INTERNATIONAL ISO
STANDARD 1172
Second edition
1996-12-15
Textile-glass-reinforced plastics -
Prepregs, moulding compounds and
laminates - Determination of the textile-
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glass and mineral-filler content -
Calcination methods
(standards.iteh.ai)
ISO 1172:1996
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Plas tiques ren forcks de verre textile - Preimpr@gn&, compositions de
9d60-169486c58f85/iso-1172-1996
moulage et s tra tifies - Determination des taux de verre textile et de
Charge mirGrale - M6 thodes par calcina tion
Reference number
ISO 1172:1996(E)
ISO 1172:1996(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
(IEC) 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 1172 was prepared by Technical Committee
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ISO/TC 61, Plastics, Subcommittee SC 13, Composites and rehforcement
fibres.
(standards.iteh.ai)
This second edition cancels and replaces the first edition (ISO 1 172:1975),
which has been technically revised (an additional method, ISO 1172:1996
method B, has
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been included and the annex, which concerned the estimation of the
Standard deviation, has been replaced by annex 9d60-169486c58f85/iso-1172-1996
A describing an alternative
method of separating chopped glass fibre from mineral filier).
Annex A of this International Standard is for information only.
0 ISO 1996
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 mechanical, including
photocopying and microfilm, without Permission in writing from the publisher.
International Orga nization for Standardization
Case Postale 56 l CH-1 21 1 Geneve 20 l Switzerland
Printed in Switzerland
ii
INTERNATIONAL STANDARD @ ISO ISO 1172:1996(E)
Textile-glass-reinforced plastics - Prepregs, moulding compounds
and laminates - Determination of the textile-glass and mineral-
filler content - Calcination methods
WARNING - This International Standard does not give details of the precautions that should be taken to
meet health and safety requirements. The test methods described require the use of high temperatures and
concentrated acids. lt is the responsibility of the User of this International Standard to follow the
appropriate health and safety procedures.
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1 Scope
(standards.iteh.ai)
This International Standard specifies two calcination methods for the determination of the textile-glass
ISO 1172:1996 and mineral-
filier content of glass-reinforced plastics:
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9d60-169486c58f85/iso-1172-1996
Method A: for the determination of the textile-glass content when no mineral fillers are present.
Method B: for the determination of the textile-glass and mineral-filler content when both components are
present.
This International Standard is applicable to the following types of material:
- prepregs made from yarns, rovings, tapes or fabrics;
- SMC, BMC and DMC moulding compounds;
- textile-glass-reinforced thermoplastic moulding materials and granules;
- filled or unfilled textile-glass laminates made with thermosetting or thermoplastic resins.
The methods are not applicable to the following types of reinforced plastic:
- those containing reinforcements other than textile glass;
- those containing materials which do not completely burn off at the test temperature (for example, those based
on Silicone resin);
- those containing mineral fillers which degrade at temperatures below the minimum calcination temperatute.
For these materials, ISO 1 1667, Fibre-reinforced plastics - Maulding compounds and prepregs - Determination
of resin, reinforcement-fibre and mineral-filler content - Dissolution method, may be used.
ISO 1172:1996(E) @ ISO
2 Normative references
The following Standards contain provisions which, through reference in this text, constitute provisions of this
International Standard. At the time of publication, the editions indicated were valid. All Standards are subject to
revision, and Parties to agreements based on this International Standard are encouraged to investigate the
possibility of applying the most recent editions of the Standards indicated below. Members of IEC and ISO maintain
registers of currently valid International Standards.
ISO 472:1988, Plastics - Vocabulary.
ISO 4793: 1980, Laboratory sintered (fritted) filters - Porosity gradhg, classifica tjon and designa tion.
ISO 8604: 1988, Plastics - Prepregs - Definitions of terms and Symbols for deslgnations.
3 Definitions
For the purposes of this International Standard, the definitions given in ISO 472 and ISO 8604 apply.
4 Principle
A test specimen is weighed and subsequently calcinated at a defined temperature. The specimen is then
reweighed and the non-combustible matter content (glass + filier) obtained by determining the differente in mass
of a test specimen before and after calcination in one of the following ways:
a)
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In the case of materials containing no fillers the glass content is calculated directly from the differente in mass
(method A);
(standards.iteh.ai)
b) In the case of materials containing both glass and filler, the glass and filier remaining after calcination are
separated by dissolution of the filier in hydrochloricISOacid. The differente between the mass of the specimen
1172:1996
before calcination and the mass of the dried specimen after reaction with acid is used to measure the glass
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content. The filier content is obtained by9d60-169486c58f85/iso-1172-1996
calculating the differente between the mass of the specimen after
calcination and the mass of the dried specimen after reaction with acid (method B).
