DEUTSCHE NORM October 2004

DIN EN ISO 306 DIN

ICS 83.080.20 Supersedes January 1997
edition.

Plastics
Thermoplastic materials
Determination of Vicat softening temperature (VST)
(ISO 306: 2004)
English version of DIN EN ISO 306

Kunststoffe - Thermoplaste - Bestimmung der Vicat-

Erweichungstemperatur (VST) (ISO 306: 2004)

European Standard EN ISO 306: 2004 has the status of a DIN Standard.

A comma is used as the decimal marker.

National foreword
This standard has been published in accordance with a decision taken by CEN/TC 249 to adopt, without
alteration, International Standard ISO 306 as a European Standard.
The responsible German body involved in its preparation was the Normenausschuss Kunststoffe (Plastics
Standards Committee), Technical Committee Mechanische Eigenschaften and ProbekOrperherstellung.
The DIN Standards corresponding to the International Standards referred to in clause 2 of the EN are as
follows:
ISO Standard DIN Standard
ISO 291 DIN EN ISO 291
ISO 293 DIN EN ISO 293
ISO 294-1 DIN EN ISO 294-1
ISO 294-2 DIN EN ISO 294-2
ISO 294-3 DIN EN ISO 294-3
ISO 2818 DIN EN ISO 2818
ISO 3167 DIN EN ISO 3167

Amendments
This standard differs from the January 1997 edition in that it has been completely revised.

Previous editions
DIN 53460: 1965-10, 1969-09, 1976-12; DIN ISO 306: 1990-09; DIN EN ISO 306: 1997-01.

Continued overleaf.
Document comprises 13 pages.

© No part of this standard may be reproduced without the prior permission of English price group 10
DIN Deutsches Institut fur Normung a V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,
has the exclusive right of sale for German Standards (DIN-Normen).
www.din.de
www.beuth.de
11)2111119M
Page 2
DIN EN ISO 306 : 2004-10

National Annex NA
Standards referred to
(and not included in Normative references)
DIN EN ISO 291 Plastics — Standard atmospheres for conditioning and testing (ISO 291 : 1997)
DIN EN ISO 293 Plastics — Compression moulding test specimens of thermoplastic materials
(ISO 293:1986)
DIN EN ISO 294-1 Plastics — Injection moulding of test specimens of thermoplastic materials — Part 1: General
principles, and moulding of multi-purpose and bar test specimens (ISO 294-1 : 1996)
DIN EN ISO 294-2 Injection moulding of test specimens of thermoplastic materials — Part 2: Small tensile bars
(ISO 294-2 : 1996)
DIN EN ISO 294-3 Plastics — Injection moulding of test specimens of thermoplastic materials — Part 3: Small
plates (ISO 294-3 : 2002)
DIN EN ISO 2818 Plastics — Preparation of test specimens by machining (ISO 2818: 1994)
DIN EN ISO 3167 Plastics — Multi-purpose test specimens (ISO 3167: 2002)

EUROPEAN STANDARD EN ISO 306
NORME EUROPEENNE

EUROPAISCHE NORM July 2004

ICS 83.080.20

English version

Plastics
Thermoplastic materials
Determination of Vicat softening temperature (VST)
(ISO 306: 2004)

Plastiques — Matieres thermoplasti- Kunststoffe — Thermoplaste — Bestim-

ques — Determination de la tempe- mung der Vicat-Erweichungstempera-
rature de ramollissement Vicat (VST) tur (VST) (ISO 306 : 2004)
(ISO 306 : 2004)

This European Standard was approved by CEN on 2004-07-07.

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.
The European Standards exist 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, Cyprus, the
Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary,
Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, the Netherlands,
Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland, and
the United Kingdom.

