ISO 13548:2025
(Main)Copper and zinc sulfide concentrates — Determination of fluorine content by sodium hydroxide fusion and fluoride ion selective electrode detection
Copper and zinc sulfide concentrates — Determination of fluorine content by sodium hydroxide fusion and fluoride ion selective electrode detection
This document specifies a procedure for the determination of fluorine in copper and zinc sulfide concentrates by sodium hydroxide fusion and fluoride ion selective electrode (FISE) detection. Fluoride ions are leached from the sodium hydroxide fusion and presented to the FISE. Potential interfering ions are masked by the use of a complexing agent and control of solution pH. If the aluminium content in the concentrate is up to a mass fraction of 4,5 %, there is no effect of aluminium in this method. However, if the aluminium content in the concentrate exceeds a mass fraction of 4,5 %, there is a possibility that it can affect the analytical results. The method is applicable to fluorine in the following ranges: — copper concentrates: mass fraction of 0,008 % to 0,3 %; — zinc concentrates: mass fraction of 0,005 % to 0,1 %. The results of the trueness test can be found in Annex C.
Concentrés sulfurés de cuivre et de zinc — Dosage du fluor par fusion à l'hydroxyde de sodium et détection par électrode sélective des ions fluorure
General Information
Buy Standard
Standards Content (Sample)
International
Standard
ISO 13548
First edition
Copper and zinc sulfide
2025-08
concentrates — Determination
of fluorine content by sodium
hydroxide fusion and fluoride ion
selective electrode detection
Concentrés sulfurés de cuivre et de zinc — Dosage du fluor
par fusion à l'hydroxyde de sodium et détection par électrode
sélective des ions fluorure
Reference number
© ISO 2025
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
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents . 2
6 Apparatus . 3
7 Instrument operating parameters . 4
8 Sampling and sample preparation . 4
8.1 Laboratory sample .4
8.2 Test sample .4
9 Procedure . 4
9.1 Number of determinations .4
9.2 Test portion .4
9.3 Blank test .5
9.4 Dissolution of the test portion by NaOH fusion .5
9.5 Leaching .5
9.6 Preparation of the leach solution .5
9.7 Preparation of solution for introduction to fluoride ion selective electrode.6
9.8 Preparation of the calibration solutions and stabilization solution .6
9.9 Preparation of fluorine calibration .6
9.9.1 General .6
9.9.2 Conditioning of the fluoride ion selective electrode .6
9.9.3 Potential stabilization .7
9.9.4 Temperature control .7
9.9.5 Electrode handling for concentration measurement .7
9.9.6 Procedure for reducing measurement variability.7
9.9.7 Calibration graph plotting method .7
9.10 Determination of fluorine content in the test solutions .7
10 Calculations . 7
11 Procedure for obtaining the final result . 9
12 Test report . 9
13 Precision . 9
13.1 Expression of precision .9
13.2 Procedure for obtaining the final result .10
13.3 Interlaboratory precision .10
13.4 Check of trueness .11
13.4.1 General .11
13.4.2 Type of certified reference material or reference material .11
Annex A (normative) Procedure for obtaining the final results .12
Annex B (informative) Procedure for the preparation and determination of the mass of a
predried test portion .13
Annex C (informative) Trueness test .15
Bibliography .18
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 183, Copper, lead, zinc and nickel ores and
concentrates.
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.
iv
International Standard ISO 13548:2025(en)
Copper and zinc sulfide concentrates — Determination of
fluorine content by sodium hydroxide fusion and fluoride ion
selective electrode detection
WARNING — This document can involve hazardous materials and equipment. It is the responsibility
of the user of this document to establish appropriate health and safety practices and determine the
applicability of regulatory limitations prior to use.
