ISO/DTS 4189

Magnesium and magnesium alloys — Determination of sodium — Inductively coupled plasma optical emission spectrometric method

Titre manque

General Information

• Status: Not Published
• ICS: 77.120.20 - Magnesium and magnesium alloys
• Technical Committee: ISO/TC 79/SC 5 - Magnesium and alloys of cast or wrought magnesium
• Drafting Committee: ISO/TC 79/SC 5/WG 4 - Analysis of magnesium and magnesium alloys

Standards Content (Sample)

FINAL
TECHNICAL ISO/DTS
DRAFT
SPECIFICATION 4189
ISO/TC 79/SC 5
Magnesium and magnesium
Secretariat: SAC
alloys — Determination of sodium —
Voting begins on:
2023-07-31 Inductively coupled plasma optical
emission spectrometric method
Voting terminates on:
2023-09-25
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
Reference number
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. © ISO 2023

FINAL
TECHNICAL ISO/DTS
DRAFT
SPECIFICATION 4189
ISO/TC 79/SC 5
Magnesium and magnesium
Secretariat: SAC
alloys — Determination of sodium —
Voting begins on:
Inductively coupled plasma optical
emission spectrometric method
Voting terminates on:
© ISO 2023
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.
RECIPIENTS OF THIS DRAFT ARE INVITED TO
ISO copyright office
SUBMIT, WITH THEIR COMMENTS, NOTIFICATION
OF ANY RELEVANT PATENT RIGHTS OF WHICH
CP 401 • Ch. de Blandonnet 8
THEY ARE AWARE AND TO PROVIDE SUPPOR TING
CH-1214 Vernier, Geneva
DOCUMENTATION.
Phone: [phone]
IN ADDITION TO THEIR EVALUATION AS
Reference number
Email: [e-mail]
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO­
Website: www.iso.org
LOGICAL, COMMERCIAL AND USER PURPOSES,
DRAFT INTERNATIONAL STANDARDS MAY ON
Published in Switzerland
OCCASION HAVE TO BE CONSIDERED IN THE
LIGHT OF THEIR POTENTIAL TO BECOME STAN­
DARDS TO WHICH REFERENCE MAY BE MADE IN
ii
NATIONAL REGULATIONS. © ISO 2023

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 1
6 Apparatus . 2
7 Sampling and sample preparation . 3
8 Procedure .3
8.1 General . 3
8.2 Test portion . 3
8.3 Determination . 3
8.3.1 Preparation of the test solution . 3
8.3.2 Preparation of the calibration solutions . 3
8.4 Adjustment of the apparatus . 4
8.5 Measurement of the calibration solutions . 4
8.6 Calibration curve . 4
8.7 Measurements of the test solution . 4
9 Expression of results . 4
9.1 Method of calculation . 4
9.2 Precision . . . 5
10 Test report . 5
Annex A (normative) Limit of detection .6
Annex B (informative) Information on the precision test . 7
Annex C (informative) Graphical representation of precision data . 8
Bibliography . 9
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 non­governmental, 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 79, Light metals and their alloys,
Subcommittee SC 5, Magnesium and alloys of cast or wrought magnesium.
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
Introduction
Magnesium and magnesium alloys are one kind of light metallic materials and show several
advantageous properties such as low density, high specific stiffness and strength, good damping
capacity, castability, weldability and machinability, etc. Sodium, as one of the hazardous impurities,
creates hot brittleness of magnesium and magnesium alloys, thereby producing cracks during forging
and rolling. Sodium content should be controlled and monitored in order to check if its content remains
at trace level. In ISO 8287, sodium contents are specified to be less than 0,001 % or less than 0,01 %.
v
TECHNICAL SPECIFICATION ISO/DTS 4189:2023(E)
Magnesium and magnesium alloys — Determination of
sodium — Inductively coupled plasma optical emission
spectrometric method
1 Scope
This document specifies an inductively coupled plasma atomic emission spectrometric method for the
determination of sodium contents between 0,002 % (mass fraction) and 0,050 % (mass fraction) in
magnesium and magnesium alloys.
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 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
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
After dissolution of a test portion with nitric acid and hydrochloric acid, the solution is nebulized into
an inductively coupled plasma optical emission spectrometer and the intensity of the emitted light from
sodium is measured. The concentrations of sodium in the test solutions are derived from magnesium­
based calibration curves.
5 Reagents
During the analysis, use only reagents of recognized analytical grade and only grade 2 water as
specified in ISO 3696, or water of equivalent purity.
5.1 Pure magnesium, purity ≥99,99 % (mass fraction), free from sodium.
5.2 Sodium chloride, purity ≥99,99 % (mass fraction).
5.3 Hydrochloric acid, ρ about 1,19 g/ml.
5.4 Nitric acid, ρ about 1,42 g/ml.
5.5 Hydrochloric acid solution 1 + 1.
Add 500 ml of hydrochloric acid (5.3) to 500 ml of water and mix.
5.6 Nitric acid solution 1 + 1.
Add 500 ml of nitric acid (5.4) to 500 ml of water and mix.
5.7 Sodium standard solution (1 g/l).
Weigh, to the nearest 1 mg, 2,543 0 g of sodium chloride (5.2) previously calcined at a temperature
between 500 °C and 600 °C to constant mass, and transfer into a 500 ml glass beaker.
Add 60 ml of water and, if necessary, heat gently to complete the dissolution.
Allow to cool and transfer the solution quantitatively into a 1 000 ml one-mark volumetric flask. Dilute
to the mark with water and mix.
1 ml of this solution contains 1,0 mg of sodium.
Store the solution in a polyethylene bottle.
5.8 Sodium standard solution (0,1 g/l).
Transfer 10,00 ml of sodium standard solution (5.7) into a 100 ml volumetric flask, add 10 ml nitric acid
solution (5.6), dilute to the mark with water, and mix well.
1 ml of this solution contains 0,1 mg of sodium.
5.9 Sodium standard solution (0,01 g/l).
Transfer 10,00 ml of sodium standard solution (5.8) into a 100 ml volumetric flask, add 10 ml nitric acid
solution (5.6), dilute to the mark with water, and mix well.
1 ml of this solution contains 0,01 mg of sodium.
6 Apparatus
All volumetric glassware shall be class A and calibrated in accordance with ISO 648 or ISO 1042, as
appropriate.
6.1 Inductively coupled plasma optical emission spectrometry (ICP-OES)
6.1.1 General
The instrument used first shall be optimized in accordance with the manufacturer’s instructi
...

