BS EN ISO 4946:2016

BSI Standards Publication

Steel and cast iron —

Determination of copper—
2,2'-Biquinoline
spectrophotometric method
BS EN ISO 4946:2016 BRITISH STANDARD

National foreword
This British Standard is the UK implementation of EN ISO 4946:2016.
It supersedes BS 6200-3.12.2:1985 which is withdrawn.
The UK participation in its preparation was entrusted to Technical
Committee ISE/102, Methods of Chemical Analysis for Iron and Steel.
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.
© The British Standards Institution 2016.
Published by BSI Standards Limited 2016
ISBN 978 0 580 81538 6
ICS 77.080.01
Compliance with a British Standard cannot confer immunity from
legal obligations.
This British Standard was published under the authority of the
Standards Policy and Strategy Committee on 31 March 2016.
Amendments/corrigenda issued since publication
Date Text affected
EUROPEAN STANDARD EN ISO 4946
NORME EUROPÉENNE
EUROPÄISCHE NORM March 2016

ICS 77.080.01 Supersedes EN 24946:1990

English Version

Steel and cast iron - Determination of copper - 2,2'-

Biquinoline spectrophotometric method (ISO 4946:2016)
Aciers et fontes - Détermination du cuivre - Méthode Stahl und Gusseisen - Bestimmung des Kupferanteils -
spectrophotométrique au 2,2'-biquinolyle (ISO Spektrophotometrisches Verfahren mit 2,2'-
4946:2016) Biquinoline (ISO 4946:2016)

This European Standard was approved by CEN on 21 November 2015.

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

COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2016 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 4946:2016 E
worldwide for CEN national Members.
BS EN ISO 4946:2016
EN ISO 4946:2016 (E)

European foreword

This document (EN ISO 4946:2016) has been prepared by Technical Committee ISO/TC 17 “Steel” in
collaboration with Technical Committee ECISS/TC 102 “Methods of chemical analysis for iron and steel”
the secretariat of which is held by SIS.

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 2016, and conflicting national standards
shall be withdrawn at the latest by September 2016.

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.

This document supersedes EN 24946:1990.

This document has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association.

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 4946:2016 has been approved by CEN as EN ISO 4946:2016 without any modification.

3
 BS EN ISO 4946:2016
ISO 4946:2016(E)


Contents Page

Foreword......................................................................................................................................................................................................................................... iv
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Principle......................................................................................................................................................................................................................... 1
4 Reagents......................................................................................................................................................................................................................... 1
5 Apparatus...................................................................................................................................................................................................................... 2
6 Sampling......................................................................................................................................................................................................................... 2
7 Procedure..................................................................................................................................................................................................................... 3
7.1 Test portion................................................................................................................................................................................................. 3
7.2 Blank test...................................................................................................................................................................................................... 3
7.3 Determination.......................................................................................................................................................................................... 3
7.3.1 Preparation of the test solution........................................................................................................................... 3
7.3.2 Colour development....................................................................................................................................................... 3
7.3.3 Preparation of the compensating solution................................................................................................. 4
7.3.4 Spectrophotometric measurement................................................................................................................... 4
7.4 Establishment of the calibration graph.............................................................................................................................. 4
7.4.1 Preparation of the calibration solutions....................................................................................................... 4
7.4.2 Spectrophotometric measurement................................................................................................................... 4
7.4.3 Calibration graph.............................................................................................................................................................. 4
8 Expression of results......................................................................................................................................................................................... 5
9 Precision........................................................................................................................................................................................................................ 5
9.1 General ........................................................................................................................................................................................................... 5
9.2 Repeatability ............................................................................................................................................................................................. 6
9.3 Reproducibility ....................................................................................................................................................................................... 6
10 Test report.................................................................................................................................................................................................................... 6
Annex A (informative) Additional information on the international interlaboratory test......................... 7
Annex B (informative) Graphical representation of precision data..................................................................................... 8
Bibliography................................................................................................................................................................................................................................. 9

© ISO 2016 – All rights reserved  iii

BS EN ISO 4946:2016
ISO 4946:2016(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. 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.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1.  In particular the different approval criteria needed for the
different types of ISO documents should be noted.  This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
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.  Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical
Barriers to Trade (TBT) see the following URL:  Foreword - Supplementary information.
The committee responsible for this document is ISO/TC 17, Steel, Subcommittee SC 1, Methods of
determination of chemical composition.
This second edition cancels and replaces the first edition (ISO 4946:1984), which has been technically
revised to include the following changes:
— correction of the specification of plotting the calibration graphs in 7.4.3;
— editorial revision of some items in accordance with the updated ISO/IEC Directives, Part 2.

iv  © ISO 2016 – All rights reserved

 BS EN ISO 4946:2016
INTERNATIONAL STANDARD ISO 4946:2016(E)

Steel and cast iron — Determination of copper —

2,2’-Biquinoline spectrophotometric method

1 Scope
This International Standard specifies a spectrophotometric method for the determination of copper in
steel and cast iron by 2,2’-biquinoline.
The method is applicable to the determination of copper mass fraction in the range of 0,02 % and 5 %.

