BRITISH STANDARD BS EN

196-21:1992

Methods of testing
cement —
Part 21: Determination of the chloride,
carbon dioxide and alkali content of
cement
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The European Standard EN 196-21:1989 has the status of a

British Standard
 BS EN 196-21:1992

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 Standardiseringsraad
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
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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 the Technical Sector
Board for Building and Civil
Engineering, was published
under the authority of the
Standards Board and comes Amendments issued since publication
into effect on
15 June 1992
Amd. No. Date Comments
© BSI 01-1999

The following BSI references

relate to the work on this
standard:
Committee reference B/516
Draft for comment 87/10353 DC

ISBN 0 580 20680 7

 BS EN 196-21:1992

Contents

Page
Cooperating organizations Inside front cover
National foreword ii
Brief history 2
Foreword 2
Text of EN 196-21 5
National annex NA (informative) Test method for the
alkali content of cement to be used for the purpose of
calculating the reactive alkali content of concrete 16
National annex NB (informative) Committees responsible Inside back cover
National annex NC (informative) Cross-references Inside back cover
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© BSI 01-1999 i
 BS EN 196-21:1992

National foreword

This British Standard has been prepared under the direction of the Technical
Sector Board for Building and Civil Engineering. It is the English language
version of EN 196-21:1989 “Methods of testing cement; Determination of the
chloride, carbon dioxide and alkali content of cement”, published by the European
Committee for Standardization (CEN). EN 196-21 was drawn up by Technical
Committee 51, Cement and building limes, as Part 21 of a series on testing
cement which was accepted by CEN on 3 October 1989. The UK gave a negative
vote at the final voting stage, but under the CEN Rules now in force, is bound to
abide by the majority decision and to implement this Part. Thus, the European
test procedures have been introduced, where relevant, into the 1991 revisions of
British Standards for cement BS 12, BS 146, BS 4027, BS 4246, BS 6588 and
BS 6610. This British Standard supersedes clauses 16 and 17 of BS 4550-2 which
are withdrawn.
The UK negative vote on this Part was due to the fact that the European
methods for alkalis give values for Na2O equivalent of cement higher by
approximately 0.025 % absolute than those obtained using either the current BS
or the ASTM methods which have been used in the UK for the purpose of
calculating the “reactive” alkali content of concrete.
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In consequence, the BS 4550-2:1970 test method is retained as national annex

NA to be used only for the determination of the alkali content of cement for the
purpose of calculations to check compliance with the maximum value of 3.0 kg/m3
of Na2O equivalent for the reactive alkali content of a concrete mix, recommended
when aggregate containing an alkali reactive constituent, or when an unfamiliar
cement/aggregate combination, is in use (see 4.2.4 of BS 5328-1:19911)).
However, the European test method is called up in 8.3 of BS 4027:19912) which
specifies the maximum permitted alkali content of sulfate-resisting Portland
cement, type Low Alkali.
National annex NB gives the committees responsible for the UK participation in
the preparation of this standard.
National annex NC gives details of corresponding British Standards for
international standards referred to in the European Standard.
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 20, 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.

1) BS 5328 Concrete, Part 1:1991 Guide to specifying concrete

2) BS 4027:1991 Specification for sulfate-resisting Portland cement

ii © BSI 01-1999
 EUROPEAN STANDARD EN 196-21
NORME EUROPÉENNE
EUROPÄISCHE NORM December 1989

UDC 666.94:691.54:620.1:543.84

Descriptors: Cements, tests, chemical analysis, determination of content, chlorides, carbon dioxide, alkali

English version

Methods of testing cement; Determination of the chloride,

carbon dioxide and alkali content of cement

Méthodes d’essais des ciments; Détermination Prüfverfahren für Zement; Bestimmung des
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de la teneur en chlorures, en dioxide de carbone Chlorid-, Kohlenstoffdioxid- und Alkalianteils

et en alcalis dans les ciments von Zement

This European Standard was approved by CEN on 1989-06-16. 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

© CEN 1989 Copyright reserved to CEN members

Ref. No. EN 196-21:1989 E
 EN 196-21:1989
Brief history
This European Standard was prepared by Technical
Committee CEN/TC 51 “Cement”, the Secretariat of
which is held by IBN.
It is intended, in a revision of European Standard
EN 196-2, to adopt the methods of test in this
standard into EN 196-2, so that this standard will
then contain all methods of test required for the
chemical analysis of cement.
In accordance with the Common CEN/CENELEC
Rules, 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 and United Kingdom.
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2 © BSI 01-1999
Foreword
The standard EN 196 on methods of testing cement
consists of the following parts:
— Part 1: Determination of strength;
— Part 2: Chemical analysis of cement;
— Part 3: Determination of setting time and
soundness;
— Part 4: Quantitative determination of
constituents;
— Part 5: Pozzolanicity test for pozzolanic
cements;
— Part 6: Determination of fineness;
— Part 7: Methods of taking and preparing
samples of cement;
— Part 21: Determination of the chloride, carbon
dioxide and alkali content of cement.
 EN 196-21:1989

Contents
Page Page
Brief history 2 7.7 Expression of results 13
Foreword 2 7.8 Repeatability and reproducibility 13
1 Object and field of application 5 8 Determination of the alkali content
2 References 5 (alternative method) 13
3 General requirements for testing 5 8.1 Principle 13
3.1 Number of tests 5 8.2 Reagents 13
3.2 Repeatability and reproducibility 5 8.3 Apparatus 14
3.3 Expression of masses, volumes 8.4 Plotting the calibration curve 14
and results 5 8.5 Procedure 14
3.4 Determination of constant mass 5 8.6 Expression of results 14
3.5 Preparation of the cement sample 5 8.7 Repeatability and reproducibility 15
3.6 Reagents 5 Figure 1 — Apparatus for the
3.7 Volumetric glassware 6 determination of the carbon dioxide content
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(reference method) 8
4 Determination of the chloride content 6
Figure 2 — Apparatus for the
4.1 Principle 6
determination of the carbon dioxide content
4.2 Reagents 6 (alternative method) 10
4.3 Apparatus 6 Table 1 — Volumes of solutions for the
4.4 Procedure 6 preparation of calibration solutions and their
4.5 Expression of results 6 sodium oxide and potassium oxide
concentrations 12
4.6 Repeatability and reproducibility 7
Table NA.1 — Solutions for checking
5 Determination of the carbon purity of calcium solution 17
dioxide content reference method) 7
Table NA.2 — Solutions for calibrating
5.1 Principle 7
flame photometer 18
5.2 Reagents 7
5.3 Apparatus 7
5.4 Procedure 8
5.5 Expression of results 9
5.6 Repeatability and reproducibility 9
6 Determination of carbon dioxide
content (alternative method) 9
6.1 Principle 9
6.2 Reagents 9
6.3 Apparatus 9
6.4 Procedure 9
6.5 Expression of results 10
6.6 Repeatability and reproducibility 10
7 Determination of the alkali content
(reference method) 11
7.1 Principle 11
7.2 Reagents 11
7.3 Apparatus 11
7.4 Preparation of calibration solutions
and calibration graphs 11
7.5 Dissolution of the test portion 11
7.6 Procedure 12

