EN ISO 15512:2009

SLOVENSKI STANDARD
01-december-2009
1DGRPHãþD
SIST EN ISO 15512:2004
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Plastics - Determination of water content (ISO 15512:2008)
Kunststoffe - Bestimmung des Wassergehaltes (ISO 15512:2008)
Plastiques - Dosage de l'eau (ISO 15512:2008)
Ta slovenski standard je istoveten z: EN ISO 15512:2009
ICS:
83.080.01 Polimerni materiali na Plastics in general
splošno
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN ISO 15512
NORME EUROPÉENNE
EUROPÄISCHE NORM
July 2009
ICS 83.080.01 Supersedes EN ISO 15512:2003
English Version
Plastics - Determination of water content (ISO 15512:2008)
Plastiques - Dosage de l'eau (ISO 15512:2008) Kunststoffe - Bestimmung des Wassergehaltes (ISO
15512:2008)
This European Standard was approved by CEN on 20 June 2009.
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 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 Management Centre has the same status as the
official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2009 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 15512:2009: E
worldwide for CEN national Members.

Contents Page
Foreword .3

Foreword
The text of ISO 15512:2008 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 15512:2009 by
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 January 2010, and conflicting national standards shall be withdrawn at
the latest by January 2010.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN ISO 15512:2003.
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, Cyprus, Czech
Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.
Endorsement notice
The text of ISO 15512:2008 has been approved by CEN as EN ISO 15512:2009 without any modification.

INTERNATIONAL ISO
STANDARD 15512
Second edition
2008-05-15
Plastics — Determination of water
content
Plastiques — Dosage de l'eau
Reference number
ISO 15512:2008(E)
©
ISO 2008
ISO 15512:2008(E)
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ii © ISO 2008 – All rights reserved

ISO 15512:2008(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope . 1
2 Normative references . 1
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. 2
3.5 Procedure . 3
3.6 Expression of results . 3
3.7 Precision. 4
4 Method B — Water vaporization. 4
4.1 Principle. 4
4.2 Reagents. 4
4.3 Apparatus . 5
4.4 Preparation of sample . 6
4.5 Procedure . 6
4.6 Expression of results . 8
4.7 Precision. 8
5 Method C — Manometric method. 8
5.1 Principle. 8
5.2 Reagent. 8
5.3 Apparatus . 9
5.4 Preparation of sample . 9
5.5 Procedure . 11
5.6 Expression of results . 13
5.7 Precision. 13
6 Test report . 13
Annex A (informative) Selection of the optimum heating temperature for the water content
determination . 14
Bibliography . 16

ISO 15512:2008(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 2.
The main task of technical committees is to prepare International Standards. 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.
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.
ISO 15512 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-
chemical properties.
This second edition cancels and replaces the first edition (ISO 15512:1999), which has been technically
revised.
iv © ISO 2008 – All rights reserved

ISO 15512:2008(E)
Introduction
The inter-laboratory comparability of water content determinations is often low. Major causes for this are the
sample packaging, sample handling and differences between equipment and settings. In order to be able to
compare data between two laboratories, special care needs to be taken with sample packaging and sample
handling. Samples should e.g. be packed in special glass containers or water barrier sealed bags. Sample
handling should preferably be carried out in a dry nitrogen or air environment. To improve the repeatability and
reproducibility, the procedure specified in this International Standard should be followed strictly.
The temperature settings for the vaporization method described in this International Standard are not specified
in the 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 should 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 International Standard, 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 inter-laboratory
comparability.
INTERNATIONAL STANDARD ISO 15512:2008(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 referenced documents are indispensable for the application 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 760, Determination of water — Karl Fischer method (General method)
ISO 15512:2008(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.
3.2.1 Methanol, anhydrous, having a water content less than 0,1 % by mass.
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.
2 © ISO 2008 – All rights reserved

ISO 15512:2008(E)
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.
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
Carefully dry the apparatus.
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.
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.
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
The water content w, expressed as a percentage by mass, for each of the two determinations is given by the
following formula:
VV− T
()
w=×100
m
where
V is the volume, expressed in millilitres, of Karl Fischer reagent used for the determination;
V is the volume, expressed in millilitres, of Karl Fischer reagent used for the blank test;
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.
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.
The result is expressed as the average of these two determinations, rounded to the nearest 0,01 % by mass.
ISO 15512:2008(E)
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.
4 Method B — Water vaporization
4.1 Principle
A test portion 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 → 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 → I + 2e
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
...