SIST ISO 4689-3:2005
(Main)Iron ores -- Determination of sulfur content -- Part 3: Combustion/infrared method
Iron ores -- Determination of sulfur content -- Part 3: Combustion/infrared method
ISO 4689-3:2004 specifies a combustion/infrared method, using a high-frequency induction furnace, for the determination of the sulfur content of iron ores.
This method is applicable to sulfur contents between 0,002 % (mass fraction) and 0,25 % (mass fraction) in natural iron ores, iron ore concentrates and agglomerates, including sinter products. The method is not applicable to iron ores containing more than 1,0 % (mass fraction) of combined water. The apparatus, of which the metal filter is equipped with a heating device, can be applied to iron ores containing less than 3,0 % (mass fraction) of combined water.
Minerais de fer -- Dosage du soufre -- Partie 3: Méthode par combustion et infrarouge
Železove rude – Določevanje žvepla – 3. del: Metoda s sežiganjem/infrardeča metoda
General Information
Relations
Standards Content (Sample)
INTERNATIONAL ISO
STANDARD 4689-3
First edition
2004-04-01
Iron ores — Determination of sulfur
content —
Part 3:
Combustion/infrared method
Minerais de fer — Dosage du soufre —
Partie 3: Méthode par combustion et infrarouge
Reference number
ISO 4689-3:2004(E)
©
ISO 2004
---------------------- Page: 1 ----------------------
ISO 4689-3:2004(E)
PDF disclaimer
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not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
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Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the
unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
© ISO 2004
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or
ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
©
ii ISO 2004 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 4689-3:2004(E)
Contents Page
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Reagents . 2
5 Apparatus . 2
6 Sampling and samples . 5
7 Procedure . 5
8 Expression of results . 6
9 Test report . 9
Annex A (normative) Flowsheet of the procedure for the acceptance of analytical values for test
samples . 10
Annex B (informative) Derivation of repeatability and permissible tolerance equations . 11
Annex C (informative) Precision data obtained by international analytical trial . 12
Bibliography . 14
©
ISO 2004 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 4689-3:2004(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 4689-3 was prepared by Technical Committee ISO/TC 102, Iron ore and direct reduced iron, Subcommittee
SC 2, Chemical analysis.
This first edition, in part cancels and replaces ISO 4690:1986, which has been technically revised.
ISO 4689 consists of the following parts, under the general title Iron ores — Determination of sulfur content:
— Part 2: Combustion/titration method
— Part 3: Combustion/infrared method
The following part is under preparation:
— Part 1: Barium sulfate gravimetric method
©
iv ISO 2004 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 4689-3:2004(E)
Introduction
This part of ISO 4689 is a new procedure. ISO 4689-2 was originally published as ISO 4690:1986, Iron ores —
Determination of sulfur content — Combustion method. Under a policy of rationalization of the numbering
system used in ISO/TC 102, it has been decided to re-designate ISO 4690:1986 as ISO 4689-2. It was further
decided to introduce a combustion/infrared method, numbered ISO 4689-3, i.e. this part of ISO 4689.
When next revised, ISO 4689:1986, Iron ores — Determination of sulfur content — Barium sulfate gravimetric
method, will be re-designated 4689-1.
©
ISO 2004 – All rights reserved v
---------------------- Page: 5 ----------------------
.
vi
---------------------- Page: 6 ----------------------
INTERNATIONAL STANDARD ISO 4689-3:2004(E)
Iron ores — Determination of sulfur content —
Part 3:
Combustion/infrared method
WARNING — This part of ISO 4689 may involve hazardous materials, operations and equipment. This
part of ISO 4689 does not purport to address all of the safety problems associated with its use. It is the
responsibility of the user of this part of ISO 4689 to establish appropriate health and safety practices
and determine the applicability of regulatory limitations prior to use.
1Scope
This part of ISO 4689 specifies a combustion/infrared method, using a high-frequency induction furnace, for the
determination of the sulfur content of iron ores.
0,002 % 0,25 %
This method is applicable to sulfur contents between (mass fraction) and (mass fraction) in
natural iron ores, iron ore concentrates and agglomerates, including sinter products. The method is not
1,0 %
applicable to iron ores containing more than (mass fraction) of combined water. The apparatus, of which
the metal filter is equipped with a heating device, can be applied to iron ores containing less than 3,0 % (mass
fraction) of combined water.
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 385-1:1984, Laboratory glassware — Burettes — Part 1: General requirements
ISO 648:1977, Laboratory glassware — One-mark pipettes
ISO 1042:1998, Laboratory glassware — One-mark volumetric flasks
ISO 3082:2000, Iron ores — Sampling and sample preparation procedures
ISO 7764:1985, Iron ores — Preparation of predried test samples for chemical analysis
3 Principle
The sample is mixed with a flux containing iron, tin and tungsten and heated in a high-frequency induction
furnace, using oxygen as a supporting fuel and carrier gas.
