BRITISH STANDARD EN ISO

BS ISO
1628-5:2015
1628-5:1998
BS 2782-7:
2782-7:
Method
Method
732E:1998
732E:1998

Plastics —
Determination of the
viscosity of polymers in
dilute solution using
capillary viscometers —
Part 5: Thermoplastic polyester (TP)
homopolymers and copolymers

ICS 83. 080. 20

BS EN ISO 1628-5:2 0 15

National fore word

This British Standard is the UK implementation of EN ISO 1628-5:2015.
It is identical to ISO 1628-5:1998. It supersedes BS ISO 1628-5:1998, which
is withdrawn.
The UK participation in its preparation was entrusted to Technical
Committee PRI/21, Testing of plastics.
A list of organizations represented on this committee can be obtained on
request to its secretary.
This publication does not purport to include all the necessary provisions of a
contract. Users are responsible for its correct application.
C ompliance w ith a British Standard cannot confer immunity from
legal ob ligations.

This British Standard, having

been prepared under the
direction of the Sector Board
for Materials and Chemicals, Amendments/corrigenda issued since pub lication
was published under the
authority of the Standards
Board and comes into effect Date Comments
on 15 June 1998
31 March 2015 This corrigendum renumbers BS ISO 1628-5:1998 as
© The British Standards BS EN ISO 1628-5:2015
Institution 2015.
Published by BSI Standards
Limited 2015

ISBN 978 0 580 872 0 3 7

EUROPEAN STANDARD EN ISO 1 628-5
NORME EUROPÉENNE
EUROPÄISCHE NORM March 201 5

ICS 83.080.20

English Version

Plastics - Determination of the viscosity of polymers in dilute

solution using capillary viscometers - Part 5: Thermoplastic
polyester (TP) homopolymers and copolymers (ISO 1 628-
5:1 998)
Plastiques - Détermination de la viscosité des polymères en Kunststoffe - Bestimmung der Viskosität von Polymeren in
solution diluée à l'aide de viscosimètres à capillaires - verdünnter Lösung durch ein Kapillarviscosimeter - Teil 5:
Partie 5: Homopolymères et copolymères des polyesters Thermoplastische Polyester(TP) Homopolymere und
thermoplastiques (TP) (ISO 1 628-5:1 998) Copolymere (ISO 1 628-5:1 998)

This European Standard was approved by CEN on 1 March 201 5.

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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION

C O M I T É E U R O P É E N D E N O RM A L I S A T I O N
E U RO P Ä I S C H E S KO M I T E E F Ü R N O RM U N G

CEN-CENELEC Management Centre: Avenue Marnix 1 7, B-1 000 Brussels

© 201 5 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 1 628-5:201 5 E
worldwide for CEN national Members.
BS EN ISO 1628-5:2 0 15
EN ISO 1628-5:2 0 15 (E) EN ISO 1 628-5:201 5 (E)

Foreword
The text of ISO 1 628-5:1 998 has been prepared by Technical Committee ISO/TC 61 “Plastics” of the
International Organization for Standardization (ISO) and has been taken over as EN ISO 1 628-5:201 5 by
Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by NBN.
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 September 201 5, and conflicting national standards shall be
withdrawn at the latest by September 201 5.
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 organizations 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, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.

Endorsement notice
The text of ISO 1 628-5:1 998 has been approved by CEN as EN ISO 1 628-5:201 5 without any modification.

ii 3
© The British Standards Institution 2015
 BS ISO 1628-5:2015
BS EN 1628-5:1998
BS ISO 1628-5:1998
Contents
Contents
Page
National foreword Page
Inside front cover
National foreword
Foreword Inside front cover
iii
1 Scope 1
2 Normative references 1
3 Principle 1
4 Solvents 1
5 Apparatus 2
6 Solvent and solution 2
7 Procedure 3
8 Expression of results 4
9 Test report 4
Annex A (informative) Round-robin testing 5
Figure A. 1 — Viscosity number of PET in
phenol/1 , 2- dichlorobenzene (50/50) relative to that in other solvents 6
Figure A. 2 — Viscosity number of PBT in m-cresol
relative to that in other solvents 7
Table A. 1 5

