ISO 4625-1:2020
(Main)Binders for paints and varnishes — Determination of softening point — Part 1: Ring-and-ball method
Binders for paints and varnishes — Determination of softening point — Part 1: Ring-and-ball method
Liants pour peintures et vernis — Détermination du point de ramollissement — Partie 1: Méthode de l'anneau et de la bille
Le présent document spécifie des méthodes d'essai pour la détermination du point de ramollissement des résines (y compris la colophane) et des produits assimilés, au moyen de l'appareil à anneau et à bille. Les méthodes manuelle et automatique sont spécifiées, la méthode automatique étant la méthode de référence.
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INTERNATIONAL ISO
STANDARD 4625-1
Second edition
2020-07
Binders for paints and varnishes —
Determination of softening point —
Part 1:
Ring-and-ball method
Liants pour peintures et vernis — Détermination du point de
ramollissement —
Partie 1: Méthode de l'anneau et de la bille
Reference number
ISO 4625-1:2020(E)
©
ISO 2020
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ISO 4625-1:2020(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
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Phone: +41 22 749 01 11
Email: copyright@iso.org
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Published in Switzerland
ii © ISO 2020 – All rights reserved
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ISO 4625-1:2020(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Sampling and preparation of test pieces . 2
5.1 Sampling . 2
5.2 Preparation of test pieces by the pour method. 2
5.2.1 Field of application . 2
5.2.2 Apparatus . 2
5.2.3 Procedure . 2
5.3 Preparation of test pieces from samples with a low softening point (up to 35 °C) . 2
5.3.1 Apparatus . 2
5.3.2 Procedure . 3
6 Materials (heating-bath liquids) . 3
7 Automated ring-and-ball method (reference method) . 3
7.1 Apparatus . 3
7.2 Calibration . 4
7.3 Procedure for materials with a softening point between 35 °C and 80 °C . 4
7.4 Procedure for materials with a softening point between 80 °C and 150 °C . 4
7.5 Procedure for materials with a softening point above 150 °C . 4
8 Manual ring-and-ball method (alternate method) . 4
8.1 Apparatus . 4
8.2 Calibration . 7
8.3 Procedure . 7
8.3.1 Procedure for materials with a softening point between 35 °C and 80 °C . 7
8.3.2 Procedure for materials with a softening point between 80 °C and 150 °C . 8
8.3.3 Procedure for materials with a softening point above 150 °C . 8
8.3.4 Procedure for materials with a softening point below 35 °C . 8
9 Expression of results . 8
10 Precision and bias . 8
10.1 Precision of the automated method . 8
10.1.1 General. 8
10.1.2 Precision data . 8
10.2 Precision of the manual method . 9
10.2.1 General. 9
10.2.2 Precision data . 9
10.3 Bias . 9
11 Test report .10
Bibliography .11
© ISO 2020 – All rights reserved iii
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ISO 4625-1:2020(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 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 35, Paints and varnishes, in collaboration
with the European Committee for Standardization (CEN) Technical Committee CEN/TC 139, Paints and
varnishes, in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna
Agreement).
This second edition cancels and replaces the first edition (ISO 4625-1:2004), which has been technically
revised. The main changes compared to the previous edition are as follows:
— the automated method has been classified to be the reference method;
— an introduction with information on all three methods described in the three parts of ISO 4625
series has been added;
— CAS-numbers have been added to the chemicals used;
— the text has been editorially revised;
— the normative references have been updated.
A list of all parts in the ISO 4625 series can be found on the ISO website.
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
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ISO 4625-1:2020(E)
Introduction
The ISO 4625 series specifies three widely used procedures for the measurement of the softening point
of rosin-based resins. This document presents the ring-and-ball method, which has been the accepted
standard for many years. ISO 4625-2 presents the Mettler cup-and-ball method. A new method, called
the Mettler method without the ball, is to be presented in a future document.
This document is still the only standard test method accepted in regulatory documents such as Title 21
of the Code of Federal Regulations (CFR) – Food and Drugs.
Other parts of the ISO 4625 series concern Mettler cup-and-ball methods. Although the recommended
testing conditions differ, the only difference between the equipment required in such methods is that
Mettler method without the ball does not use a ball. Surveys have shown that the Mettler cup-and-ball
method specified in ISO 4625-2 is the most widely used in the USA, while the Mettler method without
the ball is the most widely used in Europe. These methods are less time consuming than the ring-and-
ball manual method and the equipment is less expensive than the ring-and-ball automated method.
As a consequence of the thermoplastic nature of the test resins, the softening points obtained using the
recommended test conditions for all three methods are not generally the same. Consequently, the test
method and the testing conditions used should be noted in the final report.
