ISO 2554:1974
(Main)Plastics — Unsaturated polyester resins — Determination of hydroxyl value
Plastics — Unsaturated polyester resins — Determination of hydroxyl value
Plastiques — Résines de polyesters non saturés — Détermination de l'indice d'hydroxyle
Polimerni materiali - Nenasičene poliestrske smole - Določanje hidroksilnega števila
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INTERNATIONAL STANDARD 2554
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION .MEXnYHAPOnHiUI OPTAHMJALIHR IT0 CTAHnAPTH3AUHH .ORGANISATION INTERNATIONALE DE NORMALISATION
Plastics - Unsaturated polyester resins - Determination of
i hydroxyl value
-gtiques - Résines de polyesters non saturés - Détermination de l’indice d‘hydroxyle
First edition - 1974-06-01
1
UDC 678.674 : 541.64 : 543.241 Ref. No. IS0 2554-1974 (E)
Descriptors : plastics, polyester resins, unsaturated chains, chemical analysis, hydroxyl value, determination.
Price based on 2 pages
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FOREWORD
IS0 (the International Organization for Standardization) is a worldwide federation
of national standards institutes (IS0 Member Bodies). The work of developing
International Standards is carried out through IS0 Technical Committees. Every
Member Body interested in a subject for which a Technical Committee has been set
up 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.
Draft International Standards adopted by the Technical Committees are circulated
to the Member Bodies fob approval before their acceptance as International
Standards by the IS0 Council.
International Standard IS0 2554 was drawn up by Technical Committee ISO/TC 61,
Plastics, and circulated to the Member Bodies in September 1971.
It has been approved by the Member Bodies of the following countries
Austria Hungary Romania
Nuth Africa, Rep. of
Belgium India
Brazil Israel Sweden
Canada Italy Switzerland
Thailand
Czechoslovakia Japan
Netherlands Turkey
Egypt, Arab Rep. of
Finland New Zealand United Kingdom
France Poland U.S.A.
Germany Portugal U.S.S.R.
No Member Body expressed disapproval of the document.
O Intariutiond Omniution for Standardization, 1974
Printed in Switzerland
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IS0 2554-1974 (E)
INTE RNATl ONAL STANDARD
Plastics - Unsaturated polyester resins - Determination of
hydroxyl value
1 SCOPE AND FIELD OF APPLICATION 5.2 Ethyl acetate, anhydrous
This International Standard specifies a method for
5.3 Pyridine/water mixture, 3 + 2 (V/V).
determining the hydroxyl value of unsaturated polyester
resins.
Mix 3 volumes of pyridine, analytical reagent quality, with
2 volumes of water.
In fact, this method determines the difference between the
hydroxyl value and the acid value; it is therefore necessary
to determine the acid value separately, in order to calculate
5.4 Butanol-l/toluene mixture, 2 + 1 (V/V)
the hydroxyl value.
NOTE - The hydroxyl yalue of saturated polyester resins (for
5.5 Mixed indicator solution.
example, polyester resin used for the manufacture of polyurethanes
and polymeric plasticizers) and of certain types of alkyd resins may
Mix 3 volumes of a 0,l % ethanolic solution of thymol blue
also be determined by this method.
with 1 volume of a 0.1 % ethanolic solution of cresol red.
2 REFERENCE
5.6 Potassium hydroxide, 0,5 N standard volumetric
solution in methanol.
IS0 21 14, Plastics - Unsaturated polyester resins -
Determination of acid value.
6 APPARATUS
3 DEFINITION
Ordinary laboratory apparatus, and
hydroxyl value : The number of milligrams of potassium
acetic acid which will
hydroxide necessary to neutralize the
combine by acetylation with 1 g of the unsaturated 6.1 Conical flask, capacity 250 ml, with a ground glass
polyester resin. stopper.
6.2 Magnetic stirrer, with a magnetic bar covered with a
4 PRINCIPLE
corrosion-resistant material (for example PTFE).