The test method requires that all weighings be made at constant mass after repeated calcination and/or drying. In
those cases where known materials are being tested regularly, a minimum time for the calcination and drying
stages may be determined by experiment to ensure that constant mass has been reached.
NOTES
1 If the material tested contains a resin which is combustible under the test conditions and/or fillers which do not degrade by
calcination, then the loss on ignition is equal to the resin content. lt should be noted that the resin content calculated in this
way includes the combustible part of the other components in the composition (glass size, Pigments, etc.) but this is usually
small compared to the resin content.
2 In those cases where fillers are present that are degraded at the test temperature, it is not possible to obtain an accurate
determination of the glass, resin or filier content.
5 Sampling
5.1 The determination of the glass and filier contents is shall be carried out in parallel on two specimens which
are as near identical as possible. The result of the test is the average of the measurements on the two specimens,
provided that the differente between the two measurements is less than 5 %. If this is not the case, a third
specimen shall be tested which is as near identical to the other two as possible. The three values shall then be
used to calculate the test result.
5.2 In Order to carry out an evaluation test the result of which is as representative as possible of the glass and
filier content of the elementary unit or laboratory Sample, this test procedure may need to be repeated a certain
number of times, at specific locations in the elementary unit examined. The number of times and the actual
0 ISO ISO 1172:1996(E)
locations will be defined either in the product specification or by the person reques tin g the analysis. In the latter
case, the number and location will be decided by experience or as the result 0 f previo us work.
5.3 For all tests other than those on elementary units, take specimens that are as representative of the material
under test as circumstances allow.
6 Preparation of test specimens
The test specimen s shal I be fully representative of the piece or batch examined. They shall be obtained in
accordance with cla use 5.
Unless otherwise specified, it is recommended that the specimens be tut out in a shape which allows them to fit
into a silica boat or porcelain crucible.
The mass of each specimen shall be within the range
2 g to 20 g for prepregs and moulding compounds;
2 g to 10 g for laminates.
For each test result, use a minimum of two specimens (see 5.1).
In the case of prepregs and moulding compounds which contain solvents or free monomer, care shall be taken to
avoid loss of volatile matter. For SMC, the protective release film shall not be removed from the laboratory Sample
or the test specimen until just before commencing the test procedure. All prepreg and moulding-compound
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laboratory samples, including SMC, shall be sealed in a vapourproof plastic bag immediately after the laboratory
Sample has been taken.
(standards.iteh.ai)
ISO 1172:1996
7 Determination
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9d60-169486c58f85/iso-1172-1996
The choice of method used to determine the glass and filler content will depend on the presence or absence of
filler. The methods described in this International Standard are
Method A: for the determination of the glass content when no fillers are present.
Method B: for the determination of the glass and filler content when both components are present.
7.1 Method A
7.1.1 Reagents
No reagents are required for method A.
7.1.2 Apparatus
Normal laboratory apparatus, plus the following:
7.1.2.1 Balance, graduated to 0,l mg.
7.1.2.2 Silica boat or porcelain crucible, of a suitable size to contain a specimen.
7.1.2.3 Muffle furnace, located under a ventilated hood and capable of maintaining the Chosen temperature (see
7.1.3.2) to within st 20 “C.
7.1.2.4 Desiccator, containing a suitable drying agent (e.g. silica gel).
3
ISO 1172:1996(Ei)
7.1.2.5 Ventilated drying oven, set at 105 “C + 3 “C.
7.1.3 Procedure
For each specimen, proceed as follows:
7.1.3.1 Preparation of the boat or crucible
Weigh the clean, dry boat or crucible (7.1.2.2) to the nearest 0,l mg on the balance (7.121). Place in the muffle
furnace (7.123) set to the Chosen temperature (see 7.1.3.2) and leave for 10 min. After cooling to ambient
temperature in the desiccator (7.124) verify that the mass has not changed. If there has been a Change, repeat
these operations until constant mass is reached.
