Plastics — Polypropylene (PP) — Determination of isotactic index by low-resolution nuclear magnetic resonance spectrometry

This document specifies a relative method for the determination of polypropylene (PP) isotactic index by low-resolution pulsed nuclear magnetic resonance spectroscopy (LR-NMR). This method enables the identification and coding of types H propylene (PP-H) plastics according to ISO 19069‑1. This method is suitable for base polymers and is not applicable for mixtures. NOTE The direct method for the determination of polypropylene isotactic index is specified in ISO 9113.

Plastiques — Polypropylène (PP) — Détermination de l'indice isotactique par spectrométrie de résonance magnétique nucléaire à basse résolution

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Status
Published
Publication Date
31-Jan-2021
Current Stage
6060 - International Standard published
Start Date
01-Feb-2021
Completion Date
01-Feb-2021
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INTERNATIONAL ISO
STANDARD 24076
First edition
2021-02
Plastics — Polypropylene (PP) —
Determination of isotactic index by
low-resolution nuclear magnetic
resonance spectrometry
Plastiques — Polypropylène (PP) — Détermination de l'indice
isotactique par spectrométrie de résonance magnétique nucléaire à
basse résolution
Reference number
ISO 24076:2021(E)
ISO 2021
---------------------- Page: 1 ----------------------
ISO 24076:2021(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 24076:2021(E)
Contents Page

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

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

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

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

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

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

5 Apparatus ..................................................................................................................................................................................................................... 2

6 Preparation of sample .................................................................................................................................................................................... 2

6.1 General ........................................................................................................................................................................................................... 2

6.2 Reference samples ............................................................................................................................................................................... 2

7 Method A — Ratio method ......................................................................................................................................................................... 2

7.1 Procedure .................................................................................................................................................................................................... 2

7.1.1 Measurement of reference samples by n-heptane extraction .................................................. 2

7.1.2 LR-NMR measurement procedure of reference samples .............................................................. 3

7.1.3 LR-NMR measurement procedure of test samples ............................................................................. 3

7.2 Calculation .................................................................................................................................................................................................. 3

7.2.1 Calibration curve ............................................................................................................................................................. 3

7.2.2 Calculation of isotactic index II ........................................................................................................................

na 4

8 Method B — Absolute method ................................................................................................................................................................ 4

8.1 Procedure .................................................................................................................................................................................................... 4

8.1.1 Measurement of reference samples by n-heptane extraction .................................................. 4

8.1.2 LR-NMR measurement procedure of reference samples .............................................................. 4

8.1.3 LR-NMR measurement procedure of test samples ............................................................................. 4

8.2 Calculation .................................................................................................................................................................................................. 4

8.2.1 Calibration curve ............................................................................................................................................................. 4

8.2.2 Calculation of isotactic index II ........................................................................................................................

nb 5

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

10 Test report ................................................................................................................................................................................................................... 5

Annex A (informative) Example of a calibration curve for method A ................................................................................. 7

Annex B (informative) Example of a calibration curve for method B ................................................................................. 8

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

© ISO 2021 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 24076:2021(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

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 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 24076:2021(E)
Introduction

The LR-NMR method in this document is a relative method established with ISO 9113 as the absolute

method. The method and concept of isotactic index of polypropylene are specified in ISO 9113, that is,

the polypropylene sample is separated into the extractable and the unextractable matter by n-heptane

extraction, and the percentage of unextractable matter in the sample is calculated as isotactic index.

Isotactic index in ISO 9113 sounds similar to tacticity (isotacticity or stereotacticity) of polymer chain,

but the concept and result are different. The result is related to but not equal to the tacticity (isotacticity

or stereotacticity) of molecular chain, which can be determined by high resolution carbon-13 nuclear

magnetic resonance and infrared method. The result of ISO 9113 is also related to crystallization,

molecular weight, chain entanglement of the sample, solvent solubility and other effects.

For solid polymers, extraction always takes a long time for the diffusion of long molecular chain from

polymer to solvent. To improve test efficiency, relative methods are developed. This document provides

a relative non-destructive method for the determination of isotactic index by low-resolution nuclear

magnetic resonance spectrometry through a calibration curve establishing with magnetic signal and

isotactic index determined by ISO 9113. No solvent is used, and the determination efficiency is improved

during samples measurement procedure except for the calibration part.
© ISO 2021 – All rights reserved v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 24076:2021(E)
Plastics — Polypropylene (PP) — Determination of
isotactic index by low-resolution nuclear magnetic
resonance spectrometry
1 Scope

This document specifies a relative method for the determination of polypropylene (PP) isotactic index

by low-resolution pulsed nuclear magnetic resonance spectroscopy (LR-NMR).

