ISO/FDIS 7692
(Main)Ferrotitanium — Determination of titanium content — Titrimetric method
Ferrotitanium — Determination of titanium content — Titrimetric method
The method is applicable to ferrotitanium having titanium contents between 20 and 80 % (m/m). Specifies principle, reagents, apparatus, sample, procedure, expression of results and test report. Figures show the Bunsen valve and the apparatus for titration.
Ferro-titane — Dosage du titane — Méthode titrimétrique
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International
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ISO/TC 132
Ferrotitanium — Determination
Secretariat: SAC
of titanium content — Titrimetric
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2024-10-11
Ferro-titane — Dosage du titane — Méthode titrimétrique
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Reference number
FINAL DRAFT
International
Standard
ISO/TC 132
Ferrotitanium — Determination
Secretariat: SAC
of titanium content —
Voting begins on:
Titrimetric method
Ferro-titane — Dosage du titane — Méthode titrimétrique
Voting terminates on:
RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT,
WITH THEIR COMMENTS, NOTIFICATION OF ANY
RELEVANT PATENT RIGHTS OF WHICH THEY ARE AWARE
AND TO PROVIDE SUPPOR TING DOCUMENTATION.
© ISO 2024
IN ADDITION TO THEIR EVALUATION AS
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO
LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
or ISO’s member body in the country of the requester.
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland Reference number
ii
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 1
6 Apparatus . 3
7 Sample . 5
8 Procedure . 5
8.1 Test portion .5
8.2 Blank test and check test .5
8.3 Determination .6
8.3.1 Decomposition of the test portion .6
8.3.2 Absence of interfering elements .6
8.3.3 Separation of interfering elements .6
8.3.4 Reduction .6
8.3.5 Titration .7
9 Expression of results . 7
10 Precision . 7
10.1 Expression of precision .7
10.2 Calculation of final results .8
11 Test report . 8
Annex A (informative) Original data from the verification test . 9
Annex B (informative) Graphical representation of the precision date .10
Annex C (informative) Flow chart for the acceptance procedure of test results .11
Bibliography .12
iii
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.
The procedures used to develop this document and those intended for its further maintenance are described
in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the different types
of ISO document should be noted. This document was drafted in accordance with the editorial rules of the
ISO/IEC Directives, Part 2 (see www.iso.org/directives).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent
rights in respect thereof. As of the date of publication of this document, ISO had not received notice of (a)
patent(s) which may be required to implement this document. However, implementers are cautioned that
this may not represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and expressions
related to conformity assessment, as well as information about ISO's adherence to the World Trade
Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 132, Ferroalloys.
This second edition cancels and replaces the first edition (ISO 7692:1983), which has been technically
revised.
The main changes are as follows:
— in 5.5 (previously in 4.6), hydrofluoric acid has been replaced with fluoboric acid;
— in 5.13 (previously in 4.17), the concentration of titanium standard solution has been changed;
— in 5.13.1 (previously in 4.17.1), the amount of titanium(IV) dioxide has been reduced and the decomposition
of titanium(IV) dioxide has been changed;
— in 5.13.2 (previously in 4.17.2), potassium hexafluorotitanate has been replaced with a titanium sponge
and the preparation has been changed;
— in Clause 6 (previously in Clause 5), PTE beakers has been replaced with conical flask;
— in Clause 7 (previously in Clause 6), the mesh size of the sieve has been changed;
— the paragraph of the definition of test portion has been changed in 8.1 and the amount of test portion in
8.1 (previously 7.1) has been reduced from 1,0 g to 0,50 g;
— in 8.2.1, (previously in 7.4.1), the method using titanium sponge has been removed;
— in 8.3.1 (previously 7.5.1), the amount of acids has been reduced;
— in 8.3.4 (previously 7.5.3.2), the amount of the aluminium has been reduced from 4,0 g to 3,0 g ± 0,2 g;
— in Clause 9 (previously in Clause 8), the expression of results has been changed;
— in Clause 10, the precision has been added;
— in Clause 11 (previously in Clause 9), the test report has been changed;
iv
— Annex A has been added;
— Annex B has been added;
— Annex C has been added.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
v
FINAL DRAFT International Standard ISO/FDIS 7692:2024(en)
Ferrotitanium — Determination of titanium content —
Titrimetric method
1 Scope
This document specifies a titrimetric method for the determination of the titanium content of ferrotitanium.
The method is applicable to titanium contents of a mass fraction between 20,0 % and 80,0 % in ferrotitanium.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content constitutes
requirements 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, Laboratory glassware — Burettes
ISO 648, Laboratory glassware — Single-volume pipettes
ISO 1042, Laboratory glassware — One-mark volumetric flasks
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 3713, Ferroalloys — Sampling and preparation of samples — General rules
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Principle
The test portion shall be dissolved with sulfuric, fluoboric, nitric and hydrochloric acids. And the interfering
elements (chromium, vanadium, molybdenum and tin), if present, shall be separated by precipitation of
3+
titanium hydroxide in the presence of hydrogen peroxide. Then, the titanium shall be reduced to Ti by
3+
aluminium metal in an atmosphere of carbon dioxide or nitrogen. Finally, the Ti shall be titrated with
standard volumetric iron(III) ammonium sulfate solution in the presence of thiocyanate as indicator.