© ISO 2020 – All rights reserved v
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INTERNATIONAL STANDARD ISO 4625-1:2020(E)
Binders for paints and varnishes — Determination of
softening point —
Part 1:
Ring-and-ball method
1 Scope
This document specifies the test methods for determining the softening point of resins (including rosin)
and similar materials by means of ring-and-ball apparatus.
Both manual and automated methods are specified, the automated method being the reference method.
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 4618, Paints and varnishes — Terms and definitions
ISO 15528, Paints, varnishes and raw materials for paints and varnishes — Sampling
IEC 60751, Industrial platinum resistance thermometer and platinum temperature sensors
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 4618 and the following apply.
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/
3.1
softening point
temperature at which a disc of sample held within a horizontal ring is forced downward a distance of
25 mm under the weight of a steel ball as the disc is heated at a prescribed rate in a water, glycerol,
silicone oil, ethylene glycol/water or glycerol/water bath
4 Principle
In general, with materials of the types mentioned in Clause 1, softening does not take place at a definite
temperature. As the temperature rises, these materials gradually change from brittle or exceedingly
thick and slow-flowing materials to softer and less viscous liquids. For this reason, the determination
of the softening point shall be made by a fixed, closely defined method if the results obtained are to be
comparable.
For the purpose of these test methods, the definition of softening point given in Clause 3 applies.
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ISO 4625-1:2020(E)
5 Sampling and preparation of test pieces
5.1 Sampling
Take a representative sample of the product to be tested, as described in ISO 15528.
The sample shall consist of freshly broken lumps free of oxidized surfaces. For samples received as
small lumps, scrape off the surface layer of the lumps immediately before use, avoiding inclusion of
finely divided material or dust.
5.2 Preparation of test pieces by the pour method
5.2.1 Field of application
This preparation procedure is suitable for resins (including rosin) and other substances that can be
heated and poured without adverse effects on the softening point.
5.2.2 Apparatus
5.2.2.1 Container, in which the sample can be melted.
5.2.2.2 Knife or spatula.
5.2.2.3 Oven, hot-plate, sand bath or oil bath.
5.2.3 Procedure
Take a quantity of the sample (see 5.1) which is at least twice that necessary to fill the desired number
of rings (7.1.1), but in no case less than 40 g, and melt it immediately in a clean container (5.2.2.1)
using an oven, hot-plate, sand bath or oil bath (5.2.2.3) to prevent local overheating. Take care to
avoid incorporating air bubbles in the sample. Melt the sample completely, but do not heat it above
the minimum temperature necessary to pour it easily. The time from the beginning of heating to the
pouring of the sample shall not exceed 15 min.
For materials that are heat-sensitive, continuously inert the atmosphere in the container holding the
sample with nitrogen (N ) during the melting procedure.
2
For materials that tend to crack or shrink in the rings on cooling, preheat the rings immediately before
filling them to approximately the temperature at which the material is to be poured. The rings, while
being filled, shall rest on a suitable metal surface. Pour a sufficient quantity of the sample into the ring
so as to leave an excess on cooling. Allow to cool for at least 30 min and trim off the surplus material
at the periphery of the ring. To remove excess material from the top, cut the excess material off cleanly
with a slightly
...
NORME ISO
INTERNATIONALE 4625-1
Deuxième édition
2020-07
Liants pour peintures et vernis —
Détermination du point de
ramollissement —
Partie 1:
Méthode de l'anneau et de la bille
Binders for paints and varnishes — Determination of softening point —
Part 1: Ring-and-ball method
Numéro de référence
ISO 4625-1:2020(F)
©
ISO 2020
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ISO 4625-1:2020(F)
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2020
Tous droits réservés. Sauf prescription différente ou nécessité dans le contexte de sa mise en œuvre, aucune partie de cette
publication ne peut être reproduite ni utilisée sous quelque forme que ce soit et par aucun procédé, électronique ou mécanique,
y compris la photocopie, ou la diffusion sur l’internet ou sur un intranet, sans autorisation écrite préalable. Une autorisation peut
être demandée à l’ISO à l’adresse ci-après ou au comité membre de l’ISO dans le pays du demandeur.
