ISO/DTS 4177

Magnesium and magnesium alloys - Determination of chromium - 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
• Current Stage: 5098 - Project deleted
• Start Date: 02-Nov-2023
• Completion Date: 13-Dec-2025

Overview

ISO/DTS 4177:2023 specifies a precision analytical method for the determination of chromium content in magnesium and magnesium alloys using Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). This draft technical specification addresses the need for accurate, reliable testing of chromium concentrations ranging from 0.001% to 0.050% by mass fraction in these lightweight metal materials. Magnesium alloys are widely valued in various industries due to their low density, high stiffness, and machinability, but controlling the chromium content is critical due to its environmental and health hazards.

This ICP-OES method is tailored especially for alloys containing specific limitations of cerium, gadolinium, neodymium, and manganese. It provides guidance on sample preparation, instrument calibration, detection limits, and measurement procedures, helping laboratories to ensure compliance with international safety and quality standards.

Key Topics

• Scope and Application: The method applies to magnesium alloys with specific element content thresholds and targets the determination of low-level chromium content (0.0010% to 0.050% mass fraction).
• Analytical Principle: Chromium in the sample is dissolved using nitric and hydrochloric acid, then nebulized into an ICP optical emission spectrometer where chromium concentration is quantified by measuring emitted light intensity at selected wavelengths.
• Calibration and Sensitivity: Calibration solutions prepared with pure magnesium and chromium standards enable accurate measurement. The recommended wavelength, Cr 267.716 nm, optimizes sensitivity with minimal interference.
• Detection Limits: The method requires a limit of detection of ≤ 0.005 μg/ml, ensuring detection of trace chromium levels necessary for regulatory compliance.
• Sample Preparation: Emphasizes careful sampling and preparation, including cleaning oily or greasy samples, to prevent contamination. Samples should be finely milled or chipped for best results.
• Reagents and Apparatus: Calls for high-grade reagents including ultrapure water, acids, and certified chromium standards, along with class A volumetric glassware to ensure precision and accuracy in measurements.
• Precision and Reporting: Detailed specifications on the expression of results, including calculation methods and test report requirements, ensure consistent and reliable data across laboratories.

Applications

• Quality Control in Magnesium Alloy Production: Assess chromium levels in raw materials and finished products to maintain quality and ensure compliance with industry standards.
• Regulatory Compliance for Safety: Support testing for hazardous metal content in magnesium alloys, especially for applications in food, medical, and environmental sectors where low chromium content is mandatory.
• Research and Development: Enable metallurgical researchers and material scientists to precisely characterize magnesium alloy compositions and improve formulations by controlling chromium additions.
• Environmental Monitoring: Assist in monitoring chromium contamination risks associated with magnesium alloy manufacturing and processing.

This ICP-OES method enhances the accuracy and reliability of chromium testing, which is vital for maintaining magnesium alloy safety, performance, and environmental standards.

Related Standards

• ISO 8287 – Limits sum of cadmium, mercury, arsenic, and chromium in magnesium alloys
• ISO 3696 – Water for analytical laboratory use specifications, ensuring reagent purity
• ISO 648 & ISO 1042 – Standards for laboratory volumetric glassware ensuring measurement precision
• Other ISO standards related to light metals and their alloys developed by ISO/TC 79/SC 5

Using ISO/DTS 4177 in conjunction with these related standards strengthens quality management systems for metal alloy analysis and supports international harmonization in material testing.

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Keywords: ISO DTS 4177, magnesium alloys, chromium determination, ICP-OES method, inductively coupled plasma optical emission spectrometry, chromium testing, magnesium alloy analysis, heavy metal control, analytical method, metal alloy standards.

Standards Content (Sample)

FINAL
TECHNICAL ISO/DTS
DRAFT
SPECIFICATION 4177
ISO/TC 79/SC 5
Magnesium and magnesium alloys —
Secretariat: SAC
Determination of chromium —
Voting begins on:
2023-07-24 Inductively coupled plasma optical
emission spectrometric method
Voting terminates on:
2023-09-18
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 4177
ISO/TC 79/SC 5
Magnesium and magnesium alloys —
Secretariat: SAC
Determination of chromium —
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
6.1 Inductively coupled plasma optical emission spectrometer . 2
6.1.1 General . 2
6.1.2 Wavelength . 2
6.1.3 Limit of detection . 3
6.1.4 Linearity of the calibration curve . 3
7 Sampling and sample preparation . 3
8 Procedure .3
8.1 General . 3
8.2 Test sample . 3
8.3 Preparation of the test solution . 3
8.4 Preparation of the calibration solutions . 3
8.5 Adjustment of the apparatus . 4
8.6 Measurement of the calibration solutions . 4
8.7 Calibration curve . 4
8.8 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 the light metallic materials and show several
advantageous properties, such as such as low density, high specific stiffness and strength, good damping
capacity, castability, weldability and machinability, etc. Chromium, as one of the hazardous elements,
has negative effects on the environment and health, so its content needs to be strictly controlled within
a certain low content. The sum of the mass contents of cadmium (Cd), mercury (Hg), arsenic (As) and
chromium (Cr) given in ISO 8287 is defined to be less than 0,01 % in magnesium and its alloys, which
needs be inspected if used in food and medicine fields.
v
TECHNICAL SPECIFICATION ISO/DTS 4177:2023(E)
Magnesium and magnesium alloys — Determination of
chromium — Inductively coupled plasma optical emission
spectrometric method
1 Scope
This document specifies an inductively coupled plasma optical emission spectrometric method (ICP-
OES) for the determination of chromium contents between 0,001 0 % (mass fraction) and 0,050 %
(mass fraction) in magnesium and magnesium alloys.
The method is limited to magnesium alloys containing less than 1,0 % (mass fraction) of cerium,
3,2 % (mass fraction) of gadolinium, 0,2 % (mass fraction) of neodymium and 1,6 % (mass fraction) of
manganese.
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
...