5 Reagents
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only
grade 3 water specified in ISO 3696.
5.1 Aluminium, of minimum purity 99,5 %, in the form of foil 0,05 mm thick, and free from titanium.
5.2 Sodium hydrogen carbonate (NaHCO ).
5.3 Nitric acid, with a ρ of 1,38 g/ml to 1,42 g/ml.
5.4 Sulfuric acid, ρ = 1,84 g/ml.
5.5 Hydrochloric acid, with a ρ of 1,16 g/ml to 1,19 g/ml.
5.6 Fluoboric acid, with a mass fraction of 40 % (ρ = 1,39 g/ml).
5.7 Sulfuric acid, ρ = 1,84 g/ml, diluted 1 + 1. Add carefully 1 volume of the sulfuric acid (5.4) to 1 volume
of water. Cool while mixing.
5.8 Sulfuric acid, ρ = 1,84 g/ml, diluted 1 + 4. Add carefully 1 volume of the sulfuric acid (5.4) to 4 volume
of water. Cool while mixing.
5.9
...
ISO/DISFDIS 7692:2024(en)
Date: 2024-06
ISO/TC 132/WG 4
Secretariat: SAC
Date: 2024-09-27
Ferrotitanium — Determination of titanium content — Titrimetric
method
Ferro-titane — Dosage du titane — Méthode titrimétrique
FDIS stage
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this
publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including
photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested
from either ISO at the address below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: + 41 22 749 01 11
Fax: +41 22 749 09 47
EmailE-mail: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
Contents
Foreword . iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 1
6 Apparatus . 3
7 Sample . 5
8 Procedure . 5
8.1 Test portion . 5
8.2 Blank test and check test . 5
8.3 Determination . 6
9 Expression of results . 7
10 Precision . 8
10.1 Expression of precision . 8
10.2 Calculation of final results . 8
11 Test report . 8
Annex A (informative) Original data from the verification test . 10
Annex B (informative) Graphical representation of the precision date . 11
Annex C (informative) Flow chart for the acceptance procedure of test results . 12
Bibliography . 13
iii
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.
The procedures used to develop this document and those intended for its further maintenance are described
in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the different types
of ISO document should be noted. This document was drafted in accordance with the editorial rules of the
ISO/IEC Directives, Part 2 (see www.iso.org/directives).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent
rights in respect thereof. As of the date of publication of this document, ISO [had/had not] received notice of
(a) patent(s) which may be required to implement this document. However, implementers are cautioned
that this may not represent the latest information, which may be obtained from the patent database
available at www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent
rights.
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and expressions
related to conformity assessment, as well as information about ISO's adherence to the World Trade
Organization (WTO) principles in the Technical Barriers to Trade (TBT), see
www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 132, Ferroalloys.
This second edition cancels and replaces the first edition (ISO 7692:1983), which has been technically
revised.
The main changes are as follows:
— in 5.5 (previously in 4.6), hydrofluoric acid has been replaced with fluoboric acid;
— in 5.13 (previously in 4.17), the concentration of titanium standard solution has been changed;
— in 5.13.1 (previously in 4.17.1), the amount of titanium(IV) dioxide has been reduced and the
decomposition of titanium(IV) dioxide has been changed;
— in 5.13.2 (previously in 4.17.2), potassium hexafluorotitanate has been replaced with a titanium
sponge and the preparation has been changed;
— in Clause 6 (previously in Clause 5), PTE beakers has been replaced with conical flask;
— in Clause 7 (previously in Clause 6), the mesh size of the sieve has been changed;
— the paragraph of the definition of test portion has been changed in 8.1 and the amount of test portion
in 8.1 (previously 7.1) has been reduced from 1,0 g to 0,50 g;
— in 8.2.1, (previously in 7.4.1), the method using titanium sponge has been removed;
iv
— in 8.3.1 (previously 7.5.1), the amount of acids has been reduced;
— in 8.3.4 (previously 7.5.3.2), the amount of the aluminium has been reduced from 4,0 g to
3,0 g ± 0,2 g;
— in Clause 9 (previously in Clause 8), the expression of results has been changed;
— in Clause 10, the precision has been added;
— in Clause 11 (previously in Clause 9), the test report has been changed;
— Annex A has been added;
— Annex B has been added;
— Annex C has been added.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
This second edition cancels and replaces the first edition (ISO 7692:1983), which has been technically
revised.