© BSI 01-1999 3
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4
blank

1 Object and field of application
This European Standard lays down the methods for
the determination of the chloride, carbon dioxide
and alkali content of cement.
The standard describes the reference methods and,
in certain cases, an alternative method which can be
considered as giving equivalent results.
If other methods are used, their results shall be
shown to be equivalent to the results given by the
reference methods. In the case of a dispute, only the
reference methods are applicable.
This standard applies to cements and also to their
constituent materials, such as clinker and
blastfurnace slag.
2 References
EN 196-2, Methods of testing cement — Chemical
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analysis of cement.
EN 196-7, Methods of testing cement — Methods of
taking and preparing samples of cement.
ISO 3534-1977, Statistics — Vocabulary and
symbols.
3 General requirements for testing
3.1 Number of tests
The number of tests for the various determinations
(clauses 4 to 8) shall be two (see also 3.3).
3.2 Repeatability and reproducibility
The standard deviation of repeatability gives the
closeness of agreement between successive results
obtained with the same method on identical test
material, under the same conditions (same operator,
same apparatus, same laboratory and short time
interval3)).
The standard deviation of reproducibility gives the
closeness of agreement between individual results
obtained with the same method on identical test
material but under different conditions (different
operators, different apparatus, different
laboratories and/or different times3)).
The standard deviations of repeatability and
reproducibility are expressed in absolute percent.
3.3 Expression of masses, volumes and results
State masses in grams to the nearest 0,0001 g and
volumes from burettes in millilitres to the
nearest 0,05 ml.
Express the results, given by the mean of two
determinations, as a percentage generally to two
decimal places.
3)
As defined in ISO 3534.
© BSI 01-1999
BS EN 196-21:1992
If the results of two determinations differ by more
than twice the standard deviation for repeatability,
repeat the test and take the mean of the two closest
values as the result.
3.4 Determination of constant mass
Determine constant mass by making
successive 15 min ignitions followed each time by
cooling and then weighing. Constant mass is
reached when the difference between two successive
weighings is less than 0,0005 g.
3.5 Preparation of the cement sample
Before starting the determinations, treat the
laboratory sample, taken in accordance with
EN 196-7, as follows to obtain a sample for testing.
Take approximately 100 g of the sample using a
sample divider or by quartering. Sieve this portion
on a 150 µm or 125 µm sieve until the residue
remains constant. Remove the metallic iron from
the material retained on the sieve by means of a
magnet. Then grind the iron free fraction of the
retained material so that it completely passes
the 150 µm or 125 µm sieve. If this sample contains
particles of metallic iron such as those that may be
introduced accidentally during grinding, remove
these iron particles completely using a magnetic
stirrer in a suspension, for example in cyclohexane.
Transfer the sample to a clean dry flask with an
airtight closure and shake vigorously to mix it
thoroughly.
Carry out all operations as quickly as possible to
ensure that the sample is exposed to ambient air
only for the minimum time.
3.6 Reagents
Use only reagents of analytical quality and distilled
water, or water of equal purity, during the analysis.
Unless otherwise stated % means percent by mass.
The concentrated liquid reagents used in this
standard have the following densities (r)
(in g/cm3 at 20 °C):
hydrochloric acid 1,18 to 1,19
hydrofluoric acid 1,13
nitric acid 1,40 to 1,42
perchloric acid 1,60 to 1,67
phosphoric acid 1,71 to 1,75
sulphuric acid 1,84
5
 EN 196-21:1989
The degree of dilution is always given as a
volumetric sum, for example, dilute hydrochloric
acid 1 + 2 means that 1 volume of concentrated
hydrochloric acid is to be mixed with 2 volumes of
water.
3.7 Volumetric glassware
The volumetric glassware shall be of analytical
accuracy, i.e. class A as defined in the ISO
standards on laboratory glassware.
4 Determination of the chloride
content
4.1 Principle
This method gives the total halogen content except
for fluoride and expresses the result as Cl−. The
cement sample is decomposed with boiling dilute
nitric acid. Sulphides are oxidized into sulphates
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and do not interfere. The dissolved chloride is
precipitated using a known volume of a standard
silver nitrate solution. After boiling, the precipitate
is washed with dilute nitric acid and discarded. The
filtrate and washings are cooled to less than 25 °C
and the residual silver nitrate is titrated with a
standard ammonium thiocyanate solution using an
iron (III) salt as indicator.
4.2 Reagents
4.2.1 Concentrated nitric acid (HNO3).
4.2.2 Dilute nitric acid 1 + 2.
4.2.3 Dilute nitric acid 1 + 100.
4.2.4 Silver nitrate (AgNO3), dried at 150 °C.
4.2.5 Silver nitrate solution 0,05 mol/l.
Dissolve 8,494 g of silver nitrate in water in
a 1 000 ml volumetric flask and make up to the
mark. Store the solution in a brown glass flask and
protect it from the light.
4.2.6 Ammonium thiocyanate (NH4SCN).
4.2.7 Ammonium thiocyanate solution,
approximately 0,05 mol/l. Dissolve 3,8 g of
ammonium thiocyanate in water and make up
to 1 000 ml.
4.2.8 Ammonium iron (III) sulphate
(NH4Fe(SO4)2.12H2O).
4.2.9 Indicator solution. Add 10 ml of dilute nitric
acid 1 + 2 to 100 ml of a cold saturated solution of
ammonium iron (III) sulphate in water.
4.3 Apparatus
4.3.1 Balance, capable of weighing to the
nearest 0,0001 g.
4.3.2 10 ml burette, graduated to 0,1 ml.
4.3.3 Desiccator, containing anhydrous magnesium
perchlorate (Mg(ClO4)2).
6 © BSI 01-1999
4.3.4 Filter paper, coarse (pore diameter
approximately 20 µm).
4.3.5 5 ml pipette
4.4 Procedure
Weigh (5 ± 0,05) g of cement and place in a 250 ml
beaker, add 50 ml of water and, while stirring with
a glass rod, 50 ml of dilute nitric acid 1 + 2 (4.2.2).
Heat the mixture to boiling, stirring occasionally,
and boil for 1 min. Add 5 ml of silver nitrate
solution (4.2.5) by pipette (4.3.5) into the boiling
solution. Then boil for a maximum of 1 min and
filter through a filter paper (4.3.4) washed before
use with dilute nitric acid 1 + 100 (4.2.3) into
a 500 ml flask. Wash the beaker, glass rod and filter
paper with dilute nitric acid 1 + 100 until the
volume of the filtrate and the washings is 200 ml.
Cool the filtrate and washings to below 25 °C.
Add 5 ml indicator solution (4.2.9) and titrate with
the ammonium thiocyanate solution (4.2.7) shaking
vigorously until a drop of this solution produces a
faint reddish-brown colouration which no longer
disappears on shaking. Record the volume V1.
If the chloride content of cement exceeds 0,17 %, it
will be necessary to start the test again with a
smaller quantity of cement.
Carry out the same procedure with no cement
sample and record the volume, V2, of ammonium
thiocyanate solution used in the blank titration.
4.5 Expression of results
Calculate the chloride content (in %) from the
formula:
(1)
where:
m1 is the mass of the cement test portion;
V1 is the volume of the ammonium
thiocyanate solution used for the titration
of the test solution;
V2 is the volume of the ammonium
thiocyanate solution used for the titration
of the blank solution.
The mean of the two results shall be rounded to the
nearest 0,01 %.

