BRITISH STANDARD BS EN

196-5:1995

Methods of testing
cement —
Part 5: Pozzolanicity test for pozzolanic
cements

The European Standard EN 196-5:1994 has the status of a

British Standard
BS EN 196-5:1995

Cooperating organizations

The European Committee for Standardization (CEN), under whose supervision

this European Standard was prepared, comprises the national standards
organizations of the following countries:

Austria Oesterreichisches Normungsinstitut

Belgium Institut belge de normalisation
Denmark Dansk Standard
Finland Suomen Standardisoimisliito, r.y.
France Association française de normalisation
Germany Deutsches Institut für Normung e.V.
Greece Hellenic Organization for Standardization
Iceland Technological Institute of Iceland
Ireland National Standards Authority of Ireland
Italy Ente Nazionale Italiano di Unificazione
Luxembourg Inspection du Travail et des Mines
Netherlands Nederlands Normalisatie-instituut
Norway Norges Standardiseringsforbund
Portugal Instituto Portuguès da Qualidade
Spain Asociación Española de Normalización y Certificación
Sweden Standardiseringskommissionen i Sverige
Switzerland Association suisse de normalisation
United Kingdom British Standards Institution

This British Standard, having

been prepared under the
direction of Technical
Committee B/516, was
published under the authority
of the Standards Board and
comes into effect on
15 March 1995 Amendments issued since publication
© BSI 02-1999
Amd. No. Date Comments

The following BSI references

relate to the work on this
standard:
Committee reference B/516
Special announcement in
BSI News December 1992

ISBN 0 580 21525 3

 BS EN 196-5:1995

Contents

Page
Cooperating organizations Inside front cover
National foreword ii
Foreword 2
Text of EN 196-5 3
National annex NA (informative) Determination
of endpoints Inside back cover
National annex NB (informative) Committees responsible Inside back cover
National annex NC (informative) Cross-references Inside back cover

© BSI 02-1999 i
BS EN 196-5:1995

National foreword

This British Standard has been prepared under the direction of Technical
Committee B/516, Cement and lime. It is the English language version of
EN 196-5:1994 Methods of testing cement — Part 5: Pozzolanicity test for
pozzolanic cement published by the European Committee for Standardization
(CEN). EN 196-5 was drawn up by CEN Technical Committee 51, Cement and
building limes, as Part 5 of a series on testing cement which was originally
accepted by CEN on 15 November 1985 and made available on 12 May 1987. The
UK gave a negative vote at the final voting stage and, under the CEN Rules then
in force, was not obliged to implement this Part. A second formal vote was taken
in November 1992 when the UK again gave a negative vote but, under the CEN
Rules now in force, is obliged to implement this Part. This British Standard
supersedes clause 15 of BS 4550-2:1970 and this clause is now deleted.
In this Part the reference procedure requires the endpoint of titrations to be
determined visually. However, for the standardization of the EDTA solution and
the determination of the calcium oxide concentration a more satisfactory
photometric procedure using the same indicator exists in EN 196-2. In the UK
this photometric endpoint determination, as indicated in National annex NA, is
preferred as an alternative.
A British Standard does not purport to include all the necessary provisions of a
contract. Users of British Standards are responsible for their correct application.
Compliance with a British Standard does not of itself confer immunity
from legal obligations.

Summary of pages
This document comprises a front cover, an inside front cover, pages i and ii,
the EN title page, pages 2 to 6, an inside back cover and a back cover.
This standard has been updated (see copyright date) and may have had
amendments incorporated. This will be indicated in the amendment table on
the inside front cover.

ii © BSI 02-1999
EUROPEAN STANDARD EN 196-5
NORME EUROPÉENNE
December 1994
EUROPÄISCHE NORM

ICS 91.100.10 Supersedes EN 196-5:1987

Descriptors: Cements, pozzolans, chemical tests, determination of content, calcium hydroxide, EDTA, chemical reagents, apparatus

