Polyolefin pipes and fittings -- Determination of carbon black content by calcination and pyrolysis -- Test method

This document specifies test methods for the determination of the carbon black content of polyolefin compositions used in particular for the manufacture of pipes and fittings, and provides a basic specification for polyethylene pipes and fittings.
This document applies equally to the material for manufacture and to any material taken from a pipe or fitting.

Tubes et raccords en polyoléfines -- Détermination de la teneur en noir de carbone par calcination et pyrolyse -- Méthode d'essai

Poliolefinske cevi in fitingi - Določanje vsebnosti saj s kalcinacijo in pirolizo - Preskusna metoda

General Information

Status
Published
Publication Date
09-Jun-2021
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-Jun-2021
Due Date
06-Aug-2021
Completion Date
10-Jun-2021

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SLOVENSKI STANDARD
SIST ISO 6964:2021
01-julij-2021
Nadomešča:
SIST ISO 6964:1996

Poliolefinske cevi in fitingi - Določanje vsebnosti saj s kalcinacijo in pirolizo -

Preskusna metoda

Polyolefin pipes and fittings -- Determination of carbon black content by calcination and

pyrolysis -- Test method

Tubes et raccords en polyoléfines -- Détermination de la teneur en noir de carbone par

calcination et pyrolyse -- Méthode d'essai
Ta slovenski standard je istoveten z: ISO 6964:2019
ICS:
23.040.20 Cevi iz polimernih materialov Plastics pipes
SIST ISO 6964:2021 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST ISO 6964:2021
---------------------- Page: 2 ----------------------
SIST ISO 6964:2021
INTERNATIONAL ISO
STANDARD 6964
Second edition
2019-02
Polyolefin pipes and fittings —
Determination of carbon black
content by calcination and pyrolysis —
Test method
Tubes et raccords en polyoléfines — Détermination de la teneur en
noir de carbone par calcination et pyrolyse — Méthode d'essai
Reference number
ISO 6964:2019(E)
ISO 2019
---------------------- Page: 3 ----------------------
SIST ISO 6964:2021
ISO 6964:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019

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
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved
---------------------- Page: 4 ----------------------
SIST ISO 6964:2021
ISO 6964:2019(E)
Contents Page

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

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

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

3 Principle ........................................................................................................................................................................................................................ 1

4 Method A: Electrical tube furnace ...................................................................................................................................................... 2

4.1 Reagents........................................................................................................................................................................................................ 2

4.2 Apparatus .................................................................................................................................................................................................... 2

4.3 Procedure .................................................................................................................................................................................................... 2

4.3.1 Test conditions................................................................................................................................................................... 2

4.3.2 Sampling.................................................................................................................................................................................. 2

4.3.3 Conditioning ........................................................................................................................................................................ 2

4.3.4 Silica sample boat preparation for the test ............................................................................................... 2

4.3.5 Test portion .......................................................................................................................................................................... 3

4.3.6 Determination .................................................................................................................................................................... 3

4.4 Calculation and expression of results (Method A) ................................................................................................... 3

5 Method B1 or B2: Muffle furnace (conventional B1) or (microwave B2) ..................................................4

5.1 Apparatus .................................................................................................................................................................................................... 4

5.2 Procedure .................................................................................................................................................................................................... 4

5.2.1 Test conditions................................................................................................................................................................... 4

5.2.2 Conditioning ........................................................................................................................................................................ 4

5.2.3 Sampling.................................................................................................................................................................................. 4

5.2.4 Crucible preparation for the test ....................................................................................................................... 4

5.2.5 Test portion .......................................................................................................................................................................... 5

5.2.6 Determination .................................................................................................................................................................... 5

5.3 Calculation and expression of results (Method B1 and B2) ............................................................................. 6

6 Method C: Thermogravimetric analyzer (TGA) ....................................................................................................................6

6.1 Apparatus .................................................................................................................................................................................................... 6

6.2 Procedure .................................................................................................................................................................................................... 6