ISO/TC 79/SC 5
Date:2023-05
ISO/TC 79/SC 5
Secretariat: SAC
Date: 2023-07-17
Magnesium and magnesium alloys -- — Determination of sodium -
-— Inductively coupled plasma optical emission spectrometric
method
Magnésiumetalliages de magnésium - Détermination du sodium - Méthode par
spectrométried'émissionatomique avec source à plasma induit
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
E-mail: [e-mail]
Website: www.iso.org
Published in Switzerland
Contents
Foreword . vi
Introduction .vi i
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 1
6 Apparatus . 2
7 Sampling and sample preparation . 3
8 Procedure . 3
8.1 General . 3
8.2 Test portion . 3
8.3 Determination . 3
8.3.1 Preparation of the test solution . 3
8.3.2 Preparation of the calibration solutions . 3
8.4 Adjustment of the apparatus . 4
8.5 Measurement of the calibration solutions . 4
8.6 Calibration curve . 4
8.7 Measurements of the test solution . 4
9 Expression of results . 4
9.1 Method of calculation . 4
9.2 Precision . 5
10 Test report . 5
Annex A (normative) Limit of detection . 6
Annex B (informative) Information on the precision test . 8
Annex C (informative) Graphical representation of precision data . 9
Bibliography . 12

Foreword iii
Introduction iv
1 Scope 1
2 Normative references 1
3 Terms and definitions 1
4 Principle 1
iv
5 Reagents 1
6 Apparatus 2
7 Sampling and sample preparation 3
8 Procedure 3
8.1 General 3
8.2 Test portion 3
8.3 Determination 4
8.4 Adjustment of the apparatus 4
8.5 Measurement of the calibration solutions 5
8.6 Calibration curve 5
8.7 Measurements of the test solution 5
9 Expression of results 5
9.1 Method of calculation 5
9.2 Precision 5
10 Test report 6
Annex A  (normative) Detection limit 7
Annex B (informative) Information on the precision test 8
Annex C (informative) Graphical representation of precision data 9
Bibliography 错误！未定义书签。0
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 documentsdocument 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).
Field Code Changed
Attention is drawnISO draws attention to the possibility that some of the elementsimplementation of this
document may beinvolve the subjectuse 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. Details of any patent rights identified during the
development of the document will be in the Introduction and/or on the ISO list of patent declarations
received (see www.iso.org/patents).
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’sISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see
www.iso.org/iso/foreword.html), see www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 79, Light metals and their alloys,
Subcommittee SC 5, Magnesium and alloys of cast or wrought magnesium.
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.htmlwww.iso.org/members.html.
vi
Introduction
Magnesium and magnesium alloys are one kind of light metallic materials and show several advantageous
properties such as low density, high specific stiffness and strength, good damping capacity, castability,
weldability and machinability, etc. Sodium is, as one of the hazardous impurities leading to, creates hot
brittleness of magnesium and magnesium alloys, thereby producing crackcracks during forging and
rolling,. Sodium content should be controlled and monitored in order to check if its content remains at
trace level. In ISO 8287:2021, sodium contents are specified to be less than 0,001 % or less than 0,01 %.