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1 Scope
This part of ISO 1 628 specifies a method for the
determination of the viscosity number (also referred
to as “reduced viscosity”) of dilute solutions of
thermoplastic polyesters (TPs) in certain specified
solvents. The method is applicable to poly(ethylene
terephthalate) (PET), poly(butylene terephthalate)
(PBT), poly-(cyclohexylenedimethylene
terephthalate) (PCT), and poly(ethylene
naphthalate) (PEN), as well as to copolyesters and
other polyesters, defined in ISO 7792-1 , that are
soluble in one of the specified solvents under the
specified conditions.
The viscosity number is determined by the general
procedure specified in ISO 1 628-1 , observing the
particular conditions specified in this part of
ISO 1 628.
The determination of the viscosity number of a
thermoplastic polyester provides a measure of the
relative molecular mass of the polymer.
2 Normative references
The following standards contain provisions which,
through reference in this text, constitute provisions
of this part of ISO 1 628. At the time of publication,
the editions indicated were valid. All standards are
subj ect to revision, and parties to agreements based
on this part of ISO 1 628 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
current valid International Standards.
ISO 1 628-1 : —, P stics — Determi
la tio of the
viscosity of po ymers i di ute so utio usi g
l n l l
c pi ry viscometers — P rt 1: Ge er pri cip es .
a lla a n
ISO 31 05: 1 994, G ss c pi ry i em tic
la a lla
viscometers — Specific tio s d oper ti g a n
i structio s.
n n
ISO 3451 -2: 1 984, P stics — Determila tio of 4.5 Dichloroacetic acid, analytical grade.
ash — P rt 2: Po y y e e terephth tes.
a l alk l n
4.6 Phenol/2,4,6-trichlorophenol
ISO 7792-1 : 1 997, P stics — Thermop stic
la
po yester (TP) mou di g d extrusio m teri s — grade)
l l n
Weight out 6 parts by mass of phenol (analytical
an
P rt 1: Desig tio system d sis for
a na n an
specific tio s.a n
of 2, 4, 6-trichlorophenol (analytical grade).
1)
To be published. (Revision of ISO 1 628- 1 : 1 984)
© BSI
© The 04-1
British
999Standards Institution 2015
BS EN ISO 1628-5:2015
BS ISO 1628-5:1998
3 Principle
The times of flow of a solvent and a solution of resin
in the solvent at a concentration of 0, 005 g/ml are
measured at 25 °C by conventional methods. The
viscosity number is calculated from these
measurements and from the known concentration of
the solution. Specific gravity difference and kinetic
energy corrections are small in this method and are
not applied.
4 Solvents
WARNING — The solvents used are
hazardous. Avoid contact with the skin and
inhalation of the vapours.
4.1 Phenol/1,2-dichlorobenzene
Weigh out 1 part by mass of phenol (analytical
grade) and dissolve in 1 part by mass
of 1 , 2-dichlorobenzene (analytical grade). Work to
an accuracy of 1 % or better in the weighings.
4.2 Phenol/1,1,2,2-tetrachloroethane
Weigh out 6 parts by mass of phenol (analytical
grade) and dissolve in 4 parts by mass
of 1 , 1 , 2, 2-tetrachloroethane (analytical grade), or
weigh out 1 part by mass of phenol and dissolve in 1
part by mass of 1 , 1 , 2, 2-tetrachloroethane. Work to
an accuracy of 1 % or better in the weighings.
4.3 o- Chlorophenol, analytical grade.
4.4 m- Cresol, meeting the following specifications:
appearance: clear and colorless;
m-cresol content: 99 % (m/m) min. ;
na n o-cresol content: 0, 3 % (m/m) max. ;
n n water content: 0, 1 % (m /m ) max.
al n l
1)
NOTE A solvent of the required purity can be obtained by
k n a m distillation of chemically pure -cresol, preferably in vacuo,
an a n
pressure compensation being effected with nitrogen in order to
avoid oxidation. The purity of the solvent may be checked by gas
chromatography.
na n
ala
la
n a al
and dissolve in 4 parts by mass
ba
NOTE 2, 4, 6- trichlorophenol of the required purity can be
obtained by distillation of chemically pure 2, 4, 6-trichlorophenol.
4.7 Storage of the solvents
Protect the solvents from light by storing them, for
example, in stoppered brown- glass bottles.
11
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5 Apparatus
5.1 Mill, to reduce the sample to a grain size of
about 0, 5 mm.
5.2 Volumetric flask, of capacity 1 00 ml, fitted with
a ground- glass stopper.
5.3 Conical flask, of capacity 1 50 ml, fitted with a
ground-glass stopper.