English version

Methods of testing cement — Part 5: Pozzolanicity test for

pozzolanic cement

Méthodes d’essais des ciments — Prüfverfahren für Zement —

Partie 5: Essai de pouzzolanicité des ciments Teil 5: Prüfung der Puzzolanität von
pouzzolaniques Puzzolanzementen

This European Standard was approved by CEN on 1994-12-12. CEN members

are bound to comply with the CEN/CENELEC Internal Regulations which
stipulate the conditions for giving this European Standard the status of a
national standard without any alteration.
Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the Central Secretariat or to any
CEN member.
This European Standard exists in three official versions (English, French,
German). A version in any other language made by translation under the
responsibility of a CEN member into its own language and notified to the
Central Secretariat has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium,
Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy,
Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and
United Kingdom.

CEN
European Committee for Standardization
Comité Européen de Normalisation
Europäisches Komitee für Normung
Central Secretariat: rue de Stassart 36, B-1050 Brussels

© 1994 Copyright reserved to CEN members

Ref. No. EN 196-5:1994 E
EN 196-5:1994

Foreword Contents
This European Standard was drawn up by Page
Technical Committee CEN/TC 51, Cement and Foreword 2
building limes, of which the secretariat is held by
1 Scope 3
IBN.
2 Normative references 3
The European Standard on the methods of testing
cement comprises the following Parts: 3 General requirements for testing 3
EN 196-1, Methods of testing cement — 4 Preparation of a cement sample 3
Part 1: Determination of strength. 5 Principle 3
EN 196-2, Methods of testing cement — 6 Reagents 3
Part 2: Chemical analysis of cement. 7 Apparatus 4
EN 196-3, Methods of testing cement — 8 Standardization of solutions 4
Part 3: Determination of setting time and
9 Procedure 5
soundness.
10 Results 6
ENV 196-4, Methods of testing cement —
Part 4: Quantitative determination of constituents. Figure 1 — Diagram for assessing pozzolanicity 6
EN 196-5, Methods of testing cement —
Part 5: Pozzolanicity test for pozzolanic cements.
EN 196-6, Methods of testing cement —
Part 6: Determination of fineness.
EN 196-7, Methods of testing cement —
Part 7: Methods of taking and preparing samples of
cement.
EN 196-21, Methods of testing cement —
Part 21: Determination of the chloride, carbon
dioxide and alkali content of cement.
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
June 1995, and conflicting national standards shall
be withdrawn at the latest by June 1995.
This European standard supersedes EN 196-5:1987.
According to the CEN/CENELEC Internal
Regulations, the following countries are bound to
implement this European Standard: Austria,
Belgium, Denmark, Finland, France, Germany,
Greece, Iceland, Ireland, Italy, Luxembourg,
Netherlands, Norway, Portugal, Spain, Sweden,
Switzerland, United Kingdom.

