SIST EN ISO 15512:2019
(Main)Plastics - Determination of water content (ISO 15512:2019)
Plastics - Determination of water content (ISO 15512:2019)
This document specifies methods for the determination of the water content of plastics in the form of
powder, granules, and finished articles. These methods do not test for water absorption (kinetics and
equilibrium) of plastics as measured by ISO 62.
Method A is suitable for the determination of water content as low as 0,1 % with an accuracy of 0,1 %.
Method B and Method C are suitable for the determination of water content as low as 0,01 % with an
accuracy of 0,01 %. Method D is suitable for the determination of water content as low as 0,01 % with an
accuracy of 0,01 %. Method E is suitable for the determination of water content as low as 0,001 % with
an accuracy of 0,001 %. The stated accuracies are detection limits which depend also on the maximal
possible sample mass. The water content is expressed as a percentage mass fraction of water.
Method D is suitable for polyamide (PA), polycarbonate (PC), polypropylene (PP), polyethylene (PE), epoxy
resin, polyethylene terephthalate (PET), polyester, polytetrafluoroethylene (PTFE), polyvinyl chloride
(PVC), polylactide (PLA), polyamidimid (PAI), it is especially not recommended for samples which can
release NH3. Methods A, B, C and E are generally suitable for all types of plastic and moisture level.
Water content is an important parameter for processing materials and is expected to remain below the
level specified in the appropriate material standard.
Six alternative methods are specified in this document.
— Method A is an extraction method using anhydrous methanol followed by a Karl Fischer titration
of the extracted water. It can be used for all plastics and is applicable to granules smaller than
4 mm × 4 mm × 3 mm. The method can also be used for, e.g. prepolymer materials in the form of a
powder that are insoluble in methanol.
— Method B1 is a vaporization method using a tube oven. The water contained in the test portion is
vaporized and carried to the titration cell by a dry air or nitrogen carrier gas, followed by a Karl
Fischer titration or a coulometric determination by means of a moisture sensor of the collected
water. It can be used for all plastics and is applicable to granules smaller than 4 mm × 4 mm × 3 mm.
— Method B2 is a vaporization method using a heated sample vial. The water contained in the test
portion is vaporized and carried to the titration cell by a dry air or nitrogen carrier gas, followed
by a Karl Fischer titration of the collected water. It can be used for all plastics and is applicable to
granules smaller than 4 mm × 4 mm × 3 mm.
— Method C is a manometric method. The water content is determined from the increase in pressure,
which results when the water is evaporated under a vacuum. This method is not applicable to plastic
samples containing volatile compounds, other than water, in amounts contributing significantly
to the vapour pressure at room temperature. Checks for the presence of large amounts of volatile
compounds are to be carried out periodically, for example by gas chromatography. Such checks are
particularly required for new types or grades of material.
— Method D is a thermocoulometric method using a diphosphorus pentoxide (P2O5) cell for the
detection of the vaporized water. The water contained in the test portion is vaporized and carried
to the sensor cell by a dry air or nitrogen carrier gas, followed by a coulometric determination of
the collected water. This method is not applicable to plastic samples containing volatile compounds,
other than water, in amounts contributing significantly to the vapour pressure at room temperature.
This is specially related to volatile components which can react with the acidic coating of the
diphosphorus pentoxide sensor, e.g. ammonia or any kind of amines. Checks for the presence of
large amounts of volatile compounds are to be carried out periodically. Such checks are particularly
required for new types or grades of material.
Method E...
Kunststoffe - Bestimmung des Wassergehaltes (ISO 15512:2019)
Dieses Dokument legt Verfahren zur Bestimmung des Wassergehalts von Kunststoffen fest, die als Pulver, Granulat oder Fertigerzeugnis vorliegen. Bei diesen Verfahren wird nicht, wie nach ISO 62, die Wasseraufnahme (Kinetik und Gleichgewicht) von Kunststoffen geprüft.