ISO copyright office
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CH-1214 Vernier, Genève
Tél.: +41 22 749 01 11
E-mail: copyright@iso.org
Web: www.iso.org
Publié en Suisse
ii © ISO 2020 – Tous droits réservés
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ISO 4625-1:2020(F)
Sommaire Page
Avant-propos .iv
Introduction .v
1 Domaine d'application . 1
2 Références normatives . 1
3 Termes et définitions . 1
4 Principe . 1
5 Échantillonnage et préparation des éprouvettes . 2
5.1 Échantillonnage . 2
5.2 Préparation des éprouvettes par la méthode par coulage . 2
5.2.1 Champ d'application . 2
5.2.2 Appareillage . 2
5.2.3 Mode opératoire . 2
5.3 Préparation des éprouvettes à partir d'échantillons ayant un point de
ramollissement bas (jusqu'à 35 °C) . 3
5.3.1 Appareillage . 3
5.3.2 Mode opératoire . 3
6 Matériaux (liquides de bains de chauffage) . 3
7 Méthode automatique de l'anneau et de la bille (méthode de référence) .4
7.1 Appareillage. 4
7.2 Étalonnage . 4
7.3 Mode opératoire applicable pour les produits ayant un point de ramollissement
compris entre 35 °C et 80 °C . 4
7.4 Mode opératoire applicable pour les produits ayant un point de ramollissement
compris entre 80 °C et 150 °C . 4
7.5 Mode opératoire applicable pour les produits ayant un point de ramollissement
supérieur à 150 °C . 5
8 Méthode manuelle de l'anneau et de la bille (méthode alternative) .5
8.1 Appareillage. 5
8.2 Étalonnage . 8
8.3 Mode opératoire . 8
8.3.1 Mode opératoire applicable pour les produits ayant un point de
ramollissement compris entre 35 °C et 80 °C . 8
8.3.2 Mode opératoire applicable pour les produits ayant un point de
ramollissement compris entre 80 °C et 150 °C . 9
8.3.3 Mode opératoire applicable pour les produits ayant un point de
ramollissement supérieur à 150 °C . 9
8.3.4 Mode opératoire applicable pour les produits ayant un point de
ramollissement inférieur à 35 °C . 9
9 Expression des résultats. 9
10 Fidélité et biais . 9
10.1 Fidélité de la méthode automatique . 9
10.1.1 Généralités . 9
10.1.2 Données de fidélité .10
10.2 Fidélité de la méthode manuelle .10
10.2.1 Généralités .10
10.2.2 Données de fidélité .10
10.3 Biais .11
11 Rapport d'essai .11
Bibliographie .12
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ISO 4625-1:2020(F)
Avant-propos
L'ISO (Organisation internationale de normalisation) est une fédération mondiale d'organismes
nationaux de normalisation (comités membres de l'ISO). L'élaboration des Normes internationales est
en général confiée aux comités techniques de l'ISO. Chaque comité membre intéressé par une étude
a le droit de faire partie du comité technique créé à cet effet. Les organisations internationales,
gouvernementales et non gouvernementales, en liaison avec l'ISO participent également aux travaux.
L'ISO collabore étroitement avec la Commission électrotechnique internationale (IEC) en ce qui
concerne la normalisation électrotechnique.
Les procédures utilisées pour élaborer le présent document et celles destinées à sa mise à jour sont
décrites dans les Directives ISO/IEC, Partie 1. Il convient, en particulier de prendre note des différents
critères d'approbation requis pour les différents types de documents ISO. Le présent document a été
rédigé conformément aux règles de rédaction données dans les Directives ISO/IEC, Partie 2 (voir www
.iso .org/ directives).
L'attention est attirée sur le fait que certains des éléments du présent document peuvent faire l'objet de
droits de propriété intellectuelle ou de droits analogues. L'ISO ne saurait être tenue pour responsable
de ne pas avoir identifié de tels droits de propriété et averti de leur existence. Les détails concernant
les références aux droits de propriété intellectuelle ou autres droits analogues identifiés lors de
l'élaboration du document sont indiqués dans l'Introduction et/ou dans la liste des déclarations de
brevets reçues par l'ISO (voir www .iso .org/ brevets).
Les appellations commerciales éventuellement mentionnées dans le présent document sont données
pour information, par souci de commodité, à l'intention des utilisateurs et ne sauraient constituer un
engagement.
Pour une explication de la nature volontaire des normes, la signification des termes et expressions
spécifiques de l'ISO liés à l'évaluation de la conformité, ou pour toute information au sujet de l'adhésion
de l'ISO aux principes de l'Organisation mondiale du commerce (OMC) concernant les obstacles
techniques au commerce (OTC), voir le lien suivant: www .iso .org/ iso/ fr/ avant -propos.
Le présent document a été élaboré par le comité technique ISO/TC 35, Peintures et vernis, en collaboration
avec le comité technique CEN/TC 139 du Comité européen de la normalisation (CEN) Peintures et vernis,
conformément à l'Accord de coopération technique entre l'ISO et le CEN (Accord de Vienne).