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.
ISO 648, Laboratory glassware — Single-volume pipettes
ISO 1042, Laboratory glassware — One-mark volumetric flasks
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 14284, Steel and iron — Sampling and preparation of samples for the determination of chemical
composition

3 Principle
Dissolution of a test portion in appropriate acids.
Fuming with perchloric acid to remove hydrochloric and nitric acids and dehydrate silicic acid.
Reduction of copper(II) to copper(I) in hydrochloric acid solution by means of ascorbic acid. Formation
of a coloured compound of copper(I) with 2,2’-biquinoline.
Spectrophotometric measurement at a wavelength of about 545 nm.

4 Reagents
During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only
grade 2 water as specified in ISO 3696.

4.1 High-purity iron, containing copper 0,001 % (mass fraction) or less.

4.2 Hydrochloric acid, ρ approximately 1,19 g/ml.

4.3 Nitric acid, ρ approximately 1,40 g/ml.

4.4 Perchloric acid, ρ approximately 1,54 g/ml.

WARNING — Perchloric acid vapour might cause explosions in the presence of ammonia, nitrous
fumes or organic material in general.

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ISO 4946:2016(E)


Perchloric acid, ρ approximately 1,67 g/ml, may also be used. 100 ml of perchloric acid, ρ approximately
1,54 g/ml is equivalent to 79 ml of perchloric acid, ρ approximately 1,67 g/ml.

4.5 Perchloric acid, ρ approximately 1,54 g/ml, diluted 1 + 7.

4.6 Dimethylformamide (N,N-dimethylformamide), ρ approximately 0,944 g/ml.

WARNING — Dimethylformamide is a hazardous substance and can cause birth defects. It should
be handled with safety gloves in a fume hood.

4.7 Ascorbic acid, 200 g/l solution.

Dissolve 20 g of ascorbic acid in water, dilute to 100 ml with water and mix.
Prepare this solution immediately before use.

4.8 2,2’-Biquinoline solution.

Dissolve 0,60 g of 2,2’-biquinoline (cuproine, 2,2’-diquinolyl) in dimethylformamide (4.6), dilute to 1 l

with the same dimethylformamide and mix.
Keep this solution in a dark-coloured glass flask and protect it from the light.

4.9 Copper standard solution, 1 g/l.

Weigh, to the nearest 0,001 g, 1,000 g of high purity copper and dissolve in the minimum of nitric acid
(4.3).
Heat to boiling to remove nitrous fumes. Cool and transfer the solution quantitatively to a 1 000 ml one-
mark volumetric flask, dilute to the mark with water and mix.
1 ml of this standard solution contains 1 mg of copper.

4.10 Copper standard solution, 0,05 g/l.

Transfer 25,0 ml of the copper standard solution (4.9) to a 500 ml one-mark volumetric flask, dilute to
the mark with water and mix.
1 ml of this standard solution contains 0,05 mg of copper.

5 Apparatus
All volumetric glassware shall be Class A, in accordance with ISO 648 and ISO 1042.
Ordinary laboratory apparatus and the following shall be used.
Spectrophotometer, suitable for measuring the absorbance of the solution at a wavelength of 545 nm
with cells of 2 cm or 4 cm optical path length.

6 Sampling
Carry out sampling in accordance with ISO 14284 or appropriate national standards for steel and cast
iron.

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 BS EN ISO 4946:2016
ISO 4946:2016(E)


7 Procedure

7.1 Test portion

Weigh, to the nearest 0,001 g, approximately 0,5 g of the test sample.

7.2 Blank test

In parallel with the determination and following the same procedure, carry out two blank tests using
the same quantities of all the reagents but using, to the nearest 0,001 g, approximately 0,5 g of pure iron
(4.1) instead of test portion.

