EN ISO 14896:2001
(Main)Plastics - Polyurethane raw materials - Determination of isocyanate content (ISO 14896:2000)
Plastics - Polyurethane raw materials - Determination of isocyanate content (ISO 14896:2000)
Migrated from Progress Sheet (TC Comment) (2000-07-10): Revision of EN ISO 9369:1997 (CC/000626)
Kunststoffe - Polyurethanrohstoffe - Bestimmung des Isocyanatanteils (ISO 14896:2000)
Diese Internationale Norm legt zwei Verfahren zur Bestimmung des Isocyanatanteils von aromatischen Isocyanaten fest, die als Polyurethanrohstoff verwendet werden. Verfahren A ist in erster Linie auf reines Toluoldiisocyanat (TDI), 4,4´-Methylendi-(phenylisocyanat) (MDI) und deren Vorpolymere anwendbar. Verfahren B ist auf reine, rohe oder modifizierte, von Toluoldiisocyanat, 4,4´-Methylendi-(phenylisocyanat) und Polymethylen-polyphenylisocyanat abgeleitete Isocyanate anwendbar. Es kann auch bei Isomergemischen von Toluoldiiso-cyanat, 4,4´-Methylendi-(phenylisocyanat) und Polymethylenpolyphenylisocyanat Anwendung finden. Wenn die Eignung des Verfahrens vorsorglich nachgewiesen wurde, dürfen auch andere aromatische Isocyanate damit analysiert werden. Das Verfahren ist nicht auf inaktivierte Isocyanate anwendbar.
Plastiques - Matières premières des polyuréthannes - Détermination de la teneur en isocyanate (ISO 14896:2000)
Polimerni materiali - Surovine za poliuretane - Določevanje izocianata (ISO 14896.2000)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 14896:2002
01-februar-2002
1DGRPHãþD
SIST EN ISO 9369:1999
3ROLPHUQLPDWHULDOL6XURYLQH]DSROLXUHWDQH'RORþHYDQMHL]RFLDQDWD ,62
Plastics - Polyurethane raw materials - Determination of isocyanate content (ISO
14896:2000)
Kunststoffe - Polyurethanrohstoffe - Bestimmung des Isocyanatanteils (ISO 14896:2000)
Plastiques - Matieres premieres des polyuréthannes - Détermination de la teneur en
isocyanate (ISO 14896:2000)
Ta slovenski standard je istoveten z: EN ISO 14896:2001
ICS:
83.080.10 Duromeri Thermosetting materials
SIST EN ISO 14896:2002 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 14896:2002
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SIST EN ISO 14896:2002
EUROPEAN STANDARD
EN ISO 14896
NORME EUROPÉENNE
EUROPÄISCHE NORM
August 2001
ICS 83.080.10 Supersedes EN ISO 9369:1997
English version
Plastics - Polyurethane raw materials - Determination of
isocyanate content (ISO 14896:2000)
Plastiques - Matières premières des polyuréthannes - Kunststoffe - Polyurethanrohstoffe - Bestimmung des
Détermination de la teneur en isocyanate (ISO Isocyanatanteils (ISO 14896:2000)
14896:2000)
This European Standard was approved by CEN on 15 June 2001.
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,
Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
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© 2001 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 14896:2001 E
worldwide for CEN national Members.
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SIST EN ISO 14896:2002
EN ISO 14896:2001 (E)
CORRECTED 2002-02-06
Foreword
The text of the International Standard from Technical Committee ISO/TC 61 "Plastics" of the
International Organization for Standardization (ISO) has been taken over as a European
Standard by Technical Committee CEN/TC 249 "Plastics", the secretariat of which is held by
IBN.
This document supersedes EN ISO 9369:1997.
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 February 2002, and conflicting national
standards shall be withdrawn at the latest by February 2002.
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, Iceland, Ireland, Italy, Luxembourg,
Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom.
Endorsement notice
The text of the International Standard ISO 14896:2000 has been approved by CEN as a
European Standard without any modifications.
NOTE Normative references to International Standards are listed in annex ZA (normative).
2
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SIST EN ISO 14896:2002
EN ISO 14896:2001 (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 3696 1987 Water for analytical laboratory use - EN ISO 3696 1995
Specification and test methods
3
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SIST EN ISO 14896:2002
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SIST EN ISO 14896:2002
INTERNATIONAL ISO
STANDARD 14896
First edition
2000-09-01
Plastics — Polyurethane raw materials —
Determination of isocyanate content
Plastiques — Matières premières des polyuréthannes — Détermination de
la teneur en isocyanate
Reference number
ISO 14896:2000(E)
© ISO 2000
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SIST EN ISO 14896:2002
ISO 14896:2000(E)
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©
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SIST EN ISO 14896:2002
ISO 14896:2000(E)
Contents Page
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Application . 2
6 Interferences . 2
7 Sampling . 2
8 Test conditions . 3
9 Reagents . 3
10 Apparatus . 3
11 Method A — Toluene/dibutylamine with aqueous HCl . 4
12 Method B — Toluene/TCB/DBA with methanolic HCl . 6
©
ISO 2000 – All rights reserved iii
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SIST EN ISO 14896:2002
ISO 14896:2000(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 com-
mittees. 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 liai-
son 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.
Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights.
International Standard ISO 14896 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12,
Thermosetting materials.
This first edition cancels and replaces ISO 9369:1997, which has been technically revised.
An International Standard dealing with the analysis of refined aromatic diisocyanates and their prepolymers has
been published (see ISO 9369). Method A of this International Standard incorporates the methodology of ISO 9369,
therefore ISO 9369 will be deleted after publication of this International Standard. Method B of this International
Standard is based on Test Method C of ASTM D 5515-91, Standard Test Method for Polyurethane Raw Materials —
Determination of the Isocyanate Content of Aromatic Isocyanates.
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SIST EN ISO 14896:2002
INTERNATIONAL STANDARD ISO 14896:2000(E)
Plastics — Polyurethane raw materials — Determination of
isocyanate content
CAUTION — Persons using this International Standard should be familiar with normal laboratory practice.
This International Standard does not purport to address all of the safety problems, if any, associated with its
use. It is the responsibility of the user of this International Standard to establish appropriate safety and
health practices and to ensure compliance with any national regulatory conditions prior to use.
1 Scope
This International Standard specifies two methods for the measurement of the isocyanate content of aromatic iso-
cyanates used as polyurethane raw materials. Method A is primarily applicable to refined toluene diisocyanate (TDI),
methylene-bis-(4-phenylisocyanate) (MDI) and their prepolymers. Method B is applicable to refined, crude or modi-
fied isocyanates derived from toluene diisocyanate, methylene-bis-(4-phenylisocyanate) and polymethylene
polyphenylisocyanate. It can also be used for isomer mixtures of toluene diisocyanate, methylene-bis-(4-phenyl-
isocyanate) and polymethylene polyphenylisocyanate. Other aromatic isocyanates may be analysed by this method
if precautions are taken to verify suitability. It is not applicable to blocked isocyanates.
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 publica-
tions do not apply. However, parties to agreements based on this International Standard are encouraged to investi-
gate 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 reg-
isters of currently valid International Standards.
ISO 385-1:1984, Laboratory glassware — Burettes — Part 1: General requirements.
ISO 648:1977, Laboratory glassware — One-mark pipettes.
ISO 3696:1987, Water for analytical laboratory use — Specification and test methods.
ISO 4787:1984, Laboratory glassware — Volumetric glassware — Methods for use and testing of capacity.
ISO 4788:1980, Laboratory glassware — Graduated measuring cylinders.
ISO 6353-1:1982, Reagents for chemical analysis — Part 1: General test methods.
ISO 6353-2:1983, Reagents for chemical analysis — Part 2: Specifications — First series.
ISO 6353-3:1987, Reagents for chemical analysis — Part 3: Specifications — Second series.
ISO 14898:1999, Plastics — Aromatic isocyanates for use in the production of polyurethane — Determination of
acidity.
3 Terms and definitions
For the purposes of this International Standard, the following terms and definitions apply.
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SIST EN ISO 14896:2002
ISO 14896:2000(E)
3.1
polyurethane
a polymer prepared by the reaction of an organic di- or polyisocyanate with compounds containing two or more
hydroxyl groups
NOTE Polyurethanes may be thermosetting, thermoplastic, rigid or soft and flexible, cellular or non-cellular.
3.2
assay
the percent by mass of a specific isocyanate present in a sample
3.3
isocyanate content
NCO content
the percent by mass of the NCO groups present in a sample
3.4
amine equivalent
the mass of sample that will combine with 1 gram-equivalent of dibutylamine
4Principle
4.1 Method A
The isocyanate sample is reacted with an excess of dibutylamine in toluene to form the corresponding substituted
urea. After cooling to room temperature, acetone is added as a cosolvent, then the reaction mixture is back-titrated
with standardized aqueous HCl using potentiometric or colorimetric end point determination.
4.2 Method B
The isocyanate sample is reacted with an excess of dibutylamine in a toluene/trichlorobenzene solvent to form the
corresponding substituted urea. After cooling to room temperature, the reaction mixture is diluted with methanol and
back-titrated potentiometrically or colorimetrically with methanolic hydrochloric acid.
5 Application
These test methods can be used for research or for quality control purposes to characterize isocyanates used in
polyurethane products.
6 Interferences
Phosgene, the carbamyl chloride of the isocyanate, hydrogen chloride and any other acidic or basic compounds will
interfere. In refined isocyanates, these impurities are usually present in such small amounts that they do not affect
the determination; however, some crude or modified isocyanates may contain acidities of up to approximately 0,3 %,
so the value reported for the NCO content of unrefined isocyanates should preferably be designated as “corrected”
or “uncorrected” for acidity.
7 Sampling
Since organic isocyanates react with atmospheric moisture, take special precautions in sampling (see warning).
Usual sampling methods (for exampl
...
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