BRITISH STANDARD BS EN ISO

176:2005
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Plastics —
Determination of loss of
plasticizers —
Activated carbon
method

The European Standard EN ISO 176:2005 has the status of a

British Standard

ICS 83.080.01

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 BS EN ISO 176:2005
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National foreword
This British Standard is the official English language version of EN ISO 176:2005. It is
identical with ISO 176:2005. It supersedes BS EN ISO 176:2000 which is withdrawn.
The UK participation in its preparation was entrusted to Technical Committee PRI/21,
Testing of plastics, which has the responsibility to:

— aid enquirers to understand the text;

— present to the responsible international/European committee any enquiries
on the interpretation, or proposals for change, and keep the UK interests
informed;
— monitor related international and European developments and promulgate
them in the UK.

A list of organizations represented on this committee can be obtained on request to its

secretary.
Additional information
When a container specified in 3.4 is to be placed in a liquid bath the ingress of liquid
may be prevented by fixing one end of a short length of tubing into the hole in the lid so
that the free end of the tubing is above the surface of the liquid when the container is
immersed.
The grain size of the activated carbon referred to in 3.6 is not critical provided that all
dust which tends to adhere to the sample is eliminated. A suitable carbon is activated
charcoal for chromatographic purposes, grain size 1.4 mm to 2.8 mm. The carbon is
sieved through a sieve of nominal mesh size 1.4 mm complying with the requirements
of BS 410, Test sieves, and the residue remaining on the sieve is retained for use.
Warning note
This British Standard method which is identical with EN ISO 176 does not necessarily
detail all the precautions necessary to meet the requirements of the Health and Safety
at Work etc. Act 1974. Attention should be paid to any necessary safety precautions, and
the method should only be operated by trained personnel.
Cross-references
The British Standards which implement international or European publications
referred to in this document may be found in the BSI Catalogue under the section
entitled “International Standards Correspondence Index”, or by using the “Search”
facility of the BSI Electronic Catalogue or of British Standards Online.
This publication does not purport to include all the necessary provisions of a contract.
Users are responsible for its correct application.
Compliance with a British Standard does not of itself confer immunity from
legal obligations.

This British Standard, was Summary of pages

published under the authority
of the Standards Policy and This document comprises a front cover, an inside front cover, the EN ISO title
Strategy Committee on page, the EN ISO foreword page, the ISO title page, pages ii and iii, a blank
17 February 2005 page, pages 1 to 4, an inside back cover and a back cover.
The BSI copyright notice displayed in this document indicates when the
document was last issued.

Amendments issued since publication

Amd. No. Date Comments

© BSI 17 February 2005

ISBN 0 580 45488 6

 EUROPEAN STANDARD EN ISO 176
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NORME EUROPÉENNE
EUROPÄISCHE NORM February 2005

ICS 83.080.01 Supersedes EN ISO 176:1999

English version

Plastics - Determination of loss of plasticizers - Activated carbon

method (ISO 176:2005)

Matières plastiques - Détermination des pertes en Kunststoffe - Bestimmung der Weichmacherabgabe -

plastifiants - Méthode au charbon actif (ISO 176:2005) Aktivkohleverfahren (ISO 176:2005)

This European Standard was approved by CEN on 4 November 2004.

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 Central Secretariat 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 Central Secretariat has the same status as the official
versions.

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

EUROPEAN COMMITTEE FOR STANDARDIZATION

COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG

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

© 2005 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 176:2005: E
worldwide for CEN national Members.
 EN ISO 176:2005
I NESO 71:6002( 5E)
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Foreword

This document (EN ISO 176:2005) has been prepared by Technical Committee ISO/TC 61
"Plastics" in collaboration with Technical Committee CEN/TC 249 "Plastics", the secretariat of
which is held by IBN.

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 August 2005, and conflicting national
standards shall be withdrawn at the latest by August 2005.

This document supersedes EN ISO 176:1999.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of

the following countries are bound to implement this European Standard: Austria, Belgium,
Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary,
Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

Endorsement notice

The text of ISO 176:2005 has been approved by CEN as EN ISO 176:2005 without any
modifications.