Magnesium and magnesium alloys -- — Determination of sodium --
— Inductively coupled plasma optical emission spectrometric
method
1 Scope
This document specifies an inductively coupled plasma atomic emission spectrometric method (ICP-OES)
for the determination of sodium contents between 0,00 2002 % (mass fraction) and 0,050 % (mass
fraction) in magnesium and magnesium alloys.
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 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
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminologicalterminology databases for use in standardization at the following
addresses:
— — ISO Online browsing platform: available at https://www.iso.org/obphttps://www.iso.org/obp
— — IEC Electropedia: available at http://www.electropedia.org/https://www.electropedia.org/
4 Principle
After dissolution of a test portion with nitric acid and hydrochloric acid, the solution is nebulized into an
inductively coupled plasma optical emission spectrometry (ICP-OES)spectrometer and the intensity of
the sodium emitted light from sodium is measured. The concentrations of sodium in the test solutions
are derived from magnesium -based calibration curves.
5 Reagents
During the analysis, use only reagents of recognized analytical grade and only grade 2 water as specified
in ISO 3696, or water of equivalent purity.
5.1 Pure magnesium, purity ≥99,99 % (mass fraction), free from sodium.
5.2 Sodium chloride, purity ≥99,99 % (mass fraction).
5.3 Hydrochloric acid, ρ about 1,19g19 g/ml.
5.4 Nitric acid, ρ about 1,42 g/ml.
5.5 Hydrochloric acid solution 1 + 1.
Add 500 ml of hydrochloric acid (5.3)(5.3) to 500 ml of water and mix.
5.6 Nitric acid solution 1 + 1.
Add 500 ml of nitric acid (5.4)(5.4) to 500 ml of water and mix.
5.7 Sodium standard solution (1 g / /l)).
Weigh, to the nearest 1 mg, 2,543 0 g of sodium chloride (5.2)(5.2) previously calcined at a temperature
between 500 °C and 600 °C to constant mass, and transfer into a 500 ml glass beaker.
Add 60 ml of water and, if necessary, heat gently to complete the dissolution.
Allow to cool and transfer the solution quantitatively into a 10001 000 ml one-mark volumetric flask.
Dilute to the mark with water and mix.
1 ml of this solution contains 1,0 mg of sodium.
Store the solution in a polyethylene bottle.
5.8 Sodium standard solution (0.,1 g / /l)).
Transfer 10,00 ml of sodium standard solution (5.7)(5.7) into a 100 ml volumetric flask, add 10 ml nitric
acid solution(5.6), (5.6), dilute to the mark with water, and mix well.
1 ml of this solution contains 0,1 mg of sodium.
5.9 Sodium standard solution (0.,01 g / /l)).
Transfer 10,00 ml of sodium standard solution (5.8)(5.8) into a 100 ml volumetric flask, add 10 ml nitric
acid solution (5.6),(5.6), dilute to the mark with water, and mix well.
1 ml of this solution contains 0,01 mg of sodium.
6 Apparatus
All volumetric glassware shall be class A and calibrated in accordance with ISO 648 or ISO 1042, as
appropriate.
6.1 Inductively coupled plasma optical emission spectrometry. (ICP-OES)
6.1.1 General
The instrument used first shall be optimized in accordance with the manufacturer’s instructions and then
shall meet the performance criteria given in 6.1.3 to 6.1.4.6.1.3 to 6.1.4.
6.1.2 Wavelengths
This method does not specify any particular wavelength. Each laboratory shall carefully investigate
investigates the wavelengths available on its own equipment to find the most suitable ones regarding the
sensitivity and the absence of interferences.
In Table1, howeve
...