Plastics — Polyethylene (PE) and polypropylene (PP) thermoplastics — Determination of metal content by ICP-OES

This document specifies a method for the determination of metal content in polyethylene (PE) and polypropylene (PP) by inductively coupled plasma optical emission spectrometry (ICP-OES). This document is applicable to the determination of the content of magnesium (Mg), aluminium (Al), calcium (Ca), zinc (Zn), chromium (Cr), titanium (Ti), iron (Fe), antimony (Sb), copper (Cu), lead (Pb), cadmium (Cd), etc. This document is not applicable to the determination of mercury (Hg) due to its volatility. This method is suitable for base polymers of PE, PP, PE/PP copolymer and their blends.

Plastiques — Polyéthylène (PE) et polypropylène (PP) — Détermination de la teneur en métal par ICP-OES

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Status
Published
Publication Date
16-Feb-2021
Current Stage
6060 - International Standard published
Start Date
17-Feb-2021
Completion Date
17-Feb-2021
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INTERNATIONAL ISO
STANDARD 24047
First edition
2021-02
Plastics — Polyethylene (PE) and
polypropylene (PP) thermoplastics
— Determination of metal content by
ICP-OES
Plastiques — Polyéthylène (PE) et polypropylène (PP) —
Détermination de la teneur en métal par ICP-OES
Reference number
ISO 24047:2021(E)
ISO 2021
---------------------- Page: 1 ----------------------
ISO 24047:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

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 © ISO 2021 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 24047:2021(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 1

5 Reagents ........................................................................................................................................................................................................................ 2

6 Apparatus ..................................................................................................................................................................................................................... 2

7 Sample preparation ........................................................................................................................................................................................... 2

7.1 Cleaning glassware .............................................................................................................................................................................. 2

7.2 Preparation of working standard solutions ................................................................................................................... 3

7.3 Preparation of test solution ......................................................................................................................................................... 3

8 Procedure..................................................................................................................................................................................................................... 3

8.1 Instrument set up ................................................................................................................................................................................. 3

8.2 Preparation of calibration curve .............................................................................................................................................. 3

8.3 Sample analysis ...................................................................................................................................................................................... 4

9 Expression of results ........................................................................................................................................................................................ 5

10 Precision ....................................................................................................................................................................................................................... 5

11 Test report ................................................................................................................................................................................................................... 5

Annex A (informative) Summary of precision data ............................................................................................................................... 6

Bibliography ................................................................................................................................................................................................................................ 9

© ISO 2021 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 24047:2021(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 electro

technical 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 documents 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).

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. 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'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 61, Plastics, Subcommittee SC 9,

Thermoplastic materials.

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 © ISO 2021 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 24047:2021(E)
Introduction

Metal elements in polyethylene (PE) and polypropylene (PP) can lead to increased ash content and can

impact material mechanical properties. In addition, some elements are also environmentally hazardous.

This document provides a method to determine the metal content in PE and PP and it can serve as a

measure for additive monitoring, quality control and post-reactor studies.

In this document, inductively coupled plasma optical emission spectrometry (ICP-OES) is used to

determine the concentrations of certain elements in PE and PP. The main advantages of ICP-OES over

atomic absorption spectroscopy (AAS) include multi-element measurement capability, longer linear

dynamic range and less condensed phase interferences.
© ISO 2021 – All rights reserved v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 24047:2021(E)
Plastics — Polyethylene (PE) and polypropylene (PP)
thermoplastics — Determination of metal content by ICP-
OES

WARNING — Persons using this document should be familiar with normal laboratory practice,

if applicable. This document does not purport to address all of the safety concerns, if any,

associated with its use. It is the responsibility of the user to establish appropriate safety and

health practices.
1 Scope

This document specifies a method for the determination of metal content in polyethylene (PE) and

polypropylene (PP) by inductively coupled plasma optical emission spectrometry (ICP-OES).

This document is applicable to the determination of the content of magnesium (Mg), aluminium (Al),

calcium (Ca), zinc (Zn), chromium (Cr), titanium (Ti), iron (Fe), antimony (Sb), copper (Cu), lead (Pb),

cadmium (Cd), etc. This document is not applicable to the determination of mercury (Hg) due to its

volatility.

This method is suitable for base polymers of PE, PP, PE/PP copolymer and their blends.