2
 EN ISO 176:2005
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INTERNATIONAL ISO
STANDARD 176

Second edition
2005-02-01

Plastics — Determination of loss of

plasticizers — Activated carbon method
Matières plastiques — Détermination des pertes en plastifiants —
Méthode au charbon actif

Reference number
ISO 176:2005(E)

© OSI 5002
 EN ISO O5002(E)
IS:671 176:2005
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 EN ISOO5002(E)
IS:671 176:2005
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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. 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 liaison 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 2.

The main task of technical committees is to prepare International Standards. 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 document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.

ISO 176 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 6, Ageing, chemical
and environmental resistance.

This second edition cancels and replaces the first edition (ISO 176:1976), Clause 8 of which is now Clause 9
and a new Clause 8 has been added.

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5002:671 OSI NE

blank
 EN ISO 176:2005
INTENRATIONAL TSANDADR IS:671 O5002(E)
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Plastics — Determination of loss of plasticizers — Activated

carbon method

1 Scope
This International Standard specifies two empirical methods for the quantitative determination of the loss of
mass from a plastic material under defined conditions of time and temperature, in the presence of activated
carbon.

These methods are used, in particular, for the quantitative determination of the loss on heating of plasticizers
from plasticized plastic materials, in which case it is generally assumed that no significant amounts of other
volatile materials are present.

These are empirical test methods, suitable only for a rather rapid comparison of the losses of plasticizers or, in
general, of volatile compounds, from different plastics.

They may also be employed for the comparison of different types of plasticizers; in this case, standard
compounds should be prepared, on the basis of a well characterized resin, with known ratios of resin to
plasticizer.

NOTE These comparisons are possible only if the test specimens are of the same thickness. If it can be assumed
that, after reconditioning, the moisture content of the exposed specimens is equal to that obtaining after the original
conditioning, the effect of moisture may be ignored.

Two methods are specified:

 Method A: The test specimens are in direct contact with the carbon; this method is particularly useful
for materials that have to be tested at relatively low temperatures because they flow at
higher temperatures.

 Method B: The test specimens are placed in wire cages that prevent direct contact between the test
specimens and the carbon.

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

3 Apparatus and materials

3.1 Analytical balance, accurate to 0,000 1 g.

3.2 Micrometer, accurate to 0,01 mm.

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3.3 Thermostatic bath or oven, capable of maintaining the temperature to within ± 1 °C of the test
temperature, in the range of 50 °C to 150 °C.

3.4 Containers, metal cans, of cylindrical form, about 100 mm in diameter and 120 mm in height, provided
with a non-air-tight cover; a lid with a small vent hole of 3 mm diameter may be suitable.

3.5 Wire cages, constructed from bronze gauze having apertures of approximately 500 µm with a diameter
of 60 mm and a height of 6 mm, formed by soldering a strip of the gauze a right angles to the periphery of a
disk of the gauze, with a similar but slightly larger cylinder acting as a lid.

3.6 Activated carbon, with a grain-size of about 4 mm to 6 mm, free from powder.

The carbon shall be of a well determined type and grade, in order to obtain concordant results.1)

Before use, the carbon should be sieved and dried to constant mass at 70 °C, preferably under vacuum and
then stored in an air-tight container. Use fresh material for each test.

4 Test specimens

The test specimens shall be in the form of disks 50 mm ± 1 mm in diameter and 1 mm ± 0,1 mm in thickness,
cut from a compression-moulded sheet of the appropriate thickness. Refer to the provisions of ISO 293.

If the test is carried out for the determination of the characteristics of specific plasticizers, standard
compounds of a given composition, as agreed between vendor and purchaser, shall be used.

At least three test specimens shall be tested for each material.

NOTE For special purposes, the use of specimens of different shape and thickness might be necessary. However, a
comparison of the values obtained is possible only for specimens of the same thickness.

Coated fabrics and other supported plastics films may be tested by this method using specimens cut directly
from the sample as received.

