SVENSK STANDARD

SS-EN 6041:2018
Fastställd/Approved: 2018-01-24
Publicerad/Published: 2018-02-09
Utgåva/Edition: 1
Språk/Language: engelska/English
ICS: 49.025.01

Flyg- och rymdteknik – Icke-metalliska material –

Provningsmetod – Analys av icke-metalliska material (ohärdade)
med hjälp av differentiell skanningskalorimetri (DSC)

Aerospace series – Non-metallic materials – Test method –

Analysis of non-metallic materials (uncured) by Differential
Scanning Calorimetry (DSC)
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Europastandarden EN 6041:2018 gäller som svensk standard. Detta dokument innehåller den officiella
engelska versionen av EN 6041:2018.

The European Standard EN 6041:2018 has the status of a Swedish Standard. This document contains the
official version of EN 6041:2018.

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sidor.

© Copyright SIS, Swedish Standards Institute, Stockholm, Sweden. All rights reserved. The use of this product is
governed by the end-user licence for this product. You will find the licence in the end of this document.

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EUROPEAN STANDARD EN 6041

SS-EN 6041:2018 (E)
NORME EUROPÉENNE
EUROPÄISCHE NORM January 2018

ICS 49.025.01

English Version

Aerospace series - Non-metallic materials - Test method -

Analysis of non-metallic materials (uncured) by
Differential Scanning Calorimetry (DSC)
Série aérospatiale - Matériaux non métalliques -
Méthode d'essai - Analyse Enthalpique Différentielle
(AED) des matériaux non métalliques (non
polymérisés)
Luft- und Raumfahrt - Nichtmetallische Werkstoffe -
Prüfverfahren - Analyse von nichtmetallischen
Werkstoffen (ungehärtet) mittels dynamischer
Differenzkalorimetrie (DSC)

This European Standard was approved by CEN on 28 August 2017.

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-CENELEC 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-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION

COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2018 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 6041:2018 E
worldwide for CEN national Members.
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SS-EN 6041:2018 (E)

Contents Page

European foreword ...................................................................................................................................................... 3

1 Scope .................................................................................................................................................................... 4
2 Normative references .................................................................................................................................... 4
3 Symbols and definitions ............................................................................................................................... 4
4 Principle of the method ................................................................................................................................ 5
5 Designation of the method........................................................................................................................... 5
6 Apparatus........................................................................................................................................................... 5
7 Test specimens................................................................................................................................................. 6
8 Procedure .......................................................................................................................................................... 8
9 Presentation of the results .......................................................................................................................... 8
10 Test report ......................................................................................................................................................... 8
Annex A (informative) Equipment ......................................................................................................................... 13
A.1 Mettler TA 3000/TA 2100 - DSC 20/DSC 30 ........................................................................................ 13
A.2 DuPont 9900 ................................................................................................................................................... 13
A.3 Perkin Elmer DSC 2/DSC 4/DSC 7 ........................................................................................................... 13

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SS-EN 6041:2018 (E)

European foreword

This document (EN 6041:2018) has been prepared by the Aerospace and Defence Industries
Association of Europe - Standardization (ASD-STAN).

After enquiries and votes carried out in accordance with the rules of this Association, this Standard has
received the approval of the National Associations and the Official Services of the member countries of
ASD, prior to its presentation to CEN.

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 July 2018, and conflicting national standards shall be
withdrawn at the latest by July 2018.

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.

According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.

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SS-EN 6041:2018 (E)

1 Scope
This test method defines the procedure for the determination of the curing-characteristic and glass
transition temperature of non-metallic materials (e.g. preimpregnated and neat resin systems,
adhesives) for aerospace use by Differential Scanning Calorimetry (DSC).

The results obtained by this method may be useful for:

 derivation of the optimum cure cycle (only together with other test methods e.g. Tg determination)

 assessment of the condition of the resin

 assessment of the ageing behavior of the resin

This European Standard does not give any directions necessary to meet the health and safety
requirements. It is the responsibility of the user of this European Standard to adopt appropriate health
and safety precautions.

2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.

EN 2331, Aerospace series — Textile glass fibre preimpregnates — Test methods for the determination of
the resin and fibre content and mass of fibre per unit area

EN 2559, Aerospace series — Carbon fibre preimpregnates — Determination of the resin and fibre content
and the mass of fibre per unit area

EN 2743, Aerospace series — Fibre reinforced plastics — Standard procedures for conditioning prior to
testing unaged materials

3 Symbols and definitions

For the purposes of this document, the following symbols and definitions apply.

The determination of these parameters shall be agreed upon between manufacturer and purchaser in
case of non-ideal curves or different instrument types.

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SS-EN 6041:2018 (E)

3.1
curing reaction (see Figure 3)
θ is the heating rate, in °C /min or °K /min;
Tos is the onset temperature, in °C or °K;
Tp is the peak maximum temperature, in °C or °K;
∆H is the reaction enthalpy, in J/g;
∆H100 is the reaction enthalpy corrected to 100 % resin content, in J/g.

3.2
calibration (see 6.5)
Tm is the melting temperature, in °C or °K;
∆Hm is the enthalpy of fusion, in J/g.