Verfahren A ist für die Bestimmung des Wassergehalts bis hinab zu 0,1 % mit einer Messunsicherheit von 0,1 % geeignet. Verfahren B und C sind für die Bestimmung des Wassergehalts bis hinab zu 0,01 % mit einer Messunsicherheit von 0,01 % geeignet. Verfahren D ist für die Bestimmung des Wassergehalts bis hinab zu 0,01 % mit einer Messunsicherheit von 0,01 % geeignet. Verfahren E ist für die Bestimmung des Wassergehalts bis hinab zu 0,001 % mit einer Messunsicherheit von 0,001 % geeignet. Die angegebenen Messunsicherheiten sind Nachweisgrenzen, die außerdem von der größten möglichen Probenmasse abhängen. Der Wassergehalt wird als Massenanteil an Wasser in Prozent ausgedrückt.
Verfahren D ist geeignet für Polyamid (PA), Polycarbonat (PC), Polypropylen (PP), Polyethylen (PE), Epoxidharz, Polyethylenterephthalat (PET), Polyester, Polytetrafluorethylen (PTFE), Polyvinylchlorid (PVC), Polylactid (PLA), Polyamidimid (PAI), wird jedoch insbesondere für Proben, die NH3 freisetzen können, nicht empfohlen. Die Verfahren A, B, C und E sind im Allgemeinen für alle Arten von Kunststoffen und für jeden Feuchtegehalt geeignet.
Der Wassergehalt ist ein wichtiger Parameter bei der Verarbeitung von Werkstoffen, und es wird erwartet, dass er stets unter dem in den entsprechenden Werkstoffnormen festgelegten Wert bleibt.
In diesem Dokument sind sechs alternative Verfahren festgelegt:
— Verfahren A ist ein Extraktionsverfahren mit wasserfreiem Methanol und anschließender Titration des extrahierten Wassers nach dem Karl-Fischer-Verfahren. Es kann für alle Kunststoffe verwendet werden und ist auf Granulate mit einer Korngröße kleiner als 4 mm × 4 mm × 3 mm anwendbar. Das Verfahren kann z. B. auch auf Vorpolymer-Pulvermaterialien angewendet werden, die in Methanol unlöslich sind.
— Verfahren B1 ist ein Verdampfungsverfahren unter Anwendung eines Rohrofens. Das in der Analysenmenge enthaltene Wasser wird verdampft und durch trockene Luft oder Stickstoff als Trägergas in die Titrationszelle überführt, in der anschließend entweder die Titration des gesammelten Wassers nach dem Karl-Fischer-Verfahren oder eine coulometrische Bestimmung des gesammelten Wassers mit Hilfe eines Feuchtesensors erfolgt. Es kann auf alle Kunststoffe angewendet werden und ist auf Granulate mit einer Korngröße kleiner als 4 mm × 4 mm × 3 mm anwendbar.
Plastiques - Dosage de l'eau (ISO 15512:2019)
Le présent document spécifie des méthodes pour le dosage de l'eau dans les plastiques sous forme de poudre, de granulés et d'articles finis. Ces méthodes ne contrôlent pas l'absorption d'eau (cinétique et équilibre) des plastiques, cet aspect étant traité dans l'ISO 62.
La Méthode A est applicable au dosage de l'eau à des niveaux aussi faibles que 0,1 % avec une précision de 0,1 %. La Méthode B et la Méthode C sont applicables au dosage de l'eau à des niveaux aussi faibles que 0,01 % avec une précision de 0,01 %. La Méthode D est applicable au dosage de l'eau à des niveaux aussi faibles que 0,01 % avec une précision de 0,01 %. La Méthode E est applicable au dosage de l'eau à des niveaux aussi faibles que 0,001 % avec une précision de 0,001 %. Les précisions indiquées sont les limites de détection qui dépendent également du poids maximal possible de l'échantillon. La teneur en eau est exprimée en pourcentage (fraction massique) d'eau.
La Méthode D convient pour le polyamide (PA), le polycarbonate (PC), le polypropylène (PP), le polyéthylène (PE), la résine époxyde, le poly(téréphtalate d'éthylène) (PET), le polyester, le polytétrafluoroéthylène (PTFE), le poly(chlorure de vinyle) (PVC), l'acide polylactique (PLA), le polyamide-imide (PAI). Elle est en particulier déconseillée pour les échantillons pouvant libérer du NH3. Les méthodes A, B, C et E convient généralement pour tout type de plastique et tout degré d'humidité.
