SIST EN ISO 15512:2004
(Main)Plastics - Determination of water content (ISO 15512:1999)
Plastics - Determination of water content (ISO 15512:1999)
Will replace EN ISO 960:1997 (CC/010807)
Kunststoffe - Bestimmung des Wassergehaltes - (ISO 15512:1999)
1.1 Diese Internationale Norm legt Verfahren zur Bestimmung des Wassergehaltes von Kunststoffen fest, die als Granulat oder Fertigartikel vorliegen.
Diese Verfahren prüfen nicht die Wasseraufnahme (Kinetik und Gleichgewicht) von Kunststoffen, wie diese in ISO 62 gemessen wird. Diese Verfahren sind zur Bestimmung von Wassergehalten bis hinunter zu folgenden Werten vorgesehen:
- Verfahren A 0,1 % oder besser
- Verfahren B 0,01 % oder besser
- Verfahren C 0,01 % oder besser
Der Wassergehalt ist ein wichtiger Parameter bei der Verarbeitung von Werkstoffen und sollte stets unter dem in den entsprechenden Werkstoff-Normen festgelegten Wert bleiben.
1.2 In dieser Internationalen Norm sind drei alternative Verfahren festgelegt.
Verfahren A ist ein Extraktionsverfahren mit wasserfreiem Methanol und anschließender Titration des Wassers nach dem Karl-Fischer-Verfahren. Es kann für alle Kunststoffe verwendet werden und ist auf Granulat mit der maximalen Korngröße von 4 mm × 4 mm × 3 mm anwendbar.
Verfahren B ist ein Verdampfungsverfahren, bei dem mit aufgeheizter Luft oder Stickstoffgas Wasser verdampft wird und anschließender Titration des gesammelten Wassers nach dem Karl-Fischer-Verfahren. Es kann für alle Kunststoffe verwendet werden und ist auf Granulat kleiner als 4 mm × 4 mm × 3 mm anwendbar.
Verfahren C ist ein manometrisches Verfahren. Der Wassergehalt wird aus dem Druckanstieg nach dem Verdampfen des Wassers unter Vakuum bestimmt. Das Verfahren kann nicht auf Kunststoffproben angewendet werden, die andere flüchtige Bestandteile als Wasser in solchen Mengen haben, dass diese signifikant zum Dampfdruck bei Raumtemperatur beisteuern. In regelmäßigen Abständen sollten, z. B. durch Gaschromatographie, die Anwesenheit großer Mengen von flüchtigen Bestandteilen überprüft werden. Diese Überprüfungen sind insbesondere notwendig bei neuen Typen oder Klassen von Werkstoffen.
Plastiques - Dosage de l'eau (ISO 15512:1999)
Polimerni materiali - Določevanje vode (ISO 15512:1999)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 15512:2004
01-februar-2004
1DGRPHãþD
SIST EN ISO 960:2000
3ROLPHUQLPDWHULDOL'RORþHYDQMHYRGH ,62
Plastics - Determination of water content (ISO 15512:1999)
Kunststoffe - Bestimmung des Wassergehaltes - (ISO 15512:1999)
Plastiques - Dosage de l'eau (ISO 15512:1999)
Ta slovenski standard je istoveten z: EN ISO 15512:2003
ICS:
83.080.01 Polimerni materiali na Plastics in general
splošno
SIST EN ISO 15512:2004 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 15512:2004
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SIST EN ISO 15512:2004
EUROPEAN STANDARD
EN ISO 15512
NORME EUROPÉENNE
EUROPÄISCHE NORM
November 2003
ICS 83.080.01 Supersedes EN ISO 960:1997
English version
Plastics - Determination of water content (ISO 15512:1999)
Plastiques - Dosage de l'eau (ISO 15512:1999) Kunststoffe - Bestimmung des Wassergehaltes - (ISO
15512:1999)
This European Standard was approved by CEN on 3 November 2003.
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 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 Management Centre has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,
Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and United
Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36 B-1050 Brussels
© 2003 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 15512:2003 E
worldwide for CEN national Members.
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SIST EN ISO 15512:2004
EN ISO 15512:2003 (E)
Foreword
The text of ISO 15512:1999 has been prepared by Technical Committee ISO/TC 61 "Plastics” of
the International Organization for Standardization (ISO) and has been taken over as EN ISO
15512:2003 by Technical Committee CEN/TC 249 "Plastics", the secretariat of which is held by
IBN.
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 May 2004, and conflicting national standards
shall be withdrawn at the latest by May 2004.
This document supersedes EN ISO 960:1997.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of
the following countries are bound to implement this European Standard: Austria, Belgium, Czech
Republic, Denmark, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,
Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and
the United Kingdom.