5.4 Burette, graduated in divisions of 0, 1 ml.
o-chlorophenol, m- cresol,
5.5 Steam bath, or other means to heat the contents phenol/1 , 2-dichlorobenzene (50/50) or dichloroacetic
of a flask to 90 to 1 00 ° C.
5.6 Oil bath, capable of being controlled
at 1 35 to 1 40 ° C, or other means to heat the
contents of a flask to that temperature range.
5.7 Magnetic stirrer, or other equipment to
continuously agitate the contents of a stoppered
flask.
5.8 Thermostatic bath, capable of being maintained
at 25 ± 0, 05 ° C.
5.9 Viscometer, suspended-level Ubbelohde type,
size No. 1 B, 1 C or 2, in accordance with ISO 31 05.
Other types of viscometer listed in ISO 31 05 may be
used, provided that the results are equivalent to
those of the Ubbelohde viscometers specified above.
However, in cases of dispute, Ubbelohde
viscometers shall be used.
5.10 Stainless-steel sieve, with a nominal aperture
size of 63 to 90 4m, or sintered-glass filter funnel
with 40 to 1 00 4m pore diameter.
5.11 Analytical balance, accurate to 0,1 mg.
5.12 Stopw atch, accurate to 0,1 s.
5.13 Vacuum dryer, capable of being maintained
at about 130 ° C under vacuum.
6 Solvent and solution
6.1 Selection of the solvent
6.1.1 The value of the viscosity number of a
saturated polyester depends on the solvent used. Six
different solvents are described in this part of
ISO 1 628: phenol/1 , 2-dichlorobenzene ( 4.1 ),
4.2 ),
phenol/1 , 1 , 2, 2- tetrachloroethane (
o- chlorophenol (4.3), m-cresol (4.4 ), dichloroacetic
acid ( 4.5 ) and phenol/2, 4, 6-trichlorophenol (4.6 ).
The flow times of the solvents shall be determined at
least once each day that they are used (see 7.2 ). If
the flow time of a solvent differs by more than 1 %
from the initial value at the time of preparation, the
solvents shall be discarded and fresh solvent
prepared.
The solvent or solvents to be used for a particular
saturated polyester are specified below.
22
6.1.2 For PET, use phenol/1 , 2- dichlorobenzene
(50/50), phenol/1 , 1 , 2, 2-tetrachloroethane
(50/50 or 60/40), o-chlorophenol or dichloroacetic
acid as solvent.
NOTE Equations for the interconversion of viscosity number
determined in these four solvents are presented in Annex A,
subclause A.3.1 .
6.1.3 For PBT and corresponding copolyesters, use
phenol/1 , 1 , 2, 2-tetrachloroethane (50/50 or 60/40),
acid as solvent.
NOTE Equations for the interconversion of viscosity number
determined in these four solvents are presented in Annex A,
subclause A.3.2 .
6.1.4 For PCT, use
phenol/1 , 1 , 2, 2-tetrachloroethane (60/40) as solvent.
6.1.5 For amorphous PEN, use
phenol/1 , 1 , 2, 2-tetrachloroethane (60/40) as solvent
and for crystalline PEN use
phenol/2, 4, 6-trichlorophenol (60/40).
6.1.6 For other TP homopolymers and copolymers,
m-cresol is the recommended solvent.
6.2 Determination of inorganic materials or
other additives in the sample
Contents of inorganic materials or other additives
exceeding 0, 5 % ( m/m) each shall be taken into
account in the preparation of the test solution ( 6.4).
6.2.1 Determination of the content of inorganic
materials
If the sample contains inorganic materials, such as
fillers or glass fibres, determine the content in
accordance with ISO 3451 -2.
6.2.2 Determination of the content of other
additives
If the sample contains other additives, such as
polyalkenes or flame retardants, determine the
content in an appropriate way. Report the
procedure(s) used.
NOTE When a polyester is a compound consisting of many
components (flame retardants, fillers, antioxidants, impact
modifiers), the analysis of the polyester content is more specific.
This can be achieved by hydrolysis of the polyester and
subsequent analysis of the monomer(s).
6.3 Sample
The sample shall be representative of the material
to be tested. Predry the sample at 1 20 ° C under
vacuum for 3 h to avoid a decrease in VN by
hydrolysis with residual water.
© BSI 04-1
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6.4 Preparation of solution
Use one of the following procedures:
6.4.1 Procedure A
Weigh out, to the nearest 0, 2 mg, a test portion
in the range
0, 5
i o
---------------------------------------------
1 – [ ( + ) ⁄ 1 00 ]
± 0, 01
where
i is the content of inorganic materials, expressed
as a percentage by mass, in the sample,
determined in accordance with
o is the content of other additives, expressed as a
