ISO 1159:1978
(Main)Plastics — Vinyl chloride-vinyl acetate copolymers — Determination of vinyl acetate
Plastics — Vinyl chloride-vinyl acetate copolymers — Determination of vinyl acetate
Plastiques — Copolymères chlorure de vinyle-acétate de vinyle — Détermination de la teneur en acétate de vinyle
Polimerni materiali - Kopolimeri vinilklorid-vinilacetat - Določanje odstotka vinilacetata
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INTERNATIONAL STANDARD
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION.ME)YHAPO~HAR OPTAHM3AL@lR I-IO CTAH,QAPTbl3A~MM.ORGANlSATlON INTERNATIONALE DE NORMALISATION
Plastics - Vinyl chloride-vinyl acetate copolymers -
Determination of vinyl acetate .
Plastiques - Copolymkes chlorure de vinyle-a&ate de vinyle - Dbermination de
la teneur en a&ate de vin yle
First edition - 1978-09-01
Ref. No. IS0 1159-1978 (E)
UDC 678.743-13 : 543.24 : 547.292 ’26
Descriptors : plastics, copolymers, vinyl chloride, vinyl acetate, chemical analysis, determination of content.
Price based on 4 pages
6
c
i3elsgP,
-1
43
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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 for approval before their acceptance as International
Standards by the IS0 Council.
International Standard IS0 1159 was developed by Technical Committee
I SO/TC 6 1, Plastics.
It was submitted directly to the IS0 Council, in accordance with clause 6.13.1
of the Directives for the technical work of ISO. It cancels and replaces
IS0 Recommendation R 11594970, which had been approved by the member
bodies of the following countries :
Australia Germany Romania
Austria Greece Sweden
Belgium Hungary Switzerland
Brazil India Turkey
Canada Ireland
United Kingdom
Chile Italy
U.S.A.
Czechoslovakia Japan U.S.S.R.
Egypt, Arab Rep. of Netherlands Yugoslavia
Finland New Zealand
France Poland
No member body had expressed disapproval of the document.
Cc> International Organization for Standardization, 1978 l
Printed in Switzerland
---------------------- Page: 2 ----------------------
IS0 11594978 (E)
INTERNATIONAL STANDARD
- vinyl chloride-vinyl acetate copolymers -
Plastics
.
Determination of vinyl acetate
3.6 Silver nitrate, 0,05 N standard volumetric solution.
1 SCOPE AND FIELD OF APPLICATION
This International Standard specifies a method for deter-
3.7 Pure tetrahydrofuran, further purified as described
mining the percentage of vinyl acetate in vinyl chloride-
in 7.2.
vinyl acetate copolymers.
3.8 Ethanol-water mixture (I : 1 by volume), neutralized
to thymol blue, prepared from freshly boiled distilled
2 PRINCIPLE
water.
Dissolution of a test portion in purified tetrahydrofuran,
and hydrolysis of the acetate groups by ethanolic potassium
3.9 Thymol blue indicator solution.
hydroxide solution.
Dissolve 0,l g of thymol blue in 100 ml of ethanol.
Back-titration of excess potassium hydroxide with sul-
phuric acid, using thymol blue as indicator.
3.10 Potassium hydroxide, solid pellets.
Argentometric titration of hydrogen chloride liberated
during hydrolysis.
3.11 Potassium chromate, 50 g/l solution.
3 REAGENTS
4 APPARATUS
3.1 Potassium hydroxide, ethanolic solution approxi-
4.1 Burette, 25 ml, for acidimetry.
mately 0,5 N.
Dissolve 33 g of solid potassium hydroxide (KOH) in
4.2 Burette, IO ml, for argentometry.
500 ml of ethanol. Make up to 1 000 ml, allow to stand
overnight and decant the clear portion of the solution.
4.3 Electromagnetic stirrer.
3.2 Potassium hydroxide, ethanolic solution approxi-
4.4 Thermostatically controlled water bath, to maintain a
mately 02 N.
temperature of 30 +, 0,5 “C (see 7.1).