2 © BSI 02-1999

1 Scope
This European Standard describes the method of
measuring the pozzolanicity of pozzolanic cements
conforming to ENV 197-1. This standard does not
apply to Portland pozzolana cements or to
pozzolanas.
This method constitutes the reference procedure.
2 Normative references
This European Standard incorporates by dated or
undated reference, provisions from other
publications. These normative references are cited
at the appropriate places in the text and the
publications are listed hereafter. For dated
references, subsequent amendments to or revisions
of any of these publications apply to this European
Standard only when incorporated in it by
amendment or revision. For undated references the
latest edition of the publication referred to applies.
EN 196-2, Methods of testing cement —
Part 2: Chemical analysis of cement.
EN 196-7, Methods of testing cement —
Part 7: Methods of taking and preparing samples of
cement.
ENV 197-1, Cement — Composition, specifications
and conformity criteria — Part 1: Common cements.
ISO 385-1:1984, Laboratory glassware —
Burettes — Part 1: General requirements.
ISO 835-1:1981, Laboratory glassware —
Graduated pipettes — Part 1: General requirements.
ISO 3534:1977, Statistics — Vocabulary and
symbols.
3 General requirements for testing
3.1 Expression of masses, volumes and factors
Express masses in grams to the nearest 0,0001 g
and volumes from the burette in millilitres to the
nearest 0,05 ml. Express the factors of solutions,
given by the mean of three determinations, to three
places of decimals.
3.2 Number of tests
The number of tests shall be two (see also 3.3).
3.3 Expression of results
Express the results of the determinations in
millimoles per litre to the nearest 0,1 mmol/l.
Give the final result as the mean of two
determinations to one place of decimals.
1)
Definitions taken from ISO 3534.
2)
8 days are sufficient if the test is positive at this stage (see 10.2).
© BSI 02-1999
EN 196-5:1994
If the difference between two determinations is
more than twice the standard deviation for
repeatability, repeat the test and take the mean of
the two closest values.
3.4 Repeatability and reproducibility
The standard deviation of repeatability gives the
closeness of agreement between successive results
obtained with the same method on identical
material tested under the same conditions (same
operator, same apparatus, same laboratory and
short intervals of time1)).
The standard deviation of reproducibility gives the
closeness of agreement between individual results
obtained with the same method on identical
material but tested under different conditions
(different operators, different apparatus, different
laboratory and/or different time1)).
The standard deviations of repeatability and
reproducibility are expressed in millimoles per litre.
4 Preparation of a cement sample
Take a sample by the method described in
EN 196-7. Treat this laboratory sample as described
in EN 196-2.
5 Principle
The pozzolanicity is assessed by comparing the
quantity of calcium hydroxide present in the
aqueous solution in contact with the hydrated
cement, after a fixed period of time, with the
quantity of calcium hydroxide capable of saturating
a solution of the same alkalinity. The test is
considered positive if the concentration of calcium
hydroxide in the solution is lower than the
saturation concentration.
Experiment has shown that a mixture of 20 g of
cement and 100 ml of water at 40 °C achieves
equilibrium after a period of 8 days or 15 days2).
To evaluate the results it is therefore necessary to
know the solubility at 40 °C of calcium hydroxide in
a solution of which the alkalinity varies from 35 to
about 100 mmol OH– per litre.
6 Reagents
Use only reagents of recognized analytical quality
and freshly boiled water, distilled or of equivalent
purity, during the analysis.
6.1 Concentrated hydrochloric acid (HCl),
approximately 12 mol/l (ï = 1,18 g/cm3
to 1,19 g/cm3).
3
EN 196-5:1994
6.2 Dilute hydrochloric acid: about 0,1 mol/l. Using
the 50 ml precision burette (7.8), add 8,5 ml of
concentrated hydrochloric acid (6.1) to a 1 litre
volumetric flask (7.10) containing about 500 ml of
water. Then make up the volume with water.
6.3 Dilute hydrochloric acid (1 + 2): add 250 ml of
concentrated hydrochloric acid to 500 ml water.
6.4 Methyl orange (dimethylaminoazobenzene
p-sodium sulfonate).
6.5 Methyl orange indicator: dissolve 0,02 g of
methyl orange in water and make up to 1 000 ml.
6.6 Sodium hydroxide (NaOH).
6.7 Sodium hydroxide solution: dissolve 100 g of
sodium hydroxide in water and make up to 1 000 ml.
6.8 Calcium carbonate (CaCO3): dried at 110 °C.
6.9 Potassium chloride (KCl): dried at 110 °C.
6.10 Murexide (ammonium purpurate).
6.11 Murexide indicator: grind and mix 1 g of
murexide with 100 g of dry potassium chloride.
6.12 EDTA (disodium dihydrate salt of
ethylenediaminetetra-acetic acid).
6.13 EDTA solution about 0,025 mol/l :
dissolve 9,306 g of EDTA in water and make up
to 1 000 ml.
6.14 Sodium carbonate (Na2CO3): dried at 260 °C.
7 Apparatus
7.1 500 ml cylindrical polyethylene container of
about 70 mm diameter with a pressure seal-plug
locked by a screw plug.
7.2 Wide stem funnel
7.3 Porcelain Buchner funnel of 60 mm inner
diameter.
7.4 Filter paper with low porosity (mean pore
diameter of about 2 4m).
7.5 250 ml vacuum flask.
7.6 250 ml and 400 ml beakers.
7.7 50 ml and 100 ml precision pipettes (class A of
ISO 835-1:1981).
7.8 50 ml precision burette (class A of
ISO 385-1: 1984).
7.9 Uniform temperature enclosure controlled
thermostatically at (40 ± 0,5) °C.
7.10 500 ml and 1 000 ml volumetric flasks.
7.11 250 ml conical flask.
4 © BSI 02-1999
8 Standardization of solutions
8.1 Standardization of the EDTA solution
Weigh approximately 1 g of calcium carbonate (6.8)
to the nearest 0,0001 g and introduce into
the 250 ml beaker (7.6). Add approximately 100 ml
of water and, very carefully, 50 ml of dilute
hydrochloric acid (6.3) keeping the beaker covered
with a watch glass.
Stir with a glass rod and ensure that dissolution is
complete. Then transfer the solution into the 500 ml
volumetric flask (7.10), wash the beaker and watch
glass carefully with water, adding the washings to
the solution and make up the volume with water.
Pipette 50 ml of the solution into the 400 ml
beaker (7.6), dilute with approximately 150 ml of
water and add the quantity of sodium hydroxide
solution (6.7) necessary to achieve pH 13 (check the
pH by means of a pH meter or by indicator papers).
Add approximately 50 mg of murexide
indicator (6.11) and titrate by means of the
burette (7.8) against the EDTA solution (6.13) until
there is a steady colour change from purple to violet.
From the volume of EDTA solution used, calculate
the factor f1 of the EDTA solution by the formula:
(1)
where
f1 is the factor of the ETDA solution;
m1 is the mass of calcium carbonate, in
grams;
V1 is the volume of EDTA solution used for
the titration, in millilitres;
100,09 is the molecular mass of calcium
carbonate.
8.2 Standardization of the 0,1 mol/l solution of
hydrochloric acid
Weigh approximately 0,2 g of sodium
carbonate (6.14), add it to the 250 ml flask (7.11)
and dissolve it in 50 ml to 75 ml of water. Add five
drops of the methyl orange indicator (6.5) to the
solution and titrate with the 0,1 mol/l dilute
hydrochloric acid (6.2) until the colour changes from
yellow to orange.