percentage by mass, in the sample, determined
in accordance with 6.2.2 .
The corrections for i and o need only be applied if
they exceed 0, 5 % (m /m ) each.
Transfer the test portion to the volumetric
flask ( 5.2 ), add 60 ml of solvent, stopper the flask
and warm on the steam bath ( 5.5 ), with occasional
stirring, until the polymer has dissolved completely.
On the steam bath, no degradation of the polymer
occurs. If, however, long waiting times are
undesirable for other reasons, the dissolution may
be accelerated by agitating the flask continuously,
for example with the magnetic stirrer (
Samples of highly crystalline poly(ethylene
terephthalate), such as postcondensed moulding
chips, which may have crystallinities of
around 65 %, will not dissolve on the steam bath,
not even with continuous stirring. To dissolve such
samples, grind the material in the mill ( 5.1 ) and
dissolve at a temperature of 1 35 to 1 40 ° C (5.6 ) with
continuous stirring. At 1 35 to 140 °C, some
degradation of the polymer occurs. Therefore, avoid
heating times over 30 min.
After dissolution, cool the flask and its contents
to 25 ± 2 °C, make up to 1 00 ml with solvent held at
this temperature, and mix well. If, in dissolving, a
magnetic stirrer has been used, first remove it from
the solution and rinse it with the make- up solvent,
ensuring that all the washings enter the flask. The
concentration of the polymer in the solution,
expressed in grams per millilitre, used in
calculating the viscosity number (clause
by the formula
0, 01 (1 –
i+o m )
1
1 00
NOTE Usually, the concentration will differ slightly
from 0, 005 g/ml. The effect on the viscosity number can be
neglected, however, since, over the range considered, the
viscosity relative increment may be considered to be a linear
function of the concentration.
© BSI
© The 04-1
British
999Standards Institution 2015
BS EN ISO 1628-5:2015
BS ISO 1628-5:1998
6.4.2 Procedure B
Weigh out, to the nearest 0, 2 mg, a test portion m 2
in the range 0, 4 to 0, 6 g.
m Transfer the test portion to the conical flask ( 5.3 ).
1
Add by burette ( 5.4 ), to the nearest 0, 1 ml, a volume
of solvent, in millilitres, equal to
i+o m
grams
200 (1 – ) 2
1 00
where i and o have the same meaning as in 6.4.1 .
The corrections for i and o need only be applied if
6.2.1 they exceed 0, 5 % (m /m ) each. The solvent added
shall be at 25 ± 2 °C.
Stopper the flask. Dissolve the polymer by heating
the flask on the steam bath, or, if required, in the oil
bath, following the procedures and observing the
6.4.1 . After dissolution,
precautions mentioned in
cool the flask to room temperature.
7 Procedure
7.1 Preparatory operations
With phenol/1 , 2-dichlorobenzene,
phenol/1 , 1 , 2, 2-tetrachloroethane, o- chlorophenol
and phenol/2, 4, 6-trichlorophenol as the solvent, use
a No. 1 C viscometer. With m-cresol, use a No. 2
5.7 ). viscometer. With dichloroacetic acid, use a No. 1 B
viscometer.
Filter the test solution through the screen or
sintered- glass filter ( 5.10 ) into the viscometer. The
volume shall be such that, after draining, the level
lies between the filling marks. Carry out this filling
operation away from the thermostatic bath ( 5.8) to
prevent contamination of the bath in the case of
accidental spills.
Mount the viscometer in the thermostatic bath,
ensuring that the tube is vertical and that the upper
graduation mark is at least 30 mm below the
surface of the bath liquid. Allow at least 1 5 min for
the charged viscometer to attain the temperature of
the bath, (25 ± 0, 05 ° C).
7.2 Measurement of flow time
Determine the flow time of the solution several
times, without emptying and recharging, until two
8) is given successive flow times agree to within 0, 25 %. Take
the mean of these two flow times as the flow time of
the test solution.
Determine the mean flow time of the solvent in the
same viscometer and in the same manner as for the
test solution. It is sufficient to measure this time
once for each series of determinations. However,
measure the time at least once each day the solvent
is used. If two successive determinations of the
mean flow time differ by more than 0, 4 s, clean the
viscometer.
33
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ISO 1628-5:1998
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8 Expression of results 9 Test report