Prepare the solution in the same way as in 3.1, but dissolv-
ing only 13,5 g of solid potassium hydroxide in the ethanol.
4.5 Analytical balance, to weigh to an accuracy of
+ 0,000 1 g.
3.3 Sulphuric acid, 0,l N standard volumetric solution.
4.6 Volumetric flask, 100 ml capacity, with ground glass
stopper.
3.4 Sulphuric acid, 0,05 N standard volumetric solution. _
4.7 Pipettes, of 1, 5, 20 and 30 ml capacity.
3.5 Silver nitrate, 0,l N standard volumetric solution.
---------------------- Page: 3 ----------------------
ISO1159-1978(E)
6 EXPRESSION OF RESULTS
5 PROCEDURE
5.1 The time necessary for a quantitative saponification 6.1 When using 0,l N sulphuric acid and silver nitrate
of vinyl acetate groups depends on the vinyl acetate solutions, the vinyl acetate content, as a percentage by
content, the concentration of the ethanolic potassium mass, is given by the formula :
hydroxide solution used, the temperature and the mass
0,860 9 (V, - v, - V,)
of the test portion. Consequently, choose the appropriate
m
conditions as indicated in the table below, taking into
account the assumed vinyl acetate content of the copolymer
and the temperature at which saponification will take place.
6.2 When using 0,05 N sulphuric acid and silver nitrate
solutions, the vinyl acetate content, as a percentage by
mass, is given by the formula :
5.2 Accurately weigh-- out the test portion of dry
copolymer indicated in the- table into the flask (4.6) (see
0,4304(V, -v2-V3)
7.3) and add 20 ml of tetrahydrofuran (3.7) by means of
m
a pipette. The dissolution of the copolymer is facilitated
by using the magnetic stirrer (4.3). After complete dis-
where
solution, immerse the flask in the thermostatted bath at
30 “C and leave it for 10 min; add 5 ml of ethanolic pot- VI is the volume, in millilitres, of sulphuric acid used
assium hydroxide solution of the concentration indicated in the blank test;
in the table and thoroughly mix the contents of the flask
V, is the volume, in millilitres, of sulphuric acid used
by a gentle swirling motion. In case partial precipitation
...
SLOVENSKI STANDARD
SIST ISO 1159:1996
01-junij-1996
3ROLPHUQLPDWHULDOL.RSROLPHULYLQLONORULGYLQLODFHWDW'RORþDQMHRGVWRWND
YLQLODFHWDWD
Plastics -- Vinyl chloride-vinyl acetate copolymers -- Determination of vinyl acetate
Plastiques -- Copolymères chlorure de vinyle-acétate de vinyle -- Détermination de la
teneur en acétate de vinyle
Ta slovenski standard je istoveten z: ISO 1159:1978
ICS:
83.080.20 Plastomeri Thermoplastic materials
SIST ISO 1159:1996 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
---------------------- Page: 1 ----------------------
SIST ISO 1159:1996
---------------------- Page: 2 ----------------------
SIST ISO 1159:1996
INTERNATIONAL STANDARD
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION.ME)YHAPO~HAR OPTAHM3AL@lR I-IO CTAH,QAPTbl3A~MM.ORGANlSATlON INTERNATIONALE DE NORMALISATION
Plastics - Vinyl chloride-vinyl acetate copolymers -
Determination of vinyl acetate .
Plastiques - Copolymkes chlorure de vinyle-a&ate de vinyle - Dbermination de
la teneur en a&ate de vin yle
First edition - 1978-09-01
Ref. No. IS0 1159-1978 (E)
UDC 678.743-13 : 543.24 : 547.292 ’26
Descriptors : plastics, copolymers, vinyl chloride, vinyl acetate, chemical analysis, determination of content.