3.3
glass transition (see Figure 2)
Tgos is the onset temperature of transition, in °C or °K;
Tge is the end temperature of transition, in degrees °C or °K;
Tg is the glass transition temperature, in degrees °C or °K.

4 Principle of the method

Differential Scanning Calorimetry (DSC) measures the temperatures and the heat flow associated with
transitions in materials as a function of time and temperature.

5 Designation of the method

The designation of the method used shall be drawn up according to the following example:

Description block Identity block

ANALYSIS OF NON-METALLIC
MATERIALS (UNCURED)
BY DIFFERENTIAL SCANNING CALORIMETRY (DSC) EN6041

Number of this standard

6 Apparatus

6.1 The test shall be performed in a Differential Scanning Calorimeter (DSC) capable of operating
within the limits laid down in the test procedure.

Instruments are given in the Annex A of this European Standard.

If the DSC-apparatus of the manufacturer and the purchaser are different, a cross-check for comparison
of the test results is necessary.

6.2 Balance with an accuracy of 0,01 mg.

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SS-EN 6041:2018 (E)

6.3 Ancillary items such as sharp cutting knife and tweezers.

6.4 Nitrogen (dry, min. 99,99 % purity).

6.5 Calibration.

The equipment shall be controlled using a pure indium sample to maintain a temperature accuracy to
± 0,5 °C and a calorimetric precision within 1 % during test. Periodically the temperature and cell
constant shall be calibrated using pure samples of the materials specified in Table 1 (type and values
according to DSC manufacturer recommendations).

Temperature calibration shall be performed using two or preferably three materials over the
temperature range of interest.

Sub-ambient temperature operation shall be achieved by the application of sub-ambient accessories

specifically designed for use with the particular instrument being used (see Clause 8).

For sub-ambient operations ice (H2O or cyclohexane) shall also be used for calibration (the starting
temperature shall be below ‒ 40 °C).

The heating rate for calibration shall be the same as used in the subsequent experiments i.e. 10 °C/min
for standard operation (see Clause 8).

The instrument calibration shall be performed using the same sample pan type, purge/purge rate and
equivalent thermal mass samples as will be used in subsequent experiments.

The base line and the cell shall be checked periodically (interval to be agreed between the parties). The
base line drift for a pair of empty pans or pans containing an inert substance shall not exceed 1,0 mW
over the range ‒ 50 °C to 300 °C.

7 Test specimens
7.1 Preparation
7.1.1 General

Test specimens shall be selected in accordance with the sampling procedure defined in the material
specification.

Each sample shall comprise approximately the equivalent of 7 mg to 10 mg of neat resin (for example
20 mg of prepreg). In case of extreme enthalpy of reaction the sample size of the material may be
adjusted to achieve acceptable curves in the diagram.

The sample mass shall be determined to 0,01 mg (see 6.2). For quantitative measurements it is
necessary to correct the ∆H to 100 % resin content (∆H100), the resin content shall be determined using
the test methods of 7.1.2 or 7.1.3.

A minimum of two test specimens shall be used for standard operations (e.g. release testing). For
determination of standard deviations a minimum of six specimens are necessary (i.e. qualification
programs).

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SS-EN 6041:2018 (E)

7.1.2 Determination of actual fibre/resin content

Carbon composite : according to EN 2559;

Glass composite : according to EN 2331;

Aramid composite : according to EN 2559 but using HNO3/DMSO.

If an insoluble filler (such as SiO2) is present, it shall be determined separately (after the removal of the
fibre) by centrifuging and its mass added to the reinforcement content.

7.1.3 Determination of actual carrier/resin content for adhesives

Usual extraction technique: use ultrasonic bath and appropriate solvent such as DMF, DMSO, NMP.

Determine the carrier weight after twice flushing with solvents such as acetone or MEK and thorough
drying.

If an insoluble filler is present, it shall be determined separately (after the removal of the carrier) by
centrifuging and its mass added to the reinforcement content.

Actual resin content: mresin = madhesive − mcarrier

7.2 Conditioning
7.2.1 Conditioning of material stored at ambient temperature

For material stored at ambient temperature, the amount of material (together with the release film on
it) required for testing shall be sampled and conditioned in the standard atmosphere (defined in EN
2743) for a minimum of 2 h, unless otherwise specified.

7.2.2 Conditioning of material stored below ambient temperature

For material stored at temperatures lower than ambient temperature, the material, suitably packed in
an airtight bag (containing a suitable desiccant) to prevent moisture pick-up, shall be allowed to reach
ambient temperature over a period of time according to the mass of the package.

The actual time shall be recorded in the report. When the material has reached ambient temperature,
the amount (together with the release film on it) required for testing shall be sampled and conditioned
in the standard atmosphere (defined in EN 2743) for a minimum of 2 h, unless otherwise specified.

7.2.3 Standard atmosphere for testing

The test equipment shall be at (23 ± 2) °C and (50 ± 5) % relative humidity (EN 2743 B conditions). The
actual test environment is controlled inside the equipment.

7.2.4 Time interval between conditioning and testing

After conditioning, the test shall be carried out within 6 h, unless otherwise specified, the specimen
being kept in the standard atmosphere until the test is carried out.