The evolved sulfur dioxide is carried by oxygen into the cell of an infrared detector, where the absorption scale
is read.
©
ISO 2004 – All rights reserved 1
---------------------- Page: 7 ----------------------
ISO 4689-3:2004(E)
4Reagents
During analysis, use only reagents of recognized analytical grade, and only distilled water or water of equivalent
purity.
4.1 Metallic iron, particle size 0,2 mm to 1,2 mm and containing less than 0,001 % sulfur.
4.2 Magnesium perchlorate, Mg(ClO ) anhydrous, free flowing, particle size 0,5 mm to 2 mm.
4 2
4.3 Iron(III) oxide, containing less than 0,003 % sulfur.
4.4 Metallic tin, particle size 0,2 mm to 1,2 mm, containing less than 0,001 % sulfur.
4.5 Metallic tungsten, particle size 0,2 mm to 1,2 mm, containing less than 0,001 % sulfur.
4.6 Soda-asbestos, particle size 0,5 mm to 2 mm.
4.7 Sodium hydroxide, particle size 0,5 mm to 2 mm.
4.8 Standard sulfur solution, prepared as follows.
◦ ◦
Dry 8g of potassium sulfate (purity > 99,9 % (mass fraction) to constant mass at 105C1 to 10 C and cool in
a desiccator. Weigh the dried masses of potassium sulfate specified in Table 1 and dissolve each portion in
water. Cool, transfer each portion to separate 100 ml volumetric flasks and dilute to volume with water.
Table 1 — Sulfur standard solution (calibration series)
Solution No. Mass of potassium sulfate Concentration of sulfur
gmg/ml
1 0,543 5 1,00
2 1,087 0 2,00
3 1,902 2 3,50
4 2,717 4 5,00
5 Apparatus
Ordinary laboratory apparatus, including one-mark pipettes and one-mark volumetric flasks complying with the
specifications of ISO 648:1977 and ISO 1042 respectively as well as the following.
5.1 Oxygen supply.
5.2 Absorption tower, containing soda-asbestos (4.6) or sodium hydroxide (4.7).
5.3 Drying tower, containing magnesium perchlorate (4.2).
5.4 High-frequency induction furnace, having a heating induction coil (height 30 mm to 55 mm, 4 to 5 rolls),
◦
capable of heating to a temperature of 1 200 C.
An example of a combustion furnace, with combustion gas-refining section, is given in Figure 1.
5.5 Combustion tube, quartz.
5.6 Refractory combustion crucible.
©
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ISO 4689-3:2004(E)
Key
1 metal filter
2 heating device
3 quartz combustion tube
4 dust trap
5 high-frequency induction coil
6crucible
7 holder
a
Oxygen.
b
Combustion gas.
Figure 1 — Example of combustion furnace with combustion gas-refining section
©
ISO 2004 – All rights reserved 3
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ISO 4689-3:2004(E)
5.7 Tin capsule.
The following dimensions may be used as guidelines.
Combustion tube Combustion crucible Tin capsule
Length 140 m to 220 m Height 26 mm Diameter 6 mm
Outer diameter 30 mm to 44 mm Internal diameter 10 mm Height 18 mm
Inner diameter 26 mm to 37 mm Outer diameter 26 mm Mass 0,3 g
Volume 0,4 ml
5.8 Metal filter.
5.9 Dust trap, containing glass wool.
5.10 Detector for infrared absorption, an example of which is shown in Figure 2.
5.11 Micro-pipette, 100µl1 capacity, accurate to µl.
Key
1 chopper
2 measuring cell
3 infrared detector
4motor
5 infrared source
6filter cell
7 reference cell
a
Combustion gas.
b
Oxygen.
Figure 2 — Example of an infrared detection system
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ISO 4689-3:2004(E)
6 Sampling and samples
6.1 Laboratory sample
For analysis, use a laboratory sample of −100µm particle size which has been taken and prepared in
accordance with ISO 3082. In the case of ores having significant contents of combined water or oxidizable
compounds, use a particle size of −160µm.
NOTE A guideline on significant contents of combined water and oxidizable compounds is incorporated in ISO 7764.
6.2 Preparation of predried test samples
Thoroughly mix the laboratory sample and, taking multiple increments, extract a test sample in such a manner
◦ ◦
that i
...