Calculate the viscosity number, expressed in The test report shall include the following
millilitres per gram, from the formula information:

t t
–
0
a) a reference to this part of ISO 1 628;

tc 0
b) all details necessary for complete identification
of the sample tested;
where
c) if the sample contains more than 0, 5 % ( m /m )
t is the flow time, in seconds, of the test solution; of other additives (see 6.2.2 ), a description of the
t is the flow time, in seconds, of the solvent;
0
procedures used for their determination;

c is the concentration of the polymer in the test d) details of the viscometer used if it differs from
solution, in grams per millilitre. the No. 1 B, 1 C or 2 Ubbelohde type as specified in
ISO 31 05;
When procedure A has been used to prepare the test
solution, calculate c as described in 6.4.1 . When e) the viscosity number obtained;
procedure B has been used, c is equal to 0, 005 g/ml. f) the date of the test.
With each polymer sample, carry out at least two
determinations of the viscosity number, each time
using a fresh solution, until two successive values
differ by no more than 3 %. Report the mean of these
two values, rounded off to the nearest whole
number, as the viscosity number of the sample.

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BS ISO 1628-5:1998

Annex A (informative)
Round-robin testing
A.1 General
Round- robin testing was carried out by nine laboratories (six Japanese, one German, one French and one
in the USA) in 1 991 -1 992 to check the interconvertibility of viscosity number of PET and PBT between
different solvents.
A.2 Repeatability and reproducibility
The repeatability and reproducibility of the determination of the viscosity number depend on the solvent
used. The values are given in Table A. 1 .
Table A.1
Solvent Repeatability Reproducibility
% %

PET PBT PET PBT

Phenol/1 , 2-dichlorobenzene (50/50) 1,2 0, 9 3, 2 1,5

Phenol/1 , 1 , 2, 2- tetrachloroethane (60/40) 1,1 0, 8 --- ---

Phenol/1 , 1 , 2, 2-tetrachloroethane (50/50) 0, 6 1,3 --- ---

o-Chlorophenol 2, 0 1,5 2,0 3, 4

m-Cresol --- 1,2 --- 3, 4

Dichloroacetic acid 1,0 1,8 7,3 5, 4

A.3 Interconversion of the viscosity numbers determined in different solvents

The relationship between the viscosity numbers determined in different solvents was determined to be as
follows:
A.3.1 Viscosity number of PET
Graphs of the relationships between the viscosity number of PET in phenol/1 , 2- dichlorobenzene (50/50)
and in phenol/1 , 1 , 2, 2- tetrachloroethane (50/50, 60/40), o-chlorophenol and dichloroacetic acid are
presented in Figure A. 1 .
From Figure A. 1 , linear relationships are obtained, described by the following equations:
a) phenol/1 , 2- dichlorobenzene (50/50) and phenol/1 , 1 , 2, 2- tetrachloroethane (50/50)
y = 1 , 07x – 2, 00
b) phenol/1 , 2- dichlorobenzene (50/50) and phenol/1 , 1 , 2, 2- tetrachloroethane (60/40)
y = 0, 83x + 1 1 , 07
c) phenol/1 , 2-dichlorobenzene (50/50) and o-chlorophenol
y = 0, 82 x + 8, 40
d) phenol/1 , 2-dichlorobenzene (50/50) and dichloroacetic acid
y = 0, 83x + 1 5, 00
where y is the viscosity number in the alternative solvent and x is that in
phenol/1 , 2-dichlorobenzene (50/50).
A.3.2 Viscosity number of PBT
Graphs of the relationships between the viscosity number of PBT in m- cresol and in
phenol/1 , 1 , 2, 2- tetrachloroethane (50/50, 60/40), o-chlorophenol and dichloroacetic acid are presented in
Figure A. 2.
From Figure A. 2 [for the solvents in a), c) and d)] and from data not shown in Figure A. 2 [for the solvents
in b) and e)] , the following equations are obtained:
a) m-cresol and phenol/1 , 1 , 2, 2-tetrachloroethane (50/50)
y = 1 , 43x – 8, 00
b) m -cresol and phenol/1 , 1 , 2, 2-tetrachloroethane (60/40)

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y = 1 , 75 x – 51 , 1 3
c) m -cresol and o- chlorophenol
y = 1 , 1 8x – 3, 70
d) m -cresol and dichloroacetic acid
y = 1 , 43 x – 1 0, 50
e) m -cresol and phenol/1 , 2-dichlorobenzene (50/50)
y = 1 , 34x – 1 , 28
where y is the viscosity number in the alternative solvent and x is that in m -cresol.

Figure A.1 — Viscosity number of PET in phenol/1,2-dichlorobenzene (50/50) relative

to that in other solvents

66 © BSI 04-1
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BS ISO 1628-5:1998

Figure A.2 — Viscosity number of PBT in m-cresol relative to that in other solvents

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999Standards Institution 2015 77
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