EN ISO 10548:1996

SLOVENSKI STANDARD
SIST EN ISO 10548:1999
01-maj-1999
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Carbon fibre - Determination of size content (ISO 10548:1994)
Kohlenstoffasern - Bestimmung des Präparationsmassenanteils (ISO 10548:1994)
Fibres de carbone - Détermination du taux d'ensimage (ISO 10548:1994)
Ta slovenski standard je istoveten z: EN ISO 10548:1996
ICS:
59.100.20 Ogljikovi materiali Carbon materials
SIST EN ISO 10548:1999 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 10548:1999

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SIST EN ISO 10548:1999

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SIST EN ISO 10548:1999

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SIST EN ISO 10548:1999

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SIST EN ISO 10548:1999

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SIST EN ISO 10548:1999
INTERNATIONAL
ISO
STANDARD
10548
First edition
19944 1-01
Carbon fibre
- Determination of size
content
Fibfes de cafbone - Dbtermination du taux d ’ensimage
Reference number
ISO 10548:1994(E)

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SIST EN ISO 10548:1999
ISO 10548:1994(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. Esch 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
(1 EC) on all matters of electrotechnical standardization.
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 10548 was prepared by Technical Committee
ISOnC 61, Mastics, Subcommittee SC 13, Composites and reinforce-
men t fibres.
0 ISO 1994
All rights reserved. Unless otherwise specified# no part of this publication may be reproduced
or utilized in any form or by any means, electronie or mechanrcal, rncludrng photocopyrng and
microfilm, without Permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-l 211 Geneve 20 l Switzerland
Printed in Switzerland
ii

