ISO 17710:2023

Plastics - Polyols for use in the production of polyurethanes - Determination of degree of unsaturation by microtitration

This document specifies a microtitration method to measure the degree of unsaturation in polyether polyols used in the production of polyurethanes. It is based on the reaction of mercuric acetate with double bonds in the polyol. It does not apply to compounds in which the unsaturation is conjugated with carbonyl, carboxyl or nitrile groups.

Plastiques — Polyols pour la production des polyuréthannes — Détermination du degré de non-saturation par microtitrage

General Information

• Status: Published
• Publication Date: 19-Jun-2023
• ICS: 83.080.10 - Thermosetting materials
• Technical Committee: ISO/TC 61/SC 12 - Thermosetting materials
• Drafting Committee: ISO/TC 61/SC 12 - Thermosetting materials
• Current Stage: 6060 - International Standard published
• Start Date: 20-Jun-2023
• Due Date: 14-Mar-2024
• Completion Date: 20-Jun-2023

Relations

• Revises: ISO 17710:2002 - Plastics - Polyols for use in the production of polyurethane - Determination of degree of unsaturation by microtitration
• Effective Date: 17-Sep-2022

Overview

ISO 17710:2023 - Plastics - Polyols for use in the production of polyurethanes - Determination of degree of unsaturation by microtitration - defines a microtitration test method for measuring the degree of unsaturation in polyether polyols used to make polyurethanes. The method is based on the reaction of mercuric acetate with carbon–carbon double bonds and quantifies the acetic acid released by potentiometric titration with methanolic KOH. This second-edition standard adapts the chemistry of existing methods (e.g., ASTM D4671) into a microtitration procedure that uses smaller reagent volumes and reduces mercury waste.

Key topics and requirements

• Principle: Unsaturated sites react with methanolic mercuric acetate to form acetoxymercuric products and acetic acid; released acid is titrated potentiometrically with 0.05 mol/L methanolic KOH. Sodium bromide is added to convert excess mercuric acetate to non-interfering mercuric bromide prior to titration.
• Scope limits: Excludes unsaturation conjugated with carbonyl, carboxyl or nitrile groups.
• Reagents & concentrations: Typical reagents include 0.05 mol/L methanolic mercuric acetate, 0.05 mol/L methanolic KOH, 0.05 mol/L methanolic HCl, NaBr and methanol. Water quality per ISO 3696.
• Apparatus: Autotitrator with appropriate electrodes, analytical balance (0.1 mg), 2 mL pipette (ISO 4787), and 50–100 mL titration vessel.
• Sampling & preparation: Samples must be dry, free of inorganic halides, handled in dry borosilicate glassware, and protected from CO2. Test portion sizing is controlled so ≤ 0.033 meq unsaturation per gram in the portion.
• Calculations & corrections: Results are reported in meq/g and corrected for sample acidity or basicity (separate titrations without mercuric reagent). Blank titration is required.
• Precision & bias: The standard provides repeatability and reproducibility criteria (interlaboratory data and r/R limits) to judge acceptability.

Applications and users

ISO 17710:2023 is suited for:

• Quality control and specification testing of polyether polyols used in flexible and rigid polyurethane foams, elastomers and coatings.
• R&D labs monitoring side reactions (unsaturated chain ends) that affect functionality and molecular-weight distribution.
• Contract testing laboratories performing standardized unsaturation analysis for manufacturers and formulators.

Primary users: polymer chemists, QC analysts, materials laboratories, and manufacturers of polyurethanes.

Related standards

• ASTM D4671 (methodal chemistry basis)
• JIS K 1557 (related polyol testing)
• ISO 3696 (laboratory water), ISO 4787 (volumetric glassware), ISO 6353 series (reagent specifications)

Note: The method uses mercury-containing reagents; follow all safety, handling and hazardous-waste regulations when implementing ISO 17710:2023.

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 17710
Second edition
2023-06
Plastics — Polyols for use in the
production of polyurethanes
— Determination of degree of
unsaturation by microtitration
Plastiques — Polyols pour la production des polyuréthannes —
Détermination du degré de non-saturation par microtitrage
Reference number
© ISO 2023
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
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Published in Switzerland
ii
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Application .2
6 Interferences . 2
7 Reagents . 2
8 Apparatus . 3
9 Sampling . 3
10 Procedure .3
11 Expression of results . 4
12 Precision and bias .5
12.1 Precision . . . 5
12.2 Bias . 5
13 Test report . 6
Bibliography . 7
iii
Foreword
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electrotechnical standardization.
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described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO document should be noted. This document was drafted in accordance with the
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www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12,
Thermosetting materials.
This second edition cancels and replaces the first edition (ISO17710:2002), of which it constitutes a
minor revision.
The changes are as follows:
— the title has been changed to plural form to read: "Plastics — Polyols for use in the production of
polyurethanes — Determination of degree of unsaturation by microtitration"
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
iv
Introduction
Standards have been published which deal with the measurement of the degree of unsaturation in
polyols used for the production of polyurethane plastics (ASTM D 4671, JIS K 1557, part 6.7). These
standards are based on the reaction of mercuric acetate with the unsaturation present in the molecule.
The method described in this document relies on the same chemistry, but is a microtitration method
which uses less reagent and therefore reduces the disposal problems associated with mercury
compounds. It is based primarily on ASTM D 4671.
v
INTERNATIONAL STANDARD ISO 17710:2023(E)
Plastics — Polyols for use in the production of
polyurethanes — Determination of degree of unsaturation
by microtitration
WARNING — Persons using this document should be familiar with normal laboratory practice.
This document does not purport to address all of the safety problems, if any, associated with its
use. It is the responsibility of the user to establish appropriate safety and health practices, and
to determine applicable national regulatory conditions prior to the application of this document.
1 Scope
This document specifies a microtitration method to measure the degree of unsaturation in polyether
polyols used in the production of polyurethanes. It is based on the reaction of mercuric acetate with
double bonds in the polyol. It does not apply to compounds in which the unsaturation is conjugated with
carbonyl, carboxyl or nitrile groups.
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 3696, Water for analytical laboratory use — Specification and test methods
ISO 4787, Laboratory glassware — Volumetric glassware — Methods for use and testing of capacity
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.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
3.1
unsaturation
property of a compound or polymer distinguished by the presence of a carbon-to-carbon double bond
3.2
polyol
organic compound which contains two or more hydroxyl groups capable of reacting with isocyanates
to form polyurethanes
...