7.1.3.2 Calcination
Weigh the clean, dry boat or crucible, prepared as indicated in 7.1.3.1. Record the mass in grams as ml.
Place a specimen in the boat or crucible and dry in the ventilated drying oven (7.125) at 105 “C to constant mass.
Cool to ambient temperature in the desiccator and reweigh. Record the mass in grams as m2.
In the case of specimens which contain volatile matter, care is needed to avoid loss of the volatile matter. Omit the
drying Stage therefore. Remove the specimen from the vapourproof bag and remove any release film. Place the
specimen in the boat or crucible, weigh and record the mass in grams as mg.
Place the boat or crucible con taining the test specimen in the muffle furnace, preheated to a temperature of 625 “C
and h eat to constant mass. iTeh STANDARD PREVIEW
For reinforced products with glass or filier (standards.iteh.ai)
which will not withstand this calcination temperature, a temperature
between 500 “C and 600 “C may be used, in accordance with the specification for the glass or filler. lt is essential
to maintain the Chosen temperature constant to & 20 “C.
ISO 1172:1996
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Allow the boat or crucible, togeth er with the residue, to cool in the desiccator to ambient temperature
9d60-169486c58f85/iso-1172-1996 and reweigh.
Record the mass in grams as m3.
7.1.4 Expression of results
Calculate, for each specimen, the glass content MgrasS, expressed as a percentage of the initial mass, using
equation (1):
m3 . . . (1)
Mglass = -ml XI00
m2 -m1
m1 is the initial mass, in grams, of the dry boat or crucible;
m2 is the initial mass, in grams, of the dry boat or crucible plus dried specimen;
m3 is the final mass, in grams, of the boat or crucible plus residue after calcination.
In the case of specimens containing volatile matter, when the drying Stage was omitted, replace m2 in equation (1)
by mg, where m6 is the initial mass, in grams, of the dry boat or crucible plus undried test piece.
If the results of the individual measurements differ by more than 5 % in relative value, carry out an additional
determination on a third specimen taken from the same location in the elementary unit or laboratory Sample.
Express the result of the test as the average of the two (or three) individual measurements.
0 ISO ISO 1172:1996(E)
7.2 Method B
7.2.1 Reagents
The following reagents are required for method B.
7.2.1.1 Hydrochlorit acid, 35 % (V/V) concentration, commercial grade.
7.2.1.2 Denatured ethanol.
7.2.1.3 Chromic acid mixture, for cleaning.
The recommended composition of the mixture is 7 % sodium dichromate in concentrated sulfuric acid.
7.2.2 Apparatus
The apparatus given in 7.12, plus the following:
7.2.2.1 40 mm diameter sintered-glass filter, porosity P 160, i.e. 100 Pm to 160 Pm (see ISO 4793).
7.2.2.2 250 mlbeaker.
7.2.2.3 Suction flask.
7.2.2.4 Glass rod.
7.2.2.5 Tweezers. iTeh STANDARD PREVIEW
7.2.3 Procedure
(standards.iteh.ai)
For each test specimen, proceed as follows:
ISO 1172:1996
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7.2.3.1 Preparation of boats or crucibles 9d60-169486c58f85/iso-1172-1996
Follow the procedure given in 7.1.3.1.
7.2.3.2 Preparation of sintered-glass filter
Before each test, clean the sintered-glass filter (7.221) by soaking in the chromic acid mixture (721.3). Place the
filter on the suction flask (7.2.2.3), apply the suction, and rinse the filter first with warm water, then with denatured
ethanol (7.2.1.2). Dry the filter in the drying oven (7.1.2.5) to constant mass. Record the mass in grams as m4.
7.2.3.3 Calcination
Follow the procedure given in 7.1.3.2.
7.2.3.4 Separation of glass and filier when filier completely dissolves in hydrochloric acid
Separate the filier from the glass as follows:
Place into the 250 ml beaker (7.2.2.2) 5 ml of hydrochloric acid (7.2.1 .l) per gram of residue remaining in the
boat or crucible after calcination.
Using the glass rod, slowly add the residue in the boat or crucible to the acid in the beaker. Stir carefully to
ensure that all the residue has reacted with the acid, taking care that the effervescence caused by the acid
reacting with the carbonate fillers does not Cause droplets to spit out of the beaker.
