Bsi bs en 00480 10 2009

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BRITISH STANDARD

Admixtures for
concrete, mortar and
grout — Test methods
Part 10: Determination of water
soluble chloride content

ICS 91.100.30

NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW

BS EN
480-10:2009


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BS EN 480-10:2009

National foreword
This British Standard is the UK implementation of EN 480-10:2009. It
supersedes BS EN 480-10:1997 which is withdrawn.
The UK participation in its preparation was entrusted to Technical
Committee B/517/3, Admixtures.
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.

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 January 2010

Amendments/corrigenda issued since publication
Date

Comments

© BSI 2010

ISBN 978 0 580 65577 7

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BS EN 480-10:2009

EUROPEAN STANDARD

EN 480-10

NORME EUROPÉENNE
EUROPÄISCHE NORM

July 2009

ICS 91.100.30

Supersedes EN 480-10:1996

English Version

Admixtures for concrete, mortar and grout - Test methods - Part
10: Determination of water soluble chloride content
Adjuvants pour béton, mortier et coulis - Méthodes d'essai Partie 10: Détermination de la teneur en chlorure soluble
dans l'eau

Zusatzmittel für Beton, Mörtel und Einpressmörtel Prüfverfahren - Teil 10: Bestimmung des wasserlöslichen
Chloridgehaltes

This European Standard was approved by CEN on 23 June 2009.
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 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 Management Centre has the same status as the
official versions.

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CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,

France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2009 CEN

All rights of exploitation in any form and by any means reserved
worldwide for CEN national Members.

Ref. No. EN 480-10:2009: E


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BS EN 480-10:2009
EN 480-10:2009 (E)

Contents

Page

Foreword ..............................................................................................................................................................3 
1

Scope ......................................................................................................................................................5 

2

Principle ..................................................................................................................................................5 

3
3.1
3.2
3.3
3.4

Apparatus ...............................................................................................................................................5 
pH meter .................................................................................................................................................5 
Electrodes ...............................................................................................................................................5
Additional apparatus .............................................................................................................................6
Reagents .................................................................................................................................................6 

4
4.1
4.2

Procedure ...............................................................................................................................................6 
Preparation of sample ...........................................................................................................................6 
Determination .........................................................................................................................................6 

5

Results ....................................................................................................................................................7 

6

Test report ..............................................................................................................................................8 

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2
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BS EN 480-10:2009
EN 480-10:2009 (E)

Foreword
This document (EN 480-10:2009) has been prepared by Technical Committee CEN/TC 104 “Concrete and
related products”, the secretariat of which is held by DIN.
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 January 2010, and conflicting national standards shall be withdrawn at
the latest by January 2010.
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 480-10:1996.
It has been drafted by Subcommittee 3 (SC 3) of TC 104 "Admixtures for concrete, mortar and grout".
This draft European Standard is part of the series EN 480 "Admixtures for concrete, mortar and grout – Test
methods" which comprises the following:


Part 1

Reference concrete and reference mortar for testing



Part 2

Determination of setting time



Part 4

Determination of bleeding of concrete



Part 5

Determination of capillary absorption



Part 6

Infrared analysis



Part 8

Determination of the conventional dry material content



Part 10 Determination of water soluble chloride content



Part 11 Determination of air void characteristics in hardened concrete



Part 12 Determination of the alkali content of admixtures



Part 13 Reference masonry mortar for testing mortar admixtures



Part 14 Determination of the effect on corrosion susceptibility of reinforcing steel by potentiostatic
electro-chemical test.

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This standard is applicable together with the other standards of the EN 480 series for testing admixtures in
accordance with the EN 934 series of standards.
The following amendments have been made to the 1996-09 edition of this standard:


editorial revision;



detailing of used reagents;



detailing of the procedure applied for Method 1 to Method 3.

3


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BS EN 480-10:2009
EN 480-10:2009 (E)

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

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4
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BS EN 480-10:2009
EN 480-10:2009 (E)

1

Scope

This draft European Standard specifies methods for determining water soluble halogens (except fluorides) in
admixtures.
The total water soluble halogen content is expressed as the chloride content.

2

Principle

The object of the test is to determine the content of chloride ions (including other halogen ions except
fluorides) in an admixture by precipitation of the chloride ions with a silver nitrate solution, according to the
reaction:

Cl − + Ag + → AgCl (solid)
The end point of this reaction is determined with the aid of a pH meter.
The volume of the sample required for this test has been calculated for an admixture of which the chloride
content is lower than 0,1 % by mass. If the chloride content is known, or can be assumed to be higher, the
admixture has to be diluted in a precise ratio before carrying out the test.

3

Apparatus

3.1

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pH meter

Either:
a)

a pH millivoltmeter in which case the graph is plotted point by point, or

b)

a recording pH millivoltmeter connected to an automatic burette.

3.2

Electrodes

Either:
a)

b)

a combination of two electrodes consisting of:
1)

an indicator: silver;

2)

a reference: mercuric sulphate (electrolyte KNO3) or calomel with agar gel (electrolyte KNO3); or

a combined electrode (indicator and reference) Ag - AgCl (electrolyte KNO3).

NOTE

Other electrodes such as ion selective electrodes may be used provided the results will be unaffected.