1 Scope
This document specifies a procedure for the determination of fluorine in copper and zinc sulfide concentrates
by sodium hydroxide fusion and fluoride ion selective electrode (FISE) detection. Fluoride ions are leached
from the sodium hydroxide fusion and presented to the FISE. Potential interfering ions are masked by the
use of a complexing agent and control of solution pH. If the aluminium content in the concentrate is up to a
mass fraction of 4,5 %, there is no effect of aluminium in this method. However, if the aluminium content in
the concentrate exceeds a mass fraction of 4,5 %, there is a possibility that it can affect the analytical results.
The method is applicable to fluorine in the following ranges:
— copper concentrates: mass fraction of 0,008 % to 0,3 %;
— zinc concentrates: mass fraction of 0,005 % to 0,1 %.
The results of the trueness test can be found in Annex C.
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 3696, Water for analytical laboratory use — Specification and test methods
ISO 9599, Copper, lead, zinc and nickel sulfide concentrates — Determination of hygroscopic moisture content of
the analysis sample — Gravimetric method
ISO 12743, Copper, lead, zinc and nickel concentrates — Sampling procedures for determination of metal and
moisture content
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
...
FINAL DRAFT
International
Standard
ISO/FDIS 13548
ISO/TC 183
Copper and zinc sulfide
Secretariat: SA
concentrates — Determination
Voting begins on:
of fluorine content by sodium
2025-06-05
hydroxide fusion and fluoride ion
Voting terminates on:
selective electrode detection
2025-07-31
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.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO
LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
Reference number
ISO/FDIS 13548:2025(en) © ISO 2025
FINAL DRAFT
ISO/FDIS 13548:2025(en)
International
Standard
ISO/FDIS 13548
ISO/TC 183
Copper and zinc sulfide
Secretariat: SA
concentrates — Determination
Voting begins on:
of fluorine content by sodium
hydroxide fusion and fluoride ion
Voting terminates on:
selective electrode detection
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 2025
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
ISO/FDIS 13548:2025(en) © ISO 2025
ii
ISO/FDIS 13548:2025(en)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents . 2
6 Apparatus . 3
7 Instrument operating parameters . 4
8 Sampling and sample preparation . 4
8.1 Laboratory sample .4
8.2 Test sample .4
9 Procedure . 4
9.1 Number of determinations .4
9.2 Test portion .4
9.3 Blank test .5
9.4 Dissolution of the test portion by NaOH fusion .5
9.5 Leaching .5
9.6 Preparation of the leach solution .5
9.7 Preparation of solution for introduction to fluoride ion selective electrode.6
9.8 Preparation of the calibration solutions and stabilization solution .6
9.9 Preparation of fluorine calibration .6
9.9.1 General .6
9.9.2 Conditioning of the fluoride ion selective electrode .6
9.9.3 Potential stabilization .7
9.9.4 Temperature control .7
9.9.5 Electrode handling for concentration measurement .7
9.9.6 Procedure for reducing measurement variability.7
9.9.7 Calibration graph plotting method .7
9.10 Determination of fluorine content in the test solutions .7
10 Calculations . 7
11 Procedure for obtaining the final result . 9
12 Test report . 9
13 Precision . 10
13.1 Expression of precision .10
13.2 Procedure for obtaining the final result .10
13.3 Interlaboratory precision .10
13.4 Check of trueness .11
13.4.1 General .11
13.4.2 Type of certified reference material or reference material .11
Annex A (normative) Procedure for obtaining the final results .13
Annex B (informative) Procedure for the preparation and determination of the mass of a
predried test portion . 14
Annex C (informative) Trueness test . 16
Bibliography . 19
iii
ISO/FDIS 13548:2025(en)
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 183, Copper, lead, zinc and nickel ores and
concentrates.
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.
iv
FINAL DRAFT International Standard ISO/FDIS 13548:2025(en)
Copper and zinc sulfide concentrates — Determination of
fluorine content by sodium hydroxide fusion and fluoride ion
selective electrode detection
WARNING — This document can involve hazardous materials and equipment. It is the responsibility
of the user of this document to establish appropriate health and safety practices and determine the
applicability of regulatory limitations prior to use.
