Plastics -- Polyols for use in the production of polyurethanes -- Determination of basicity (total amine value), expressed as percent nitrogen

The method specified in ISO 25761:2014 measures the basic constituents in polyols that are soluble in glacial acetic acid and reactive with perchloric acid. Samples containing 0,3 % to 10 % of nitrogen have been evaluated by this method. The method is applicable to amine-based polyols, polyether polyols and polyether polyol blends that are used in polyurethane reactions. The results are measures of batch-to-batch uniformity and may be used to estimate reactivity in polyurethane reactions.

Plastiques -- Polyalcools utilisés pour la production de polyuréthannes -- Détermination de la basicité (valeur totale d'amines) en pourcentage d'azote

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Status
Published
Publication Date
13-Feb-2014
Current Stage
6060 - International Standard published
Start Date
04-Feb-2014
Completion Date
14-Feb-2014
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ISO 25761:2014 - Plastics -- Polyols for use in the production of polyurethanes -- Determination of basicity (total amine value), expressed as percent nitrogen
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INTERNATIONAL ISO
STANDARD 25761
Second edition
2014-03-01
Plastics — Polyols for use in the
production of polyurethanes —
Determination of basicity (total amine
value), expressed as percent nitrogen
Plastiques — Polyalcools utilisés pour la production de
polyuréthannes — Détermination de la basicité (valeur totale
d’amines) en pourcentage d’azote
Reference number
ISO 25761:2014(E)
ISO 2014
---------------------- Page: 1 ----------------------
ISO 25761:2014(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2014

All rights reserved. Unless otherwise specified, 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.
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Published in Switzerland
ii © ISO 2014 – All rights reserved
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ISO 25761:2014(E)
Contents Page

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

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

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

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

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

4 Principle ........................................................................................................................................................................................................................ 2

5 Sampling ........................................................................................................................................................................................................................ 2

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

7 Interference ............................................................................................................................................................................................................... 2

8 Reagents ........................................................................................................................................................................................................................ 2

9 Procedure..................................................................................................................................................................................................................... 3

10 Expression of results ........................................................................................................................................................................................ 4

11 Precision and bias ............................................................................................................................................................................................... 4

11.1 General ........................................................................................................................................................................................................... 4

11.2 Precision ....................................................................................................................................................................................................... 5

11.3 Bias .................................................................................................................................................................................................................... 5

12 Test report

................................................................................................................................................................................................................... 5

Annex A (informative) Determination of the factor F for 0,1 mol/l perchloric acid in acetic acid ......6

Bibliography ................................................................................................................................................................................................................................ 7

© ISO 2014 – All rights reserved iii
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ISO 25761:2014(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 on the meaning of ISO specific terms and expressions related to conformity

assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers

to Trade (TBT) see the following URL: Foreword - Supplementary information.

The committee responsible for this document is ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting

materials.

This second edition cancels and replaces the first edition (ISO 25761:2008), which has been technically

revised.
iv © ISO 2014 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 25761:2014(E)
Introduction

Polyurethanes are produced by the catalysed reaction of isocyanates with polyols. The basicity of the

polyol employed affects the rate of reaction and speed of cure of the product. It is therefore necessary to

determine the basicity in order to predict reactivity and monitor product quality.

© ISO 2014 – All rights reserved v
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INTERNATIONAL STANDARD ISO 25761:2014(E)
Plastics — Polyols for use in the production of
polyurethanes — Determination of basicity (total amine
value), expressed as percent nitrogen

SAFETY STATEMENT — 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 and to ensure compliance with any regulatory requirements.
1 Scope

The method specified in this International Standard measures the basic constituents in polyols that

are soluble in glacial acetic acid and reactive with perchloric acid. Samples containing 0,3 % to 10 % of

nitrogen have been evaluated by this method. The method is applicable to amine-based polyols, polyether

polyols and polyether polyol blends that are used in polyurethane reactions. The results are measures of

batch-to-batch uniformity and may be used to estimate reactivity in polyurethane reactions.

It is also permissible to express the results in equivalents of base per gram of sample.

NOTE This method is technically equivalent to that in ASTM D 6979.
2 Normative references

The following referenced documents are indispensable for the application 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 1042, Laboratory glassware — One-mark volumetric flasks
ISO 4788, Laboratory glassware — Graduated measuring cylinders
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 6353-1, Reagents for chemical analysis — Part 1: General test methods

ISO 6353-2, Reagents for chemical analysis — Part 2: Specifications — First series

ISO 6353-3, Reagents for chemical analysis — Part 3: Specifications — Second series

3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
polyol

polymer based on ethylene oxide and/or propylene oxide which contains two or more hydroxyl groups

3.2
polyurethane

polymer prepared by the reaction of an organic di- or polyisocyanate with a compound containing two

or more hydroxyl groups
3.3
percent nitrogen

quantity of perchloric-acid-titratable base in a sample, expressed as a mass percentage of nitrogen

© ISO 2014 – All rights reserved 1
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ISO 25761:2014(E)
3.4
alkalinity

quantity of perchloric-acid-titratable base in a sample, expressed as mg of KOH/g of sample

3.5
total amine value

quantity of perchloric-acid-titratable base in a sample, identified only as amines and expressed as mg of

KOH/g of sample
4 Principle

A test portion of the sample is dissolved in glacial acetic acid. The resulting single-phase solution is

titrated at room temperature to a potentiometric end point with a standardized solution of perchloric

acid in acetic acid. The result is reported as percent nitrogen or mg of KOH/g of sample.

5 Sampling

Draw samples from a well-mixed vessel into a thoroughly cleaned and dry borosilicate-glass container

(soft-glass containers are not acceptable). If sampling from a line or valve, flush the line thoroughly with

the product before starting to draw the sample. Seal the sample until analysis.
6 Apparatus
6.1 One-mark volumetric flask, of capaci
...

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