La teneur en eau est un paramètre important de la mise en œuvre des matériaux et elle doit rester en dessous du niveau spécifié dans la norme de produit appropriée.
1.1 Six méthodes possibles sont spécifiées dans le présent document.
— La Méthode A consiste en une extraction de l'eau à l'aide de méthanol anhydre suivie d'un titrage de l'eau extraite par la méthode de Karl Fischer. Elle peut être utilisée pour tous les plastiques et est applicable aux granulés de moins de 4 mm × 4 mm × 3 mm. Cette méthode peut également être utilisée, par exemple, pour les poudres de prépolymères insolubles dans le méthanol.
— La Méthode B1 procède par vaporisation dans un four tubulaire. L'eau contenue dans la prise d'essai est transformée en vapeur, qui est transférée à l'aide d'un gaz vecteur d'air sec ou d'azote dans la cuve de titrage; l'eau recueillie est ensuite titrée par la méthode de Karl Fischer ou un dosage coulométrique au moyen d'un capteur d'humidité. Cette méthode peut être utilisée pour tous les plastiques et est applicable aux granulés de moins de 4 mm × 4 mm × 3 mm.
— La Méthode B2 procède par vaporisation dans une fiole à échantillon chauffée. L'eau contenue dans la prise d'essai est transformée en vapeur, qui est transférée à l'aide d'un gaz vecteur d'air sec ou d'azote dans la cuve de titrage; l'eau recueillie est ensuite titrée par la méthode de Karl Fischer. Cette méthode peut être utilisée pour tous les plastiques et est applicable aux granulés de moins de 4 mm × 4 mm × 3 mm.
— La Méthode C est une méthode manométrique. Le dosage de l'eau se fonde sur l'augmentation de pression après évaporation de l'eau sous vide. Cette méthode n'est pas applicable aux échantillons de plastiques contenant des composés volatils, autres que l'eau, en quantité suffisante pour avoir un effet significatif sur la pression de vapeur à température ambiante. Il faut effectuer périodiquement des vérifications de la présence de grandes quantités de composés volatils, par exemple par chromatographie en
Polimerni materiali - Določevanje vode (ISO 15512:2019)
V tem dokumentu je določenih šest alternativnih metod.
– Metoda A je metoda ekstrakcije z brezvodnim metanolom, ki mu sledi titracija ekstrahirane vode po Karlu Fischerju. Uporabiti jo je mogoče za vse polimerne elemente in velja za granule, manjše od 4 mm × 4 mm × 3 mm. Metoda se lahko uporablja tudi npr. za predpolimerne materiale v obliki praška, ki niso topni v metanolu.
– Metoda B1 je metoda izparevanja s cevasto pečjo. Voda v preskusni količini izpari in se prenese v titracijsko celico prek nosilnega plina (suh zrak ali dušik), čemur sledi titracija zbrane vode po Karlu Fischerju ali kulometrično določanje s senzorjem vlage. Uporabiti jo je mogoče za vse polimerne elemente in velja za granule, manjše od 4 mm × 4 mm × 3 mm.
– Metoda B2 je metoda izparevanja z ogrevano preskusno stekleničko. Voda v preskusni količini izpari in se prenese v titracijsko celico prek nosilnega plina (suh zrak ali dušik), čemur sledi titracija zbrane vode po Karlu Fischerju. Uporabiti jo je mogoče za vse polimerne elemente in velja za granule, manjše od 4 mm × 4 mm × 3 mm.
– Metoda C je manometrska metoda. Vsebnost vode se določi na podlagi povečanja tlaka, do katerega pride, ko voda izhlapi v vakuumu. Ta metoda se ne uporablja za vzorce polimernih materialov, ki vsebujejo hlapne spojine, ki niso voda, v količinah, ki znatno prispevajo k parnemu tlaku pri sobni temperaturi. Redno je treba preverjati prisotnost velikih količin hlapnih spojin, na primer s plinsko kromatografijo. Tako preverjanje je zlasti potrebno za nove tipe ali razrede materiala.