SLOVENSKI STANDARD
SIST ISO 4689-3:2005
01-november-2005
äHOH]RYHUXGH±'RORþHYDQMHåYHSOD±GHO 0HWRGDVVHåLJDQMHPLQIUDUGHþD
PHWRGD
Iron ores -- Determination of sulfur content -- Part 3: Combustion/infrared method
Minerais de fer -- Dosage du soufre -- Partie 3: Méthode par combustion et infrarouge
Ta slovenski standard je istoveten z: ISO 4689-3:2004
ICS:
73.060.10 Železove rude Iron ores
SIST ISO 4689-3:2005 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
SIST ISO 4689-3:2005
---------------------- Page: 2 ----------------------
SIST ISO 4689-3:2005
INTERNATIONAL ISO
STANDARD 4689-3
First edition
2004-04-01
Iron ores — Determination of sulfur
content —
Part 3:
Combustion/infrared method
Minerais de fer — Dosage du soufre —
Partie 3: Méthode par combustion et infrarouge
Reference number
ISO 4689-3:2004(E)
©
ISO 2004
---------------------- Page: 3 ----------------------
SIST ISO 4689-3:2005
ISO 4689-3:2004(E)
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but shall
not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the
unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
© ISO 2004
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or
ISO's member body in the country of the requester.
ISO copyright office
Case postale 56 CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
©
ii ISO 2004 – All rights reserved
---------------------- Page: 4 ----------------------
SIST ISO 4689-3:2005
ISO 4689-3:2004(E)
Contents Page
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Reagents . 2
5 Apparatus . 2
6 Sampling and samples . 5
7 Procedure . 5
8 Expression of results . 6
9 Test report . 9
Annex A (normative) Flowsheet of the procedure for the acceptance of analytical values for test
samples . 10
Annex B (informative) Derivation of repeatability and permissible tolerance equations . 11
Annex C (informative) Precision data obtained by international analytical trial . 12
Bibliography . 14
©
ISO 2004 – All rights reserved iii
---------------------- Page: 5 ----------------------
SIST ISO 4689-3:2005
ISO 4689-3:2004(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 4689-3 was prepared by Technical Committee ISO/TC 102, Iron ore and direct reduced iron, Subcommittee
SC 2, Chemical analysis.
This first edition, in part cancels and replaces ISO 4690:1986, which has been technically revised.
ISO 4689 consists of the following parts, under the general title Iron ores — Determination of sulfur content:
— Part 2: Combustion/titration method
— Part 3: Combustion/infrared method
The following part is under preparation:
— Part 1: Barium sulfate gravimetric method
©
iv ISO 2004 – All rights reserved
---------------------- Page: 6 ----------------------
SIST ISO 4689-3:2005
ISO 4689-3:2004(E)
Introduction
This part of ISO 4689 is a new procedure. ISO 4689-2 was originally published as ISO 4690:1986, Iron ores —
Determination of sulfur content — Combustion method. Under a policy of rationalization of the numbering
system used in ISO/TC 102, it has been decided to re-designate ISO 4690:1986 as ISO 4689-2. It was further
decided to introduce a combustion/infrared method, numbered ISO 4689-3, i.e. this part of ISO 4689.
When next revised, ISO 4689:1986, Iron ores — Determination of sulfur content — Barium sulfate gravimetric
method, will be re-designated 4689-1.
©
ISO 2004 – All rights reserved v
---------------------- Page: 7 ----------------------
SIST ISO 4689-3:2005
.
vi
---------------------- Page: 8 ----------------------
SIST ISO 4689-3:2005
INTERNATIONAL STANDARD ISO 4689-3:2004(E)
Iron ores — Determination of sulfur content —
Part 3:
Combustion/infrared method
WARNING — This part of ISO 4689 may involve hazardous materials, operations and equipment. This
part of ISO 4689 does not purport to address all of the safety problems associated with its use. It is the
responsibility of the user of this part of ISO 4689 to establish appropriate health and safety practices
and determine the applicability of regulatory limitations prior to use.
1Scope
This part of ISO 4689 specifies a combustion/infrared method, using a high-frequency induction furnace, for the
determination of the sulfur content of iron ores.
0,002 % 0,25 %
This method is applicable to sulfur contents between (mass fraction) and (mass fraction) in
natural iron ores, iron ore concentrates and agglomerates, including sinter products. The method is not
1,0 %
applicable to iron ores containing more than (mass fraction) of combined water. The apparatus, of which
the metal filter is equipped with a heating device, can be applied to iron ores containing less than 3,0 % (mass
fraction) of combined water.