7.3 Determination

7.3.1 Preparation of the test solution

Introduce the test portion (7.1) into a 250 ml beaker. Add 10 ml of hydrochloric acid (4.2) and 5 ml of
nitric acid (4.3). Cover the beaker with a watch-glass and heat until acids action ceases.
NOTE For samples of high chromium content, first dissolve in hydrochloric acid (4.2) and then, when all
effervescence has ceased, oxidize by adding nitric acid (4.3), drop by drop.

Add 10 ml of perchloric acid (4.4) and evaporate to fuming. Continue fuming for 3 min.
Cool, dissolve the salts with 20 ml of water, transfer the solution quantitatively to a one-mark volumetric
flask of suitable capacity (see Table 1), dilute to the mark with water and mix.
Filter by decantation through a dry filter to remove any residue or precipitate, e.g. graphite, silica,
tungstic acid. Collect the filtrate in a dry beaker, discarding the first fractions of the filtrate.

7.3.2 Colour development

Take an aliquot portion, according to the expected copper content, as indicated in Table 1.

Table 1 — Volume of test solution and aliquot portion

Volume of
Copper content Volume of test solution
aliquot portion
% (mass fraction) ml ml
0,02 to 0,3 100 10
0,3 to 0,6 100 5
0,6 to 1,5 250 5
1,5 to 5,0 500 5

Transfer the selected aliquot portion to a 50 ml one-mark volumetric flask. If the aliquot portion is 5 ml,
add 5 ml of perchloric acid (4.5).
Add, in the following order, shaking after each addition:
— 5 ml of ascorbic acid solution (4.7);
— 25 ml of 2,2’-biquinoline solution (4.8).
Dilute to the mark with water and mix. Cool for 5 min in a water-bath at about 20 °C.
Finally, readjust the volume and mix again.

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ISO 4946:2016(E)


7.3.3 Preparation of the compensating solution

Transfer an aliquot portion of the test solution (7.3.1) similar to the aliquot portion for the development
of the colour (7.3.2) to a 50  ml one-mark volumetric flask. If the aliquot portion is 5  ml, add 5  ml of
perchloric acid (4.5).
Add, in the following order, shaking after each addition:
— 5 ml of ascorbic acid solution (4.7);
— 25 ml of dimethylformamide solution (4.6).
Dilute to the mark with water and mix. Cool for 5 min in a water-bath at about 20 °C.
Finally, readjust the volume and mix again.

7.3.4 Spectrophotometric measurement

Carry out the spectrophotometric measurement of the test solution (7.3.1) at a wavelength of about
545 nm, in a cell of 2 cm optical path length, after adjusting the spectrophotometer (Clause 5) to zero
absorbance in relation to the compensating solution (7.3.3).
For copper contents below 0,06  % (mass fraction), 4  cm cells may be used if the sensitivity of the
spectrophotometer is not sufficient with 2 cm cells.

7.4 Establishment of the calibration graph

7.4.1 Preparation of the calibration solutions

Into each of a series of 100  ml beakers, add 0,5  g  ±  0,01  g of high purity iron (4.1) and 10 ml of
hydrochloric acid (4.2). Cover with a watch-glass and heat gently until dissolved, then oxidize by adding
nitric acid (4.3) drop by drop. Add the following volumes of the standard copper solution (4.10) to the
beakers, respectively: 0 ml, 2 ml, 5 ml, 10 ml, 20 ml, 30 ml, 40 ml and 50 ml.
Add 10 ml of perchloric acid (4.4) and evaporate to fumes. Continue fuming for 3 min.
Cool, dissolve the salts with 20 ml of water; transfer the solutions quantitatively to 100 ml one-mark
volumetric flasks, dilute to the mark with water and mix.
From each volumetric flask, take 10,0 ml of the solution and transfer respectively into a series of 50 ml
one-mark volumetric flasks. The zero term represents the compensating solution.
For the colour development, proceed as directed in 7.3.2, beginning at “Add, in the following order...”.
The copper concentrations in the 50 ml calibration solutions are respectively 0 μg, 0,2 μg, 0,5 μg, 1 μg,
2 μg, 3 μg, 4 μg and 5 μg of copper per millilitre.

7.4.2 Spectrophotometric measurement

Carry out the spectrophotometric measurement of absorbance of each calibration solution (7.4.1) at
a wavelength of about 545 nm, in a cell of 2 cm optical path length, using the zero term calibration
solution as the compensating solution as described in 7.3.4.

7.4.3 Calibration graph

Establish the calibration graph by plotting the net absorbance values against the copper concentrations,
expressed in micrograms per millilitre, in the calibration solutions.