Price based on 4 pages
6
c
i3elsgP,
-1
43
---------------------- Page: 3 ----------------------
SIST ISO 1159:1996
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 for approval before their acceptance as International
Standards by the IS0 Council.
International Standard IS0 1159 was developed by Technical Committee
I SO/TC 6 1, Plastics.
It was submitted directly to the IS0 Council, in accordance with clause 6.13.1
of the Directives for the technical work of ISO. It cancels and replaces
IS0 Recommendation R 11594970, which had been approved by the member
bodies of the following countries :
Australia Germany Romania
Austria Greece Sweden
Belgium Hungary Switzerland
Brazil India Turkey
Canada Ireland
United Kingdom
Chile Italy
U.S.A.
Czechoslovakia Japan U.S.S.R.
Egypt, Arab Rep. of Netherlands Yugoslavia
Finland New Zealand
France Poland
No member body had expressed disapproval of the document.
Cc> International Organization for Standardization, 1978 l
Printed in Switzerland
---------------------- Page: 4 ----------------------
SIST ISO 1159:1996
IS0 11594978 (E)
INTERNATIONAL STANDARD
- vinyl chloride-vinyl acetate copolymers -
Plastics
.
Determination of vinyl acetate
3.6 Silver nitrate, 0,05 N standard volumetric solution.
1 SCOPE AND FIELD OF APPLICATION
This International Standard specifies a method for deter-
3.7 Pure tetrahydrofuran, further purified as described
mining the percentage of vinyl acetate in vinyl chloride-
in 7.2.
vinyl acetate copolymers.
3.8 Ethanol-water mixture (I : 1 by volume), neutralized
to thymol blue, prepared from freshly boiled distilled
2 PRINCIPLE
water.
Dissolution of a test portion in purified tetrahydrofuran,
and hydrolysis of the acetate groups by ethanolic potassium
3.9 Thymol blue indicator solution.
hydroxide solution.
Dissolve 0,l g of thymol blue in 100 ml of ethanol.
Back-titration of excess potassium hydroxide with sul-
phuric acid, using thymol blue as indicator.
3.10 Potassium hydroxide, solid pellets.
Argentometric titration of hydrogen chloride liberated
during hydrolysis.
3.11 Potassium chromate, 50 g/l solution.
3 REAGENTS
4 APPARATUS
3.1 Potassium hydroxide, ethanolic solution approxi-
4.1 Burette, 25 ml, for acidimetry.
mately 0,5 N.
Dissolve 33 g of solid potassium hydroxide (KOH) in
4.2 Burette, IO ml, for argentometry.
500 ml of ethanol. Make up to 1 000 ml, allow to stand
overnight and decant the clear portion of the solution.
4.3 Electromagnetic stirrer.
3.2 Potassium hydroxide, ethanolic solution approxi-
4.4 Thermostatically controlled water bath, to maintain a
mately 02 N.
temperature of 30 +, 0,5 “C (see 7.1).
Prepare the solution in the same way as in 3.1, but dissolv-
ing only 13,5 g of solid potassium hydroxide in the ethanol.
4.5 Analytical balance, to weigh to an accuracy of
+ 0,000 1 g.
3.3 Sulphuric acid, 0,l N standard volumetric solution.
4.6 Volumetric flask, 100 ml capacity, with ground glass
stopper.
3.4 Sulphuric acid, 0,05 N standard volumetric solution. _
4.7 Pipettes, of 1, 5, 20 and 30 ml capacity.
3.5 Silver nitrate, 0,l N standard volumetric solution.
---------------------- Page: 5 ----------------------
SIST ISO 1159:1996
ISO1159-1978(E)
6 EXPRESSION OF RESULTS
5 PROCEDURE
5.1 The time necessary for a quantitative saponification 6.1 When using 0,l N sulphuric acid and silver nitrate
of vinyl acetate groups depends on the vinyl acetate solutions, the vinyl acetate content, as a percentage by
content, the concentration of the ethanolic potassium mass, is given by the formula :
hydroxide solution used, the temperature and the mass
0,860 9 (V, - v, - V,)
of the test portion. Consequently, choose the appropriate
m
conditions as indicated in the table below, taking into
account the assumed vinyl acetate content of the copolymer
and the temperature at which saponification will take place.