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SIST EN ISO 10548:1999
INTERNATIONAL STANDARD 0 ISO ISO 10548:1994(E)
Carbon fibre - Determination of size content
Method B: size removal by Chemical digestion us-
1 Scope
ing a mixture of sulfuric acid and hydrogen per-
Oxide, used when the size is partially hardened and
This International Standard specifies test methods for
not completely soluble in solvents.
the determination of the size content of carbon fibre
yarn. lt is applicable to continuous-filament yarns and
Method C: size decomposition by pyrolysis at high
staple-fibre yarns.
temperature in an atmosphere of nitrogen, used
when the size is completely removed by pyrolysis.
2 Normative reference
The test methods require all weighings to be made to
The following Standard contains provisions which,
constant mass by repetition of the drying or dissol-
through reference in this text, constitute provisions
ution stages. In those cases where known materials
of this International Standard. At the time of publica-
are being tested regularly, it is permitted to define,
tion, the edition indicated was valid. All Standards are
by experiment, a minimum time for dissolution and
subject to revision, and Parties to agreements based
drying which will ensure that constant mass has been
on this International Standard are encouraged to in-
obtained.
vestigate the possibility of applying the most recent
edition of the Standard indicated below. Members of
IEC and ISO maintain registers of currently valid
5 Test specimens
International Standards.
Two test specimens shall be taken adjacent to one
ISO 1886: 1990, ßeinforcement fibres - Sampling
another from each elementary unit or yarn Sample.
Plans applicable to received ba tches.
The size content is taken as the average of the two
determinations. Esch test specimen shall have a
minimum mass of 2 g.
3 Definitions
If the determination is carried out for the purpose of
For the purposes of this International Standard, the
lot acceptance, the lot received shall be sampled in
following definitions apply.
accordance with ISO 1886.
3.1 size: Any material applied to fibres to facilitate
When handling test specimens, gloves shall be worn
the handling and use of the fibres.
or tweezers used to avoid darnage to the specimens.
3.2 size content: The mass of the size expressed
NOTE 1 The specification or the person requiring the test
as a percentage of the sized carbon fibre yarn.
may stipulate that additional determinations be carried out
at different places within the elementary unit.
4 Principle
6 Conditioning
Test specimens are weighed before and after removal
of the size by one of the following three methods:
Elementary units and yarn samples shall be allowed
to attain laboratory temperature before testing. Before
Method A: size removal by Soxhlet extraction, to
be used when the size is completely soluble in a weighing the yarn, it shall always be dried for 1 h at
suitable solvent. a temperature of 110 “C + 5 “C.
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SIST EN ISO 10548:1999
0 ISO
ISO 10548:1994(E)
7.1.2.2 Weigh the thimble to the nearest 0,l mg
7 Test methods
( 1
*1 -
7.1 Method A: Solvent extraction
7.1.2.3 Place a test specimen in the thimble and
weigh to the nearest 0,l mg (4).
7.1 .l Apparatus and materials
7.1.2.4 Place the thimble and its contents in the si-
7.1.1.1 Balance, accurate to 0,5 mg, readable to phon chamber of the Soxhlet apparatus (7.1 .1.4),
0,l mg. place a sufficient volume of solvent in the flask to
ensure Operation of the Siphon during the reflux cy-
cles.
7.1.1.2 Hot-air oven, capable of being controlled to
+ 5 “C.
-
7.1.2.5 Extract for 2 h. Adjust the heating mantle
(7.1 .1.8) so that at least four reflux cycles occur during
7.1 .1.3 Desiccator, containing a suitable desiccant,
the 2 h extraction period.
for example silica gel, anhydrous Calcium chloride or
phosphorus pentoxide.
7.1.2.6 Turn off the heating mantle. Wait 10 min for
the apparatus to cool. Remove the thimble and con-
7.1.1.4 Soxhlet extractor, 200 ml capacity, with a
tents. Allow to stand at ambient temperature for
500 ml flask.
10 min to allow excess solvent to evaporate.
7.1.1.5 Soxhlet extraction thimbles, measuring
7.1.2.7 Dry the thimble and contents for 1 h in the
41 mmxl23mm.
oven (7.1 .1.2) at 110 “C + 5 “C and allow to cool in a
desiccator. Weigh to the nearest 0,l mg.
NOTE 2 The sizes of the Soxhlet extractor, the flask and
the Soxhlet extraction thimbles are given as an indication
only and may be varied to suit individual requirements. If the solvent used has a boiling Point higher than
100 “C, adjust the oven to a temperature 10 “C above
IMPORTANT - The extraction and all handling the boiling Point of the solvent.
of organic solvents should be carried out in a fume
cupboard.
7.1.2.8 Repeat the drying and weighing procedure
until the differente in mass between two successive
7.1.1.6 Rubber gloves or tweezers. weighings (9) is less than + 0,2 mg.
7.1 .1.7 Cutting blade.
7.1.3 Procedure 2
7.1.1.8 Heating mantle, fitted with a power regula-
7.1.3.1 If the specimen is free of loose fibre and tan
tor capable of controlling the boiling rate of the sol-
be coiled into a form which tan be inserted into the
vent.
Soxhlet extraction chamber without the danger of loss
of fibre during extraction, an extraction thimble need
7.1.1.9 Distilled water, or an organic solvent such not be used.
as butan-2-one (methyl ethyl ketone), tetrahydrofuran,
dichloromethane (methylene chloride), acetone or
7.1.3.2 Weigh the test specimen to the nearest
dichloroethane.
OJ mg ( 1
*4 -
NOTE 3 The choice of solvent depends upon the type of
7.1.3.3 Carry out the extraction as described in Pro-
size applied to the carbon fibre under test. This choice is
cedure 1, but without the extraction thimble.
best made by consultation between the customer and the
supplier.
7.1.3.4 Dry the Spesimen for 1 h at 110 “C + 5 “C
-
and allow to cool in a desiccator. Weigh to the nearest
7.1.2 Procedure 1
0,l mg.
7.1.2.1 Dry an extraction thimble (7.1 .1.5) at
7.1.3.5 Repeat the drying, cooling and weighing
105 “C + 5 “C in the oven (7.1 .1.2) for 1 h and allow
-
procedure until the differente in mass between two
to cool to room temperature in the desiccator
success
...