5 Conditioning
Unless otherwise specified, test specimens shall be conditioned in one of the atmospheres specified in
ISO 291.

6 Procedure

6.1 Method A — Test specimen in direct contact with activated carbon

6.1.1 After conditioning, weigh each test specimen to the nearest 0,001 g and determine its mean thickness
to the nearest 0,01 mm.

6.1.2 Place one specimen on the bottom of a metal container (3.4) and spread about 120 cm3 of activated
carbon (3.6) over this specimen. Place two additional specimens in the container, each covered by 120 cm3 of
carbon. Finally, put the lid on the container.

6.1.3 Only test specimens of the same composition shall be placed in one container, in order to avoid the
possibility of plasticizers or other volatile components migrating from one specimen to another.

1) Suitable brands of activated carbon are available commercially. Detailed information may be obtained from the
Secretariat of ISO/TC 61 or from the ISO Central Secretariat.

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6.1.4 Place the container in the oven or thermostatic bath controlled at a temperature of 70 °C ± 1 °C.

6.1.5 After 24 h, remove the container from the oven or bath and allow it to cool at room temperature.
Remove the specimens from the container, carefully brush them free from any trace of carbon particles and
recondition under the same conditions as those to which they were subjected before the original weighing.

6.1.6 Reweigh each specimen to the nearest 0,001 g.

6.2 Method B — Test specimens in wire cages

The procedure is similar to that used in method A, with the differences (1) that each test specimen is put into a
small metal wire-mesh cage (3.5), thus avoiding direct contact between the plastic and the carbon, and (2)
that the test temperature is 100 °C ± 1 °C.

After 24 h, remove the specimens from the container, recondition and reweigh (as specified in 6.1.5 and 6.1.6)

For different materials, different temperatures and durations of test may be agreed between the interested
parties, maintaining the same test procedures.

7 Expression of results

The change in mass, ∆m, expressed as a percentage is given by Equation (1):

m 0 − m1
∆m = × 100 (1)
m0

where

m0 is the mass, in grams, of the test specimen after conditioning;

m1 is the mass, in grams, of the test specimen after treatment in the oven or thermostatic bath and
reconditioning.

Record the arithmetic mean of the values obtained from the three test specimens as the loss of plasticizers
from the material under test.

8 Precision
Precision data are shown in Table 1.

Table 1 — Precision data for three different plasticizer materials tested according to method A

Plasticizer Volatility Average Within- Between Repeatability limit Reproducibility

material loss in laboratory laboratory within a single limit between
24 h standard standard laboratory laboratories
deviation of the deviation of the
(%) average average

1 high 19,46 0,70 2,43 1,98 6,88

2 medium 3,83 0,35 0,87 0,98 2,48
3 low 0,81 0,12 0,42 0,35 1,20
NOTE This precision statement is based on tests of three materials conducted by five different laboratories. All samples were
prepared by one source, but individual specimens were prepared by the laboratory that tested them. Each test result was the average of
23 individual determinations.

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For tests conducted in a single laboratory using the same equipment on the same day, two test specimens
should be judged as not equivalent if they differ by more than the repeatability limit within a single laboratory.

For tests conducted by different operators using different equipment on different days, two test results should
be judged as not equivalent if they differ by more than the reproducibility limit between laboratories.

Any judgement made according to these criteria would have 95 % probability of being correct.

9 Test report
The report shall include the following information:

a) reference to this International Standard;

b) complete identification of the sample and the procedure used for preparing the specimens;

c) thickness of each test specimen, to the nearest 0,01 mm;

d) conditioning procedure used;

e) test temperature, duration of the test and the method employed (i.e. method A or method B);

f) mass, in grams, of each test specimen before the test and the gain or loss in mass, in milligrams, during
the test;

g) mass change, expressed as a percentage of the original mass, of each test specimen (see Clause 7);

h) arithmetic mean of the values obtained from three test specimens;

i) observations on any change in appearance of the test specimens;

j) date of test.

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 BS EN ISO
176:2005
BSI — British Standards Institution
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