This method enables the identification and coding of types H propylene (PP-H) plastics according to

ISO 19069-1.
This method is suitable for base polymers and is not applicable for mixtures.

NOTE The direct method for the determination of polypropylene isotactic index is specified in ISO 9113.

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 a
...

FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 24076
ISO/TC 61/SC 9
Plastics — Polypropylene (PP) —
Secretariat: KATS
Determination of isotactic index by
Voting begins on:
2020­11­03 low-resolution nuclear magnetic
resonance spectrometry
Voting terminates on:
2020­12­29
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 24076:2020(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 24076:2020(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 24076:2020(E)
Contents Page

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

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

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

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

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

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

5 Apparatus ..................................................................................................................................................................................................................... 2

6 Preparation of sample .................................................................................................................................................................................... 2

6.1 General ........................................................................................................................................................................................................... 2

6.2 Reference samples ............................................................................................................................................................................... 2

7 Method A — Ratio method ......................................................................................................................................................................... 2

7.1 Procedure .................................................................................................................................................................................................... 2

7.1.1 Measurement of reference samples by n-heptane extraction .................................................. 2

7.1.2 LR­NMR measurement procedure of reference samples .............................................................. 3

7.1.3 LR­NMR measurement procedure of test samples ............................................................................. 3

7.2 Calculation .................................................................................................................................................................................................. 3

7.2.1 Calibration curve ............................................................................................................................................................. 3

7.2.2 Calculation of isotactic index II ........................................................................................................................

na 4

8 Method B — Absolute method ................................................................................................................................................................ 4

8.1 Procedure .................................................................................................................................................................................................... 4

8.1.1 Measurement of reference samples by n-heptane extraction .................................................. 4

8.1.2 LR­NMR measurement procedure of reference samples .............................................................. 4

8.1.3 LR­NMR measurement procedure of test samples ............................................................................. 4

8.2 Calculation .................................................................................................................................................................................................. 4

8.2.1 Calibration curve ............................................................................................................................................................. 4

8.2.2 Calculation of isotactic index II ........................................................................................................................

nb 5

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

10 Test report ................................................................................................................................................................................................................... 5

Annex A (informative) Example of a calibration curve for method A ................................................................................. 7

Annex B (informative) Example of a calibration curve for method B ................................................................................. 8

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

© ISO 2020 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO/FDIS 24076:2020(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

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 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 24076:2020(E)
Introduction

The LR­NMR method in this document is a relative method established with ISO 9113 as the absolute

method. The method and concept of isotactic index of polypropylene are specified in ISO 9113, that is,

the polypropylene sample is separated into the extractable and the unextractable matter by n-heptane

extraction, and the percentage of unextractable matter in the sample is calculated as isotactic index.

Isotactic index in ISO 9113 sounds similar to tacticity (isotacticity or stereotacticity) of polymer chain,

but the concept and result are different. The result is related to but not equal to the tacticity (isotacticity

or stereotacticity) of molecular chain, which can be determined by high resolution carbon-13 nuclear

magnetic resonance and infrared method. The result of ISO 9113 is also related to crystallization,

molecular weight, chain entanglement of the sample, solvent solubility and other effects.

For solid polymers, extraction always takes a long time for the diffusion of long molecular chain from

polymer to solvent. To improve test efficiency, relative methods are developed. This document provides

a relative non-destructive method for the determination of isotactic index by low-resolution nuclear

magnetic resonance spectrometry through a calibration curve establishing with magnetic signal and

isotactic index determined by ISO 9113. No solvent is used, and the determination efficiency is improved

during samples measurement procedure except for the calibration part.
© ISO 2020 – All rights reserved v
---------------------- Page: 5 ----------------------
FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 24076:2020(E)
Plastics — Polypropylene (PP) — Determination of
isotactic index by low-resolution nuclear magnetic
resonance spectrometry
1 Scope

This document specifies a relative method for the determination of polypropylene (PP) isotactic index

by low-resolution pulsed nuclear magnetic resonance spectroscopy (LR-NMR).

This method provides for the identification and coding of types H propylene (PP-H) plastics according

to ISO 19069­1.
This method is suitable for base polymers and is not applicable for mixtures.

NOTE The direct method for the determination of polypropylene isotactic index is specified in ISO 9113.

2 Normative references

The following documents are referred to in the text in such a way that some or all of t

...

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