Cette deuxième édition annule et remplace la première édition (ISO 4625-1:2004), qui a fait l'objet d'une
révision technique. Les principales modifications par rapport à l'édition précédente sont les suivantes :
— la méthode automatique est classée comme la méthode de référence ;
— une présentation des trois méthodes décrites dans les trois parties de la série ISO 4625 a été ajoutée ;
— le numéro CAS des produits chimiques utilisés a été ajouté ;
— le texte a fait l'objet d'une révision éditoriale ;
— les références normatives ont été mises à jour.
Une liste de toutes les parties de la série ISO 4625 est disponible sur le site de l'ISO.
Il convient que l'utilisateur adresse tout retour d'information ou toute question concernant le présent
document à l'organisme national de normalisation de son pays. Une liste exhaustive desdits organismes
se trouve à l'adresse www .iso .org/ fr/ members .html.
iv © ISO 2020 – Tous droits réservés
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ISO 4625-1:2020(F)
Introduction
La série de normes ISO 4625 spécifie trois modes opératoires largement répandus pour la détermination
du point de ramollissement des résines à base de colophane. Le présent document présente la méthode
de l'anneau et de la bille, qui a été la norme acceptée pendant de nombreuses années. L'ISO 4625-2
présente la méthode de la coupe et de la bille de Mettler. Une nouvelle méthode, appelée méthode de
Mettler sans la bille, doit être présentée dans un prochain document.
Le présent document reste à ce jour la seule méthode d'essai normalisée acceptée dans des documents
réglementaires tels que le Titre 21 du Code des règlements fédéraux (CFR) de la FDA (Administration
américaine des denrées alimentaires et des médicaments).
Les autres parties de la série ISO 4625 concernent les méthodes de la coupe et de la bille de Mettler.
Bien que les conditions d'essai recommandées diffèrent, la seule différence entre les équipements
requis dans ces méthodes est que la méthode de Mettler sans la bille n'utilise pas de bille. Des études
ont montré que la méthode de la coupe et de la bille de Mettler spécifiée dans l'ISO 4625-2 est la plus
largement utilisée aux États-Unis, tandis que la méthode de Mettler sans la bille est la plus répandue
en Europe. Ces méthodes sont moins longues que la méthode manuelle de l'anneau et de la bille, et
l'équipement est moins cher que dans la méthode automatique de l'anneau et de la bille.
En raison de la nature thermoplastique des résines d'essai, les points de ramollissement obtenus dans
les conditions d'essai recommandées pour les trois méthodes ne sont en général pas identiques. Par
conséquent, il convient de consigner la méthode d'essai et les conditions d'essai dans le rapport final.
© ISO 2020 – Tous droits réservés v
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NORME INTERNATIONALE ISO 4625-1:2020(F)
Liants pour peintures et vernis — Détermination du point
de ramollissement —
Partie 1:
Méthode de l'anneau et de la bille
1 Domaine d'application
Le présent document spécifie des méthodes d'essai pour la détermination du point de ramollissement
des résines (y compris la colophane) et des produits assimilés, au moyen de l'appareil à anneau et à bille.
Les méthodes manuelle et automatique sont spécifiées, la méthode automatique étant la méthode de
référence.
2 Références normatives
Les documents suivants sont cités dans le texte de sorte qu’ils constituent, pour tout ou partie de leur
contenu, des exigences du présent document. Pour les références datées, seule l’édition citée s’applique.
Pour les références non datées, la dernière édition du document de référence s'applique (y compris les
éventuels amendements).
ISO 4618, Peintures et vernis — Termes et définitions
ISO 15528, Peintures, vernis et matières premières pour peintures et vernis — Échantillonnage
IEC 60751, Thermomètres à résistance de platine industriels et capteurs thermométriques en platine
3 Termes et définitions
Pour les besoins du présent document, les termes et définitions donnés dans l'ISO 4618 ainsi que les
suivants s'appliquent.
L'ISO et l'IEC tiennent à jour des bases de données terminologiques destinées à être utilisées en
normalisation, consultables aux adresses suivantes :
— ISO Online browsing platform : disponible à l'adresse https:// www .iso .org/ obp
— IEC Electropedia : disponible à l'adresse http:// www .electropedia .org/
3.1
point de ramollissement
température à laquelle un disque de l'échantillon, maintenu dans un anneau horizontal, est poussé
vers le bas sur une distance de 25 mm sous le poids d'une bille en acier lorsque le disque est chauffé à
une vitesse déterminée dans un bain d'eau, de glycérol, d'huile de silicone, d'éthylène glycol/eau ou de
glycérol/eau
4 Principe
En général, avec des produits des types mentionnés dans l'Article 1, le ramollissement ne se produit
pas à une température définie. Lorsque la température s'élève, ces matériaux initialement peu fluides,
cassants et excessivement épais prennent graduellement la forme de liquides plus mous et moins
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ISO 4625-1:2020(F)
visqueux. Pour cette raison, la détermination du point de ramollissement doit être effectuée à l'aide
d'une méthode fixée, parfaitement définie, pour que les résultats obtenus soient comparables.