6.2.1 Conditioning ........................................................................................................................................................................ 6

6.2.2 Sampling.................................................................................................................................................................................. 6

6.2.3 Test portion .......................................................................................................................................................................... 6

6.2.4 Temperature scanning program ......................................................................................................................... 7

6.2.5 Gas-flow rate ....................................................................................................................................................................... 7

6.2.6 Determination .................................................................................................................................................................... 7

6.3 Calculation and expression of results (Method C) ................................................................................................... 7

7 Test report ...................................................................................................................................................................................................................8

© ISO 2019 – All rights reserved iii
---------------------- Page: 5 ----------------------
SIST ISO 6964:2021
ISO 6964:2019(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 138, Plastics pipes, fittings and valves

for the transport of fluids, Subcommittee SC 5, General properties of pipes, fittings and valves of plastic

materials and their accessories — Test methods and basic specifications.

This second edition cancels and replaces the first edition (ISO 6964:1986), which has been technically

revised. The main changes compared with the last edition are the following:

— Conventional and microwave muffle furnace test methods, and a thermogravimetric analyzer (TGA)

test method have been added.

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 2019 – All rights reserved
---------------------- Page: 6 ----------------------
SIST ISO 6964:2021
INTERNATIONAL STANDARD ISO 6964:2019(E)
Polyolefin pipes and fittings — Determination of carbon
black content by calcination and pyrolysis — Test method
1 Scope

This document specifies test methods for the determination of the carbon black content of polyolefin

compositions used in particular for the manufacture of pipes and fittings, and provides a basic

specification for polyethylene pipes and fittings.

This document applies equally to the material for manufacture and to any material taken from a pipe or

fitting.
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 11358-1, Plastics — Thermogravimetry (TG) of polymers — Part 1: General principles

3 Principle

It is possible to determine the carbon black content of polyolefin compositions by one of the following

three methods:

a) Pyrolysis of the sample at (550 ± 50) °C in a stream of nitrogen for 45 min followed by calcination at

(900 ± 25) °C, by using an electrical tube furnace (Method A).

b) Pyrolysis of the sample in a quartz crystal crucible with lid, by using a muffle furnace. According to

the type of muffle furnace used there are two different procedures:

1) Conventional muffle furnace (Method B1): pyrolysis from (325 ± 25) °C to (550 ± 25) °C at

15 °C/min and at (550 ± 25) °C for (10 ± 0,5) min followed by calcination at (900 ± 25) °C.

2) Microwave muffle furnace (Method B2): pyrolysis at (520 ± 25) °C for (10 ± 0,5) min followed

by calcination at (900 ± 25) °C.

c) Pyrolysis of the sample at a constant rate in a thermogravimetric analyzer (TGA) under inert

atmosphere at 800 °C followed by calcination under oxidizing atmosphere at 900 °C (Method C).

NOTE 1 Carbon black is decomposed from 500 °C in air or oxygen. Therefore, the loss observed between

500 °C and 700 °C in air or oxygen corresponds to the overall decomposition of the carbon black.

NOTE 2 If the composition contains, in addition to the carbon black, additives likely to decompose at 900 °C,

for example ingredients such as calcium carbonate, the calculation can lead to an over-estimation of the carbon

black content. If the ash yield is more than 1 %, further investigation can be required.

Calculate the carbon black content from the difference in mass before and after calcination and

pyrolysis.
© ISO 2019 – All rights reserved 1
---------------------- Page: 7 ----------------------
SIST ISO 6964:2021
ISO 6964:2019(E)
4 Method A: Electrical tube furnace
4.1 Reagents

4.1.1 Dry nitrogen, having an oxygen content less than 20 ppm, under pressure in a steel cylinder

provided with a pressure-reducing valve and flow meter.

NOTE If required, the nitrogen can be purified by bubbling the gas through a pyrogallol solution or by

passing it over heated copper tinsel, foil, wire or turnings or by passing it through a gas purifier prior to passing

into the furnace.
4.2 Apparatus
4.2.1 Silica combustion sample boat, with a sleeve of 50 mm to 60 mm long.

