 3
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SIST EN ISO 21068-2:2008
ISO 21068-2:2008(E)
Key
1 valve for pressure control 5 argon cylinder 9 combustion boat
2 cold zone B 6 glass wool 10 gas flowmeter
3 cold zone A 7 magnesium perchlorate
4 ceramic tube 8 resistance furnace
Figure 1 — Apparatus set-up for determination of loss on calcination in argon
4.3.3 Reagents
4.3.3.1 Argon, 99,997 %.
4.3.4 Procedure
4.3.4.1 Check of test assembly, blank value determination
To check a newly set up test assembly or to carry out routine checks, a few samples of known volatile-matter
content shall be calcined as described in 4.3.4.2 before examining the analytical sample.
The difference between the result found in accordance with 4.3.4.2 and the known volatile-matter content shall
be taken into account as the blank value.
4.3.4.2 Determination
Carry out at least two determinations.
Before use, flush the apparatus for at least 15 min with argon.
Weigh the empty combustion boat that has previously been heated at (750 ± 25) °C and record the mass m .
0
Weigh 2 g of the sample to the nearest 0,001 g into the combustion boat and record the mass m .
1
Place the combustion boat and sample in cold zone A of the apparatus at u 200 °C. Pass argon through it at
a rate that ensures five changes of gas in the tube within 15 min.
Place the sample in the centre of the heating zone and calcine for 20 min at (750 ± 25) °C, without interruption
of the argon stream.
Move the combustion boat into cold zone B and cool in the argon stream at u 200 °C.
NOTE A period of 20 min is usually required to cool the sample.
Allow the boat to cool to room temperature in a desiccator, weigh to the nearest 0,001 g and record the final
mass, m .
2
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SIST EN ISO 21068-2:2008
ISO 21068-2:2008(E)
Repeat the calcination in the argon stream at (750 ± 25) °C until constant mass is obtained, i.e. when two
measurements taken at an interval of 30 min do not differ by more than 5 mg.
If the residue is required for the determination of other components, homogenize it and keep it in a closed
weighing bottle in a desiccator.
4.3.5 Calculation
Calculate the loss on calcination in argon at 750 °C, LOI , as a percentage by mass, using Equation (2).
Ar
mm−
12
LOI=×100 (2)
Ar
mm−
10
where
m is the mass of the empty combustion boat, in grams;
0
m is the mass of the combustion boat plus sample before ignition, in grams;
1
m is the mass of the combustion boat plus sample after ignition, in grams.
2
NOTE The decrease in mass is denoted by a minus sign.
4.4 Determination of the change in mass by heat pretreatment in air
For resin- and pitch-bonded materials, a sample pretreatment shall be performed in accordance with
ISO 10060, or the following procedure shall be followed.
Usually before crushing and grinding, subject a sample of approximately 1 kg to heat treatment as follows:
a) resin-bonded materials: 200 °C for 18 h in air;
b) pitch-bonded materials: 400 °C for 18 h in air.
Calculate the change in mass at 200 °C/400 °C, D, as a percentage by mass, using Equation (3).
mm−
12
D=×100 (3)
mm−
10
where
m is the mass of the empty container, in grams;
0
m is the mass of the container plus sample before heat pretreatment, in grams;
1
m is the mass of the container plus sample after ignition, in grams.
...
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