Pour les besoins de ces méthodes d'essai, la définition du point de ramollissement donnée dans
l'Article 3 s'applique.
5 Échantillonnage et préparation des éprouvettes
5.1 Échantillonnage
Prélever un échantillon représentatif du produit à soumettre à l'essai, conformément à la description
donnée dans l'ISO 15528.
Cet échantillon doit être constitué de morceaux fraîchement coupés, sans surfaces oxydées. Pour les
échantillons reçus sous forme de petits morceaux, racler la couche superficielle immédiatement avant
utilisation, en évitant d'introduire des produits finement divisés ou de la poussière.
5.2 Préparation des éprouvettes par la méthode par coulage
5.2.1 Champ d'application
Ce mode de préparation convient pour les résines (y compris la colophane) et autres substances qui
peuvent être chauffées et versées sans entraîner d'effet défavorable sur le point de ramollissement.
5.2.2 Appareillage
5.2.2.1 Récipient, dans lequel on peut faire fondre l'échantillon.
5.2.2.2 Couteau ou spatule.
5.2.2.3 Étuve, plaque chauffante, bain de sable ou bain d'huile.
5.2.3 Mode opératoire
Prélever une quantité d'échantillon (voir 5.1) au moins égale au double de la quantité nécessaire
pour remplir le nombre voulu d'anneaux (7.1.1), en aucun cas inférieure à 40 g, et la faire fondre
immédiatement dans un récipient propre (5.2.2.1) en utilisant une étuve, une plaque chauffante, un
bain de sable ou un bain d'huile (5.2.2.3) pour empêcher toute surchauffe locale. Éviter d'incorporer
des bulles d'air dans l'échantillon. Faire fondre l'échantillon complètement mais ne pas le faire chauffer
au-dessus de la température minimale nécessaire pour le faire couler. Le laps de temps, séparant le
début du chauffage de l'écoulement de l'échantillon, ne doit pas dépasser 15 min.
Pour les matériaux thermosensibles, maintenir en permanence inerte l'atmosphère à l'intérieur du
récipient contenant l'échantillon avec de l'azote (N ), pendant la fusion.
2
Pour les matériaux qui ont tendance à se fissurer ou à présenter un retrait dans les anneaux lors du
refroidissement, préchauffer les anneaux juste avant de les remplir environ jusqu'à la température
à laquelle le produit sera versé. Lors du remplissage, les anneaux doivent reposer sur une surface
métallique appropriée. Verser une quantité suffisante d'échantillon dans l'anneau de façon à obtenir un
excès de produit au refroidissement. Laisser refroidir au moins 30 min et détacher l'excès de produit
sur le bord de l'anneau. Pour retirer l'excès de produit de la partie supérieure, découper proprement
l'excès du produit au moyen d'une spatule ou d'un couteau légèrement chauffé (5.2.2.2) ou saisir
l'anneau à l'aide de pinces et frotter la surface supérieure de l'éprouvette rapidement et fermement
contre la surface d'une plaque métallique chaude. Si la détermination est de nouveau effectuée, utiliser
un récipient propre et une nouvelle quantité d'échantillon.
2 © ISO 2020 – Tous droits réservés
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ISO 4625-1:2020(F)
5.3 Préparation des éprouvettes à partir d'échantillons ayant un point de
ramollissement bas (jusqu'à 35 °C)
5.3.1 Appareillage
5.3.1.1 Feuille d'aluminium.
5.3.1.2 Glace sèche [CO (solide)] ou congélateur.
2
5.3.1.3 Couteau ou spatule.
5.3.2 Mode opératoire
Prélever une quantité appropriée d'échantillon (voir 5.1). Placer l'un des anneaux (7.1.1) sur une feuille
d'aluminium (5.3.1.1). Verser le produit à soumettre à l'essai dans l'anneau. Ensuite, dispose
...