4.6 Repeatability and reproducibility
The standard deviation of repeatability is 0,005 %.
The standard deviation of reproducibility
is 0,010 %.
5 Determination of the carbon dioxide
content (reference method)
5.1 Principle
The cement sample is treated with phosphoric acid
to decompose the carbonate present. The carbon
dioxide liberated is entrained in a current of carbon
dioxide-free gas or air through a series of absorption
tubes. The first two remove hydrogen sulphide and
water and the following then absorb carbon dioxide.
Two absorption tubes, each containing a granular
absorbent for carbon dioxide and anhydrous
magnesium perchlorate to retain the water formed
during the absorption reaction are weighed to
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determine the mass of carbon dioxide released.
5.2 Reagents
5.2.1 Copper sulphate (CuSO4.5H2O).
5.2.2 Copper sulphate solution, saturated.
5.2.3 Absorbent for hydrogen sulphide. Place a
weighed quantity of dried pumice stone with a grain
size between 1,2 mm and 2,4 mm into a flat dish and
cover with a volume of saturated copper sulphate
solution so the mass of the copper sulphate solution
is approximately half that of the pumice stone.
Evaporate the mixture to dryness, while stirring
frequently with a glass rod. Dry the contents of the
dish for at least 5 h in an oven at a temperature
of (155 ± 5) °C. Allow the solid mixture to cool in a
desiccator and store in an airtight bottle.
5.2.4 Absorbent for water, anhydrous magnesium
perchlorate (Mg(ClO4)2) with a particle size
between 0,6 mm and 1,2 mm.
5.2.5 Absorbent for carbon dioxide, synthetic
silicates with a particle size between 0,6 mm
to 1,2 mm4) impregnated with sodium hydroxide
(NaOH).
5.2.6 Concentrated phosphoric acid (H3PO4).
5.2.7 Concentrated sulphuric acid (H2SO4).
4)
The absorbent can be obtained ready for use.
© BSI 01-1999
EN 196-21:1989
5.3 Apparatus
5.3.1 Apparatus for the determination of the carbon
dioxide content. Figure 1 shows a typical piece of
apparatus which can be fitted with either a
cylindrical pressure container, a small electrical
compressor or a suitable suction pump which will
ensure an even flow of gas or air.
The gas (air or nitrogen) entering the apparatus has
previously had its carbon dioxide removed by first
being passed through an absorbent tube or tower
containing the carbon dioxide absorbent (5.2.5). The
apparatus consists of a 100 ml reaction flask (A)
fitted with a three neck adaptor. Neck B1 is
connected to a dropping funnel (O), neck B2 to a
connecting tube and neck C to a water cooled
condenser. The funnel onto B1 and the connecting
tube onto B2 are joined together by means of a
Y-piece (P), so that the carbon dioxide-free air can
flow either through the connecting tube or the
funnel by means of a Mohr clip (N). After the
condenser (L), the gas is passed through
concentrated sulphuric acid (D), then through
absorption tubes containing the absorbent for
hydrogen sulphide (5.2.3) (E) and for
water (5.2.4) (F) and subsequently through two
absorption tubes (G,H) which can be weighed and
which are three-quarters filled with the absorbent
for carbon dioxide (5.2.5) and a quarter with the
absorbent for water (5.2.4). The absorbent for
carbon dioxide (5.2.5) is placed upstream of the
absorbent for water (5.2.4) with respect to the gas
flow. Absorption tube (H) is followed by an
additional absorption tube (I), which also contains
the absorbent for carbon dioxide and water, which is
fitted in order to protect absorption tube (H) against
penetration by carbon dioxide and water from the
air.
The absorption tubes (G) and (H) which are to be
weighed may have, for example, the following sizes.
External distance between branches 45 mm
Internal diameter 20 mm
Distance between the lower part of 75 mm
the tube and the upper part of the
ground section
Tube wall thickness 1,5 mm
7
 EN 196-21:1989
5.3.2 Balance, capable of weighing to the
nearest 0,0001 g.
5.3.3 Electric oven, which can be set at (105 ± 5) °C
and at (155 ± 5) °C.
5.3.4 Desiccator, containing anhydrous magnesium
perchlorate (Mg(ClO4)2).
5.4 Procedure
Weigh (1 ± 0,05) g of cement and place it in a
dry 100 ml distillation flask. Connect the flask to
the apparatus (5.3.1) as shown in Figure 1, but
without the two absorption tubes (G) and (H). Pass
a current of carbon dioxide-free gas through the
apparatus for 15 min at approximately 3 bubbles
per second (bubble counter) via the connecting tube
onto B2 (branch onto B1, Mohr clip closed). Release
the Mohr clip and remove the gas supply from the
funnel (O). Add 30 ml concentrated phosphoric acid
into the dropping funnel and reconnect the gas
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supply to fill the funnel (O).
Figure 1 — Apparatus for the determination of the carbon dioxide content (reference method)
8 © BSI 01-1999
Condition the closed absorption tubes (G) and (H)
for 15 min in the balance case in order to achieve
temperature equilibrium. Then weigh each tube
separately. Shut off the flow of gas and attach the
tubes to the apparatus as shown in Figure 1.
Wear protective gloves when carrying out this
operation.
Then reopen the gas flow. After 10 min close
absorption tubes (G) and (H), remove them, place
them in the balance case for 15 min and then weigh
them separately. Repeat the passage of gas, removal
and weighing of absorption tubes (G) and (H) for as
long as is required for the results of two successive
weighings of a tube not to differ by more
than 0,0005 g.
If the change in mass of the absorption tubes (G)
and (H) remains greater than 0,0005 g, renew the
absorbents in tubes (E) and (F).