The main changes are as follows:
— in 5.5 (previously in 4.6), the hydrofluoric acid has been replaced with the fluoboric acid;
— in 5.13 (previously in 4.17), the concentration of titanium standard solution has been changed;
—in 5.13.1 (previously in 4.17.1), the amount of titanium(IV) dioxide has been reduced, the decomposition of
titanium(IV) dioxide have been changed;
— in 5.13.2 (previously in 4.17.2), the potassium hexafluorotitanate has been replaced with titanium sponge ,
and the preparation has been changed;
— in Clause 6(previously in Clause 5), the PTE beakers has been replaced with the conical flask;
— in Clause 7(previously in Clause 6), the mesh size of the sieve has been changed;
— in Clause 8, the paragraph of the definition of test portion has been changed in 8.1 and the amount of test
portion in 8.1 (previously 7.1) has been reduced from 1,0 g to 0,50 g;
— (previously in 7.4.1), the method using titanium sponge has been removed;
— in 8.3.1 (previously 7.5.1), the amount of acids has been reduced;
— in 8.3.4 (previously 7.5.3.2), the amount of the aluminium has been reduced from 4,0 g to 3,0 g ± 0,2 g;
— in Clause 9(previously in Clause 8), the expression of results has been changed;
— in Clause 10, the precision has been added;
— in Clause 11(previously in Clause 9), the test report has been changed;
— Annex A, “Original data of the verification test” has been added;
— Annex B, “Graphical representation of the precision date” has been added.
v
— Annex C, “Flow chart for the acceptance procedure of test results” has been added.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found .
vi
Ferrotitanium — Determination of titanium content -— Titrimetric
method
1 Scope
This document specifies a titrimetric method for the determination of the titanium content of ferrotitanium.
The method is applicable to titanium contents of a mass fraction between 20,0 % and 80,0% (mass
fraction) % in ferrotitanium.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content constitutes
requirements 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, Laboratory glassware — Burettes
ISO 648, Laboratory glassware — Single-volume pipettes
ISO 1042, Laboratory glassware — One-mark volumetric flasks
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 3713, Ferroalloys — Sampling and preparation of samples — General rules
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— — IEC Electropedia: available at
— — ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at https://www.electropedia.org/
4 Principle
The test portion shall be dissolved with sulfuric, fluoboric, nitric and hydrochloric acids. And the interfering
elements (chromium, vanadium, molybdenum and tin), if present, shall be separated by precipitation of
3+
titanium hydroxide in the presence of hydrogen peroxide. Then, the titanium shall be reduced to Ti by
3+
aluminium metal in an atmosphere of carbon dioxide or nitrogen. Finally, the Ti shall be titrated with
standard volumetric iron(III) ammonium sulfate solution in the presence of thiocyanate as indicator.
5 Reagents
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only grade
3 water as specified in ISO 3696.
5.1 5.1 Aluminium, of minimum purity 99,5 %, in the form of foil 0,05 mm thick, and free from
titanium.
5.2 5.2 Sodium hydrogen carbonate (NaHCO ).
5.3 5.3 Nitric acid, with a ρ of 1,38 g/ml to 1,42 g/ml.
5.4 5.4 Sulfuric acid, ρ = 1,84 g/ml.
5.5 5.5 Hydrochloric acid, with a ρ of 1,16 g/ml to 1,19 g/ml.
5.6 5.6 Fluoboric acid, 40 %with a mass fraction of 40 % (ρ = 1,39 g/ml).
5.7 5.7 Sulfuric acid, ρ = 1,84 g/ml, diluted 1 + 1. Add carefully 1 volume of the sulfuric acid
(5.4(5.4)) to 1 volume of water. Cool while mixing.
5.8 5.8 Sulfuric acid, ρ = 1,84 g/ml, diluted 1 + 4. Add carefully 1 volume of the sulfuric acid
(5.4(5.4)) to 4 volume of water. Cool while mixing.
5.9 5.9 Sodium hydroxide (NaOH),) solution, of 100 g/l.
5.10 5.10 Sodium hydroxide (NaOH),) solution, of 20 g/l.
5.11 5.11 Hydrogen peroxide (H O ), 30 % by) solution, of a volume solution.fraction of 30 %.
2 2
5.12 5.12 Iron(III) sulfate (Fe (SO ) ),) solution, of 15 g/l.
2 4 3
5.13 5.13 Titanium standard solution, of 1,0 mg/ml, prepared by one of the following methods.
5.13.1 5.13.1 Preparation from titanium(IV) dioxide
Weigh 0,417 2 g ± 0,000 1 g of titanium(IV) dioxide (spectrum pure), which has been previously calcined for
2 h at 800 °C. In a 250 ml dry conical flask, dissolve the titanium(IV) dioxide with 10 g of ammonium sulfate
and 20 ml of the sulfuric acid (5.4(5.4).). Heat the conical flask on a hot-plate until the white sulfuric fumes
appear, then allow to cool. Transfer quantitatively to a 250 ml volumetric flask,. after cooling, dilute to the
mark with water and mix.
5.13.2 5.13.2 Preparation from titanium sponge (99,8 % minimum purity)
In a 250 ml polytetrafluoroethylene (PTFE) beaker, dissolve 0,250 0 g ± 0,000 1 g of titanium sponge
(99,8 % minimum purity) with 40 ml of the sulfuric acid (5.7(5.7)) and 5 ml of the hydrofluoric acid. Cover
the beaker with a PTFE cover. Oxidize while cold by adding 5 ml of the nitric acid (5.3(5.3)) drop by drop.
Heat the PTFE beaker on a hot-plate until the white sulfuric fumes appear,
...
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