– Metoda D je termokulometrična metoda z uporabo celice difosforjevega pentoksida (P2O5) za odkrivanje izparjene vode. Voda v preskusni količini izpari in se prenese v celico senzorja prek nosilnega plina (suh zrak ali dušik), čemur sledi kulometrično določanje zbrane vode. Ta metoda se ne uporablja za vzorce polimernih materialov, ki vsebujejo hlapne spojine, ki niso voda, v količinah, ki znatno prispevajo k parnemu tlaku pri sobni temperaturi.
To je posebej povezano s hlapnimi komponentami, ki lahko reagirajo s kislim premazom senzorja difosforjevega pentoksida, npr. z amoniakom ali katero koli vrsto aminov. Redno je treba preverjati prisotnost velikih količin hlapnih spojin. Tako preverjanje je zlasti potrebno za nove tipe ali razrede materiala.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 15512:2019
01-september-2019
Nadomešča:
SIST EN ISO 15512:2017
Polimerni materiali - Določevanje vode (ISO 15512:2019)
Plastics - Determination of water content (ISO 15512:2019)
Kunststoffe - Bestimmung des Wassergehaltes (ISO 15512:2019)
Plastiques - Dosage de l'eau (ISO 15512:2019)
Ta slovenski standard je istoveten z: EN ISO 15512:2019
ICS:
83.080.01 Polimerni materiali na Plastics in general
splošno
SIST EN ISO 15512:2019 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 15512:2019
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SIST EN ISO 15512:2019
EN ISO 15512
EUROPEAN STANDARD
NORME EUROPÉENNE
May 2019
EUROPÄISCHE NORM
ICS 83.080.01 Supersedes EN ISO 15512:2016
English Version
Plastics - Determination of water content (ISO
15512:2019)
Plastiques - Dosage de l'eau (ISO 15512:2019) Kunststoffe - Bestimmung des Wassergehaltes (ISO
15512:2019)
This European Standard was approved by CEN on 4 May 2019.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 15512:2019 E
worldwide for CEN national Members.
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SIST EN ISO 15512:2019
EN ISO 15512:2019 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 15512:2019
EN ISO 15512:2019 (E)
European foreword
This document (EN ISO 15512:2019) has been prepared by Technical Committee ISO/TC 61 "Plastics"
in collaboration with Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by
NBN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by November 2019, and conflicting national standards
shall be withdrawn at the latest by November 2019.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN ISO 15512:2016.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Endorsement notice
The text of ISO 15512:2019 has been approved by CEN as EN ISO 15512:2019 without any modification.
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SIST EN ISO 15512:2019
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SIST EN ISO 15512:2019
INTERNATIONAL ISO
STANDARD 15512
Fifth edition
2019-05
Plastics — Determination of water
content
Plastiques — Dosage de l'eau
Reference number
ISO 15512:2019(E)
©
ISO 2019
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SIST EN ISO 15512:2019
ISO 15512:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019
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.