INTERNATIONAL ISO
STANDARD 4625-1
Second edition
2020-07
Binders for paints and varnishes —
Determination of softening point —
Part 1:
Ring-and-ball method
Liants pour peintures et vernis — Détermination du point de
ramollissement —
Partie 1: Méthode de l'anneau et de la bille
Reference number
ISO 4625-1:2020(E)
©
ISO 2020
---------------------- Page: 1 ----------------------
ISO 4625-1:2020(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
CH-1214 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 4625-1:2020(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Sampling and preparation of test pieces . 2
5.1 Sampling . 2
5.2 Preparation of test pieces by the pour method. 2
5.2.1 Field of application . 2
5.2.2 Apparatus . 2
5.2.3 Procedure . 2
5.3 Preparation of test pieces from samples with a low softening point (up to 35 °C) . 2
5.3.1 Apparatus . 2
5.3.2 Procedure . 3
6 Materials (heating-bath liquids) . 3
7 Automated ring-and-ball method (reference method) . 3
7.1 Apparatus . 3
7.2 Calibration . 4
7.3 Procedure for materials with a softening point between 35 °C and 80 °C . 4
7.4 Procedure for materials with a softening point between 80 °C and 150 °C . 4
7.5 Procedure for materials with a softening point above 150 °C . 4
8 Manual ring-and-ball method (alternate method) . 4
8.1 Apparatus . 4
8.2 Calibration . 7
8.3 Procedure . 7
8.3.1 Procedure for materials with a softening point between 35 °C and 80 °C . 7
8.3.2 Procedure for materials with a softening point between 80 °C and 150 °C . 8
8.3.3 Procedure for materials with a softening point above 150 °C . 8
8.3.4 Procedure for materials with a softening point below 35 °C . 8
9 Expression of results . 8
10 Precision and bias . 8
10.1 Precision of the automated method . 8
10.1.1 General. 8
10.1.2 Precision data . 8
10.2 Precision of the manual method . 9
10.2.1 General. 9
10.2.2 Precision data . 9
10.3 Bias . 9
11 Test report .10
Bibliography .11
© ISO 2020 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 4625-1:2020(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 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 35, Paints and varnishes, in collaboration
with the European Committee for Standardization (CEN) Technical Committee CEN/TC 139, Paints and
varnishes, in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna
Agreement).
This second edition cancels and replaces the first edition (ISO 4625-1:2004), which has been technically
revised. The main changes compared to the previous edition are as follows:
— the automated method has been classified to be the reference method;
— an introduction with information on all three methods described in the three parts of ISO 4625
series has been added;
— CAS-numbers have been added to the chemicals used;
— the text has been editorially revised;
— the normative references have been updated.
A list of all parts in the ISO 4625 series can be found on the ISO website.
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 4625-1:2020(E)
Introduction
The ISO 4625 series specifies three widely used procedures for the measurement of the softening point
of rosin-based resins. This document presents the ring-and-ball method, which has been the accepted
standard for many years. ISO 4625-2 presents the Mettler cup-and-ball method. A new method, called
the Mettler method without the ball, is to be presented in a future document.
This document is still the only standard test method accepted in regulatory documents such as Title 21
of the Code of Federal Regulations (CFR) – Food and Drugs.
Other parts of the ISO 4625 series concern Mettler cup-and-ball methods. Although the recommended
testing conditions differ, the only difference between the equipment required in such methods is that
Mettler method without the ball does not use a ball. Surveys have shown that the Mettler cup-and-ball
method specified in ISO 4625-2 is the most widely used in the USA, while the Mettler method without
the ball is the most widely used in Europe. These methods are less time consuming than the ring-and-
ball manual method and the equipment is less expensive than the ring-and-ball automated method.
As a consequence of the thermoplastic nature of the test resins, the softening points obtained using the
recommended test conditions for all three methods are not generally the same. Consequently, the test
method and the testing conditions used should be noted in the final report.
© ISO 2020 – All rights reserved v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 4625-1:2020(E)
Binders for paints and varnishes — Determination of
softening point —
Part 1:
Ring-and-ball method
1 Scope
This document specifies the test methods for determining the softening point of resins (including rosin)
and similar materials by means of ring-and-ball apparatus.
Both manual and automated methods are specified, the automated method being the reference method.
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 4618, Paints and varnishes — Terms and definitions
ISO 15528, Paints, varnishes and raw materials for paints and varnishes — Sampling
IEC 60751, Industrial platinum resistance thermometer and platinum temperature sensors
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 4618 and the following apply.
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/
3.1
softening point
temperature at which a disc of sample held within a horizontal ring is forced downward a distance of
25 mm under the weight of a steel ball as the disc is heated at a prescribed rate in a water, glycerol,
silicone oil, ethylene glycol/water or glycerol/water bath
4 Principle
In general, with materials of the types mentioned in Clause 1, softening does not take place at a definite
temperature. As the temperature rises, these materials gradually change from brittle or exceedingly
thick and slow-flowing materials to softer and less viscous liquids. For this reason, the determination
of the softening point shall be made by a fixed, closely defined method if the results obtained are to be
comparable.