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 3451-1, Plastics — Determination of ash — Part 1: General methods
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
4 Principle

PE and PP samples are incinerated and digested. Metal elements within are dissolved in aqueous solution.

The solution is converted into aerosol via a nebulizer, and then injected into argon supported ICP-OES.

At high temperature, the plasma atomizes metal elements in the solution and gives characteristic

optical emission. The intensity of emission is proportional to the concentration of element. The content

of metal elements in the sample is then calculated
...

FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 24047
ISO/TC 61/SC 9
Plastics — Polyethylene (PE) and
Secretariat: KATS
polypropylene (PP) thermoplastics
Voting begins on:
2020­11­23 — Determination of metal content by
ICP-OES
Voting terminates on:
2021­01­18
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
ISO/FDIS 24047:2020(E)
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 2020
---------------------- Page: 1 ----------------------
ISO/FDIS 24047:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020

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
CH­1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 2 ----------------------
ISO/FDIS 24047:2020(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 1

5 Reagents ........................................................................................................................................................................................................................ 2

6 Apparatus ..................................................................................................................................................................................................................... 2

7 Sample preparation ........................................................................................................................................................................................... 2

7.1 Cleaning glassware .............................................................................................................................................................................. 2

7.2 Preparation of working standard solutions ................................................................................................................... 3

7.3 Preparation of test solution ......................................................................................................................................................... 3

8 Procedure..................................................................................................................................................................................................................... 3

8.1 Instrument set up ................................................................................................................................................................................. 3

8.2 Preparation of calibration curve .............................................................................................................................................. 3

8.3 Sample analysis ...................................................................................................................................................................................... 4

9 Expression of results ........................................................................................................................................................................................ 5

10 Precision ....................................................................................................................................................................................................................... 5

11 Test report ................................................................................................................................................................................................................... 5

Annex A (informative) Summary of precision data ............................................................................................................................... 6

Bibliography ................................................................................................................................................................................................................................ 9

© ISO 2020 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO/FDIS 24047:2020(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 non­governmental, in liaison with ISO, also take part in the work. ISO

collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electro

technical 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 documents 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).

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. 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'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 61, Plastics, Subcommittee SC 9,

Thermoplastic materials.

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 © ISO 2020 – All rights reserved
---------------------- Page: 4 ----------------------
ISO/FDIS 24047:2020(E)
Introduction

Metal elements in polyethylene (PE) and polypropylene (PP) can lead to increased ash content and can

impact material mechanical properties. In addition, some elements are also environmentally hazardous.

This document provides a method to determine the metal content in PE and PP and it can serve as a

measure for additive monitoring, quality control and post-reactor studies.

In this document, inductively coupled plasma optical emission spectrometry (ICP-OES) is used to

determine the concentrations of certain elements in PE and PP. The main advantages of ICP­OES over

atomic absorption spectroscopy (AAS) include multi-element measurement capability, longer linear

dynamic range and less condensed phase interferences.
© ISO 2020 – All rights reserved v
---------------------- Page: 5 ----------------------
FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 24047:2020(E)
Plastics — Polyethylene (PE) and polypropylene (PP)
thermoplastics — Determination of metal content by ICP-
OES

WARNING — Persons using this document should be familiar with normal laboratory practice,

if applicable. This document does not purport to address all of the safety concerns, if any,

associated with its use. It is the responsibility of the user to establish appropriate safety and

health practices.
1 Scope

This document specifies a method for the determination of metal content in polyethylene (PE) and

polypropylene (PP) by inductively coupled plasma optical emission spectrometry (ICP-OES).

This document is applicable to the determination of the content of magnesium (Mg), aluminium (Al),

calcium (Ca), zinc (Zn), chromium (Cr), titanium (Ti), iron (Fe), antimony (Sb), copper (Cu), lead (Pb),

cadmium (Cd), etc. This document is not applicable to the determination of mercury (Hg) due to its

volatility.

This method is suitable for base polymers of PE, PP, PE/PP copolymer and their blends.

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 3451­1, Plastics — Determination of ash — Part 1: General methods
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
4 Principle

PE and PP samples are incinerated and digested. Metal elements within are dissolved in aqueous solution.

The solution is converted into aerosol via a nebulizer, and then injected into argon supported ICP-OES.

At high temperatu
...

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