Attach the weighed absorption tubes (G) and (H) to
the apparatus, as shown in Figure 1.
Open the funnel tap and allow the phosphoric acid
to drop into the distillation flask (A). After the
reaction has ceased, heat the contents of the flask to
boiling and boil gently for 5 min. Maintain the gas
flow through the apparatus until the flask has
cooled to room temperature.
Close absorption tubes (G) and (H), remove them
and place them in the balance case for 15 min and
then weigh them separately. The increase in mass of
each tube is used for the calculation of the carbon
dioxide content (see 5.5).
The carbon dioxide is practically completely
absorbed by tube (G). If the increase in mass of
tube (H) exceeds 0,0005 g, renew the absorbent in
tube (G) and start the test again.
5.5 Expression of results
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Calculate the carbon dioxide content (in %) of the
cement from the formula:
(3)
where
m2 is the mass of cement test portion;
m3 is the increase in mass of tube G after
absorption;
m4 is the increase in mass of tube H after
absorption.
The mean of the two results shall be rounded to the
nearest 0,01 %.
If the carbon dioxide content calculated from
equation (2) is less than 0,5 %, repeat the
determination with a cement sample weighing 2 g.
5.6 Repeatability and reproducibility
The standard deviation of repeatability is 0,07 %.
The standard deviation of reproducibility is 0,10 %.
6 Determination of the carbon dioxide
content (alternative method)
6.1 Principle
The carbon dioxide is driven off by means of
sulphuric acid, absorbed by sodium hydroxide and
determined gravimetrically. Any hydrogen sulphide
present which may distort the results is absorbed by
mercuric (II) chloride.
5)
See page 6.
© BSI 01-1999
EN 196-21:1989
6.2 Reagents
6.2.1 Mercuric (II) chloride (HgCl2).
6.2.2 Absorbent for carbon dioxide, synthetic
silicates with a particle size between 0,6 mm
and 1,2 mm5) impregnated with sodium hydroxide,
(NaOH).
6.2.3 Concentrated sulphuric acid (H2SO4).
6.2.4 Dilute sulphuric acid 1 + 4.
6.2.5 Absorbent for water, anhydrous magnesium
perchlorate (Mg(ClO4)2) with a particle size
between 0,6 mm and 1,2 mm.
6.3 Apparatus
6.3.1 Apparatus for the determination of the carbon
dioxide content. The apparatus is shown in Figure 2.
A small vacuum pump is used to generate reduced
pressure in the apparatus.
6.3.2 Balance, capable of weighing to the
nearest 0,0001 g.
6.4 Procedure
Place (1 ± 0,05) g of cement into the 100 ml
distillation flask A of the apparatus (6.3.1). Mix this
cement with a small (about 50 mg) amount of
mercuric (II) chloride (6.2.1) using a spatula and
then add enough water to form a slurry. Connect the
flask to the ground joint of the dropping funnel (O).
Then draw air for 15 min through the apparatus,
passing the air through an absorption tower (J)
filled with absorbent (6.2.2) to remove the carbon
dioxide before the air passes into the flask.
After stopping the flow of air add 25 ml to 30 ml of
sulphuric acid (6.2.4) from the dropping funnel (O)
into the flask. Take care to ensure that some of the
acid remains in the dropping funnel as a seal.
Turn the vacuum pump on again, so that the current
of air carries the liberated carbon dioxide through
the condenser (L) and the first two absorption
tubes (F), filled with magnesium perchlorate (6.2.5)
for the purposes of drying the air, to the two
previously weighed absorption tubes (G) filled with
absorbent (6.2.2). An absorption tube (I) filled with
magnesium perchlorate (6.2.5) and
absorbent (6.2.2) is fitted after these tubes in order
to prevent penetration by the ambient air. A gas
washing bottle (D) filled with sulphuric acid (6.2.3)
is connected to this as a bubble counter.
9
 EN 196-21:1989

After about 10 min heat the contents of the flask to where

boiling and boil gently for 5 min. Maintain the air
flow through the apparatus until the flask has
m5 is the mass of the cement test portion;
cooled to room temperature. Close the taps and
remove the absorption tubes (G), place them in the m6 is the increase in mass of the absorption
balance case for 15 min in order to achieve tubes G after absorption.
temperature equilibrium and then weigh them.
The mean of the two results shall be rounded to the
6.5 Expression of results nearest 0,01 %.
Calculate the carbon dioxide content (in %) from the 6.6 Repeatability and reproducibility
formula:
The standard deviation of repeatability is 0,07 %.
The standard deviation of reproduciblity is 0,10 %.
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Figure 2 — Apparatus for the determination of the carbon dioxide content

(alternative method)