For the purpose of these test methods, the definition of softening point given in Clause 3 applies.
© ISO 2020 – All rights reserved 1
---------------------- Page: 6 ----------------------
ISO 4625-1:2020(E)
5 Sampling and preparation of test pieces
5.1 Sampling
Take a representative sample of the product to be tested, as described in ISO 15528.
The sample shall consist of freshly broken lumps free of oxidized surfaces. For samples received as
small lumps, scrape off the surface layer of the lumps immediately before use, avoiding inclusion of
finely divided material or dust.
5.2 Preparation of test pieces by the pour method
5.2.1 Field of application
This preparation procedure is suitable for resins (including rosin) and other substances that can be
heated and poured without adverse effects on the softening point.
5.2.2 Apparatus
5.2.2.1 Container, in which the sample can be melted.
5.2.2.2 Knife or spatula.
5.2.2.3 Oven, hot-plate, sand bath or oil bath.
5.2.3 Procedure
Take a quantity of the sample (see 5.1) which is at least twice that necessary to fill the desired number
of rings (7.1.1), but in no case less than 40 g, and melt it immediately in a clean container (5.2.2.1)
using an oven, hot-plate, sand bath or oil bath (5.2.2.3) to prevent local overheating. Take care to
avoid incorporating air bubbles in the sample. Melt the sample completely, but do not heat it above
the minimum temperature necessary to pour it easily. The time from the beginning of heating to the
pouring of the sample shall not exceed 15 min.
For materials that are heat-sensitive, continuously inert the atmosphere in the container holding the
sample with nitrogen (N ) during the melting procedure.
2
For materials that tend to crack or shrink in the rings on cooling, preheat the rings immediately before
filling them to approximately the temperature at which the material is to be poured. The rings, while
being filled, shall rest on a suitable metal surface. Pour a sufficient quantity of the sample into the ring
so as to leave an excess on cooling. Allow to cool for at least 30 min and trim off the surplus material
at the periphery of the ring. To remove excess material from the top, cut the excess material off cleanly
with a slightly
...
FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 4625-1
ISO/TC 35
Binders for paints and varnishes —
Secretariat: NEN
Determination of softening point —
Voting begins on:
2020-04-03
Part 1:
Voting terminates on:
Ring-and-ball method
2020-05-29
Liants pour peintures et vernis — Détermination du point de
ramollissement —
Partie 1: Méthode de l'anneau et de la bille
ISO/CEN PARALLEL PROCESSING
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 4625-1:2020(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 4625-1:2020(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
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 2020 – All rights reserved
---------------------- Page: 2 ----------------------
ISO/FDIS 4625-1:2020(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Sampling and preparation of test pieces . 2
5.1 Sampling . 2
5.2 Preparation of test pieces by the pour method. 2
5.2.1 Field of application . 2
5.2.2 Apparatus . 2
5.2.3 Procedure . 2
5.3 Preparation of test pieces from samples with a low softening point (up to 35 °C) . 2
5.3.1 Apparatus . 2
5.3.2 Procedure . 3
6 Materials (heating-bath liquids) . 3
7 Automated ring-and-ball method (reference method) . 3
7.1 Apparatus . 3
7.2 Calibration . 4
7.3 Procedure for materials with a softening point between 35 °C and 80 °C . 4
7.4 Procedure for materials with a softening point between 80 °C and 150 °C . 4
7.5 Procedure for materials with a softening point above 150 °C . 4
8 Manual ring-and-ball method (alternate method) . 4
8.1 Apparatus . 4
8.2 Calibration . 7
8.3 Procedure . 7
8.3.1 Procedure for materials with a softening point between 35 °C and 80 °C . 7
8.3.2 Procedure for materials with a softening point between 80 °C and 150 °C . 8
8.3.3 Procedure for materials with a softening point above 150 °C . 8
8.3.4 Procedure for materials with a softening point below 35 °C . 8
9 Expression of results . 8
10 Precision and bias . 8
10.1 Precision of the automated method . 8
10.1.1 General. 8
10.1.2 Precision data . 8
10.2 Precision of the manual method . 9
10.2.1 General. 9
10.2.2 Precision data . 9
10.3 Bias . 9
11 Test report .10
Bibliography .11
© ISO 2020 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO/FDIS 4625-1:2020(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 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 35, Paints and varnishes, in collaboration
with the European Committee for Standardization (CEN) Technical Committee CEN/TC 139, Paints and
varnishes, in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna
Agreement).
