BS 

EN 10136:2019

BSI Standards Publication

Steels and cast irons - Determination of

nickel content - Flame atomic absorption
spectrometric method (FAAS)
BS EN 10136:2019 BRITISH STANDARD

National foreword
This British Standard is the UK implementation of EN 10136:2019. It
supersedes BS EN 10136:1991, which is withdrawn.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 2019
Published by BSI Standards Limited 2019
ISBN 978 0 580 99841 6
ICS 77.080.01; 77.040.30
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 30 June 2019.

Amendments/corrigenda issued since publication

Date Text affected
 BS EN 10136:2019

EUROPEAN STANDARD EN 10136

NORME EUROPÉENNE
EUROPÄISCHE NORM June 2019

ICS 77.040.30 Supersedes EN 10136:1989

English Version

Steels and cast irons - Determination of nickel content -

Flame atomic absorption spectrometric method (FAAS)
Aciers et fontes - Détermination de la teneur en nickel - Stahl und Gusseisen - Bestimmung des Nickelanteils -
Méthode par spectrométrie d'absorption atomique Flammenatomabsorptionsspektrometrisches
dans la flamme (SAAF) Verfahren (FAAS)

This European Standard was approved by CEN on 22 April 2019.

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

© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 10136:2019 E
worldwide for CEN national Members.
BS EN 10136:2019
EN 10136:2019 (E)

Contents Page
European foreword....................................................................................................................................................... 3
1 Scope .................................................................................................................................................................... 4
2 Normative references .................................................................................................................................... 4
3 Terms and definitions ................................................................................................................................... 4
4 Principle ............................................................................................................................................................. 4
5 Reagents ............................................................................................................................................................. 4
6 Apparatus........................................................................................................................................................... 6
6.1 Ordinary laboratory apparatus ................................................................................................................. 6
6.2 Atomic absorption spectrometer .............................................................................................................. 6
6.2.1 General ................................................................................................................................................................ 6
6.2.2 Minimum precision ........................................................................................................................................ 6
6.2.3 Additional performance requirements ................................................................................................... 6
7 Sampling ............................................................................................................................................................. 6
8 Procedure........................................................................................................................................................... 7
8.1 Test portion ....................................................................................................................................................... 7
8.2 Blank test ........................................................................................................................................................... 7
8.3 Determination .................................................................................................................................................. 7
8.3.1 Preparation of the test solution ................................................................................................................. 7
8.3.2 Treatment of the test solution .................................................................................................................... 7
8.3.3 Preparation of the calibration solutions ................................................................................................ 8
8.3.4 Adjustment of the atomic absorption spectrometer .......................................................................... 9
8.3.5 Spectrometric measurements .................................................................................................................... 9
9 Expression of results................................................................................................................................... 10
9.1 Use of the calibration curve...................................................................................................................... 10
9.2 Use of bracketing method ......................................................................................................................... 10
10 Test report ...................................................................................................................................................... 11
Annex A (informative) Precision ........................................................................................................................... 12
Bibliography ................................................................................................................................................................. 13

2
 BS EN 10136:2019
EN 10136:2019 (E)

European foreword

This document (EN 10136:2019) has been prepared by Technical Committee CEN/TC 459 “ECISS -
European Committee for Iron and Steel Standardization” 1, the secretariat of which is held by AFNOR.

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 December 2019, and conflicting national standards
shall be withdrawn at the latest by December 2019.

Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN 10136:1989.

In comparison with EN 10136:1989, the following significant technical changes were made:

— Clause 1: lower limit of the scope changed;

— Normative references: revised;

— Clause 4: possibility for using other suitable radiation sources added;

— Clause 5: preparation of iron base solutions added;

— 8.3: details regarding the preparation of the test solution added;

— 8.3.3: calibration solutions expanded;

— 8.3.4: background correction specified;

— 8.3.5 and Clause 9: bracketing method for the spectrometric measurements added;

— Clause 10: editorially updated;

— Bibliography: added.

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.

1 Through its subcommittee SC 2 “Methods of chemical analysis for iron and steel” (secretariat: SIS)

3
BS EN 10136:2019
EN 10136:2019 (E)

1 Scope
This document specifies a flame atomic absorption spectrometric method (FAAS) for the determination
of nickel content in steels and cast irons.
The method is applicable to nickel contents between 0,004 % (weight percent) and 2,0 % (weight
percent).
The method can be adapted to lower or higher nickel contents by changing the test portion or the
dilution process, provided the criteria in 6.2.2 and 6.2.3 are still met.