10 © BSI 01-1999

7 Determination of the alkali content
(reference method)
7.1 Principle
A butane or propane flame is used to excite the
alkalis to emit their characteristic spectrum in the
visible range. The emission is proportional to the
alkali content at low concentrations. The influence
of large quantities of calcium on the sodium
determination is suppressed by means of phosphoric
acid.
7.2 Reagents
7.2.1 General requirements
References to water mean distilled water or water of
the same degree of purity with an electrical
conductivity of approximately 2 µS/cm. Use
reagents of analytical quality (see also 3.6); their
alkali content shall be tested by means of this
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method. If the alkali content of a reagent
exceeds 0,01 %, the batch concerned is unsuitable
and shall therefore be replaced by another which
shall be tested in the same way.
7.2.2 Concentrated hydrochloric acid (HCl).
7.2.3 Dilute hydrochloric acid 1 + 19.
7.2.4 Concentrated phosphoric acid (H3PO4).
7.2.5 Dilute phosphoric acid 1 + 19; store this
solution in a polyethylene flask.
7.2.6 Concentrated nitric acid (HNO3).
7.2.7 Concentrated perchloric acid (HClO4).
7.2.8 Concentrated hydrofluoric acid (HF).
7.2.9 Sodium chloride (NaCl), dried at 105 °C to
constant mass.
7.2.10 Potassium chloride (KCl), dried at 105 °C to
constant mass.
7.2.11 Alkali stock solution. Weigh about 0,566 g of
sodium chloride and about 0,475 g of potassium
chloride, transfer them to a 1 000 ml volumetric
flask, add 100 ml each of dilute hydrochloric
acid 1 + 19 and dilute phosphoric acid 1 + 19,
dissolve and make up to the mark with water. This
solution contains approximately 0,300 g each of
Na2O and K2O. The actual contents can be
determined from the original quantities from the
following formulae:
K2O (in g/l) = 0,6138 × actual mass of
potassium chloride in g (4)
Na2O (in g/l) = 0,5303 × actual mass of
sodium chloride in g (5)
© BSI 01-1999
EN 196-21:1989
7.3 Apparatus
7.3.1 Balance, capable of weighing to the
nearest 0,0001 g.
7.3.2 Calibrated burettes.
7.3.3 Flame photometer, with which the intensities
of the sodium line at 589 nm and the potassium line
at 768 nm can be measured: a sufficiently stable
apparatus shall be used.
7.3.4 Platinum dish.
7.3.5 Filter paper, medium pore size (pore diameter
approximately 7 µm).
7.3.6 Platinum stirrer.
7.4 Preparation of calibration solutions and
calibration graphs
Prepare the calibration solutions using the
volumes of alkali stock solution, dilute hydrochloric
acid 1 + 19 and dilute phosphoric acid 1 + 19 listed
in Table 1. The volumes listed in lines 1 to 8 shall be
made up to 1 000 ml with water. Store these
calibration solutions in polyethylene bottles.
Spray the calibration solutions into the flame of the
flame photometer (7.3.3). Spray the blank
solution (Table 1, line 1) first and set the indication
on the apparatus to 0. Then spray the other
calibration solutions in the order of increasing
concentration (lines 2 to 8). Measure the intensities
for Na2O at 589 mm and for K2O at 768 nm.
Plot graphs of the measured intensities against the
corresponding concentrations of sodium oxide and
potassium oxide in the calibration solutions.
7.5 Dissolution of the test portion
7.5.1 Cements completely soluble in acid
(content of insoluble residue < 3 %)
Weigh 0,1 g cement into a 50 ml beaker, make into
a slurry with 10 ml of water and add 10 ml of dilute
hydrochloric acid 1 + 19. Warm the mixture until
the cement has dissolved, breaking any lumps down
with a glass rod. Filter the suspension through the
filter paper (7.3.5) into a 100 ml volumetric flask
washing through with boiling water. Wash the filter
paper and residue with boiling water until there is a
quantity of approximately 80 ml in the 100 ml
volumetric flask. Then allow the filtrate and
washing water to cool to ambient temperature.
Add 10 ml of dilute phosphoric acid 1 + 19 to the
solution, make up to the mark and mix thoroughly.
11
 EN 196-21:1989

7.5.2 Cements not completely soluble in acid 7.6 Procedure

Use the method described below where the content
of insoluble residue, determined in accordance with
clause 9 of EN 196-2, exceeds 3 %.
Weigh 0,2 g of cement into a platinum dish and
add 5 ml of concentrated nitric acid (7.2.6). Heat
the mixture, for example, on a hot-plate, and
evaporate to dryness. Disperse the residue from
evaporation in 5 ml of water, add 2 ml of
concentrated perchloric acid6) (7.2.7) and then
add 10 ml of concentrated hydrofluoric acid (7.2.8).
Heat the mixture and evaporate to dryness. Prevent
overheating by frequent agitation by means of the
platinum stirrer (7.3.6). Add 40 ml of water
and 20 ml of dilute hydrochloric acid 1 + 19 to the
residue from evaporation and heat until the residue
has dissolved. Filter the suspension through the
filter paper (7.3.5) into a 200 ml volumetric flask
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Spray the measuring solution produced as described
in 7.5.1 or 7.5.2 into the flame of the flame
photometer (7.3.3). Measure the intensity of the
sodium line at 589 nm and the potassium line
at 768 nm. Obtain the sodium oxide or potassium
oxide concentration in the solution respectively by
means of a linear interpolation from the intensities
and the associated concentrations of the calibration
solutions measured as described in 7.4.
Use the graphs plotted as in 7.4 to obtain the
sodium oxide and potassium oxide concentrations of
the solution in mg/l or use the intensities and the
associated concentrations of the calibration
solutions with the next higher and the next lower
intensity for the calculation as follows.
Calculate the sodium oxide (CNa2 O ) or potassium
oxide (CK 2 O ) concentration of the sample from the

washing through with hot water. Wash the filter

paper and residue with hot water until the 200 ml intensities l Na2O or lK2O respectively using the
volumetric flask contains a volume of following formulae:
approximately 150 ml. Then allow the filtrate and
washing water to cool to ambient temperature.
Add 20 ml of dilute phosphoric acid 1 + 19 to the (6)
solution, make up to the mark with water and mix
thoroughly.

(7)

Table 1 — Volumes of solutions for the preparation of calibration solutions and their sodium
oxide and potassium oxide concentrations
Line Alkali stock solution Dilute hydrochloric acid Dilute phosphoric acid Na2O and K2O
(7.2.11) 1 + 19 1 + 19 concentrations
ml ml ml mg/l
1 — 100,0 100,0 Blank solution
2 3,3 99,6 99,6 1,0
3 8,3 99,1 99,1 2,5
4 16,7 98,3 98,3 5,0
5 25,0 97,5 97,5 7,5
6 33,3 96,6 96,6 10,0
7 41,7 95,8 95,8 12,5
8 50,0 95,0 95,0 15,0

6) Perchloric
acid vapours form explosive mixtures with organic materials. It is therefore necessary to take special precautionary
measures when working with perchloric acid: the use of fume cupboards flushed with water and a general ban on the use of
organic substances in the same fume cupboard.