4.2.2 Electric tube furnace, fitted with a device to allow the sample boat to be inserted and

withdrawn. The tube is fitted with nozzles to admit the nitrogen and to evacuate the fumes. A diaphragm

closed by means of a glass-wool bung placed behind the entry nozzle ensures that the nitrogen stream is

distributed uniformly.

The minimum length of the electric tube furnace should be ≥ 3 times the length of the sample boat, and

the minimum length of the quartz tube should be ≥ 7 times the length of the sample boat.

4.2.3 Desiccator, capable of holding the silica sample boat (4.2.1).
4.2.4 Balance, with an accuracy of ± 0,1 mg.
4.2.5 Timer, with an accuracy of
...

INTERNATIONAL ISO
STANDARD 6964
Second edition
2019-02
Polyolefin pipes and fittings —
Determination of carbon black
content by calcination and pyrolysis —
Test method
Tubes et raccords en polyoléfines — Détermination de la teneur en
noir de carbone par calcination et pyrolyse — Méthode d'essai
Reference number
ISO 6964:2019(E)
ISO 2019
---------------------- Page: 1 ----------------------
ISO 6964:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019

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
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 6964:2019(E)
Contents Page

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

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

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

3 Principle ........................................................................................................................................................................................................................ 1

4 Method A: Electrical tube furnace ...................................................................................................................................................... 2

4.1 Reagents........................................................................................................................................................................................................ 2

4.2 Apparatus .................................................................................................................................................................................................... 2

4.3 Procedure .................................................................................................................................................................................................... 2

4.3.1 Test conditions................................................................................................................................................................... 2

4.3.2 Sampling.................................................................................................................................................................................. 2

4.3.3 Conditioning ........................................................................................................................................................................ 2

4.3.4 Silica sample boat preparation for the test ............................................................................................... 2

4.3.5 Test portion .......................................................................................................................................................................... 3

4.3.6 Determination .................................................................................................................................................................... 3

4.4 Calculation and expression of results (Method A) ................................................................................................... 3

5 Method B1 or B2: Muffle furnace (conventional B1) or (microwave B2) ..................................................4

5.1 Apparatus .................................................................................................................................................................................................... 4

5.2 Procedure .................................................................................................................................................................................................... 4

5.2.1 Test conditions................................................................................................................................................................... 4

5.2.2 Conditioning ........................................................................................................................................................................ 4

5.2.3 Sampling.................................................................................................................................................................................. 4

5.2.4 Crucible preparation for the test ....................................................................................................................... 4

5.2.5 Test portion .......................................................................................................................................................................... 5

5.2.6 Determination .................................................................................................................................................................... 5

5.3 Calculation and expression of results (Method B1 and B2) ............................................................................. 6

6 Method C: Thermogravimetric analyzer (TGA) ....................................................................................................................6

6.1 Apparatus .................................................................................................................................................................................................... 6

6.2 Procedure .................................................................................................................................................................................................... 6

6.2.1 Conditioning ........................................................................................................................................................................ 6

6.2.2 Sampling.................................................................................................................................................................................. 6

6.2.3 Test portion .......................................................................................................................................................................... 6

6.2.4 Temperature scanning program ......................................................................................................................... 7

6.2.5 Gas-flow rate ....................................................................................................................................................................... 7

6.2.6 Determination .................................................................................................................................................................... 7

6.3 Calculation and expression of results (Method C) ................................................................................................... 7

7 Test report ...................................................................................................................................................................................................................8

© ISO 2019 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 6964:2019(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 138, Plastics pipes, fittings and valves

for the transport of fluids, Subcommittee SC 5, General properties of pipes, fittings and valves of plastic

materials and their accessories — Test methods and basic specifications.

This second edition cancels and replaces the first edition (ISO 6964:1986), which has been technically

revised. The main changes compared with the last edition are the following:

— Conventional and microwave muffle furnace test methods, and a thermogravimetric analyzer (TGA)

test method have been added.