2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements 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.
EN ISO 648, Laboratory glassware — Single-volume pipettes (ISO 648)

EN ISO 1042, Laboratory glassware — One-mark volumetric flasks (ISO 1042)

EN ISO 14284, Steel and iron — Sampling and preparation of samples for the determination of chemical
composition (ISO 14284)

3 Terms and definitions

No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at http://www.electropedia.org/

— ISO Online browsing platform: available at http://www.iso.org/obp

4 Principle
Dissolution of a test portion in a mixture of appropriate acids and fuming with perchloric acid.
Nebulisation of the test solution into an air/acetylene flame of an atomic absorption spectrometer.
Spectrometric measurement of the atomic absorption of the 232,0 nm or 352,5 nm spectral line emitted
by a nickel hollow-cathode lamp.
NOTE Other suitable radiation sources can also be used, provided the criteria in 6.2.2 and 6.2.3 are still met.

5 Reagents
During the analysis, use only reagents of recognized analytical grade and only distilled water or water
of equivalent purity.
The following concentrations and amounts can be modified, provided the changes are taken into
account in 8.3 and Clause 9.
5.1 Pure iron, with nickel content < 0,000 5 %.

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EN 10136:2019 (E)

5.2 Hydrochloric-nitric acids mixture.

Mix three volumes of hydrochloric acid (ρ20 = 1,19 g/ml approximately), one volume of nitric
acid (ρ20 = 1,40 g/ml approximately) and two volumes of water.
This mixture shall be prepared immediately before use.
5.3 Nitric-perchloric acids mixture.

Mix 100 ml of nitric acid (ρ20 = 1,40 g/ml approximately) with 800 ml of perchloric acid (ρ20 = 1,54 g/ml
approximately). Dilute to one litre with water and mix.
Perchloric acid (ρ20 = 1,67 g/ml approximately) may also be used. 100 ml of perchloric
acid (ρ20 = 1,54 g/ml approximately) are equivalent to 79 ml of perchloric acid (ρ20 = 1,67 g/ml
approximately).
5.4 Nickel standard solution, 1 g/l.

Weigh (0,500 ± 0,001) g of nickel (Ni ≥ 99,9 %) and transfer into a heat-resistant glassware of suitable
size. Add 25 ml of nitric acid (ρ20 = 1,40 g/ml approximately), diluted 1 + 1. Cover with a watch glass,
and, if necessary, heat gently to assist dissolution. When dissolution is complete, boil to remove
nitrogen oxides. Allow to cool to room temperature and transfer the solution quantitatively into a
500 ml one-mark volumetric flask. Dilute to the mark with water and mix.
1 ml of this solution contains 1,0 mg of nickel.
5.5 Nickel standard solution, 0,04 g/l.

Transfer 10,0 ml of nickel standard solution (5.4) into a 250 ml one-mark volumetric flask. Dilute to the
mark with water and mix.
Prepare this solution immediately prior to use.
1 ml of this solution contains 0,04 mg of nickel.
5.6 Iron base solution, 40 g/l.

Weigh, to the nearest 0,01 g, 10,00 g of pure iron (5.1) and transfer into a heat-resistant glassware of
suitable size. Add 100 ml of the hydrochloric-nitric acids mixture (5.2), cover the glassware with a
watch glass and heat gently until the iron is dissolved. Add 150 ml of the nitric-perchloric acids mixture
(5.3) and heat until dense white fumes of perchloric acid appear. Continue heating for one minute and
allow to cool.
In order to get a better mastery of the acidity (volume of free perchloric acid) of the sample solutions
and of the calibration solutions, perchloric fumes may be maintained until iron crystallizes.
Add 100 ml of water and heat gently to dissolve the salts. Cool again and transfer the solution
quantitatively into a 250 ml one-mark volumetric flask. Dilute to the mark with water and mix.
5.7 Iron base solution, 2 g/l.

Transfer 10,0 ml of iron base solution (5.6) into a 200 ml one-mark volumetric flask. Dilute to the mark
with water and mix.