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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 2019 – All rights reserved
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SIST EN ISO 15512:2019
ISO 15512:2019(E)
Contents Page
Foreword .v
Introduction .vi
1 Scope . 1
2 Normative references . 2
3 Terms and definitions . 2
4 Method A — Extraction with anhydrous methanol . 2
4.1 Principle . 2
4.2 Reagents. 2
4.3 Apparatus . 2
4.4 Preparation of test sample . 3
4.4.1 Granules or powder . 3
4.4.2 Finished articles . 3
4.5 Procedure . 3
4.5.1 Precautions . 3
4.5.2 Preparation of test portions . 3
4.5.3 Determination . 3
4.6 Expression of results . 4
4.7 Precision . 4
5 Method B1 — Water vaporization using a heating tube oven . 4
5.1 Principle . 4
5.2 Reagents. 4
5.3 Apparatus . 5
5.4 Preparation of test sample . 7
5.5 Procedure . 7
5.5.1 Precautions . 7
5.5.2 Preparation of apparatus . 7
5.5.3 Equipment checks . 7
5.5.4 Determination . 8
5.6 Expression of results . 8
5.7 Precision . 9
6 Method B2 — Water vaporization using a heated sample vial . 9
6.1 Principle . 9
6.2 Reagents. 9
6.3 Apparatus .10
6.4 Preparation of test sample .11
6.5 Procedure .12
6.5.1 Preparation of apparatus .12
6.5.2 Equipment check .12
6.5.3 Determination .12
6.6 Expression of results .14
6.7 Precision .14
7 Method C — Manometric method .15
7.1 Principle .15
7.2 Reagents.15
7.3 Apparatus .15
7.4 Preparation of test sample .16
7.5 Procedure .16
7.5.1 Equipment .16
7.5.2 Outgassing .17
7.5.3 Calibration .17
7.5.4 Determination .19
7.6 Expression of results .20
© ISO 2019 – All rights reserved iii
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SIST EN ISO 15512:2019
ISO 15512:2019(E)
7.7 Precision .20
8 Method D — Water detection by using a diphosphorus pentoxide cell .20
8.1 Principle .20
8.2 Reagents.21
8.3 Apparatus .21
8.4 Preparation of test sample .22
8.5 Procedure .23
8.5.1 Preparation of apparatus .23
8.5.2 Rinsing the system .23
8.5.3 Tare measurement .23
8.5.4 Cell factor.23
8.5.5 Equipment check .23
8.5.6 Determination .24
8.6 Expression of results .24
8.7 Precision .25
9 Method E — Determination of water content by calcium hydride method .25
9.1 Principle .25
9.2 Reagents.26
9.3 Apparatus .26
9.4 Preparation of test sample .27
9.5 Procedure .27
9.5.1 Equipment check .27
9.5.2 Calibration .28
9.5.3 Determination .28
9.5.4 Expression of results .29
9.6 Precision .29
10 Test report .29
Annex A (informative) Alternative sample preparation methods and titration methods .30
Annex B (informative) Selection of the optimum heating temperature and heating time for
the water content determination .31
Annex C (normative) Determination of the water content of a water standard .33
Bibliography .34
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SIST EN ISO 15512:2019
ISO 15512:2019(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 61, Plastics, Subcommittee SC 5, Physical-
chemical properties.
This fifth edition cancels and replaces the fourth edition (ISO 15512:2016), which has been technically
revised. The main change compared to the previous edition is as follows:
— addition of two alternative methods for water determination (Methods D and E).
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.
© ISO 2019 – All rights reserved v
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SIST EN ISO 15512:2019
ISO 15512:2019(E)
Introduction
The interlaboratory comparability of the water content determination of plastics is often low. Major
causes for this are the sample packaging, sample handling, and differences between equipment and
settings. Samples should, e.g. be packed in special glass containers or water barrier sealed bags.
Sample handling is preferably to be carried out in a dry nitrogen or air environment. For improving the
repeatability and reproducibility, the procedure prescribed in this document is intended to be followed
strictly.
The temperature settings for the vaporization method are not specified in this document. For the
manometric method, a temperature of 200 °C is often used. However, for some condensation materials,
this might be too high and could, e.g. cause generation of water due to a condensation reaction.
The heating temperature needs to be optimized depending on the material to be tested, the equipment
in use, and the practical circumstances. If the temperature is too low, the total amount of water in the
material to be tested will not be evaporated completely, whereas too high temperatures cause water
generation due to effects like degradation and condensation reactions.
In this document, a procedure is included for optimization of the heating temperature in order to
choose the correct temperature for the water content determination and to improve the interlaboratory
comparability.
vi © ISO 2019 – All rights reserved
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SIST EN ISO 15512:2019
INTERNATIONAL STANDARD ISO 15512:2019(E)
Plastics — Determination of water content
1 Scope
This document specifies methods for the determination of the water content of plastics in the form of
powder, granules, and finished articles. These methods do not test for water absorption (kinetics and
equilibrium) of plastics as measured by ISO 62.