CEN
European Committee for Standardization
Comite Europeen de Normalisation
Europaisches Komitee fur Normung

Management Centre: rue de Stassart 36, B-1050 Brussels

© 2004. CEN - All rights of exploitation in any form and by any means Ref. No. EN ISO 306: 2004 E
reserved worldwide for CEN national members.
Page 2
EN ISO 306 : 2004

Foreword
International Standard
ISO 306 : 2004 Plastics — Thermoplastic materials — Determination of Vicat softening temperature (VST),
which was prepared by ISO/TC 61 'Plastics' of the International Organization for Standardization, has been
adopted by Technical Committee CEN/TC 249 'Plastics', the Secretariat of which is held by IBN, as a European
Standard.
This European Standard shall be given the status of a national standard, either by publication of an identical
text or by endorsement, and conflicting national standards withdrawn, by January 2005 at the latest.
In accordance with the CEN/CENELEC Internal Regulations, the national standards organizations of the follo-
wing countries are bound to implement this European Standard:
Austria, Belgium, Cyprus, the Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary,
Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland, Portugal, Slo-
vakia, Slovenia, Spain, Sweden, Switzerland, and the United Kingdom.

Endorsement notice
The text of the International Standard ISO 306 : 2004 was approved by CEN as a European Standard without
any modification.

Contents Page

1 Scope 3
2 Normative references 3
3 Principle 3
4 Apparatus 4
5 Test specimens 7
6 Conditioning 8
7 Procedure 8
8 Repeatability 8
9 Test report 8
Annex A (informative) Comparison of VST results obtained with heating bath and direct-contact
heating unit 9
Annex B (informative) Repeatability 11
 Page 3
EN ISO 306 : 2004

1 Scope

1.1 This International Standard specifies four methods for the determination of the Vicat softening
temperature (VST) of thermoplastic materials:
— Method A50 using a force of 10 N and a heating rate of 50 °C/h
— Method B50 using a force of 50 N and a heating rate of 50 ° C/h
— Method Al20 using a force of 10 N and a heating rate of 120 °C/h
— Method B120 using a force of 50 N and a heating rate of 120 ° C/h.

1.2 The methods specified are applicable only to thermoplastics, for which they give a measure of the
temperature at which the thermoplastics start to soften rapidly.

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 291, Plastics — Standard atmospheres for conditioning and testing

ISO 293, Plastics — Compression moulding of test specimens of thermoplastic materials

ISO 294-1, Plastics — Injection moulding of test specimens of thermoplastic materials — Part 1: General
principles, and moulding of multipurpose and bar test specimens

ISO 294-2, Plastics — Injection moulding of test specimens of thermoplastic materials — Part 2: Small tensile
bars

ISO 294-3, Plastics — Injection moulding of test specimens of thermoplastic materials — Part 3: Small plates

ISO 2818, Plastics — Preparation of test specimens by machining

ISO 3167, Plastics — Multipurpose test specimens

3 Principle

The temperature at which a standard indenting tip with a flat point penetrates 1 mm into the surface of a plastic
test specimen is determined. The indenting tip exerts a specified force perpendicular to the test specimen, while
the specimen is heated at a specified and uniform rate.

The temperature, in degrees Celsius, of the specimen, measured as close as possible to the indented area at
1 mm penetration, is quoted as the VST.
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EN ISO 306 : 2004

4 Apparatus
The apparatus consists essentially of the following:

4.1 Rod, provided with a weight-carrying plate or other suitable load-applying device (see 4.4), held in a
rigid metal frame in a liquid-filled bath or direct-contact heating unit so that it can move freely in the
vertical direction. In either case, the base of the frame supports the test specimen under the indenting tip at the
end of the rod (see Figures 1 and 2).

Unless the rod has the same linear thermal expansion coefficient as the rigid metal frame, the differential
change in the length of these parts introduces an error in the indentation readings. A blank test shall therefore
be carried out on each rod and frame assembly, using a test specimen made of rigid material having a known,
low coefficient of expansion. 1) The blank test shall cover the temperature range typical of the type of material to
be tested. A correction factor shall be determined for at least each 10 ° C change in temperature, for each rod
and frame assembly. If the correction factor is 0,02 mm or greater near the VST for that material, its algebraic
sign shall be noted and the factor applied to each test result by adding it algebraically to the apparent
indentation reading. It is recommended that the apparatus be constructed of low thermal expansion material.

4.2 Indenting tip, preferably of hardened steel, 1,5 mm to 3 mm long, of circular cross-section, and of area
1,000 mm 2 + 0,015 mm 2 (corresponding to an indenting-tip diameter of 1,128 mm ± 0,008 mm), fixed at the
bottom of the rod (4.1). The surface of the indenting tip in contact with the specimen shall be plane and
perpendicular to the axis of the rod, and free from burrs.