5


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BS EN 480-10:2009
EN 480-10:2009 (E)

3.3

Additional apparatus

3.3.1

Balance with an accuracy of 0,1 mg reading up to 200 g

3.3.2

20 ml burette graduated with accuracy of 0,05 ml

3.3.3

250 ml and 500 ml beakers

3.3.4

1 000 ml measuring flask

3.3.5

Heating device with a magnetic stirrer

3.3.6

10 ml, 20 ml and 50 ml graduated flasks

3.4

Reagents

All reagents shall be of analytical grade.
3.4.1

Concentrated nitric acid (HNO3)

3.4.2

Hydrogen peroxide (H2O2), 30 % by mass (110 volumes)

3.4.3

Sodium hydroxide solution (naOH), 33 % by mass

3.4.4

Distilled or demineralized water

3.4.5

Ethanol (C2H5OH)

3.4.6

Acetone (C3H7O)

3.4.7

Silver nitrate solution (AgNO3), pre-prepared 0,01 mol/l, normality N determined to ± 0,0001

4

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Procedure

4.1
4.1.1

Preparation of sample
Liquid admixture

From a liquid admixture a sample of (10 ± 1) g is weighed to 0,01 g and placed into a 250 ml or a 500 ml
beaker.
4.1.2

Powder admixture

From a powder admixture a sample (5 ± 1) g is weighed to 0,01 g. The sample is placed into a 250 ml or a
500 ml beaker.

4.2
4.2.1

Determination
General

Depending upon the composition of the admixture one of the following methods shall be used.

6
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BS EN 480-10:2009
EN 480-10:2009 (E)

4.2.2

Method 1

If the admixture does not contain constituents that will interfere with the test, such as lignosulphonates,
thiocyanates or reducing agents, dilute the sample or dissolve it and make the solution up to 100 ml with
distilled or demineralized water. Then add 80 ml of acetone followed by dilute nitric acid until the pH is (2,0 +
0,5) and carry out the titration of the chloride ions with the silver nitrate solution, recording the volume (V)
used to 0,05 ml.
Carry out a blank titration under the same conditions and record the volume (Vo) to 0,05 ml.
4.2.3

Method 2

If the admixture does contain, or can be assumed to contain lignosulphonate or reducing agents, the sample
shall be diluted or dissolved and made up to 100 ml with distilled or demineralized water. Then add 5 ml of
sodium hydroxide solution followed by 10 ml of hydrogen peroxide. This can cause an exothermic reaction.
In order to avoid loss of chloride ions, make sure that the pH remains above 8,5 by adding, if necessary, more
sodium hydroxide solution. Bring the solution very slowly to the boiling point by means of a heating device with
a magnetic stirrer and boil for 30 minutes1).
o

Leave the solution to cool to (20 + 2) C. Then add 80 ml of acetone followed by dilute nitric acid until the pH
is (2,0 + 0,5) and carry out the titration of the chloride ions using the silver nitrate solution, recording the
volume used (V) to 0,05 ml.
Carry out a blank titration under the same conditions and record the volume (Vo) to 0,05 ml.
4.2.4

Method 3

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NOTE

Carry out this test in an extraction cabinet to minimise the risk from the exothermic reaction and the escape of
hydrogen cyanide. The operator should wear suitable protective clothing.

If the admixture does contain, or can be assumed to contain thiocyanate, dissolve the sample if necessary
and dilute to 100ml using distilled or demineralised water then place the sample in a 500 ml beaker in order to
avoid losses by overflow.
Carefully add 5 ml of sodium hydroxide solution followed by 10 ml of hydrogen peroxide. This can cause an
extremely exothermic reaction. After this reaction has subsided, add again 10 ml of hydrogen peroxide and
repeat the addition three times. In order to avoid loss of chloride ions and minimise the escape of hydrogen
cyanide, make sure that the pH remains above 8,5 at all times by adding, if necessary, more sodium
hydroxide solution.
Heat the solution slowly to the boiling point and keep it boiling for 2 h. Leave the solution to cool slowly to (20
o
+ 2) C. Then transfer the solution into a 250 ml beaker using distilled or demineralized water to wash out the
500 ml beaker.
Add 80 ml of acetone followed by dilute nitric acid until the pH is (2,0 + 0,5) and carry out the titration of the
chloride ions using the silver nitrate solution, recording the volume used (V) to 0,05 ml.
Carry out a blank titration under the same conditions and record the volume (Vo) to 0,05 ml

5

Results

The results shall be expressed in % by mass.

1)

Some admixtures may foam while boiling. This may be reduced by the addition of ethanol.

7

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BS EN 480-10:2009
EN 480-10:2009 (E)

Chloride content wcl =

3,55 (V − Vo ) n
% by mass
m

where
V

is the volume of silver nitrate solution used in the test in millilitres;

Vo is the volume of silver nitrate solution used in the blank titration in millilitres;

6

N

is the normality of silver nitrate solution in mol per litre;

m

is the mass of the sample in grams.

Test report

The test report shall include at least the following information:
a)

Name or code of admixture tested (with information relating to its marking);

b)

Date of test;

c)

Name of the laboratory;

d)

Name of operator;

e)

Number of test standard (EN 480-10)

f)

Details of the equipment used;

g)

Method of test used (i.e. method 1, 2 or 3).; if method 2 or 3 has been used, the volume of hydrogen

peroxide, the boiling time and any other necessary comments shall be included;

h)

Origin of the sample and date when taken;

i)

Chloride ion content that shall be reported to the nearest 0,01 %.

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NOTE
All three methods give the total halogen ion content (except fluoride) as chloride. In the case of method 2, any
thiocyanate will also be included as chloride.

8
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BS EN 480-10:2009

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BS EN
480-10:2009

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