1 Scope
This document specifies a procedure for the determination of fluorine in copper and zinc sulfide concentrates
by sodium hydroxide fusion and fluoride ion selective electrode (FISE) detection. Fluoride ions are leached
from the sodium hydroxide fusion and presented to the FISE. Potential interfering ions are masked by the
use of a complexing agent and control of solution pH. If the aluminium content in the concentrate is up to a
mass fraction of 4,5 %, there is no effect of aluminium in this method. However, if the aluminium content in
the concentrate exceeds a mass fraction of 4,5 %, there is a possibility th
...
ISO/DIS FDIS 13548:2024(en)
ISO/TC 183/WG 16
Secretariat: SA
Date: 2024-12-232025-05-22
Copper and zinc sulfide concentrates — Determination of fluorine
content by sodium hydroxide fusion and fluoride ion selective
electrode detection
DISFDIS stage
ISO/FDIS 13548:2025(en)
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
E-mail: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
ISO/FDIS 13548:2025(en)
Contents
Foreword . iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 2
6 Apparatus . 3
7 Instrument operating parameters . 4
8 Sampling and sample preparation . 4
8.1 Laboratory sample . 4
8.2 Test sample . 4
9 Procedure . 4
9.1 Number of determinations . 4
9.2 Test portion . 4
9.3 Blank test . 4
9.4 Dissolution of the test portion by NaOH fusion . 5
9.5 Leaching. 5
9.6 Preparation of the leach solution . 5
9.7 Preparation of solution for introduction to fluoride ion selective electrode . 6
9.8 Preparation of the calibration solutions and stabilization solution . 6
9.9 Preparation of fluorine calibration . 6
9.10 Determination of fluorine content in the test solutions . 7
10 Calculations . 7
11 Procedure for obtaining the final result . 9
12 Test report . 9
13 Precision . 9
13.1 Expression of precision . 9
13.2 Procedure for obtaining the final result . 9
13.3 Interlaboratory precision . 10
13.4 Check of trueness. 10
Annex A (normative) Procedure for obtaining the final results . 12
Annex B (informative) Procedure for the preparation and determination of the mass of a
predried test portion . 13
Annex C (informative) Trueness test . 15
Bibliography . 19
iii
ISO/FDIS 13548:2025(en)
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 183, Copper, lead, zinc and nickel ores and
concentrates.
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.
iv
Copper and zinc sulfide concentrates — Determination of fluorine
content by sodium hydroxide fusion and fluoride ion selective
electrode detection
WARNING — This document can involve hazardous materials and equipment. It is the responsibility
of the user of this document to establish appropriate health and safety practices and determine the
applicability of regulatory limitations prior to use.
1 Scope
This document specifies a procedure for the determination of fluorine in copper and zinc sulfide concentrates
by sodium hydroxide fusion and fluoride ion selective electrode (FISE) detection. Fluoride ions are leached
from the sodium hydroxide fusion and presented to the FISE. Potential interfering ions are masked by the use
of a complexing agent and control of solution pH. If the aluminium content in the concentrate is up to a mass
fraction of 4,5 %, there is no effect of aluminium in this method. However, if the aluminium content in the
concentrate exceeds a mass fraction of 4,5 %, there is a possibility that it can affect the analytical results.
The method is applicable to fluorine in the following ranges:
— copper concentrates: mass fraction of 0,008 % to 0,3 %;
— zinc concentrates: mass fraction of 0,005 % to 0,1 %.
The results of the trueness test can be found in Annex C.
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 3696, Water for analytical laboratory use — Specification and test methods
ISO 9599, Copper, lead, zinc and nickel sulfide concentrates — Determination of hygroscopic moisture content of
the analysis sample — Gravimetric method
ISO 12743, Copper, lead, zinc and nickel concentrates — Sampling procedures for determination of metal and
moisture content
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 is decomposed by fusion with sodium hydroxide. Fluorine is then determined by ion selective
electrode after masking of potential interfering ions by use of a complexing agent and pH control.