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ISO 4946:2016(E)


8 Expression of results
Convert the absorbance (7.3.4) into the corresponding concentration, expressed in micrograms of
copper per millilitre, in the colour-developed test solution by using the calibration graph (7.4.3).
The copper content (CCu), expressed as a mass fraction (%), is given by Formula  (1), Formula  (2)
and Formula(3):

V0 Vt
C Cu = ( ρ Cu1 − ρ Cu 0 ) ×
1
× × × 100 (1)
10 6 V1 m

V0
C Cu = ( ρ Cu1 − ρ Cu 0 ) ×
1 50
× × × 100 (2)
10 6 V1 m

5V0
C Cu = ( ρ Cu1 − ρ Cu 0 ) × (3)
103 V1 m
where

m is the mass of the test portion (7.1), in grams;

V0 is the volume of the test solution (see Table 1), in millilitres;

V1 is the volume of the aliquot portion (see Table 1), in millilitres;

Vt is the volume of the colour-developed test solution (7.3.2), in millilitres;

ρCu0 is the concentration, of copper in the blank test solution (corrected for its compensating
solution), expressed in micrograms per millilitre;

ρCu1 is the concentration of copper in the test solution (corrected for its compensating solu-
tion), expressed in micrograms per millilitre.

9 Precision

9.1 General
A planned trial of this method was carried out by six laboratories, at five levels of copper, each laboratory
making three to five determinations at each level.
The results obtained were treated statistically in accordance with ISO 5725:1986[1].
The data obtained showed a logarithmic relationship between copper content and repeatability or
reproducibility of the test results, as summarized in Table 2. The graphic presentation of the data is
given in Annex B.

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BS EN ISO 4946:2016
ISO 4946:2016(E)


Table 2 — Repeatability and reproducibility limits

Copper content
Repeatability limit Reproducibility limit
level
r R
% (mass fraction)
0,02 0,000 5 0,003 2
0,05 0,001 3 0,006 0
0,10 0,002 4 0,009 6
0,20 0,004 6 0,015
0,50 0,011 0,029
1,00 0,021 0,046
2,00 0,040 0,073
5,00 0,093 0,137

9.2 Repeatability
The difference between two single and independent results found on identical test material by one
analyst using the same apparatus within a short time interval in the normal and correct operation of
the test method will exceed the repeatability, r, only in one case in 20 cases.

9.3 Reproducibility
The difference between two single and independent results found by two operators working in different
laboratories on identical test material in the normal and correct operation of the test method will
exceed the reproducibility, R, only in one case in 20 cases.

10 Test report
The test report shall include the following information:
a) all information necessary for the identification of the sample, the laboratory and the date of analysis
or of the test report;
b) method used with reference to this International Standard, i.e. ISO 4946;
c) results and unit in which they are expressed;
d) any unusual features noted during the determination;
e) any operation not specified in this International Standard or any optional operation which might
have influenced the results.

6  © ISO 2016 – All rights reserved

 BS EN ISO 4946:2016
ISO 4946:2016(E)


Annex A
(informative)

Additional information on the international interlaboratory test

Data given in Table 2 has been derived from the results of the international trial carried out in 1978 on
four steel samples and two cast iron samples in three countries involving six laboratories.
The results of the trial were reported in document 17/1 N 432, September 1980.
The test samples used are given in Table A.1.

Table A.1 — Test samples

Copper content
Sample % (mass fraction)
Certified Found
BCS 434 (Plain carbon steel) 0,017 0,016 9
BCS 407 (Low alloy steel) 0,43 0,434
BCS 172/3 (Alloy cast iron) 1,50 1,521
BCS 365 (Alcomax III) 2,70 2,719
BCS 173/1 (Austenitic cast iron) 5,05 5,105

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BS EN ISO 4946:2016
ISO 4946:2016(E)


Annex B
(informative)

Graphical representation of precision data

0,1

r (%)
Y 0,01 R (%)
r
R
0,001

0,000 1
0,01 0,1 1 10
X

Key
X copper content, %(mass fraction)
Y precision, %(mass fraction)
lg r =0,941 3 lg WCu – 1,679
lg R =0,680 2 lg WCu – 1,339

Figure B.1 — Relationship between copper content and repeatability (r) and reproducibility (R)

8  © ISO 2016 – All rights reserved

 BS EN ISO 4946:2016
ISO 4946:2016(E)


Bibliography

[1] ISO 5725:1986,1)Precision of test methods — Determination of repeatability and reproducibility for

a standard test method by inter-laboratory tests

1) Withdrawn. (Replaced with the ISO 5725 series.)

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