Method A is suitable for the determination of water content as low as 0,1 % with an accuracy of 0,1 %.
Method B and Method C are suitable for the determination of water content as low as 0,01 % with an
accuracy of 0,01 %. Method D is suitable for the determination of water content as low as 0,01 % with an
accuracy of 0,01 %. Method E is suitable for the determination of water content as low as 0,001 % with
an accuracy of 0,001 %. The stated accuracies are detection limits which depend also on the maximal
possible sample mass. The water content is expressed as a percentage mass fraction of water.
Method D is suitable for polyamide (PA), polycarbonate (PC), polypropylene (PP), polyethylene (PE), epoxy
resin, polyethylene terephthalate (PET), polyester, polytetrafluoroethylene (PTFE), polyvinyl chloride
(PVC), polylactide (PLA), polyamidimid (PAI), it is especially not recommended for samples which can
release NH . Methods A, B, C and E are generally suitable for all types of plastic and moisture level.
3
Water content is an important parameter for processing materials and is expected to remain below the
level specified in the appropriate material standard.
Six alternative methods are specified in this document.
— Method A is an extraction method using anhydrous methanol followed by a Karl Fischer titration
of the extracted water. It can be used for all plastics and is applicable to granules smaller than
4 mm × 4 mm × 3 mm. The method can also be used for, e.g. prepolymer materials in the form of a
powder that are insoluble in methanol.
— Method B1 is a vaporization method using a tube oven. The water contained in the test portion is
vaporized and carried to the titration cell by a dry air or nitrogen carrier gas, followed by a Karl
Fischer titration or a coulometric determination by means of a moisture sensor of the collected
water. It can be used for all plastics and is applicable to granules smaller than 4 mm × 4 mm × 3 mm.
— Method B2 is a vaporization method using a heated sample vial. The water contained in the test
portion is vaporized and carried to the titration cell by a dry air or nitrogen carrier gas, followed
by a Karl Fischer titration of the collected water. It can be used for all plastics and is applicable to
granules smaller than 4 mm × 4 mm × 3 mm.
— Method C is a manometric method. The water content is determined from the increase in pressure,
which results when the water is evaporated under a vacuum. This method is not applicable to plastic
samples containing volatile compounds, other than water, in amounts contributing significantly
to the vapour pressure at room temperature. Checks for the presence of large amounts of volatile
compounds are to be carried out periodically, for example by gas chromatography. Such checks are
particularly required for new types or grades of material.
— Method D is a thermocoulometric method using a diphosphorus pentoxide (P O ) cell for the
2 5
detection of the vaporized water. The water contained in the test portion is vaporized and carried
to the sensor cell by a dry air or nitrogen carrier gas, followed by a coulometric determination of
the collected water. This method is not applicable to plastic samples containing volatile compounds,
other than water, in amounts contributing significantly to the vapour pressure at room temperature.
This is specially related to volatile components which can
...