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BS EN 10136:2019
EN 10136:2019 (E)

6 Apparatus
6.1 Ordinary laboratory apparatus

All volumetric glassware shall be class A, in accordance with EN ISO 648 or EN ISO 1042, as
appropriate.
6.2 Atomic absorption spectrometer
6.2.1 General

The spectrometer shall be equipped with a nickel hollow-cathode lamp or other suitable radiation
source and supplied with air and acetylene sufficiently pure to give a steady clear fuel-lean flame, free
from water and oil, and free from nickel.
The atomic absorption spectrometer used will be satisfactory if, after optimization according to 8.3.4,
the limit of detection and characteristic concentration are in reasonable agreement with the values
given by the manufacturer and it meets the performance criteria given in 6.2.2 and 6.2.3.
6.2.2 Minimum precision

The standard deviation of 10 measurements of the absorbance of the most concentrated calibration
solution shall not exceed 1,0 % of the mean absorbance of this solution.
The standard deviation of 10 measurements of the absorbance of the least concentrated calibration
solution (excluding the zero member) shall not exceed 0,5 % of the mean absorbance of the most
concentrated calibration solution.
6.2.3 Additional performance requirements

6.2.3.1 General

The instrument should also conform to the additional performance requirements given in 6.2.3.2 and
6.2.3.3.
6.2.3.2 Characteristic concentration

The characteristic concentration for nickel in a matrix similar to the final test solution shall be lower
than 0,40 µg/ml.
6.2.3.3 Limit of detection

The limit of detection is a number, expressed in units of concentration (or amount) that describes the
lowest concentration level (or amount) of an element that can be determined to be statistically different
from an analytical blank.
The limit of detection of nickel in a matrix similar to the final test solution shall be less than 0,15 µg/ml.

7 Sampling
Carry out sampling in accordance with EN ISO 14284 or appropriate national standards for steels and
cast irons.

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 BS EN 10136:2019
EN 10136:2019 (E)

8 Procedure
WARNING — Perchloric acid vapour may cause explosions in the presence of ammonia, nitrous fumes
or organic matter in general. All evaporations shall be carried out in fume cupboards suitable for use
with perchloric acid.

NOTE The following concentrations, amounts and glassware volumes can be modified, provided the changes
are taken into account in all appropriate subclauses of Clauses 8 and 9.

8.1 Test portion

Weigh to the nearest 1 mg, approximately 1,0 g of the test sample.

8.2 Blank test

In parallel with the determination and following the same procedure, carry out a blank test using the
same quantities of all reagents as used for the determination.
8.3 Determination
8.3.1 Preparation of the test solution

Transfer the test portion (8.1) into a 250 ml beaker. Add 10 ml of hydrochloric-nitric acids
mixture (5.2), cover the beaker with a watch glass and heat gently until the acid action ceases.
NOTE If the test portion is readily soluble in the nitric-perchloric acids mixture (5.3), the addition of the
hydrochloric-nitric acids mixture (5.2) can be omitted. In that case, the test portion is dissolved in the nitric-
perchloric acids mixture (5.3) and the solution thus obtained is heated as described below.

Add 15 ml of nitric-perchloric acids mixture (5.3) and heat until dense white fumes of perchloric acid
appear. Continue heating for one minute and allow to cool.
In order to ensure that the acid concentration in the sample solutions and in the calibration solutions is
the same, the solution should be fumed until crystallisation occurs.
8.3.2 Treatment of the test solution

8.3.2.1 Nickel contents up to 0,10 %

Add 25 ml of water and heat gently to dissolve the salts. Cool again and transfer the test solution
quantitatively into a 100 ml one-mark volumetric flask.
Dilute to the mark with water and mix.
If some residue has been left in the solution due to silicon, tungsten, niobium or tantalum, filter the
solution through a dry, medium-texture filter paper and collect the filtrate in a dry beaker, after
discarding the first portions.
8.3.2.2 Nickel contents between 0,08 % and 2,0 %

Transfer 10,0 ml of the filtrate (8.3.2.1) into a 200 ml one-mark volumetric flask, dilute to the mark with
water and mix.
If the test solution has to be diluted, the blank test solution shall be diluted in the same way.

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BS EN 10136:2019
EN 10136:2019 (E)

8.3.3 Preparation of the calibration solutions

8.3.3.1 General

Table 1 and Table 2 contain typical sets of calibration solutions. The range of concentrations in a set of
solutions may be changed in order to better bracket the expected sample solution concentration.
8.3.3.2 Nickel contents up to 0,10 %

Into each of a series of 100 ml one-mark volumetric flasks, introduce the volumes of nickel standard
solution (5.5) shown in Table 1 and 25 ml of the iron base solution (5.6). Dilute to the mark with water
and mix.
Table 1 — Calibration for nickel contents up to 0,1 %
Nickel standard Corresponding Corresponding nickel Corresponding
solution volume (5.5) nickel mass concentration after nickel content in the
final dilution sample
ml mg mg/ml %
0 0 0 0
1,0 0,04 0,000 4 0,004
2,0 0,08 0,000 8 0,008
2,5 0,10 0,001 0,010
5,0 0,20 0,002 0,020
10,0 0,40 0,004 0,040
15,0 0,60 0,006 0,060
20,0 0,80 0,008 0,080
25,0 1,00 0,010 0,10
8.3.3.3 Nickel contents between 0,08 % and 2,0 %