ISO/FDIS 13548:2025(en)
5 Reagents
During the analysis, only reagents of analytical grade and grade 2 water of ISO 3696 shall be used. Particular
care should be taken to ensure all reagents are fluorine free., except for 5.2 and the solutions in 5.10, 5.11 and
5.12.
5.1 Sodium hydroxide (NaOH) pellets, AR grade.
5.2 Sodium fluoride (NaF > 99,90 %), AR grade.
5.3 Sodium nitrate (NaNO3), AR grade.
5.4 Tri-sodium citrate dihydrate (Na C H O ·2H O).
3 6 5 7 2
5.5 Nitric acid (ρ20 = 1,38 g/ml).
5.6 200 g/l tri-sodium citrate solution.
Dissolve 200 g of tri-sodium citrate dihydrate (5.4) in 1 000 ml of water.
5.7 Nitric acid (1+1).
5.8 Nitric acid (1+99).
5.9 5 g/l sodium hydroxide solution.
Dissolve 0,5 g of sodium hydroxide (5.1) in 100 ml of water.
5.10 Working fluorine standard (1 000 mg/l).
Dissolve 2,210 × 100/A g (A is the purity of a mass fraction of NaF % (m/m)) of sodium fluoride (5.2), dried
from between 500 °C to 550 °C for 1 h by using a platinum dish (6.24), in 400 ml of water. Transfer the solution
quantitatively into a 1 000 ml plastic volumetric flask (6.8). Dilute to volume with water. Store in a labelled
plastic bottle.
Alternatively, purchase a suitable high-quality prepared standard.
NOTE There are reference solutions with metrological traceability secured.
5.11 Working fluorine standard solution A (100 mg/l).
Pipette 10,0 ml of 1 000 mg/l fluorine standard solution (5.10) into a 100 ml plastic volumetric flask (6.8).
Dilute to volume with water. Store in a labelled plastic bottle.
Alternatively, purchase a suitable high-quality prepared standard.
NOTE There are reference solutions with metrological traceability secured.
5.12 Working fluorine standard solution B (10 mg/l).
Pipette 10,0 ml of 100 mg/l fluorine standard solution (5.11) into a 100 ml plastic volumetric flask (6.8). Dilute
to volume with water. Store in a labelled plastic bottle.
Alternatively, purchase a suitable high-quality prepared standard.
NOTE There are reference solutions with metrological traceability secured.
ISO/FDIS 13548:2025(en)
6 Apparatus
All laboratory glassware and equipment shall be shown to be free of fluorine contamination.
6.1 Balance, accurate and readable to ± 0,000 1 g.
6.2 Top loading balance, accurate and readable to ± 0,001 g.
6.3 Meker burner.
6.4 Muffle furnace, with temperature controller.
6.5 Laboratory hot plate, with temperature controller.
6.6 Laboratory timer.
6.7 Polypropylene or polytetrafluoroethylene beakers, 50 ml, 100 ml, 250 ml, 500 ml and
1 000 ml.
6.8 Polypropylene volumetric flasks, 100 ml and 1 000 ml.
6.9 Plastic funnels.
6.10 Watch glasses.
6.11 Plastic volumetric pipette.
6.12 Filter paper, with an ash content of a mass fraction of 0.,06 % or less and a nominal particle retention
of about 8 µm.
6.13 Adjustable micro pipette.
6.14 Reagent dispensers.
6.15 Nickel or zirconium crucibles, 30 ml to 50 ml, with covers.
6.16 pH meter and electrode.
6.17 Combined ion selective fluoride electrode or single ion selective fluoride electrode and
reference electrode.
6.18 Temperature sensor.
6.19 mV meter or ion meter which allows direct readings in concentration.
6.20 M
...
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