Calculate the factor f2 of the hydrochloric acid
solution by the formula:
(2) the 250 ml beaker (7.6). Add five drops of methyl
where
f2 is the factor of the hydrochloric acid;
m2 is the mass of sodium carbonate, in
grams;
V2 is the volume of hydrochloric acid used
for the titration, in millilitres;
105,989 is the molecular mass of sodium
carbonate.
9 Procedure
9.1 Storage and filtration
Pipette 100 ml of freshly boiled water into the
polyethylene container (7.1) and place the sealed
container in the thermostatic enclosure (7.9) until
equilibrium is reached (about 1 h). Remove the
container from the thermostatic enclosure.
Pour (20 ± 0,01) g of the cement to be examined into
it, using the wide stem funnel (7.2). Immediately
seal the container hermetically.
Shake vigorously for about 20 s to avoid formation of
cement lumps. A horizontal rotary motion has to be
used to prevent any part of the sample or liquid
being thrown up and remaining separated from the
rest of the solution.
Replace the container in the thermostatic enclosure,
making sure that its base is perfectly horizontal so
that the deposited layer of cement has a uniform
thickness. Perform all operations outside the
thermostatic enclosure as quickly as possible
(in 1 min maximum) to avoid any appreciable
lowering in temperature of the contents of the
container.
After a period of 8 days or 15 days3) in the
thermostatic enclosure, remove the container and
filter the solution immediately under vacuum
through the Buchner funnel (7.3) into the vacuum
flask (7.5) using dry double filter paper (7.4) in less
than 30 s (to avoid absorption of atmospheric carbon
dioxide and any appreciable lowering in
temperature of the solution). Seal the vacuum flask
immediately and let the filtrate cool to room
temperature.
3)
8 days are sufficient if the test is positive at this stage (see 10.2).
© BSI 02-1999
EN 196-5:1994
9.2 Determination of the hydroxyl ion
concentration
Shake the vacuum flask (7.5) to homogenise the
filtrate and pipette 50 ml of the solution into
orange indicator (6.5) and determine the total
alkalinity with the dilute hydrochloric acid (6.2).
The titration end-point corresponds to the colour
change from yellow to orange.
Calculate the hydroxyl ion concentration [OH– ] by
the formula:
(3)
where
[OH– ] is the hydroxyl ion concentration in
millimoles per litre;
V3 is the volume of 0,1 mol/l hydrochloric
acid solution used for the titration, in
millilitres;
f2 is the factor of 0,1 mol/l hydrochloric acid
solution, in grams per millilitre.
9.3 Determination of the calcium oxide
concentration
To the same solution remaining after
completing 9.2, add 5 ml of sodium hydroxide
solution (6.7), approximately 50 mg of murexide
indicator (6.11) and titrate the calcium oxide with
EDTA solution (6.13) by means of the burette (7.8)
until there is a steady colour change from purple to
violet.
Before and after titration, the pH value of the
solution shall be at least 13, if not, add the requisite
amount of sodium hydroxide solution.
Calculate the calcium oxide concentration [CaO] by
the formula:
(4)
where
[CaO] is the calcium oxide concentration in
millimoles per litre;
V4 is the volume of EDTA solution used for
the titration, in millilitres;
f1 is the factor of the EDTA solution.
5
EN 196-5:1994