Into each of a series of 100 ml one-mark volumetric flasks, introduce the volumes of nickel standard
solution (5.5) shown in Table 2 and 25 ml of the iron base solution (5.7). Dilute to the mark with water
and mix.
Table 2 — Calibration for nickel contents between 0,08 % and 2,0 %

Nickel standard Corresponding nickel Corresponding nickel Corresponding

solution volume (5.5) mass concentration after nickel content in
final dilution the sample
ml mg mg/ml %

0 0 0 0
1,0 0,04 0,000 4 0,08
2,5 0,10 0,001 0,20
5,0 0,20 0,002 0,40
10,0 0,40 0,004 0,80
15,0 0,60 0,006 1,20
20,0 0,80 0,008 1,60
25,0 1,00 0,010 2,00

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 BS EN 10136:2019
EN 10136:2019 (E)

8.3.4 Adjustment of the atomic absorption spectrometer

Fit the nickel hollow-cathode lamp (see 6.2) to the atomic absorption spectrometer (6.2) as well as a
deuterium lamp (for the correction of the non-specific absorption), switch on the current and allow it to
stabilize. Adjust the wavelength in the region of 232,0 nm to minimum absorbance, if possible.
Following manufacturer's instructions, fit the correct burner, light the flame and allow the burner
temperature to stabilize. Taking careful note of the manufacturer's instructions regarding the minimum
flow rate of acetylene, aspirate the calibration solution of highest concentration of analyte and adjust
the burner configuration and gas flows to obtain maximum absorbance.
NOTE 1 Other suitable radiation sources can also be used.

NOTE 2 At the wavelength of 352,5 nm the signal-to-noise ratio is higher than at the wavelength of 232,0 nm.
Generally, use of the 352,5 nm line will lead to a better reproducibility. However, as the sensitivity at 352,5 nm is
less than the sensitivity at 232,0 nm, with some instruments the use of the longer wavelength will lead to higher
detection limits.

Evaluate the criteria given in 6.2 to ensure that the instrument is suitable for the determination.
WARNING — The manufacturer's recommendations should be closely followed and particular attention
is drawn to the following safety points:

a) the explosive nature of acetylene and regulations concerning its use;

b) the need to shield the eyes of the operator from ultraviolet radiation by means of tinted glass;

c) the need to keep the burner head clear of deposits because a badly clogged burner may cause a
flashback;

d) the need to ensure that the liquid trap is filled with water;

e) the need to always spray water between the test solutions, blank solution and/or calibration
solutions.

8.3.5 Spectrometric measurements

NOTE If pure metals and reagents have been used, the blank test and zero member will likely give very small
absorbance readings with a negligibly small difference.

8.3.5.1 Spectrometric measurement of the calibration solutions

Aspirate the relevant series of calibration solutions (8.3.3.2 or 8.3.3.3) depending on the expected nickel
content in succession into the flame and measure the absorbance for each solution. Take care to keep
the aspiration rate constant throughout the preparation of the calibration curve. Spray water through
the burner after each measurement.
NOTE For certain types of apparatus, it is preferable to use a solution containing the attack reagents in the
same concentrations as in the test solutions, instead of water.

Establish the calibration curve using the measured absorbances and corresponding analyte amounts.
Use appropriate spectrometer software or an off-line computer for regression calculations or prepare a
graphical representation.

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BS EN 10136:2019
EN 10136:2019 (E)

8.3.5.2 Spectrometric measurement of the test solutions

8.3.5.2.1 Preliminary spectrometric measurement

Carry out a preliminary measurement on the test solution (8.3.2.1 or 8.3.2.2) at the same time as the
spectrometric measurements are carried out on the calibration solutions (see 8.3.5.1). Estimate the
preliminary analyte amount by using the calibration curve (8.3.5.1).
8.3.5.2.2 Spectrometric measurement
8.3.5.2.2.1 Use of the calibration curve

Measure the absorbance of the blank test solution and repeat the measurements of the test solution;
derive the corresponding concentrations directly from the calibration curve.
8.3.5.2.2.2 Use of bracketing method

Carry out a second measurement on the test solution (see 8.3.5.2) by bracketing between the two
calibration solutions having nickel concentrations slightly higher and slightly lower than the estimated
nickel concentration of the test solution.