4.3 Calibrated micrometer dial gauge (or other suitable measuring instrument), to measure to ± 0,01 mm
the penetration of the indenting tip into the test specimen. The thrust of the dial gauge, which contributes to the
thrust on the test specimen, shall be recorded (see 4.4).

NOTE 1 In certain types of apparatus, the force of the dial gauge spring is directed upwards and is subtracted from the
load; in other types, this force acts downwards and is added to the load.

NOTE 2 Since the force exerted by the spring in certain dial gauges varies considerably over the stroke, this force is
measured at the position where the indenting tip has penetrated 1 mm into the specimen.

4.4 Weight-carrying plate, fitted to the rod (4.1), and suitable weights added centrally so that the total load
applied to the test specimen can be made up to 10 N ± 0,2 N for methods A50 and Al20 and 50 N ± 1 N for
methods B50 and 8120. The combined downward thrust, determined during calibration of the apparatus, due to
the rod, the indenting tip, the weight-carrying plate and the upward or downward force exerted by the dial gauge
spring in the measurement range used during the test, shall not exceed 1 N.

Other suitable devices for applying the load can be used provided the requirements specified above are met.

1) lnvar and borosilicate glass have been found suitable for this purpose.
 Page 5
EN ISO 306: 2004

Key
1 micrometer dial gauge
2 replaceable weight
3 weight-carrying plate
4 rod with indenting tip
5 approximate level of liquid
6 indenting tip
7 test specimen
8 test-specimen support

Figure 1 — Example of apparatus with a liquid-filled heating bath for determination of the VST
Page 6
EN ISO 306 : 2004

Key
1 weight
2 displacement-measurement device
3 heater
4 heating block
5 rod with indenting tip
6 temperature-measurement unit
7 test specimen

Figure 2 — Example of apparatus with a direct-contact heating unit for determination of the VST

4.5 Heating equipment, consisting of a heating bath (4.5.1) containing a liquid or of a direct-contact heating
unit (4.5.2). The heating equipment shall be provided with temperature-control means enabling the temperature
to be raised at a uniform rate of 50 ° C/h + 5 ° C/h or 120 ° C/h + 10 ° C/h

The heating rate shall be verified

— either by checking the automatically read temperature;

— or by checking manually the temperature change at intervals of, at the most, 6 min during the whole of the
test.

The requirement for the heating rate shall be considered satisfied if, over every 6 min interval during the test, the
temperature change is 5 ° C + 0,5 ° C or 12 ° C ± 1 °C, respectively. For multi-position baths, the heating rate
shall be verified at each test station.
 Page 7
EN ISO 306 : 2004

The apparatus may be designed to shut off the heat automatically and sound an alarm when the specified
indentation has been reached (see 7.5).

4.5.1 Heating bath, containing a liquid in which the test specimen can be immersed to a depth of at least
35 mm. An efficient stirrer shall be provided. It shall be established that the liquid chosen is stable at the
temperature used and does not affect the material under test, for example by swelling or cracking.

When a heating bath is used, the temperature of the liquid, measured close to the test specimen, shall be taken
as the VST.

NOTE Liquid paraffin, transformer oil, glycerol and silicone oil are suitable liquid heat-transfer media, but other liquids may
be used.

4.5.2 Direct-contact heating unit, containing heaters and blocks which, through conductive heating, raise the
temperature of the specimen at a controlled rate until the VST is reached.

4.6 Temperature-measuring instrument

4.6.1 For a heating bath

Use a mercury-in-glass thermometer of the partial-immersion type, or another suitable temperature-measuring

instrument, of appropriate range and accurate to within 0,5 ° C. Mercury-in-glass thermometers shall be
calibrated at the depth of immersion required by 7.2. For mechanical and thermal reasons, the temperature-
measuring instrument shall not make direct contact with the specimen.

4.6.2 For a direct-contact heating unit

Use a suitable temperature-measuring instrument of appropriate range and accurate to within 0,5 ° C. The
sensor shall be positioned as close as possible to both the indenting tip and the specimen, but avoiding direct
contact between the sensor and specimen.