Endorsement notice
The text of ISO 15512:1999 has been approved by CEN as EN ISO 15512:2003 without any
modifications.
NOTE Normative references to International Standards are listed in Annex ZA (normative).
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SIST EN ISO 15512:2004
EN ISO 15512:2003 (E)
Annex ZA
(normative)
Normative references to international publications
with their relevant European publications
This European Standard incorporates by dated or undated reference, provisions from other
publications. These normative references are cited at the appropriate places in the text and the
publications are listed hereafter. For dated references, subsequent amendments to or revisions of
any of these publications apply to this European Standard only when incorporated in it by
amendment or revision. For undated references the latest edition of the publication referred to
applies (including amendments).
NOTE Where an International Publication has been modified by common modifications, indicated
by (mod.), the relevant EN/HD applies.
Publication Year Title EN Year
ISO 62 1999 Plastics - Determination of water EN ISO 62 1999
absorption
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SIST EN ISO 15512:2004
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SIST EN ISO 15512:2004
INTERNATIONAL ISO
STANDARD 15512
First edition
1999-07-01
Plastics — Determination of water content
Plastiques — Dosage de l'eau
A
Reference number
ISO 15512:1999(E)
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SIST EN ISO 15512:2004
ISO 15512:1999(E)
Contents
1 Scope .1
2 Normative references .1
3 Method A — Extraction with anhydrous methanol .2
4 Method B — Water vaporization.4
5 Method C — Manometric method.8
6 Test report .12
© ISO 1999
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic
or mechanical, including photocopying and microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case postale 56 • CH-1211 Genève 20 • Switzerland
Internet iso@iso.ch
Printed in Switzerland
ii
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SIST EN ISO 15512:2004
© ISO
ISO 15512:1999(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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3.
Draft International Standards adopted by the technical committees are circulated to the member bodies for voting.
Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.
International Standard ISO 15512 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5,
Physical-chemical properties.
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SIST EN ISO 15512:2004
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SIST EN ISO 15512:2004
INTERNATIONAL STANDARD © ISO ISO 15512:1999(E)
Plastics — Determination of water content
1 Scope
1.1 This International Standard specifies methods for the determination of the water content of plastics in the form
of granules and finished articles. These methods do not test for water absorption (kinetics and equilibrium) of
plastics as measured by ISO 62. The methods are suitable for the determination of water content as low as the
following levels:
Method A 0,1 % or better;
Method B 0,01 % or better;
Method C 0,01 % or better.
Water content is an important parameter for processing materials, and should remain below the level specified in
the appropriate material standard.
1.2 Three alternative methods are specified in this International Standard.
a) 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 having a maximum size of
4 mm ´ 4 mm ´ 3 mm.
b) Method B is a vaporization method using heated, dry air or nitrogen gas to evaporate the water, 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.
c) 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 should be carried out
periodically, for example by gas chromatography. Such checks are particularly required for new types or
grades of material.
2 Normative references
The following normative documents contain provisions which, through reference in this text, constitute provisions of this
International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do
not apply. However, parties to agreements based on this International Standard are encouraged to investigate the
possibility of applying the most recent editions of the normative documents indicated below. For undated references,
the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of
currently valid International Standards.
ISO 62, Plastics — Determination of water absorption.
ISO 760:1978, Determination of water — Karl Fischer method (General method).
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SIST EN ISO 15512:2004
© ISO
ISO 15512:1999(E)
3 Method A — Extraction with anhydrous methanol
3.1 Principle
A test portion is extracted with anhydrous methanol and the extracted water determined by titration using the Karl
Fischer method.
3.2 Reagents
During the analysis, use only reagents of recognized analytical grade.
anhydrous, having a water content less than 0,1 % by mass.
3.2.1 Methanol,
3.2.2 Karl Fischer reagent, with an equivalence factor of approximately 3 mg/ml to 5 mg/ml of water. If the
reagent is prepared, check its equivalence factor as specified in ISO 760.
3.3 Apparatus
Ordinary laboratory apparatus and the following:
3.3.1 Glass flasks, 250 ml capacity, provided with ground-glass or rubber stoppers.
3.3.2 Conical titration flasks, 150 ml capacity, with standard ground necks and provided with ground-glass
stoppers.
3.3.3 Reflux condensers, with ground neck capable of being fitted on to the flasks (3.3.2) and on to the tubes
(3.3.4).