12 © BSI 01-1999

where
CBn is the concentration of the sodium oxide or
potassium oxide respectively in the
calibration solution having a lower
concentration than the measuring
solution in mg/l;
CBh is the concentration of the sodium oxide or
potassium oxide respectively in the
calibration solution having a higher
concentration than the measuring
solution in mg/l;
IBn is the intensity of the calibration solution
having a lower concentration than the
measured solution;
IBh is the intensity of the calibration solution
having a higher concentration than the
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measuring solution.
7.7 Expression of results
Calculate the contents of sodium oxide or potassium
oxide as percentages in the cement from the
following equations using the corresponding
concentrations as determined in accordance
with 7.6.
Na2O = 0,1 CNa 2 O
K2O = 0,1 CK2 O
where
CNa 2 O is the sodium oxide concentration of
the measuring solution as calculated
by formula (6) (in mg/l);
CK2 O is the potassium oxide concentration
of the measuring solution as
calculated by formula (7) (in mg/l).
The mean of the two results for each oxide shall be
rounded to the nearest 0,01 %.
The total alkali content, A, is obtained by converting
the potassium oxide content to equivalent sodium
oxide from the formula:
A = Na2O + 0,658 K2O
7)
These solutions can also be obtained made up ready for use.
© BSI 01-1999
EN 196-21:1989
7.8 Repeatability and reproducibility
The standard deviation of repeatability is:
0,01 % for the determination of Na2O;
0,02 % for the determination of K2O.
The standard deviation of reproducibility is:
0,02 % for the determination of Na2O;
0,03 % for the determination of K2O.
8 Determination of the alkali content
(alternative method)
8.1 Principle
Cements which are completely soluble are treated
with hydrochloric acid. Cements which are
incompletely soluble are first evaporated with
hydrofluoric acid/sulphuric acid. The alkali contents
of the solutions are determined by means of flame
photometry.
8.2 Reagents
8.2.1 Concentrated hydrochloric acid (HCl).
8.2.2 Dilute hydrochloric acid 1 + 9.
8.2.3 Concentrated hydrofluoric acid (HF).
8.2.4 Concentrated sulphuric acid (H2SO4).
8.2.5 Lithium chloride (LiCl); dried at 120 ºC.
(8) 8.2.6 Sodium chloride (NaCl); dried at 105 ºC to
constant mass.
(9)
8.2.7 Potassium chloride (KCl); dried at 105 ºC to
constant mass.
8.2.8 Stock solution7)
Dissolve 0,610 g of lithium chloride, 0,2542 g of
sodium chloride and 0,1907 g of potassium chloride
in water in a 1 000 ml volumetric flask and make up
to the mark.
8.2.9 Caesium chloride (CsCl).
8.2.10 Aluminium nitrate (Al(NO3)3.9H2O).
8.2.11 Buffer solution7)
Dissolve 50 g of caesium chloride and 250 g of
aluminium nitrate in water and make up
to 1 000 ml.
(10)
13
 EN 196-21:1989

8.3 Apparatus
8.3.1 Balance, capable of weighing to the
nearest 0,0001 g.
8.3.2 Electric oven, which can be set at (105 ± 5) °C
and at (120 ± 5) °C.
8.3.3 Flame photometer, capable of measuring the
intensities of the sodium line at 589 nm and the
potassium line at 768 nm. The flame photometer
shall be operated with a propane-air flame at a
relatively low temperature in order to avoid
distortion of the determination by alkaline earths.
8.3.4 Filter paper, medium porosity (pore diameter
approximately 7 µm).
8.3.5 Platinum dish.
8.3.6 Heating lamp.
8.3.7 Calibrated burette.
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Spray the calibration solutions into the flame of the
flame photometer (8.3.3). Spray the blank
solution 1 first and set the indication on the
apparatus to 0. Then spray the other
calibration solutions in order of increasing
concentration (2 to 7). Measure the intensities
for Na2O at 589 nm and for K2O at 768 nm. Plot
graphs of the measured intensities against the
corresponding concentrations of sodium oxide and
potassium oxide in the calibration solutions.
If a sufficiently stable photometer is used, it is only
necessary to establish the calibration curves from
time to time. However, the values measured for
flasks 1 and 7 shall be checked for each analysis.
8.5 Procedure
8.5.1 Cements completely soluble in acid
(content of insoluble residue < 3 %)
Weigh 0,2 g cement into the platinum dish (8.3.5),

8.4 Plotting the calibration curve

make into a slurry with 3 ml of water and evaporate
In the case of cements which are completely soluble
to dryness after adding 20 ml of dilute hydrochloric
in hydrochloric acid, evaporate 20 ml of hydrochloric
acid 1 + 9. Add hot water and 2 ml of dilute
acid 1 + 9 to dryness, and, in the case of cements not
hydrochloric acid 1 + 9 to the residue and filter
completely soluble in acid, evaporate 15 ml of
through the filter paper (8.3.4) into a 100 ml
hydrofluoric acid (8.2.3) and 5 ml of sulphuric volumetric flask which already contains 10 ml of the
acid (8.2.4) to dryness for the purposes of preparing buffer solution (8.2.11). Wash the residue with hot
the calibration solutions for each calibration point.
water until the volumetric flask is almost filled to
In both cases dissolve the residue from evaporation the mark. Then cool to 20 °C and make up to the
with 2 ml of hydrochloric acid 1 + 9 and 3 ml of mark with water.
water. Transfer the solution to a 100 ml volumetric
Measure the solution in the flame
flask and add 10 ml of buffer solution (8.2.11). Add photometer (8.3.3). The scale values read off in
the following quantities of the stock solution (8.2.8) conjunction with the calibration curves (8.4) give
to the individual volumetric flasks using the
the concentrations of K2O and Na2O in mg/l
calibrated burette (8.3.7).
respectively.
8.5.2 Cements not completely soluble in acid
Volumetric flasks 1 2 3 4 5 6 7
Weigh 0,2 g cement into the platinum dish (8.3.5).
Stock solution (ml) 0 1 3 5 10 20 30 Make into a slurry with 3 ml of water and evaporate
Then make up the volumetric flasks to the mark after adding 5 ml of concentrated sulphuric
with distilled water: acid (8.2.4) and 15 ml of concentrated hydrofluoric
acid (8.2.3). Evaporate to dryness under the heating
With an original quantity of sample of 0,2000 g, the lamp (8.3.6). Mix the residue with hot water
values measured for flasks 1 to 7 correspond to a and 2 ml of hydrochloric acid 1 + 9 and continue the
K2O and Na2O content of: procedure as described in 8.5.1.
8.6 Expression of results
Volumetric 1 2 3 4 5 6 7
flasks Calculate the content of alkali as a percentage for an
original sample weight of 0,2000 g.
Na2O 0 0,07 0,20 0,34 0,67 1,35 2,02
The mean of the two results for each oxide shall be
content (%) rounded to the nearest 0,01 %.
K 2O 0 0,06 0,18 0,30 0,60 1,20 1,81 Convert the potassium oxide content to the
content (%) equivalent sodium oxide content using formula (10).
State the sum of the sodium oxide values as the total
alkali content A.