10 Results 10.2 Assessment of results

10.1 Expression of results
Plot the mean concentrations (see 3.3) of hydroxyl
ions and calcium oxide in the solution, obtained in
accordance with 9.2 and 9.3, as a point on Figure 1
which shows the saturation concentration of
calcium oxide in the solution as a function of the
hydroxyl ion concentration at 40 °C.
The cement satisfies the pozzolanicity test when the
point plotted is below the curve of calcium oxide
saturation concentration shown on Figure 1.
10.3 Repeatability and reproducibility
The standard deviation for repeatability is:
for calcium oxide : 0,2 mmol/l;
for hydroxyl ion : 0,5 mmol/l.
The standard deviation for reproducibility is:
for calcium oxide : 0,5 mmol/l;
for hydroxyl ion : 1,0 mmol/l.

Figure 1 — Diagram for assessing pozzolanicity

6 © BSI 02-1999
 BS EN 196-5:1995

National annex NA (informative)

Determination of endpoints
NA.1 Standardization of the EDTA solution
A standardized solution of EDTA (see 8.1) is required for the determination of the calcium oxide
concentration (see 9.3). This standard specifies that the titration endpoint is determined visually, using
murexide as the indicator. However, the method described in 4.53.3 a) of BS EN 196-2:1995 utilizes a
photometric endpoint detector (see 5.11 of that standard), set at 620 nm when murexide indicator is used,
and is the preferred technique for EDTA standardization in the UK.
NA.2 Determination of the calcium oxide concentration
The determination of calcium oxide in cement (see 9.3) is described in 13.14 of BS EN 196-2:1995. That
method also utilizes a photometric endpoint detector (see NA.1) and is the preferred technique for calcium
oxide determination in the UK.

National annex NB (informative)

Committees responsible
The United Kingdom participation in the preparation of this European Standard was entrusted by
Technical Committee B/516 Cement and lime, to Subcommittee B/516/4, upon which the following bodies
were represented.

British Cement Association

British Civil Engineering Test Equipment Manufacturers’ Association
British Ready Mixed Concrete Association
Cementitious Slag Makers’ Association
Department of the Environment (Building Research Establishment)
Electricity Association
Quality Ash Association
Society of Chemical Industry

National annex NC (informative)

Cross-references

Publication referred to Corresponding British Standard

ISO 3534:1977 BS 5532 Statistical terminology

Part 1:1978Glossary of terms relating to probability and general terms relating to
statistics

The British Standards corresponding to the European Standards referred to in the text are identical in
number and title with those given in clause 2.

© BSI 02-1999
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