When the effervescence finished, three-quarters fill the boat or crucible with water and pour it all into the
250 ml beaker, repeating if necessary until all the residue has been transferred to the beaker.
Add an additional 50 ml of water to the beaker.
ISO 1172:1996(E) 0 ISO
Place the filter, dried and weighed as described in 7.2.3.2, on the suction flask and apply the suction.
Slowly pour the acid over the glass on to the filter.
Rinse the glass in the beaker with water and pour the water on to the filter; then rinse with denatured alcohol,
agitating with a glass rod, and pour alcohol on to the filter.
Repeat this Operation four or five times until the glass is thoroughly clean.
Transfer the glass on to the filter using the glass rod and a jet of denaturated ethanol.
Rinse twice with denaturated ethanol.
Dry the filter to constant mass in the drying oven.
Allow to cool in the desiccator to ambient temperature and weigh. Record the mass in grams as “5.
Alternatively, if the fibre length is greater than 12 mm, the procedure described in informative annex A may be
used. The procedure given in 7.2.3.4 shall always be used as the reference method, however.
7.2.3.5 Separation of glass and filler when filler does not completely dissolve in hydrochloric acid
If filler insoluble in hydrochloric acid remains on the filler on filtering, determine the mass mg as described in 7.2.3.4,
continue as follows:
Using tweezers (7.2.2.5), pick out all the glass from the filter. Reweigh the filter with the insoluble filler on it.
Record this mass in grams as m7.
NOTE - If the glass filaments are very short, it may not be possible to separate them from the filier manually. In this case,
the method given in this International Standard is not capable of giving accurate values of the glass and filier contents
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separately, although the combined filier and glass content tan be determined.
7.2.4 Expression of results
(standards.iteh.ai)
Calc ulate, for each specimen, the glass CO ntentQass ISO 1172:1996
and the filler content Mfiirer, expre ssed as a percentage of
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the i nitial mas s, usi ng equations (2 1 and (31, respectively
9d60-169486c58f85/iso-1172-1996
m5 -m4 XI00
Qass = . . . (2)
m2 -m1
m3 - rnj - mg - m4 \
Mfiller = XI00 . . . (31
t m2 - ml m2 - ml 1
where
m1 is the initial mass, in grams, of the dry boat or crucible;
m2 is the initial mass, in grams, of the dry boat or crucible plus the dried specimen;
m3 is the final mass, in grams, of the boat or crucible plus residue after calcination;
m4 is the mass, in grams, of the dry filter;
"5 is the mass, in grams, of the filter plus contents after reacting the residue with acid.
In the case of moulding compounds containing vo latile m atter, when the drying Stage was omit ted, replace m2 in
th e equation by mg, where m6 iS the initial mass rn grams, of the dry boat or crucible plus undried test piece.
If filler insoluble in hydrochloric acid rema ined on th e filter on fi ltering, repla ce rn4 in equations (2) and (3) by m7,
where m7 is the mass, in grams, of ahe dry filter plus undissolved minera filler
lf the results of the individual measurements differ by more than 5 % in relative value, carry out an additional
determination on a third specimen taken from the Same location in the elementary unit or laboratory Sample.
Express the result of the test as the average of the two (or three) individual measurements.
@ ISO ISO 1172:1996(E)
8 Precision
The precision of thi s test method is not known because in t,er-Iaboratory data are not yet available. When inter-
laboratory data have been obtained, a precision Statement wil be added at the following revision.
NOTE - he inte r-laboratory trials will include an investigation of the relative precision of the procedure given in 723.4 and
that given annex A.
9 Test report
The test report shall include the following:
a) the number of this International Standard;
b) whether method A or method B was used;
d all details necessary for complete identification of the material tested;
d) the sampling method used;
d the number of specimens tested;
fl the dimensions and/or mass of the specimens;
9) the calcination temperature, if different from 625 “C + 20 “C;
t-4 the test result for the textile-glass content;
i) the test result for the mineral-filler content if method B was used;
0 the date of the test; iTeh STANDARD PREVIEW
kl details of any anomaly (standards.iteh.ai)
or incident likely to have had an effect on the results, specifically:
1) the presence of any undissolved filler,
2)
ISO 1172:1996
any difficulty experienced in manually separating the textile glass and undissolved filler.
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9d60-169486c58f85/iso-1172-1996