14 © BSI 01-1999
 BS EN 196-21:1992

8.7 Repeatability and reproducibility

The standard deviation of repeatability is:
0,01 % for the determination of Na2O;
0,02 % for the determination of K2O.
The standard deviation of reproducibility is
0,02 % for the determination of Na2O;
0,03 % for the determination of K2O.
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© BSI 01-1999 15
 BS EN 196-21:1992
National annex NA (informative)
Test method for the alkali content of
cement to be used for the purpose of
calculating the reactive alkali content
of concrete
NA.1 General
This method of test is intended to be used for the
determination of the alkali content of cement only
for the purpose of calculating the reactive alkali
content of the concrete mix when aggregate
containing an alkali reactive constituent, or when
an unfamiliar cement/aggregate combination, is in
use (see 4.2.4 of BS 5328-1).
NA.2 Apparatus
NA.2.1 Simple flame photometers, burning natural
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or bottled gas and incorporating interchangeable
filters which select light of the appropriate
wavelengths, are generally suitable. Use in
accordance with the manufacturers’ instructions.
NA.3 Reagents
Prepare reagents by the following methods and
store in well stoppered rigid polyethylene or
polypropylene bottles.
NA.3.1 Sodium stock solution, (100 mg of Na2O
per litre.) Dry a quantity of analytical reagent
grade, or purer, NaCl at 250 °C, weigh 0.1886 g,
dissolve in water and dilute to 1 000 ml.
NA.3.2 Potassium stock solution, (100 mg of K2O
per litre.) Dry a quantity of analytical reagent
grade, or purer, KCl at 250 °C, weigh 0.1583 g,
dissolve in water and dilute to 1 000 ml.
8) There should be a suitably rated fuse in the circuit to protect the power supply.
9) With a current of 8 A approximately 20 g of aluminium is dissolved in 21/2 h. A lower current for a longer time is permissible.
16
NA.3.3 Aluminium solution, (20 g of Al per litre.)
Prepare this solution by dissolving super-purity
aluminium metal in nitric acid. The following
alternative methods have been found to be
convenient.
a) From a sheet of super-purity aluminium,
between 0.5 mm and 3 mm thick, cut two pieces,
one about 120 mm × 360 mm and the other
about 120 mm × 200 mm. Bend the larger piece
to fit inside a 2 l borosilicate glass or plastics
beaker, then bend the smaller piece to fit inside
the larger one. Near the middle of the top edge of
each piece drill a hole and twist a separate piece
of thick aluminium wire through each one to
make electrical connections. Clean both sheets by
washing successively in dilute hydrochloric
acid (1 + 9), water and industrial methylated
spirits. Allow the sheets to dry, weigh them
to ± 0.05 g and place them in the beaker ensuring
that they do not make contact with each other.
Cover the beaker with a plastics cover and take
the wire leads out through holes in the cover.
Place the beaker and contents in a fume
cupboard. Connect the lead from the outer
aluminium sheet to the positive terminal and the
lead from the inner sheet to the negative terminal
of a source of direct current which can be varied
from 0 V to 12 V8).
While stirring, add 200 ml of nitric acid
to 800 ml of warm water (about 50 °C) in a
separate beaker and transfer this solution to the
beaker containing the electrodes. Switch on the
power supply and increase the applied voltage to
obtain a current of about 8 A. When it is
considered that sufficient aluminium has
dissolved9), switch off and disconnect the power
supply. Remove, wash, dry and reweigh the
aluminium sheets together with any pieces that
may have become detached.
Calculate from the loss of mass the volume the
solution should occupy to contain 20.0 g of
aluminium per litre. Dilute to this volume with
water.
b) Cut sufficient super-purity aluminium sheet or
wire into small pieces and wash successively
with dilute hydrochloric acid (1 + 9), water and
industrial methylated spirits. Dry, weigh
out 20.0 g and transfer a little at a time, using
clean tongs, to a gently boiling solution of 100 ml
of nitric acid in 500 ml of water to which 2 ml of
saturated mercuric chloride solution have been
added.
© BSI 01-1999
 BS EN 196-21:1992

Maintain the volume at about 600 ml by
adding water as necessary. When all the metal
has dissolved, cool the solution and dilute
to 1 000 ml.
NA.3.4 Calcium solution, (6.3 g of CaO per litre.)
Weigh 11.25 g of analytical reagent grade, or purer.
CaCO3 into a beaker, cover with 100 ml of water and
carefully add 25 ml of HNO3. When solution is
complete dilute to 1 000 ml with water.
Test for sodium and potassium contamination by
the following procedure.
Prepare solutions A, B and C, using the quantities
given in Table NA.1.
With the sodium light filter in place, set the flame
photometer to read 0 with solution A and 100 with
solution B. Spray solution C and record the reading.
Replace the sodium light filter by the potassium
light filter and repeat the procedure. If readings
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NOTE 1 For instruments using internal standardization, add
the internal standard solution to the calibration solutions in
accordance with the manufacturers’ instructions.
NOTE 2 In some cases different Na 2O and/or K 2O
concentration ranges may be required. Should this be necessary,
modify the alkali contents of the calibration solutions as
appropriate but take the Al, Ca and HNO3 additions from
Table NA.2. The concentration of the scale-100 solution should
not exceed that recommended by the instrument manufacturer.
NA.5 Procedure
NA.5.1 Determination of alkalis soluble in
nitric acid
NOTE This procedure is generally applicable to cements, and
other materials, which are almost completely decomposed by
nitric acid solution.
Weigh out 500 mg of sample into a beaker made
from a material which will not yield sodium or
potassium to the solution. Add about 50 ml of cold
water, disperse the powder by swirling and add 5 ml

of nitric acid. Swirl again, add hot water to

higher than 2 for Na2O (0.1 mg/l) or higher than 1
about 150 ml total volume, bring to the boil and
for K2O (0.1 mg/l) are obtained reject the calcium
simmer for 5 min to 10 min. Cool, transfer to
solution and prepare a new solution using a purer
a 500 ml volumetric flask, add 50 ml of the
source of CaCO3.
aluminium solution, dilute to the mark with
NA.4 Calibration water10) and mix thoroughly.
Allow to settle and pour off sufficient solution for the
Prepare calibration solutions using the quantities
flame determinations. If necessary, centrifuge or
given in Table NA.2.
filter the solution before spraying.
With the sodium light filter in place set the flame
photometer to read 0 with scale-zero solution
and 100 with scale-100 solution. Record the
readings obtained for each of the intermediate
calibration solutions, checking and adjusting if
necessary, the 0 and 100 settings between each
reading. Replace the sodium light filter by the
potassium light filter and repeat the calibration
procedure. Construct the calibration graphs of
instrument reading against milligrams per litre of
Na2O or K2O.
Table NA.1 — Solutions for checking purity of calcium solution
Solution Sodium stock Potassium stock Aluminium Calcium HNO3 Water to make
solution solution solution solution
ml ml ml ml ml ml