6.2 When using 0,05 N sulphuric acid and silver nitrate
solutions, the vinyl acetate content, as a percentage by
mass, is given by the formula :
5.2 Accurately weigh-- out the test portion of dry
copolymer indicated in the- table into the flask (4.6) (see
0,4304(V, -v2-V3)
7.3) and add 20 ml of tetrahydrofuran (3.7) by means of
m
a pipette. The dissolution of the copolymer is facilitated
by using the magnetic stirrer (4.3). After complete dis-
where
solution, immerse the flask in the thermostatted ba
...
NORME INTERNATIONALE @
INTERNATIONAL ORGANIZATION FOR STANDARDIZATlON.MEMYHAPOnHAR OPrAHM3AUMR no CTAH~APTH3AUMM.ORGANlSATlON INTERNATIONALE DE NORMALIS=
Plastiques - Copolymères chlorure de vinyle-acétate de
vinyle - Détermination de la teneur en acétate de vinyle
Plastics - Vinyl chloride-vinyl acetate copolymers - Determination of vinyl acetate
Première édition - 1978-09-01
..
U
1
CDU 678.743-13 543.24 : 547.292'26 Réf. no : IS0 1159-1978 (F)
CI
e
Descripteun : plastique, copolymère, chlorure de vinyle, acétate de vinyle, analyse chimique, dosage.
m
Ln
-
-
U
2
Prix basé sur 4 pages
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AVANT-PROPOS
L'ISO (Organisation internationale de normalisation) est une fédération mondiale
d'organismes nationaux de normalisation (comités membres de I'ISO). L'élaboration
des Normes internationales est confiée aux comités techniques de I'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 membres pour approbation, avant leur acceptation comme
Normes internationales par le Conseil de 1'1S0.
La Norme internationale JSO 1159 a été élaborée par le comité technique
ISO/TC 61, Plastiques.
Elle fut soumise directement au Conseil de I'ISO, conformément au paragraphe
6.13.1 des Directives pour les travaux techniques de I'ISO. Elle annule et remplace
la Recommandation ISO/R 1159-1970, qui avait été approuvée par les comités
membres des pays suivants :
Allemagne Grèce Royaume-Uni
Australie Hongrie Suède
Autriche Inde
Suisse
Belgique Irlande Tchécoslovaquie
Brésil Italie Turquie
Canada Japon U.R.S.S.
Chili Nouvelle-Zélande U.S.A.
Egypte, Rép. arabe d' Pays-Bas Yougoslavie
Fin I ande Pologne
France Roumanie
Aucun comité membre ne l'avait désapprouvée.
'3 Organisation internationale de normalisation, 1978
Imprimé en Suisse
---------------------- Page: 2 ----------------------
NORME INTERNATIONALE IS0 1159-1978 (F)
Plastiques - Copolymères chlorure de vinyle-acétate de
vinyle - Détermination de la teneur en acétate de vinyle
1 OBJET ET DOMAINE D‘APPLICATION 3.5 Nitrate d‘argent, solution titrée 0,l N.
La présente Norme internationale spécifie une méthode
3.6 Nitrate d‘argent, solution titrée 0,05 N.
de dosage de l’acétate de vinyle dans les copolymeres
chlorure de vinyle-acétate de vinyle.
3.7 Tétrahydrofurane pur, purifié comme indiqué en 7.2.
2 PRINCIPE
3.8 Mélange éthanol-eau (1 : 1 en volume), préparé à pat-
tir d’eau distillée bouillie, neutralisé en présence de bleu de
Dissolution de la prise d‘essai dans du tétrahydrofurane
thymol.
purifié et hydrolyse des groupes acétate par l’hydroxyde
de potassium en solution éthanolique.