5 Test specimens

5.1 At least two test specimens shall be used to test each sample. The test specimens shall be between 3 mm
and 6,5 mm thick and at least 10 mm square or of 10 mm diameter. Their surfaces shall be flat and parallel and
free from flash. They shall be made in accordance with the specifications, if any, for the material under test. In
the absence of such specifications, any suitable procedure may be used for the preparation of test specimens
as agreed upon by the interested parties.

5.2 If the samples submitted for test are in the form of moulding materials (for example, powder or granulated
materials), these shall be moulded into specimens 3 mm to 6,5 mm thick, in accordance with the specifications
relating to the material under test, or in accordance with ISO 293, ISO 294-1, ISO 294-2, ISO 294-3 or
ISO 3167 if no material specification exists. If these are not applicable, other procedures maybe used as agreed
between the interested parties.

5.3 For sheet materials, the thickness of the test specimens shall be equal to the thickness of the sheet,
except as follows:
a) If the thickness exceeds 6,5 mm, the test specimens shall be reduced in thickness to 3 mm to 6,5 mm by
machining one surface (see ISO 2818), the other surface being left intact. The test surface shall be the
intact one.
b) If the thickness of the sheet is less than 3 mm, not more than three pieces shall be stacked together in direct
contact to give a total thickness between 3 mm and 6,5 mm and the thickness of the upper (measured)
piece shall be at least 1,5 mm. Stacking of pieces of lesser thickness does not always give the same test
result.

5.4 The test results obtained may depend on the moulding conditions used in the preparation of the test
specimens, although such a dependence is not common. When testing materials for which the results do
Page 8
EN ISO 306 : 2004

depend on the moulding conditions, special annealing or preconditioning procedures may be used before
testing provided they are agreed to by the interested parties.

6 Conditioning

Condition in accordance with ISO 291 or with the appropriate material specification.

7 Procedure
7.1 If using a heating bath (4.5.1), mount the test specimen horizontally under the indenting tip (4.2) of the
unloaded rod (4.1), perpendicular to the indenting tip. If using a direct-contact heating unit (4.5.2), place the test
specimen horizontally and perpendicular to the direction of travel of the indenting tip, without placing the
indenting tip on the specimen.

The indenting tip shall at no point be nearer than 3 mm to the edge of the test specimen. The surface, of the test
specimen in contact with the base of the apparatus shall be flat.

7.2 If using a heating bath, place the rod/frame assembly in the bath. If using a direct-contact heating unit,
position the specimen between the two blocks and lower the indenting tip on to the specimen. The temperature
of the heating equipment shall be a maximum of 25 °C at the start of each test, unless previous tests have
shown that, for the material under test, no error is caused by starting at another temperature. When a heating
bath is used, the bulb of the thermometer or the sensor of the temperature-measuring instrument (see 4.6.1)
shall be at the same level as, and as close as possible to, the test specimen. If using a direct-contact heating
unit, the sensor shall be positioned in the heating block, as close as possible to the specimen as specified in
4.6.2.

7.3 With the indenting tip still in position, add a sufficient weight to the weight-carrying plate (4.4) (or load the
indenting tip in another suitable way), so that the total thrust on the test specimen will be 10 N ± 0,2 N for
methods A50 and Al20 and 50 N ± 1 N for methods B50 and B120. After 5 min with the load applied, note the
reading of the indentation-measuring instrument) (see 4.3) or set the instrument to zero.

7.4 Increase the temperature at a uniform rate of 50 ° C/h ± 5 ° C/h or 120 ° C/h + 10 ° C/h. When a heating
bath is used, stir the liquid well during the test. For referee tests, a rate of 50 ° C/h shall be used.

NOTE For some materials tested at the higher heating rate (120 ° C/h), Vicat softening temperatures can be observed
which are up to 10 ° C higher than those obtained when testing at 50 ° C/h.

7.5 Note the temperature of the bath (see 4.6.1) or the heating block (see 4.6.2) when the indenting tip has
penetrated into the test specimen by 1 mm ± 0,01 mm from its starting position as defined in 7.3, and record it
as the VST of the test specimen.