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 2019 – All rights reserved
---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 6964:2019(E)
Polyolefin pipes and fittings — Determination of carbon
black content by calcination and pyrolysis — Test method
1 Scope

This document specifies test methods for the determination of the carbon black content of polyolefin

compositions used in particular for the manufacture of pipes and fittings, and provides a basic

specification for polyethylene pipes and fittings.

This document applies equally to the material for manufacture and to any material taken from a pipe or

fitting.
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 11358-1, Plastics — Thermogravimetry (TG) of polymers — Part 1: General principles

3 Principle

It is possible to determine the carbon black content of polyolefin compositions by one of the following

three methods:

a) Pyrolysis of the sample at (550 ± 50) °C in a stream of nitrogen for 45 min followed by calcination at

(900 ± 25) °C, by using an electrical tube furnace (Method A).

b) Pyrolysis of the sample in a quartz crystal crucible with lid, by using a muffle furnace. According to

the type of muffle furnace used there are two different procedures:

1) Conventional muffle furnace (Method B1): pyrolysis from (325 ± 25) °C to (550 ± 25) °C at

15 °C/min and at (550 ± 25) °C for (10 ± 0,5) min followed by calcination at (900 ± 25) °C.

2) Microwave muffle furnace (Method B2): pyrolysis at (520 ± 25) °C for (10 ± 0,5) min followed

by calcination at (900 ± 25) °C.

c) Pyrolysis of the sample at a constant rate in a thermogravimetric analyzer (TGA) under inert

atmosphere at 800 °C followed by calcination under oxidizing atmosphere at 900 °C (Method C).

NOTE 1 Carbon black is decomposed from 500 °C in air or oxygen. Therefore, the loss observed between

500 °C and 700 °C in air or oxygen corresponds to the overall decomposition of the carbon black.

NOTE 2 If the composition contains, in addition to the carbon black, additives likely to decompose at 900 °C,

for example ingredients such as calcium carbonate, the calculation can lead to an over-estimation of the carbon

black content. If the ash yield is more than 1 %, further investigation can be required.

Calculate the carbon black content from the difference in mass before and after calcination and

pyrolysis.
© ISO 2019 – All rights reserved 1
---------------------- Page: 5 ----------------------
ISO 6964:2019(E)
4 Method A: Electrical tube furnace
4.1 Reagents

4.1.1 Dry nitrogen, having an oxygen content less than 20 ppm, under pressure in a steel cylinder

provided with a pressure-reducing valve and flow meter.

NOTE If required, the nitrogen can be purified by bubbling the gas through a pyrogallol solution or by

passing it over heated copper tinsel, foil, wire or turnings or by passing it through a gas purifier prior to passing

into the furnace.
4.2 Apparatus
4.2.1 Silica combustion sample boat, with a sleeve of 50 mm to 60 mm long.

4.2.2 Electric tube furnace, fitted with a device to allow the sample boat to be inserted and

withdrawn. The tube is fitted with nozzles to admit the nitrogen and to evacuate the fumes. A diaphragm

closed by means of a glass-wool bung placed behind the entry nozzle ensures that the nitrogen stream is

distributed uniformly.

The minimum length of the electric tube furnace should be ≥ 3 times the length of the sample boat, and

the minimum length of the quartz tube should be ≥ 7 times the length of the sample boat.

4.2.3 Desiccator, capable of holding the silica sample boat (4.2.1).
4.2.4 Balance, with an accuracy of ± 0,1 mg.
4.2.5 Timer, with an accuracy of ± 1 s.
4.3 Procedure
4.3.1 Test conditions

Determination of mass shall be carried out in a room at standard temperature (23 ± 2) °C.

4.3.2 Sampling

Test specimen may be in the form of pellet or finished product. In the last case, the specimen shall be

reduced to small fragments.
4.3.3 Conditioning
The test sample shall be conditioned for 24 h at (23 ± 2) °C before preparation.
4.3.4 Silica sample boat preparation for the test
Take the silica sample boat which s
...

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