Acetylation of the hydroxyl groups by acetic anhydride is
carried out on an ethyl acetate solution of the resin in the
6.3 Burette, capacity 50 ml, graduated in 0,05 ml.
presence of toluene-4-sulphonic acid catalyst. The excess
acetic anhydride is hydrolyzed by a pyridine/water mixture
6.4 Water bath, controlled at a temperature of 50 f 1 OC.
and the resultant acetic acid titrated with standard
volumetric methanolic potassium hydroxide solution.
6.5 Pipette, capacity 10 ml (for the acetylating solution).
In this titration, the free acid groups which exist in the
6.6 If necessary : Apparatus for potentiometric titration.
resin are also neutralized by the potassium hydroxide. The
hydroxyl value is finally calculated by taking into account
the acid value determined separately.
7 PROCEDURE
Weigh, to the nearest 1 mg, in the 250 ml conical flask
5 REAGENTS
(6.1 1, a test portion of the resin containing approximately
5 milli-equivalents of OH (the mass in grams of the
5.1 Acetic anhydride acetylating solution, approximately
sample = 280/hydroxyl value).
1 M, in ethyl acetate.
NOTE - If the approximate hydroxyl value is not known,
Dissolve 1,4 g of pure, dry toluene-4-çulphonic acid in
pre
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.GURNVLOQHJDãWHYLODPlastiques -- Résines de polyesters non saturés -- Détermination de l'indice d'hydroxylePlastics -- Unsaturated polyester resins -- Determination of hydroxyl value83.080.10DuromeriThermosetting materialsICS:Ta slovenski standard je istoveten z:ISO 2554:1974SIST ISO 2554:1996en01-junij-1996SIST ISO 2554:1996SLOVENSKI
STANDARD
SIST ISO 2554:1996
INTERNATIONAL STANDARD 2554 INTERNATIONAL ORGANIZATION FOR STANDARDIZATION .MEXnYHAPOnHiUI OPTAHMJALIHR IT0 CTAHnAPTH3AUHH .ORGANISATION INTERNATIONALE DE NORMALISATION Plastics - Unsaturated polyester resins - Determination of i hydroxyl value -gtiques - Résines de polyesters non saturés - Détermination de l’indice d‘hydroxyle 1 First edition - 1974-06-01 UDC 678.674 : 541.64 : 543.241 Ref. No. IS0 2554-1974 (E) Descriptors : plastics, polyester resins, unsaturated chains, chemical analysis, hydroxyl value, determination. Price based on 2 pages -- ./ - SIST ISO 2554:1996
FOREWORD IS0 (the International Organization for Standardization) is a worldwide federation of national standards institutes (IS0 Member Bodies). The work of developing International Standards is carried out through IS0 Technical Committees. Every Member Body interested in a subject for which a Technical Committee has been set up 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. Draft International Standards adopted by the Technical Committees are circulated to the Member Bodies fob approval before their acceptance as International Standards by the IS0 Council. International Standard IS0 2554 was drawn up by Technical Committee ISO/TC 61, Plastics, and circulated to the Member Bodies in September 1971. It has been approved by the Member Bodies of the following countries Austria Belgium Brazil Canada Czechoslovakia Egypt, Arab Rep. of Finland France Germany Hungary India Israel Italy Japan Netherlands New Zealand Poland Portugal No Member Body expressed disapproval of the document. Romania Nuth Africa, Rep. of Sweden Switzerland Thailand Turkey United Kingdom U.S.A. U.S.S.R. O Intariutiond Omniution for Standardization, 1974 Printed in Switzerland SIST ISO 2554:1996