3.3.4 Water-absorption tubes with ground joints, containing calcium chloride or other drying agent.
3.3.5 Electrical or hot-air heaters, for the flasks (3.3.2).
3.3.6 Pipettes, 50 ml capacity. (Automatic filling pipettes are acceptable.)
3.3.7 Woulfe bottles, with two tubes.
3.3.8 Curved or U-shaped water-absorption tubes, filled with calcium chloride.
3.3.9 Rubber pipette filler.
3.3.10 Pipette, 10 ml capacity.
3.3.11 Desiccator, containing calcium chloride.
3.3.12 Analytical balance, accurate to 0,2 mg.
3.3.13 Karl Fischer apparatus, for determining water content in accordance with ISO 760.
3.4 Preparation of test sample
3.4.1 Granules
Take a representative sample of approximately 100 g. Put the sample into a pre-dried glass flask (3.3.1) and
immediately close it with a stopper.
NOTE It is desirable to pre-dry the container in an oven, then cool it over a suitable water absorbent, for instance silica gel.
3.4.2 Finished articles
Cut or saw the sample into pieces of appropriate size, i.e. having a maximum size of 4 mm ´ 4 mm ´ 3 mm.
Proceed quickly to minimize moisture absorption.
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SIST EN ISO 15512:2004
© ISO
ISO 15512:1999(E)
3.5 Procedure
3.5.1 Precautions
Due to the low quantities of water measured, maximum care shall be exercised at all times to avoid contaminating
the sample with water from the sample container, the atmosphere or transfer equipment. Hygroscopic resin
samples shall be protected from the atmosphere.
3.5.2 Preparation of test portions
Conduct the test on two test portions from the same sample. Use test portions containing 10 mg to 20 mg of water
based on the estimated water content of the sample.
3.5.3 Determination
3.5.3.1 Carefully dry the apparatus.
3.5.3.2 Weigh each test portion to the nearest 1 mg into a conical titration flask (3.3.2) fitted with a ground-glass
stopper. Pipette 50 ml (3.3.6) of anhydrous methanol (3.2.1) into the conical flask containing the test portion. At the
same time, add 50 ml of anhydrous methanol to another conical flask for a blank test. Stopper the flasks. Keep the
stoppered flasks in the desiccator (3.3.11) pending continuation of the test.
3.5.3.3 Unstopper the flasks and quickly attach them to reflux condensers (3.3.3) fitted with calcium chloride tubes
(3.3.4). Reflux the contents of the conical flasks for 3 h, then leave them for 45 min to cool to room temperature.
Separate the flasks from the condensers, quickly stopper them and place them in the desiccator.
3.5.3.4 Use the Karl Fischer apparatus (3.3.13) to titrate the contents of each flask with Karl Fischer reagent
(3.2.2).
3.6 Expression of results
3.6.1 The water content w, expressed as a percentage by mass, for each of the two determinations is given by the
following formula:
VV T
()-
12
w =·100
m
where:
V is the volume, expressed in millilitres, of Karl Fischer reagent used for the determination;
1
is the volume, expressed in millilitres, of Karl Fischer reagent used for the blank test;
V
2
T is the water equivalent, expressed in grams of water per millilitre of reagent, of Karl Fischer reagent;
m is the mass, in grams, of the test portion.
3.6.2 The two values for the water content shall not differ by more than 10 % relative or 0,02 % absolute,
whichever is the greater. If the difference is greater, repeat the measurements until acceptable consecutive values
are obtained and discard all unacceptable results.
3.6.3 The result is expressed as the average of these two determinations, rounded to the nearest 0,01 % by mass.
3.7 Precision
The precision of this test method is not known because interlaboratory data are not available. If and when
interlaboratory data are obtained, a precision statement will be added at a subsequent revision.
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SIST EN ISO 15512:2004
© ISO
ISO 15512:1999(E)
4 Method B — Water vaporization
4.1 Principle
The sample is weighed then placed in an oven. The water contained in the test portion is vaporized and carried to
the titration cell by a dry nitrogen carrier gas. The water is then titrated using the coulometric Karl Fischer method.
This method is based on the reduction of iodine by sulfur dioxide in the presence of water to form sulfur trioxide and
hydroiodic acid as follows:
I + SO + H O fi 2HI + SO
2 2 2 3
Unlike the conventional Karl Fisher reagents that include iodine, the coulometric technique generates the iodine
electrolytically from iodide
- -
2I fi I + 2e
2
with 10,71 C of generating current corresponding to 1 mg of water in accordance with Faraday’s law.
4.2 Reagents
During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent
purity.
4.2.1 Anode solution, containing iodide ions (to generate iodine in the reaction mixture), pyridine (or another base
such as dipyridylpropane, alkylaminopyridine, imidazole or diethanolamine), sulfur dioxide and methanol (or another
suitable organic solvent), prepared in accordance with the equipment manufacurer's instructions.
4.2.2 Cathode solution, containing a suitable salt in methanol (or another suitable organic solvent), prepared in
accordance with the equipment manufacturer’s instruc
...
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