This second edition cancels and replaces the first edition (ISO 4625-1:2004), which has been technically
revised. The main changes compared to the previous edition are as follows:
— the automated method has been classified to be the reference method;
— an introduction with information on all three methods described in the three parts of ISO 4625 has
been added;
— CAS-numbers have been added to the chemicals used;
— the text has been editorially revised;
— the normative references have been updated.
A list of all parts in the ISO 4625 series can be found on the ISO website.
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 4625-1:2020(E)
Introduction
The ISO 4625 series specifies three widely used procedures for the measurement of the softening point
of rosin-based resins. This document presents the ring-and-ball method, which has been the accepted
standard for many years. ISO 4625-2 presents the Mettler cup-and-ball method. A new method, called
the Mettler method without the ball, is to be presented in a future document.
This document is still the only standard test method accepted in regulatory documents such as Title 21
of the Code of Federal Regulations (CFR) – Food and Drugs.
Other parts of the ISO 4625 series concern Mettler cup-and-ball methods. Although the recommended
testing conditions differ, the only difference between the equipment required in such methods is that
Mettler method without the ball does not use a ball. Surveys have shown that the Mettler cup-and-ball
method specified in ISO 4625-2 is the most widely used in the USA, while the Mettler method without
the ball is the most widely used in Europe. These methods are less time consuming than the ring-and-
ball manual method and the equipment is less expensive than the ring-and-ball automated method.
As a consequence of the thermoplastic nature of the test resins, the softening points obtained using the
recommended test conditions for all three methods are not generally the same. Consequently, the test
method and the testing conditions used should be noted in the final report.
© ISO 2020 – All rights reserved v
---------------------- Page: 5 ----------------------
FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 4625-1:2020(E)
Binders for paints and varnishes — Determination of
softening point —
Part 1:
Ring-and-ball method
1 Scope
This document specifies the test methods for determining the softening point of resins (including rosin)
and similar materials by means of ring-and-ball apparatus.
Both manual and automated methods are specified, the automated method being the reference method.
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 4618, Paints and varnishes — Terms and definitions
ISO 15528, Paints, varnishes and raw materials for paints and varnishes — Sampling
IEC 60751, Industrial platinum resistance thermometer sensors
3 Terms and definitions
For the purposes of this document, the terms and definitions given in ISO 4618 and the following apply.
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/
3.1
softening point
temperature at which a disc of sample held within a horizontal ring is forced downward a distance of
25 mm under the weight of a steel ball as the disc is heated at a prescribed rate in a water, glycerol,
silicone oil, ethylene glycol/water or glycerol/water bath
4 Principle
In general, with materials of the types mentioned in Clause 1, softening does not take place at a definite
temperature. As the temperature rises, these materials gradually change from brittle or exceedingly
thick and slow-flowing materials to softer and less viscous liquids. For this reason, the determination
of the softening point shall be made by a fixed, closely defined method if the results obtained are to be
comparable.
For the purpose of these test methods, the above definition of softening point (3.1) applies.
© ISO 2020 – All rights reserved 1
---------------------- Page: 6 ----------------------
ISO/FDIS 4625-1:2020(E)
5 Sampling and preparation of test pieces
5.1 Sampling
Take a representative sample of the product to be tested, as described in ISO 15528.
The sample shall consist of freshly broken lumps free of oxidized surfaces. For samples received as
small lumps, scrape off the surface layer of the lumps immediately before use, avoiding inclusion of
finely divided material or dust.
5.2 Preparation of test pieces by the pour method
5.2.1 Field of application
This preparation procedure is suitable for resins (including rosin) and other substances that can be
heated and poured without adverse effects on the softening point.
5.2.2 Apparatus
5.2.2.1 Container, in which the sample can be melted.
5.2.2.2 Knife or spatula.
5.2.2.3 Oven, hot-plate, sand bath or oil bath.
5.2.3 Procedure
Take a quantity of the sample (see 5.1) which is at least twice that necessary to fill the desired number
of rings (7.1.1), but in no case less than 40 g, and melt it immediately in a clean container (5.2.2.1)
using an oven, hot-plate, sand bath or oil bath (5.2.2.3) to prevent local overheating. Take care to
avoid incorporating air bubbles in the sample. Melt the sample completely, but do not heat it above
the minimum temperature necessary to pour it easily. The time from the beginning of heating to the
pouring of the sample shall not exceed 15 min.
For materials that are heat-sensitive, continuously inert the atmosphere in the container holding the
sample with nitrogen (N ) during the melting procedure.
2
For materials that tend to crack or shrink in the rings on cooling, preheat the rings immediately before
filling them to approximately the temperature at which the material is to be poured. The rings, while
being filled, shall rest on a suitable metal surface.
...
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