INTE RNATl ONAL STANDARD IS0 2554-1974 (E) Plastics - Unsaturated polyester resins - Determination of hydroxyl value 1 SCOPE AND FIELD OF APPLICATION This International Standard specifies a method for determining the hydroxyl value of unsaturated polyester resins. In fact, this method determines the difference between the hydroxyl value and the acid value; it is therefore necessary to determine the acid value separately, in order to calculate the hydroxyl value. NOTE - The hydroxyl yalue of saturated polyester resins (for example, polyester resin used for the manufacture of polyurethanes and polymeric plasticizers) and of certain types of alkyd resins may also be determined by this method. 2 REFERENCE IS0 21 14, Plastics - Unsaturated polyester resins - Determination of acid value. 3 DEFINITION hydroxyl value : The number of milligrams of potassium hydroxide necessary to neutralize the acetic acid which will combine by acetylation with 1 g of the unsaturated polyester resin. 4 PRINCIPLE Acetylation of the hydroxyl groups by acetic anhydride is carried out on an ethyl acetate solution of the resin in the presence of toluene-4-sulphonic acid catalyst. The excess acetic anhydride is hydrolyzed by a pyridine/water mixture and the resultant acetic acid titrated with standard volumetric methanolic potassium hydroxide solution. In this titration, the free acid groups which exist in the resin are also neutralized by the potassium hydroxide. The hydroxyl value is finally calculated by taking into account the acid value determined separately. 5 REAGENTS 5.1 Acetic anhydride acetylating solution, approximately 1 M, in ethyl acetate. Dissolve 1,4 g of pure, dry toluene-4-çulphonic acid in 111 ml of anhydrous ethyl acetate. When completely dissolved, slowly add, while mixing, 12 ml of freshly distilled acetic anhydride and store in a dry atmosphere. 5.2 Ethyl acetate, anhydrous 5.3 Pyridine/water mixture, 3 + 2 (V/V). Mix 3 volumes of pyridine, analytical reagent quality, with 2 volumes of water. 5.4 Butanol-l/toluene mixture, 2 + 1 (V/V) 5.5 Mixed indicator solution. Mix 3 volumes of a 0,l % ethanolic solution of thymol blue with 1 volume of a 0.1 % ethanolic solution of cresol red. 5.6 Potassium hydroxide, 0,5 N standard volumetric solution in methanol. 6 APPARATUS Ordinary laboratory apparatus, and 6.1 Conical flask, capacity 250 ml, with a ground glass stopper. 6.2 Magnetic stirrer, with a magnetic bar covered with a corrosion-resistant material (for example PTFE). 6.3 Burette, capacity 50 ml, graduated in 0,05 ml. 6.4 Water bath, controlled a
...
NORME INTERNATIONALE 2554
INTERNATIONAL ORGANIZATION FOR STANDAROIZATION .MEXnYHAWIIHAR OPiAHWUUHR no CTAHnAPTW3AUHH -ORGANISATION INTERNATIONALE DE NORMALISATION
iWtièm@stiques - Résines de polyesters non saturés -
Détermination de l'indice d'hydroxyle
Plastics - Unsaturated polyester resins - Determination of h ydroxyl value
*
Première édition - 1974-06-01
CDU 678.674 : 541.64 : 543.241 Réf. NO : IS0 2554-1974 (F)
Descripteurs : matière plastique, polyester. chaîne non saturée, analyse chimique, indice hydroxyle, détermination.
Prix base sur 2 pages
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AVANT-PROPOS
L'ISO (Organisation Internationale de Normalisation) est une fédération mondiale
ISO). L'élaboration de
d'organismes nationaux de normalisation (Comités Membres
Normes Internationales est confiée aux Comités Techniques ISO. Chaque Comité
Membre intéressé par une étude a le droit de faire partie du Comité Technique
correspondant. Les organisations internationales, gouvernementales et non
gouvernementales, en liaison avec I'ISO, participent également aux travaux.
Les Projets de Normes Internationales adoptés par les Comités Techniques sont
soumis aux Comités Membks pour approbation, avant leur acceptation comme
Normes Internationales par le Conseil de I'ISO.
La Norme lnternati nale IS0 2554 a été établie par le Comité Technique
61, Me@ibm~astiques, et soumise aux Comités Membres en septembre
ISO/TC
1971.
Elle a été approuvée par les Comités Membres des pays suivants :
Afrique du Sud, Rép. d' Roumanie
Hongrie
Allemagne Royaume-Uni
Inde
Israël Suède
Autriche
Belgique Italie Suisse
Brésil Japon Tchécoslovaquie
Canada Nouvelle-Zélande Thaïlande
Egypte, Rép. arabe d' Pays-Bas Turquie
Finlande Po log ne U.R.S.S.