SLOVENSKI STANDARD
oSIST prEN ISO 15512:2018
01-julij-2018
3ROLPHUQLPDWHULDOL'RORþHYDQMHYRGH ,62',6
Plastics - Determination of water content (ISO/DIS 15512:2018)
Kunststoffe - Bestimmung des Wassergehaltes (ISO/DIS 15512:2018)
Plastiques - Dosage de l'eau (ISO/DIS 15512:2018)
Ta slovenski standard je istoveten z: prEN ISO 15512
ICS:
83.080.01 Polimerni materiali na Plastics in general
splošno
oSIST prEN ISO 15512:2018 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 15512:2018
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oSIST prEN ISO 15512:2018
DRAFT INTERNATIONAL STANDARD
ISO/DIS 15512
ISO/TC 61/SC 5 Secretariat: DIN
Voting begins on: Voting terminates on:
2018-04-25 2018-07-18
Plastics — Determination of water content
Plastiques — Dosage de l'eau
ICS: 83.080.01
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
ISO/CEN PARALLEL PROCESSING
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 15512:2018(E)
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 SUPPORTING DOCUMENTATION. ISO 2018
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oSIST prEN ISO 15512:2018
ISO/DIS 15512:2018(E) ISO/DIS 15512:2018(E)
Contents Page
Foreword . v
Introduction . vi
1 Scope .1
2 Normative references .2
3 Method A — Extraction with anhydrous methanol .2
3.1 Principle .2
3.2 Reagents .2
3.3 Apparatus .2
3.4 Preparation of test sample .3
3.4.1 Granules or powder .3
3.4.2 Finished articles .3
3.5 Procedure .3
3.5.1 Precautions .3
3.5.2 Preparation of test portions .3
3.5.3 Determination.3
3.6 Expression of results .4
3.7 Precision .4
4 Method B1 — Water vaporization using a heating tube oven .4
4.1 Principle .4
4.2 Reagents .5
4.3 Apparatus .5
4.4 Preparation of test sample .7
4.5 Procedure .7
4.5.1 Precautions .7
4.5.2 Preparation of apparatus .7
4.5.3 Equipment check .8
4.5.4 Determination.8
4.6 Expression of results .9
4.7 Precision .9
5 Method B2 — Water vaporization using a heated sample vial . 10
5.1 Principle . 10
5.2 Reagents . 10
5.3 Apparatus . 11
5.4 Preparation of test sample . 12
5.5 Procedure . 13
COPYRIGHT PROTECTED DOCUMENT
5.5.1 Preparation of apparatus . 13
© ISO 2018 5.5.2 Equipment check . 13
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may 5.5.3 Determination. 13
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
5.6 Expression of results . 15
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
5.7 Precision . 16
below or ISO’s member body in the country of the requester.
ISO copyright office
6 Method C — Manometric method . 16
CP 401 • Ch. de Blandonnet 8
6.1 Principle . 16
CH-1214 Vernier, Geneva
6.2 Reagents . 16
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
6.3 Apparatus . 17
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
© ISO 2018 – All rights reserved
iii
ii © ISO 2018 – All rights reserved
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oSIST prEN ISO 15512:2018
ISO/DIS 15512:2018(E)
Contents Page
Foreword . v
Introduction . vi
1 Scope .1
2 Normative references .2
3 Method A — Extraction with anhydrous methanol .2
3.1 Principle .2
3.2 Reagents .2
3.3 Apparatus .2
3.4 Preparation of test sample .3
3.4.1 Granules or powder .3
3.4.2 Finished articles .3
3.5 Procedure .3
3.5.1 Precautions .3
3.5.2 Preparation of test portions .3
3.5.3 Determination.3
3.6 Expression of results .4
3.7 Precision .4
4 Method B1 — Water vaporization using a heating tube oven .4
4.1 Principle .4
4.2 Reagents .5
4.3 Apparatus .5
4.4 Preparation of test sample .7
4.5 Procedure .7
4.5.1 Precautions .7
4.5.2 Preparation of apparatus .7
4.5.3 Equipment check .8
4.5.4 Determination.8
4.6 Expression of results .9
4.7 Precision .9
5 Method B2 — Water vaporization using a heated sample vial . 10
5.1 Principle . 10
5.2 Reagents . 10
5.3 Apparatus . 11
5.4 Preparation of test sample . 12
5.5 Procedure . 13
5.5.1 Preparation of apparatus . 13
5.5.2 Equipment check . 13
5.5.3 Determination. 13
5.6 Expression of results . 15
5.7 Precision . 16
6 Method C — Manometric method . 16
6.1 Principle . 16
6.2 Reagents . 16
6.3 Apparatus . 17
© ISO 2018 – All rights reserved
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oSIST prEN ISO 15512:2018
ISO/DIS 15512:2018(E)
6.4 Preparation of test sample . 17
6.5 Procedure. 18
6.5.1 Equipment . 18
6.5.2 Outgassing . 19
6.5.3 Calibration . 20
6.5.4 Determination . 21
6.6 Expression of results . 22
6.7 Precision . 23
7 Method D — Water detection by using a diphosphorus pentoxide cell . 23
7.1 Principle . 23
7.2 Reagents . 23
7.3 Apparatus . 24
7.4 Preparation of test sample . 24
7.5 Procedure. 25
7.5.1 Preparation of apparatus . 25
7.5.2 Set the gas flow . 25
7.5.3 Rinsing the system . 25
7.5.4 Tare measurement . 25
7.5.5 Cell factor . 25