3.9 Bleu de thymol (indicateur).
Titrage en retour de l’excès d‘hydroxyde de potassium
Dissoudre 0,l g de bleu de thymol dans 100 ml d’éthanol.
par l’acide sulfurique, en présence de bleu de thymol
comme indicateur.
3.10 Hydroxyde de potassium solide, en pastilles.
Titrage argentimétrique de l’acide chlorhydrique libéré
pendant I ’hydrolyse.
3.11 Chromate de potassium, solution à 50 g/I
3 REACTIFS
3.1 Hydroxyde de potassium, solution éthanolique 0,5 N
4 APPAREILLAGE
environ.
4.1
Dissoudre 33 g d‘hydroxyde de potassium (KOH) solide Burette de 25 ml pour l’acidimétrie.
dans 500 ml d‘éthanol. Compléter a 1 O00 ml, laisser
reposer une nuit et décanter ia portion limpide de la so-
4.2 Burette de 10 ml pour I’argentimétrie.
lution.
4.3 Agitateur électromagnétique.
3.2 Hydroxyde de potassium, solution éthanolique 0,2 N
environ.
4.4 Bain thermorégularisé, permettant de maintenir la
température a 30 2 0,5 “C (voir 7.1).
Préparer la solution comme indiqué en 3.1, mais en ne
dissolvant que 13,5 g d’hydroxyde de potassium solide
4.5 Balance analytique, précise a 0,000 1 g.
dans l’éthanol.
4.6 Fiole jaugée de 100 ml, avec bouchon rodé en verre.
3.3 Acide sulfurique, solution titrée 0,l N.
3.4 Acide sulfurique, solution titrée 0,05 N. 4.7 Pipettes de 1, 5, 20 et 30 ml de capacité.
1
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5 MODE OPERATOIRE 6 EXPRESSION DES RÉSULTATS
5.1 Le temps nécessaire a une saponification quanti- 6.1 Lorsque des solutions 0.1 N d'acide sulfurique et de
tative des groupes acétate de vinyle dépend de la teneur nitrate d'argent sont utilisées, la teneur en acétate de
en acétate de vinyle, de la concentration de la solution vinyle, en pourcentage en masse, est donnée par la formule
éthanolique d'hydroxyde de potassium utilisée, de la
0,860 9 (V, - V, - V,)
température et de la masse de la prise d'essai. En consé-
rn
quence, choisir les conditions appropriées, comme indiqué
au tableau, ci-dessous, en tenant compte de la teneur présu-
mée en acétate de vinyle dans le copolymère et de la 6.2 Lorsque des solutions 0,05 N d'acide sulfurique et
température à laquelle a lieu la saponification. de nitrate d'argent sont utilisées, la teneur en acétate de
vinyle, en pourcentage en masse, est donnée par la formule
5.2 Peser avec précision, dans la fiole (4.6) (voir 7.3), une
O,4304(V, -V,-V,)
prise d'essai de copolymère sec, déterminée selon les indi-
rn
cations du tableau. Au moyen d'une pipette, ajouter
20 ml de tétrahydrofurane (3.7). L'agitateur électroma-
où
gnétique (4.3) permet d'obtenir une dissolution plus
facile du copolymère. Après dissolution complete, immer-
V, est le volume, en millilitres, d'acide sulfurique
ger le flacon pendant 10 min dans le bain thermorégu-
utilisé dans l'essai à blanc;
larisé a 30 OC; ajouter 5 ml de la solution éthanolique
V, est le volume, en millilitres, d'acide sulfurique
d'hydroxyde de potassium de la concentration indiquée
utilisé dans la détermination;
dans le tableau; assurer le mélange parfait par une légère
agitation circulaire. Au cas où une précipitation partielle
est le volume, en millilitres, de solution de nitrate
V,
du copolymere survient a ce stade, agiter pour redissoudre.
d'argent utilisé;
...
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