9 Expression of results
9.1 Use of the calibration curve
Calculate the nickel content (wNi), in percent (%), as follows:
ρ1
w Ni    × Dr × 100
=     (1)
m
where
ρ1 is the nickel concentration from the calibration curve, in milligram per millilitre;
m is the mass of the test portion, in gram;
Dr is the dilution ratio.
NOTE 1 For 8.3.2.2, Dr = 20.

NOTE 2 To adapt this calculation to a different test solution volume divide by 100 ml and multiply by the test
solution volume, in millilitres.

9.2 Use of bracketing method

Calculate the nickel content (wNi), in percent (%), as follows:
ρ2
w Ni    × Dr × 100
=     (2)
m
where
ρ2 is the nickel concentration, calculated using Formula (3), in milligrams per millilitre;
m is the mass of the test portion, in gram;
Dr is the dilution ratio.
NOTE 1 For 8.3.2.2, Dr = 20.

NOTE 2 To adapt this calculation to a different test solution volume divide by 100 ml and multiply by the test
solution volume, in millilitres.

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 BS EN 10136:2019
EN 10136:2019 (E)

S −  S 1
ρ 2 =   
ρ 3  ( −ρ × 0
+ ρ 4 3 )
S 2 −  S 1
(3)

where
ρ3 is the lower nickel concentration of the calibration solution used, in milligrams per millilitre;
ρ4 is the higher nickel concentration of the calibration solution used, in milligrams per millilitre;
S0 is the absorbance value of the test portion solution;
S1 is the absorbance value of the calibration solution corresponding to concentration ρ3;
S2 is the absorbance value of the calibration solution corresponding to concentration ρ4.

10 Test report
The test report shall contain the following information:
a) identification of the test sample;

b) test method used by reference to the present document;

c) results as well as the unit in which they are expressed;

d) any unusual characteristics noted during the determination;

e) any operation not included in this document or in the document to which reference is made or
regarded as optional;

f) date of the test and/or date of preparation or signature of the test report;

g) signature of the responsible person.

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BS EN 10136:2019
EN 10136:2019 (E)

Annex A
(informative)

Precision

A.1 General
Planned trials of this method were carried out by analysts from 6 to 19 laboratories: 2 to 5
determinations were carried out by each analyst on each sample.
From the results obtained the 95 % confidence limits have been calculated in accordance with
ISO 5725:1986 and are summarized in Table A.1.
Table A.1 — Statistical information
Certified Alloy type Nickel Number of Repeatability Reproducibility
reference content laboratories
material (%) (r) (R)
BCS 260/4 High purity iron 0,003 18 0,001 3 0,002 2
ECRM 077-1 Plain carbon steel 0,031 6 0,002 5 0,003 1
BCS 431 Plain carbon steel 0,069 18 0,003 7 0,009 6
--- Cast iron 0,070 17 0,002 4 0,010 2
--- Low alloy iron 0,080 19 0,007 6 0,011 8
--- Low alloy iron 0,112 16 0,007 3 0,016 1
ECRM 278-1 Cr-Mo steel 0,236 7 0,022 1 0,031 7
--- Low alloy iron 0,329 14 0,013 2 0,031 4
--- Low alloy iron 0,423 19 0,014 6 0,062 1
BCS 341 24% Cr steel 0,56 18 0,024 1 0,044 9
--- Ni-Cr-Mo-Cu iron 0,955 12 0,018 7 0,059 9
ECRM 177-1 Low alloy steel 1,015 7 0,019 5 0,029 7
BCS 225/2 Ni-Cr-Mo steel 1,43 18 0,040 9 0,051 3
BCS 406 Low alloy steel 1,69 18 0,046 6 0,090 3
--- Low alloy iron 1,708 15 0,041 8 0,096 1
BCS 410 Low alloy steel 2,04 18 0,059 8 0,078 4

A.2 Repeatability
The difference between two single results found on identical material by one analyst using the same
apparatus within a short time-interval will exceed the repeatability, r, not more than once in twenty
cases in normal and correct operation of the method.

A.3 Reproducibility
The difference between two single and independent results found by two operators working in
different laboratories on identical test materials will exceed the reproducibility, R, on average not more
than once in twenty cases in normal and correct operation of the method.

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Bibliography

[1] EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696)

[2] ISO 5725:1986 2, Precision of test methods — Determination of repeatability and reproducibility
for a standard test method by inter-laboratory tests

2 Withdrawn. (Replaced by the ISO 5725 series.)

13
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