A 0 0 50 0 5 500
B 25 50 50 0 5 500
C 0 0 50 50 5 500

10) Beforemaking up to volume, add, where necessary, sufficient of the standard calcium solution to bring the concentration of
calcium oxide in the diluted solution to approximately 630 mg/l, and, for instruments using internal standardization, also add
the internal standard solution in accordance with the manufacturer’s instructions.

© BSI 01-1999 17
 BS EN 196-21:1992

Table NA.2 — Solutions for calibrating flame photometer

Calibration Sodium Potassium Aluminium Calcium HNO3 Water to Equivalent
solution stock stock solution solution make concentrations
solution solution
Na2O K2 O

ml ml ml ml ml ml ml ml

Scale-zero 0 0 100 100 10 1 000 0 0

Scale-100 50 100 100 100 10 1 000 5 10
Nominal 20 5 10 50 50 5 500 1 2
Nominal 40 10 20 50 50 5 500 2 4
Nominal 60 15 30 50 50 5 500 3 6
Nominal 80 20 40 50 50 5 500 4 8
With the sodium light filter in place set the flame CAUTION. Perchloric acid fumes can react
photometer to read 0 with scale-zero solution explosively with some absorbent organic materials.
and 100 with scale-100 solution. Spray the sample Fume cupboards for use with perchloric acid should
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solution and take several readings, checking and
adjusting if necessary, the 0 and 100 settings
between each reading. Replace the sodium light
filter by the potassium light filter and again set the
flame photometer to read 0 with scale-zero solution
and 100 with scale-100 solution. Spray the sample
solution and take several readings, checking, and
adjusting if necessary, the 0 and 100 settings
between each reading.
If the sample gives a reading of more than 100 for
either sodium or potassium, transfer 50 ml of
sample solution to a 100 ml graduated flask, dilute
to the mark with scale-zero solution and re-spray. In
exceptional cases a further dilution may be
required.
NA.5.2 Determination of total alkalis
Weigh 500 mg of sample into a platinum basin and
remove carbon or carbonaceous matter by careful
ignition at 925 ± 25 °C. Cool the sample and
add 20 ml of water and 10 ml of perchloric acid. Stir,
add 20 ml of hydrofluoric acid and evaporate the
solution to strong fumes of perchloric acid in a
mechanically ventilated fume cupboard. Add 20 ml
of water and 5 ml of perchloric acid and again
evaporate until fumes just cease to be emitted.
never be constructed in wood but polyvinyl chloride
and stainless steel have been found suitable. All
materials of construction should be non-absorbent
and interior surfaces should be free from crevices
and ledges that could prevent complete washing
down. Guidance on the suitability of a fume
cupboard for use with perchloric acid should be
sought from the manufacturer.
Recommendations on all aspects of fume cupboards
are given in BS 725811).
Add 5 ml of nitric acid, cool and transfer to a 500 ml
volumetric flask. Add 50 mL of the aluminium
solution, dilute to 500 ml with water12) and mix
thoroughly. Then repeat the procedure in NA.5.1
from the second paragraph onwards.
Make blank determinations following the above
procedure with no sample present.
NA.6 Calculation
From the respective calibration graphs for Na2O
and K2O (see NA.4) convert flame photometer
readings to concentrations (milligrams per litre).
For the determination of total alkalis deduct the
blank determinations from the readings given
by Na2O and K2O respectively.
Where dilution of the original solution has been
made apply the dilution factor.

11)
BS 7258 Laboratory fume cupboards.
12) Beforemaking up to volume, add, where necessary, sufficient of the standard calcium solution to bring the concentration of
calcium oxide in the diluted solution to approximately 630 mg/l, and, for instruments using internal standardization, also add
the internal standard solution in accordance with the manufacturer’s instructions.

18 © BSI 01-1999
 BS EN 196-21:1992

Calculate the alkali contents as percentages by the

formula:
alkali oxide = 0.1D(C – B)
where

C is the concentration of alkali (milligrams

per litre);
B is the blank reading (when determining
alkalis soluble in nitric acid this is zero);
D is the dilution factor, i.e.
volume of diluted solution (ml)
------------------------------------------------------------------------------------
volume of aliquot taken (ml)
(where no dilution has been made this
equals one).
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© BSI 01-1999 19
 BS EN 196-21:1992

National annex NB (informative)

Committees responsible
The United Kingdom participation in the preparation of this European Standard was entrusted by the
Technical Sector Board for Building and Civil Engineering (B/-) to Technical Committee B/516 upon which
the following bodies were represented:

British Aggregate Construction Materials Industries

British Cement Association
British Precast Concrete Federation
British Ready Mixed Concrete Association
Cement Admixtures Association
Cementitious Slag Makers Association
Concrete Society
County Surveyors’ Society
Department of the Environment (Building Research Establishment)
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Department of the Environment (Property Services Agency)

Department of Transport
Federation of Civil Engineering Contractors
Mortar Producers Association
National Rivers Authority
Quality Ash Association
Society of Chemical Industry
Water Services Association of England and Wales

National annex NC (informative)

Cross-references

Publication referred to Corresponding British Standard

BS EN 196 Methods of testing cement

EN 196-2 Part 2:1992a Chemical analysis of cement
EN 196-7 Part 7:1992 Methods of taking and preparing samples of cement
ISO 3534:1977 BS 5532 Statistical terminology
Part 1:1978 Glossary of terms relating to probability and general terms relating
to statistics
a
In preparation.

20 © BSI 01-1999
Licensed copy:Hyder Consulting, 13/02/2005, Uncontrolled Copy, © BSI

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Licensed copy:Hyder Consulting, 13/02/2005, Uncontrolled Copy, © BSI

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