7.6 Express the VST of the material under test as the arithmetic mean of the VSTs of the specimens tested,
unless the range of individual results exceeds 2 ° C. If the range is greater than 2 ° C, record the individual
results [see Clause 9, item h)] and repeat the test a second time using an additional set of at least two
specimens (see 5.1). In the event of repeat testing, report the individual values from both the first and second
tests. Report the VST to three significant figures.

8 Repeatability

See Annex B.

9 Test report
The test report shall include the following information:
a) a reference to this International Standard;
b) full identification of the material tested;
 Page 9
EN ISO 306: 2004

c) the method employed (A50, Al20, B50 or B120);

d) the thickness and the number of layers of composite test specimens (i.e. specimens consisting of more than
one layer) if these are used;
e) the method of preparation of the test specimens used;
f) the method used to heat the specimens;
g) the conditioning and annealing procedures used, if any;
h) the mean Vicat softening temperature (VST) of the material, in degrees Celsius, unless the range of the first
set of results exceeds 2 ° C in which case all the individual results shall be reported;
i) any unusual characteristics of the test specimens noted during the test or after removal from the apparatus;
j) the date of the test.

Annex A
(informative)

Comparison of VST results obtained with heating bath and

direct-contact heating unit

A study was conducted to determine the VST of 10 materials measured using a heating bath containing silicone
oil and a direct-contact heating technique in which heat was transmitted to the specimens by direct contact with
metal surfaces. The results are shown in Table A.1 and Figure A.1, all values falling within a scatter band of
± 2 %. The slope of the regression curve is 1,008, suggesting that the difference in VST between the two
heating techniques is less than 1 %. Hence, for practical purposes the two techniques can be considered to give
identical values.

Table A.1 - Results of comparative study (heating rate 50 °C/h)

VST using heating bath VST using direct-contact heating
Test material Type of material
10 N load 50 N load 10 N load 50 N load
PE 4261 A Polyethylene 125,6 ° C - 125,9 ° C -
PE Sample 1 Polyethylene 91,4 ° C - 91,7 ° C -
PE Sample 2 Polyethylene 97,4 ° C - 97,7 ° C -
Terluran GP-22 ABS 105,8 ° C 99,6 ° C 105,0 ° C 98,5 ° C
Terluran GP-35 ABS 103,7 ° C 96,4 ° C 102,3 ° C 96,2 ° C
Terluran H1-10 ABS 104,9 ° C 98,5 ° C 105,1 ° C 97,0 ° C
Terluran EGP-7 ABS 108,2 ° C 100,1 ° C 107,1 ° C 100,5 ° C
Terluran HH-112 ABS 119,3 ° C 111,8 ° C 119,7 ° C 110,3 ° C
Terluran 967K ABS 103,0 ° C 94,9 ° C 102,8 ° C 93,5 ° C
PS 143 E Polystyrene - 84,0 ° C - 83,7 ° C
Page 10
EN ISO 306: 2004

0 ISO 306/A
A ISO 306/B
— y x
--- -2%
-- +2%

90

80
80 90 100 110 120 130
X
Key
X VST using heating bath, ° C
Y VST using direct-contact heater, ° C
Linear regression:
y = — 1,291 23 + 1,007 94x
R2 = 0,994 65

Figure A.1 — Plot of data presented in Table A.1

 Page 11
EN ISO 306 : 2004

Annex B
(informative)

Repeatability

The data given in Table B.1 are based on a repeatability study, using method Al20, involving one laboratory
testing four materials. Three replicates were tested at two different times.

Table B.1 — Results of repeatability study

Material Average sra rb

PC 154,50 0,71 1,98
ABS 108,40 0,14 0,40
PP 145,60 0,21 0,59
PMMA 125,10 0,07 0,20
a sr = within-laboratory standard deviation
b r = 2,83s,

r is the interval representing the critical difference (95 % confidence level) between two test results for the same
material obtained by the same operator using the same equipment in the same laboratory.

This explanation of r is only intended to present a meaningful way of considering the approximate repeatability
of the test method. The data in Table B.1 should not be rigorously applied to acceptance or rejection of material,
as they are specific to the study and may not be representative of other lots, conditions, materials or
laboratories.