ISO TC 79/SC 5
Date: 2023-05
ISO/TC 79/SC 5
Secretariat: SAC
Date: 2023-07-10
Magnesium and magnesium alloys – — Determination of
chromium –— Inductively coupled plasma optical emission
spectrometric method
Magnésium et alliages de magnésium - Détermination de l' chrome - Méthode par
spectrométrie d'émission atomique avec source à plasma induit

©ISO 2018 - All rights reserved i

FDIS stage
©ISO 2018 - All rights reserved 2

ISO/DIS 4177:20XX(E)
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
©ISO 2018 - All rights reserved iii

Contents
Foreword . viii
Introduction . ix
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 1
6 Apparatus . 2
6.1 Inductively coupled plasma optical emission spectrometer . 2
6.1.1 General . 2
6.1.2 Wavelength . 2
6.1.3 Limit of detection . 3
6.1.4 Linearity of the calibration curve . 3
7 Sampling and sample preparation . 3
8 Procedure . 3
8.1 General . 3
8.2 Test sample . 3
8.3 Preparation of the test solution . 3
8.4 Preparation of the calibration solutions. 3
8.5 Adjustment of the apparatus . 4
8.6 Measurement of the calibration solutions . 4
8.7 Calibration curve . 4
8.8 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
©ISO 2018 - All rights reserved iv

ISO/DIS 4177:20XX(E)
Bibliography . 10

©ISO 2018 - All rights reserved v

Foreword iv
Introduction vi
1 Scope １
2 Normative references １
3 Terms and definitions １
4 Principle １
5 Reagents ２
6 Apparatus ２
6.1  Inductively coupled plasma optical emission spectrometer. ２
6.1.1 General ２
6.1.2 Wavelength ３
6.1.3 Limit of detection ３
6.1.4 Linearity of the calibration curve ３
7 Sampling and sample preparation ３
8 Procedure ３
8.1 General ３
8.2 Test sample ４
8.3 Preparation of the test solution ４
8.4 Preparation of the calibration solutions ４
8.5 Adjustment of the apparatus ４
8.6 Measurement of the calibration solutions ５
8.7 Calibration curve ５
8.8 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)  Limit of detection ７
Annex B (informative)  Information on the precision test ８
Annex C (informative)  Graphical representation of precision data ９
©ISO 2018 - All rights reserved vi

ISO/DIS 4177:20XX(E)
Bibliography １０
©ISO 2018 - All rights reserved vii

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.html.
Field Code Changed
©ISO 2018 - All rights reserved viii

ISO/DIS 4177:20XX(E)
Introduction
Magnesium and magnesium alloys are one kind of the light metallic materials and show several
advantageous properties, such as such as low density, high specific stiffness and strength, good damping
capacity, castability, weldability and machinability, etc. Chromium, as one of the hazardous elements will
have bad, has negative effects on the environment and the health, so its content mustneeds to be strictly
controlled within a certain low contentscontent. The sum of the mass contents of cadmium (Cd), mercury
(Hg), arsenic (As) and chromium (Cr) given in ISO 8287 is defined to be less than 0,01 % in magnesium
and its alloys, which mustneeds be inspected if used in food and medicine fields.
©ISO 2018 - All rights reserved ix

ISO/DISDTS 4177:2021(:(E)
x ©ISO 201©8 -IS AOll r 20ig2h3t s r– Aellse rrivgehdts r eserved x

Magnesium and magnesium alloys – — Determination of chromium
–— Inductively coupled plasma optical emission spectrometric
method
1 Scope
This document specifies an inductively coupled plasma optical emission spectrometric method (ICP-OES)
for the determination of chromium contents between 0,001 0 % (mass fraction) and 0,050 % (mass
fraction) in magnesium and magnesium alloys.
The method is limited to magnesium alloys containing less than 1,0 % (mass fraction) of cerium, 3,2 %
(mass fraction) of gadolinium, 0,2 % (mass fraction) of neodymium and 1,6 % (mass fraction) of
manganese.
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 sample with nitric acid and hydrochloric acid, the solution is nebulized into an
inductively coupled plasma optical emission spectrometer and the intensity of the chromium emitted
light is measured. The concentrations of chromium in the test solutions are derived from a magnesium -
based calibration curve.
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 magnes
...