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 385-1:1984, Laboratory glassware — Burettes — Part 1: General requirements
ISO 648:1977, Laboratory glassware — One-mark pipettes
ISO 1042:1998, Laboratory glassware — One-mark volumetric flasks
ISO 3082:2000, Iron ores — Sampling and sample preparation procedures
ISO 7764:1985, Iron ores — Preparation of predried test samples for chemical analysis
3 Principle
The sample is mixed with a flux containing iron, tin and tungsten and heated in a high-frequency induction
furnace, using oxygen as a supporting fuel and carrier gas.
The evolved sulfur dioxide is carried by oxygen into the cell of an infrared detector, where the absorption scale
is read.
©
ISO 2004 – All rights reserved 1
---------------------- Page: 9 ----------------------
SIST ISO 4689-3:2005
ISO 4689-3:2004(E)
4Reagents
During analysis, use only reagents of recognized analytical grade, and only distilled water or water of equivalent
purity.
4.1 Metallic iron, particle size 0,2 mm to 1,2 mm and containing less than 0,001 % sulfur.
4.2 Magnesium perchlorate, Mg(ClO ) anhydrous, free flowing, particle size 0,5 mm to 2 mm.
4 2
4.3 Iron(III) oxide, containing less than 0,003 % sulfur.
4.4 Metallic tin, particle size 0,2 mm to 1,2 mm, containing less than 0,001 % sulfur.
4.5 Metallic tungsten, particle size 0,2 mm to 1,2 mm, containing less than 0,001 % sulfur.
4.6 Soda-asbestos, particle size 0,5 mm to 2 mm.
4.7 Sodium hydroxide, particle size 0,5 mm to 2 mm.
4.8 Standard sulfur solution, prepared as follows.
◦ ◦
Dry 8g of potassium sulfate (purity > 99,9 % (mass fraction) to constant mass at 105C1 to 10 C and cool in
a desiccator. Weigh the dried masses of potassium sulfate specified in Table 1 and dissolve each portion in
water. Cool, transfer each portion to separate 100 ml volumetric flasks and dilute to volume with water.
Table 1 — Sulfur standard solution (calibration series)
Solution No. Mass of potassium sulfate Concentration of sulfur
gmg/ml
1 0,543 5 1,00
2 1,087 0 2,00
3 1,902 2 3,50
4 2,717 4 5,00
5 Apparatus
Ordinary laboratory apparatus, including one-mark pipettes and one-mark volumetric flasks complying with the
specifications of ISO 648:1977 and ISO 1042 respectively as well as the following.
5.1 Oxygen supply.
5.2 Absorption tower, containing soda-asbestos (4.6) or sodium hydroxide (4.7).
5.3 Drying tower, containing magnesium perchlorate (4.2).
5.4 High-frequency induction furnace, having a heating induction coil (height 30 mm to 55 mm, 4 to 5 rolls),
◦
capable of heating to a temperature of 1 200 C.
An example of a combustion furnace, with combustion gas-refining section, is given in Figure 1.
5.5 Combustion tube, quartz.
5.6 Refractory combustion crucible.
©
2 ISO 2004 – All rights reserved
---------------------- Page: 10 ----------------------
SIST ISO 4689-3:2005
ISO 4689-3:2004(E)
Key
1 metal filter
2 heating device
3 quartz combustion tube
4 dust trap
5 high-frequency induction coil
6crucible
7 holder
a
Oxygen.
b
Combustion gas.
Figure 1 — Example of combustion furnace with combustion gas-refining section
©
ISO 2004 – All rights reserved 3
---------------------- Page: 11 ----------------------
SIST ISO 4689-3:2005
ISO 4689-3:2004(E)
5.7 Tin capsule.
The following dimensions may be used as guidelines.
Combustion tube Combustion crucible Tin capsule
Length 140 m to 220 m Height 26 mm Diameter 6 mm
Outer diameter 30 mm to 44 mm Internal diameter 10 mm Height 18 mm
Inner diameter 26 mm to 37 mm Outer diameter 26 mm Mass 0,3 g
Volume 0,4 ml
5.8 Metal filter.
5.9 Dust trap, containing glass wool.
5.10 Detector for infrared absorption, an example of which is shown in Figure 2.
5.11 Micro-pipette, 100µl1 capacity, accurate to µl.
Key
1 chopper
2 measuring cell
3 infrared detector
4motor
5 infrared source
6filter cell
7 reference cell
a
Combustion gas.
b
Oxygen.
Figure 2 — Example of an infrared detection system
©
4 ISO 2004 – All rights reserved
---------------------- Page: 12 ----------------------
SIST ISO 4689-3:2005
ISO 4689-3:2004(E)
6 Sampling and samples
6.1 Laboratory sample
For analysis, use a laboratory sample of −100µm parti
...
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