France Portugal U.S.A.
Aucun Comité Membre n'a désapprouvé le document.
O Otganisation Internationale de Normalisation, 1974 a
Imprimé en Suisse
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NORME INTERNATIONALE IS0 2554-1974 (F)
4AaMiwWastiques - Résines de polyesters non satures -
Détermination de l‘indice d’hydroxyle
7 OBJET ET DOMAINE D’APPLICATION Dissoudre 1.4 g d’acide toluene-4-sulfonique pur et sec dans
11 1 ml d’acétate d’éthyle anhydre. Quand la dissolution est
La présente Norme lrternationale spécifie une méthode
totale, ajouter lentement, en agitant, 12 ml d‘anhydride
pour déterminer l‘indice d’hydroxyle des résines de
acétique fraîchement distillé et conserver en atmosphère
polyesters non saturés.
sèche
Cette méthode détermine en fait la différence entre l’indice
5.2 Acétate d’éthyle, anhydre
d’hydroxyle et l’indice d’acide; il est donc nécessaire d‘avoir
déterminé pnr riilleurs l‘indice d’acide du produit pour
5.3 Pyridine/eau. mélange à 3 + 2 (ViV).
calculer I’indir:e d‘hydroxyle.
Mélanger 3 volumes de pyridine, pure pour analyse, à
NOTE - L’indice d‘hydroyyle de résines de polyesters saturés (par
exemple les résines polyesters utilisées pour la fabrication des 2 volumes d‘eau.
polyuréthannes et les plastifiants polymeriques) et de certains types
de résines alkydes. peut également être détermine par cette
5.4 Butanol-l/toluène, mélange à 2 + 1 (V/V)
méthode
5.5 Indicateur mixte, solution
2 RÉFÉRENCE
Mélanger 3 volumes d’une solution éthanolique de bleu de
thymol à 0,l % avec 1 volume d‘une solution éthanolique
IS0 21 14, Matières plastiques - Résines de polyesters non
de rouge de crésol, à 0.1 %.
saturés - Détermination de l’indice d‘acide.
5.6 Hydroxyde de potassium, solution titrée 0.5 N dans le
méthanol.
3 DÉFINITION
indice d‘hydroxyle : Nombi e de milligrammes d’hydroxyde
de potassium nécessaire pour neutraliser l’acide acétique qui
6 APPAREILLAGE
se combine par acétylation a 1 y de iésine de polyester non
Matériel courant de laboratoire. et
saturé
6.1 Fiole conique, a bouchon rodé, capacité 250 ml
4 PRINCIPE
6.2 Agitateur magnétique, muni d‘un barreau aimanté
L’acétylation des groupes hydroxyles par l’anhydride
recouvert de produit inattaquable (PTFE par exemple).
acétique est réalisée en solution d’acétate d‘éthyle en
présence d’acide toluene-4-sulfonique comme catalyseur.
6.3 Burette, capacité 50 ml, graduée en 0,05 ml.
L‘excès d‘anhydride acétique est hydrolysé par un mélange
de pyridine et d‘eau et l’acide acétique résultant est titré
par une solution volumétrique méthanolique titrée
6.4 Bain d’eau, réglable à 50 ? 1 OC.
d‘hydroxyde de potassium.
6.5 Pipette, capacité 10 ml (pour la solution acétylante).
Au cours de ce titrage, les groupes acides libres qui existent
dans la résine sont aussi neutralisés par l‘hydroxyde de
6.6 Si besoin est : Dispositif de titrage potentiométrique.
potassium.
L’indice d‘hydroxyle est finalement calculé en tenant
7 MODE OPÉRATOIRE
compte de la valeur de l‘indice d’acide déterminé
séparément.
Dans la fiole conique de 250 ml (6.1 1, peser, à 1 mg près,
une prise d‘essai
...
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