7.5.6 Equipment check . 26
7.5.7 Determination . 26
7.6 Expression of results . 27
7.7 Precision . 28
8 Method E — Determination of water content by calcium hydride method . 28
8.1 Principle . 28
8.2 Reagents . 28
8.3 Apparatus . 28
8.4 Preparation of test sample . 29
8.5 Procedure. 30
8.5.1 Equipment check . 30
8.5.2 Calibration . 30
8.5.3 Determination . 30
8.5.4 Expression of results . 31
8.6 Precision . 31
9 Test report . 31
Annex A (informative) Alternative sample preparation methods and titration methods . 33
A.1 General . 33
A.2 Titration in solution . 33
A.3 Continuous titration in suspension . 33
A.4 Discontinuous titration in suspension . 33
A.5 External extraction of water . 33
Annex B (informative) Selection of the optimum heating temperature for the water content
determination . 34
B.1 Procedure. 34
B.2 Interpretation of results . 34
Annex C (normative) Determination of the water content of a water standard . 36
Bibliography . 37
© ISO 2018 – All rights reserved
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oSIST prEN ISO 15512:2018
ISO/DIS 15512:2018(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national
standards bodies (ISO member bodies). The work of preparing International Standards is normally
carried out through ISO technical committees. Each member body interested in a subject for which a
technical committee has been established has the right to be represented on that committee.
International organizations, governmental and non-governmental, in liaison with ISO, also take part in
the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all
matters of electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the 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 the following
URL: www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-
chemical properties.
This fifth edition cancels and replaces the fourth edition (ISO 15512:2016), which has been technically
revised by adding two alternative methods for water determination (Methods D and E).
© ISO 2018 – All rights reserved
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oSIST prEN ISO 15512:2018
ISO/DIS 15512:2018(E)
Introduction
The interlaboratory comparability of the water content determination of plastics is often low. Major
causes for this are the sample packaging, sample handling, and differences between equipment and
settings. Samples have to, e.g. be packed in special glass containers or water barrier sealed bags. Sample
handling is preferably to be carried out in a dry nitrogen or air environment. For improving the
repeatability and reproducibility, the procedure prescribed in this document is intended to be followed
strictly.
The temperature settings for the vaporization method are not specified in this document Standard. For
the manometric method, a temperature of 200 °C is often used. However, for some condensation
materials, this might be too high and could, e.g. cause generation of water due to a condensation
reaction.
The heating temperature has to be optimized concerning the material to be tested, the equipment in
use, and the practical circumstances. If the temperature is too low, the total amount of water in the
material to be tested will not be evaporated completely, whereas too high temperatures cause water
generation due to effects like degradation and condensation reactions.
In this document, a procedure is included for optimization of the heating temperature in order to
choose the correct temperature for the water content determination and to improve the interlaboratory
comparability.
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oSIST prEN ISO 15512:2018
DRAFT INTERNATIONAL STANDARD ISO/DIS 15512:2018(E)
Plastics — Determination of water content
1 Scope
1.1 This document specifies methods for the determination of the water content of plastics in the
form of powder, granules, and finished articles. These methods do not test for water absorption
(kinetics and equilibrium) of plastics as measured by ISO 62.
Method A is suitable for the determination of water content as low as 0,1 % with an accuracy of 0,1 %.
Method B and Method C are suitable for the determination of water content as low as 0,01 % with an
accuracy of 0,01 %. Method D is suitable for the determination of water content as low as 0,01% with an
accuracy of 0,01%. Method E is suitable for the determination of water content as low as 0,001% with
an accuracy of 0,001%. The stated accuracies are detection limits which depend also on the maximal
possible sample weight. Percentage means percentage of water content.
Method D is suitable for polyamide (
...
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